CN1275569A - Novel process for production of vitamin C - Google Patents
Novel process for production of vitamin C Download PDFInfo
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- CN1275569A CN1275569A CN 99112238 CN99112238A CN1275569A CN 1275569 A CN1275569 A CN 1275569A CN 99112238 CN99112238 CN 99112238 CN 99112238 A CN99112238 A CN 99112238A CN 1275569 A CN1275569 A CN 1275569A
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- sodium
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- colombate
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Abstract
A new process for producing vitamin C is mainly characterized by directly making sodium gulonate crystal implement esterification reaction, and undergo conversion reaction and acidification reaction to produce vitamin c. The sodium gulonate crystal is obtained by using sodium gulonate solution through the process of concentration and crystallization, so that it has no need of drying step. Said invention can greatly save water for technological process, solve environmental pollution, shorten production period, reduce production cost, and raise product yield.
Description
The present invention relates to ascorbic production technique.
The production of vitamin C technology of prior art is: by obtaining sodium colombate solution behind sorbyl alcohol, corn steep liquor, light calcium carbonate, urea, sal epsom, yellow soda ash, potassium primary phosphate, Glacial acetic acid, bubble enemy, the glucose fermentation, through flocculating settling, remove protein, the stillness of night is through Zeo-karb, remove sodium ion, become ancient imperial acid solution, concentrate through two-stage vacuum, crystallisation by cooling, centrifugation De Gulong acid crystal, under vacuum, be warming up to 65 ℃ of dryings 1 hour again, make qualified ancient dragon acid.Whole process need 72 hours.Ancient dragon acid adds quantitative methyl alcohol, sulfuric acid again under 69 ℃ condition, carry out esterification 14 hours, and dropped into quantitative sodium bicarbonate and carry out conversion reaction 6 hours, be cooled to-2 ℃, separate the Vc sodium crystal, VC sodium adds 82 ~ 84% methyl alcohol, sulfuric acid again, regulates PH and is 2.0 ~ 2.5 and carry out acidification reaction, generates Vc solution, through concentrated, crystallization, separate thick Vc, being converted into thick Vc by the imperial acid of Gu needs 64 hours, thick Vc is again through making the vitamins C of white powder.
The characteristics of above-mentioned technology are to produce vitamins C with the imperial acid crystal of Gu, make ancient imperial acid crystal by sodium colombate solution through cation-exchange step.In carrying out this step, after Zeo-karb is saturated, need with a large amount of tap water backwashes, add 4% liquid caustic soda regeneration 2 hours then, again with tap water soda to PH be 8, added 7 ~ 8% regeneration of hydrochloric acid 2 hours, with washing acid from the beginning to PH be 4, add pure water again and soak standby.This step need consume a large amount of tap water, and discharging spent acid salkali waste, and environmental pollution is serious.Simultaneously, because ancient imperial acid crystal contains crystal water, need to carry out esterification again through baking step.Whole process cycle is long, and facility investment is many, the cost height, and yield is low.
The objective of the invention is to overcome the deficiencies in the prior art, improve ascorbic production technique, make production technique of the present invention significantly reduce water, solve environmental pollution, shorten the production cycle, reduce production costs, improve product yield.
Novel process for production of vitamin C of the present invention, its major technique characteristics are directly to carry out esterification by the sodium colombate crystal, produce Vc through conversion reaction, acidification reaction again.
The present invention overcomes prior art sodium colombate solution must remove sodium ion, and with the process characteristic of the imperial acid crystal production of Gu Vc, but directly with sodium colombate crystal production Vc, roughly production craft step thereafter is substantially with former technology.
The sodium colombate crystal is obtained through concentrated, crystallization by sodium colombate solution, and need not pass through baking step, directly carries out esterification.Described sodium colombate solution can be that the mode with prior art makes, be by sorbyl alcohol, corn steep liquor, light calcium carbonate, urea, sal epsom, yellow soda ash, potassium primary phosphate, Glacial acetic acid, bubble enemy, glucose by fermentation after, obtain through behind the flocculating settling again.
Sodium colombate solution generally concentrates through two-stage, described two-stage concentrates, the first step concentrates through triple-effect evaporator, adopt the mode of reduction vaporization, the first single-effect evaporator controlled temperature is 56～59 ℃, and vacuum tightness is-0.068Mpa, the second single-effect evaporator temperature is 50～52 ℃, vacuum tightness-0.083Mpa, the third effect evaporator temperature is 40～43 ℃, vacuum tightness-0.09～-0.093Mpa; The second stage concentrates, and controlled temperature is 42～45 ℃, vacuum tightness-0.09～-0.095Mpa.Carry out centrifugation after the process two-stage concentrates, obtain the sodium colombate crystal, wash with methanol solution when centrifugal.
Esterification is undertaken by sodium colombate crystal and methyl alcohol, the vitriol oil, and the consumption of each material is: sodium colombate crystal: methyl alcohol=1kg: (2～3) rise, sodium colombate crystal: sulfuric acid=1kg of 98%: (0.17～0.2) rises.
Add sodium bicarbonate after the esterification and carry out conversion reaction, sodium colombate crystal: sodium bicarbonate=1kg: (0.45～0.55) kg.
In technology of the present invention, can filter earlier after the esterification of sodium colombate crystal and carry out conversion reaction after removing sodium salt, can not filter earlier yet.After conversion reaction obtains containing the mixed solution of Vc sodium crystal, can obtain the Vc sodium crystal through centrifugal, filtration.Can not separate earlier yet, crystallization, the direct acidifying of this mixed solution, Vc sodium crystal generation acidification reaction wherein filters after the acidifying again, removes sodium salt.
Acidification reaction is to be that 82～84% methyl alcohol, dilute sulphuric acid carry out by Vc sodium crystal and concentration, and regulating PH is 2.0～2.4, obtains Vc solution after the filtration.Make with extra care then and obtain Vc.
Describe the present invention with embodiment below:
By obtaining sodium colombate solution behind raw material sorbyl alcohol, corn steep liquor, light calcium carbonate, urea, sal epsom, yellow soda ash, potassium primary phosphate, Glacial acetic acid, bubble enemy, the glucose fermentation, through flocculating settling, clear liquid directly passes through vacuum concentration and crystallisation by cooling.During vacuum concentration, order through vacuum tightness is-0.068Mpa, temperature is 59 ℃ first single-effect evaporator, vacuum tightness-0.083Mpa, temperature is 52 ℃ second single-effect evaporator, vacuum tightness-0.09Mpa, temperature is 43 ℃ a third effect evaporator, carry out the second stage then and concentrate, controlled temperature is below 45 ℃, vacuum tightness-0.09Mpa.Vapor pressure when the first step concentrates is 0.3～0.4Mpa, and the spissated vapor pressure in the second stage is 0.15～0.3Mpa.Concentrate through the first step, the concentration of sodium colombate solution reaches 40%, concentrates through the second stage, and the concentration of sodium colombate solution reaches 85%.With methanol solution (concentration can reach more than 99.5%) flushing, mother liquor was recyclable, obtains the sodium colombate crystal when crystallization was centrifugal.Sodium colombate and quantitative methyl alcohol (concentration is more than 99.5%), the vitriol oil carried out esterification 6 hours under 69 ℃, sodium colombate: methyl alcohol=1 (kg): 2.5 (L), sodium colombate: 98% sulfuric acid=1 (kg): 0.19 (L), add quantitative sodium bicarbonate and carried out conversion reaction 6 hours, sodium colombate: sodium bicarbonate=1: 0.5 (weight), add 82～84% methyl alcohol, 50% dilute sulphuric acid again, regulate PH2.0 ~ 2.4 and carried out acidification reaction 2 hours, Vc sodium decolour simultaneously with gac: gac=1: 0.02 (weight ratio).10 ℃ are filtered down then, remove sodium sulfate, obtain Vc solution, concentrate, and evaporate methyl alcohol, and crystallization is centrifugal to obtain thick Vc, further obtain smart Vc with dissolved in distilled water, crystallization are centrifugal again, obtain white Powdered Vc after 65 ℃ of oven dry.
Advantage of the present invention:
1, gulonate solution of the present invention without ion-exchange, has been saved water, hydrochloric acid, liquid caustic soda, with former worker Skill is compared, but 400 cubic metres of product using water wisely per ton, 1.7 tons of hydrochloric acid, 0.4 ton of liquid caustic soda has fundamentally solved water The problem of source deficiency has solved problem of environmental pollution substantially. After the ion-exchange of former technology gulonate is 2-KLG solution, Through Vacuum Concentration, when crystallization is centrifugal, need to use alcohol flushing, because 2-KLG is dissolved in methyl alcohol, and the present invention can directly use first The alcohol flushing, finished product per ton can be saved 0.2 ton of ethanol.
2, reduce equipment investment, shortened the production cycle, reduced production cost, improved product yield. By former 10 operating posts of technology change 7 posies into, have removed cationic ion-exchange resin post, oven dry post and Vc sodium 45 hours production cycles are shortened in centrifugal post, and wherein production process need be with 40 hours, than former worker before the esterification Skill shortens 32 hours; Need with 51 hours, shorten 13 hours than former technology by esterification to obtaining thick Vc. Reduced the product loss because of operations such as ion-exchange, oven dry, yield is brought up to more than 60% by original 54%, On the basis of existing equipment, drop into a small amount of fund, increase equipment component, output is by 100 tons of growths of original monthly output It is 200 tons. 5 tons of finished product steam savings per ton, electricity 1800 degree, 2800～3000 yuan of ton costs.
3, the protein that sedimentation in producing is gone out through processing, can be used as the feed of aquaculture, a small amount of waste liquor, Can be used as oxalic acid production usefulness, a large amount of sodium sulphate is processed through reprocessing, can be used as papermaking, glass, pottery, washing powder Deng additive, thereby turn waste into wealth, basically solved problem of environmental pollution.
4, not affecting product quality, below is the survey report that adopts the Vc of explained hereafter of the present invention:
| Interventions Requested | Quality standard | Assay |
| Differentiate | Should be positive reaction | Be positive reaction |
| Outward appearance | White crystalline powder | White crystalline powder |
| Fusing point | 190～192 ℃ (191 ~ 192 ℃ of top grades) | 191.7～191.8℃ |
| Specific rotation (20 ℃) | 20.5～21.5℃ | 21.35℃ |
| Content | 99.0～100.5％ | 99.80％ |
| Residue on ignition | ≤0.1％ | 0.05％ |
| Heavy metal | ≤ 0.001% (top grade 0.0005%) | ＜3ppm |
| Clarity of solution | Should clarify≤8ml (top grade 5ml) | ＜5ml |
| Solution colour | (1) solution A≤0.02 (top grade 0.01) (2) baking A≤0.06 (top grade 0.03) | (1)0.005 (2)0.018 |
| Trichobothrium | ≤ 10/3g (3 of top grades/3g) | 5/3g |
| Readily carbonizable substance | ≤ Y4 (top grade) | ＜Y4 |
| PH value | 2.1 ~ 2.6 (top grades) | 2.21 |
| Oxalic acid | ≤ 0.2% (top grade) | ＜0.2％ |
| Molysite | ≤ 0.0002% (top grade) | ＜2ppm |
| Mantoquita | ≤ 0.0005% (top grade) | / |
| Fineness | More than 40 orders≤15% 40 ~ 80 order 〉=50% (top grade) | / |
| Conclusion: primes | ||
Claims (10)
1, a kind of novel process for production of vitamin C is characterized in that directly participating in esterification by the sodium colombate crystal, produces Vc through conversion reaction, acidification reaction again.
2, novel process for production of vitamin C according to claim 1 is characterized in that obtaining the sodium colombate crystal by sodium colombate solution through concentrated, crystallization.
3, novel process for production of vitamin C according to claim 2, it is characterized in that sodium colombate solution be by raw material by fermentation after, again through obtaining behind the flocculating settling.
4, novel process for production of vitamin C according to claim 2, it is characterized in that sodium colombate solution concentrates through two-stage, the first step concentrates through triple-effect evaporator, adopt the mode of reduction vaporization, the first single-effect evaporator controlled temperature is 56～59 ℃, and vacuum tightness is-0.068Mpa, the second single-effect evaporator temperature is 50～52 ℃, vacuum tightness-0.083Mpa, the third effect evaporator temperature is 40～43 ℃, vacuum tightness-0.09～-0.093Mpa; The second stage concentrates, and controlled temperature is 42～45 ℃, vacuum tightness-0.09～-0.095Mpa, wash with methanol solution when crystallization is centrifugal.
5, novel process for production of vitamin C according to claim 1, it is characterized in that the sodium colombate crystal through esterification, add sodium bicarbonate and carry out the mixed solution that conversion reaction obtains containing the Vc sodium crystal, through separation, crystallization, obtain the Vc sodium crystal, the Vc sodium crystal carries out acidification reaction.
6, novel process for production of vitamin C according to claim 1, it is characterized in that the sodium colombate crystal through esterification, add sodium bicarbonate and carry out the mixed solution that conversion reaction obtains containing the Vc sodium crystal, the direct acidifying of this mixed solution, Vc sodium crystal generation acidification reaction wherein.
7, according to claim 5,6 described novel process for production of vitamin C, it is characterized in that the sodium colombate esterification after, carry out conversion reaction after filtration again.
8, according to claim 5,6 described novel process for production of vitamin C, it is characterized in that Vc sodium crystal and methyl alcohol, sulfuric acid carry out acidification reaction, obtain Vc solution after the filtration, through concentrate, crystallization is centrifugal obtains thick Vc, further refining again, oven dry obtains white powder Vc.
9, according to claim 1,5,6 described novel process for production of vitamin C, it is characterized in that sodium colombate crystal and methyl alcohol, the vitriol oil carry out esterification, sodium colombate crystal: methyl alcohol=1kg: (2～3) L, sodium colombate crystal: sulfuric acid=1kg of 98%: (0.17～0.2) L, add sodium bicarbonate after the esterification and carry out conversion reaction, sodium colombate crystal: sodium bicarbonate=1kg: (0.45～0.55) kg.
10, novel process for production of vitamin C according to claim 8 is characterized in that Vc sodium crystal and concentration are that 82～84% methyl alcohol, dilute sulphuric acid carry out acidification reaction, and regulating PH is 2.0～2.4, obtains Vc solution after the filtration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99112238 CN1275569A (en) | 1999-06-01 | 1999-06-01 | Novel process for production of vitamin C |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99112238 CN1275569A (en) | 1999-06-01 | 1999-06-01 | Novel process for production of vitamin C |
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| CN1275569A true CN1275569A (en) | 2000-12-06 |
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| CN 99112238 Pending CN1275569A (en) | 1999-06-01 | 1999-06-01 | Novel process for production of vitamin C |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1327838C (en) * | 2004-07-08 | 2007-07-25 | 北京科信必成医药科技发展有限公司 | Vitamin C oral disintegration tablet and its preparing method |
| CN1332666C (en) * | 2004-05-26 | 2007-08-22 | 中国科学院生物物理研究所 | Compound preparation for resisting senile dementia |
| CN1332667C (en) * | 2004-05-26 | 2007-08-22 | 中国科学院生物物理研究所 | Compound preparation for resisting Parkinson's disease |
| CN100344619C (en) * | 2004-04-23 | 2007-10-24 | 徐建涛 | Vitamine C refining process |
| CN100441659C (en) * | 2006-12-06 | 2008-12-10 | 中国科学院沈阳应用生态研究所 | Antibiotic soil modifier made by gulconic acid mother liquor and method for preparing same |
| CN101353337B (en) * | 2008-09-08 | 2011-04-06 | 陈星� | Vitamin c clean production method |
| CN101397286B (en) * | 2008-11-18 | 2011-12-21 | 江苏江山制药有限公司 | Method for continuous crystallisation of vitamin C |
| CN101381353B (en) * | 2008-11-05 | 2011-12-21 | 江苏江山制药有限公司 | Esterification and conversion technology of low consumption vitamin C |
| CN103087018A (en) * | 2012-11-14 | 2013-05-08 | 江苏江山制药有限公司 | Preparation method of erythorbic acid |
| CN103113334A (en) * | 2013-03-14 | 2013-05-22 | 乔敏 | Method for separating mycelium in vitamin C fermentation broth by environment-friendly montmorillonite flocculant |
| CN104152507A (en) * | 2014-07-10 | 2014-11-19 | 东北制药集团股份有限公司 | Method for preparing gulonic acid methanol solution |
-
1999
- 1999-06-01 CN CN 99112238 patent/CN1275569A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100344619C (en) * | 2004-04-23 | 2007-10-24 | 徐建涛 | Vitamine C refining process |
| CN1332666C (en) * | 2004-05-26 | 2007-08-22 | 中国科学院生物物理研究所 | Compound preparation for resisting senile dementia |
| CN1332667C (en) * | 2004-05-26 | 2007-08-22 | 中国科学院生物物理研究所 | Compound preparation for resisting Parkinson's disease |
| CN1327838C (en) * | 2004-07-08 | 2007-07-25 | 北京科信必成医药科技发展有限公司 | Vitamin C oral disintegration tablet and its preparing method |
| CN100441659C (en) * | 2006-12-06 | 2008-12-10 | 中国科学院沈阳应用生态研究所 | Antibiotic soil modifier made by gulconic acid mother liquor and method for preparing same |
| CN101353337B (en) * | 2008-09-08 | 2011-04-06 | 陈星� | Vitamin c clean production method |
| CN101381353B (en) * | 2008-11-05 | 2011-12-21 | 江苏江山制药有限公司 | Esterification and conversion technology of low consumption vitamin C |
| CN101397286B (en) * | 2008-11-18 | 2011-12-21 | 江苏江山制药有限公司 | Method for continuous crystallisation of vitamin C |
| CN103087018A (en) * | 2012-11-14 | 2013-05-08 | 江苏江山制药有限公司 | Preparation method of erythorbic acid |
| CN103113334A (en) * | 2013-03-14 | 2013-05-22 | 乔敏 | Method for separating mycelium in vitamin C fermentation broth by environment-friendly montmorillonite flocculant |
| CN104152507A (en) * | 2014-07-10 | 2014-11-19 | 东北制药集团股份有限公司 | Method for preparing gulonic acid methanol solution |
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