CN101798295B - Method for preparing vitamin C - Google Patents
Method for preparing vitamin C Download PDFInfo
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- CN101798295B CN101798295B CN2009100659906A CN200910065990A CN101798295B CN 101798295 B CN101798295 B CN 101798295B CN 2009100659906 A CN2009100659906 A CN 2009100659906A CN 200910065990 A CN200910065990 A CN 200910065990A CN 101798295 B CN101798295 B CN 101798295B
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- acid solution
- vitamin
- vitamins
- crude product
- sodium
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- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 title claims abstract description 137
- 235000019154 vitamin C Nutrition 0.000 title claims abstract description 113
- 239000011718 vitamin C Substances 0.000 title claims abstract description 113
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 229930003268 Vitamin C Natural products 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000002253 acid Substances 0.000 claims abstract description 93
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 40
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 claims abstract description 35
- 150000003839 salts Chemical class 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 93
- 239000012043 crude product Substances 0.000 claims description 38
- 235000010378 sodium ascorbate Nutrition 0.000 claims description 31
- 229960005055 sodium ascorbate Drugs 0.000 claims description 31
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 claims description 31
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 239000000706 filtrate Substances 0.000 claims description 22
- 238000011084 recovery Methods 0.000 claims description 22
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 15
- 238000002425 crystallisation Methods 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 230000008025 crystallization Effects 0.000 claims description 14
- 239000000047 product Substances 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 10
- 238000009413 insulation Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000007670 refining Methods 0.000 claims description 6
- 239000012266 salt solution Substances 0.000 claims description 5
- 238000010612 desalination reaction Methods 0.000 claims description 4
- -1 sodium-chlor, sodium-chlor Chemical compound 0.000 claims description 3
- 238000003828 vacuum filtration Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 230000020477 pH reduction Effects 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 14
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 14
- 239000007789 gas Substances 0.000 description 7
- 238000000967 suction filtration Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical group S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 229960005070 ascorbic acid Drugs 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000005342 ion exchange Methods 0.000 description 3
- 238000001953 recrystallisation Methods 0.000 description 3
- 230000008033 biological extinction Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000008520 organization Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- PFTAWBLQPZVEMU-DZGCQCFKSA-N (+)-catechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-DZGCQCFKSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000006806 disease prevention Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention relates to a method for preparing vitamin C, which comprises the following steps that: acidification: vitamin C sodium solution is prepared according to the weight ratio of the vitamin C sodium and water of 1:0.341 to 0.894, hydrochloric acid or HCl gas is added during the mixing process of the vitamin C sodium solution, the weight ratio of VcNa: HCl is 1: 0.175 to 0.215, so the vitamin C sodium solution is adequately reacted to obtain acid solution; and the vitamin C is precisely prepared through separation, salt removal and recycling. The production process of the method can greatly reduce the consumption of water, acid and alkaline, reduce the energy consumption, solve the environmental pollution, shorten the production period, reduce the production cost, and improve the product yield and the quality of the finished product.
Description
Technical field
The invention belongs to the method for preparing VITAMIN, relate in particular to the ascorbic method of a kind of preparation.
Background technology
Vitamins C, chemical name: L-2,3,5,6-tetrahydroxy-2-hexenoic acid-gamma lactone, English name L-2,3,5,6-tetrahydroxy-2-hexenic acid-γ-lactone different name: xitix, AscorbiC acid, structural formula is:
Molecular formula and molecular weight: C
6H
8O
6=176.13
Vitamins C is one of 26 kinds of definite jointly essential drugses of the World Health Organization and the United Nations Industrial Development Organization, be that needed by human and self can not synthetic nutritions, its disease-prevention health function and assisting therapy effect are played more and more important effect to health of people, therefore, ascorbic industrial scale constantly enlarges, and Technology is being updated.
It is sulfuric acid acidation method and ion exchange method that sodium ascorbate is produced the present industry method in common of vitamins C, and wherein the sulfuric acid acidation method is superseded substantially, and ion exchange method has become present main production.Usually ion exchange process be with sodium ascorbate with water dissolution after, solution is removed sodium ion through Zeo-karb, generates vitamin c solution, through concentrating under reduced pressure, crystallisation by cooling, centrifugation gets crude product vitamin C, the crystallization of re-refining gets the finished product vitamins C.The use meeting of Zeo-karb consumes a large amount of tap water, and a large amount of spent acid, the salkali waste of discharging, and environmental pollution is serious, do not meet the requirement of cleaner production, this vitamin c solution concentration lower (15～20%) that makes from the friendship method needs just can produce crude product vitamin C through a large amount of evaporation concentration simultaneously, and this makes that whole process cycle is long, product is easy to go bad, crude product vitamin C is of poor quality, and yield is low, the energy consumption height, facility investment is many, the cost height.
Summary of the invention
The purpose of this invention is to provide a kind of is raw material with the sodium ascorbate, is that souring agent carries out the novel method that acidifying prepares crude product vitamin C with hydrochloric acid, to overcome the deficiency that prior art exists.
In order to arrive above-mentioned purpose by the following technical solutions: the ascorbic method of a kind of preparation may further comprise the steps:
Step 1, acidifying: according to the weight ratio of sodium ascorbate and water is 1: 0.341～0.894 to make the sodium ascorbate aqueous solution, the sodium ascorbate aqueous solution adds hydrochloric acid or feeds HCl gas under whipped state, wherein VcNa: HCl is 1: 0.175～0.215 by pure weight ratio, it is fully reacted, get acid solution;
Step 2, separate: the described acid solution of step 1 is lowered the temperature while stirring, and acid solution is cooled to-5～5 ℃, and keeps 1～3 hour, and vitamins C is separated out from acid solution, filter the acid solution behind crude product vitamin C and the liberating vitamin C;
Step 3, desalination: get the described acid solution of separating out behind the crude product vitamin C of step 2, be evaporated to Vitamin C content 50～60%, make vitamins C be in nearly state of saturation under 65～70 ℃ of temperature, temperature is controlled at 65～70 ℃ of insulations and filters, remove sodium-chlor, obtain filtrate;
Step 4, reclaim: the described filtrate of step 3 is lowered the temperature again is cooled to-5～5 ℃, and keeps 2～10 hours, crystallization, filter the recovery article crude product vitamin C;
Step 5, refining: crude product vitamin C and recovery article vitamins C that step 2,4 is obtained add dissolving rear decoloring filtration in the no salt solution, and cooling, crystallization, separation, oven dry had both got the finished product vitamins C.
In the step 1, add gac in the gained acid solution, additional proportion is warming up to 65～70 ℃ of decolourings then and is incubated filtration again for the 1L acid solution adds 2～10g gac, generates the acid solution that purifies.
Vacuum filtration is adopted in described filtration, and crude product vitamin C that obtains in step 2 and the step 4 and recovery article vitamins C are with frozen water and ice methanol wash.
In the step 3, remove by filter sodium-chlor, sodium-chlor then becomes food grade salt after washing and drying.
No salt solution described in the step 5 is deionized water.
Preparation method's of the present invention chemical principle is the face reaction formula as follows:
The difference of utilizing sodium-chlor and vitamins C solubility with temperature to change, sodium ascorbate is directly generated the aqueous solution of vitamins C and sodium-chlor with hcl acidifying, adopt hot filter, cooling, concentration method, reach progressively separating of vitamins C and sodium-chlor, prepare crude product vitamin C and byproduct sodium-chlor, the crude product vitamin C recrystallization of re-refining gets the finished product vitamins C, and through check, the every index of gained finished product vitamins C all meets 2000 editions two ministerial standards of Chinese Pharmacopoeia.Production technique of the present invention can significantly reduce water, acid, alkali, cuts down the consumption of energy, and solves environmental pollution, shortens the production cycle, reduces production costs, and improves product yield and final product quality, is a kind of cost-effective vitamins C preparation method.
Embodiment
Embodiment 1
The ascorbic method of a kind of preparation is characterized in that this method may further comprise the steps:
Step 1, acidifying: according to the weight ratio of sodium ascorbate and water is 1: 0.341～0.894 to make the sodium ascorbate aqueous solution, the sodium ascorbate aqueous solution adds hydrochloric acid or feeds HCl gas under whipped state, wherein VcNa: HCl is 1: 0.175～0.215 by pure weight ratio, it is fully reacted, get acid solution.In described acid solution, add gac, ratio is warming up to 65～70 ℃ of decolourings then and is incubated filtration again for the 1L acid solution adds 2～10g gac, generates the acid solution that purifies;
Step 2, separate: the described acid solution of step 1 is lowered the temperature while stirring, and acid solution is cooled to-5～5 ℃, and keeps 1～3 hour, and vitamins C is separated out from acid solution, filter the acid solution behind crude product vitamin C and the liberating vitamin C;
Step 3, desalination: get the described acid solution of separating out behind the crude product vitamin C of step 2, be evaporated to Vitamin C content 50～60%, make vitamins C be in nearly state of saturation under 65～70 ℃ of temperature, temperature is controlled at 65～70 ℃ of insulations and filters, obtain filtrate, remove by filter sodium-chlor, sodium-chlor then becomes food grade salt after washing and drying;
Step 4, reclaim: the described filtrate of step 3 is lowered the temperature again is cooled to-5～5 ℃, and keeps 2～10 hours, crystallization, filter the recovery article crude product vitamin C;
Step 5, refining: crude product vitamin C and recovery article vitamins C that step 2,4 is obtained add dissolving rear decoloring filtration in the no salt solution, and cooling, crystallization, separation, oven dry had both got the finished product vitamins C.
Embodiment 2
Step 1, acidifying: getting content is sodium ascorbate 1096 grams (pure 990 grams) of 90.3% (weight content), join in the 550mL water, under whipped state, slowly add 35% hydrochloric acid 521 grams (pure 182 grams) 2 hours reaction times, fully reaction, survey PH=1.0, obtain acid solution, then the gained acid solution is heated to 70 ℃ of temperature, add gac 20 grams, decoloured 10 minutes, vacuumizing filtration is removed the impurity insolubles, is purified acid solution;
Step 2, separation: step 1 gained is purified acid solution be cooled to 0 ℃, suction filtration is also with a small amount of frozen water and ice methanol wash, crude product vitamin C 810 gram (pure 808.4 grams) of content 99.8%, molar yield is 91.9%, obtains the acid solution behind the liberating vitamin C;
Step 3, desalination: the acid solution behind the liberating vitamin C that obtains in the step 2 is evaporated to Vitamin C content 55%, is heated to 70 ℃, filtered while hot is removed sodium-chlor, obtains filtrate, and sodium-chlor gets food grade salt 250 grams after the water washing oven dry;
Step 4, recovery: filtrate is cooled to-3 ℃ again, and also with a small amount of frozen water and ice methanol wash, the recovery article vitamins C 25.6 that gets content 98.9% restrains (pure 25.3 restrain) to suction filtration, and reclaiming yield is that 2.88%, twice molar yield is 94.74% altogether;
Step 5, refining: crude product vitamin C and recovery article vitamins C crystal are added the 800mL deionized water, heating for dissolving decolouring recrystallization separates drying and had both got finished product vitamins C 793 grams, content 99.8%, optically-active=+ 21 °, extinction value is 0.038, and other indexs all meet 2000 editions two ministerial standards of Chinese Pharmacopoeia.
Embodiment 3
In the step 1, getting content is sodium ascorbate 1110 grams (pure 997 grams) of 89.8% (weight content), joins in the 880mL water, under whipped state, slowly feed hydrogen chloride gas 185 grams, keep 1 hour reaction times, fully reaction, survey PH=1.2, get acid solution;
In step 2 and the step 4, get crude product vitamin C 825 grams (pure 821 grams) of content 99.5%, yield is 92.65%; Recovery article Catergen 8 grams of content 99.1% (pure 27.7 grams), reclaiming yield is that 3.13%, twice molar yield is 95.78% altogether;
In the step 5, obtain finished product vitamins C 810 gram, content 99.5%, optically-active=+ 21 °, extinction value is 0.038, other indexs all meet 2000 editions two ministerial standards of Chinese Pharmacopoeia.
Other steps are with embodiment 2.
Embodiment 4
In the step 1, getting content is sodium ascorbate 1000 grams (pure 900 grams) of 90.0% (weight content), joins in the 395mL water, hydrochloric acid 590 grams of slowly adding 30% under whipped state (pure 177 grams) are kept 4 hours reaction times, PH=1.4 is surveyed in fully reaction, obtains acid solution, then the gained acid solution is heated to 65 ℃ of temperature, add gac 16 grams, decoloured vacuumizing filtration 15 minutes, remove the impurity insolubles, be purified acid solution;
In the step 2, gained in the step 1 is purified acid solution be cooled to-5 ℃, suction filtration also respectively washs 2 times with frozen water and ice methyl alcohol, gets the acid solution behind crude product vitamin C and the liberating vitamin C;
In the step 3, the acid solution behind the gained liberating vitamin C in the step 2 is evaporated to Vitamin C content 50%, is heated to 65 ℃, filtered while hot is removed sodium-chlor, obtains filtrate, and sodium-chlor gets food grade salt after the water washing oven dry;
In the step 4, gained filtrate in the step 3 is cooled to-5 ℃ again, suction filtration also respectively washs 2 times with a small amount of frozen water and ice methyl alcohol, gets the recovery article vitamins C;
In the step 5, gained crude product vitamin C in step 2 and the step 4 and recovery article vitamins C crystal are added deionized water, heating for dissolving decolouring recrystallization separates drying and had both got the finished product vitamins C.
Other steps are with embodiment 1.
Embodiment 5
In the step 1, getting content is sodium ascorbate 950 grams (pure 903 grams) of 95.0% (weight content), joins in the 800mL water, under whipped state, slowly feed hydrogen chloride gas 185 grams, keep 3 hours reaction times, fully reaction, survey PH=1.4, obtain acid solution, then acid solution is heated to 67 ℃ of temperature, add gac 22 grams, decoloured 20 minutes, vacuumizing filtration is removed the impurity insolubles, is purified acid solution;
In the step 2, gained in the step 1 is purified acid solution be cooled to 5 ℃, suction filtration also respectively washs 3 times with frozen water and ice methyl alcohol, gets the acid solution behind content crude product vitamin C and the liberating vitamin C;
In the step 3, the acid solution with behind the gained liberating vitamin C in the step 2 is evaporated to Vitamin C content 60%, is heated to 68 ℃, and filtered while hot is removed sodium-chlor, obtains filtrate, and sodium-chlor gets food grade salt after the water washing oven dry;
In the step 4, gained filtrate in the step 3 is cooled to 5 ℃ again, suction filtration also respectively washs 3 times with a small amount of frozen water and ice methyl alcohol, gets the recovery article vitamins C.
Other steps are with embodiment 1.
Embodiment 6
In the step 1, the sodium ascorbate aqueous solution is added hydrochloric acid under whipped state, according to sodium ascorbate: the weight ratio of water: HCl is 1: 0.341: 0.212, and it is fully reacted, acid solution.In described acid solution, add gac, ratio is warming up to 65 ℃ of decolourings then and is incubated filtration again for the 1L acid solution adds the 2g gac, generates the acid solution that purifies;
In the step 2, gained in the step 1 is purified acid solution lower the temperature while stirring, acid solution is cooled to-5 ℃, and keeps 1 hour, and vitamins C is separated out from acid solution, filter the acid solution behind crude product vitamin C and the liberating vitamin C;
In the step 3, gained in the step 2 is separated out acid solution behind the crude product vitamin C, be evaporated to Vitamin C content 50%, temperature is controlled at 65 ℃ of insulations and filters, and removes by filter sodium-chlor, obtains filtrate, and sodium-chlor then becomes food grade salt after washing and drying;
In the step 4, gained filtrate in the step 3 lowered the temperature again is cooled to-5 ℃, and keeps 2 hours, crystallization, filter the recovery article vitamins C;
In the step 5, crude product vitamin C and the recovery article vitamins C that obtains in step 2 and the step 4 added deionized water, the dissolving rear decoloring filters, and cooling, crystallization, separation, oven dry had both got the finished product vitamins C.
Other steps are with embodiment 1.
Embodiment 7
In the step 1, the sodium ascorbate aqueous solution is fed HCl gas under whipped state, according to sodium ascorbate: the weight ratio of water: HCl is 1: 0.894: 0.184, it is fully reacted, get acid solution, in described acid solution, add gac, ratio is warming up to 70 ℃ of decolourings then and is incubated filtration again for the 1L acid solution adds the 10g gac, generates the acid solution that purifies;
In the step 2, gained in the step 1 is purified acid solution lower the temperature while stirring, acid solution is cooled to 5 ℃, and keeps 3 hours, and vitamins C is separated out from acid solution, filter the acid solution behind crude product vitamin C and the liberating vitamin C;
In the step 3, gained in the step 2 is separated out acid solution behind the crude product vitamin C, be evaporated to Vitamin C content 60%, temperature is controlled at 70 ℃ of insulations and filters, and removes by filter sodium-chlor, obtains filtrate;
In the step 4, gained filtrate in the step 3 lowered the temperature again is cooled to 5 ℃, and keeps 10 hours, crystallization, filter the recovery article vitamins C;
In the step 5, gained crude product vitamin C in step 2 and the step 4 and recovery article vitamins C are added deionized water, the dissolving rear decoloring filters, and cooling, crystallization, separation, oven dry had both got the finished product vitamins C.
Other steps are with embodiment 6.
Embodiment 8
In the step 1, the sodium ascorbate aqueous solution adds hydrochloric acid under whipped state, according to sodium ascorbate: water: the HCl weight ratio is 1: 0.341: 0.52, get acid solution, in described acid solution, add gac, ratio adds the 5g gac for the 1L acid solution, be warming up to 67 ℃ of decolourings then and be incubated filtration again, generate the acid solution that purifies;
In the step 2, gained in the step 1 is purified acid solution lower the temperature while stirring, acid solution is cooled to 0 ℃, and keeps 2 hours, and vitamins C is separated out from acid solution, filter the acid solution behind crude product vitamin C and the liberating vitamin C;
In the step 3, gained in the step 2 is separated out acid solution behind the crude product vitamin C, be evaporated to Vitamin C content 55%, temperature is controlled at 67 ℃ of insulations and filters, and obtains filtrate;
In the step 4, with in the step 3 filtrate lower the temperature again and be cooled to 0 ℃, and kept 6 hours, crystallization, filter the recovery article vitamins C.
Other steps are with embodiment 6.
Embodiment 9
In the step 1, the sodium ascorbate aqueous solution adds feeding gas under whipped state, and according to sodium ascorbate: water: the HCl weight ratio is 1: 0.67: 0.74, acid solution;
In the step 2, the acid solution for purifying of gained in the step 1 is cooled to-3 ℃, and kept 1 hour, vitamins C is separated out from acid solution, filter the acid solution behind crude product vitamin C and the liberating vitamin C;
In the step 3, gained in the step 2 is separated out acid solution behind the crude product vitamin C, be evaporated to Vitamin C content 53%, temperature is controlled at 66 ℃ of insulations and filters, and obtains filtrate;
In the step 4, gained filtrate in the step 3 lowered the temperature again is cooled to-3 ℃, and keeps 4 hours, crystallization, filter the recovery article vitamins C.
Other steps are with embodiment 7.
Embodiment 10
In the step 1, the sodium ascorbate aqueous solution adds hydrochloric acid under whipped state, according to sodium ascorbate: water: the HCl weight ratio is 1: 0.55: 0.65, it is fully reacted, get acid solution, in described acid solution, add gac, ratio is warming up to 68 ℃ of decolourings then and is incubated filtration again for the 1L acid solution adds the 7g gac, generates the acid solution that purifies;
In the step 2, gained in the step 1 is purified acid solution lower the temperature while stirring, acid solution is cooled to 3 ℃, and keeps 2 hours, and vitamins C is separated out from acid solution, filter the acid solution behind crude product vitamin C and the liberating vitamin C;
In the step 3, gained in the step 2 is separated out acid solution behind the crude product vitamin C, be evaporated to Vitamin C content 57%, make vitamins C be in nearly state of saturation under 69 ℃ of temperature, temperature is controlled at 66 ℃ of insulations and filters, and obtains filtrate;
In the step 4, gained filtrate in the step 3 lowered the temperature again is cooled to 3 ℃, and keeps 8 hours, crystallization, filter the recovery article vitamins C.
Other steps are with embodiment 6.
Embodiment 11
In the step 1, the sodium ascorbate aqueous solution adds hydrochloric acid under whipped state, and according to sodium ascorbate: water: the HCl weight ratio is 1: 0.50: 0.60, and it is fully reacted, acid solution.
Other steps are with embodiment 6.
Embodiment 12
In the step 1, the sodium ascorbate aqueous solution feeds gas under whipped state, and according to sodium ascorbate: water: the HCl weight ratio is 1: 0.65: 0.55, and it is fully reacted, acid solution.
Other steps are with embodiment 7.
Claims (5)
1. one kind prepares ascorbic method, it is characterized in that this method may further comprise the steps:
Step 1, acidifying: the weight ratio according to sodium ascorbate and water is 1: 0.341～0.894, make the sodium ascorbate aqueous solution, the sodium ascorbate aqueous solution adds concentrated hydrochloric acid or feeds HCl gas under whipped state, wherein VcNa: HCl is 1: 0.175～0.215 by pure weight ratio, it is fully reacted, get acid solution;
Step 2, separate: the described acid solution of step 1 is lowered the temperature while stirring, and acid solution is cooled to-5～5 ℃, and keeps 1～3 hour, and vitamins C is separated out from acid solution, filter the acid solution behind crude product vitamin C and the liberating vitamin C;
Step 3, desalination: get the described acid solution of separating out behind the crude product vitamin C of step 2, be evaporated to Vitamin C content 50～60%, make vitamins C be in nearly state of saturation under 65～70 ℃ of temperature, temperature is controlled at 65～70 ℃ of insulations and filters, remove sodium-chlor, obtain filtrate;
Step 4, reclaim: the described filtrate of step 3 is lowered the temperature again, is cooled to-5～5 ℃, and kept 2～10 hours, crystallization, filter the recovery article crude product vitamin C;
Step 5, refining: crude product vitamin C and recovery article vitamins C that step 2,4 is obtained add dissolving rear decoloring filtration in the no salt solution, cooling, crystallization, separation, the oven dry vitamins C that gets product.
2. the ascorbic method of a kind of preparation according to claim 1, it is characterized in that: in the step 1, add gac in the gained acid solution, additional proportion adds 2～10g gac for the 1L acid solution, be warming up to 65～70 ℃ of decolourings then and be incubated filtration again, generate the acid solution that purifies.
3. the ascorbic method of a kind of preparation according to claim 1 and 2 is characterized in that: vacuum filtration is adopted in described filtration, and crude product vitamin C that obtains in step 2 and the step 4 and recovery article vitamins C are with frozen water and ice methanol wash.
4. the ascorbic method of a kind of preparation according to claim 1 is characterized in that: in the step 3, remove by filter sodium-chlor, sodium-chlor then becomes food grade salt after washing and drying.
5. the ascorbic method of a kind of preparation according to claim 1, it is characterized in that: the no salt solution described in the step 5 is deionized water.
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| CN101798295B true CN101798295B (en) | 2011-08-31 |
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| CN101798295A (en) | 2010-08-11 |
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