CN114014950A - Method for preparing polydextrose by using glucose raffinate - Google Patents
Method for preparing polydextrose by using glucose raffinate Download PDFInfo
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- DLRVVLDZNNYCBX-UHFFFAOYSA-N Polydextrose Polymers OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(O)O1 DLRVVLDZNNYCBX-UHFFFAOYSA-N 0.000 title claims abstract description 118
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 title claims abstract description 60
- 239000008103 glucose Substances 0.000 title claims abstract description 60
- 229920001100 Polydextrose Polymers 0.000 title claims abstract description 59
- 239000001259 polydextrose Substances 0.000 title claims abstract description 59
- 229940035035 polydextrose Drugs 0.000 title claims abstract description 59
- 235000013856 polydextrose Nutrition 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000005342 ion exchange Methods 0.000 claims abstract description 41
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 36
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims abstract description 22
- 239000000600 sorbitol Substances 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 16
- 239000006227 byproduct Substances 0.000 claims abstract description 15
- DLRVVLDZNNYCBX-RTPHMHGBSA-N isomaltose Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)C(O)O1 DLRVVLDZNNYCBX-RTPHMHGBSA-N 0.000 claims abstract description 14
- 239000000047 product Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000007670 refining Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- AYRXSINWFIIFAE-SCLMCMATSA-N Isomaltose Natural products OC[C@H]1O[C@H](OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O)[C@@H](O)[C@@H](O)[C@@H]1O AYRXSINWFIIFAE-SCLMCMATSA-N 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000011347 resin Substances 0.000 claims description 30
- 229920005989 resin Polymers 0.000 claims description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 21
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- 150000001768 cations Chemical class 0.000 claims description 9
- 239000012043 crude product Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000004042 decolorization Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- 150000001450 anions Chemical class 0.000 claims description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 3
- 239000000460 chlorine Substances 0.000 claims description 3
- 229910052801 chlorine Inorganic materials 0.000 claims description 3
- 150000002016 disaccharides Chemical class 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 239000003957 anion exchange resin Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 238000000605 extraction Methods 0.000 claims 2
- 238000009835 boiling Methods 0.000 abstract description 5
- 230000005540 biological transmission Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- 238000013375 chromatographic separation Methods 0.000 description 9
- 238000005349 anion exchange Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 230000000379 polymerizing effect Effects 0.000 description 6
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 4
- 239000003456 ion exchange resin Substances 0.000 description 4
- 229920003303 ion-exchange polymer Polymers 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- NOEGNKMFWQHSLB-UHFFFAOYSA-N 5-hydroxymethylfurfural Chemical compound OCC1=CC=C(C=O)O1 NOEGNKMFWQHSLB-UHFFFAOYSA-N 0.000 description 3
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 3
- RJGBSYZFOCAGQY-UHFFFAOYSA-N hydroxymethylfurfural Natural products COC1=CC=C(C=O)O1 RJGBSYZFOCAGQY-UHFFFAOYSA-N 0.000 description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 2
- 235000013373 food additive Nutrition 0.000 description 2
- 239000002778 food additive Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 229920002261 Corn starch Polymers 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008120 corn starch Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 235000013325 dietary fiber Nutrition 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000005417 food ingredient Substances 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229920001542 oligosaccharide Polymers 0.000 description 1
- 150000002482 oligosaccharides Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0009—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Glucans, e.g. polydextrose, alternan, glycogen; (alpha-1,4)(alpha-1,6)-D-Glucans; (alpha-1,3)(alpha-1,4)-D-Glucans, e.g. isolichenan or nigeran; (alpha-1,4)-D-Glucans; (alpha-1,3)-D-Glucans, e.g. pseudonigeran; Derivatives thereof
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Sustainable Development (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Saccharide Compounds (AREA)
Abstract
The invention discloses a method for preparing polydextrose by using glucose raffinate, which comprises the steps of taking isomaltose hypgather byproduct glucose raffinate as a raw material, sequentially carrying out decoloration, ion exchange and concentration, mixing the concentrated glucose raffinate with sorbitol, heating to 140-160 ℃, keeping the temperature for 50-120 min, then adding citric acid, heating to 220-240 ℃, carrying out polymerization reaction for 60-150 min, adding water to melt the materials to obtain crude polydextrose, and refining to obtain the finished polydextrose. The glucose raffinate is refined, so that the sugar boiling temperature of the glucose raffinate is increased, the light transmission, chromaticity and other qualities of the crude polydextrose are improved, the refining cost of the polydextrose is reduced, and the quality of a finished product and the utilization rate of byproducts are improved.
Description
Technical Field
The invention belongs to the technical field of polydextrose preparation, and particularly relates to a method for preparing polydextrose by using glucose raffinate.
Background
Polydextrose is a novel water-soluble dietary fiber, is obtained by taking glucose and sorbitol as raw materials and carrying out polymerization reaction under acidic and vacuum conditions, has been approved by more than fifty countries as a health food ingredient to be used so far, is used for manufacturing a large amount of fiber-reinforced food, and has the function of keeping intestines and stomach unobstructed after being eaten. Research on polydextrose relatively early in the united states and japan, polydextrose has been approved by the FDA in the united states as a safe food additive. The research on polydextrose in China starts late, but develops rapidly, and at present, polydextrose is also included in food additives. The production of polydextrose is mainly characterized by that it is made up by using powdered glucose and sorbitol as raw material through the processes of polymerization at high-temp. and vacuum condition at home and abroad. However, the cost for preparing polydextrose is high at present, and the taste of polydextrose is influenced by the presence of some byproducts (such as 5-hydroxymethylfurfural) in the preparation process, so that the further processing and application of polydextrose are hindered.
Isomaltooligosaccharides are functional oligosaccharides and are widely used. At present, corn starch is mostly used as a raw material and is produced by using a biological enzyme technology, but the production of glucose is accompanied in the enzymolysis process, in order to improve the purity of isomaltooligosaccharide, the glucose is separated as a byproduct and is directly sold as glucose liquid, and the cost, the added value and the utilization rate are low.
Therefore, the method has important significance for improving the quality of the polydextrose, reducing the production cost of the polydextrose and comprehensively utilizing the glucose raffinate generated in the isomaltooligosaccharide production process.
Disclosure of Invention
Aiming at the problems of high content of polydextrose by-products, high production cost and waste of resources of glucose raffinate serving as a by-product in the production process of isomaltooligosaccharide in the prior art, the invention provides a method for preparing polydextrose by using glucose raffinate, wherein the glucose raffinate is refined, so that the sugar boiling temperature of the glucose raffinate is increased, the light transmission, chromaticity and other qualities of crude polydextrose are further improved, the refining cost of polydextrose is reduced, and the quality of a finished product and the utilization rate of the by-product are improved.
The invention is realized by the following technical scheme:
a method for preparing polydextrose by utilizing glucose raffinate comprises the following steps:
(1) using a glucose raffinate which is a byproduct of isomaltose hypgather as a raw material, and sequentially carrying out decoloration, ion exchange and concentration;
(2) mixing the concentrated glucose raffinate obtained in the step (1) with sorbitol, heating to 140-160 ℃, keeping the temperature for 50-120 min, adding citric acid, heating to 220-240 ℃, performing polymerization reaction for 60-150 min, and adding water to melt the materials to obtain a crude product of polydextrose;
(3) refining: refining the crude polydextrose in the step (2) to obtain a finished polydextrose product.
Further, in the step (1), the glucose raffinate contains 95-98wt% of glucose, 2-4wt% of disaccharide and 45-55 wt% of sugar.
Further, the decolorization in the step (1) adopts high-temperature high-sugar concentrated granular activated carbon for decolorization; the ion exchange is carried out by using sodium type cation and chlorine type anion resin; the concentration adopts a four-effect concentration process.
Further, in the step (1), the decoloring temperature is 75-80 ℃, the sugar concentration is 45-55%, and the flow rate is 0.8-1.2 BV/h; the ion exchange temperature is 45-55 ℃, the sugar concentration is 45-55%, and the flow rate is 2.5-4.5 BV/h.
Further, the sugar concentration after concentration in the step (1) is 60-65%.
Further, the dry basis ratio of the glucose solution to sorbitol to citric acid in the step (2) is 89:11: 0.45-0.65.
Further, the vacuum degree of the polymerization reaction in the step (2) is-0.07-0.1 MPa.
Further, the refining step in the step (3) is as follows: decolorizing, ion-exchanging, concentrating and drying.
Further, decoloring by using a high-sugar-concentration granular carbon column at 75-80 ℃, at 45-55% of sugar concentration and at a flow rate of 0.4-0.5 BV/h; the ion exchange adopts cation-anion-decolorizing resin-cation resin decolorizing ion exchange, and the cation: yin: decolorizing resin: yang =2:3:3:2, the ion exchange temperature is 45-55 ℃, the sugar concentration is 45-55%, and the flow rate is 2.5-4.5 BV/h.
Further, the decolorizing resin is chlorine type anion exchange resin.
In order to reduce the production cost of polydextrose and improve the utilization rate of byproducts, the method takes the chromatographic separation raffinate of isomaltooligosaccharide as a raw material, refines the raffinate through decolorization, ion exchange and other treatments after optimizing parameters, improves the sugar boiling temperature of the raffinate, further improves the light transmittance, chromaticity and other qualities of the polymerized crude polydextrose, improves the utilization rate of byproducts, reduces the production cost and improves the quality of finished products.
Advantageous effects
The method takes the glucose raffinate which is a chromatographic separation byproduct of isomaltose hypgather as a raw material to prepare the polydextrose, and can improve the utilization rate of the byproduct; the refining process of the raffinate is optimized, so that the sugar boiling temperature of the raffinate is increased, the light transmittance and the chromaticity of the material liquid after the polymerization of the polydextrose can be increased, the generation of byproducts is reduced, and the production cost is reduced.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
The glucose raffinates used in the following examples and comparative examples were those obtained after chromatographic separation of isomaltooligosaccharides, in which the glucose content (95-98) wt%, the disaccharide content (2-4) wt% and the sugar concentration (45-55)%.
Example 1
(1) Taking glucose raffinate obtained after chromatographic separation of isomaltooligosaccharide as a raw material, and decoloring by adopting high-temperature high-sugar-concentration granular activated carbon, wherein the decoloring temperature is 78 ℃, the sugar concentration is 50%, and the flow rate is 1.0 BV/h; performing ion exchange on the decolorized glucose raffinate, wherein Na is selected as ion exchange resin+Type cation and Cl-Type anion resin, ion exchange temperature is 50 ℃, sugar concentration is 50%, flow rate is 3 BV/h, and glucose is treated after ion exchangeGlucose raffinate is concentrated to 60% of sugar concentration by adopting four effects;
(2) putting the concentrated glucose raffinate into a polymerization reaction kettle, adding sorbitol into the reaction kettle, heating the reaction kettle to 150 +/-5 ℃ for 90min at a dry basis ratio of the glucose liquid to the sorbitol, and keeping the vacuum degree at-0.07 to-0.1 MPa; adding citric acid accounting for 0.53 percent of the total dry basis mass of the glucose and the sorbitol, keeping the vacuum degree at minus 0.07 to minus 0.1MPa, heating to 230 +/-5 ℃, polymerizing for 110min, and adding water to melt the materials to obtain a crude product of the polydextrose;
(3) and (3) decoloring the crude polydextrose by using a high-sugar concentrated granular carbon column at the decoloring temperature of 78 ℃, at the sugar concentration of 50 percent and at the flow rate of 0.5 BV/h, and performing ion exchange by using cation-anion-chloride anion exchange resin-cation resin after decoloring, wherein the resin ratio is positive: yin: decolorizing resin: and (3) sun =2:3:3:2, the ion exchange temperature is 50 ℃, the sugar concentration is 50 ℃, the flow rate is 3.5BV/h, and then the concentration and the drying are carried out to obtain the finished product of the polydextrose.
Example 2
(1) Taking glucose raffinate obtained after chromatographic separation of isomaltooligosaccharide as a raw material, and decoloring by adopting high-temperature high-sugar-concentration granular activated carbon at the decoloring temperature of 75 ℃, the sugar concentration of 45 percent and the flow rate of 1.2 BV/h; performing ion exchange on the decolorized glucose raffinate, wherein Na is selected as ion exchange resin+Type cation and Cl—The ion exchange temperature of the type anion resin is 50 ℃, the sugar concentration is 45 percent, the flow rate is 4.5BV/h, and the glucose raffinate after the ion exchange is concentrated to the sugar concentration of 60 percent by four effects;
(2) putting the concentrated glucose raffinate into a polymerization reaction kettle, adding sorbitol into the reaction kettle, heating the reaction kettle to 145 +/-5 ℃ at a dry basis ratio of 89:11, treating for 120min, and keeping the vacuum degree at-0.07 to-0.1 MPa; adding citric acid accounting for 0.53 percent of the total dry basis mass of the glucose and the sorbitol, keeping the vacuum degree at minus 0.07 to minus 0.1MPa, heating to 225 +/-5 ℃, polymerizing for 150min, and adding water to melt the materials to obtain a crude product of the polydextrose;
(3) and (3) decoloring the crude polydextrose by using a high-sugar concentrated granular carbon column at the decoloring temperature of 75 ℃, at the sugar concentration of 45 percent and at the flow rate of 0.5 BV/h, and performing ion exchange by using cation-anion-chloride anion exchange resin-cation resin after decoloring, wherein the resin ratio is positive: yin: decolorizing resin: and (4) sun =2:3:3:2, the ion exchange temperature is 50 ℃, the sugar concentration is 45 ℃, and the flow rate is 4.5BV/h, and then the concentration and the drying are carried out to obtain the finished product of the polydextrose.
Example 3
(1) Taking glucose raffinate obtained after chromatographic separation of isomaltooligosaccharide as a raw material, and decoloring by adopting high-temperature high-sugar-concentration granular activated carbon, wherein the decoloring temperature is 80 ℃, the sugar concentration is 55%, and the flow rate is 0.8 BV/h; performing ion exchange on the decolorized glucose raffinate, wherein Na is selected as ion exchange resin+Type cation and Cl—The ion exchange temperature is 55 ℃, the sugar concentration is 55 percent, the flow rate is 2.5BV/h, and the glucose raffinate after the ion exchange is concentrated to the sugar concentration of 60 percent by four effects;
(2) putting the concentrated glucose raffinate into a polymerization reaction kettle, adding sorbitol into the reaction kettle, heating the reaction kettle to 155 +/-5 ℃ for treatment for 60min, and keeping the vacuum degree at-0.07 to-0.1 MPa; adding citric acid accounting for 0.58 percent of the total dry basis mass of the glucose and the sorbitol, keeping the vacuum degree at minus 0.07 to minus 0.1MPa, heating to 235 +/-5 ℃, polymerizing for 70min, and adding water to melt the materials to obtain a crude product of the polydextrose;
(3) and (3) decoloring the crude polydextrose by using a high-sugar concentrated granular carbon column, wherein the decoloring temperature is 80 ℃, the sugar concentration is 55 percent, the flow rate is 0.4 BV/h, and after decoloring, carrying out ion exchange by adopting cation-anion-chloride anion exchange resin-cation resin, wherein the resin ratio is positive: yin: decolorizing resin: and (3) sun =2:3:3:2, the ion exchange temperature is 55 ℃, the sugar concentration is 55 ℃, the flow rate is 2.5BV/h, and then the concentration and the drying are carried out to obtain the finished product of the polydextrose.
Comparative example 1
(1) Concentrating glucose raffinate after chromatographic separation of isomaltooligosaccharide to 60% of sugar concentration;
(2) putting the glucose raffinate into a polymerization reaction kettle, adding sorbitol into the reaction kettle according to the dry basis ratio of the glucose liquid to the sorbitol of 89:11, heating to 160 ℃, treating for 60min, and keeping the vacuum degree at-0.07 to-0.1 MPa; adding citric acid accounting for 0.58 percent of the total dry basis mass of the glucose and the sorbitol, keeping the vacuum degree at minus 0.07 to minus 0.1MPa, heating to 235 +/-5 ℃, polymerizing for 70min, and adding water to melt the materials to obtain a crude product of the polydextrose;
(3) and (3) decoloring the crude polydextrose by using a high-sugar concentrated granular carbon column, wherein the decoloring temperature is 80 ℃, the sugar concentration is 55 percent, the flow rate is 0.4 BV/h, and after decoloring, carrying out ion exchange by adopting cation-anion-chloride anion exchange resin-cation resin, wherein the resin ratio is positive: yin: decolorizing resin: and (3) sun =2:3:3:2, the ion exchange temperature is 55 ℃, the sugar concentration is 55 ℃, the flow rate is 2.5BV/h, and then the concentration and the drying are carried out to obtain the finished product of the polydextrose.
Comparative example 2
(1) Performing carbon decolorization on glucose raffinate powder after chromatographic separation of isomaltooligosaccharide at 80 ℃, the sugar concentration of 30 percent and the flow rate of 1.2BV/h, performing ion exchange on 102 cation resin and 202 anion resin after decolorization at 40 ℃, the sugar concentration of 25 percent and the flow rate of 3.5BV/h, and performing four-effect concentration on the glucose raffinate after ion exchange until the sugar concentration is 60 percent;
(2) adding the glucose raffinate into a polymerization reaction kettle, adding sorbitol into the reaction kettle according to the dry basis ratio of the glucose liquid to the sorbitol of 89:11, heating to 155 +/-5 ℃, treating for 60min, and keeping the vacuum degree at minus 0.07 to minus 0.1 MPa; adding citric acid accounting for 0.58 percent of the total dry basis mass of the glucose and the sorbitol, keeping the vacuum degree at minus 0.07 to minus 0.1MPa, heating to 235 +/-5 ℃, polymerizing for 70min, and adding water to melt the materials to obtain a crude product of the polydextrose;
(3) and (3) decoloring the crude polydextrose by using a high-sugar concentrated granular carbon column, wherein the decoloring temperature is 80 ℃, the sugar concentration is 30 percent, the flow rate is 0.4 BV/h, and after decoloring, ion exchange is carried out by adopting cation-anion-chloride anion exchange resin-cation resin, and the resin ratio is positive: yin: decolorizing resin: and (3) sun =2:3:3:2, the ion exchange temperature is 40 ℃, the sugar concentration is 25 ℃, the flow rate is 2.5BV/h, and then the concentration and the drying are carried out to obtain the finished product of the polydextrose.
Comparative example 3
(1) Taking glucose raffinate obtained after chromatographic separation of isomaltooligosaccharide as a raw material, and decoloring by adopting high-temperature high-sugar-concentration granular activated carbon, wherein the decoloring temperature is 80 ℃, the sugar concentration is 55%, and the flow rate is 0.8 BV/h; performing ion exchange on the decolorized glucose raffinate, wherein Na is selected as ion exchange resin+Type cation and Cl—The ion exchange temperature is 55 ℃, the sugar concentration is 55 percent, the flow rate is 2.5BV/h, and the glucose raffinate after the ion exchange is concentrated to the sugar concentration of 60 percent by four effects;
(2) and (3) pumping the concentrated glucose raffinate into a polymerization reaction kettle, adding sorbitol and citric acid into the reaction kettle, wherein the ratio of glucose liquid to sorbitol: the dry basis ratio of citric acid is 89:11: 0.58, heating to 235 +/-5 ℃, polymerizing for 120min, and adding water to melt the materials to obtain a crude product of polydextrose;
(3) and (3) decoloring the crude polydextrose by using a high-sugar concentrated granular carbon column, wherein the decoloring temperature is 80 ℃, the sugar concentration is 55 percent, the flow rate is 0.4 BV/h, and after decoloring, carrying out ion exchange by adopting cation-anion-chloride anion exchange resin-cation resin, wherein the resin ratio is positive: yin: decolorizing resin: and (3) sun =2:3:3:2, the ion exchange temperature is 55 ℃, the sugar concentration is 55 ℃, the flow rate is 2.5BV/h, and then the concentration and the drying are carried out to obtain the finished product of the polydextrose.
And (3) polydextrose performance detection:
the polydextrose of examples 1 to 3 and comparative examples 1 to 3 was examined for the temperature of boiling of the glucose raffinate (. degree. C.), the transmittance of the crude polydextrose (%) and the content (%) of 5-hydroxymethylfurfural of the finished product, with the results shown in Table 1 below:
TABLE 1 results of testing the Performance of polydextrose in examples 1-3 and comparative examples 1-3
As can be seen from Table 1, increasing the temperature for decocting glucose and the distribution and polymerization of the polymerization process are beneficial to improving the light transmittance of the polymerized crude product polydextrose material liquid, influence the content of the by-product 5-hydroxymethylfurfural, and improve the quality of the finished product.
Claims (10)
1. A method for preparing polydextrose by using glucose raffinate is characterized by comprising the following steps:
(1) using a glucose raffinate which is a byproduct of isomaltose hypgather as a raw material, and sequentially carrying out decoloration, ion exchange and concentration;
(2) mixing the concentrated glucose raffinate obtained in the step (1) with sorbitol, heating to 140-160 ℃, keeping the temperature for 50-120 min, adding citric acid, heating to 220-240 ℃, performing polymerization reaction for 60-150 min, and adding water to melt the materials to obtain a crude product of polydextrose;
(3) refining: refining the crude polydextrose in the step (2) to obtain a finished polydextrose product.
2. The method according to claim 1, wherein the glucose raffinate in step (1) has a glucose content of 95-98wt%, a disaccharide content of 2-4wt% and a sugar concentration of 45-55%.
3. The preparation method according to claim 1, wherein the decolorization in step (1) is performed by high-temperature high-sugar concentrated granular activated carbon; the ion exchange is carried out by using sodium type cation and chlorine type anion resin; the concentration adopts a four-effect concentration process.
4. The preparation method according to claim 3, wherein the decolorizing temperature in the step (1) is 75-80 ℃, the sugar concentration is 45-55%, and the flow rate is 0.8-1.2 BV/h; the ion exchange temperature is 45-55 ℃, the sugar concentration is 45-55%, and the flow rate is 2.5-4.5 BV/h.
5. The method according to claim 1, wherein the concentration of the sugar after the concentration in the step (1) is 60 to 65%.
6. The preparation method according to claim 1, wherein the dry basis ratio of the glucose solution to sorbitol to citric acid in step (2) is 89:11: 0.45-0.65.
7. The preparation method according to claim 1, wherein the degree of vacuum in the polymerization reaction in the step (2) is-0.07 to 0.1 MPa.
8. The extraction method according to claim 1, wherein the refining step (3) is: decolorizing, ion-exchanging, concentrating and drying.
9. The extraction method according to claim 8, wherein the decolorization is carried out by using a high-sugar concentrated granular carbon column at 75-80 ℃, a sugar concentration of 45-55% and a flow rate of 0.4-0.5 BV/h; the ion exchange adopts cation-anion-decolorizing resin-cation resin decolorizing ion exchange, and the cation: yin: decolorizing resin: yang =2:3:3:2, the ion exchange temperature is 45-55 ℃, the sugar concentration is 45-55%, and the flow rate is 2.5-4.5 BV/h.
10. The method according to claim 9, wherein the decolorizing resin is a chlorine-type anion exchange resin.
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| CN115926015A (en) * | 2023-01-30 | 2023-04-07 | 山东百龙创园生物科技股份有限公司 | Low-polymerization-degree polydextrose and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR930001318B1 (en) * | 1990-04-19 | 1993-02-25 | 선일포도당 주식회사 | Polydextrose and process therefor |
| CN104212854A (en) * | 2014-09-22 | 2014-12-17 | 吉林省轻工业设计研究院 | Method for producing isomalto-oligosaccharide by using high-concentration starch |
| CN104356251A (en) * | 2014-10-27 | 2015-02-18 | 山东广博生物技术服务有限公司 | Method for producing polydextrose by taking starch as raw material |
| CN108084294A (en) * | 2017-12-27 | 2018-05-29 | 人良生物科技（上海）有限公司 | A kind of production technology of high-purity polydextrose |
-
2021
- 2021-12-17 CN CN202111548439.4A patent/CN114014950A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR930001318B1 (en) * | 1990-04-19 | 1993-02-25 | 선일포도당 주식회사 | Polydextrose and process therefor |
| CN104212854A (en) * | 2014-09-22 | 2014-12-17 | 吉林省轻工业设计研究院 | Method for producing isomalto-oligosaccharide by using high-concentration starch |
| CN104356251A (en) * | 2014-10-27 | 2015-02-18 | 山东广博生物技术服务有限公司 | Method for producing polydextrose by taking starch as raw material |
| CN108084294A (en) * | 2017-12-27 | 2018-05-29 | 人良生物科技（上海）有限公司 | A kind of production technology of high-purity polydextrose |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115926015A (en) * | 2023-01-30 | 2023-04-07 | 山东百龙创园生物科技股份有限公司 | Low-polymerization-degree polydextrose and preparation method thereof |
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