CN103539686A - Method for producing aminopropionic acid - Google Patents
Method for producing aminopropionic acid Download PDFInfo
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- CN103539686A CN103539686A CN201210235178.5A CN201210235178A CN103539686A CN 103539686 A CN103539686 A CN 103539686A CN 201210235178 A CN201210235178 A CN 201210235178A CN 103539686 A CN103539686 A CN 103539686A
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Abstract
The invention discloses a method for producing an aminopropionic acid. The product belongs to the field of manufacturing of an amino acid. The method comprises the following steps: by taking propionic acid, red phosphorus, liquid chlorine, ammonia water, urotropine and methanol as raw materials, taking a chlorination reaction kettle, an ammonification reaction kettle, a crystallization kettle, a centrifugal machine and a vacuum drier as equipments, preparing the product by the procedures of chlorination reaction, ammonolysis reaction, crystallization, centrifugal separation, drying and the like. The production method has a series of advantages of being simple in technology, free of three wastes emission, free of high-temperature and high-pressure reaction, easy to produce and operate, low in production cost, high in yield, good in product quality and the like, utilizes general equipment, and can carry out mass production; the aminopropionic acid with high quality can be produced.
Description
Technical field
The invention belongs to amino acid and manufacture field, relate in particular to a kind of production method of L-Ala.
Background technology
A kind of aliphatic nonpolar amino acid of L-Ala, it is the fundamental unit that forms protein, its molecular formula is C3H7O2N, outward appearance is white crystals or crystalline powder, has fragrance, and taste is sweet, easily molten in water, insoluble in ethanol, acetone or ether, L-Ala has α-alanine and two kinds of isomerss of Beta-alanine, and relative molecular mass is 89.063.L-Ala is the fundamental unit that forms protein, one of 21 seed amino acids that form human body protein, α-alanine also claims 2-alanine, 200 ℃ of above distillations, it is a kind of composition of constitutive protein matter, in trophology, belong to the nonessential amino acid of human body, how from fermentation method and natural product, to produce at present, also available chemical process is synthetic; Beta-alanine also claims 3-alanine, clear crystal, 198 ℃ of fusing points, for the synthesis of pantothenic acid and plating, also for the research of microbiology and biological chemistry etc., can and refine by proteolysis such as silk gum, gelatin, zeins and form, also available chemical process is synthetic.L-Ala is mainly for the manufacture of vitamin B6, synthetic pantothenic acid calcium and other organic compound raw materials, make an addition to the seasoning effect that can strengthen chemical seasoning in food, improve sense of taste and the organic acid tart flavour of sweeting agent, improve the quality containing alcoholic beverage, prevent oils oxidation and improve infusion of food local flavor etc.; Also can be used as biochemical reagents, for biological chemistry and microbe research aspect.The technique of producing L-Ala reach ten several, the present invention is produce this Product Process a kind of, with propionic acid, red phosphorus, liquid chlorine, ammoniacal liquor, urotropine, methyl alcohol is raw material, with chlorination reaction still, aminating reaction still, crystallization kettle, whizzer, Vacuumdrier is equipment, pass through chlorination reaction, aminating reaction, crystallization, centrifugation, the operations such as oven dry make finished product, this production method compared to the prior art, there is technique simple, use general-purpose equipment, three-waste free discharge, without high-temperature high-voltage reaction, be easy to production operation, production cost is low and productive rate is high, the series of advantages such as good product quality, can be mass, can produce high-quality L-Ala.
Summary of the invention
The problem that the present invention mainly solves is to provide a kind of production method of L-Ala, the method is with propionic acid, red phosphorus, liquid chlorine, ammoniacal liquor, urotropine, methyl alcohol is raw material, with chlorination reaction still, aminating reaction still, crystallization kettle, whizzer, Vacuumdrier is equipment, pass through chlorination reaction, aminating reaction, crystallization, centrifugation, the operations such as oven dry make finished product, it is simple that this production method has technique, use general-purpose equipment, three-waste free discharge, without high-temperature high-voltage reaction, be easy to the advantages such as production operation, the proportioning raw materials that the present invention uses is: propionic acid 18%-20%, red phosphorus 1%, liquid chlorine 19%-21, ammoniacal liquor 58%, urotropine 2%, methyl alcohol is appropriate.
The present invention can be achieved through the following technical solutions:
A production method for L-Ala, is characterized in that consisting of following steps:
(1) by the propionic acid of formula ratio in sending into after the assay was approved chlorination reaction still, reactor is sealed, warming while stirring, to 102-104 ℃, first adds the red phosphorus of formula ratio, then passes into slowly the liquid chlorine of formula ratio, start pressurization, pressure regulation power is 0.4Mpa, and chlorination reaction 2-2.4 hour is carried out in insulation, stops stirring, be cooled to 65 ℃, obtain 2-chloropropionic acid.
(2) 2-chloropropionic acid is sent into aminating reaction still, by reactor sealing, the temperature of controlling in reactor is 56-58 ℃, the urotropine that adds while stirring formula ratio, the ammoniacal liquor that adds formula ratio after 5 minutes, stirring reaction 3-3.2 hour, obtains 2-alanine.
(3) 2-alanine is sent into crystallization kettle, send into the methyl alcohol that is about 3 times of 2-alanine volumes, stir after 30 minutes and stop stirring, standing 24 hours, crystallization was complete.
(4) liquid in crystallization kettle is discharged, the xln of lower floor's L-Ala is sent into whizzer and is carried out solid-liquid separation, L-Ala solid after solid-liquid separation is sent into Vacuumdrier to be dried, dry 11-13 hour at 75 ℃-85 ℃, after being dried, can fragmentation sieve, then packing obtains L-Ala finished product.
Temperature of reaction in step (1) chlorination reaction still is 103 ℃.
Drying temperature in step (4) in drying machine is 80 ℃, and be 12 hours time of drying.
The invention has the beneficial effects as follows: a kind of method of producing L-Ala is provided, this production method have technique simple, use general-purpose equipment, without high-temperature high-voltage reaction, be easy to the series of advantages such as production operation, production cost are low, good product quality, can produce high-quality L-Ala.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
By accounting for total amount, be that 18% propionic acid is in sending into after the assay was approved chlorination reaction still, reactor is sealed, warming while stirring is to 102-104 ℃, by accounting for total amount, is first that 1% red phosphorus adds, then pass into slowly account for total amount be 21% liquid chlorine, start pressurization, pressure regulation power is 0.4Mpa, and insulation is carried out chlorination reaction 2 hours, stops stirring, be cooled to 65 ℃, obtain 2-chloropropionic acid; 2-chloropropionic acid is sent into aminating reaction still, and by reactor sealing, the temperature of controlling in reactor is 56-58 ℃, add while stirring that to account for total amount be 2% urotropine, after 5 minutes, add that to account for total amount be 58% ammoniacal liquor, stirring reaction 3.2 hours, obtains 2-alanine; 2-alanine is sent into crystallization kettle, send into the methyl alcohol that is about 3 times of 2-alanine volumes, stir after 30 minutes and stop stirring, standing 24 hours, crystallization was complete; Liquid in crystallization kettle is discharged, the xln of lower floor's L-Ala is sent into whizzer and is carried out solid-liquid separation, by obtaining L-Ala solid after removal moisture, send into Vacuumdrier and be dried, dry 11-13 hour at 75 ℃-85 ℃, after being dried, can fragmentation sieve, then packing obtains L-Ala finished product.
Embodiment 2
By accounting for total amount, be that 19% propionic acid is in sending into after the assay was approved chlorination reaction still, reactor is sealed, warming while stirring is to 102-104 ℃, by accounting for total amount, is first that 1% red phosphorus adds, then pass into slowly account for total amount be 20% liquid chlorine, start pressurization, pressure regulation power is 0.4Mpa, and insulation is carried out chlorination reaction 2.2 hours, stops stirring, be cooled to 65 ℃, obtain 2-chloropropionic acid; 2-chloropropionic acid is sent into aminating reaction still, and by reactor sealing, the temperature of controlling in reactor is 56-58 ℃, add while stirring that to account for total amount be 2% urotropine, after 5 minutes, add that to account for total amount be 58% ammoniacal liquor, stirring reaction 3.1 hours, obtains 2-alanine; 2-alanine is sent into crystallization kettle, send into the methyl alcohol that is about 3 times of 2-alanine volumes, stir after 30 minutes and stop stirring, standing 24 hours, crystallization was complete; Liquid in crystallization kettle is discharged, the xln of lower floor's L-Ala is sent into whizzer and is carried out solid-liquid separation, by obtaining L-Ala solid after removal moisture, send into Vacuumdrier and be dried, dry 11-13 hour at 75 ℃-85 ℃, after being dried, can fragmentation sieve, then packing obtains L-Ala finished product.
Embodiment 3
By accounting for total amount, be that 20% propionic acid is in sending into after the assay was approved chlorination reaction still, reactor is sealed, warming while stirring is to 102-104 ℃, by accounting for total amount, is first that 1% red phosphorus adds, then pass into slowly account for total amount be 19% liquid chlorine, start pressurization, pressure regulation power is 0.4Mpa, and insulation is carried out chlorination reaction 2.4 hours, stops stirring, be cooled to 65 ℃, obtain 2-chloropropionic acid; 2-chloropropionic acid is sent into aminating reaction still, and by reactor sealing, the temperature of controlling in reactor is 56-58 ℃, add while stirring that to account for total amount be 2% urotropine, after 5 minutes, add that to account for total amount be 58% ammoniacal liquor, stirring reaction 3 hours, obtains 2-alanine; 2-alanine is sent into crystallization kettle, send into the methyl alcohol that is about 3 times of 2-alanine volumes, stir after 30 minutes and stop stirring, standing 24 hours, crystallization was complete; Liquid in crystallization kettle is discharged, the xln of lower floor's L-Ala is sent into whizzer and is carried out solid-liquid separation, by obtaining L-Ala solid after removal moisture, send into Vacuumdrier and be dried, dry 11-13 hour at 75 ℃-85 ℃, after being dried, can fragmentation sieve, then packing obtains L-Ala finished product.
Claims (2)
1. a production method for L-Ala, the proportioning raw materials of use is: propionic acid 18%-20%, red phosphorus 1%, liquid chlorine 19%-21, ammoniacal liquor 58%, urotropine 2%, methyl alcohol are appropriate; It is characterized in that: step (1) by the propionic acid of formula ratio in sending into after the assay was approved chlorination reaction still, reactor is sealed, warming while stirring, to 102-104 ℃, first adds the red phosphorus of formula ratio, then passes into slowly the liquid chlorine of formula ratio, start pressurization, pressure regulation power is 0.4Mpa, and chlorination reaction 2-2.4 hour is carried out in insulation, stops stirring, be cooled to 65 ℃, obtain 2-chloropropionic acid; Step (2) is sent 2-chloropropionic acid into aminating reaction still, and by reactor sealing, the temperature of controlling in reactor is 56-58 ℃, the urotropine that adds while stirring formula ratio, the ammoniacal liquor that adds formula ratio after 5 minutes, stirring reaction 3-3.2 hour, obtains 2-alanine; Step (3) is sent 2-alanine into crystallization kettle, sends into the methyl alcohol that is about 3 times of 2-alanine volumes, stirs after 30 minutes and stops stirring, and standing 24 hours, crystallization was complete; Step (4) is discharged the liquid in crystallization kettle, the xln of lower floor's L-Ala is sent into whizzer and is carried out solid-liquid separation, L-Ala solid after solid-liquid separation is sent into Vacuumdrier to be dried, dry 11-13 hour at 75 ℃-85 ℃, after being dried, can fragmentation sieve, then packing obtains L-Ala finished product.
The production method of a kind of L-Ala according to claim 1, the feature of its step (1) is: the temperature of reaction in described chlorination reaction still is 103 ℃.
2. the production method of a kind of L-Ala according to claim 1, the feature of its step (4) is: the drying temperature in described drying machine is 80 ℃, be 12 hours time of drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210235178.5A CN103539686A (en) | 2012-07-09 | 2012-07-09 | Method for producing aminopropionic acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210235178.5A CN103539686A (en) | 2012-07-09 | 2012-07-09 | Method for producing aminopropionic acid |
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| CN103539686A true CN103539686A (en) | 2014-01-29 |
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| CN201210235178.5A Pending CN103539686A (en) | 2012-07-09 | 2012-07-09 | Method for producing aminopropionic acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105037186A (en) * | 2015-06-17 | 2015-11-11 | 苏州敬业医药化工有限公司 | Preparation method of aminomethylbenzoic acid |
| CN113683521A (en) * | 2021-08-25 | 2021-11-23 | 宁夏友奇药业有限公司 | Novel method for producing 2-amino-1, 3-propylene glycol by JIT method |
-
2012
- 2012-07-09 CN CN201210235178.5A patent/CN103539686A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105037186A (en) * | 2015-06-17 | 2015-11-11 | 苏州敬业医药化工有限公司 | Preparation method of aminomethylbenzoic acid |
| CN113683521A (en) * | 2021-08-25 | 2021-11-23 | 宁夏友奇药业有限公司 | Novel method for producing 2-amino-1, 3-propylene glycol by JIT method |
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Application publication date: 20140129 |