Method for preparing low-molecular pectin

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention refers to methods for preparing low-molecular pectin and may be used in pharmaceutical industry for preparing new therapeutic and preventive drugs, low-molecular sorbents. The method provides pectin hydrolysis in an aqueous solution of mineral acid with heating and liquid phase separation from an insoluble residue of pectin. The low-molecular products of pectin hydrolysis are recovered from the liquid phase by settling them in an organic solvent with water. A hydrolysis feed material is low-etherified pectin of ratio max. 30%. The hydrolysis process is continuous in a continuous-flow machine. Temperature in a working chamber of the machine is maintained at 70-100°C. Feeding speed of mineral acid into the chamber is calculated by specific formula. The prepared liquid phase is exposed to additional heat treatment in a flow heat exchange following the hydrolysis process. Temperature of the additional heat treatment process coincides with hydrolysis temperature. Heat exchange section capacity is determined by specific formula. The prepared liquid phase is neutralised to pH min. 4.0. Thereafter, the prepared liquid phase is used to settle the low-molecular products of pectin hydrolysis.

EFFECT: invention enables producing low-molecular pectin with no process loss of the feed material, substantially reducing oligogalacturonide destruction accompanying the hydrolysis process, and thereby improving the end product yield.

5 cl, 1 dwg, 4 ex

 

The invention relates to methods of producing low-molecular pectin and can be used in various branches of industry and medicine, in particular in the pharmaceutical industry to create new therapeutic and prophylactic agents and low-molecular adsorbents.

Receiving low-molecular pectin (oligoglycosides) is usually carried out by depolymerization of natural high-molecular pectin. This can be used a number of methods.

There is a method of hydrolysis of pectin at high temperature (WO 2009/004153, C08B 37/06, publ. 08.01.2009). According to this method, a 1% solution of pectin with a pH of 4-5 is heated under pressure at 110°C for 30-60 minutes, then the solution is cooled, the precipitated oligosaccaride with isopropanol and dried. The resulting product consists of 95% oligoglycosides with degree of polymerization 4-11 (0,7-2 kDa). The yield of the final product by the authors is not given.

The disadvantage of this method is that at temperatures over 100°C dramatically speeds up the process of thermal decomposition oligoglycosides - breaks pyranose cycle, oxidation, decarboxylation, formation of furfural and its derivatives. This is accompanied by a decrease in the output oligoglycosides and pollution of the hydrolyzate products of their decomposition (Kertesz Z.I. The pectic substances. Interscience Publishers, Inc., N.Y., L., 1951, 576 p.). With hee the practical point of view, oligosaccaride, having in the molecular structure of the products of thermal degradation of the galacturonic acid, can not fully be considered oligosaccaride.

The known method of depolymerization of polyuronides of alginates and pectins using the oxidant is hydrogen peroxide (U.S. Pat. USA US 2002/0016453(A1), C08B 37/06, publ. 07.02.2002). According to this method pechova acid in the form of pectate lithium is oxidized by hydrogen peroxide concentration of about 2% in the presence of ferric sulfate for 4 hours. Then oligosaccaride precipitated with acetic acid, washed with propanol and dried. The average degree of polymerization oligoglycosides - 16 (or 2.8 kDa). The product yield is 38%.

The disadvantages of this method include, firstly, the low yield of product. Secondly, the hydrogen peroxide simultaneously with the depolymerization of pectin causes significant destruction of the remnants of the galacturonic acid decarboxylation, breaks pyranose cycle, oxidation of the alcohol group and, as noted in the previous example, the resulting products can not fully be considered oligosaccaride (Kertesz Z.I. The pectic substances. Interscience Publishers, Inc., N.Y., L., 1951, 576 p.).

A common disadvantage of the above methods is used for hydrolysis of pectin solutions with a low initial concentration of raw materials - 1-2%. Another common drawback is that the process floor the treatment oligoglycosides is periodic and, therefore, formed at the beginning of the process oligosaccaride remain in the reaction medium until the end of the period and may partially collapse.

The closest to the technical nature of the claimed method is a method of obtaining low molecular weight pectin (oligoglycosides) from flax pectin by acid hydrolysis (Bedouet L., Courtois B., Courtois J. Methods for obtaining neutral and acid oligosaccharides from flax pectins // Biotechnol. Lett. 2005. Vol.27. P. 34, 36, table 1 and table 37). The method includes the following operations: obtaining an aqueous solution of pectin hydrolysis, cooling, separation of the liquid phase, the subsequent allocation of the target product by precipitation with an organic solvent miscible with water, centrifuging the precipitate and drying.

This method, in particular, is as follows. From a sample of pectin mass of 50 mg, containing 22.9 mg (45.8%) of uronic the galacturonic acids, preparing an aqueous solution of pectin concentration of 5 mg/ml (0.5%). Then add 12 M hydrochloric acid solution to a concentration of 100 mm (0.1 g-EQ./l) and carry out the hydrolysis at 80°C for 24 hours the resulting hydrolyzate is cooled to room temperature. The liquid phase containing the low-molecular products of hydrolysis, is separated from the high molecular polygalacturonic acid by centrifugation at 4°C and a relative centrifugal acceleration of 20,000 g for 30 minutes. Then n is scimolecular products of hydrolysis - oligosaccaride precipitated from the liquid phase with isopropanol and separated by centrifugation. The average degree of polymerization oligoglycosides - 15 (2,6 kDa). Output oligoglycosides is 33,9% of the initial content of the galacturonic acid.

A significant disadvantage of this method is the low initial concentration of pectin in the solution. The result is, first, the low rate of hydrolysis, as she continued constant of hydrolysis is proportional to the concentration of pectin in the solution. Secondly, the low initial concentration of pectin results in a corresponding low concentration of the final product in a ready hydrolysate - content oligoglycosides ready hydrolysate obtained by the method described above is only 0,78 mg/ml for 24 hours of hydrolysis (the yield is calculated by multiplying the initial concentration of pectin in the solution on the relative content of the galacturonic acid in pectin and the relative output galacturonic, and is respectively 5 mg/ml × 0,458 × 0,339=0,78 mg/ml), and this, in turn, leads to higher unit production cost of a unit mass of product. In this case, for example, costs associated with thermoregulation for a long time the total volume of hydrolyzed at 80°C and a flow rate of acid hydrolysis.

Ven is tsteam for a significant increase in the concentration of pectin in the solution is the fact that that high molecular weight pectins already at a concentration of about 1% form a sufficiently viscous solutions and the use of more concentrated solutions of pectin can create certain technological difficulties. Highly viscous solutions at low concentrations form almost all commercial pectins, as it is with this ability is closely connected with one of the main directions of their use as thickeners and structuring agents in the food industry. For example, the viscosity of a 1.5% solution of the most common commercial pectin - Apple and citrus (producer - Herbstreith &Fox KG, Germany) in 25-30 times the viscosity of water.

Another disadvantage is the low technological efficiency of the method, which leads to a low yield of product. Yield - oligoglycosides is about 34%, 33% is the remainder of macromolecular polygalacturonic acid and 33% loss oligoglycosides due to their structural degradation. Thus, loss of the product is almost the same value as its output. Technological disadvantage is that the separation of the liquid phase containing the finished product requires very strict conditions: the relative centrifugal acceleration - 20000 g for most industrial C is Tripp and separators or unattainable, or close to their maximum operating mode, the necessity of cooling to 4°C also creates additional technical problems and leads to higher process. The main technological disadvantage is that the process is conducted in a variety of devices, and for receiving subsequent portions of the finished product, the process is repeated from the beginning. A significant drawback of such a periodic manner of hydrolysis of pectin is that, as noted above, formed in the beginning of the process of hydrolysis oligosaccaride remain in the reaction medium until the end of the process (cycle) and inevitably undergo further structural degradation, which leads, eventually, to the loss of part of the target fraction (1-5 kDa) and, respectively, to yield the finished product.

The goal of the invention is to obtain a low-molecular pectin-enriched fraction oligoglycosides with a molecular mass of 1-5 kDa, increasing the yield of the target product, by reducing structural degradation oligoglycosides during hydrolysis, the simplification and cheapening of the way.

This objective is achieved in that in the known method of obtaining low molecular weight pectin (oligoglycosides), including the hydrolysis of pectin in an aqueous solution of mineral acid when heated,separating the liquid phase from the insoluble residue of pectin, the release of her low-molecular products of the hydrolysis of pectin by precipitation with an organic solvent miscible with water, followed by separation of the target product, according to the invention as a feedstock for hydrolysis using viscoelastically pectin with a degree of esterification of not more than 30%, the hydrolysis are continuously in a flow apparatus, consisting of the application, site, download the raw materials and the working chamber separated by filtration partitions into three departments: the Department of the input solution of mineral acid, separating the hydrolysis of pectin and the Department of the conclusion of the hydrolysate, and the feed rate of solution of mineral acid in the device is calculated by the empirical formula

where υ is the velocity solution of mineral acid in the system, l/h;

V is the volume of the chamber occupied by the Department of hydrolysis of pectin, l;

C - concentration of acid = 0.1 to 2.0 mol/l;

t - temperature process = 70-100°C;

K is a dimensionless empirical coefficient, determined experimentally, the values of which are in the range of 0.075-0,100;

the liquid phase (ready hydrolysate) after exiting the apparatus is directed to a flow-through heat exchanger and subjected to additional heat treatment at the same temperature, which was held n ocess hydrolysis, the volume of compartment heat exchanger, which is intended to receive the liquid phase from the apparatus (V1), calculated by the empirical formula

where V1- the volume of the compartment of the heat exchanger, which is intended to receive the liquid phase from the apparatus, l;

V is the volume of the chamber occupied by the Department of hydrolysis of pectin, l;

K1- empirical coefficient, determined experimentally, the values of which are within 0,17-0,22;

before deposition of low molecular weight products of the hydrolysis of pectin organic solvent liquid phase is neutralized to a pH of at least 4.0.

Use as feedstock for hydrolysis nizkoenergeticheskogo pectin with a degree of esterification of not more than 30%, with limited expansion in the acidic environment, allows the process of acid hydrolysis in heterophase system: gel nizkoenergeticheskogo pectin (solid phase) is the solution of mineral acid (liquid phase), which ultimately allows in practice to increase its concentration in the suspension to 8-26% (calculated on the dry matter of pectin). Such a high concentration of pectin suspension is achieved also due to the fact that the process of hydrolysis is conducted in a flow apparatus, which do not require mixing of the suspension (and it is the poet who can have the highest density), instead, there is a movement of the liquid phase through a stationary suspension of pectin. This also eliminates the need for a mixing device.

Using the process flow of the device allows to carry out the process continuously, as a result there is a constant updating of the liquid phase in the apparatus from it continuously displays the resulting oligosaccaride, while the remaining material is subjected to further hydrolysis. The end result, it is possible to fully utilize the raw materials, to prevent degradation oligoglycosides in the liquid phase, thereby increasing the yield of the target product and lowering the unit cost of its receipt, and also to provide the possibility of using, in comparison with the prototype, high concentrations of raw materials that ceteris paribus (at the same degree of hydrolysis of pectin), allows to obtain hydrolysates with correspondingly large percentage of the final product - oligoglycosides with the desired molecular weight, which significantly reduces the unit cost of production of a unit mass of product. And, as a consequence, leads to the simplification and cheapening of the process of obtaining the target product.

When using a pectin having a degree of esterification greater than 30%, there is a sharp increase in nabus the th gel pectin and a significant reduction in its mechanical strength, which complicates subsequent separation of the pectin gel from the liquid phase, it is also possible to introduce high-molecular pectin in the liquid phase.

For carrying out the proposed method can be used for virtually any commercial pectin. For this purpose, we first conduct a decrease in its degree of esterification to the required size in the range 0-30%, using any of the known methods of deesterification: alkaline, acidic or enzymatic. The most convenient and cost-effective, according to the authors, can be considered a method of alkaline deesterification pectin in a medium of an organic solvent, for example ethanol or isopropanol. This method is provided below, in the description of the implementation of the proposed method.

To achieve the stated technical result and the process of hydrolysis of the flow-through apparatus includes (scheme presented in the figure) thermostating system 1, the host substrate 2 and the working chamber 3 separated by filtration walls 4 and 5 in three branches: the branch input 6 solution of mineral acid, separating the hydrolysis of 7 pectin and the Department of the output 8 of the hydrolyzate. Details of a running system, direct contact with the solution of mineral acid, is made from acid - and heat-resistant materials: glass, PTFE, stainless steel (in the line is the use of nitric or sulfuric acids). Filtering partition 4 and 5, the limiting separation of the hydrolysis of 7 working chamber 3 in which is hydrolyzable raw materials, make more uniform flow and distribution of the acid solution on the cross-sectional area of the working chamber and allow automatic and continuous separation of the finished hydrolysate (liquid phase) from the non-hydrolyzed residue of the raw material (solid phase). The presence of the design of the device the two filter walls 4 and 5 at the bottom and top of the working chamber - allows movement of the liquid phase in the apparatus during hydrolysis in either direction, both top-down and bottom-up. During the reverse flow of the solution of mineral acid, a branch of the conclusion of the hydrolysate will perform the role of the branch input of mineral acid, and separating the input mineral acids, respectively, will act as a branch of the output of the hydrolyzate. With the ability to direct the movement of the liquid phase from the bottom up, in the device proposed design can be used for hydrolysis of pectins form a gel with a low mechanical strength (for example, pectins with a degree of esterification is close to 30%). This gel during hydrolysis may deform and form a dense sediment, preventing the flow of the liquid phase. When the movement of the liquid phase in the apparatus from the bottom up, it degenarative effects of gravity on granules of pectin gel and thus, the seal prevents precipitation of the pectin.

The ratio of height separation of hydrolysis (the distance between the filtering partitions) to its internal diameter - N/D is a parameter that affects the dynamics of the process of hydrolysis. Experimental verification showed that for the normal process of hydrolysis in a flow apparatus, the value of N/D must be in the range of 0.5-10. If the value N/D lower 0,5 occurrence of stagnant zones and a violation of the uniformity of flow of the liquid phase through the amount of hydrolyzable material. This leads to deviations of the conditions of hydrolysis of optimal values at specific points of the volume of raw materials and, consequently, to decrease the yield of the target product. When values of H/D big 10 significantly increases the hydraulic resistance of the "column" of raw materials, which can not be achieved the required speed of movement of the liquid phase. This leads to deviations of the conditions of hydrolysis of optimal values throughout the volume of raw materials and, consequently, to decrease the yield of the target product.

The use of empirical formulas (I) and (II)proposed by the applicant, allows the specified temperature range (70-100°C) and acid concentration (0.1 to 2.0 mol/l) and the factor K (K=0,075-0,100) with satisfactory accuracy to calculate the feed rate of solution of a mineral is islote in the apparatus, and with the help of K1(K1=0,17-0,22) with satisfactory accuracy to calculate the volume of the compartment of the heat exchanger, which is intended to receive the liquid phase (hydrolysate) of the apparatus for carrying out additional heat treatment required to obtain the product with the highest relative content of fractions oligoglycosides 1-5 kDa, i.e., to ensure the realization of the stated technical result and obtain the target product.

It should be noted that formulas (I) and (II) are empirical and, as many empirical formula (e.g., the well-known Arrhenius equation relating temperature and the rate of chemical reactions), do not allow a strict note of dimensions of physical quantities in the left and right parts of the equation. Therefore, the coefficients K and K1in the proposed in the application of mathematical expressions are dimensionless and represent the ratio between the left and right part of the equations (I) and (II) taking into account the size (scale) of physical quantities included in the equation.

Additional heat treatment of the liquid phase flowing in the heat exchanger allows to increase the content in the final product of the target fraction oligoglycosides 1-5 kDa due to the hydrolysis of high molecular weight fractions oligoglycosides (>5 kDa). The volume of the CTD is of a heat exchanger, which is intended to receive the liquid phase of the system, calculated by the formula (II) when K1=0,17-0,22, enables additional hydrolysis of the liquid phase by an additional heat treatment in such a way that the growth of the target fraction oligoglycosides due to the hydrolysis of high molecular weight fractions oligoglycosides substantially exceeds the loss given target fraction occurring in consequence of its partial hydrolysis and transition in the low molecular weight fraction oligoglycosides (less than 1 kDa).

Holding heterophase acid hydrolysis nizkoenergeticheskogo pectin in a flow apparatus creates conditions for effective and continuous molecular separation occurring naturally in the course of the hydrolysis. Therefore oligosaccaride with a molecular mass of 1-5 kDa formed during the hydrolysis of pectin, almost completely into solution - liquid phase, while the share of such molecules remaining in pectin gel - solid phase does not exceed 1-2% of their total number.

Yield - low molecular weight pectin, obtained by the proposed method is 93.0-97,7%. Thus, the relative content of the target faction oligoglycosides 1-5 kDa in the finished product is 87.5MHz-93.1%of. It is possible to condition the receipt of such a high product yield and the content of the target fraction is the process of hydrolysis of pectin - continuously, in the apparatus flow type, with subsequent heat treatment of the resulting hydrolysate. This is due to certain advantages of the continuous process of hydrolysis (compared to the periodic (cyclic) process), which manifest themselves in the dynamics of accumulation oligoglycosides in the liquid phase and removing them from the apparatus. So, due to the fact that for continuous hydrolysis of the apparatus continuously displays the resulting oligosaccaride, their average time in the system (necessary to achieve the maximum content of the target fraction in the liquid phase) is less than the periodic process. This allows to limit the destruction oligoglycosides and to increase the yield of the target product.

Conducting the process in a flow apparatus allows to increase the relative content of the target fraction in the product, firstly, due to the greater rate of diffusion of light fractions oligoglycosides (less than 5 kDa) through polysaccharide gel compared with heavier fractions when they made their way together with the liquid phase flowing through the system; secondly, due to the presence of "chromatographic effect (separation of the molecules on the sorbent, in particular, by their molecular weight, determined by the speed of the processes of sorption/desorption oligos lecturenotes with different molecular weight in a matrix of pectin gel, because the acidic environment has a partial sorption of molecules oligoglycosides on molecules of high molecular weight pectin.

Additional heat treatment of the hydrolyzed pectin in flow heat exchanger allows the relative content of the target fraction oligoglycosides 1-5 kDa 5-8%, which is a significant improvement of the purity of the product.

The combination in this way the effect of interfacial molecular separation and technological ease of separation of the phases, and the possibility of putting in the new portions of the raw material without interrupting the process, allows hydrolysis process continuously and indefinitely. These limits of temperature and acid concentration are associated primarily with economic and technological reasons. So when the air temperature is below 70°C and an acid concentration below 0.1 g-mol/l is a significant decrease in the rate of hydrolysis of pectin and a significant increase of the process time, this leads to increased cost of production of the target product.

At temperatures over 100°C dramatically speeds up the process of thermal decomposition oligoglycosides - breaks pyranose cycle, oxidation, decarboxylation, formation of furfural and its derivatives. This is accompanied by a decrease in the output oligoglycosides and pollution gidrol is the ZAT products of their decomposition. The increase in acid concentration of more than 2.0 g-mol/l does not provide a significant increase in the rate of hydrolysis, but leads to a significant waste acid and additional costs for subsequent neutralization and release of product from the resulting salts, which, ultimately, leads to the complication of the process of obtaining the target product.

Neutralization of the liquid medium to a pH of at least 4.0 before deposition of low molecular weight products of the hydrolysis of pectin organic solvent provides the receiving sludge of low molecular weight pectin (oligoglycosides) with optimal consistency - thick, well-separated from the liquid phase. At pH below 4.0 is an increase in specific volume of sediment and the weakening of its structure, and, consequently, difficult separation of the precipitate from the liquid phase.

As the mineral acid can be used, in particular, hydrochloric, sulphuric, nitric acid.

As the organic solvent can be used known organic solvents, miscible with water, in particular, acetone, isopropanol, ethanol.

The separation of the liquid phase is finished hydrolysate from the insoluble residue of pectin in the device occurs automatically due to the presence of a filtering partition 5 that separates the working chamber 3 Department of hydrolysis of 7 and office you is ode of the hydrolyzate 8, and requires no additional effort. This significantly reduces the cost and simplifies the process of obtaining the target product in comparison with the prototype, as in the prototype, the centrifugation is carried out at the acceleration of 20,000 g and 4°C.

From an economic point of view it is advisable to maintain the hydrolysis of pectin in a constant process conditions, i.e. at a constant amount of pectin in the reaction environment, to make new additive servings of raw materials to the rest of the pectin through the loading unit of the apparatus to compensate for its consumption in the course of the hydrolysis. This allows the hydrolysis of pectin continuously and indefinitely (until exhaustion of stocks of raw materials) and to obtain any required number of the target product with the desired molecular weight, 1-5 kDa.

The advantage of the process of conducting hydrolysis continuously in a flow apparatus, the design proposed by the applicant, is the possibility of additive materials in the flow-through apparatus in any technologically or organizationally convenient time. Therefore the intervals between the additions of raw materials is determined on the spot by the manufacturers based on their own economic, technological or organizational issues.

The amount of raw materials that are added to the apparatus is determined visually by pavlonillarionov amount of pectin in the boot node when loading raw materials.

The method is as follows.

Example 1.

Hydrolysis of pectin is carried out in the apparatus, the design of which is presented on the figure, and the description of the device on 8-9 description of the application. The material of the body of the device is glass, the material of filter partitions - porous glass filter brand THEN 100. Separating the working chamber, where the hydrolysis of pectin, a branch of the hydrolysis - has the following features: inner diameter (D) of 50 mm, the height (H) is the distance between the filtering partitions - 25 mm, the ratio of height to diameter (H/D) of 0.5, the volume (V) - 49 cm3(0,049 l). The temperature control apparatus is performed with the help of the "shirts" - outer glass heat exchanger, located around the working chamber through which the pumped fluid (water or glycol) to the required temperature. The flow of the liquid phase is a solution of the acid in the apparatus is performed using a peristaltic pump with adjustable flow rate. The output of the liquid phase from the apparatus connected with flow heat exchanger, in which there is an additional heat treatment of the liquid phase. The flow-through heat exchanger is a piece of Teflon tubing (inner diameter 0.8 cm, the cross sectional area of 0.5 cm2) of a certain length, placed in a liquid thermostat (temperature control of the exchanger is of Annika and apparatus for hydrolysis is carried out using a single thermostat and accordingly, at the same temperature). Required internal volume of the heat exchanger, designed to receive the liquid phase from the apparatus (V1), calculated according to the formula (II) when K1=0,17

V1=0,17*0,049=0,0083 (l).

This volume corresponds to the length of the tubes of the heat exchanger 16.6 see

Pochtovuyu acid (Serva, No. 31680), with the content of the galacturonic acid - 82.2% degree of esterification is less than 1% of a 20% suspension in a solution of hydrochloric acid concentration of 0.1 mol/l is loaded into the apparatus through the host boot - up to complete filling of the Department of hydrolysis of the working chamber, the excess liquid phase is drained through the upper or lower branch input/output liquid phase. The download process is controlled visually and finish with the appearance of abundant raw materials in the boot node. The number loaded into the machine pectic acid, calculated on the dry matter, is for 11.55 g, its concentration in the suspension at 23.6%. After filling apparatus of raw materials it is heated up to 100°C and begin filing in the office of the hydrochloric acid concentration of 0.1 mol/l (C) through the upper branch of the input/output liquid phase with velocity (υ), calculated by the formula (I) when K=0,075

Hydrolysis of the feedstock is carried out at a given feed rate of the acid solution and the temperature of 100°C for 12 hours. It is every 2 hours in the apparatus upload a new batch of raw materials - to restore the original volume. The download process is controlled visually and finish with the appearance of abundant raw materials in the boot node. The total number loaded in the apparatus pectic acid is 15,10, Ready hydrolysate derived from the apparatus through the lower branch input/output liquid phase and is sent to the collector, where it is cooled to room temperature. The total amount of the obtained hydrolyzate is 192 ml, content oligoglycosides of 17.1 mg/ml

The hydrolysate is neutralized to pH 4,0 5,0 M solution of sodium hydroxide and the precipitated oligosaccaride the addition of 580 ml of ethanol. The mixture is intensively stirred for minutes and leave for the formation of a precipitate (sludge formation occurs in approximately 8-12 hours), then the precipitation oligoglycosides separated by centrifugation at a relative centrifugal acceleration (OTSU) - 1000-1500 g for 15 minutes and dried at 80°C. the Yield of the product is a dry powder of oligoamenorrhea sodium - and 3.72 g (content oligohaline sodium clean the galacturonic acid is 88.5%). To determine the relative (in stock) product yield, in terms of galacturonic acid, install the consumption of raw materials - the difference between the total number of pectic acid used for hydrolysis (15,10 g) and the amount remaining after GI is Raisa. For the amount of pectic acid recalculate the content the galacturonic acid, and the remaining amount of pectic acid to determine the total content of the galacturonic acid photometric method. Installed the consumption of raw materials is on the galacturonic acid 3,62, the Relative yield on the galacturonic acid are, respectively, 93,0%. According to exclusive chromatography of the resulting product in 0.05 M acetate buffer with a pH of 3.0 on a column of Sephadex G-50 superfine calibrated using a standard set of pullulan, the relative content of fractions oligoglycosides 1-5 kDa in the resulting low-molecular pectin is 87,5%.

Example 2.

Get viscoelastically pectin by controlled alkaline deesterification vysokotarifitsirovannyh pectin.

Take 50 g vysokotarifitsirovannyh citrus pectin (Herbstreith &Fox KG, Germany), suspended in 0.5 l of 60% vol. ethanol and gradually added in several portions 5.0 M solution of sodium hydroxide, controlling the degree of esterification of pectin in samples taken after adding each portion of sodium hydroxide. After reaching the value of the degree of esterification of less than 30% to the suspension, add 20 ml of concentrated hydrochloric acid (density d=1.19 g/cm3), pectin is separated by filtration, washed the t 150 ml of 50% ethanol and dried at 80°C. Output nizkoenergeticheskogo pectin - 47 g, the content of the galacturonic acid - 74,8%, the degree of esterification by 30.0%.

Hydrolysis of the resulting pectin is carried out in a flow apparatus described in the previous example. Specifications: D=50 mm, H=50 mm, H/D=1,0, V=98 cm3. Required internal volume of the heat exchanger, designed to receive the liquid phase from the apparatus (V1), calculated according to the formula (II) when K1=0,20:

V1=0,20*0,098=0,0196 (l).

This volume corresponds to the length of the tubes of the heat exchanger equal 39,2 see

Viscoelastically pectin in the form of a 5% suspension in a solution of hydrochloric acid concentration of 2.0 mol/l is loaded into the apparatus as described in the previous example. The number loaded in the apparatus of pectin, in terms of dry substance, is 8.30 g, its concentration in the suspension - of 8.47%. After filling apparatus of raw materials it is heated up to 70°C and begin filing in the office of the hydrochloric acid concentration of 2.0 mol/l (C) through the lower branch input/output liquid phase with velocity (υ), calculated by the formula (I) when K=0,088

Hydrolysis of the feedstock is carried out at a given feed rate of the acid solution and the temperature of 70°C for 24 hours. Every 4 hours in the apparatus upload a new batch of raw materials to restore pervonachalnogo. The download process is controlled visually and finish with the appearance of abundant raw materials in the boot node. The total number loaded in the apparatus of pectin is or 10.60, Ready hydrolysate derived from the apparatus through the upper branch of the I/o of the liquid phase and is sent to the collector, where it is cooled to room temperature. The total amount of the obtained hydrolyzate is 336 ml, content oligoglycosides to 14.4 mg/ml

The hydrolysate is neutralized: at the beginning of the dry sodium hydroxide to pH 1-2, and then a 5.0 M solution of sodium hydroxide to a pH of 6.0. Oligosaccaride precipitated by adding 1.0 l of ethanol. The mixture is intensively stirred for minutes and leave for the formation of the precipitate, then the precipitation oligoglycosides separated by centrifugation for 15 minutes at OTSU 1000-1500 g, then cleaned from salts: resuspended in 250 ml of 70% ethanol and re-centrifuged. The wet precipitate is dried at 80°C. the Yield of the product is a dry powder of oligoamenorrhea sodium - 5,47, the Relative yield on the galacturonic acid, defined as described in the previous example, or 97.7%. The relative content of fractions oligoglycosides 1-5 kDa in the resulting low-molecular pectin is 93.1%of.

Example 3.

Get viscoelastically pectin. To do this, in 0.5 l of 50% ethanol dissolved 20,0 g hydroxide is the atrium, then added with stirring 100.0 g vysokotarifitsirovannyh citrus pectin (Herbstreith &Fox KG, Germany). The mixture is stirred for 50 minutes, then gradually in small portions add 40,0 ml of concentrated hydrochloric acid, pectin is separated by filtration, washed with 300 ml of 50% ethanol and dried at 80°C. the Output nizkoenergeticheskogo pectin - 93,3 g, the content of the galacturonic acid - 76,5% (C1), the degree of esterification is 0%.

Hydrolysis of the resulting pectin is carried out in a flow apparatus described in the previous example. Specifications: D=50 mm, H=100 mm, H/D=2,0, V=196 cm3. Required internal volume of the heat exchanger, designed to receive the liquid phase from the apparatus (V1), calculated according to the formula (II) when K1=0,22

V1=0,22*0,196=0,0431(l).

This volume corresponds to the length of the tubes of the heat exchanger equal 86,2 see

Viscoelastically pectin in the form of a 20% suspension in a solution of sulfuric acid concentration of 0.5 mol/l is loaded into the apparatus as described in the previous example. The number loaded in the apparatus of pectin, in terms of dry substance, is 50,92 g, its concentration in the suspension - 26,0%. After filling apparatus of raw materials it is heated up to 80°C and begin filing in the office of the sulfuric acid concentration of 0.5 mol/l (C) through the upper branch enter the/output liquid phase with velocity (υ), calculated by the formula (I) when K=0,100

Hydrolysis of the feedstock is carried out at a given feed rate of the acid solution and the temperature of 80°C for 120 hours. Every 8 hours in the apparatus upload a new batch of raw material to restore the original volume. The download process is controlled visually and finish with the appearance of abundant raw materials in the boot node. The total number loaded in the apparatus of pectin is 152,5, Ready hydrolysate derived from the apparatus through the lower branch input/output liquid phase and is sent to the collector, where it is cooled to room temperature. The total amount of the obtained hydrolyzate is 4080 ml, content oligoglycosides to 18.9 mg/ml

The hydrolysate is neutralized: at the beginning of the dry sodium hydroxide to pH 1-2, and then a 5.0 M solution of sodium hydroxide to pH 5.0. Oligosaccaride precipitated by the addition of 12.0 liters of ethanol. The mixture is intensively stirred for minutes and leave for the formation of the precipitate, then the precipitation oligoglycosides separated by centrifugation for 15 minutes at OTSU 1000-1500 g, then cleaned from salts: resuspending 8.0 l of 70% ethanol and re-centrifuged. The wet precipitate is dried at 80°C. the Yield of the product is a dry powder of oligoamenorrhea sodium - 87,33, the Relative yield on the galacturonic acid set the config as described in the previous example, is 97,0%. The relative content of fractions oligoglycosides 1-5 kDa in the resulting low-molecular pectin is 92,5%.

Example 4.

Get viscoelastically pectin.

In 0.4 l of 50% vol. isopropanol was dissolved 20 g of sodium hydroxide, is then added with stirring 100 g vysokotarifitsirovannyh Apple pectin (Herbstreith &Fox KG, Germany). The mixture is stirred for 10 min, then gradually in small portions add 40 ml of concentrated hydrochloric acid, pectin is separated by filtration, washed with 300 ml of 50% isopropanol and dried at 80-100°C. the Output nizkoenergeticheskogo pectin - 94,5 g, the content of the galacturonic acid - 78,4% (C1), the degree of esterification was 13.8%.

Hydrolysis of the resulting pectin is carried out in a flow apparatus described in the previous example. Specifications: D=25 mm, H=250 mm, H/D=10,0, V=122,5 cm3. Required internal volume of the heat exchanger, designed to receive the liquid phase from the apparatus (V1), calculated according to the formula (II) when K1=0,19

V1=0,19*0,1225=0,0245 (l).

This volume corresponds to the length of the tubes of the heat exchanger is equal to 49,0, see

Viscoelastically pectin in the form of a 20% suspension in a solution of nitric acid concentration of 1.0 mol/l is loaded into the apparatus as described in the previous example. The number loaded into part pectin, in terms of dry substance, is 32.50 to g, its concentration in the suspension of 26.5%. After filling apparatus of raw materials it is heated up to 90°C and begin filing in the office of the solution of nitric acid concentration of 1.0 mol/l (C) through the lower branch input/output liquid phase with velocity (υ), calculated by the formula (I) when K=0,075

Hydrolysis of the feedstock is carried out at a given feed rate of the acid solution and the temperature of 90°C for 48 hours. Every 8 hours in the apparatus upload a new batch of raw material to restore the original volume. The download process is controlled visually and finish with the appearance of abundant raw materials in the boot node. The total number loaded in the apparatus of pectin is 84,05, Ready hydrolysate derived from the apparatus through the upper branch of the I/o of the liquid phase and is sent to the collector, where it is cooled to room temperature. The total amount of the obtained hydrolyzate is 3460 ml, content oligoglycosides - 13,4 mg/ml

The hydrolysate is neutralized: at the beginning of the dry sodium hydroxide to pH 1-2, and then a 5.0 M solution of sodium hydroxide to pH 8.0. Oligosaccaride precipitated by the addition of 10.0 l of isopropanol. The mixture is intensively stirred for minutes, and leave for the formation of the precipitate, then the precipitation oligoglycosides separate the centrifugation for 15 minutes at OTSU 1000-1500 g, then cleaned from salts: resuspending 5.0 l of 70% isopropanol and re-centrifuged. The wet precipitate is dried at 80°C. the Yield of the product is a dry powder of oligoamenorrhea sodium - 52,20, the Relative yield on the galacturonic acid, defined as described in the previous example, is to 96.2%. The relative content of fractions oligoglycosides 1-5 kDa in the resulting low-molecular pectin is 89.3 per cent.

As seen from the above examples, the inventive method heterophase hydrolysis owing to the insolubility of the original pectin acid to hydrolysis purposefully to obtain a product with the desired molecular weight and thus to use the original pectin almost completely, i.e. avoids any significant technological losses of raw materials and to increase the final yield of the product (on the galacturonic acid) in comparison with the prototype 2.7-2.8 times to 93.0-97,7% of the feedstock. In addition, in the present method, in contrast to the known method, the hydrolysis of the raw materials is carried out continuously in a flow apparatus, which continuously displays the resulting oligosaccaride, which can significantly limit the destruction oligoglycosides during hydrolysis, and as a result, further increase the yield of the target product. Moreover, we offer and the tori technical solution provides compared to prototype a higher process speed and accordingly, the reduction of unit production costs and time to production of one kilogram of the product, with significant savings of raw materials, also eliminates the use of complicated and expensive process equipment to separate the liquid phase from the remainder of pectin.

Technical result achieved, largely due to the flow in the flow-through apparatus of the mineral acid with the speed that allows you to calculate proposed by the applicant empirical formula (I), as well as additional heat treatment of the hydrolysate in flow heat exchanger, the volume of the compartment which is intended for receiving the liquid phase of the flow-through apparatus, to calculate proposed by the applicant empirical formula (II).

1. The method of obtaining the low-molecular pectin, including the hydrolysis of pectin in an aqueous solution of mineral acid when heated with separation of the liquid phase from the insoluble residue of pectin, a selection from her low-molecular products of the hydrolysis of pectin by precipitation with an organic solvent miscible with water, followed by separation of the target product, characterized in that as a feedstock for hydrolysis using viscoelastically pectin with a degree of esterification of not more than 30%, the hydrolysis are continuously in PR is exact apparatus, when this raw material is fed into the separation of the hydrolysis of pectin working chamber of the flow-through apparatus through the host substrate until filling is complete, the temperature in the chamber is maintained at the level of 70-100°C using system temperature; then the branch input of mineral acid that is separated from the separation of the hydrolysis of filter wall, serves a mineral acid with the speed calculated by the formula (I)

where v is the velocity solution of mineral acid in the system, l/h;
V is the volume of the chamber occupied by the Department of hydrolysis of pectin, l;
With the concentration of mineral acid, 0.1 to 2.0 mol/l;
t - temperature process, 70-100°C;
K is a dimensionless empirical coefficient whose values are in the range of 0.075-0,100;
obtained in the hydrolysis of the liquid phase through the filter partition separating the Department of hydrolysis of pectin working chamber and the separation of the conclusion of the hydrolysate, arrives in the Department o hydrolysate, where it is directed in a flow-through heat exchanger, where it is subjected to additional heat treatment at the same temperature, which was used during the hydrolysis process, the volume of compartment heat exchanger, which is intended to receive the liquid phase of the flow-through apparatus, calculated by the empirical formula:

where V1- the volume of the compartment of the heat exchanger, which is intended to receive the liquid phase from the apparatus, l;
V is the volume of the chamber occupied by the Department of hydrolysis of pectin, l;
K1- dimensionless empirical coefficient whose values are within 0,17-0,22,
from the resulting liquid phase is then precipitated of low-molecular products of the hydrolysis of pectin, and before deposition of the liquid phase is neutralized to a pH of at least 4.0.

2. The method according to claim 1, characterized in that to the rest of the pectin in the Department of hydrolysis of pectin working chamber of the flow-through apparatus periodically add via the download site materials a new batch of raw material to recover its original volume.

3. The method according to claim 2, characterized in that the weight load of the working chamber of the flow-through apparatus of raw materials is determined by the glut of raw materials in the site to download materials.

4. The method according to claim 1, characterized in that the ratio of the height of the separation of the hydrolysis of pectin working chamber to its internal diameter is in the range of 0.5-10.

5. The method according to claim 1, characterized in that the movement of the liquid phase in the apparatus can be carried out from top to bottom when the top input solution of mineral acid and the lower output of the hydrolyzate, and from below upwards, the lower the input solution of mineral acid and the upper output of the hydrolyzate.



 

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EFFECT: improved preparing method.

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