Method for regeneration of betaine

FIELD: preparative chemistry and technology.

SUBSTANCE: invention relates to a method for separating in fractionating a solution containing betaine and sucrose. Method involves chromatographic fractionation of this solution, nanofiltration and regeneration of fraction enriched with betaine and, possibly, fraction enriched with sucrose. Chromatographic separation is carried out in columns filled with material chosen from cation-exchange and anion-exchange resins, and nanofiltration is carried out with a membrane for nanofiltration chosen from polymeric and inorganic membranes having the limit value of passing through a column from 100 to 2500 g/mole. Solution for fractionation represents a solution prepared from sugar beet, for example, the black syrup solution.

EFFECT: improved method of betaine regeneration.

40 cl, 12 tbl, 3 dwg, 7 ex

 

The technical field to which the invention relates

The present invention relates to a method of separation for the recovery of betaine and more particularly to a method of fractionation of a solution containing betaine and sucrose, with a combination of nanofiltration and chromatography. In a typical embodiment of the invention, betaine recovered from the solution obtained from sugar beet, such as a solution of black treacle.

The level of technology

Betaine is a valuable compound, which is used in animal feed, as well as in pharmaceutical and cosmetic applications.

Betaine is found in the roots, seeds, and stems of various plants. Its concentration in sugar beet is relatively high, from 1.0 to 1.5% calculated on dry solid. When sugar beet is processed for the recovery of sucrose, betaine is concentrated in the black treacle. Beet molasses usually contains from 3 to 8% betaine dry solid.

Betaine is an amphoteric compound having the formula:

(H3C)3N+-CH2-COO-

The prior art regeneration of betaine from beet black treacle, residual molasses or vinasse ion exchange, crystallization, extraction of the organic solvent is m or chromatography.

Chromatographic method for the recovery of betaine from beet black treacle described in U.S. patent No. 4359430 (Suomen Sokeri Oy). This chromatographic method, in which the molasses, which contains betaine, such as beet molasses, is introduced into the upper part of the column containing polystyrenesulfonate cation exchange resin, usually in the form of alkaline metal. Water-washing is carried out for the recovery of betaine, sucrose and residual black treacle from the stream, extending from the layer of resin.

Another method of recovery of betaine from black treacle has been described in U.S. patent No. 5127957 (Heikkla et al.); it uses chromatographic system with a simulated moving bed having at least three chromatographic columns connected in series. Betaine and sucrose regenerated as a fraction of individual products during the same cycle of the chromatographic system with a simulated moving bed. Column chromatographic systems are usually filled with strongly acidic cation exchange resin in the monovalent ionic form, preferably sodium and/or potassium.

Another method of fractionation black treacle has been described in U.S. patent No. 6093326 (Danisco Finland Oy). In this method, at least one product fraction is recovered during a multi-step sequence of operations in two or Bo is its hinges in the chromatographic system with a simulated moving bed. One variant of implementation of this method relates to a method of separation of sucrose and betaine from black treacle for the regeneration of the sucrose fraction and betanova faction. Chromatographic system contains at least two partially filled with a layer of material. The filling material of the columns is usually strongly acidic gel-type cation exchange resin in the monovalent ionic form, preferably sodium and/or potassium.

WO 96/10650 (Cultor Oy) relates to a method for separating sucrose and optionally a second component, such as betaine, containing sucrose solution, obtained from sugar beet. The method includes the impact on the solution of two successive chromatographic fraktsionirovanii by way of a simulated moving bed to obtain one or more fractions enriched in sucrose, and one fraction enriched specified by the second component. Chromatographic separation is usually carried out in a strongly acid cation-exchanger in the sodium and/or potassium form.

In DE-OS 2362211 (Suddeutsche Zucker AG) disclosed a method of chromatographic separation to separate black molasses sugar fraction and the non-sugar fraction, using a cation-exchange resin in Ca2+-form. The method has the disadvantage that the Ca2+-form resin is not in equilibrium with Katie the Noah composition of the mobile phase.

In U.S. patent No. 4333770 (UOP Inc.) discovered a way of separating sucrose from an aqueous mixture of a source of sugar, such as molasses, contacting this mixture with an adsorbent consisting of carbon pyropolymer. How bad separates betaine salts. In U.S. patent No. 4405377 (UOP Inc.) disclosed is the method of separation of monosaccharides from a feed mixture comprising an aqueous solution of monosaccharides, by contacting the specified solution with an adsorbent containing crystalline aluminosilicate such as zeolite. Feeding the mixture is diluted with ethanol before processing the adsorbent. The feed mixture may be glucose, such as corn syrup. This method is not used for separation of betaine. In U.S. patent No. 4405378 (UOP Inc.) discovered a way of separating sucrose from an aqueous solution containing sucrose, betaine and/or mineral salts, contacting the specified solution with an adsorbent comprising powdered activated carbon, linked organic polymer (cellulose nitrate, cellulose ether or mixtures thereof). This way bad separates betaine salts.

In U.S. patent No. 6379554 (Amalgamated Research Inc.) system disclosed, where the majority of chromatographic operations division, including the first operation with a simulated moving bed, linked in one way, which is preferably applied through the I continuous displacement chromatography for the regeneration fraction, enriched with small organic molecules, especially betamovie and/or invert sugar from sucrose solutions, providing a retroactive sucrose product of high purity.

In EP 0 411780 (Kampen Willen Hemmo) disclosed a method of recovery of betaine from beet distillates obtained from fermentation and distillation of sugar beet. The method includes steps (a) clarification of distillation with the use of microfiltration with cross-flow and with inorganic membranes having a pore size in the range from 0.1 to 10 μm, to remove solids and (b) holding clarified the distillate chromatographic separation with the exception of the ions for the separation of betaine. Chromatographic separation of ion exclusion may be carried out with suitable resins, such as SM-51-Na resin (IWT), IWT-AM-63 or DOWEX 50-WX8 (Dow Chemical). In addition to betaine this method can regenerate other products, such as ethanol, glycerol, succinic acid, lactic acid, potassium sulfate and L-pyroglutamyl acid.

Nanofiltration is a relatively new method of membrane filtration under pressure to separate the soluble components supplied to the nanofiltration between reverse osmosis and ultrafiltration. Nanofiltration is typically holds divalent salts and organic is their molecules with a molar mass of greater than 300 g/mol. The most important membranes for nanofiltration are composite membranes made mipomersen polymerization. Polyethersulfone membranes, sulfonated polyethersulfone membrane, polyester membrane, polysulfone membranes, membranes from aromatic polyamide membrane of polyvinyl alcohol and paliperidone membranes are examples of widely used membranes for nanofiltration. For nanofiltration can also be used inorganic and ceramic membranes.

The prior art known to the application of nanofiltration for the separation of glucose from disaccharides and more high molecular weight saccharides. Source mixture comprising glucose, may be, for example, hydrolyzed starch. One way of separating glucose from disaccharides and higher saccharides by nanofiltration, for example, has been disclosed in WO 99/28490 (Novo Nordisk).

U.S. patent No. 4511654 (UOP Inc.) refers to the method of producing syrup high glucose or maltose processing of raw materials containing glucose/maltose, enzyme selected from amyloglucosidase and β-amylase to form a partially hydrolyzed reaction mixture, passing the received partially hydrolyzed reaction mixture through ultrafilters membrane to obtain retentate and permeate, recycling retentate n is the stage of processing enzyme and regeneration permeate, including syrup high glucose or maltose.

In WO 01/14594 A2 (Tate & Lyle Inc.) disclosed method membrane filtration to obtain sucrose from sugar beet pulp. Membrane filtration can be carried out, for example, on ultrafilterable membrane or nanoelectrode membrane. In one embodiment of this method, membrane filtration is carried out using two consecutive steps of ultrafiltration, possibly in combination with diafiltration followed by stage nanofiltration, obtaining, thus, the nanofiltration permeate and retentate nanofiltration. Retentate nanofiltration contains most of sucrose from beet. In a preferred embodiment, the method retentate nanofiltration contains approximately at least from 89 to 91 wt.% sucrose (calculated on dry substance). Permeate from nanofiltration, on the other hand, as shown, contains approximately at least 25 to 50% betaine present in the material for nanofiltration. Available nanofiltration membrane with approximately 10% tap NaCl, as shown, are well suited for stage nanofiltration.

The above link WO 01/14594 A2 also offers a chromatographic separation for further purification containing sucrose of retentate obtained from ultrafilter the AI/diafiltration. Thereby obtaining the purified sucrose fraction.

However, the combination of chromatography and nanofiltration for the recovery of betaine from solutions obtained from sugar beet, was not disclosed in the prior art and it is not necessary.

Brief description of the invention

Thus, the aim of the present invention is to develop a method of recovery of betaine from a solution containing betaine and sucrose, such as a solution obtained from sugar beet, for example a solution of black treacle. Objectives of the invention are achieved by a method which differs from that set forth in the independent claims. Preferred embodiments of the invention are disclosed in dependent claims.

The invention is based on the combination of nanofiltration and chromatography for the recovery of betaine. The method according to the invention provides high purity and/or yield of the final product of betaine. In addition, betaine can be regenerated in this way other products with good yield and/or purity. Combining nanofiltration with chromatography in accordance with the present invention, it is possible to improve the efficiency of the method and/or the separation efficiency of the entire method of separation.

Brief description of drawings

The following drawings illustrate embodiments of the invention and not the substations are designed to limit in any way the scope of the invention.

Fig. 1 is a graphical representation of a variant of implementation 6.

Fig. 2 is a graphical representation of a variant of implementation according to claim 7.

Fig. 3 is a graphical representation of a variant of implementation in item 8.

Detailed description of the invention

The invention relates to a method for the recovery of betaine from a solution containing betaine and sucrose, through the implementation of the chromatographic fractionation and nanofiltration specified solution in any desired sequence with the regeneration fraction enriched in betaine, and, if required, the fraction enriched in sucrose.

The method according to the invention may also include a stage further chromatographic fractionation and/or nanofiltration for the regeneration of another faction or other fractions enriched in betaine, and maybe another faction or other fractions enriched in sucrose, and/or fractions of other products and/or their mixtures. In these other stages of the fractions obtained from the chromatographic fractionation and/or nanofiltration, undergo further divisions to further purify the product, to increase the output and/or to regenerate the fraction of other products and/or mixtures thereof.

Such phase chromatographic fractionation and/or nanofiltration can be performed sequentially in any desire is my sequence. Phase chromatographic fractionation and/or nanofiltration can also be carried out in parallel. The method may also include the combination of serial and parallel stages chromatographic fractionation and/or nanofiltration.

The specified solution containing betaine and sucrose is usually the solution obtained from sugar beet, containing solutions obtained at various stages of processing sugar beets, and the fraction obtained from the chromatographic fractionation juice of sugar beet. This solution, obtained from sugar beet, can be selected from, for example, beetroot juice, thick juice, ultimate black treacle and uterine syrups obtained from the crystallization of sugar.

Particularly suitable raw material for the recovery of betaine is molasses sugar beet, which usually contains from 3 to 8% of betaine per dry solids. In addition to the betaine beet molasses contains, for example, sucrose, salts, amino acids and other inorganic and organic components.

In addition to the black treacle as residual molasses from the way bessarione and bard from fermentation method can have a high content of betaine and of course are also very suitable raw materials.

In one embodiment, is sushestvennee of the invention the method according to the invention comprises the following stages:

(a) implementation of the solution containing betaine and sucrose, chromatographic fractionation and regeneration fraction enriched in betaine and sucrose, and possible residual fraction,

(b) the implementation of nanofiltration specified fraction enriched in betaine and sucrose, with regeneration fraction enriched in betaine and possible fraction enriched in sucrose.

This variant embodiment of the invention shown in Fig. 1.

Chromatographic fractionation of step (a) may be performed as a periodic manner or method with a simulated moving bed. The method with simulated moving bed may be continuous or sequential. In one preferred embodiment, the chromatographic fractionation stage (a) is carried out as a continuous method with a simulated moving bed, usually provide two fractions: fraction enriched in betaine and sucrose, and the residual fraction.

In stage (b) nanofiltration of the fraction enriched in sucrose usually get as retentate nanofiltration, and a fraction enriched in betaine, receive permeate from nanofiltration.

In this embodiment of the invention the method may also include nanofiltration specified residual fraction obtained in stage (a), and the regeneration fraction enriched in betaine, a fraction of Ogadeni sucrose, fractions enriched raffinati, and/or fractions enriched coloring compounds, depending on the composition of the residual fraction. Therefore, it may be raised out of betaine and/or sucrose.

These coloring compounds are usually present as impurities in the solutions obtained from sugar beet, mainly containing large molecules with a molar mass of more than 1000 to the nearest million (g/mol).

This fraction enriched coloring compounds (unwanted impurities), and this fraction enriched raffinati, usually regenerated as retentate nanofiltration. The method may also include the regeneration of the nanofiltration permeate, which can be returned to the step (a) chromatographic fractionation to use it as eluent.

This fraction enriched in betaine and/or a specified fraction enriched in sucrose obtained in stage (b) nanofiltration may be subjected to one or two further stages nanofiltration and/or chromatographic fractionation to further purify the product and/or increasing output.

In another embodiment of the invention the method comprises the following stages:

(a) the implementation of nanofiltration specified solution containing betaine and sucrose, with regeneration fraction enriched in betaine and the possible residual fraction and/or faction, enriched with sucrose

(b) conduct on a specified fraction enriched in betaine, chromatographic fractionation with regeneration fraction enriched in betaine and possible residual fraction and/or a fraction enriched in sucrose.

This variant embodiment of the invention shown in Fig. 2.

At the stage of (a) nanofiltration specified fraction enriched in betaine, usually recovered as the nanofiltration permeate, and the said fraction enriched in sucrose is recovered as retentate nanofiltration.

In this embodiment of the invention the chromatographic fractionation stage (b) may be performed as a periodic manner or method with a simulated moving bed. In a preferred embodiment, the chromatographic fractionation is carried out as the method with simulated moving bed, which may be continuous or sequential.

This variant of the method according to the invention may also include nanofiltration or chromatographic fractionation of the specified residual fraction obtained in stage (b), and the regeneration fraction enriched in betaine, a fraction enriched in sucrose fractions enriched raffinati, and/or fractions enriched coloring compounds, depending on the composition of the residual fraction. Thus it is possible in order to increase the yield of betaine and/or sucrose.

This fraction enriched coloring compounds (unwanted impurities), and this fraction enriched raffinati, usually regenerated as retentate nanofiltration. The method may also include the regeneration of the nanofiltration permeate, which can be returned to the step (b) chromatographic fractionation to use it as eluent.

This variant of the method can also include stage where a specified fraction enriched in betaine obtained in stage (b), is subjected to nanofiltration and/or chromatography, where the regenerated second fraction enriched in betaine, and maybe another faction. Stated another faction, for example, may include sugars, amino acids and Inositol. Sugar usually contain sucrose, glucose, fructose and galactose. Sugar, amino acids and Inositol can be recovered as products.

This fraction enriched in betaine and/or a specified fraction enriched in sucrose obtained in stage (a) NF, which can be subjected to one or more further stages of nanofiltration for further purification of the product and/or increasing output.

In another embodiment of the invention the method comprises the following stages:

(a) implementation on the specified solution containing betaine and sucrose chromatographic what about the fractionation with regeneration fraction, enriched with betaine, and possibly a fraction enriched in sucrose, and/or residual fractions

followed by at least one of the following stages:

(b) nanofiltration of the specified residual fraction from the regeneration fraction enriched in sucrose, and/or a fraction enriched in betaine, and possibly one or more other fractions

(C) the implementation of nanofiltration specified fraction enriched in sucrose, with the regeneration of the second fraction enriched in sucrose, and/or a fraction enriched in betaine, and possibly one or more other fractions

(d) the implementation of nanofiltration specified fraction enriched in betaine, with the regeneration of the second fraction enriched in betaine, and perhaps one or more of the other factions.

This variant embodiment of the invention shown in Fig. 3.

Chromatographic fractionation stage (a) may be performed as a periodic manner or method with a simulated moving bed. The method with simulated moving bed may be continuous or sequential. In a preferred embodiment, the chromatographic fractionation stage (a) is carried out as a sequential method with simulated moving bed, giving usually three fractions: fraction enriched in betaine, a fraction enriched in sucrose, and residual fraction.

In this embodiment of the invention the residual, and/or sucrose and/or betainovuyu fraction obtained from the chromatographic fractionation, can be subjected to nanofiltration separately.

In stage (b) of this variant embodiment of the invention the specified one or more other fractions usually contain a fraction enriched with raffinati, and/or a fraction enriched coloring compounds. Depending on the composition of the residual fraction of betaine and sucrose regenerated to increase total output, and raffinose can also be regenerated. This fraction enriched raffinati, and this fraction enriched coloring compounds, usually regenerated as retentate nanofiltration. This fraction enriched in betaine, usually recovered as the nanofiltration permeate. The permeate obtained from the nanofiltration can be used as eluent in the chromatographic fractionation stage (a).

Specified one or more other fractions recovered at the stage (C) of this variant implementation of the invention typically contain a fraction enriched Inositol, a fraction enriched with amino acids, the fraction enriched with monosaccharides, and/or a fraction enriched in raffinati. Betaine, Inositol, amino acids, monosaccharides and raffinose can be recovered as products. Indicated the data fraction, enriched with raffinati, usually regenerated as retentate nanofiltration. This fraction enriched in betaine, usually recovered as the nanofiltration permeate. At the same time, sucrose fraction is additionally cleared from betaine, Inositol, amino acids, monosaccharides and raffinose.

Stated another faction, the regenerated on stage (d) of this variant of the invention, may contain a fraction enriched in sugars fraction enriched Inositol, and/or a fraction enriched with amino acids. Sugar, Inositol and amino acids may be recovered as products. At the same time betainovuyu fraction additionally cleared from sugars, Inositol, amino acids and other compounds. When selecting a membrane, or a combination of membranes betainovuyu fraction can simultaneously purify and concentrate that reduces the need for evaporation at the next stage.

The specified residual fraction, possibly regenerated in various embodiments of the invention usually contains salt. Salt arise from raw materials such as sugar beet, and in the early stages of processing of raw material. In accordance with the method according to the invention the salt thus can be effectively removed from betaine and/or sucrose.

Phase chromatographic practioner the training method according to the invention can be carried out, using the material for filling the columns selected from cation exchange resins and anion exchange resins.

The specified cation exchange resin may be strongly acidic cation exchange resin or a weakly acidic cation exchange resin. The resin may be monovalent and/or divalent metal, such as Na+- and/or K+form, or Ca2+-, Ba2+-, Mg2+and/or Sr2+-form.

The resins may be styrene or acrylic skeleton. Resin preferably transversely crosslinked with about 1 to 20% of divinylbenzene, preferably from about 3 to 8% divinylbenzene.

Specified anion-exchange resin is usually weakly basic anion-exchange resin, preferably having an acrylic skeleton.

The average particle size of the resin is usually from 10 to 2000 μm, preferably from 100 to 400 microns.

Resins are preferably resins in the form of a gel.

Manufacturers of resins are, for example, Finex, Dow, Bayer and Rohm & Haas.

Zeolites, pyropolymer carbon and activated carbon associated with the polymer, are also suitable materials for filling columns.

In the operation of the chromatographic fractionation cations/anions of the resin are preferably in substantial equilibrium with the cations/anions in the mobile phase of the system.

Particularly preferred is a material for filling the speakers on stage chromatographic fractionation method according to the invention is a strongly acidic cation exchange resin in the monovalent metal form, which preferably is in the form of Na+and/or K+. The resin is preferably a styrene skeleton, and the resin is preferably cross linked polystyrene.

The eluent used on stage chromatographic separation in various embodiments of the invention, described above, is preferably water, but are also solutions of salts in water. In addition, suitable suenami are alcohols, such as ethanol, and a mixture of water and alcohol, such as a mixture of water and ethanol.

The temperature of the chromatographic fractionation depends on the selected resin. The temperature of the chromatographic fractionation is typically in the range from 50 to 100°C, preferably from 55 to 90°C.

In the method with simulated moving bed chromatographic fractionation is usually carried out using from 3 to 14 columns connected in series. The columns are connected by pipelines. The flow velocity in the columns is usually from 0.5 to 10 m3/(m2·h) cross-sectional area of the column. The column is filled with material to fill all the columns selected, for example, from the materials described above. The column is equipped with feed lines and lines for products, so that the column can be filed feed solution and eluent, and from the column can be collected fraction products. Line the La products equipped with linear instruments in order to control the quality/quantity of products during the operation.

Before chromatographic fractionation feed solution may be subjected to one or more stages of preprocessing, selected from softening ionoobmennoi processing or carbonization, dilution, concentration, for example by evaporation, the pH adjustment and, for example, filtration. In a typical operation of the preprocessing of the feed solution, such as beet molasses, diluted with water to a concentration of approximately from 40 to 60 wt.% and filtered using, for example, diatomaceous earth as an aid to filtration. Before serving in the column feed solution and eluent is heated to a temperature fractionation described above (for example, to range from 50 to 85°).

During chromatographic separation with IPS feed solution is circulated through the column by means of pumps. Added eluent and going sucrose, betaine and residual fractions, as well as other possible factions products.

In one example, the chromatographic fractionation in the method according to the invention, the sucrose content in the obtained sucrose fraction may range from about 85% to about 99% (based on dry solids, and the content of betaine in sucrose fractions can vary from approximately 0.01 to approximately the 10% (based on dry solids. The content of betaine in betanova fraction may range from about 20 to about 95% (based on dry solids, and the sucrose content in betanova fraction may range from about 5 to about 40%. The sucrose content in the residual black treacle fraction may range from about 5 to about 25% (based on dry solids and the content of betaine in the residual black treacle fraction may range from about 1 to about 35% (based on dry solids.

the pH depends on the composition of the initial solution and the membrane used for nanofiltration, and from the stability of the recovered components. If you want, before nanofiltration adjust the pH of the initial solution to the desired value. Nanofiltration for the recovery of betaine is usually carried out at a pH of from 1 to 12, preferably from 4 to 12.

Nanofiltration is usually carried out at a pressure of from 10 to 50 bar, preferably from 15 to 35 bar. The typical temperature nanofiltration from 5 to 95°C, preferably from 30 to 80°C. Nanofiltration for the recovery of betaine is usually conducted at a temperature of from 5 to 95°C, preferably from 30 to 80°C.

Nanofiltration is usually carried out at a flow of from 5 to 100 l/(m2·h).

Membrane for nanofiltration used in the present invention may be selected from polymeric and inorganic membranes having is elicina bandwidth 100-2500 g/mol, preferably 150-1000 g/mol, most preferably 150-500 g/mol.

Typical polymeric membranes for nanofiltration used in the present invention include, for example, polyethersulfone membranes, sulfonated polyethersulfone membrane, polyester membrane, polysulfone membrane, membranes of aromatic polyamides, membranes of polyvinyl alcohol and paliperidone membranes and combinations thereof. Membranes for nanofiltration used in the present invention, can also be selected from cellulose acetate membranes.

Typical inorganic membranes include, for example, ZrO2and Al2O3-membrane.

Membranes for nanofiltration, which are used in the present invention, can have a negative or positive charge. The membrane may be ionic membranes, i.e. they may contain cationic or anionic groups, but are also used neutral membrane. Membranes for nanofiltration can be selected from a hydrophobic or hydrophilic membranes.

One form of membranes for nanofiltration is flat film form. The configuration of the membranes may also be selected, for example, tubes, spiral membranes and hollow fibers. Can also be used membranes with high shear, such as a vibrating membrane and a rotating membrane.

Lane is d procedure nanofiltration membranes for nanofiltration can be pre-processed, for example, alkaline detergent or ethanol.

In a typical operation nanofiltration processed syrup, such as syrup black treacle, is fed through the membrane for nanofiltration under conditions of temperature and pressure described above. The syrup thus fractionized on the fraction of low molar mass, including betaine (permeate), and the fraction with a high molar mass, including sucrose or other macromolecular components of the solution black treacle (retentate).

Equipment for nanofiltration used in the present invention contains at least one membrane element for nanofiltration, separating the feed material on retentate and permeate part. Equipment for nanofiltration is typically also includes means for controlling pressure and flow, such as pumps and valves and flow meters and pressure controllers. The equipment may also include multiple membrane elements for nanofiltration in various combinations, arranged in parallel or sequentially.

The permeate stream is changed in accordance with pressure. Generally in the normal range, the higher the pressure, the higher the flow. The flow also varies with temperature. Increasing the operating temperature increases the flow. However, at higher temperatures and at higher pressures there is tsya increased propensity to rupture. For inorganic membranes can be used in higher temperature ranges and pressures and pH than for polymeric membranes.

Nanofiltration in accordance with the present invention may be performed periodically or continuously. Procedure nanofiltration can be repeated one or more times. Can also be used for recirculation of the permeate and/or retentate back to the supply tank.

In addition to the stages of chromatographic fractionation and nanofiltration described above, the method according to the invention may include other processing, selected from, for example, softening ionoobmennoi processing or carbonization, dilution, concentration, for example by evaporation, pH adjustment and filtration before, after and/or between stages of chromatographic fractionation and nanofiltration.

Betaine obtained from chromatographic separation and/or nanofiltration, described above, may be concentrated by evaporation and then further purified by crystallization, ion exchange and/or other conventional cleaning methods.

In the examples and throughout the description and in the claims, we used the following definitions:

DS refers to the dry matter content measured by titration according to Karl Fischer and expressed in wt.%.

Flow refers to the amount (liters) of the solution penetrate the through the membrane for nanofiltration within one hour, calculated per square meter of membrane surface, l/(m2·h).

Retention refers to the share of metered connections held by the membrane. The higher the value of the holding, the less the number of connections that are transferred through the membrane:

Retention (%)= [(Power - Permeate)/Power] × 100,

where "Power" refers to the concentration in the feeding solution (expressed, for example, in g/l) and "Permeate" refers to the concentration in permeate solution (expressed, for example, in g/l).

HPLC means of liquid chromatography.

SMB mean chromatography simulated moving bed.

NF means nanofiltration.

DVB means divinylbenzene.

For example, the present invention uses the following membrane.

- Prolonged operation-5 DK (four-layer membrane consisting of a layer of polyester, polysulfone layer and two proprietary layers, with the maximum bandwidth from 150 to 300 g/mol, permeability (25° (C) 5.4 l/(m2·h·bar) and MgSO4-retention of 98% (2 g/l), manufacturer Osmonics),

- Prolonged operation-5 DL (four-layer membrane consisting of a layer of polyester, polysulfone layer and two proprietary layers, with the maximum bandwidth from 150 to 300 g/mol, permeability (25° (C) to 7.6 l/(m2·h·bar), MgSO4-retention of 96% (2 g/l), manufacturer Osmonics),

- NTR-7450 (IU the bran of sulfated polyethersulfone, with a maximum bandwidth of 500 to 1000 g/mol, permeability (25° (C) 9,4 l/(m2·h·bar), NaCl-retention of 51% (5 g/l), manufacturer Nitto Denco), and

- NF-200 (polimyeraznoi membrane having a maximum bandwidth of 200 g/mol, permeability (25° (C) 7-8 l/(m2·h·bar), NaCl-retention of 70%, the manufacturer Dow Deutschland),

TS-80 (manufacturer Trisep),

- AFT-60 (manufacturer PTI Advanced Filtration Inc.),

- Prolonged operation AG (manufacturer Osmonics),

- Prolonged operation G10 (thin-film membrane of the aromatic polyamide/polysulfone material, having a maximum bandwidth of 2500 g/mol, permeability (25° (C) 3.4 l/(m2·h·bar), NaCl-retention of 10%, retention of dextran (1500 g/ml) 95%, retention of glucose 50%, the manufacturer Osmonics),

- ASP 10 (membrane consisting of sulfonated polysulfone on the polysulfone having a permeability (25° (C) 16 l/(m2·h·bar), NaCl-retention of 10%, a manufacturer of Advanced Membrane Technology),

TS 40 (membrane consisting of a wholly aromatic polyamide having a permeability (25° (C) 5.6 l/(m2·h·bar), manufacturer TriSep),

- ASP 20 (membrane consisting of sulfonated polysulfone on the polysulfone having a permeability (25° (C) 12.5 l/(m2·h·bar), NaCl-retention of 20%, a manufacturer of Advanced Membrane Technology),

- UF-PES-4H (membrane consisting of Polief is sulfona on the polypropylene, with a maximum bandwidth of about 4000 g/mol, permeability (25° (C) from 7 to 17 l/(m2·h·bar), manufacturer Hoechst),

- NF-PES-10 (polyethersulfone membrane having a maximum bandwidth of 1000 g/mol, permeability (25° (C) from 5 to 11 l/(m2·h·bar), NaCl-retention of less than 15% (5 g/l), manufacturer Hoechst),

- NF45 (membrane consisting of aromatic polyamide having a permeability (25° (C) 4.8 l/(m2·h·bar), NaCl-retention 45%, manufacturer Dow Deutschland),

- SR-1 (manufacturer Koch),

- XN-40 (manufacturer Trisep),

- MPF-34 (composite membrane having a maximum bandwidth of 200 g/mol and retention of glucose 95% to 5% glucose solution, the manufacturer Koch).

Preferred and outreach to consumers for nanofiltration for the regeneration of the betaine is selected from sulfonated polysulfone membranes and paliperidone membranes. For example, special membranes used are: prolonged operation-5 DK and prolonged operation-5 DL for nanofiltration (manufacturer Osmonics), NF-45 and NF-200 for nanofiltration (manufacturer Dow Deutschland), SR-1 for nanofiltration (manufacturer Koch) and NTR-7450 for nanofiltration (manufacturer Nitto Denko).

The following examples illustrate the invention. The examples shall not be interpreted for any limitation of the invention.

Example 1

The separation of betaine and sucrose by nanofiltration

This example illustrates the separation of betaine and sucrose using different membranes for nanofiltration. The feeding solution used for nanofiltration, was a solution obtained from crystals of sucrose and betaine containing 50% betaine and 50% sucrose. Feed solution had a pH of 9.2 and a DS of 12.7%. Equipment used for nanofiltration, DSS was Labsta M20-filter. The nanofiltration was carried out using the full filter in the recirculation mode (constant concentration of power). Pressure nanofiltration was 30 bar, the speed of the cross flow of about 0.7 m/s and temperatures from 65 to 70°C. the Membranes used for nanofiltration below in Table 1.

Table 1 shows the content of the betaine (%) permeate-based chromatographic analysis (the sum of sucrose and betaine is 100%).

Table 1< / br>
The content of betaine in the permeate obtained during nanofiltration of the solution containing betaine and sucrose
MembraneThe content of betaine in the permeate, % DS
Prolonged operation-5 DL96
NF-4594
SR-184
NF-20069
XN-4089

Re ulitity show what nanofiltration significantly increases the amount of betaine in the dry matter of the nanofiltration permeate.

Example 2:Fractionation of beet black treacle chromatography

For fractionation was used experienced sequential chromatographic equipment with SMB. The equipment consisted of 6 series-connected columns, feed pump, pumps for circulation and pump for suantai water, as well as the intake valves and valves for the products in the treated streams. Each column had a height of 4.0 m and a diameter 0,111 M. Each column filled with a strongly acidic cation exchange resin in the form of a gel in Na+form with an average particle size of the resin 0.36 mm and DVB-content of 5.5%. The column temperature was 80°and as eluent water was used. Before chromatographic separation of beet molasses was carbonitriles sodium carbonate (dose 1.5% of the dry matter, temperature 60°C, reaction time 3 hours) and filtered Seitz filter under pressure using auxiliary filtering means Kenite 300 (predpochtite 1 kg/m2, thickening power of 1.0% of dry matter).

Chromatographic separation was carried out in 9-step sequence as follows (operations a, b and C occur simultaneously):

Step 1: Power nakachi the elk in column 1 and dilution fraction was washed from the column 6.

Step 2A: Power was pumped into the column 1 and the residual fraction was washed from the column 1.

Step 2b: Water was supplied to column 2 and the residual fraction was washed from the column 4.

Step 2c: Water was fed to the column 5 and dilution fraction was washed from the column 6.

Step 3A: Power was pumped into the column 1 and the residual fraction was washed from the column 1.

Step 3b: Water was supplied to column 2 and the residual fraction was washed from the column 4.

Step 3C: Water was fed to the column 5, and a sucrose fraction was washed from the column 6.

Step 4: Power was pumped to column 1, and a sucrose fraction was washed from the column 6.

Step 5: Water was supplied to column 1 and sucrose fraction enriched in betaine, for nanofiltration was washed from the column 6.

Step 6A: Water was supplied to column 1 and the residual fraction was washed from the column 2.

Step 6b: Water was supplied to column 3, and the residual fraction was washed from the column 5.

Step 6C: Water was supplied to column 6 and betainovuyu fraction was washed from the column 6.

Stage 7: Water was supplied to column 1 and betainovuyu fraction was washed from the column 6.

Step 8A: Water was supplied to column 1 and the residual fraction was washed from the column 3.

Step 8b: Water was fed to the column 4 and the residual fraction was washed from the column 6.

Step 9: Circulation is about all columns.

The volume and velocity of flows in different stages are shown in Table 2.

40,0
Table 2< / br>
Volume (litres) and flow rate (litres/hour)steps 1-9
12A2b2c3a3b3c456a6b6c78a8b9
Power3,01,3--6,5--4,3--------
Residual1,31,2-6,57,7---9,39,3--9,19,1-
Dilution3,0--3,0------ ------
Sucrose------12,64,3--------
Sucrose

for NF
--------6,9-------
Betainovuyu-----------4,012,2---
Circulation---------------9,3
The flow velocity40,030,027,769,230,035,558,255,055,055,023,755,055,055,055,0

Steps 1-9 was repeated (5 to 7 times)until he reached substantial equilibrium. The method was continued in the equilibrium stage. Fractions were collected and analysed by HPLC (resin Na+forms, 0.8 ml/min, 0,002 M Na2SO4, 85°). Structures of power and the collected fractions are shown in Table 3.

Table 3< / br>
The concentration and composition of food and the collected fractions
PowerCombined residualDilutionSucroseSucrose< / br>
for NF
Betainovuyu
Concentration, g/100 ml68,4a 4.9the 15.632,911,33,2
Sucrose, % DS63,18,649,5a 94.283,70,1
Betaine, % on DS5,90,20,00,014,295,6
Others, % on DS31,091,250,5/td> 5,82,14,4

Example 3. Nanofiltration sucrose fraction enriched in betaine obtained from chromatographic separation

Enriched with betaine sucrose fraction containing 80,9% sucrose and 14.5% betaine, obtained according to Example 2, was subjected to nanofiltration.

The nanofiltration was carried out using the same equipment as in Example 1. The power supplied to the nanofiltration, had DS 15.6 g/100 ml, temperature nanofiltration was 70°and pressure nanofiltration was 28 bar. Membranes for nanofiltration were prolonged operation-5 DL and prolonged operation-5 DK. The content of betaine in the nanofiltration permeate obtained from nanofiltration with prolonged operation-5 DL, was of 65.4%and the sucrose content in the permeate was 31.1 per cent. When used prolonged operation-5 DK as a membrane for nanofiltration, the content of betaine in the nanofiltration permeate, thus obtained, was 61,2% and the sucrose content in the permeate was 31,3 from DS.

Example 4: Nanofiltration enriched sucrose betanova fractions obtained from the chromatographic separation

Beet molasses was subjected to chromatographic fractionation, as described in Example 2, and was collected enriched sucrose betainovuyu fraction containing 17.9 percent sucrose from DS and 76.6% of betaine from DS. Thus obtained solution was preceded by the correctly processed to adjust the concentration of the solution to 17.3 g/100 ml, then he was subjected to nanofiltration.

The nanofiltration was carried out using the same equipment as in Example 1. The power supplied to the nanofiltration, had a DS of 15.3 g/100 ml, temperature nanofiltration was 70°and pressure nanofiltration was 48 bar. Membranes for nanofiltration were prolonged operation-5 DL and prolonged operation-5 DK. The content of betaine in the nanofiltration permeate obtained from nanofiltration with prolonged operation-5 DL, was to 79.2% and the sucrose content was 1.5% of the DS. When used prolonged operation-5 DK as a membrane for nanofiltration, the content of betaine in the nanofiltration permeate, thus obtained, was 81,3% and the sucrose content in the permeate was 1.3% of DS.

Betainovuyu fraction obtained from the chromatographic separation was therefore purified by nanofiltration to obtain the nanofiltration permeate, containing only minor amounts of sucrose. At the same time sucrose were regenerated from betanova faction by its concentration in retentate nanofiltration.

Example 5: Chromatographic fractionation of beet black treacle

In the fractionation was used sequential chromatographic equipment with SMB. The equipment consisted of three series-connected columns, feed pump, circulation pumps and pump for suantai water, and the intake valve and valves for the products to be processed flows. The column had a total length of 11.1 m (columns 1, 2 and 3 had a length of respectively 4,35 m 2,70 m 4,05 m) and a column diameter of 0.20 m Column was filled with a strongly acidic cation exchange resin in the form of a gel in Na+form, the average particle size of the resin was 0,41 mm and a DVB content of 6.5%. The column temperature was 80°C and water was used as eluent. Before chromatographic separation of the feed solution was filtered by filter Seitz under pressure using as an auxiliary means for filtering Kenite 300 (predpochtite 1 kg/m2submitted thickener 1% calculated on dry substance).

Chromatographic separation was carried out in 7-step sequence as follows (operations a, b and C occur simultaneously):

Step 1A: Power was pumped into the column 1 and the residual fraction was washed from the column 2.

Step 1b: Water was supplied to column 3 and betainovuyu fraction was washed from the column 3.

Stage 2: the Power was pumped to column 1 and betainovuyu fraction was washed from the column 3.

Step 3: Circulation in all columns.

Step 4A: Water was supplied to column 1 and the residual fraction was washed from the column 1.

Step 4b: Water was supplied to column 2 and the residual fraction was washed from the column 3.

Step 5: Water was supplied to column 1 and the residual fraction was washed from the column 3.

The stupa is 6: Water was supplied to column 1 and the fraction contains sucrose and betaine, was washed from the column 3.

Stage 7: Water was supplied to column 3, and the residual fraction was washed from the column 2.

The volume and velocity of flows in different stages are shown in Table 4.

Table 4< / br>
Volume (litres) and flow rate (litres/hour) in steps 1-7
1A1b234a4b567
Power3,0-20,0------
Residual3,0---18,018,022,022,018,0
Betainovuyu-32,020,0------
Sucrose+betainovuyu on NF-------6,0-
Circulation- --22,0-----
The flow velocity75,0140,0100,0115,0115,0115,0115,0115,0115,0

Steps 1-7 were repeated (5 to 7 times) until a balance is reached. The method is continued in the equilibrium state. Fractions were collected and analysed by HPLC (resin in the Na+form, 0.8 ml/min, 0,002 M Na2SO4, 85°C). Structures of power and the collected fractions are shown in Table 5.

Table 5.< / br>
The concentration and composition of food and the collected fractions
PowerSucrose+< / br>
betainovuyu on NF
ResidualBetainovuyu
Concentration, g/100 ml50,26,74,514.4V
Sucrose, % DS17,154,342,00,9
Betaine, % on DS48,66,00,385,9
Others, % on DS34,339,750,713,2

Example 6. Nanofiltration fractions containing sucrose and betaine obtained from the chromatographic fractionation

The fraction containing 45.9% of sucrose and 5.1% betaine obtained from the chromatographic fractionation carried out in accordance with Example 5 was subjected to nanofiltration.

The nanofiltration was carried out with the same equipment as in Example 1. Conditions nanofiltration were as follows: pH of 10.1, temperature 70°C, the speed of the cross flow is about 0.5 m/s Membrane for nanofiltration was prolonged operation-5 DL. The nanofiltration was carried out using diafiltration. She stopped when about 50% of the initial dry solids was passed through the membrane. The amount of food was 5 liters and the volume of concentrate in the end was 3.6 litres.

Feed composition and permeate obtained from nanofiltration, are shown in Table 6. Retention is shown in Table 7.

td align="center"> Amino acids
Table 6< / br>
Feed composition and permeate nanofiltration
NFDS,%% DS% DS
RaffinoseSucroseGlucoseInositolBetaineNaKCaClNO3SO4
Power13,30,745,92,00,35,1of 21.9the 3.654,570,020,180,170,12
Prolonged operation-5

DL(1)
8,710,018,0the 4.70,49,439,43,205,140,010,390,350,03
Power20,361,455,10,70,22,214,71,221,460,03<0,0050,010,14
Prolonged operation-5

DL(2)
2,330,014,33,40,37,139,84,274,910,010,130,11<0,086

Example 7: Chromatographic fractionation of beet black treacle

In fractionation was used experimental sequence the aspects of chromatographic equipment with SMB. Equipment, resin and conditions used for chromatography were the same as described in Example 2, except that the chromatographic separation was carried out in accordance with the following 9-step sequence of operations a, b and C occur simultaneously):

Step 1: Power was pumped into the column 1 and the diluted fraction was washed from the column 6.

Step 2A: Power was pumped into the column 2 and the residual fraction was washed from the column 1.

Step 2b: Water was supplied to column 2 and the residual fraction was washed from the column 4.

Step 2C: Water was fed to the column 5 and the diluted fraction was washed from the column 6.

Step 3A: Power was pumped into the column 1 and the residual fraction was washed from the column 1.

Step 3b: Water was supplied to column 2 and the residual fraction was washed from the column 4.

Step 3C: Water was fed to the column 5, and a sucrose fraction was washed from the column 6.

Step 4: Power was pumped to column 1, and a sucrose fraction was washed from the column 6.

Step 5: Water was pumped to column 1 and a fraction containing sucrose and betaine (sucrose+betainovuyu fraction)was washed from the column 6.

Step 6A: Water was supplied to column 1 and the residual fraction was washed from the column 2.

Step 6b: Water was supplied to column 3, and the residual fraction was washed out to the lance 5.

Step 6C: Water was supplied to column 6 and betainovuyu fraction was washed from the column 6.

Stage 7: Water was supplied to column 1 and betainovuyu fraction was washed from the column 6.

Step 8A: Water was supplied to column 1 and the residual fraction was washed from the column 3.

Step 8b: Water was fed to the column 4 and the residual fraction was washed from the column 6.

Step 9: Circulation in all columns.

The volume and velocity of flows in different stages are shown in Table 8.

Table 8< / br>
Volume (litres) and the flow velocity in steps 1-9
12A2b2c3a3b3c456a6b6c78a8b9
Power3,01,3--6,5--4,3--------
Residual-1,31,2 6,58,310,2--9,59,5--9,59,5-
Diluted3,0--3,0------------
Sucrose-------4,3--------
Sucrose + betainovuyu on NF--------6,9-------
Betainovuyu-----------4,012,2---
Circulation ---------------9,3
The flow velocity40,030,027,769,240,051,162,840,055,055,055,023,255,055,055,055,0

Steps 1-9 was repeated (5 to 7 times) until a balance is reached. The method is continued in the equilibrium state. Fractions were collected and analysed by HPLC (resin Na+forms, 0.8 ml/min, 0,002 M Na2SO4, 85°). The concentration and composition of food and the collected fractions are shown in Table 9.

Table 9< / br>
The concentration and composition of food and the collected fractions
PowerUnited residualDilutedSucroseSucrose + betainovuyu< / br>
for NF
Betainovuyu
Concentration, g/100 ml68,45,1 17,834,5a 12.73,3
Sucrose

% DS
63,110,760,895,987,50,1
Betaine,

% DS
5,90,20,00,011,094,6
Other,

% DS
31,0of 89.139,24,11,65,3

Example 8. Nanofiltration fractions containing 88% sucrose and 10% betaine obtained from chromatographic separation

The fraction containing 88% sucrose and 10% betaine (sucrose+betainovuyu fraction)obtained from the chromatographic fractionation, made in accordance with Example 7 was subjected to nanofiltration. The nanofiltration was carried out with the same equipment as in Example 1, a membrane for nanofiltration was NTR-7450, pressure nanofiltration was 15 bar and other conditions nanofiltration presented in Table 13. The food had a DS of 8.7%. In operation nanofiltration permeate and concentrate (retentate) were regenerated back into the supply tank (constant power).

The content of sucrose and betaine in the nanofiltration permeate is presented in Table 10.

the table 10 < / br>
Conditions nanofiltration and composition of the permeate
Nutrition: 10% betaine, 88% sucrose DSThe flows of mass, g/(m2h)The composition of the permeate,< / br>
% DS
Temperature< / br>
°With
Flow, l/(m2h)SucroseBetaineSucroseBetaine
405612705006726
607417406707126

Example 9: Chromatographic separation of nanofiltration

The permeate obtained from the nanofiltration of Example 8 was subjected to chromatographic fractionation for the separation of sucrose and betaine. In fractionation was used experienced sequential chromatographic equipment with SMB. The equipment consisted of 3 series-connected columns, feed pump, circulation pumps and pump for suantai water, as well as the intake valves and valves for the products to be processed flows. Each column had a height of 4.0 m and a diameter 0,111 m Columns were filled with strongly acidic cation exchange resin in the form of the El in Na +form, the average particle size of the resin was 0.35 mm and a DVB content of 5.5%. The column temperature was 80°C and water was used as eluent. Before chromatographic separation nanofiltered concentrated to a dry matter content of 51.5%.

Chromatographic separation was carried out in 8-step sequence as follows (operations a, b and C occur simultaneously).

Step 1: Power was pumped into the column 1 and the diluted fraction was washed from the column 3.

Step 2A: the Food was pumped to column 1, and a sucrose fraction was washed from the column 1.

Step 2b: Water was supplied to column 2 and diluted fraction was washed from the column 3.

Step 3A: Power was pumped to column 1, and a sucrose fraction was washed from the column 1.

Step 3b: Water was supplied to column 2 and betainovuyu fraction was washed from the column 3.

Step 4: Circulation in all columns.

Step 5: Water was supplied to column 3, and a sucrose fraction was washed from the column 2.

Step 6: Circulation in all columns.

Stage 7: Water was supplied to column 1, and a sucrose fraction was washed from the column 3.

Step 8: Circulation in all columns.

The volume and velocity of flows in different stages are shown in Table 11.

45,0
Table 11< / br> Volume (litres) and flow rate (litres/hour) in steps 1-8
12A2b3a3b45678
Power2,02,0-4,0------
Diluted2,0-2,0-------
Sucrose-2,0-4,0--10,5-10,5-
Betainovuyu----9,0-----
Circulation-----14,0-14,0-to 12.0
The flow velocity40,040,040,029,566,850,050,050,050,0

Steps 1 to 8 was repeated (5 to 7 times)until a balance is reached. The method is continued in the equilibrium state. Fractions were collected and analysed by HPLC (resin in the Na+form, 0.8 ml/min, 0,002 M Na2SO4, 85°C). The concentration and composition of nutrition and fractions are shown in Table 12.

Table 12< / br>
The concentration and composition of food and the collected fractions
PowerDilutedSucroseBetainovuyu
Concentration,

g/100 ml
63,76,913,5a 12.7
Sucrose

% DS
71,919,297,41,8
Betaine,

% DS
26,280,70,097,9
Another,

% DS
1,900,12,60,3

The output of sucrose in the chromatographic separation was 99.4 per cent and the output of betaine was 100,0%.

For the specialist in this area it is obvious that as technology developed the concept of the invention can be implemented p is slicznym way. The invention and its variants implementation is not limited to the above examples but may vary within the scope of the claims.

1. Method of regeneration of betaine from a solution containing betaine and sucrose, characterized in that the said solution is subjected to chromatographic separation and nanofiltration in any desired sequence with the regeneration fraction enriched in betaine and possible fraction enriched in sucrose, and chromatographic separation is carried out with the use of the material to fill all the columns selected from cation exchange resins and anion exchange resins, and the nanofiltration is carried out with the membrane for nanofiltration selected from polymeric and inorganic membranes having the maximum transmittance from 100 to 2500 g/mol.

2. The method according to claim 1, characterized in that the method comprises a stage further chromatographic fractionation and/or nanofiltration for the regeneration of another faction or other fractions enriched in betaine, and maybe another faction or other fractions enriched in sucrose and/or other factions products.

3. The method according to claim 1, characterized in that the said phase chromatographic fractionation and/or nanofiltration carried out successively in any desired sequence.

4. The method according to claim 1, the best of the decomposing those the method comprises a combination of successive stages of chromatographic fractionation and/or nanofiltration.

5. The method according to claim 1, characterized in that the method comprises a stage (a) on the specified solution containing betaine and sucrose, chromatographic fractionation with regeneration fraction enriched in betaine and sucrose, and possibly residual fraction,

(b) the implementation of nanofiltration specified fraction enriched in betaine and sucrose, with regeneration fraction enriched in betaine, and possibly a fraction enriched in sucrose.

6. The method according to claim 1, characterized in that the method comprises a stage (a) implementation of nanofiltration specified solution containing betaine and sucrose, with regeneration fraction enriched in betaine, and possibly a fraction enriched in sucrose

(b) implementation at a specified fraction enriched in betaine, chromatographic fractionation with the regeneration of the second fraction enriched in betaine, and possibly residual fraction.

7. The method according to claim 1, characterized in that the method comprises a stage (a) on the specified solution containing betaine and sucrose, chromatographic fractionation with regeneration fraction enriched in betaine, and possibly a fraction enriched in sucrose, and/or residual fraction, after which the trail is t at least one of the following stages:

(b) implementation of nanofiltration specified residual fraction from the regeneration fraction enriched in sucrose, and/or a fraction enriched in betaine, and possibly one or more other fractions

(c) implementation of nanofiltration specified fraction enriched in sucrose, with the regeneration of the second fraction enriched in sucrose, and/or a fraction enriched in betaine, and possibly one or more other fractions

(d) implementation of nanofiltration specified fraction enriched in betaine, with the regeneration of the second fraction enriched in betaine, and possibly one or more of the other factions.

8. The method according to claim 7 according to stage (b), characterized in that the specified one or more other factions include the fraction enriched with raffinati, and/or a fraction enriched coloring connections.

9. The method according to claim 8, characterized in that the fraction enriched with raffinati, regenerated as retentate nanofiltration.

10. The method according to claim 8, characterized in that the fraction enriched coloring compounds is regenerated as retentate nanofiltration.

11. The method according to claim 7 according to stage (b), further characterized by the regeneration of the nanofiltration permeate and return it in the chromatographic fractionation stage (a), to use it as eluent.

12. The method according to claim 7 according to stage (C), the tives such as those that the specified one or more other factions include the fraction enriched Inositol, a fraction enriched with amino acids, the fraction enriched with monosaccharides, and/or a fraction enriched in raffinati.

13. The method according to item 12, characterized in that the fraction enriched with raffinati, regenerated as retentate nanofiltration.

14. The method according to claim 7 according to stage (d), characterized in that the specified one or more other factions include the fraction enriched in sugars fraction enriched Inositol, and/or a fraction enriched with amino acids.

15. The method according to claim 1, characterized in that on the stage nanofiltration method, the fraction enriched in betaine, is recovered as the nanofiltration permeate.

16. The method according to claim 1, characterized in that on the stage nanofiltration method, the fraction enriched in sucrose is recovered as retentate nanofiltration.

17. The method according to claim 1, characterized in that the fraction enriched in betaine and/or a specified fraction enriched in sucrose, and/or the specified one or more other fractions are subjected to one or more other stages nanofiltration and/or chromatographic fractionation.

18. The method according to claim 5, characterized in that the residual fraction is enriched in salts.

19. The method according to claim 1, characterized in that the chromatographic fractionation method Prov who is using the material to fill in the columns, selected from cation exchange resins.

20. The method according to claim 19, characterized in that the specified cation exchange resin is a strongly acidic cation exchange resin.

21. The method according to claim 19, characterized in that the specified cation exchange resin is a weakly acidic cation exchange resin.

22. The method according to claim 1, characterized in that the chromatographic fractionation is carried out with the use of the material to fill all the columns selected from anion exchange resins.

23. The method according to item 22, wherein the specified anion-exchange resin is a weakly basic anion-exchange resin.

24. The method according to claim 19, characterized in that the resin is in the form of a monovalent metal.

25. The method according to paragraph 24, characterized in that said monovalent metal is predominantly Na+and/or+.

26. The method according to claim 19, characterized in that the resin is in the form of a divalent metal.

27. The method according to p, characterized in that said divalent metal is predominantly CA2+.

28. The method according to claim 19, characterized in that the resin has a styrene skeleton.

29. The method according to claim 19, characterized in that the resin is an acrylic skeleton.

30. The method according to claim 19, characterized in that the resin cross linked polystyrene.

31. The method according to claim 1, characterized in that Thu is in chromatographic fractionation method, the material to fill all the columns are selected from strongly acidic cation exchange resin, which is mostly in Na+and/or+the form and which has a styrene skeleton and cross-linked divinylbenzene.

32. The method according to claim 1, characterized in that the chromatographic fractionation method is performed as a periodic way.

33. The method according to claim 1, characterized in that the chromatographic fractionation method is carried out as the method with simulated moving bed.

34. The method according to claim 5, characterized in that the chromatographic fractionation method is carried out as a continuous method with a simulated moving bed.

35. The method according to claim 7, characterized in that the chromatographic fractionation method is carried out as a sequential way with the simulated moving bed.

36. The method according to claim 1, characterized in that the nanofiltration method is carried out with the membrane for nanofiltration selected from polymeric and inorganic membranes having a marginal amount of bandwidth from 150 to 1000 g/mol, preferably from 150 to 500 g/mol.

37. The method according to p, characterized in that stage nanofiltration method is carried out with the membrane for nanofiltration selected from the membranes for nanofiltration prolonged operation-5 DK, prolonged operation-5 DL, NF-45, NF-200, SR-1 and NTR-7450.

38. The method according to clause 37, wherein the membrane for nanofiltration choose from membranes for nanofiltration prolonged operation-5 DL and NTR-7450.

39. The method according to claim 1, the tives such as those the specified solution containing betaine and sucrose solution is obtained from sugar beets.

40. The method according to § 39, characterized in that said solution obtained from sugar beets, is a solution of black treacle.



 

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