CN101024617A - Method for preparing d-2 amino-butyl-alcohol-1 - Google Patents
Method for preparing d-2 amino-butyl-alcohol-1 Download PDFInfo
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- CN101024617A CN101024617A CN 200610024029 CN200610024029A CN101024617A CN 101024617 A CN101024617 A CN 101024617A CN 200610024029 CN200610024029 CN 200610024029 CN 200610024029 A CN200610024029 A CN 200610024029A CN 101024617 A CN101024617 A CN 101024617A
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- amino butanol
- racemization
- high pressure
- butanol
- reaction
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Abstract
The invention relates to a manufacturing method for a d-2-amino group butyl alcohol that transforms left-handed rotation amino group butanol to mixed rotation amino group butanol. The main device of high pressure racemism producing is G2Z-5/300-400 film compressor, ZJ-40/400 plunger type metering pump, high pressure reactor. The adopted medium is industrial liquid ammonia, content 99.6% industrial using hydrogen, cobalt touching coal as catalyst, and taking high pressure racemism reaction after hydrogenation activation. The pressure of high pressure racemism reaction is 20-22MPa, and reaction temperature is 170-190 degree centigrade. It would be changed into right-hand split material, and changed into right-hand amino group butanol after taking resin dissociation. The benefits of the invention are that changes three industrial wastes into products and lowers producing cost.
Description
Technical field
The present invention relates to a kind of manufacture method of d-2-amino butanol-1, relate in particular to a kind of method of making d-2-amino butanol-1 by left-handed amino butanol.
Background technology
The DL amino butanol is the important source material of medicine and chemical industry, becomes dextrorotatory form and levo form through fractionation, and levo form does not still have the report of practical application at present, industrial one-tenth " three wastes " owing to parmacodynamics-less activity.
Existing d-2-amino butanol-1 manufacture method is to split through resolving agent by dl-2-amino butanol-1, becomes dextrorotation salt and left-handed salt, and is free through ion-exchange again, the elutriant distillation and d-2-amino butanol-1 and 1-2-amino butanol-1.
Summary of the invention
The technical issues that need to address of the present invention have provided a kind of manufacture method of d-2-amino butanol-1, are intended to solve the above problems.
In order to solve the problems of the technologies described above, the present invention realizes by following steps:
Left-handed amino butanol is converted into the DL amino butanol through the high pressure racemization:
High pressure racemization production technique major equipment has: G2Z-5/300-400 diaphragm type compressor, ZJ-40/400 plunger type metering pump, high-pressure reactor; The medium that adopts is industrial liquefied ammonia, and content 99.60% and industrial hydrogen, cobalt catalyst are as catalyzer, and hydrogenation activates laggard horizontal high voltage racemization; High pressure racemization pressure is 20～22Mpa, 170～190 ℃ of temperature of reaction;
Become dextrorotation by fractionation and split thing: as resolving agent, anhydrous methanol is as solvent with d-tartrate for the resolution process formula, under anhydrous situation, and through dl-amino butanol dropwise reaction, insulation, cooling, crystallization is centrifugally got rid of filter and is obtained dextrorotation and split thing;
By the free dextrorotation amino butanol that becomes of resin: dextrorotation splits thing and dilutes through deionized water, the cation-adsorption resins exchange, and the ammoniacal liquor wash-out, elutriant obtains dextrorotation amino butanol finished product through normal pressure distillation and rectification under vacuum.
Compared with prior art, the invention has the beneficial effects as follows: become " three wastes " into precious recycle, reduced production cost.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail:
Embodiment 1
The high pressure racemization during reaction pressure 20Mpa, when left-handed amino butanol specific rotation is-9.00 °, is-0.5 °, yield 80-85% but racemization obtains DL amino butanol specific rotation when temperature of reaction is 175 ℃;
Embodiment 2
The high pressure racemization during reaction pressure 20Mpa, when left-handed amino butanol specific rotation is-9.00 °, is-0.6 °, yield 80-85% but racemization obtains DL amino butanol specific rotation when temperature of reaction is 172 ℃;
Embodiment 3
The high pressure racemization during reaction pressure 20Mpa, when left-handed amino butanol specific rotation is-9.00 °, is-0.5 °, yield 82% but racemization obtains DL amino butanol specific rotation when temperature of reaction is 178 ℃;
The existing plurality of raw materials such as cobalt thorium, cobalt rhodium, ferro-cobalt, cobalt manganese of once using prepare catalyst, the left-handed amino butanol of the effective racemization of its per kilogram catalyst is 100KG, and the present invention adopts cobalt as raw material, makes the left-handed amino butanol of the effective racemization of per kilogram catalyst bring up to 800 kilograms.
Claims (4)
1. the manufacture method of a d-2-amino butanol-1, realize by following steps:
Left-handed amino butanol is converted into the DL amino butanol through the high pressure racemization:
High pressure racemization production technique major equipment has: G2Z-5/300-400 diaphragm type compressor, ZJ-40/400 plunger type metering pump, high-pressure reactor; The medium that adopts is industrial liquefied ammonia, and content 99.60% and industrial hydrogen, cobalt catalyst are as catalyzer, and hydrogenation activates laggard horizontal high voltage racemization; High pressure racemization pressure is 20～22Mpa, 170～190 ℃ of temperature of reaction;
Become dextrorotation by fractionation and split thing: as resolving agent, anhydrous methanol is as solvent with d-tartrate for the resolution process formula, under anhydrous situation, and through dl-amino butanol dropwise reaction, insulation, cooling, crystallization is centrifugally got rid of filter and is obtained dextrorotation and split thing;
By the free dextrorotation amino butanol that becomes of resin: dextrorotation splits thing and dilutes through deionized water, the cation-adsorption resins exchange, and the ammoniacal liquor wash-out, elutriant obtains dextrorotation amino butanol finished product through normal pressure distillation and rectification under vacuum.
2. the manufacture method of d-2-amino butanol-1 according to claim 1, it is characterized in that left-handed amino butanol is being converted in the DL amino butanol through the high pressure racemization: it is 175 ℃ that temperature of reaction is worked as in the high pressure racemization, during reaction pressure 20Mpa, when left-handed amino butanol specific rotation is-9.00 °, but racemization obtains DL amino butanol specific rotation is-0.5 °, yield 80-85%.
3. the manufacture method of d-2-amino butanol-1 according to claim 1, it is characterized in that left-handed amino butanol is being converted in the DL amino butanol through the high pressure racemization: it is 172 ℃ that temperature of reaction is worked as in the high pressure racemization, during reaction pressure 20Mpa, when left-handed amino butanol specific rotation is-9.00 °, but racemization obtains DL amino butanol specific rotation is-0.6 °, yield 80-85%.
4. the manufacture method of d-2-amino butanol-1 according to claim 1, it is characterized in that left-handed amino butanol is being converted in the DL amino butanol through the high pressure racemization: it is 178 ℃ that temperature of reaction is worked as in the high pressure racemization, during reaction pressure 20Mpa, when left-handed amino butanol specific rotation is-9.00 °, but racemization obtains DL amino butanol specific rotation is-0.5 °, yield 82%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610024029 CN101024617A (en) | 2006-02-21 | 2006-02-21 | Method for preparing d-2 amino-butyl-alcohol-1 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610024029 CN101024617A (en) | 2006-02-21 | 2006-02-21 | Method for preparing d-2 amino-butyl-alcohol-1 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101024617A true CN101024617A (en) | 2007-08-29 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610024029 Pending CN101024617A (en) | 2006-02-21 | 2006-02-21 | Method for preparing d-2 amino-butyl-alcohol-1 |
Country Status (1)
| Country | Link |
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| CN (1) | CN101024617A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106810458A (en) * | 2016-12-31 | 2017-06-09 | 武汉工程大学 | A kind of method that fractionation aminopropanols of DL 2 prepare the aminopropanols of L 2 |
| CN107245038A (en) * | 2016-07-19 | 2017-10-13 | 嘉兴润博化工科技有限公司 | A kind of method for splitting of amino butanol |
-
2006
- 2006-02-21 CN CN 200610024029 patent/CN101024617A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107245038A (en) * | 2016-07-19 | 2017-10-13 | 嘉兴润博化工科技有限公司 | A kind of method for splitting of amino butanol |
| CN106810458A (en) * | 2016-12-31 | 2017-06-09 | 武汉工程大学 | A kind of method that fractionation aminopropanols of DL 2 prepare the aminopropanols of L 2 |
| CN106810458B (en) * | 2016-12-31 | 2019-05-03 | 武汉工程大学 | A method of it splitting DL-2- aminopropanol and prepares L-2- aminopropanol |
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