CN1561991A - Process for producing medicine grade natural vitamin E raw oil - Google Patents
Process for producing medicine grade natural vitamin E raw oil Download PDFInfo
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- CN1561991A CN1561991A CN 200410014547 CN200410014547A CN1561991A CN 1561991 A CN1561991 A CN 1561991A CN 200410014547 CN200410014547 CN 200410014547 CN 200410014547 A CN200410014547 A CN 200410014547A CN 1561991 A CN1561991 A CN 1561991A
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- crude oil
- pharmaceutical grade
- natural vitamin
- alpha
- grade natural
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
A medicine-class raw VE oil is prepared through proportional acetate reaction of d-alpha-VE, solvent, catalyst and dewatering agent, cooling, washing with clean water, laying aside, distilling to remove solvnet and obtain d-alpha-VE acetate, and purifying by molecular distilling.
Description
Technical field: the present invention relates to a kind of technology of preparing of medicine, particularly a kind of production technology of pharmaceutical grade natural Vitamin E crude oil.
Background technology: the pharmaceutical grade natural Vitamin E is the antioxidant vitamins that body weight for humans is wanted.At present, developed country mostly adopts process technology equipments such as process-scale chromatography, supercritical extraction to prepare pharmaceutical grade natural Vitamin E crude oil in the world.But, use this process technology equipment to prepare pharmaceutical grade natural Vitamin E crude oil, not only be difficult to realize suitability for industrialized production, but also directly cause its product cost costliness.Prepare natural Vitamin E crude oil and adopt conventional d-alpha-tocopherol esterification to react, not only the temperature of its esterification is up to 100C-150C, and its esterification yield and reaction yield are all lower, the crude oil products quality does not reach the pharmaceutical grade request of national standard more than 96%, the requirement that the content of the acidity of product and free tocopherol does not all reach regulation yet.
Summary of the invention: technical problem to be solved by this invention is: provide a kind of not only product quality height, and Technology is simple, the production technology of the pharmaceutical grade natural Vitamin E crude oil that is easy to realize suitability for industrialized production.Its technical scheme is: a kind of production technology of pharmaceutical grade natural Vitamin E crude oil is characterized in that its processing step and technology condition:
A) with content be the d-alpha-tocopherol, solvent, catalyst, dehydrant of 80-95% by 1: the weight proportion of 2.5-3.5: 0.5-1.5: 0.1-0.5 carries out the acetate reaction, reaction temperature 40-80C, response time 4-5 hour, cooling, the washing of input water purification, water steamed solvent in static minute, made d-alpha-tocopherol acetate;
B) d-alpha-tocopherol acetate separate is purified through molecular distillation, vacuum is 1-2Pa, and vapo(u)rizing temperature 140-170C, makes pharmaceutical grade vitamin E crude oil at 10-20 second heat time heating time.
Above-mentioned solvent is acetic acid, cyclohexane extraction, normal hexane, ethanol, isopropyl alcohol, diisopropyl ether.
Above-mentioned catalyst is pyridine, triethylamine, sodium phosphate, sodium carbonate.
Above-mentioned dehydrant is acetic anhydride, concentrated sulphuric acid, strong phosphoric acid.
Its technique effect is: Technology of the present invention is owing to adopt normal temperature and pressure tocopherol catalytic esterification technology and two steps of molecular distillation separation and purification, not only Technology is simple for it, reaction condition is not harsh, be easy to realize suitability for industrialized production, and its crude oil products quality that makes meets China's national standard and American Pharmacopeia USP-24 version drug standard fully.
The specific embodiment:
Embodiment 1.
Get content and be 10 kilograms of the d-alpha-tocopherols of 80-90%, add 40 kilograms of diisopropyl ethers, 3 kilograms of acetic acid, 3 kilograms of acetic anhydride, 0.4 kilogram of sodium phosphate is heated to 40-60C, back flow reaction 4 hours, cooling, drop into 60 kilograms of water purification washings, water steamed solvent recovery in static minute, made 10.5 kilograms of d-alpha-tocopherol acetates, content 91%, yield 96.7%.
The d-alpha-tocopherol acetate of above-mentioned gained is separated purification through molecular distillation, and vacuum is 1.5Pa, and vapo(u)rizing temperature 162C makes 9.45 kilograms of pharmaceutical grade vitamin E crude oil, content 96.8%, yield 95.7% 15 seconds heat time heating times.
Embodiment 2.
Get content and be 15 kilograms of 95% d-alpha-tocopherols, add 30 kilograms of heptane, 10 kilograms of acetic acid, 1 kilogram of strong phosphoric acid, 0.3 kilogram of pyridine is warming up to 60-80C, back flow reaction 5 hours, cooling, drop into 100 kilograms of water purification washings, water steamed solvent recovery in static minute, made 14.5 kilograms of d-alpha-tocopherol acetates, content 93%, yield 95.6%.
The d-alpha-tocopherol acetate of above-mentioned gained is separated purification through molecular distillation, and vacuum is 1.6Pa, and vapo(u)rizing temperature 170C makes 13.4 kilograms of pharmaceutical grade vitamin E crude oil, content 96.8%, yield 96.1% 20 seconds heat time heating times.
Claims (4)
1, a kind of production technology of pharmaceutical grade natural Vitamin E crude oil is characterized in that its processing step and technology condition:
A) with content be the d-alpha-tocopherol, solvent, catalyst, dehydrant of 80-95% by 1: the weight proportion of 2.5-3.5: 0.5-1.5: 0.1-0.5 carries out the acetate reaction, reaction temperature 40-80C, response time 4-5 hour, cooling, the washing of input water purification, water steamed solvent in static minute, made d-alpha-tocopherol acetate;
B) d-alpha-tocopherol acetate separate is purified through molecular distillation, vacuum is 1-2Pa, and vapo(u)rizing temperature 140-170C, makes pharmaceutical grade vitamin E crude oil at 10-20 second heat time heating time.
2, the production technology of a kind of pharmaceutical grade natural Vitamin E crude oil according to claim 1 is characterized in that: described solvent is acetic acid, cyclohexane extraction, normal hexane, ethanol, isopropyl alcohol, diisopropyl ether.
3, the production technology of a kind of pharmaceutical grade natural Vitamin E crude oil according to claim 1 is characterized in that: described catalyst is pyridine, triethylamine, sodium phosphate, sodium carbonate.
4, the production technology of a kind of pharmaceutical grade natural Vitamin E crude oil according to claim 1 is characterized in that: described dehydrant is acetic anhydride, concentrated sulphuric acid, strong phosphoric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410014547 CN1268330C (en) | 2004-04-02 | 2004-04-02 | Process for producing medicine grade natural vitamin E raw oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410014547 CN1268330C (en) | 2004-04-02 | 2004-04-02 | Process for producing medicine grade natural vitamin E raw oil |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1561991A true CN1561991A (en) | 2005-01-12 |
| CN1268330C CN1268330C (en) | 2006-08-09 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410014547 Expired - Fee Related CN1268330C (en) | 2004-04-02 | 2004-04-02 | Process for producing medicine grade natural vitamin E raw oil |
Country Status (1)
| Country | Link |
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| CN (1) | CN1268330C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432583A (en) * | 2011-10-25 | 2012-05-02 | 浙江华源制药科技开发有限公司 | Method for preparing low-benzopyrene high-purity d-alpha tocopherol acetate |
| CN104211673A (en) * | 2014-08-20 | 2014-12-17 | 江苏科鼐生物制品有限公司 | Concentration method for low-content natural mixed tocopherol |
| CN104211674A (en) * | 2014-08-20 | 2014-12-17 | 江苏科鼐生物制品有限公司 | Industrialized production method for producing high-content natural vitamin E by utilizing hydrolysis reduction process |
| CN109651324A (en) * | 2019-01-02 | 2019-04-19 | 安徽悦康凯悦制药有限公司 | A kind of preparation method of natural VE |
-
2004
- 2004-04-02 CN CN 200410014547 patent/CN1268330C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432583A (en) * | 2011-10-25 | 2012-05-02 | 浙江华源制药科技开发有限公司 | Method for preparing low-benzopyrene high-purity d-alpha tocopherol acetate |
| CN104211673A (en) * | 2014-08-20 | 2014-12-17 | 江苏科鼐生物制品有限公司 | Concentration method for low-content natural mixed tocopherol |
| CN104211674A (en) * | 2014-08-20 | 2014-12-17 | 江苏科鼐生物制品有限公司 | Industrialized production method for producing high-content natural vitamin E by utilizing hydrolysis reduction process |
| CN104211674B (en) * | 2014-08-20 | 2016-05-18 | 江苏科鼐生物制品有限公司 | A kind of industrialized preparing process that utilizes reductive hydrolysis method to produce high-load natural VE |
| CN109651324A (en) * | 2019-01-02 | 2019-04-19 | 安徽悦康凯悦制药有限公司 | A kind of preparation method of natural VE |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1268330C (en) | 2006-08-09 |
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Granted publication date: 20060809 Termination date: 20100402 |