CN118344413A - New process for improving trehalose yield - Google Patents
New process for improving trehalose yield Download PDFInfo
- Publication number
- CN118344413A CN118344413A CN202310067814.6A CN202310067814A CN118344413A CN 118344413 A CN118344413 A CN 118344413A CN 202310067814 A CN202310067814 A CN 202310067814A CN 118344413 A CN118344413 A CN 118344413A
- Authority
- CN
- China
- Prior art keywords
- trehalose
- solution
- trehalase
- liquid
- mother liquor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- HDTRYLNUVZCQOY-UHFFFAOYSA-N α-D-glucopyranosyl-α-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OC1C(O)C(O)C(O)C(CO)O1 HDTRYLNUVZCQOY-UHFFFAOYSA-N 0.000 title claims abstract description 162
- HDTRYLNUVZCQOY-WSWWMNSNSA-N Trehalose Natural products O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-WSWWMNSNSA-N 0.000 title claims abstract description 162
- HDTRYLNUVZCQOY-LIZSDCNHSA-N alpha,alpha-trehalose Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-LIZSDCNHSA-N 0.000 title claims abstract description 162
- 238000000034 method Methods 0.000 title claims abstract description 29
- 230000008569 process Effects 0.000 title claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 99
- 239000007788 liquid Substances 0.000 claims abstract description 58
- 102100029677 Trehalase Human genes 0.000 claims abstract description 38
- 108010087472 Trehalase Proteins 0.000 claims abstract description 38
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- 239000012452 mother liquor Substances 0.000 claims abstract description 28
- 239000013078 crystal Substances 0.000 claims abstract description 24
- 238000000909 electrodialysis Methods 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000011084 recovery Methods 0.000 claims abstract description 7
- 239000012141 concentrate Substances 0.000 claims abstract description 5
- 238000004042 decolorization Methods 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- 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 claims description 29
- 239000008103 glucose Substances 0.000 claims description 28
- 238000002425 crystallisation Methods 0.000 claims description 26
- 230000008025 crystallization Effects 0.000 claims description 26
- 238000000605 extraction Methods 0.000 claims description 22
- 238000000926 separation method Methods 0.000 claims description 18
- 238000013375 chromatographic separation Methods 0.000 claims description 13
- 238000010612 desalination reaction Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- 238000002834 transmittance Methods 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 238000000855 fermentation Methods 0.000 claims description 7
- 230000004151 fermentation Effects 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 5
- 239000010413 mother solution Substances 0.000 claims description 5
- 241000195493 Cryptophyta Species 0.000 abstract 1
- 108090000790 Enzymes Proteins 0.000 description 15
- 102000004190 Enzymes Human genes 0.000 description 15
- 229940088598 enzyme Drugs 0.000 description 15
- 238000001914 filtration Methods 0.000 description 13
- 238000005516 engineering process Methods 0.000 description 9
- 239000012528 membrane Substances 0.000 description 9
- 239000000047 product Substances 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 7
- 238000005342 ion exchange Methods 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000011033 desalting Methods 0.000 description 5
- 238000001728 nano-filtration Methods 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 description 4
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 description 4
- 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 4
- 238000004094 preconcentration Methods 0.000 description 4
- 108090000637 alpha-Amylases Proteins 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 3
- 238000005341 cation exchange Methods 0.000 description 3
- 238000004587 chromatography analysis Methods 0.000 description 3
- 235000008504 concentrate Nutrition 0.000 description 3
- 238000010924 continuous production Methods 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- -1 facial mask Substances 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 108010039327 maltooligosyl trehalose synthase Proteins 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229920000856 Amylose Polymers 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- FYGDTMLNYKFZSV-DZOUCCHMSA-N alpha-D-Glcp-(1->4)-alpha-D-Glcp-(1->4)-D-Glcp Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)O[C@H](O[C@@H]2[C@H](OC(O)[C@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O FYGDTMLNYKFZSV-DZOUCCHMSA-N 0.000 description 2
- 238000005349 anion exchange Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007071 enzymatic hydrolysis Effects 0.000 description 2
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 230000001815 facial effect Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 108010074674 maltooligosyl trehalose trehalohydrolase Proteins 0.000 description 2
- 210000000214 mouth Anatomy 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- DBTMGCOVALSLOR-UHFFFAOYSA-N 32-alpha-galactosyl-3-alpha-galactosyl-galactose Natural products OC1C(O)C(O)C(CO)OC1OC1C(O)C(OC2C(C(CO)OC(O)C2O)O)OC(CO)C1O DBTMGCOVALSLOR-UHFFFAOYSA-N 0.000 description 1
- 208000032544 Cicatrix Diseases 0.000 description 1
- RXVWSYJTUUKTEA-UHFFFAOYSA-N D-maltotriose Natural products OC1C(O)C(OC(C(O)CO)C(O)C(O)C=O)OC(CO)C1OC1C(O)C(O)C(O)C(CO)O1 RXVWSYJTUUKTEA-UHFFFAOYSA-N 0.000 description 1
- 108090000604 Hydrolases Proteins 0.000 description 1
- 102000004157 Hydrolases Human genes 0.000 description 1
- 108010028688 Isoamylase Proteins 0.000 description 1
- 239000004909 Moisturizer Substances 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 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 1
- 239000003513 alkali Substances 0.000 description 1
- 102000004139 alpha-Amylases Human genes 0.000 description 1
- 229940024171 alpha-amylase Drugs 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 108010019077 beta-Amylase Proteins 0.000 description 1
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000002016 disaccharides Chemical class 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000005452 food preservative Substances 0.000 description 1
- 235000019249 food preservative Nutrition 0.000 description 1
- 235000003599 food sweetener Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000003014 ion exchange membrane Substances 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- FYGDTMLNYKFZSV-UHFFFAOYSA-N mannotriose Natural products OC1C(O)C(O)C(CO)OC1OC1C(CO)OC(OC2C(OC(O)C(O)C2O)CO)C(O)C1O FYGDTMLNYKFZSV-UHFFFAOYSA-N 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000001333 moisturizer Effects 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 150000002840 non-reducing disaccharides Chemical class 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 231100000241 scar Toxicity 0.000 description 1
- 230000037390 scarring Effects 0.000 description 1
- 230000037387 scars Effects 0.000 description 1
- 235000011496 sports drink Nutrition 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000003765 sweetening agent Substances 0.000 description 1
- 239000006188 syrup Substances 0.000 description 1
- 235000020357 syrup Nutrition 0.000 description 1
- 108010045348 trehalose synthase Proteins 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- FYGDTMLNYKFZSV-BYLHFPJWSA-N β-1,4-galactotrioside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@H](CO)O[C@@H](O[C@@H]2[C@@H](O[C@@H](O)[C@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O FYGDTMLNYKFZSV-BYLHFPJWSA-N 0.000 description 1
Landscapes
- Saccharide Compounds (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention relates to the technical field of trehalose preparation, and particularly provides a novel process for improving the yield of trehalose. The invention takes trehalase conversion solution and the trehalase solution which is chromatographically separated after the trehalase conversion solution is recovered for one time as mixed solution, and desalts by decolorization and electrodialysis to obtain desalted solution; crystallizing when the sea algae sugar content in the desalted liquid is 90-97% and the total sugar concentration is 60-65%, so as to obtain crystal concentrated solution; centrifugally separating the crystal concentrate, and drying the solid part to obtain trehalose crystals; the liquid part is used as primary mother liquor to produce trehalose liquid. The novel process provided by the invention can effectively improve the recovery rate of trehalose in the trehalase conversion solution and improve the purity of the trehalose.
Description
Technical Field
The invention relates to the technical field of trehalose preparation, in particular to a process for improving the yield of trehalose.
Background
Trehalose is a non-reducing disaccharide formed by condensing two glucopyranose molecules through alpha-1, 1 glycosidic bonds, has the characteristic of protecting biological activity under extreme conditions, and has the reputation of being a "life sugar" in the scientific community. The trehalose has wide market prospect and multiple uses, and can be used as an excellent food preservative and an excellent anti-denaturation agent in the aspect of food application; the health care food can be developed into special health care food for diabetics, and can also be developed into sports drink for providing energy and relieving fatigue pressure; the product can be used as moisturizer, protectant, etc. added into lotion, facial mask, essence, facial cleanser, etc., and can also be used as sweetener and quality improver for lipstick, oral cavity cleaner, oral cavity aromatic, etc.; can be used as specific protectant of biological molecule and stabilizer of tissue cell in medicine.
The current method for industrially producing trehalose mainly adopts an enzyme conversion method, including a single enzyme method and a double enzyme method. The single enzyme method uses maltose as a substrate and converts the maltose into trehalose in one step. The double enzyme method is to use amylose or maltooligosaccharide as a substrate, convert the amylose or maltooligosaccharide into a mixed sugar solution which mainly contains trehalose and a small amount of partial unconverted sugar such as glucose, maltose, maltotriose and the like through the combined action of MTSase (maltooligosyl trehalose synthase) and MTHase (maltooligosyl trehalose hydrolase), then further hydrolyze the unconverted sugar through adding saccharifying enzyme, and finally obtain the enzymolysis conversion solution mainly containing glucose and trehalose.
The currently common extraction and separation processes of trehalose comprise chromatographic separation processes and nanofiltration separation processes. The specific process flow is as follows: firstly, purifying pretreatment steps such as high-temperature enzyme deactivation, active carbon decoloration, plate and frame filtration for removing proteins, ion exchange desalination and the like are carried out on enzymolysis conversion solution, then glucose and trehalose in the enzymolysis conversion solution are separated through simulated moving bed chromatography or nanofiltration membrane to obtain a sugar solution mainly containing single-component trehalose, and finally, the finished product crystalline trehalose is finally obtained through steps such as evaporation concentration, cooling crystallization or organic solvent precipitation, centrifugal separation, drying and the like.
The electrodialysis technology is one of the new membrane separation technologies, and the electrodialysis principle is to alternately arrange anion and cation exchange membranes between positive and negative electrodes, separate the anion and cation exchange membranes by a special partition plate to form two systems of desalination (desalination) and concentration, and under the action of a direct current electric field, the potential difference is used as a driving force, and the selective permeability of the ion exchange membranes is utilized to desalinate a part of water and concentrate a part of water to separate electrolyte from solution, thereby realizing concentration, desalination, refining and purification of the solution. The uncharged monosaccharides, disaccharides and the like in the sugar solution enter the desalting chamber, and anions and cations such as inorganic salts and the like in the sugar solution enter the concentrated water chamber through the anion-cation exchange membrane so as to realize the purpose of desalting. Compared with the ion exchange technology, the electrodialysis technology does not need to regenerate the resin acid and alkali, can realize continuous production, and has less produced sewage.
The DTB type evaporative crystallizer is a slurry circulation type crystallizer, the lower part of the crystallizer is connected with an elutriation column, a guide cylinder and a cylindrical baffle are arranged in the crystallizer, during operation, hot saturated feed liquid is continuously added to the lower part of a circulation pipe, is mixed with mother liquid with small crystals entrained in the circulation pipe and then is pumped to a heater, and the heated solution flows into the crystallizer near the bottom of the guide cylinder and is conveyed to the liquid level along the guide cylinder by a slowly rotating screw. The solution evaporates at the liquid level to reach a supersaturated state, wherein part of the solute is deposited on the surface of suspended particles, so that crystals grow up. A sedimentation zone is arranged at the periphery of the annular baffle plate. In the sedimentation zone, large particles are settled, while small particles are introduced into the circulation pipe along with the mother liquor and dissolved by heating. The crystals enter an elutriation column at the bottom of the crystallizer.
The existing trehalose production process adopts twice decolorization, twice ion exchange and twice concentration processes, the production process route is long, the process loss is more, and the extraction yield is low; the enzymolysis liquid is separated and purified by adopting a chromatographic separation technology or a membrane separation technology, so that the equipment treatment load is large and the investment cost is high; secondly, by adopting an evaporation concentration cooling crystallization process, crystals can adhere to the inner wall of a crystallizer to form scars, so that the heat transfer and crystallization efficiency are affected, the viscosity of sugar liquid is increased along with the reduction of the temperature, the subsequent centrifugal separation is not facilitated, the purity and the yield of a final product are affected, and by adopting the cooling crystallization process, the cooling energy consumption is high, the continuous production is not realized, the equipment utilization rate is low, and the production cost is high; the primary mother liquor after crystallization separation is not recycled or is simply concentrated and separated to recycle part of trehalose, and the secondary mother liquor is not further recycled.
Disclosure of Invention
The invention provides a novel process for improving the yield of trehalose, which is used for solving the defect of low recovery rate of the enzymatic hydrolysis conversion liquid of the trehalose in the prior art and realizing the extraction of all the trehalose in the enzymatic hydrolysis conversion liquid.
In a first aspect, the present invention provides a trehalose extraction process comprising:
(1) The trehalase conversion solution and the trehalase conversion solution are used as mixed solution, and desalted solution is obtained through decolorization and electrodialysis;
(2) Adjusting the trehalose content in the desalted liquid to 90-97%, concentrating and crystallizing at a total sugar concentration of 60-65%, and obtaining a crystallized concentrated liquid, wherein the crystallization temperature is 55-60 ℃, and the vacuum degree is-0.085 to-0.095 Mpa;
(3) Centrifugally separating the crystal concentrate, and drying the solid part to obtain trehalose crystals; the liquid fraction is used as primary mother liquor for the production of trehalose solution.
The crystallizer used in the crystallization in the step (2) is a DTB crystallizer, and the invention discovers that the most suitable trehalose concentration and total sugar concentration are obtained when the DTB crystallizer is used for the first time.
For the total sugar concentration and the trehalose concentration in the desalted liquid, when the total sugar concentration of the pre-concentration of the desalted liquid does not reach the trehalose saturation concentration, the concentrated liquid entering the DTB crystallizer cannot be immediately crystallized and separated out, so that the crystallization yield of the trehalose is low; when the concentration of total sugar in the pre-concentration of the desalted liquid exceeds the supersaturated concentration, a large amount of fine crystals are separated out after entering a DTB crystallizer, so that impurities are wrapped in the crystals, and meanwhile, mother liquor is not easy to separate from the crystals, and finally, the purity of the crystallized trehalose is lower.
In the trehalose extraction process provided by the invention, the total sugar and the trehalose content of the desalted liquid in the step (2) are adjusted by adopting the crude trehalose.
In the trehalose extraction process provided by the invention, after the primary mother liquor is concentrated, the secondary mother liquor and crude trehalose are obtained through centrifugal separation; and (3) carrying out chromatographic separation on the secondary mother solution to obtain trehalose solution and trehalase conversion solution which are used as mixed solution.
In the trehalose extraction process provided by the invention, the secondary mother liquor is subjected to chromatographic separation, and the obtained glucose solution is used for trehalase conversion fermentation.
The invention realizes the effective recovery of all substances of the trehalase conversion liquid, wherein all trehalase can be converted into trehalase crystals in multiple collection, and the glucose liquid is recovered for trehalase conversion fermentation.
In the trehalose extraction process provided by the invention, after the primary mother liquor is concentrated to 75-80% of total sugar concentration, the temperature of the primary mother liquor is reduced to 12-15 ℃ for crystallization, crude trehalose is obtained, and the crude trehalose is added into the desalted liquid in the step (2).
In the trehalose extraction process provided by the invention, the content of the trehalose in the mixed solution is 85-90%.
In the trehalose extraction process provided by the invention, electrodialysis desalination is carried out by using a filtering liquid with the light transmittance more than 95%.
In a second aspect, the invention provides trehalose, which is prepared by the preparation method, wherein the purity of the trehalose is 99.5-99.8%.
The invention also provides application of the preparation method in improving the recovery rate of trehalase conversion solution according to the understanding of the person skilled in the art.
The invention also provides the application of the preparation method in improving the purity of trehalose according to the understanding of the person skilled in the art.
The invention has the beneficial effects that:
the novel process provided by the invention can realize the extraction of all trehalose in the enzymolysis conversion solution. The invention has simple extraction process, low equipment investment and high yield of crystalline trehalose which can reach 102 percent (theoretical value 110.5 percent).
The calculation method of the theoretical yield value of the crystalline trehalose comprises the following steps: the trehalose in the solution was present in the form of trehalose with a molecular weight of 342, whereas the solid trehalose obtained by concentration crystallization was crystalline trehalose containing two crystal waters with a molecular weight of 378. For example, if 1L of trehalose is contained in a solution having a trehalose concentration of 342g/L and this portion of trehalose is completely crystallized and recovered to be crystalline trehalose, 1mol of crystalline trehalose can be recovered, and the crystalline trehalose is 378g in mass and the recovery rate of crystallization is 378/342=1.105.
Specifically, the invention adopts the DTB internal circulation crystallizer, concentrates and crystallizes simultaneously, avoids the phenomenon of inner wall scarring in the cooling crystallization process, can realize continuous production, and has high equipment utilization rate; compared with the ion exchange desalination technology, the electrodialysis desalination technology does not need repeated acid-base regeneration, saves water resources and has less sewage discharge;
The invention realizes the concentration and crystallization of the primary mother solution to recycle the crude trehalose through process optimization, the secondary mother solution can simultaneously obtain glucose solution and trehalose solution through chromatographic separation, the treatment load of chromatographic equipment is small, the investment is low, the glucose solution is recycled for fermentation enzyme production, and the trehalose solution is fully recycled.
Drawings
In order to more clearly illustrate the invention or the technical solutions of the prior art, the following description will briefly explain the drawings used in the embodiments or the description of the prior art, and it is obvious that the drawings in the following description are some embodiments of the invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow chart of a novel process for improving trehalose yield.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Measuring the DE value of liquefied liquid by referring to a measuring method of the DE value of glucose syrup in GB/T20885-2007;
trehalose and glucose determination reference high performance liquid chromatography in GB/T23529-2009;
The light transmittance is measured under the condition of a spectrophotometer at 430 nm;
The conductivity was measured using a conductivity meter.
EXAMPLE 1 preparation of trehalase-based conversion solution
Taking 25-35% of starch milk as a raw material, adding high-temperature alpha-amylase for 105 ℃ jet liquefaction to obtain liquefied liquid with DE 5-15, adding beta-amylase, pullulanase, maltose generating enzyme and trehalose synthase for conversion by a single enzyme method referring to a patent CN108048439B to obtain trehalose conversion liquid, adding pullulanase or isoamylase, MTSase and MTHase for conversion by a double enzyme method referring to a patent CN103468624B to obtain trehalose conversion liquid, adding saccharifying enzyme, and finally converting all unconverted sugar into glucose to obtain mixed sugar liquid containing 70-85% of trehalose and 15-30% of glucose.
Example 2 novel trehalose extraction Process
The embodiment provides a novel trehalose extraction process, the flow diagram is shown in fig. 1, and the specific scheme is as follows:
(1) Mixing trehalase conversion solution and chromatographic separation trehalose solution to obtain mixed solution with trehalose content of 85%, adding 0.2% of sugar carbon, maintaining at 50deg.C for 40min, and filtering with plate frame to obtain filtrate with light transmittance of more than 95%;
(2) Electrodialysis desalination is carried out on the filtered solution, and the current density is 20mA/cm < 2 > to obtain desalted solution with the conductivity less than 50 mu S/cm;
(3) Dissolving crude crystalline trehalose in desalted liquid, wherein the content of the trehalose in the desalted liquid reaches 92%, concentrating under reduced pressure by a single-effect evaporator at 70 ℃ and vacuum degree of-0.085 MPa, continuously concentrating and crystallizing when the total sugar concentration reaches 65%, and stirring at 60 ℃ and speed of 100rpm;
(4) The crystal slurry is continuously discharged from the elutriation column, and is centrifugally separated and dried for 4 hours at 60 ℃ to obtain a crystalline trehalose finished product, the purity of the trehalose can reach 99.5%, and the yield of the trehalose can reach 99.5%.
(5) And (3) performing centrifugal separation to obtain primary mother liquor, concentrating the total sugar concentration in the mother liquor to 75% by using a single-effect evaporator, cooling to 15 ℃ for crystallization, performing centrifugal separation to obtain crude crystalline trehalose, wherein the trehalose content can reach 95.4%, and adding the crude crystalline trehalose into the desalted liquid for re-dissolution.
(6) Separating the secondary mother liquor by chromatography to obtain trehalose solution and glucose solution, wherein the trehalose content in the trehalose solution is 97.2%, the glucose content in the glucose solution is 98.1%, the trehalose solution is mixed with the trehalase conversion solution in the step (1), and the glucose solution is recycled to the fermentation enzyme production process.
Example 3 novel trehalose extraction Process
(1) Mixing trehalase conversion solution and chromatographic separation trehalase solution to obtain mixed solution with trehalase content of 90%, adding 0.5% sugar carbon, maintaining at 50deg.C for 40min, and filtering with plate frame to obtain filtrate with light transmittance of more than 95%;
(2) Electrodialysis desalination is carried out on the filtered solution, and the current density is 30mA/cm < 2 > to obtain desalted solution with the conductivity less than 50 mu S/cm;
(3) Dissolving crude crystalline trehalose in desalted liquid, wherein the content of the trehalose in the desalted liquid reaches 97%, concentrating under reduced pressure by a single-effect evaporator at a concentration temperature of 60 ℃ and a vacuum degree of-0.095 MPa, continuously concentrating and crystallizing when the total sugar concentration reaches 65%, and stirring at a crystallization temperature of 55 ℃ and a stirring speed of 150rpm;
(4) The crystal slurry is continuously discharged from the elutriation column, and is subjected to centrifugal separation and drying at 60 ℃ for 4 hours to obtain a crystalline trehalose finished product, wherein the purity of the trehalose can reach 99.7%, and the yield of the trehalose can reach 102.3%.
(5) And (3) performing centrifugal separation to obtain primary mother liquor, concentrating the total sugar concentration in the mother liquor to 80% by using a single-effect evaporator, cooling to 12 ℃ for crystallization, performing centrifugal separation to obtain crude crystalline trehalose, wherein the trehalose content can reach 97.1%, and adding the crude crystalline trehalose into the desalted liquid for re-dissolution.
(6) The secondary mother liquor is subjected to chromatographic separation to obtain trehalose solution and glucose solution, wherein the trehalose content in the trehalose solution is 97.5%, the glucose content in the glucose solution is 98.2%, the trehalose solution is mixed with the trehalase conversion solution in the step (1), and the glucose solution is recycled to the fermentation enzyme production process.
Example 4 novel trehalose extraction Process
(1) Mixing trehalase conversion solution and chromatographic separation trehalose solution to obtain mixed solution with trehalose content of 88%, adding 0.4% of sugar carbon, maintaining at 55deg.C for 40min, and filtering with plate frame to obtain filtrate with light transmittance of more than 95%;
(2) Electrodialysis desalination is carried out on the filtered solution, and the current density is 25mA/cm < 2 > to obtain desalted solution with the conductivity less than 50 mu S/cm;
(3) Dissolving crude crystalline trehalose in desalted liquid, wherein the content of the trehalose in the desalted liquid reaches 95%, concentrating under reduced pressure by a single-effect evaporator at a concentration temperature of 60 ℃ and a vacuum degree of-0.09 MPa, continuously concentrating and crystallizing when the total sugar concentration reaches 65%, transferring into a DTB crystallizer, and stirring at a crystallization temperature of 55 ℃ and a stirring speed of 150rpm;
(4) The crystal slurry is continuously discharged from the elutriation column, and is centrifugally separated and dried for 4 hours at 60 ℃ to obtain a crystalline trehalose finished product, the purity of the trehalose can reach 99.8%, and the yield of the trehalose can reach 100.2%.
(5) And (3) performing centrifugal separation to obtain primary mother liquor, concentrating the total sugar concentration in the mother liquor to 80% by using a single-effect evaporator, cooling to 15 ℃ for crystallization, performing centrifugal separation to obtain crude crystalline trehalose, wherein the trehalose content can reach 96.5%, and adding the crude crystalline trehalose into the desalted liquid for re-dissolution.
(6) And (3) carrying out chromatographic separation on the secondary mother liquor to obtain trehalose solution and glucose solution, wherein the trehalose content in the trehalose solution is 97%, the glucose content in the glucose solution is 98.6%, the trehalose solution is mixed with the trehalase conversion solution in the step (1), and the glucose solution is recycled to the fermentation enzyme production process.
Comparative example 1 trehalose chromatographic separation and extraction process
(1) Taking trehalase conversion solution, wherein the trehalase content is 80%, adding 0.4% of sugar carbon, maintaining at 55 ℃ for 40min, and filtering by a plate frame to obtain a filtering solution with the light transmittance more than 95%;
(2) The filtered solution is desalted by ion exchange to obtain desalted solution with the conductivity less than 50 mu S/cm;
(3) Concentrating the desalted liquid by a single-effect evaporator under reduced pressure at a concentration temperature of 60 ℃ and a vacuum degree of-0.09 MPa until the total sugar concentration reaches 60%;
(4) Separating the concentrated solution by chromatography to obtain trehalose solution and glucose solution, wherein the trehalose content in the trehalose solution is 97%, and the glucose content in the glucose solution is 98%;
(5) Adding 0.4% of sugar into the trehalose solution, decolorizing with charcoal for the second time, maintaining at 55deg.C for 40min, and filtering with a plate frame to obtain filtrate with light transmittance higher than 98%;
(6) Desalting the filtered liquid by secondary ion exchange to obtain desalted liquid with the conductivity less than 20 mu S/cm;
(7) Concentrating the secondary desalting solution under reduced pressure by a single-effect evaporator at 60 ℃ and vacuum degree of-0.09 MPa until the total sugar concentration reaches 70%;
(8) Transferring the secondary concentrated solution into a crystallizer, cooling to 15 ℃ for crystallization, centrifuging, drying at 60 ℃ for 4 hours, and finally obtaining a crystalline trehalose finished product, wherein the purity of the trehalose is 99.1%, and the yield of the trehalose is 80%.
Comparative example 2 nanofiltration separation and extraction process of trehalose
(1) Taking trehalase conversion solution, wherein the trehalase content is 80%, adding 0.4% of sugar carbon, maintaining at 55 ℃ for 40min, and filtering by a plate frame to obtain a filtering solution with the light transmittance more than 95%;
(2) Dialyzing the filtering liquid by adding water by adopting a nanofiltration separation technology, wherein the retention molecular weight of a nanofiltration membrane is 280Da, the membrane inlet pressure is 0.22MPa, the membrane outlet pressure is 0.20MPa, the trehalose content in the finally obtained retention liquid reaches 95%, and the glucose content in the dialyzate reaches 97%;
(3) The trapped fluid is desalted by ion exchange to obtain desalted fluid with the conductivity less than 50 mu S/cm;
(7) Concentrating the desalted liquid by a single-effect evaporator under reduced pressure at a concentration temperature of 60 ℃ and a vacuum degree of-0.09 MPa until the total sugar concentration reaches 70%;
(8) Transferring the concentrated solution into a crystallizer, cooling to 15 ℃ for crystallization, centrifugally separating, recycling the separated mother solution to the step (1), drying wet crystals at 60 ℃ for 4 hours, and finally obtaining a crystalline trehalose finished product, wherein the purity of the trehalose is 99.1%, and the yield of the trehalose is 98%.
Comparative example 3 Effect of desalting solution at different Total sugar concentrations
The total sugar concentration in the desalted liquid in the step (3) of the example 3 is adjusted, the desalted liquid is respectively concentrated to different concentrations, and then enters a DTB crystallizer for continuous concentration and crystallization, and the purity and the yield of the finally obtained crystalline trehalose under different total sugar concentrations are shown in the table 1 in the rest steps as in the example 3.
TABLE 1 purity and yield of crystalline trehalose
When the total sugar concentration of the pre-concentration of the desalted liquid does not reach the trehalose saturation concentration, the concentrated liquid entering the DTB crystallizer cannot be immediately crystallized and separated out, so that the trehalose crystallization yield is low; when the concentration of total sugar in the pre-concentration of the desalted liquid exceeds the supersaturated concentration, a large amount of fine crystals are separated out after entering a DTB crystallizer, so that impurities are wrapped in the crystals, and meanwhile, mother liquor is not easy to separate from the crystals, and finally, the purity of the crystallized trehalose is lower.
Comparative example 4 Effect of different trehalose content of desalted liquid
The novel process for improving the recovery rate of the trehalose provided by the invention also depends on that crude trehalose is added into the desalted liquid, and the concentration of the trehalose in the desalted liquid is adjusted to be 90-97%.
The present comparative example provides that the yield and purity of trehalose are obtained by continuous concentration crystallization in a DTB crystallizer only by controlling the total sugar concentration in the desalted liquid to 65% and not adjusting the trehalose concentration with crude trehalose, and specifically, the scheme of the present comparative example is as follows:
(1) Decolorizing trehalase converting liquid with trehalase content of 70-85% and glucose content of 15-30%. Adding 0.2% of sugar carbon, maintaining at 50 ℃ for 40min, and filtering by a plate frame to obtain a filtering liquid with the light transmittance more than 95%;
(2) Electrodialysis desalination is carried out on the filtered solution, and the current density is 20mA/cm < 2 > to obtain desalted solution with the conductivity less than 50 mu S/cm;
(3) Concentrating the desalted liquid by a single-effect evaporator under reduced pressure at 70 ℃ and vacuum degree of-0.085 MPa, continuously concentrating and crystallizing when the total sugar concentration reaches 65% in a DTB crystallizer, and stirring at 60 ℃ and stirring speed of 100rpm;
(4) The crystal slurry is continuously discharged from the elutriation column, and is centrifugally separated and dried for 4 hours at 60 ℃ to obtain the crystalline trehalose finished product, the purity of the trehalose can reach 85-92%, and the yield of the trehalose can reach 68-75%.
The trehalase conversion solution obtained by the enzymatic conversion has low trehalase content, and the crystalline trehalase obtained by one-step concentration and direct crystallization has low trehalase content, so that the content requirement in the national standard of trehalase can not be met. Meanwhile, most of trehalose is not crystallized and remains in the mother liquor, so that the yield of the trehalose is low.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A trehalose extraction process, comprising:
(1) The trehalase conversion solution and the trehalase conversion solution are used as mixed solution, and desalted solution is obtained through decolorization and electrodialysis;
(2) Adjusting the trehalose content in the desalted liquid to 90-97%, concentrating and crystallizing at a total sugar concentration of 60-65%, and vacuum degree of-0.085 to-0.095 Mpa at a crystallization temperature of 55-60 ℃ to obtain a crystallized concentrated solution;
(3) Centrifugally separating the crystal concentrate, and drying the solid part to obtain trehalose crystals; the liquid fraction is used as primary mother liquor for the production of trehalose solution.
2. The trehalose extraction process as claimed in claim 1, wherein after concentrating the primary mother liquor, centrifugal separation is carried out to obtain secondary mother liquor and crude trehalose; and (3) carrying out chromatographic separation on the secondary mother solution to obtain trehalose solution and trehalase conversion solution which are used as mixed solution.
3. The process for extracting trehalose as claimed in claim 2, wherein the secondary mother liquor is subjected to chromatographic separation, and glucose solution is obtained for use in trehalase conversion fermentation.
4. The trehalose extraction process as claimed in claim 2 wherein said crude trehalose is added to said desalted liquid of step (2).
5. The process according to claim 4, wherein the primary mother liquor is concentrated to a total sugar concentration of 75 to 80%, and then the primary mother liquor is crystallized by cooling to 12 to 15 ℃ to obtain crude trehalose, which is added to the desalted liquid of step (2).
6. The trehalose extraction process as claimed in claim 1, wherein the trehalose content in the mixed solution in step (1) is 85-90%; the crystallizer used in the crystallization in the step (2) is a DTB crystallizer.
7. The process for extracting trehalose as claimed in claim 1, wherein electrodialysis desalination is performed with a filtrate having a transmittance of > 95%.
8. Trehalose prepared by the preparation method according to any one of claims 1 to 6, wherein the trehalose has a purity of 99.5 to 99.8%.
9. Use of the method according to any one of claims 1 to 6 for increasing the recovery of trehalase conversion solution.
10. Use of the preparation method according to any one of claims 1 to 6 for increasing the purity of trehalose.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310067814.6A CN118344413A (en) | 2023-01-16 | 2023-01-16 | New process for improving trehalose yield |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310067814.6A CN118344413A (en) | 2023-01-16 | 2023-01-16 | New process for improving trehalose yield |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN118344413A true CN118344413A (en) | 2024-07-16 |
Family
ID=91819881
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310067814.6A Pending CN118344413A (en) | 2023-01-16 | 2023-01-16 | New process for improving trehalose yield |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN118344413A (en) |
-
2023
- 2023-01-16 CN CN202310067814.6A patent/CN118344413A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP2016520093A (en) | Optimized extraction method of ferulic acid with pretreatment | |
| CN109503676A (en) | A method of preparing xylitol and mixing molasses from xylose mother liquid | |
| CN101766289A (en) | Method for preparing high fructose corn syrup | |
| CN105256079A (en) | Purification method for HFCS (high fructose corn syrup) in fructose production process | |
| CN106188167A (en) | A kind of separation and Extraction N acetyl group D glucosamine and method of D glucosamine from D-glucosamine fermentation liquid | |
| CN101586129A (en) | Method of preparing sodium gluconate from xylose crystallization mother liquor | |
| CN106591384A (en) | Comprehensive treatment method of xylose mother liquor | |
| CN114213215A (en) | System and method for co-producing xylitol and caramel pigment by using xylose mother liquor | |
| CN108484422B (en) | Purification and crystallization process for extracting beta-alanine from enzyme conversion solution and system thereof | |
| CN113512566A (en) | System and method for co-producing erythritol and liquid sorbitol by using corn starch | |
| KR20080007985A (en) | A method for purifying 5'-inosinic acid fermentation broth via crystallization process | |
| CN109369731B (en) | Method for removing glucose in xylose production process | |
| CN118344413A (en) | New process for improving trehalose yield | |
| CN103539688B (en) | A kind of method of separation and Extraction Serine from Corynebacterium glutamicum fermented liquid | |
| CN100424088C (en) | Method for preparing crystal maltitol using maltose of 45%-50% purity | |
| CN104152508A (en) | Method for direct extraction of genipin from waste liquid in gardenia yellow pigment production | |
| CN105603129A (en) | Preparation method of healthy and nutritional sugar | |
| CN1807400A (en) | Hind extraction process for producing L-phenylalanine using phenyl-pyruvic acid enzyme method | |
| CN113135965A (en) | System and method for producing crystalline xylose by using xylose mother liquor | |
| CN108034773B (en) | Method for producing crystal sugar by utilizing simulated moving bed continuous ion exchange | |
| CN102952165A (en) | Method for extracting L-arabinose from xylose mother liquid | |
| RU2646115C2 (en) | Method for yield increase output in process of dextrose production using membrane technology | |
| CN116496222B (en) | Method for separating and purifying tetrahydropyrimidine from fermentation liquor | |
| CN101818216B (en) | Method for refining corncob acid hydrolysis solution | |
| CN103319545B (en) | Co-production process for xylobiose and xylose |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |