Manufacturing method of protein containing liquid for following separation by using one or more agent forming composite with protein

FIELD: food industry.

SUBSTANCE: invention relates to production method of liquid containing proteins (especially turbidity sensitive proteins) for following separation at least turbidity causing substances by using of filtering additives. Method includes adding of complexing agent able to create composite with at least several sensitive proteins of the liquid which leads to limitation of liquid residual turbidity obtained after filtration stage.

EFFECT: invention allows to increase beer turbidity stability.

21 cl, 13 dwg

 

The scope of the invention

The invention relates to a method for preparing a fluid that contains proteins. The invention, furthermore, relates to the addition of an agent that binds a protein complex, to the liquid to obtain a limited turbidity in the final fluid obtained after phase separation.

Prerequisites to the creation of inventions

The visual aspect of liquids, particularly beer, is a key element for most consumers. In this sense, transparency and visual perception of the physical stability of beer is an important aspect of quality. Brewers perform certain manufacturing operations, each of which affects the character and quality of the resulting beer product, including, for example, the transparency of the product, in particular, "turbidity", beer.

Turbidity is a visual manifestation of the physical instability of beer, and it can be divided into three main groups: biological, microbial and non-biological. Turbidity biological origin caused by the presence of carbohydrate (e.g., unmodified starch, dextrin), beta-glucan, pentosan and/or oxalate, which is the result of inappropriate technological operations. Microbial turbidity, which cannot be eliminated, caused by infection of beer yeast, bacteria, Pletnev the m fungi or algae and stem from inadequate hygiene beer. Turbidity non-biological origin, which is also characterized as a colloidal haze, are, of course, the biggest threat to the transparency of the beer, and the present description of the invention to the patent mainly focused on them.

The precursors responsible for the non-biological instability, are proteins and polyphenols, in particular tannins. The formation of complexes increasingly enhanced by such parameters as the concentration of the precursors, high temperature, presence of oxygen, heavy metals and aldehydes and shaking. You can also define the difference between "cold haze and permanent haze.

"Cold haze formed when beer is cooled to 0°C, and again dissolves when heated to 20°C or at room temperature. It is reversible complex formed in polyphenols with low molecular weight and protein, in which hydrogen bonds are weak.

The complexes of the particles are of submicron size (<1 μm), and can be regarded as the predecessors of " irreversible clouding".

"Irreversible clouding" is present in the beer even at 20°C and does not dissolve over time. Such irreversible clouding characterized by strong bonds, such as covalent bonds, between polymerizability polyphenols and be the kami. The size of the complex is equal to 5 µm.

The intensity of turbidity is determined by the EBU (Analytica-EBC, the Way 9.29, 5th edition, 1997), which includes the measurement of light scattering at an angle of 90° to the beam falls, calibrated using a titrated solution of units. On the scale of the EBU, which is linear, the intensity of turbidity of beer is classified as follows:

- Transparent <0.5 EMU

Almost transparent: 0.5 to 1.0 EMU

Little muddled: 1,0-2,0 EMU

- Slightly turbid: 2,0-4,0 EMU

Is misty: 4,0-8,0 EMU

- Very cloudy >8.0 EMU

Some studies show that the size of the particles in the turbidity can be determined by measuring at different angles. It is recognized that the scattering angle of 90° is more sensitive to small particles, reaching approximately 0.5 µm, and sensitive to such small particles, which are hardly perceived by the human eye. The so-called "opacity at 90° "some authors referred to as the "invisible haze. On the other hand, the scattering angle of 25° is not suffering from a similar visual effect and more sensitive to large particles larger than 0.5 µm. The so-called "turbidity at 25°" some authors referred to as the "visible haze.

There are other scales starting with a good map with scale EVS:

- NTU (Nevelama the historical Unit of Turbidity), where 4 NTU equivalent to 1 EMU

- ASBC (American Society of brewing Chemists industry), where 69 ASBC is equivalent to 1 EMU.

The main components of turbidity in beer are mainly proteins and polyphenols, but also small amounts of metal ions, oxalic acid and polysaccharides.

Proteins are the cause of most of the haze of nonbiological origin. Acidic proteins (especially those that have an isoelectric point of pH 5.0) is important in the formation of the cold dimness and probably formed during mashing malt. The study showed that the Proline in proteins that cause turbidity are important for interaction with polyphenols. These specific proteins are mainly from malt and largely responsible for the cold dimness. Only 2 mg/l of protein to cause turbidity of beer in 1 unit EMU.

Tannins are important compounds in brewing and highlights, in particular, as of hops (20-30%)and malt (70-80%). They have the ability to precipitate with proteins that are denatured during cooking of wort, to form a bundle, and to form in the cold wort cooling sucks. During postfermentation process (e.g., cold storage), when the temperature is 0°C, they participate in the formation of the cold dimness and n is reversible haze.

Polyphenols cover a wide range of plant substances that have generally aromatic ring with one or more hydroxyl groups. For convenience, the polyphenols can be divided into several classes, based on the chemical structure of molecules:

- flavonols, monomers with the structure of quercetin, usually present in hops glucoside,

the flavanols, monomers with the structure of catechin,

- flavonoids, oligomers of flavanols (e.g., procyanidin B3, prodelphinidin B3)

- proanthocyanidins, also called antiangina, molecules readily cleaved by acid forming substances, which are polymerized in the presence of oxygen to pigments called anthocyanidins,

- taneity, polymers of flavanoids, which are intermediates in the formation of tannins,

- tannins, polymers of flavanoids size sufficient to precipitate proteins.

Various studies have shown that Monomeric polyphenols have little influence on the formation of turbidity, while the dimers and trimers sharply increase the formation of turbidity. Polymerization of polyphenols contributes to oxygen. The oxidation reaction can kataliziruetsa such enzymes as polyphenoloxidase and peroxidase.

Polyphenols themselves contribute little to the formation of turbidity However the turbidity consists mainly of complexes of condensed polyphenols (tannins) and proteins.

The mechanism of interaction between sensitive proteins and polyphenols in the formation of opacities described by Caupona (Chapon), etc. and reproduced in figure 1.

According to the model Capone in a complex matrix, such as beer, proteins (B) and taneity (T) are in chemical equilibrium at all stages of the production of malt and beer, the product protein/tanaid (B-T) may be in soluble form or insoluble. Formation and stability of complexes of B-T presents the result as follows:

B+T ↔ B T → B-T

(soluble) (soluble) (insoluble)

Soluble B-T rather found in the form of insoluble nanocolloid particles, too small to cause an invisible haze. However, they serve as nuclei for the growth of particles and the subsequent development of turbidity.

This chemical equilibrium depends on the nature and structure of manoilov and proteins. In addition, the interaction probability is sensitive protein and tenaida depends on their relative concentrations, mixing, and temperature.

The reaction can be shifted to the left by removing or protein, or tanoda with low probability of deposition of B-T.

In contrast, the addition of high molecular weight protein or tannin will shift the equilibrium to the right, the compositions B-T become insoluble and precipitate. Cooling beer has the W the effect of compositions B-T, which become insoluble due to the increased interaction between B and I.

You can add the third dimension, which is represented by a time during which simple polyphenols (flavanols) polymerizers to manoilov and then tannins. The polymerization rate is positively correlated with the initial concentration of polyphenols and the presence of oxygen.

There are many factors that affect the quality of beer, and in particular, its initial and long-term turbidity.

Barley varieties differ significantly from each other in their content of polyphenols. Recognized also that seaside barley varieties contain more polyphenols than continental. Most of the polyphenols are concentrated in the husk, and so winter barley has a relatively high level in comparison with spring barley. It is recognized that 6-row barley has a higher level of polyphenols than 2-row barley. Some barley varieties with low content of antiangina have been developed and are now used to improve the colloidal stability of beer. As for protein, it is not so clear whether this barley low or high level causes the turbidity of the protein, also called sensitive protein. It is reasonable to assume that a positive correlation beings the et between the potential formation of turbidity and level of nitrogen in barley. The malting process can provide a higher colloidal stability, if the malt is highly modified. The level of polyphenol in raw materials has a greater impact on the future colloidal stability than the protein level.

Replacement of barley other sources of starch or carbohydrates (such as rice, corn, syrup) will lead to the dilution of all types predecessors opacities. On the other hand, supplements based on wheat will increase the risk of formation of turbidity due to high content sensitive to increased turbidity of the protein, polyphenol composition, the presence of glucans and pentosans, if any are present.

Hops also contains polyphenols, which are in General more polymerized in comparison with polyphenols, which are present in the malt. Fragrant species tend to have higher levels of polyphenols in comparison with bitter varieties.

Grinding malt - first operation, which can affect the colloidal stability when oxygen is present together with polyphenols, leading to polymerization and therefore increasing the amount predecessors cold cloud (for example, the potential deposition of polyphenols with proteins).

Mashing involves mixing malt grains and other cereals with water to use fermentation to decompose proteins into amino acids and peptides, and starch into fermentable sugars (e.g. glucose, maltose and maltotriose) and dextrins. Water quality plays an important role, and the brewer will use water preferably with low residual alkalinity, low pH of the pulp will contribute to the enzymatic cleavage of substances with high molecular weight. High pH water can enhance the extraction of polyphenol with negative consequences for the colloidal stability of beer. It is also important that the pulp has enough calcium to ensure the precipitation of the oxalate. Mash methods affect the colloidal stability. For example, digestion is better than insisting, because increased denaturing protein extraction of polyphenol and oxidation lead to a better removal of the predecessor of the cloud by precipitation when the temperature stratification of the liquid.

Filtration of the pulp is the process of separating the liquid and solid phases, where the liquid phase is called nikolenyi the wort. The pH value of the water after washing of brewer's grains, as mentioned before, is important for colloidal stability. In addition, high temperature and large volume of water contribute to greater extraction of polyphenols. The level of polyphenol has a negative effect on colloidal stability, if polyphenols are not removed before bottling, and on the other with the parties, positive impact if they are removed (e.g., sedimentation) before bottling.

Boiling the wort, I have to sterilize the wort, removing unwanted volatile substances and extragere and isomerize substances, giving the bitterness of hops, and by removing the excess protein denaturation. This operation lasts 60-90 minutes and is essential for colloidal stability in order to produce a well-formed hot sludge, representing the deposited material, which would otherwise destabilize beer. Hot sludge is removed by decantation, centrifugation or stahovanie. The intensity of the boil (the desired vaporization at least 5-6%), the pH of the wort (preferably 5,1-5,3), agitation (as far as possible) and oxidation (negative factor for the stability of the aroma, but positive for the existence of sediment due to the oxidation of polyphenols), are the most important parameters that affect the formation of hot sludge.

Before fermentation, the wort is cooled to fermentation temperature, saturated with oxygen (from air or pure oxygen), and introduce into it the yeast. Fermentation is the conversion using yeast fermentation of carbohydrates to ethanol, carbon dioxide and other compounds that give the beer a specific character. In zavisimost and on the strain of yeast fermentation temperature varies between 10°C and 15°C for bottom-fermented yeast and between 20°C and 30°C for yeast fermented. During the stage of fermentation is the adsorption of polyphenols on the surface of yeast cells. Cold wort proteins, polyphenols and carbohydrates tend to interact with each other and the formation of insoluble submicrometer particles called "refrigeration crap". The resulting colloids can serve as nuclei for further growth of the particles of the cold dimness during the cold maturation. As the formation and destruction of refrigeration sludge, and the connection of tannins with proteins represent major changes that positively affect the colloidal stability.

After the stage of fermentation beer is usually cooled to the extent possible low temperature without freezing (for example, to -2°C). Choledochojejunostomy stage is very important for the formation of "cold cloud". Any increase in temperature will again dissolved turbidity and, therefore, will return to the beer predecessors opacities together with the risk of development of turbidity later. At this stage it is desirable to apply an illuminating means capable of sedimentrelated formed dregs.

After fermentation it is necessary clarification, because beer is very turbid due to the presence of yeast complexes of protein/polyphenol and other insoluble material, which are responsible for turbidity in beer. After a long you is eriki at low temperatures the addition of beer brightening substances and centrifugation - here are some of the ways that brewers use to remove these substances.

Can precipitate cold turbidity should be removed from the beer or during beer filtration or before it. This operation can be done simple by eliminating completely or partially at least part of the precipitated material, what brewers call "cleaning", by a transfusion from the reservoir to the tank and/or by centrifugation of beer.

Temperature control is important because of its influence can again quickly dissolve predecessors opacities without the possibility of resultant deposition rates of the complex before filtering with the consequence that the predecessors will pass through the filter in a light beer.

Is filtering in industrial process stems not only from its direct impact on the filtered material, but also because it can represent one of the last features that the manufacturer has to have a direct impact on one or more critical factors of quality of the product. In brewing, for example, filtration is the final stage before packing beer, and so, perhaps, this is the last chance that the brewer has to directly affect (and in preventive and corrective sense) on the initial quality of the beer and IP is odya of its components, on its durability when stored.

As stated (Gottkehaskamp, L, Oechsle, D.,Precoat Filtration with Horizontal Filters.Brauwelt Int. 16, 128-131, 1998), the role of the filter in the brewing includes improvements associated with the initial transparency of beer (also dealing more or less with the predecessors of incipient turbidity) and factors that may adversely affect the change in flavor after packaging, primarily due to the removal of forming clouding substances, such as complexes of protein/polyphenol extracts of hops and the like; maintain biological stability by removing at least part postfermentation cargo microorganisms; and removal of other dissolved macromolecules, such as residual starches and dextrins, and α - and β-glucan.

According Donhauser, S., Wagner, D., Crossflow-Mikrofiltration von Hefe und Bier. Brauwelt 132, 1286-1300, 1992, alluvial diatomaceous earth was more than a half century as the dominant filtration additive in beer filtration. The diatomaceous earth was first used when filtering beer in the UK at the end of the 1930-ies, - but in the form in which it is currently commonly used in the United States, his adopted later, and then later introduced in the European brewing community.

While filtering through diatomaceous earth (also known in engineering as diatom Tomoe filtering or filtering "DE") is and can be a major, if not dominant, type of filter (alluvial) using an auxiliary filtering material for brewing and other industries (for example, filtering, DE is also used in wine-making), there are many new alternative filtration technologies. Were introduced technologies such as microfiltration with cross-flow and a variety of membrane methods, although no one as yet has not received wide distribution. (See for example, Meier, J., Modem Filtration - Overview of Technology and Processes, Brauwelt Int. 11, 443-447,1993).

The term "filtering" is usually understood as the mechanical separation of different liquid/solid components of a balanced mixture of both. These "suspensions" (used here in the broad sense of the word, suspension does not mean any individual particle sizes, but only that the particle traversed by the flow of liquid or suspended in the fluid flow) flow through porous auxiliary filtering material or filter additive, and at least some of the particulates are trapped on or in the filter material, while at least partially purified liquid (i.e. the "filtrate") comes out of the filtration plant. Epiinger (Epiinger, N.M., Die Bierfiltration, Brauwelt 132, 427-428, 1992) indicates that there are many clearly different from other ways of separating the solid phase used is eat filtration media:

surface or sediment filtration (sometimes also called alluviale), in which the solid material in suspension together with the added number of filter additives (e.g., DE) delayed the supporting surface on which is formed sediment filter (layer). Here separation (separation) of the solid phase occurs only in the surface sediment;

- deep or layer-based filtering: filtering medium consists mainly of a thick layer with pores inside that trap solid particles; and,

- sieve filtration: particles that are larger than the pores of the filter are held on the surface of the material.

The invention and its elements primarily focused on the first of the above methods of filtration. In DE powder filter (alluvial) DE filter, the additive is introduced into the beer stream a little above the point where it accumulates on the lock screen. Filtering beer starts when the upper filtering layers installed and recirculating the fluid is clear. The beer stream that carries DE together with yeast and other suspended solid particles, forms a then largely "incompressible" mass, called "filter cake". To prevent clogging of the small pores of the filter and get a long filtration cycles filtrowa the additive is continuously metered in unfiltered beer as "boot material.

The porous layer provides a surface that captures solid particles, removing them from the beer, and the retaining layer "incompressible" only in the sense that beer may continue to pass through these pores, whereas the filter residue is formed, and the working pressure continues to increase as ongoing operating cycle of filtration. For the purposes of mathematical modeling of the parameters of the pass-through stream sediment is considered as compressible (see below the discussion of porosity). The continuing supply of filter additives (called "boot material") are continuously carried out by adding it into the beer stream to maintain the permeability of the sediment (layer). Not all particles will be trapped on the surface; some, especially the smallest, the particles penetrate into the filter sediment and will be captured - this process is called "depth filtration". Depth filtration is not as effective as a surface filter, but still is an important mechanism of filtration using filter additives. Despite this inefficiency, it is prudent in all cases to start phase of the boot material of the filtration cycle with high standards and dosing to decrease with decreasing differential pressure on the filter layer. The interruption of the boot is about material will cause premature contamination of the surface of the filter cake, that will lead to an undesirable reduction of the loop filter.

For alluvial filtration processes in General (and including, in particular, those processes in which the use diatomaceous earth as a filter additive) normal industrial filters can be classified according to the following typology: 1) frame filters; 2) horizontal filters; and 3) candle filters.

In this regard, it should be noted that frame filters are considered "open" and not a fully automated system. Horizontal filters and candle filters - closed and fully automated (Kolcyk, M., Oechsle, D., Kesselfiltrationssysteme fur die Anschwemmfiltration. Brauwelt 139, 294-298, 1999; and, Kolcyk, M., Vessel Filter Systems for Precoat Filtration, Brauwelt Int. 17, 225-229, 1999). To that frame filters are usually labor intensive and relatively clean, has led to systems that are based on two other types of filtering that are prevalent in industrial applications (see Leeder, G., Comparing Kieselguhr Filter Technologies, Brew. Dist. Int. 21, 21-23, 1990).

To cause the suspension to flow efficiently through the filter material (i.e., to compensate for the pressure drop in the fluid flow to the filter material), using the pressure drop (typically by a pump operating against the current) in the work of most filtration systems.

In the case of a hypothetical "ideal" filter through the filter residue with laminariaceae through an incompressible porous filter sediment incompressible Newtonian fluids, the law Darcy:

Under these conditions it follows that the specific flow and proportional to the applied pressure difference dp and inversely proportional to the dynamic viscosity of the filtered fluid ηL. In other words, the above used the differential pressure and the lower the viscosity, the higher filtrate flux per unit surface area (specific flux). In addition, the flow also affects the filtration resistance R, which, in turn, depends on the hydraulic resistance of the sediment (layer) and filter additives.

Eslinger indicates that most often, in practical reality, specific gravity and, therefore, the resistance of the filter cake (layer) is extremely increased.

In addition, with regard to the porosity of the filter layer, in fact, the statistical distribution of pore size plays an important role in filtering.

The law of Hagen-Poisseuille describes laminar flow through parallel cylindrical capillaries:

where the porosity ε, the capillary diameter d0and the height of the filter hk.

However, in reality, a function of porosity adequately described by equation Carmen-Kozeny (Carman-Kozeny), which according to the detailed analysis of Eslinger (Epiinger) demonstrates that the impact of any given change of porosity on spending the fluid is actually very high. For example, if the porosity decreases from 40% to 30%, the specific flow is reduced by 70%. The General differential equation for the filter layer will be

where the resistivity of the sediment (layer) α and the resistance of the filtering medium r0.

In practice, almost all filter layers more or less compressible, especially those that come from fine-grained and easily deformable solids.

For practical actions the Darcy law can also be written as (8)

where the permeability of the layer C.

From equation {4}, it follows that alluviation filter will behave as follows: when the specific flow rate is doubled, the pressure drop is doubled, respectively. However, because the dosage of the boot material should also be doubled to maintain the permeability of the layer for the passage of flow, the layer height is doubled. Therefore, to double the specific liquid flow rate pressure drop increases four times. However, in order to maintain the same gradient of the pressure drop during filtration when the specific flow rate increases, the rate of dose diatomaceous earth must increase by the square of the new specific fluid flow relation to the initial. It is clear that the running time of the filter is inversely proportional to the kolichestvo dosed diatomaceous earth (see for example, Leeder, G., The Performance of Kieselquhr Filtration - Can It be Improved?, Brew. Dist. Int. 23, 24-25, 1992).

Alluvial filtering further complicated options available equipment (see Leeder, G., Comparing Kieselguhr Filter Technologies, Brew. Dist. Int. 21, 21-23, 1990).

Horizontal filter (HF) consists of a monolithic vessel with two attached horizontal metal plates. The body consists of a plate filter element attached to the Central hollow shaft and able to rotate due to the drive device. The sheet usually consists of a carrier Board that supports strong coarse mesh, which, in turn, supports a fine mesh with holes, for example, only 70 µm. These elements are clamped between the peripheral terminals.

Unfiltered beer can enter a horizontal filter in two different ways depending on whether the horizontal filter filter old type S or a later type Z.

The old design has the inlet on the top metal plate and the distribution system (S-type). A mixture of diatomaceous earth and beer spread out between the wall of the vessel and the filter element over the entire height of the filter. The filtrate accumulated in each plate of the filter and is available through the hollow shaft. S-shaped horizontal filter is characterized (as an example) bandwidth is sposobnostey diatomaceous earth in 7 kg/m and a maximum working pressure of 7 bar.

Later horizontal filter Z-type was designed to obtain a more uniform distribution of unfiltered beer by providing a separate power connection filter to each element of the filter with one inlet distribution manifold. As a result of this location of the entrance, distance, covering beer, is significantly reduced. Even in the case of horizontal filter Z-type, where the filters are equipped with sheets of large diameter, the maximum distance of flow is less than 75 see This design allows even distribution of filter additives on the sheet and therefore promotes the formation of relatively more homogeneous filter layer with a more uniform height. Gottheim (Gottkehaskamp) and others (above) revealed in the trials the average height of the layer of 12 mm with a standard deviation of 0.8 mm to more than 700 checkpoint.

A short distance flow in horizontal filters filter Z-type reduce the redistribution filter additives in an unfiltered beer in the upper part of the base strip or sheet. As a result of the filter layer is very (relatively speaking) homogeneous along the entire filter, the quality of the leachate much better and the amount of soil can be minimized. In addition, the space between any two adjacent elementarily you then much better use, that, in turn, allows large volumes of produced beer, in any given cycle. Such "long cycles" are, in turn, to more economical operation of the filter.

The whole design of the horizontal filter Z-type implies that damage to the filter element through overloading of the filter diatomaceous earth is unlikely. For example, as reported, download filter 11 kg/m possible, and to cope with such high loading capacity, a horizontal filter Z-type is also designed for operating pressures in bar 9, for example. The advantage of operating at such pressures include the fact that it does not adversely affect the quality of the filtrate (again, see Gottkehaskamp and others above).

A typical candle filter consists of a cylindrical tank, which is divided by a plate on the filter and holding area. Another plate above the separating plate is used to filter the collection. The cylindrical part of the tank enters into the region of the retained material, while the conical part ensures the proper distribution of raw diatomaceous earth and collects and produces exhaust diatomaceous earth at the end of filtration. Unfiltered beer is in the tank with the lower end of the conical part. Cylindrical candles set ve is cicalino to the middle plate. They occupy approximately 55-75% of the volume of the tank. Modern candle includes trapezoidal spiral wire with eight coils, welded to a rectangular reference beams. Hole candles asymmetrically in the fact that from the outside it is 70 µm, while inside it a few more that avoids the risk of clogging. The surface of the filter element is approximately 0.1 to 0.2 m To obtain a large surface filter should be set several hundred candles (for example, 500 candles for surface 100 m). Candle filter can take the precipitate in an amount of about 7 kg of kieselguhr/m

The design of the candle filter is often designed for working pressure max 7 bar. Since there are no moving parts in the candle filter, it is called static filter system.

And a horizontal filter, candle filter are tank filter systems, which exhibit similarities. However, there are some obvious differences, which are described below.

As for the stability of the filter layer, the horizontal filter provides horizontal filter layer, which is resistant due to gravity. Therefore, filtering is not performed is interrupted when disconnecting the unit, because the filter layer may not fall off the plate. When fil is the radio with candle filter vertical filter layer should be stable differential pressure, created by the pump. Off pump leads to slippage of sediment (layer).

As for priming, candle filter should be prepared for priming immediately before the beginning of the filtration cycle. Otherwise, the filter must be kept in the working cycle, in which energy is used. In the case of horizontal filtering, the preparation of the filter can be replaced already the day before filtering, as the primer is sustainable even without cyclical work, and filtering can be started at any time, when priming is completed.

In respect of beer it is generally accepted that the presence of yeast is limited to one yeast cell per litre and turbidity is limited to 0.5 EMU with a maximum of 0.8 EMU (see the section on the measurement of turbidity) depending on the specifications of the beer. DE can be used and is used to supply these kinds of specifications of the finished product. However, there are three fundamental problems associated with the use of DE. First of all DE affects the quality of beer as it is porous particles, which cause the increase of oxygen in the beer. It also naturally contains small amounts of metal ions, which are catalysts for oxidation reactions. In addition, this material represents a health risk during treatment (e.g., inhalation). Recently this is not the Ki was added to the growing problem of placing the exhaust filter additives and the associated costs of waste disposal.

In "the Practical brewer" (Practical Brewer), 1993, master brewers Association of America (Master Brewers Association of America), indicates that reactions leading to the formation of insoluble substances, can lasteven after filteringfor solving this problem can be used a number of stabilizing treatments. Despite the filtration efficiency DE, occurs frequently, although not always, and in different degrees, and the additional need to further strengthen the colloidal stability of beer. Essentially, there are several strategies to improve the colloidal stability of beer: remove polyphenols, removal of proteins or delete parts of each. Low temperature and low oxygen levels are prerequisites for good brewing technology in relation to colloidal stabilization (and the absorption of oxygen from the DE may be contributing to the problem in this regard too).

Remove polyphenols can be achieved through adsorption on polyvinylpolypyrrolidone (PVPP) (or by deposition by means of formaldehyde, which is for security reasons, food is not allowed everywhere technology). Due to its chemical structure PVPP preferably interacts with polymerized polyphenols, flavanoids and tannins through hydrogen bonds and weak electrostatic forces. The affinity of polyphenols is PVPP above, than active to the dimness of the proteins in the beer, due to the fact that PVPP has more active sites than whites. In addition, the interaction between polyphenols and PVPP stronger and faster than between polyphenols and proteins. PVPP exists in two forms, single use PVPP, which is smaller (that is, the set of balanced small particles)than the regenerated form. PVPP disposable has a high surface/mass ratio, is dosed to the filter is usually in amounts of between 10 and 30 g/HL and removed during the stage filtering on the updated portion of the filter layer. The regenerated PVPP usually dosed continuously into the flow of light beer at the rate of 25 to a maximum of 50 g/HL and collected on a special filter (that is, separately and independently from the DE filter, where it can be restored by contact with sodium hydroxide solution. This is the most economical method for the production of strong beer, with a shelf life of up to 6 months.

Removal of proteins is possible using adsorption on silica, silicate or bentonite by deposition gallotannin or by enzymatic hydrolysis. Silica gel adsorbs proteins in its surface, and performance depend on pore size, particle size, surface area and permeability. Silica gel removes preferably form the s opacity protein, because it recognizes and interacts with the same centers on active opacity proteins, and polyphenols. Silica gels, there are three solid forms: the hydrogel with a humidity of 70%, the xerogel with 5%humidity and a modified hydrogel with a humidity of 30-35%. Dosage of silica gel can be used during cold maturation in relation to 50 g/HL or fluid before stage filtration in the ratio of 20-100 g/hl. higher rate of dose may adversely affect the stability of the foam. Silica exists in liquid form, which is colloidal silica, hereinafter called kremnezem to distinguish from the silica gel, which is a powder. Due to their large surface area, crumpsall has a high adsorption efficiency as tools for active opacity proteins. Crumpsall acts as well as acts and silica gel, and the particles have the ability to cross-linking and the formation of hydrogels with active opacity proteins, they localroot, forming eventually precipitate. Crumpsall may be included in the mash or beer. Add to a hot mash is carried out at a rate of 40-70 g/HL of congestion. When crumpsall add in beer, Sol is injected directly into the beer stream during the transition from fermentation to maturation in a ratio of about 40 g/HL of beer or Sol enter the t directly into the beer stream during the transition from puberty to filtering in a ratio of about 15 g/HL of beer. Bentonite long been used in the brewing industry, but now is rarely used due to its nonspecific compounds with proteins, removing proteins, forming and turbidity and foam. Gallotannin naturally present in plants and can be extracted from the leaves of Sumac or ink nuts. It consists of primaryservername tannic acid, which has many active centers (e.g., hydroxyl group), which interact with protein like canaidan that explain the relative specificity for active opacity proteins. Insoluble complexes that are formed, can easily be deposited and removed from the beer. Tannic acid is not harmful to the stability of the foam, if it is used in the recommended amounts. Tannic acid exist in various commercial forms, based on the purity of the product, and therefore can be used in different stages of the process: during the boiling of wort (2-6 g/HL), cold maturation of beer (5-7 g/HL) or directly before filtration of beer (2-4 g/HL). The reaction time is relatively short, and tannic acid can be dosed flow directly to the filtration of beer. Due to the formation of sediment permeability of the filter layer will decrease, and recommend the use of a larger grade DE or mix with what erlitou, to keep the same filtering ability. Proteolytic enzymes hydralicious hydrophobic proteins without preference to active turbidity in proteins and, consequently, have a negative effect on foam stability.

Various antioxidants (ascorbic acid and/or sulfites) was used to or remove oxygen from the beer, or to ignore its impact. These products can add flow during the filtration process, has a positive influence on the colloidal stability.

Hence the increasing problems associated with the use of DE, many attempts were made to use alternative alluvial filtration additives and, in particular, in the production of synthetic materials that could serve instead of DE. Some of them also recovered. Especially promising improvements are described in detail in EP 91870168.1; WO 1996/35497 and WO 96/17923. However, despite these improvements, they are limited in their ability to meet performance DE and, therefore, not widely accepted. In this regard, it should be noted the difficulty being played in accordance porosity layer synthetic filter additives porosity same with DE - although there are other opinions, which also rely on the relative performance of the product.

Accordingly, a need remains in the art for improvements synthetic alluvial accelerators filtering and/or their application, which can be used as an effective alternative to DE.

Summary of the invention

The present invention generally relates to improvements associated with alluvial filtration, and particularly to improvements in processing (conditioning) filter additives (including air-conditioned additives and methods of conditioning), and also relates to an improved filter layers and filtering methods with their use. In another embodiment, the present invention relates to improvements alluvial filtration with the use of complexing agents.

As an example, the present invention relates, in particular, to methods of preparation and/or filtering the liquid, which contains sensitive to the opacity proteins (supplemental or, in other words, compatible reagents) for subsequent separation of at least forming the turbidity of the protein material. This method includes a stage of adding one or more complexing agent capable of forming complexes that selectively delayed during filtration, with at measures which some of the sensitive opacity proteins. In brewing the desired result is to obtain turbidity at 25°C less than 0.7 EMU using synthetic polymers, or derivatives of silica, or a mixture thereof as filter additives during the aforementioned phase separation.

In accordance with another variant of the invention claimed methods of cooking and/or filtering the liquid, which contains sensitive to turbidity proteins for subsequent separation of at least forming the turbidity of the protein material, and the above-mentioned method includes a step of adding one or more agent that forms a protein complex (e.g., flocculation), capable of forming complexes (flakes) with at least some sensitive opacity proteins as compatible or additional reagents to obtain the turbidity at 25°C less than 0.7 EMU using on the stage of separation of the mixture of synthetic polymers as filter additives, in which the above mixture contains at least one polymer with an electronic charge.

In accordance with another variant of the invention claimed conditioning filter layer used for application at the stage of separation by adding one or more agent that forms a protein complex (flocculation)that can form omplex (flakes) with at least some of the sensitive opacity proteins, contained in the liquid, resulting in reduction of porosity above the filter layer, which consists of a mixture of synthetic polymers as filter additives, where at least one such polymer and the above-mentioned cereals are mutually attractive electronic charges. In addition, in brewing, it is desirable that the final filtration with the use of air-conditioned filter layer had the turbidity at 25°C less than 0.7 EMU.

The invention relates to air filtration additives, filter layer comprising these additives, and methods of production of additives, including interaction complexing agent (i.e flocculonodular agent) and compatible reagent (together they form a complex, which can be essentially detained during filtration). Preferably the reagent and the complexing agent is injected into a stream of fluid (e.g., in a fluid flow, in particular, for example, in the flow of unfiltered beer), and more preferably, the complexing agent was selected to interact with the reagent, which is peculiar to the unfiltered liquid and, in particular, the reagent filter which is designed to facilitate its removal. This complex then interacts with a synthetic additive alluvial what about the filter and makes a connection with them. Agent, reagent and/or their associated structures with a filter additive linger in the form of a filter layer on the filter sieve suitable for these purposes. Complexes, essentially, are in a bound state with the adopted filtering conditions (including flow) in the voids or pores, limited materials filter additives in the above-mentioned layer, and thus statistically condition porosity layer, reducing the spread and distribution of average pore size. This contributes to the conditioning layer, so as to be closer, such as effective porosity, comparable with a filter layer of DE.

In light of the provisions proposed by the present invention, specialists in the art will find the selection and application of various complexing agents, reagents and materials the filter additives useful in achieving the objectives of this invention.

Description of the drawings

Figure 1 - graphical representation of the equilibrium of protein and polyphenol according to prototype models Capone. The formation of turbidity is expressed as a function of the respective concentrations of tanaid and sensitive proteins present in the beer.

Figure 2 - quantitative graphical representation of a generalized relation between residual turbidity and pressure drop along the filter depending on the number of agent forming a protein complex.

Figure 3 is a graphic representation of the relationship between the pressure drop along the filter and the filtered volume of beer while passing it with different amounts of complexing agent Brewtan® from Omnichem. This drawing is also different amounts of the mixed filter additives in comparison with diatomaceous earth (DE).

4 is a graphical representation of the relationship between the amount (g/HL) Brewtan® and quantity (g/HL) of filter additives depending on the increase of pressure differential on m2filtration area (bar/HL).

5 is a graphical representation of the relationship between the amount (g/HL) LUDOX® and quantity (g/HL) of filter additives depending on the increase of pressure differential on m2filtration area (bar/HL).

6 is a graphical representation illustrating the reduction of turbidity, measured under a scattering angle of 90° and 25° at 20°C depending on the number of Brewtan®, added to the filter.

7 is a graphical representation illustrating the reduction of turbidity, measured under a scattering angle of 90° and 25° at a temperature of 0°C depending on the number of Brewtan®, added to the filter.

Fig is a graphical representation of the development of turbidity obtained after filtration, the depending on the filtered volume flow Brewtan® about 1 g/hectoliter.

Figures 9 and 10 is a graphical representation illustrating the reduction of turbidity during the filtration passage of the same portions of beer according to, respectively, the processing of 0.7 g/hectoliter Brewtan® (Fig) and 9.3 g/hectoliter LUDOX® (Fig).

11 is a graphical representation illustrating the results of turbidity during the filtration passage of the processing solution of silica and without it (LUDOX®). Turbidity, measured at 90° and 25°, is significantly increased when the termination processing.

Fig is a graphical representation of the development of turbidity, measured under a scattering angle of 90° and 25°, during the industrial testing 1200 HL (HL). Also indicates the measured values of turbidity for each tank of filtered beer.

Fig is a graphical representation of the development of turbidity, measured under a scattering angle of 90° and 25°, during the industrial testing of more than 8000 HL (HL).

Detailed description

The present invention relates to a method for preparing a liquid such as beer, uses a combination of synthetic filter additives and one or more complexing agent for the detention of colloidal particles. Such particles are present in the liquid, and they are usually difficult to remove for final filtration. Using a synthetic polymer multiple IP is the use as filter additives, applying a specific effect beaccomplished agent to create a colloidal complex is able to stay in the filtering process, leading to a significant decrease in residual turbidity, measured under a scattering angle of 90° and 25°, in the filtered fluid. The preferred number beaccomplished agent should be adjusted to restrict flow when the differential pressure increases during filtration, and to be less than the amount that is required to obtain a significant positive effect on colloidal stability, which is necessary to ensure the expected storage life of the filtered product. This invention relates preferably to the use of gallotannin to the stage filtering liquids, such as beer, where filter additive is a polymer.

Synthetic polymers

The present invention relates to the use of filter additives derived silica, including rhyolite glass, and mixtures thereof. The synthetic polymers comprise one or more polyamide, polyvinyl chloride, fluorinated products, polypropylene, polystyrene, polyethylene, polybutene, polymethylpentene, and copolymers of ethylene, a binary copolymer and ternary copolymers with acrylic fibers, olefin thermolast cnie elastomers.

Filter additives can be mixed with polyvinylpolypyrrolidone and therefore can be used for priming, as well as for deposition of material on the supporting portion of the filter during the filtration process, leading to improved colloidal stability due to the specific interaction between polyphenols and polyvinylpolypyrrolidone. Filter additive or a mixture of different filtration additives, including polyvinylpolypyrrolidone can be reused after regeneration process, which is already patented (see W096/35497).

There are at least four characteristics, which are associated with the suitability of this sample particles for use as artificial additives with "physical" point of view:

a) the First three relate to the shape of the particles and are the most important of the four:

The uniformity determined by the sphericity coefficient (SC)is the ratio of the average diameter of the actual particles and assumes near-perfect sphere area 4 pi divided by the actual length of the perimeter of the actual particles, and is a comparison between the actual particle and the area/perimeter of the right circle. The computer analyzes the microscopic image to bring up this comparison is performed using the image analyzer (at least 20 particles).

is the form Factor - it is the ratio of the smallest diameter to the largest diameter of the particles - large form factors can lead to high Delta R.

- Isotropy is defined in the patent means that all particles are more or less uniform, i.e. they all have approximately the same shape to a greater extent than, for example, a mixture of fibers and spheres;

The sphericity coefficient (SC) is the ratio of the average diameter of the actual particles to a perfect sphere. Its measurement can be performed using an image analyzer (at least 20 particles), and the computer analyzes the microscopic image to derive this comparison). For example, SC is 0.47 for polyamide 11 Rilsan mentioned in this text. Capron polyamide 6, granulated or comminuted for the purposes of this invention, for example, can have SC approximately 0,57.

The shape factor is the ratio of the smallest diameter to the largest diameter of the particles. More detail is defined in the above published patent documents. For polyamide Rilsan the shape factor is approximately equal to 0.44, and approximately 0,49 for polyamide Capron. Note that large coefficients forms (i.e. those associated with elongated fibrous particles) can be compacted to such an extent that the pressure drop over the filter layer becomes undesirable large inevitably leads to a reduction in life-cycle filter.

Isotropy is also defined in the above patent documents, but in General means that all particles are uniform, i.e. they do not contain, for example, a mixture of fibers and spheres.

In General, isotropic sampling of particles having the form factors in the range 0.4 to 0.8, preferably about 0.5) and SC in the range 0,4-0,65 (also preferably about 0.5), is particularly preferred.

Also preferably, the density of the applied materials filter additives used in this invention was less than 1.25 and can be less than 1 (as in the case of high density polyethylene 0.99 in-0,98, or even lower, although undesirable, such low as polypropylene, for example, the density of which is equal to approximately 0.85), because the difference in density between the particles and the liquid becomes too large and the tendency of the particles to the ascent very difficult to filter. As to preferred practices and material density of the particles, the preferred density, which in practice is not significantly different from the density of the liquid to be filtered (for example, water, and beer have a nominal density of approximately 1). However, oils or other liquids with low density can match the materials of the particles with lower density.

Other factors, which have been installed, clean the Dima for action synthetic alluvial filtration additives, include characteristics such as particle size, degree of homogeneity, specific surface area, and chemical nature of the polymer. Regarding the latter, the polyamides have many advantages and are preferred in practice.

Examples of particles include the examples listed in European patent application EP-A-0483099, which describes the filter, the additive is intended for use particularly in the technique of nabywania sediments in the field of brewing. This Supplement consists of spherical particles with size of 5-50 μm with an average diameter closer to 20 μm. These additives are preferably used in the form of bread, the porosity of which is equal to 0.3 to 0.5.

The preferred filter additives can include a population of individual angular particles. The angular shape of the particles is determined by the shape factor, while the population of individual particles is determined by the coefficient of uniformity.

The shape factor is the ratio between the smallest diameter Dminand the greatest diameter of Dmaxparticles, the specified aspect ratio is from 0.6 to 0.85.

Uniformity coefficient is the ratio between the diameter of 80% of particles with a diameter of 10% of the particles indicated the homogeneity coefficient of 1.8-5.

Preferably the specific surface of the particles composing additive, measured way BET, sophisticated led the lead unit weight of filter additives preferably less than 10 6m2/m3.

The specific gravity of a single angular particles of the above-mentioned filter additives not more than 25% more than the specific gravity of the suspension to be filtered, in order to avoid settling and stratification.

Angular particles preferably formed from a polymer, such as synthetic polyamide.

According to a particularly preferred variant of the invention, the number of individual angular particles is determined by the particle size distribution calculated from the volume of particles having an average diameter of approximately 30-40 μm, measured according to the method of measurement Malvern (Malvem), the fact that 70% and preferably 90% of the particles have a diameter of 15-50 μm.

Characterization of individual particles can be determined in different ways:

- form factor (φ), which is the ratio of the smallest of tests are identified as Feret diameter (Dminto the greatest tests are identified as Feret diameter (Dmax) particles (see also Particle Size Measurement - 4th Edition, Terence Alien, published by Chapman & Hall, Ltd., 1990). The shape factor is measured using an optical microscope as described in the publication "Advanced in solid liquid separation", published by Muralidhara (1986, Batelle Institute), or measured by electron microscope, for example apparatus Gemini, serial production which has a company LEO and which uses the image analyzer based on software the software SCION. The tests are identified as Feret diameter is defined as the average value of the diameters measured between two parallel tangents of the projected outline of the particle (see also et Transferts Phases Dispersees of L. Evrard & M. Giot, published by UCL).

their specific surface (S0), as measured by the method of Brauer, Emmett and teller (Brunauer, Emmet and Teller - BET), defined in the document "Powder surface area and porosity", S. Lowell and J. Shields (published by Chapman & Hall Ldt, 1991)and refined by specific gravity filtration additives (see "Filtration Equipment Selection Modeling and Process Simulation", R.J.Wakeman and E.S.Tarleton (published by Elsevier Advanced Technology, 1st edition)

- specific gravity of particles (MA)

- chemical composition,

- physical nature.

The population of individual particles can be determined in part by use of the coefficient of uniformity, which is the ratio of the D80 to D10, where D80 - 80%the diameter of the passage of particles, and D10 - 10%the diameter of the passage of particles, both determined by particle size analysis by Malvern (using a laser beam, as defined in et Transferts Phases Dispersees of L. Evrard & M. Giot, published UCL); and the diameter of the passage of a particle is the diameter represents the diameter of a given percentage of the entire sample of particles, which is less than or equal to the average particle diameter (Davecalculated from the volume of the particles, measured by the method of measurement Malvern, which determines the equivalent diameter.

OS the dock or layer (granular substance, obtained after filtration on the filter suspension (unfiltered fluid+filter additive)) is defined:

- specific resistance Rs, which is the resistance to the passage of liquid through the layer in 1 kg of dry solid material precipitated in 1 m2(Rs, measured in m/kg)

- apparent specific mass Mgs(in kg/m3).

These measurements will determine:

the porosity ε0calculated from the apparent specific gravity (see also the definition given by the Dictionary Filter (Filtration Dictionary), published by the Society Filtration (Filtration Society, 1975),

- permeability β0(in Darcy), determined by resistivity measurements and the actual specific mass Manddefined by the pycnometric one (see also "Filtration Equipment Selection Modeling and Process Simulation of R.J.Wakeman and E.S.Tarleton (published by Elsevier Advanced Technology, 1st edition)).

Protein-complexing agents

Before the final stage of filtration, carried out with the use of synthetic polymers, specific protein treatment dramatically improves the performance of the filter layer, leading to a significant decrease in the residual turbidity in the filtered fluid. Applicable, and other agents that form a complex with the protein, namely gallotannin, carrageenan, gelatin, pectin, xanthan gum, silica gel, Na-silicate, colloidal shall ramesam, chitosan, alginate, zeolite, cationic starch and various combinations of these agents form a complex with the protein. The reaction time between specific proteins and complexing agent is relatively short, within a few minutes contact time, and the product can therefore enter the thread immediately before stage filtering or offline by processing portions of unfiltered liquid and/or in an earlier stage of the process, thread or offline. Agent forming a complex with the protein, plays an active role in promoting the formation of the complex and/or precipitation of some specific proteins. Another advantage is the improvement of the future of the colloidal stability of the treated liquid, as the dependence on the quality and quantity of agent that forms a complex with the protein. As described in background of the invention, the increase in colloidal stability can be obtained by removing sensitive proteins and/or elimination of some polyphenols, which are particularly reactive with certain proteins, which leads to colloidal instability. Polyvinylpolypyrrolidone is reactive and especially polyphenols, and therefore it is recommended to reduce the required number of polyvinylpolypyrrolidone to save the same effect on colloidal stability, that is to get the same term storage of the product. Lowering the dosage of polyvinylpolypyrrolidone considerably and depends on the quality and quantity of agent that forms a complex with the protein. Polyvinylpolypyrrolidone usually dispense with the use of filter additives empirically in certain proportions established by regulation Supplement polyvinylpolypyrrolidone to full compliance with the technical requirements as a separate beer product. However, according to the invention the proportion of polyvinylpolypyrrolidone in a mixed filter additive by 10-40% less than the usual proportions that are determined empirically.

The reaction mechanism

Not wishing to be bound by any theory or hypothesis, it is believed that the lower end turbidity of the filtered fluid occurs due to the formation and detention colloidal complex between proteins that are present in unfiltered fluid, and a complexing agent, which is added at the previous stage of the filter.

First of all, create complex for a short time in the liquid and mix with filter additive throughout the stages of filtration, when both particles are trapped on the filter through the filter additives. Filter additive consists of a synthetic polymer, which has very good mechanical properties; the CSOs, this decimalise or only slightly compressible material. On the other hand, the colloidal complex has a very limited mechanical integrity and great ability to undergo compression. Due to the compressibility of the colloidal complex porosity and/or permeability of the deposited filter layer will be reduced, leading to increased increase in differential pressure, which is measured between the input and output of the filter. The amount of agent that forms a complex with the protein, preferably selected to avoid excessive intensity of pressure increase, which affects the performance of the filter and which significantly reduces the amount of filtered liquid during the same production cycle to achieve maximum working pressure filtration, vendor-defined filter. The preferred amount of complexing agent is less than required to achieve colloidal stability associated with well-known applications such complexing agents. It is helpful to understand that the reaction mechanism acts directly and positively on the final turbidity of the filtered fluid. The mechanism of this phase separation, can mainly be explained by the principle of flocculation, which includes a complexing agent with dlinnie the second polymeric molecule. The complete mechanism of precipitation cereals includes a molecular bridge or series of bridges between particles and is considered as a sequence of stages of the reaction. First, the agent forms a complex with the protein is dispersed in the liquid phase, and secondly, this complexing agent diffuses to the interface of the solid and liquid phases, the complexing agent is adsorbed on a solid surface, and the free polymer chain adsorbed on the second particle, forming bridges. These non-biodegradable "flakes" are growing, connecting bridges with other particles. In fact, the optimal dose of the agent that forms a complex with the protein, it is found experimentally, and overdose leads to the creation of a well-stabilized liquid, which is extremely difficult to separate. This deposition process is irreversible, but you should take special care to avoid excessive shaking, which leads to the destruction of the "flakes" and thus to increased turbidity of the suspension due to the presence of colloidal material.

Two options or a combination of both gripping mechanisms can explain this phenomenon.

1. The first capture mechanism based on the material properties of the sediment (layer) and, generally speaking, associated with the porosity of the layer in such a manner that:

A. Particles pomot the deposits are trapped in the formed complex due physiochemical reactions and are trapped in the filter layer without passing through the filter, leading to a significant decrease in the residual turbidity of the filtered liquid. This process applies to "deep" filtering.

b. The complex formed when he comes in contact with the filter layer partially fills the empty volume of the filter layer, leading to a slight increase in pressure. The effect this creates is comparable to the mechanical barrier for particles of turbidity, which captured the resulting occlusion of the filter layer, affecting a significant decrease in the residual turbidity of the filtered liquid. This process applies to "surface" filtering.

2. The second mechanism is based on the composition of the sediment (layer) and is associated with the presence of at least one polymer having electrostatic properties. There is electrostatic interaction between these polymers and cereals, which are formed before, during deposition between complexing agents and sensitive to increased turbidity of the protein. Residual electrostatic charges flakes are probably negative, attributed to the negative charges of polyphenols. Considering this hypothesis, the preferred electrostatic charge of the polymer is positive, which explains the electrostatic interaction between the flakes and the by iMER. Can be used in a variety of polymers, such as PVPP, and other polymers used in the technology of anionic resins (anion).

3. Probably capture mechanism Muti is not by reason only of one or another mechanism, and results in synergies between the two mechanisms. Therefore, the decrease of the residual turbidity of fresh filtered fluid is the result of a combination physiochemically connections and mechanical detention. The effect is illustrated in figure 2.

Examples

There have been several trial tests in the pilot plant, which was filtered centrifuged industrial beer.

- Was carried out by filtration distillation 20 sec, size and type of filter candle filter area of 0.54 m2and a filtration rate of approximately 11 HL/h·m2.

Before the industrial filtration spin-on beer was treated with different amounts gallotannin (Brewtan® from Omnichem): number average of 0.5-2.0 g/HL. Introduction gallotannin produced flow continuously, immediately before the filtration of beer using the appropriate dosing pump. You can also add a complexing agent, processing the portion of the beer in the tank with unfiltered beer.

In another experiment, the beer was processed before being filtered solution kolloidn the on silica instead of gallotanins. Test silicasol (Filling 300® from Stabifix or LUDOX® from GRACE Davison) has a concentration of approximately 30-31%, density 1,205-1,213 g/ml at 20°C and a specific surface area of approximately 300 m2/g due to the fact that the average particle size of about 8 nm.

- Filter additive was a mixture of polyamide 11 and PVPP 50/50. "The best working characteristics of the polyamide 11 has established the following:

- average diameter of about 33 μm, measured according to the method of the Malvern

the shape factor is approximately 0.7, the form factor is the ratio between the smallest diameter and the largest diameter of the particles,

is the coefficient of uniformity is approximately 2.8, uniformity coefficient is the ratio between the diameter of 80% of particles with a diameter of 10% particles

- specific surface area of about 0.8×106m2/m3according to the method BET,

- unit weight of approximately 1040 kg/m3.

Polyvinylpolypyrrolidone (from BASF) is a mixture of polymers disposable and reusable in the ratio of 1/2. Filter additive was added continuously during the filtration process, the doses in 50-130 g/hl. Number of filter additives adapted depending on the number gallotannin to avoid excessive increases in pressure as it will be obvious to those skilled in the Anna area, in light of the disclosure of this invention.

Figure 3 shows the increase in pressure as a function of the filtered volume at different dosages gallotannin and filter additives. For all of these dosages of gallotanins increasing pressure higher than that obtained without the addition of gallotanins. In addition, the increase in pressure below the figures obtained with diatomaceous earth (DE) with the same number of filter additives. It is also clear that the greater the dose of gallotanins for the same number of filter additives, the greater the impact on the growth pressure. At the dosage of less than 2 g/HL increase differential is below the level obtained with DE, excluding any dosage of gallotanins. We believe that the number of gallotanins should be less than 2 g/chief

Figure 4 reproduces the increase of the pressure drop at different ratio between dose of gallotanins (Brewtan®) and a dose of filter additives. The differential pressure is expressed in bar/sec divided by the area of the filter in m2that allows you to compare different filtration equipment. Exponential curve shows that the obtained filter cake is slightly compressed due to the presence of gallotanins, but also polyvinylpolypyrrolidone. When using equation it becomes clear that the brewer can calculate the ideal ratio (Brewtan® / filter is obaka) to avoid any excessive increase in pressure drop. This ratio is specific for line filtering performance of the filter, the availability and/or performance of a centrifuge, the use of brighteners etc) and quality of unfiltered beer (yeast, turbidity, colloidal particles, the temperature of the beer, and so on).

Figure 5 represents the increase in pressure drop at different ratio between dose of colloidal silica (LUDOX®) and a dose of filter additives. The differential pressure is expressed in bar/sec divided by the area of the filter in m2that allows you to compare different filtration equipment. Exponential curve shows that the obtained filter layer is slightly compressed due to the presence of gallotanins and polyvinylpolypyrrolidone. When using equation it becomes clear that the brewer can calculate the ideal ratio (LUDOX®/ filter additive) to avoid any excessive increase in pressure drop. This ratio is specific for line filtering performance of the filter, the availability and/or performance of a centrifuge, the use of adhesive substances etc) and quality of unfiltered beer (yeast, turbidity, colloidal particles, the temperature of the beer and so on).

6 and 7 depict the results of the residual turbidity in the filtered beer received thevarious dosages gallotannin at two different temperatures. The presented results show a direct reduction of residual turbidity of beer, measured under two different scattering angles, as described in the background of invention. The decrease is the same when measured at 20°C when measured at 0°C. However, the turbidity measured at 0°C, becomes slightly higher compared with the value measured at 20°C. the Specialist in the art will understand, in light of the disclosure of the present invention that at 0°C hydrogen bonds between polyphenols and proteins is significantly greater than at 20°C, this part of the cloud is also called reversible clouding. The number of 0.5-1 g/HL of gallotanins enough to significantly lower the turbidity of the beer. The more significant impact on turbidity, measured at an angle scattering at 25°than under a scattering angle of 90°. It is also known that this promotes the full dosage of colloidal stability, but it is not enough to ensure that the characteristics of the colloidal stability required by most brewers.

On Fig shows the reduction of turbidity during the filtration cycle according to treatment 1 g/HL gallotannin. At the beginning of the filtration, the turbidity decreases rapidly to become more sustainable.

Figures 9 and 10 illustrate the reduction of turbidity during the filtration cycle according to the relevant is but the processing of 0.7 g/HL of gallotanins (Fig.9) and 9.3 g/HL of silicates (figure 10). During this experiment for both treatments used the same batch of beer. Residual values of turbidity at an angle of 25° and 90°, obtained after appropriate filtration cycle, very close. This experiment proves that similar turbidity can be obtained after filtration through the use of gallotanins or colloidal silica at a corresponding normal dose.

11 shows the results of turbidity during the cycle of the filtering processing silicasol (LUDOX®) and without it. The results of turbidity, measured under a scattering angle of 90° and 25°, relatively constant and below the upper limit (0.7 EMU) during phase filter using silicates. As soon as the processing is terminated, both turbidity, measured at 90° and 25°, significantly increase in value above the upper limit of 0.7 EMU. This experiment proves that the processing of the complexing agent must be maintained during the entire filtration cycle or that a termination may affect the results of the dimness.

Industrial tests were conducted with the aim of presenting the test results in an enlarged scale. The first test was performed under the following conditions:

Beer was centrifuged prior to filtration, and centrifuged beer contained 200,000 and 500,000 cells/ml

- Temperature filtrowanie the beer was from -1°C to 1.0°C.

The density of the filtered beer was of 12.4°R.

- Filter line had a throughput 500-550 HL/hour.

Filter was a candle filter 80 m2(metal surface).

- Filter additive was a mixture of polyamides 11 and polyvinylpolypyrrolidone 50/50, as it was defined in the section "test test".

- The number of filter additives was 60-70 g/chief

The results of the first test presented on Fig which shows the reduction of turbidity, measured under a scattering angle of 90° and 25°. During this test, about 1,200 GL, which were poured in two tanks for light beer (IWT), in every 600 sec, the average dose of the agent that forms a complex with the protein, equivalent to approximately 0.45 g/HL gallotannin (Brewtan®). Lowering the opacity more substantially at an angle of 25°than at 90°. Lowering the opacity gradually reduced during the filtration cycle, and the average turbidity was measured in each AME. Turbidity, measured under the scattering angle of 25°, had a mean value of 0.4 EMU for the first AME and about 0.2 EMU for the second IWT. Turbidity, measured under a scattering angle of 90°, had a mean value of 0.5 EMU for the first AME and approximately 0,45 EMU for the second AME.

In the second duty cycle filtering, IP is the use of more than 8,000 CH, the average dose of the agent that forms a complex with the protein, was approximately 0.45 g/HL of gallotanins (Brewtan®). This experiment proves that during the entire filtration cycle both opacity at 90° and 25° are quite stable and are below the upper limit of 0.7 EMU. Turbidity, measured under rasseivajushhaja an angle of 90°, was stable up to about 0.4 EMU and was higher than the turbidity, measured under rasseivajushhaja angle of 25°, which is stabilized below 0.1 EMU.

Therefore, in General, the preferred average processing approximately 0.5 g/HL of gallotanins enough to achieve less than 0.5 EMU (measured under a scattering angle of 90° and 25° at 0°C)as the residual turbidity of the beer after filtration, and the maximum effect is obtained with the dosage of 1 g/sec, with no additional effect above this dosage. In contrast, higher doses will create excessive pressure, which will affect the number of filtered beer during the filtration cycle.

The same takes place in the preferred modes of operation, using colloidal silica as a complexing agent in the preferred average dosage of approximately 10 g/HL with a maximum average number of approximately 25 g/hl. Above this dose increase pressure becomes chrismer the m and negatively affect the number of filtered beer during the filtration cycle.

1. The production method of the liquid turbidity of less than 0.7 EMU in the measurement of light scattering at an angle of 25°, which includes stages of obtaining a liquid containing sensitive to increased turbidity of the protein to the stage separation using as filter material synthetic polymers or derivatives of silicon dioxide or mixtures thereof to remove particles from the specified fluid, characterized in that it further comprises adding to the liquid containing sensitive to increased turbidity of protein before phase separation agent selected from the group comprising protein-complexing agent and protein-flocculation agent, to form flakes or complexes are sensitive to increased turbidity of the protein, moreover, these flakes or complexes optionally separated from the specified fluid at the specified stage of separation.

2. The method according to claim 1, where at specified stages of the separation of a mixture of synthetic polymers containing at least one polymer carrying an electrostatic charge.

3. The method according to claim 1, where the stage of adding the specified agent means a stage of condensation filter cake used at this stage of separation, to reduce the porosity of the specified filter layer.

4. The method according to claim 1, which provides after phase separation, the achievement of turbidity less than 0.7 CC is at an angle of 90°.

5. The method according to claim 1, where the separation stage is the stage filtration, including how "deep" filtering and/or "surface" filtering.

6. The method according to claim 1, where sintetichekie polymers selected from the group including polyvinylpolypyrrolidone (PVPP), polyamide, polyvinyl chloride, fluorinated products, polypropylene, polystyrene, polyethylene, polybutene, polymethylpentene, and copolymers of ethylene, a binary copolymer and ternary copolymers with acrylic fibers, olefin thermoplastic elastomers and their mixture, prepolymer or products of their co-extrusion.

7. The method according to claim 1, where the specified accelerator filtering can be reused after regeneration.

8. The method according to claim 5, where the surface of the filter is an electrostatic attraction between the flakes and the polymer having an electrostatic charge.

9. The method according to claim 2, where the specified electrostatic charge is a positive charge.

10. The method according to claim 9, where the specified polymer having a specified positive electrostatic charge, means PVPP.

11. The method according to claim 10, where PVPP mixed with other polymers in a ratio depending on the content in the liquid polyphenol for a stable colloid during storage of the finished product.

12. The method according to claim 11, where K is the number of PVPP, add in the mixed accelerator filtering depends on the nature and quantity of protein flocculation agent, and 10-40 wt.% less than the specified number to meet the requirements as a specific beer product, i.e. the content of polyphenols, the stability of the colloid, the retention period.

13. The method according to claim 1, where the protein flocculation agent selected from the group including tannin, carrageenan, gelatin, pectin, xanthan gum, colloidal silica, chitosan, alginate, cationic starch.

14. The method according to item 13, where tannin is gallotannin.

15. The method according to 14, where gallotannin added in an amount of from 0.1 to a maximum of 2 g/HL depending on the content in liquid protein, sensitive to the dimness.

16. The method according to item 13, where the colloidal silica is added in an amount of from 1 to a maximum of 25 g/HL depending on the content in liquid protein, sensitive to the dimness.

17. The method according to claim 1, where the fluid is a beverage based on fruit or cereal, characterized by a pH value of from 4 to 6.

18. The method according to 17, where specified based drink grass is a drink made of malt.

19. The method according to p where based drink malt is a beverage obtained by fermentation, characterized by a pH value of from 3 to 5.

20. The method according to claim 19, where apidoc, obtained through fermentation, is a beer.

21. The method according to claim 3, where the agent is a protein-complexing agent, and the complex formed provides interaction with the specified filter and is a synthetic alluvial accelerating the filtering material, providing education with them durable associates with this complex and/or strong associat as a filter layer, comprising accelerating the filtering material, provides retention on the filter layer specified sieves, and specified the almost complex is retained in the intermediate space between the particles of the specified filter material, thus creating a statistical distribution of the porosity of the sediment.



 

Same patents:

FIELD: chemistry.

SUBSTANCE: method is implemented by the passing of the vodka through immobile bed of active granulated charcoal with granule size 0.4-6.5 mm containing platinum impregnated to it mass in amount 0.001-0.1% at the rate 30-150 dl/hrs. per 1 kg of charcoal (coconut coal can be used as charcoal). Vodka can pass in pulsing mode through immobile bed of active granulated charcoal containing silver impregnated to it mass in amount 0.05-4.0 wt % at the rate 6-30 dl/hrs. per 1 kg of charcoal. The charcoal bed is located between protective and supporting cylinders provided with through holes of the cartridge filter with end covers.

EFFECT: level enhancing of vodka purification from toxic admixtures, decrease of sulphates, iron, methanol, 2-propanol content and enhancing of the vodka organoleptic indicators.

3 cl, 2 tbl, 6 ex

FIELD: chemistry.

SUBSTANCE: invention concerns application of polymerisates containing thermoplastic polymers, as filtering auxiliary and/or stabilising substances, and method of water fluid filtration and/or stabilisation. Water fluid filtration and/or stabilisation uses polymerisate in the form of polymer powder containing the following components, wt %: (a) 20 to 95 of at least one thermoplastic polyolefin and polyamide polymer, and (b) 80 to 5 of at least one substance selected out of group including silicates, carbonates, oxides, silica gel, kieselguhr, diatomite earth and linked polyvinyllactams and their mixes. Polymer powder is obtained by compounding of thermoplastic polymer (a) and substance (b) in extruder with physical and/or chemical interaction.

EFFECT: adjustable absorption by the use of insoluble, recoverable, chemically inert, slightly inflating polymerisates with large surface area.

26 cl, 2 tbl

FIELD: food industry.

SUBSTANCE: for clarification and stabilisation of liquid food products colloid anionic silicic sol is used with pH from 1 to 4, with diameter of particles from 4 to 150 nm and area surface from 20 to 700 m2/g.

EFFECT: invention allows to prepare clarified products with high extent of stabilisation.

23 cl, 2 tbl, 1 ex

FIELD: food industry.

SUBSTANCE: water-alcohol solution and/or vodka are passed through filtration packet with the speed from 6 to 80 dhal/h, presenting diamond powder and mixture of diamond dust with activated carbon in pack made of nonwoven thermal fastened fabric. It is located between two polypropylene perforated frames, broken with two stainless steel grids or polypropylene. External grid is protected with perforated grid or nonpermeable film, with space at opposite ends, sealed with polypropylene liquid melt or end plates at frame external or internal for output and input of filtered liquid. Before passing of vodka or water-alcohol solution through the filter packet it makes use to purify water-alcohol solution with adsorbent and/or on sand, and/or ceramic filter, and/or carbonic-purgative pile. It can be similar purified after filter packet. Before passing of vodka through the filter packet water-alcohol solution is purified with passing through filter packet. After passing through filter packet vodka can pass the last stage of filtration with the help of membrane filters.

EFFECT: allows improvement of quality of purification.

6 cl, 11 ex

FIELD: mechanical engineering.

SUBSTANCE: invention can be used in food-processing industry. The device contains a cartridge connected to the bottle neck and incorporates the case with a seat to screw a die cone on the bottle neck with a clamp, a thread on the external side to screw for decorative cap and a filter from a coarse-filtration material, a sorbent and a fine-cleaning material. The device has a transfer valve incorporated a sealing element in the air feed channel outlet area, the said being made in the cartridge case.

EFFECT: higher efficiency of cleaning.

7 cl, 2 dwg

FIELD: method for beverage turbidity prevention.

SUBSTANCE: claimed method includes beverage treatment with stabilizer containing particulated silica with medium pore diameter at least 6 nm, modified by interaction with water soluble polymer having pyrrolidone side chain groups. Polymer content in silica is 5-35 mass % based on dry silica mass.

EFFECT: one-step method for beverage purification from polyphenols and polypeptides.

13 cl, 4 tbl, 4 ex

FIELD: wine production.

SUBSTANCE: claimed wine is obtained by blending of wine material or wine material and concentrated juice to provide necessary sugar content. Then blend is filtered through sterile membranes with pore size of 0.2-0.4 mum, cooled to -2 - -5°C, mixed with adsorbent and argol crystal in ratio of 99:0.5:0.5 and conditioned under agitation for 24-48 h. Then product is racked off, filtered through diatomite powder and heated up to 40-55°C for 1-10 min to increase colloidal stability. Wine is bottled in preheated up to 70-80°C bottles, oxygen from over-wine space is removed by filling with inert gas, and bottle is capped with preheated up to 70-80°C cork. Method of present invention makes it possible to increase wine stability from 3 to 6-7 months.

EFFECT: table wine with increased stability.

2 ex

The invention relates to food industry, in particular alcoholic beverage industry, and can be used when cleaning vodkas from aldehydes

The invention relates to a method of stabilizing drinks by removal of polyphenols and proteins
The invention relates to alcoholic beverage industry and can be used in the production of vodka of the highest quality

FIELD: wine production.

SUBSTANCE: claimed wine is obtained by blending of wine material or wine material and concentrated juice to provide necessary sugar content. Then blend is filtered through sterile membranes with pore size of 0.2-0.4 mum, cooled to -2 - -5°C, mixed with adsorbent and argol crystal in ratio of 99:0.5:0.5 and conditioned under agitation for 24-48 h. Then product is racked off, filtered through diatomite powder and heated up to 40-55°C for 1-10 min to increase colloidal stability. Wine is bottled in preheated up to 70-80°C bottles, oxygen from over-wine space is removed by filling with inert gas, and bottle is capped with preheated up to 70-80°C cork. Method of present invention makes it possible to increase wine stability from 3 to 6-7 months.

EFFECT: table wine with increased stability.

2 ex

FIELD: method for beverage turbidity prevention.

SUBSTANCE: claimed method includes beverage treatment with stabilizer containing particulated silica with medium pore diameter at least 6 nm, modified by interaction with water soluble polymer having pyrrolidone side chain groups. Polymer content in silica is 5-35 mass % based on dry silica mass.

EFFECT: one-step method for beverage purification from polyphenols and polypeptides.

13 cl, 4 tbl, 4 ex

FIELD: mechanical engineering.

SUBSTANCE: invention can be used in food-processing industry. The device contains a cartridge connected to the bottle neck and incorporates the case with a seat to screw a die cone on the bottle neck with a clamp, a thread on the external side to screw for decorative cap and a filter from a coarse-filtration material, a sorbent and a fine-cleaning material. The device has a transfer valve incorporated a sealing element in the air feed channel outlet area, the said being made in the cartridge case.

EFFECT: higher efficiency of cleaning.

7 cl, 2 dwg

FIELD: food industry.

SUBSTANCE: water-alcohol solution and/or vodka are passed through filtration packet with the speed from 6 to 80 dhal/h, presenting diamond powder and mixture of diamond dust with activated carbon in pack made of nonwoven thermal fastened fabric. It is located between two polypropylene perforated frames, broken with two stainless steel grids or polypropylene. External grid is protected with perforated grid or nonpermeable film, with space at opposite ends, sealed with polypropylene liquid melt or end plates at frame external or internal for output and input of filtered liquid. Before passing of vodka or water-alcohol solution through the filter packet it makes use to purify water-alcohol solution with adsorbent and/or on sand, and/or ceramic filter, and/or carbonic-purgative pile. It can be similar purified after filter packet. Before passing of vodka through the filter packet water-alcohol solution is purified with passing through filter packet. After passing through filter packet vodka can pass the last stage of filtration with the help of membrane filters.

EFFECT: allows improvement of quality of purification.

6 cl, 11 ex

FIELD: food industry.

SUBSTANCE: for clarification and stabilisation of liquid food products colloid anionic silicic sol is used with pH from 1 to 4, with diameter of particles from 4 to 150 nm and area surface from 20 to 700 m2/g.

EFFECT: invention allows to prepare clarified products with high extent of stabilisation.

23 cl, 2 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: invention concerns application of polymerisates containing thermoplastic polymers, as filtering auxiliary and/or stabilising substances, and method of water fluid filtration and/or stabilisation. Water fluid filtration and/or stabilisation uses polymerisate in the form of polymer powder containing the following components, wt %: (a) 20 to 95 of at least one thermoplastic polyolefin and polyamide polymer, and (b) 80 to 5 of at least one substance selected out of group including silicates, carbonates, oxides, silica gel, kieselguhr, diatomite earth and linked polyvinyllactams and their mixes. Polymer powder is obtained by compounding of thermoplastic polymer (a) and substance (b) in extruder with physical and/or chemical interaction.

EFFECT: adjustable absorption by the use of insoluble, recoverable, chemically inert, slightly inflating polymerisates with large surface area.

26 cl, 2 tbl

FIELD: chemistry.

SUBSTANCE: method is implemented by the passing of the vodka through immobile bed of active granulated charcoal with granule size 0.4-6.5 mm containing platinum impregnated to it mass in amount 0.001-0.1% at the rate 30-150 dl/hrs. per 1 kg of charcoal (coconut coal can be used as charcoal). Vodka can pass in pulsing mode through immobile bed of active granulated charcoal containing silver impregnated to it mass in amount 0.05-4.0 wt % at the rate 6-30 dl/hrs. per 1 kg of charcoal. The charcoal bed is located between protective and supporting cylinders provided with through holes of the cartridge filter with end covers.

EFFECT: level enhancing of vodka purification from toxic admixtures, decrease of sulphates, iron, methanol, 2-propanol content and enhancing of the vodka organoleptic indicators.

3 cl, 2 tbl, 6 ex

FIELD: food industry.

SUBSTANCE: invention relates to production method of liquid containing proteins (especially turbidity sensitive proteins) for following separation at least turbidity causing substances by using of filtering additives. Method includes adding of complexing agent able to create composite with at least several sensitive proteins of the liquid which leads to limitation of liquid residual turbidity obtained after filtration stage.

EFFECT: invention allows to increase beer turbidity stability.

21 cl, 13 dwg

FIELD: food industry.

SUBSTANCE: processing and cleaning of liquid product as well as of vodka is performed by passing it through mixture of sorbents situated between filter media. Each portion of the product poured out of the bottle into the drinking tank undergoes processing and treatment immediately before consumption by the customer himself. Processing is performed by pushing the product out of the tank (bottle) with optimal speed through the coarse filter, sorbents and fine filter located inside the cartridge located in the body secured on the tank neck due to excessive air pressure of required value in the inner cavity of the tank. The pressure is created as required by a small air pump located outside of the bottle. Besides the device can be equipped with an assembly of light effects or sound effects for advertisement purpose.

EFFECT: when placing mineral, flavour and/or other additives, a new product can be obtained at the output of the device which is different from the product in the tank.

30 cl, 16 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to stabilisation of drinks. The invention discloses a material for filtering and stabilising drinks containing polyphenols and/or sensitive proteins, especially for stabilising beer. The material is a composite consisting of microcrystalline cellulose and one or more protein and/or polyphenol sorbents. Preferably, the protein sorbent is silica in form of silicic acid derivatives: sol, hydrogel (silica gel), xerogel and or mixture thereof. The polyphenol sorbent is preferably cross-linked polyvinyl pyrrolidone.

EFFECT: invention increases colloidal stability of drinks with low consumption of sorbents.

13 cl, 5 tbl, 21 ex

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