CN110746469A - Method for separating isomaltulose mother liquor by simulated moving bed - Google Patents
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Abstract
The invention discloses a method for separating an isomaltulose mother liquor by a simulated moving bed, and relates to the technical field of separation of the isomaltulose mother liquor. The method comprises the following steps: firstly, adding water to dilute isomaltulose mother liquor, and obtaining supernatant after decoloration, centrifugation and membrane filtration concentration in sequence; then separating the supernatant by adopting a simulated moving bed, collecting solution at an extraction port and a raffinate port, and delivering the residual mother liquor to a sewage treatment station for biogas power generation; and finally, detecting the solution of the extraction opening and the raffinate opening by adopting a high performance liquid chromatography, and concentrating, crystallizing and drying to obtain isomaltulose and trehalulose products. According to the invention, the simulated moving bed continuous chromatographic separation is adopted, so that the separation of the isomaltulose and the trehalulose is realized from the isomaltulose mother liquor, the high-purity isomaltulose and trehalulose are obtained, the problems that the isomaltulose and the trehalulose in the isomaltulose mother liquor are difficult to separate and the mother liquor is wasted in industrial production are solved, the production efficiency is improved, and the production cost is saved.
Description
Technical Field
The invention relates to the technical field of separation of isomaltulose mother liquor, in particular to a method for separating isomaltulose mother liquor by a simulated moving bed.
Background
Isomaltulose (C)12H22O11·H2O), also called palatinose, is a reducing disaccharide formed by combining glucose and fructose through α -1,6 glycosidic bonds, is an isomer of sucrose and trehalulose, and naturally exists in honey and sugarcane, compared with sucrose, the palatinose is similar in taste, but has low sweetness which is only 42 percent of that of the sucrose, has the characteristics of lower melting point, no hygroscopicity and more stability under acidic conditions, has the characteristics of preventing decayed teeth and shielding peculiar smell, such as the fishy smell of DHA, the beany smell of soymilk and the like.
The preparation method of isomaltulose mainly comprises a microbial fermentation method, an enzyme conversion method, a plant transgenic method and a chemical synthesis method. The chemical synthesis method is difficult to synthesize the isomaltulose, and the technology of adopting a plant transgenic mode is not mature, so that the large-scale production cannot be realized. The production methods currently used industrially are microbial fermentation and enzymatic conversion. Microbial fermentation, which is to convert sucrose into isomaltulose by using sucrose isomerase in cells by taking microbial cells as carriers, and the production process comprises the following steps: microbial culture → bacterial filtration → decolorization → ion exchange → concentration → crystallization → separation. The enzyme conversion method is to extract sucrose isomerase from microbial cells, convert sucrose into isomaltulose by free enzyme or immobilized enzyme, and also convert glucose and fructose as raw materials to produce isomaltulose by enzyme method, and the production flow is as follows: raw material → sterilization → enzymatic conversion → decolorization → concentration → crystallization → separation → drying. The core technology of the two methods is the enzymatic catalysis for product conversion. According to the reported catalytic mechanism of sucrose isomerase, although different sucrose isomerase strains have different sources, when isomaltulose is produced by taking sucrose as a substrate, trehalulose is generated, but the proportion of the two is different. Through repeated recrystallization separation, isomaltulose in the mother liquor cannot be crystallized completely. Under the existing production conditions, mother liquor with approximate volume of 1/3 can not be utilized, the viscosity of the mother liquor is high, impurities are more, and the difficulty in extracting isomaltulose is increased; meanwhile, isomaltulose and trehalulose are isomers, and the separation difficulty is increased. Therefore, finding a suitable technique to extract more isomaltulose from the mother liquor and to obtain the byproduct trehalulose is key to improving the production process.
The separation of isomaltulose and trehalulose can be well achieved by high performance liquid chromatography using an amino chromatographic column, but this method is limited to research and analysis at low levels. CN104017028A discloses a method for separating isomaltulose and trehalulose from mother liquor by adopting a single-column method, which is small in separation amount, limited in laboratory environment and not suitable for large-scale production of isomaltulose.
Disclosure of Invention
The invention aims to provide a method for separating isomaltulose mother liquor by a simulated moving bed, which can obtain high-purity isomaltulose and trehalulose.
The invention adopts the following technical scheme:
a method for separating isomaltulose mother liquor by a simulated moving bed sequentially comprises the following steps:
s1, adding water to dilute the isomaltulose mother liquor, and obtaining supernatant after decoloring, centrifuging, membrane filtering and concentrating in sequence;
s2, separating the supernatant by adopting a simulated moving bed, collecting the solution of an extraction port and a raffinate port, and delivering the residual mother liquor to a sewage treatment station for biogas power generation;
and S3, detecting the solution of the extraction opening and the raffinate opening by adopting a high performance liquid chromatography, and concentrating, crystallizing and drying to obtain isomaltulose and trehalulose products.
As a preferred embodiment of the present invention, step S1 specifically includes: diluting the isomaltulose mother liquor with water until the sugar degree is 20-25 Be, heating the obtained diluted mother liquor to 50-55 ℃, adding activated carbon particles according to the proportion of 0.5-1% w/V for decoloring, and stirring; and centrifuging the mother liquor obtained after decolorization at 3000r/min, taking the supernatant mother liquor, and concentrating the supernatant mother liquor in a membrane filtration mode to obtain a feed liquid with the sugar degree of 60-70 Be, thereby obtaining the supernatant.
In another preferred embodiment of the present invention, in step S2, when separating the supernatant in the simulated moving bed, the adsorbent is strong acid cation exchange resin, and the eluent is deionized water.
Further, in step S2, filling the resin into a chromatographic column of a moving bed by a wet method, wherein a solvent filled in the chromatographic column is deionized water, running for 2-3 cycles at an eluent flow rate of 30-50mL/min to reach equilibrium under the assistance of a circulating pump, continuously introducing a feed liquid supernatant mother liquor and the eluent into the simulated moving bed, continuously discharging, running for 4-7 cycles to reach equilibrium under the assistance of the circulating pump, continuously collecting an isomaltulose solution at a residual extraction port, and continuously collecting a trehalulose solution at an extraction port.
Further, the separation conditions in the simulated moving bed are as follows: the temperature is 50-60 ℃, the pressure is less than or equal to 0.4Mpa, the flow rate of the feeding liquid is 60-80mL/min, the flow rate of the eluent is 100-480 mL/min, and the switching time of the valve is 300-480 s.
Further, the strong-acid cation exchange resin is K+、Ca2+Or Na+One kind of (1).
Further, the isomaltulose mother liquor mainly comprises 35-40% by mass of isomaltulose and 30-35% by mass of trehalulose.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention adopts a simulated moving bed system, realizes the separation of isomaltulose and trehalulose from the isomaltulose mother liquor, and obtains high-purity isomaltulose and trehalulose, wherein the purity of the isomaltulose is 98.7 percent at most; the purity of trehalulose is up to 96.2%.
The invention solves the problem that a large amount of isomaltulose and trehalulose are wasted because the isomaltulose mother liquor cannot be effectively utilized.
The method realizes the industrial separation of the isomaltulose mother liquor, has simple process, continuous production and high stability, reduces the production cost and improves the production efficiency.
Drawings
The invention is further described below with reference to the accompanying drawings:
FIG. 1 is a schematic structural diagram of a simulated moving bed according to the present invention;
FIG. 2 shows the use of strongly acidic Ca2+Chromatogram of resin separation result by using simulated moving bed: a-distilled water; b-isomaltulose; c-trehalulose;
FIG. 3 shows the use of strongly acidic Na+Chromatogram of separation result of type exchange resin filled simulated moving bed: a-distilled water; b-isomaltulose; c-trehalulose;
FIG. 4 shows the use of strongly acidic Na+Chromatogram of separation result of type exchange resin filled simulated moving bed: a-distilled water; b-isomaltulose; c-trehalulose;
in fig. 1: 1. the chromatographic column I, the chromatographic column II, the chromatographic column III, the chromatographic column 4, the chromatographic column IV, the chromatographic column 5, the chromatographic column V, the chromatographic column 6, the chromatographic column VI, the chromatographic column 7, the chromatographic column VII, the chromatographic column VIII, the chromatographic column VII, the chromatographic.
Detailed Description
The invention provides a method for separating isomaltulose mother liquor by a simulated moving bed, and in order to make the advantages and technical scheme of the invention clearer and clearer, the invention is explained in detail by combining specific embodiments.
As shown in fig. 1, the isomaltulose is separated by a simulated moving bed, and the simulated moving bed comprises a first chromatographic column 1, a second chromatographic column 2, a third chromatographic column 3, a fourth chromatographic column 4, a fifth chromatographic column 5, a sixth chromatographic column 6, a seventh chromatographic column 7, an eighth chromatographic column 8, a ninth chromatographic column 9, a tenth chromatographic column 10, an eleventh chromatographic column 11 and a twelfth chromatographic column 12 which are arranged side by side in sequence. Wherein, the 12 chromatographic columns are divided into I-IV areas, each area comprises 1-5 chromatographic columns, the chromatographic columns of each area are connected in series, the I area is a first chromatographic column, a second chromatographic column and a third chromatographic column, the II area is a fourth chromatographic column, a fifth chromatographic column, a sixth chromatographic column, a seventh chromatographic column and an eighth chromatographic column, the III area is a ninth chromatographic column, a tenth chromatographic column and an eleventh chromatographic column, and the IV area is a twelfth chromatographic column. The I area is positioned between the elution opening 13 and the extraction opening 14, the II area is positioned between the extraction opening 14 and the feed opening 15, the III area is positioned between the feed opening 15 and the raffinate opening 16, the I area and the VI area are communicated with eluent, the isomaltulose solution is collected by the extraction opening 14, the trehalulose solution is collected by the raffinate opening 16, and the residual mother liquor is discharged from the discharge opening 17.
The separated isomaltulose mother liquor is a liquid part which can not be further extracted by multiple concentration and crystallization in the process of producing isomaltulose by Langya platform group Hanikang company, and mainly comprises 35-40% of isomaltulose, 30-35% of trehalulose in mass fraction, and the balance of water and inevitable small amount of impurities.
The strongly acidic cation exchange resin mentioned in the present invention is K+、Ca2+Or Na+One of the crosslinking agents is styrene, which is available from Zhejiang Kogyo industries, Inc.
The purity calculation method of the invention is as follows:
the isomaltulose purity is equal to the isomaltulose mass in the product/total product mass x 100%
The purity of the trehalulose is equal to the mass of the iso-trehalulose in the product/the total mass of the product multiplied by 100%.
Example 1:
(1) adding water to dilute the isomaltulose mother liquor until the sugar degree is 25 Be, heating the diluted mother liquor to 50 ℃, adding activated carbon particles according to the proportion of 1% (w/V) for decoloring, and stirring for 20 minutes.
(2) Centrifuging the decolorized mother liquor for 10 minutes at 3000r/min, taking the supernatant mother liquor, and concentrating the supernatant mother liquor in a membrane filtration mode to obtain a feed liquid with the sugar degree of 60 Be.
(3) Separating the treated supernatant mother liquor by adopting a simulated moving bed, wherein the adsorbent is ZG SPC 106Ca2+Strong acid cation exchange resin, and eluent is deionized water. Filling the resin into a chromatographic column by adopting a wet method, wherein the solvent for filling the column is deionized water. The eluent flow rate was 50mL/min for 3 cycles to reach equilibrium with the aid of a circulation pump.
(4) Continuously introducing the feed liquid supernatant mother liquor and the eluent into the simulated moving bed, continuously discharging, operating for 6 periods to reach balance under the auxiliary action of the circulating pump, continuously collecting the isomaltulose solution at the raffinate port, and continuously collecting the trehalulose solution at the extraction port. The separation conditions were: the temperature is 60 ℃, the pressure is less than or equal to 0.4Mpa, the flow rate of the feeding liquid is 65mL/min, the flow rate of the eluent is 120mL/min, and the valve switching time is 400 s.
(5) And (4) detecting the purity of the collected isomaltulose and trehalulose by using a high performance liquid chromatography, wherein the method is as described in CN104017028A, the residual mother liquor is sent to a sewage treatment station for biogas power generation, and whether the step (6) is carried out or not is determined according to the detection effect.
(6) And (3) concentrating, crystallizing and drying the collected isomaltulose solution and trehalulose solution respectively to obtain isomaltulose and trehalulose products.
The effect before and after separation is shown in figure 2, through liquid chromatogram analysis, all the collected liquid from the extraction opening is isomaltulose solution, the collected liquid from the raffinate opening is trehalulose solution, the resin has high separation rate on isomaltulose and trehalulose, the separation effect is good, the separation of isomaltulose and trehalulose is realized, and the purity of isomaltulose obtained through calculation is 98.7% at most; the purity of trehalulose is up to 96.2%.
Example 2:
(1) adding water to dilute the isomaltulose mother liquor until the sugar degree is 25 Be, heating the diluted mother liquor to 55 ℃, adding activated carbon particles according to the proportion of 0.5% (w/V) for decoloring, and stirring for 20 minutes.
(2) Centrifuging the decolorized mother liquor for 10 minutes at 3000r/min, taking the supernatant mother liquor, and concentrating the supernatant mother liquor in a membrane filtration mode to obtain a feed liquid with the sugar degree of 60 Be.
(3) Separating the treated supernatant mother liquor by adopting a simulated moving bed, wherein an adsorbent is strong-acid cation exchange resin, and an eluant is deionized water. Filling the resin into a chromatographic column by adopting a wet method, wherein the solvent for filling the column is deionized water. Run 2 cycles at eluent flow rate of 40mL/min to reach equilibrium with the aid of a circulation pump.
(4) Continuously introducing the feed liquid supernatant mother liquor and the eluent into the simulated moving bed, continuously discharging, operating for 6 periods to reach balance under the auxiliary action of the circulating pump, continuously collecting the isomaltulose solution at the raffinate port, and continuously collecting the trehalulose solution at the extraction port. The separation conditions were: the temperature is 50 ℃, the pressure is less than or equal to 0.4Mpa, the flow rate of the feeding liquid is 60mL/min, the flow rate of the eluent is 120mL/min, and the valve switching time is 400 s.
(5) And (4) detecting the purity of the collected isomaltulose and trehalulose by using a high performance liquid chromatography, wherein the method is as described in CN104017028A, the residual mother liquor is sent to a sewage treatment station for biogas power generation, and whether the step (6) is carried out or not is determined according to the detection effect.
(6) And (3) concentrating, crystallizing and drying the collected isomaltulose solution and trehalulose solution respectively to obtain isomaltulose and trehalulose products.
As shown in FIG. 3, the effect before and after separation is poor because the resin has no degree of separation from isomaltulose and trehalulose, similar to the ratio of the content of isomaltulose to trehalulose in the initial dilution mother liquor, and the separation effect is poor, when the solution containing isomaltulose and trehalulose is collected from the extraction opening and the solution containing isomaltulose and trehalulose is collected from the raffinate opening by analyzing the liquid chromatogram.
Example 3:
(1) adding water to dilute the isomaltulose mother liquor until the sugar degree is 25 Be, heating the diluted mother liquor to 50 ℃, adding activated carbon particles according to the proportion of 1% (w/V) for decoloring, and stirring for 20 minutes.
(2) Centrifuging the decolorized mother liquor for 10 minutes at 3000r/min, taking the supernatant mother liquor, and concentrating the supernatant mother liquor in a membrane filtration mode to obtain a feed liquid with the sugar degree of 60 Be.
(3) The treated supernatant mother liquor adopts a moldPseudo-moving bed separation, wherein the adsorbent is ZG SPC 106Na+Strong acid cation exchange resin, and eluent is deionized water. Filling the resin into a chromatographic column by adopting a wet method, wherein the solvent for filling the column is deionized water. Under the assistance of a circulating pump, running for 3 periods at an eluent flow rate of 30mL/min to reach balance;
(4) continuously introducing the feed liquid supernatant mother liquor and the eluent into the simulated moving bed, continuously discharging, operating for 5 periods to reach balance under the auxiliary action of the circulating pump, continuously collecting the isomaltulose solution at the raffinate port, and continuously collecting the trehalulose solution at the extraction port. The separation conditions were: the temperature is 60 ℃, the pressure is less than or equal to 0.4Mpa, the flow rate of the feeding liquid is 70mL/min, the flow rate of the eluent is 120mL/min, and the valve switching time is 400 s.
(5) And (4) detecting the purity of the collected isomaltulose and trehalulose by using a high performance liquid chromatography, wherein the method is as described in CN104017028A, the residual mother liquor is sent to a sewage treatment station for biogas power generation, and whether the step (6) is carried out or not is determined according to the detection effect.
(6) And (3) concentrating, crystallizing and drying the collected isomaltulose solution and trehalulose solution respectively to obtain isomaltulose and trehalulose products.
As shown in FIG. 4, the effect before and after separation is shown, through liquid chromatogram analysis, the solution containing isomaltulose and a very small amount of trehalulose is collected from the extraction opening, the solution containing a small amount of isomaltulose and trehalulose is collected from the raffinate opening, the resin has a high separation degree on isomaltulose and trehalulose, the separation effect is good, the purity of isomaltulose is 86.9%, and the purity of trehalulose is 81.4%.
The parts which are not described in the invention can be realized by taking the prior art as reference.
It should be noted that: any equivalents, or obvious variations thereof, which may occur to those skilled in the art and which are commensurate with the teachings of this disclosure, are intended to be within the scope of this invention.
Claims (7)
1. A method for separating isomaltulose mother liquor by a simulated moving bed is characterized by sequentially comprising the following steps:
s1, adding water to dilute the isomaltulose mother liquor, and obtaining supernatant after decoloring, centrifuging, membrane filtering and concentrating in sequence;
s2, separating the supernatant by adopting a simulated moving bed, collecting the solution of an extraction port and a raffinate port, and delivering the residual mother liquor to a sewage treatment station for biogas power generation;
and S3, detecting the solution of the extraction opening and the raffinate opening by adopting a high performance liquid chromatography, and concentrating, crystallizing and drying to obtain isomaltulose and trehalulose products.
2. The method for separating isomaltulose mother liquor by using a simulated moving bed according to claim 1, wherein the method comprises the following steps: step S1 specifically includes: diluting the isomaltulose mother liquor with water until the sugar degree is 20-25 Be, heating the obtained diluted mother liquor to 50-55 ℃, adding activated carbon particles according to the proportion of 0.5-1% w/V for decoloring, and stirring; and centrifuging the mother liquor obtained after decolorization at 3000r/min, taking the supernatant mother liquor, and concentrating the supernatant mother liquor in a membrane filtration mode to obtain a feed liquid with the sugar degree of 60-70 Be, thereby obtaining the supernatant.
3. The method for separating isomaltulose mother liquor by using a simulated moving bed according to claim 1, wherein the method comprises the following steps: in step S2, when separating the supernatant in the simulated moving bed, the adsorbent is strong acid cation exchange resin, and the eluent is deionized water.
4. The method for separating isomaltulose mother liquor by using a simulated moving bed according to claim 3, wherein the method comprises the following steps: in step S2, filling the resin into a chromatographic column of a moving bed by a wet method, wherein a solvent filled into the chromatographic column is deionized water, operating for 2-3 periods at an eluent flow rate of 30-50mL/min to reach balance under the assistance of a circulating pump, continuously introducing a feeding liquid supernatant mother liquor and the eluent into the simulated moving bed, simultaneously discharging continuously, operating for 4-7 periods to reach balance under the assistance of the circulating pump, continuously collecting an isomaltulose solution at a raffinate port, and continuously collecting a trehalulose solution at an extraction port.
5. The method for separating isomaltulose mother liquor by using a simulated moving bed according to claim 4, wherein the method comprises the following steps: the conditions for separation in the simulated moving bed were: the temperature is 50-60 ℃, the pressure is less than or equal to 0.4Mpa, the flow rate of the feeding liquid is 60-80mL/min, the flow rate of the eluent is 100-480 mL/min, and the switching time of the valve is 300-480 s.
6. The method for separating isomaltulose mother liquor by using a simulated moving bed according to claim 3, wherein the method comprises the following steps: the strong-acid cation exchange resin is K+、Ca2+Or Na+One kind of (1).
7. The method for separating isomaltulose mother liquor by using a simulated moving bed according to claim 3, wherein the method comprises the following steps: the isomaltulose mother liquor mainly comprises 35-40% of isomaltulose and 30-35% of trehalulose by mass fraction.
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Cited By (1)
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| CN112920235A (en) * | 2021-01-29 | 2021-06-08 | 山东健奕宏生物制药有限公司 | Preparation method of isomalt |
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