CN115784838A - Method for co-producing mannitol crystal and sorbitol crystal by using crystalline glucose - Google Patents
Method for co-producing mannitol crystal and sorbitol crystal by using crystalline glucose Download PDFInfo
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- CN115784838A CN115784838A CN202211567797.4A CN202211567797A CN115784838A CN 115784838 A CN115784838 A CN 115784838A CN 202211567797 A CN202211567797 A CN 202211567797A CN 115784838 A CN115784838 A CN 115784838A
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- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 title claims abstract description 63
- 229930195725 Mannitol Natural products 0.000 title claims abstract description 63
- 239000000594 mannitol Substances 0.000 title claims abstract description 63
- 235000010355 mannitol Nutrition 0.000 title claims abstract description 63
- 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 title claims abstract description 61
- 239000000600 sorbitol Substances 0.000 title claims abstract description 61
- 239000013078 crystal Substances 0.000 title claims abstract description 52
- 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 42
- 239000008103 glucose Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000001704 evaporation Methods 0.000 claims abstract description 31
- 230000008020 evaporation Effects 0.000 claims abstract description 23
- 238000001728 nano-filtration Methods 0.000 claims abstract description 22
- 238000005342 ion exchange Methods 0.000 claims abstract description 17
- 238000006317 isomerization reaction Methods 0.000 claims abstract description 17
- 238000013375 chromatographic separation Methods 0.000 claims abstract description 16
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 238000002425 crystallisation Methods 0.000 claims abstract description 10
- 230000008025 crystallization Effects 0.000 claims abstract description 10
- 238000005119 centrifugation Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 45
- 239000000243 solution Substances 0.000 claims description 34
- 239000007788 liquid Substances 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 18
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 12
- 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 claims description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 229930091371 Fructose Natural products 0.000 claims description 7
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 7
- 239000005715 Fructose Substances 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 6
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims description 6
- 235000010262 sodium metabisulphite Nutrition 0.000 claims description 6
- 239000012752 auxiliary agent Substances 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 229940001584 sodium metabisulfite Drugs 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000007868 Raney catalyst Substances 0.000 claims description 3
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims description 3
- 229910000564 Raney nickel Inorganic materials 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000010979 pH adjustment Methods 0.000 abstract 1
- WQZGKKKJIJFFOK-QTVWNMPRSA-N D-mannopyranose Chemical compound OC[C@H]1OC(O)[C@@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-QTVWNMPRSA-N 0.000 description 3
- 230000032683 aging Effects 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
- 235000013361 beverage Nutrition 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- -1 oxygen ions Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000005846 sugar alcohols Chemical class 0.000 description 1
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Abstract
The invention relates to a method for co-producing mannitol crystals and sorbitol crystals by using crystalline glucose, which comprises the following steps: dissolving, pH adjustment, isomerization, ion exchange, decoloration, first evaporation concentration, first chromatographic separation, hydrogenation, second chromatographic separation, nanofiltration, second evaporation concentration, crystallization, third evaporation concentration, cooling crystallization and centrifugation. The method takes the crystal glucose as the raw material to co-produce the mannitol crystal and the sorbitol crystal, the technology of each operation unit is mature, the utilization rate of the raw material is high, and the yield is high; the production cost is reduced, the yield of high-value products is improved, and the economic benefit is obviously improved.
Description
Technical Field
The invention belongs to the technical field of sugar alcohol preparation, and particularly relates to a method for co-producing mannitol crystals and sorbitol crystals by using crystalline glucose.
Background
At present, the method for producing mannitol in China generally isomerizes glucose into mannose, then obtains high-purity mannose through chromatographic separation, and obtains the mannitol through hydrogenation of the mannose.
Sorbitol and mannitol are isomers, have hygroscopicity, and can be used in beverage, candy, aquatic product, etc. Sorbitol is typically produced by the hydrogenation of glucose.
The production raw materials of mannitol and sorbitol are glucose and are isomers, but a method for co-producing mannitol crystals and sorbitol crystals by using crystalline glucose as a raw material is not available at present.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for co-producing mannitol crystals and sorbitol crystals by using crystalline glucose, wherein the high-purity mannitol crystals and sorbitol crystals are obtained by using the crystalline glucose as a raw material through the working procedures of dissolution, adjustment, isomerization, ion exchange, decoloration, evaporation concentration, chromatographic separation, hydrogenation, chromatographic separation, evaporation, nanofiltration, evaporation concentration and crystallization.
The invention is realized in such a way that a method for co-producing mannitol crystals and sorbitol crystals by using crystalline glucose is provided, which comprises the following steps:
step 1, dissolving: dissolving crystalline glucose to prepare glucose solution with Baume degree of 35 to 55 degrees Be;
step 2, adjusting pH: adding sodium pyrosulfite and magnesium sulfate into the dissolved glucose solution as auxiliary agents, and simultaneously adjusting the pH to 7.0 to 8.0 by using sodium carbonate;
step 3, isomerization: and (3) carrying out an isomerization reaction on the material prepared in the step (2) in an isomerization column, and controlling the reaction temperature to be 50-60 ℃. Controlling the fructose content after isomerization to be 35 to 45 percent and the glucose content to be 55 to 65 percent;
step 4, ion exchange: the isomerized material enters an ion exchange column for ion exchange, and the conductivity of the discharged material is controlled to be less than 50 mu s/cm;
and 5, decoloring: decoloring the material after the ion exchange, controlling the reaction temperature to be 65-75 ℃, the reaction time to be 1-2h, and controlling the color value IU to be less than or equal to 12;
step 6, first evaporation and concentration: evaporating and concentrating the decolored material by using an MVR evaporator, and controlling the concentration of the material to be 50-60%;
step 7, first chromatographic separation: feeding the material subjected to the first evaporation concentration into a chromatographic column for first chromatographic separation to obtain a chromatographic extracting solution and a chromatographic raffinate, and controlling the reaction temperature to be 55-65 ℃;
step 8, hydrogenation: carrying out hydrogenation reaction on the chromatographic extract obtained in the step 7, controlling the reaction temperature to be 120-150 ℃, the reaction pressure to be 4.5-6.5 MPa, and the reaction time to be 4-6 h to obtain a mixed feed liquid of sorbitol and mannitol;
step 9, second chromatographic separation: carrying out second chromatographic separation on the mixed solution of the sorbitol and the mannitol after hydrogenation to respectively obtain a mannitol feed liquid and a sorbitol feed liquid;
step 10, nanofiltration: nanofiltration separation is carried out on the sorbitol feed liquid obtained in the step 9, and nanofiltration extracting solution and nanofiltration raffinate are obtained;
step 11, second evaporation and concentration: carrying out single-effect evaporation concentration on the nanofiltration extracting solution obtained in the step 10, and controlling the sorbitol concentration of the material to be 95-99% to obtain a sorbitol concentrated solution;
step 12, crystallization: spray-crystallizing the sorbitol concentrated solution obtained in the step 11 to obtain sorbitol crystals;
step 13, third evaporation and concentration: further evaporating and concentrating the mannitol feed liquid obtained in the step 9, and controlling the concentration of the mannitol in the feed liquid to be 70-90%;
step 14, cooling and crystallizing: cooling and crystallizing the mannitol evaporated and concentrated in the step 13 in a crystallizing cylinder;
step 15, centrifugation: and (4) carrying out centrifugal treatment on the mannitol mixed feed liquid obtained by cooling crystallization to obtain mannitol crystals.
Compared with the prior art, the method for co-producing mannitol crystals and sorbitol crystals by using crystalline glucose has the following characteristics: the method takes the crystal glucose as the raw material to co-produce mannitol crystal and sorbitol crystal, the technology of each operation unit is mature, the utilization rate of the raw material is high, and the yield is high; the production cost is reduced, the yield of high-value products is improved, and the economic benefit is obviously improved.
Drawings
FIG. 1 is a schematic diagram of a preferred embodiment of the method of the present invention for co-producing mannitol and sorbitol crystals using crystalline glucose.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to FIG. 1, a preferred embodiment of the method of the present invention for co-producing mannitol and sorbitol crystals with crystalline glucose is shown, wherein the arrows indicate the flow direction of the material. The method comprises the following steps:
step 1, dissolving: dissolving crystalline glucose to prepare glucose liquid with the baume degree of 35-55 DEG Be.
Step 2, adjusting pH: sodium metabisulfite and magnesium sulfate are added into the dissolved glucose solution as auxiliary agents, and the pH is adjusted to 7.0-8.0 by sodium carbonate. The added sodium pyrosulfite is 0.1 to 0.4 per mill, and the dosage of the magnesium sulfate is 0.2 to 0.6 per mill.
Step 3, isomerization: and (3) carrying out an isomerization reaction on the material prepared in the step (2) in an isomerization column, and controlling the reaction temperature to be 50-60 ℃. Controlling the fructose content to be 35 to 45 percent and the glucose content to be 55 to 65 percent after the isomerization is finished.
Step 4, ion exchange: and (3) feeding the isomerized material into an ion exchange column for ion exchange, and controlling the conductivity of the material to be less than 50 mu s/cm.
Step 5, decoloring: and (3) decoloring the material after the ion exchange, controlling the reaction temperature to be 65-75 ℃, the reaction time to be 1-2h, and controlling the color value IU to be less than or equal to 12. The water content of the added activated carbon is 10 to 30 percent, and the using amount is 2~5 per mill.
Step 6, first evaporation and concentration: and (5) evaporating and concentrating the decolored material by using an MVR evaporator, and controlling the concentration of the material to be 50-60%.
Step 7, first chromatographic separation: and (3) feeding the material subjected to the first evaporation concentration into a chromatographic column for first chromatographic separation to obtain a chromatographic extract and a chromatographic raffinate, and controlling the reaction temperature to be 55-65 ℃. The fructose content of the chromatographic extracting solution is 85-93%, and the glucose content is 7-15%.
Step 8, hydrogenation: and (3) carrying out hydrogenation reaction on the chromatographic extract obtained in the step (7), controlling the reaction temperature to be 120-150 ℃, the reaction pressure to be 4.5-6.5 MPa, and the reaction time to be 4-6 h to obtain a mixed feed liquid of sorbitol and mannitol. The catalyst added in the reaction is Raney nickel.
And 9, separating the second chromatogram: and (3) carrying out second chromatographic separation on the mixed solution of the sorbitol and the mannitol after hydrogenation to respectively obtain a mannitol feed liquid and a sorbitol feed liquid. The sorbitol material content of the obtained sorbitol material liquid is 94-97%, and the mannitol material content of the mannitol material liquid is 85-92%.
Step 10, nanofiltration: and (4) performing nanofiltration separation on the sorbitol feed liquid obtained in the step (9) to obtain a nanofiltration extracting solution and a nanofiltration raffinate. The sorbitol content of the nanofiltration extracting solution is 98.5 to 99 percent.
Step 11, second evaporation and concentration: and (3) carrying out single-effect evaporation concentration on the nanofiltration extracting solution obtained by nanofiltration in the step 10, and controlling the sorbitol concentration of the material to be 95-99% to obtain a sorbitol concentrated solution.
Step 12, crystallization: and (4) carrying out spray crystallization on the sorbitol concentrated solution obtained in the step (11) to obtain sorbitol crystals.
Step 13, third evaporation and concentration: and (3) further evaporating and concentrating the mannitol feed liquid obtained in the step (9), and controlling the concentration of the mannitol in the feed material to be 70-90%.
Step 14, cooling and crystallizing: and (3) cooling and crystallizing the mannitol subjected to evaporation concentration in the step 13 in a crystallizing cylinder.
Step 15, centrifugation: and (4) carrying out centrifugal treatment on the mannitol mixed feed liquid obtained by cooling crystallization to obtain mannitol crystals.
The process of the present invention for the co-production of mannitol crystals and sorbitol crystals using crystalline glucose is further illustrated by the following specific examples.
Example 1
The first embodiment of the method for co-producing mannitol crystals and sorbitol crystals using crystalline glucose of the present invention comprises the steps of:
step 1, dissolving 100t of glucose crystals in a storage tank to prepare a glucose solution with a baume degree of 44 Bee.
And 2, adding 71.43kg of sodium metabisulfite and 142.86kg of magnesium sulfate as auxiliary agents, and simultaneously adjusting the pH of the material to 7.6 by using sodium carbonate.
And 3, carrying out isomerization reaction on the materials obtained in the step 2 in an isomerization column, controlling the reaction temperature to be 57 ℃, and controlling the fructose content in the sugar solution to be 44% and the glucose content to be 56% after the isomerization.
And 4, the material obtained after the step 3 enters an ion exchange column for ion exchange, and the conductivity of the obtained material is 20 mu s/cm.
And 5, decoloring the material liquid after ion exchange by using 250kg of activated carbon with the water content of 20 percent at the decoloring temperature of 70 ℃ for 1.5h, wherein the color value IU of the material liquid after decoloring is 10.
And 6, evaporating and concentrating the material decolored in the step 5 by using an MVR evaporator, wherein the discharging concentration is 55%.
And 7, removing oxygen ions from the concentrated material by using a degassing tower, and performing chromatographic separation at the temperature of 60 ℃ to obtain an extracting solution and raffinate. The fructose content in the extract was 92.8%, and the glucose content was 6.44%.
And 8, fully mixing the extracting solution obtained in the step 7 with a catalyst Raney nickel conveyed by a diaphragm pump, and then carrying out hydrogenation reaction at 140 ℃ under the pressure of 4.5MPa for 4.5h to obtain the mixed feed liquid of sorbitol and mannitol.
And 9, separating the mixed material liquid of sorbitol and mannitol obtained in the step 8 by using chromatography to respectively obtain a sorbitol material liquid with the content of 96% and a mannitol material liquid with the content of 90%.
And step 10, performing nanofiltration separation on the sorbitol solution obtained in the step 9 by using a nanofiltration membrane system to obtain an extracting solution and a raffinate, wherein the content of the extracting solution is 99%.
And 11, performing single-effect evaporation and concentration on the extracting solution obtained in the step 10 to enable the concentration of the sorbitol concentrated solution to reach 99%.
And step 12, crystallizing by utilizing a spray drying technology to obtain 50.2t sorbitol crystals.
And step 13, evaporating and concentrating the mannitol solution obtained in the step 9 to obtain a mannitol concentrated solution with the concentration of 85%.
And step 14, cooling and crystallizing the mannitol concentrated solution in a crystallizing tank.
And 15, centrifuging the mannitol mixed solution obtained in the step 14 to obtain mannitol crystals with the water content of 1.0%, and then drying, aging and the like to obtain the mannitol crystals 44t.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (8)
1. A method for co-producing mannitol crystals and sorbitol crystals by using crystalline glucose is characterized by comprising the following steps:
step 1, dissolving: dissolving crystalline glucose to prepare glucose solution with Baume degree of 35 to 55 degrees Be;
step 2, adjusting pH: adding sodium metabisulfite and magnesium sulfate into the dissolved glucose solution as auxiliary agents, and simultaneously adjusting the pH to 7.0-8.0 by using sodium carbonate;
step 3, isomerization: and (3) carrying out an isomerization reaction on the material prepared in the step (2) in an isomerization column, and controlling the reaction temperature to be 50-60 ℃.
2. Controlling the fructose content to be 35 to 45 percent and the glucose content to be 55 to 65 percent after the isomerization is finished;
step 4, ion exchange: the isomerized material enters an ion exchange column for ion exchange, and the conductivity of the discharged material is controlled to be less than 50 mu s/cm;
and 5, decoloring: decoloring the material after ion exchange, controlling the reaction temperature to be 65-75 ℃, the reaction time to be 1-2h, and controlling the color value IU to be less than or equal to 12;
step 6, first evaporation and concentration: evaporating and concentrating the decolored material by using an MVR evaporator, and controlling the concentration of the material to be 50-60%;
step 7, first chromatographic separation: feeding the material subjected to the first evaporation concentration into a chromatographic column for first chromatographic separation to obtain a chromatographic extracting solution and a chromatographic raffinate, and controlling the reaction temperature to be 55-65 ℃;
step 8, hydrogenation: carrying out hydrogenation reaction on the chromatographic extract obtained in the step 7, controlling the reaction temperature to be 120-150 ℃, the reaction pressure to be 4.5-6.5 MPa, and the reaction time to be 4-6 h to obtain a mixed feed liquid of sorbitol and mannitol;
and 9, separating the second chromatogram: carrying out second chromatographic separation on the mixed solution of the sorbitol and the mannitol after hydrogenation to respectively obtain a mannitol feed liquid and a sorbitol feed liquid;
step 10, nanofiltration: nanofiltration separation is carried out on the sorbitol feed liquid obtained in the step 9, and nanofiltration extracting solution and nanofiltration raffinate are obtained;
step 11, second evaporation and concentration: carrying out single-effect evaporation concentration on the nanofiltration extracting solution obtained in the step 10, and controlling the sorbitol concentration of the material to be 95-99% to obtain a sorbitol concentrated solution;
step 12, crystallization: spray-crystallizing the sorbitol concentrated solution obtained in the step 11 to obtain sorbitol crystals;
step 13, third evaporation and concentration: further evaporating and concentrating the mannitol feed liquid obtained in the step 9, and controlling the concentration of the mannitol in the feed liquid to be 70-90%;
step 14, cooling and crystallizing: cooling and crystallizing the mannitol evaporated and concentrated in the step 13 in a crystallizing cylinder;
step 15, centrifugation: and (4) carrying out centrifugal treatment on the mannitol mixed feed liquid obtained by cooling crystallization to obtain mannitol crystals.
3. The method for co-producing mannitol crystals and sorbitol crystals with crystalline glucose as claimed in claim 1, wherein in step 2, the sodium metabisulfite is added in an amount of 0.1 to 0.4% and the magnesium sulfate is added in an amount of 0.2 to 0.6%.
4. The method for co-producing mannitol and sorbitol crystals with crystalline glucose according to claim 1, wherein in step 5, the activated carbon is added with a water content of 10 to 30% and an amount of 2~5 ‰.
5. The method for co-producing mannitol crystals and sorbitol crystals by using crystalline glucose according to claim 1, wherein in step 7, the chromatographic extract has a fructose content of 85 to 93% and a glucose content of 7 to 15%.
6. The method for co-producing mannitol and sorbitol crystals using crystalline glucose according to claim 1, wherein in step 8, the catalyst added for the reaction is Raney nickel.
7. The method for co-producing mannitol crystals and sorbitol crystals by using crystalline glucose as claimed in claim 1, wherein in step 9, the sorbitol material content of the obtained sorbitol material liquid is 94-97%, and the mannitol material content of the mannitol material liquid is 85-92%.
8. The method for co-producing mannitol crystals and sorbitol crystals with crystalline glucose as claimed in claim 1, wherein in step 10, the sorbitol content of the nanofiltration extract obtained is 98.5 to 99%.
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US20150307424A1 (en) * | 2012-11-22 | 2015-10-29 | Syral Belgium Nv | Process for the production and separation of mannitol and sorbitol from a mixture which was obtained by hydrogenation of a precursor |
CN104450799A (en) * | 2014-12-05 | 2015-03-25 | 浙江华康药业股份有限公司 | Process for preparing neosorb and coproducing fructose-glucose syrup |
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