CN103102294A

CN103102294A - Production method carboxymethyl cysteine

Info

Publication number: CN103102294A
Application number: CN2012100850420A
Authority: CN
Inventors: 不公告发明人
Original assignee: XINYI HANLING BIO-ENGINEERING Co Ltd
Current assignee: XINYI HANLING BIO-ENGINEERING Co Ltd
Priority date: 2012-03-28
Filing date: 2012-03-28
Publication date: 2013-05-15

Abstract

The invention discloses a production method of carboxymethyl cysteine. The product belongs to the field of manufacturing of amino acids. According to the invention, cysteine hydrochloride monohydrate is used as a main raw material, chloroacetic acid, liquid ammonia, activated carbon and refined hydrochloric acid are used as auxiliary materials, a ceramic reaction kettle, a filtering machine, a centrifugal machine and a vacuum drier are used as apparatuses, and acidification reaction, decolorizing filtration, centrifugal separation, drying and other steps are utilized to prepare the carboxymethyl cysteine. Compared with the prior art, the production method disclosed by the invention has the advantages of simple technique, fewer general-purpose apparatuses, no discharge of three wastes, no high-temperature high-pressure reaction, low production cost, high yield, high product quality and the like, is easy for production operation, and can implement mass production of high-quality carboxymethyl cysteine.

Description

A kind of production method of Carbocisteine

Technical field

The invention belongs to amino acid and make the field, relate in particular to a kind of method of producing Carbocisteine take cysteine hydrochloride monohydrate as raw material in batches.

Background technology

Carbocisteine, have another name called vinegar sulphur L-Ala, the peace bromohydrin, NA-872, Ambroxl, molecular weight is 179.1943, molecular formula is C5H9NO4S, molecular weight is 179.1943, specific optical rotation is-32.5 ℃-36.0 ℃, the pH value is 2.80-2.95, clarity of solution transmittance 〉=95.0%, halfcystine≤0.05%, muriate≤0.15%, weight loss on drying≤0.5%, residue on ignition≤0.2%, molysite≤0.001%, heavy metal≤0.002%, outward appearance is white crystalline powder, be insoluble to cold water and ethanol, acetone and other organic solvent, be soluble in acidity and alkaline aqueous solution.Carbocisteine is of many uses: 1. pharmaceutically as expectorant, bronchial mucus secretion is reduced, the viscosity of phlegm descends and is easy to expectoration, thereby can be used for being used for the treatment of the not congruent patient of thick sputum, dys-expectoration, pulmonary ventilation function that chronic tracheitis, pulmonary emphysema, pulmonary tuberculosis, bronchial asthma etc. cause; 2. can be used for the synthesizing of multi-medicament, be a kind of important medicine intermediate and industrial chemicals; 3. in daily life as hair finishing composition and conditioning agent, also can be used as anti-acne drug use.When being used for the treatment of the thick sputum that chronic tracheitis, pulmonary emphysema, pulmonary tuberculosis, bronchial asthma etc. cause, adult's consumption is 500 milligrams of every days, and minute 3-4 time oral.The technique of producing Carbocisteine is more, can make final product by different routes with different raw materials, the present invention is produce this Product Process a kind of, take cysteine hydrochloride monohydrate as main raw material, take Mono Chloro Acetic Acid, liquefied ammonia, gac, refining hydrochloric acid as auxiliary material, take ceramic reactor, filter, whizzer, Vacuumdrier as equipment, make Carbocisteine by adding the operations such as acid-respons, decolorization filtering, centrifugation, oven dry.This production method compared to the prior art, have technique simple, use general-purpose equipment and number of devices is few, three-waste free discharge, without high-temperature high-voltage reaction, be easy to production operation, the series of advantages such as production cost is low and productive rate is high, good product quality, can be mass, can produce high-quality Carbocisteine.

Summary of the invention

the problem that the present invention mainly solves is to provide a kind of production method of Carbocisteine, the method is take cysteine hydrochloride monohydrate as main raw material, with Mono Chloro Acetic Acid, liquefied ammonia, gac, refining hydrochloric acid is auxiliary material, by adding acid-respons, decolorization filtering, centrifugation, the operations such as oven dry make finished product, the raw material that the present invention uses is: 300 kilograms of cysteine hydrochloride monohydrates, 1000 liters of Mono Chloro Acetic Acids, liquefied ammonia is appropriate, 6 kilograms of gacs, refining hydrochloric acid 9.5-10.5 equivalent, the equipment that uses is 2 tons of ceramic reactors, strainer, whizzer, Vacuumdrier.

The present invention can be achieved through the following technical solutions:

A kind of production method of Carbocisteine is characterized in that being made of following steps:

(1) send into after the assay was approved 300 kilograms of cysteine hydrochloride monohydrates in ceramic reactor, add 1000 liters of Mono Chloro Acetic Acids, start agitator, rotating speed is 20 rev/mins, cysteine hydrochloride monohydrate and Mono Chloro Acetic Acid are mixed into thick liquid, add appropriate liquefied ammonia, adjust pH reaches between 9.5-10.5, stirring reaction adds the gac of 6 kilograms after 2 hours, simultaneously sending into steam to the reactor interlayer heats, transfer reactor temperature to 58 ℃-62 ℃, reaction decolouring 0.5 hour, then reactant being sent into filter filters, after filtering, filtrate is sent into ceramic reactor again, the refining hydrochloric acid that adds the 9.5-10.5 equivalent, adjust pH is 2.8-3.2, then the stirred crystallization while lowering the temperature, obtain the Carbocisteine solid.

(2) the Carbocisteine solid is sent into whizzer and carry out solid-liquid separation, obtain the Carbocisteine xln.

(3) the Carbocisteine xln is sent into Vacuumdrier and carry out drying, under 78 ℃-82 ℃ dry 3.8-4.2 hour, the parallel operation dry blending that can sieve, the packing warehouse-in namely obtains the Carbocisteine finished product.

Temperature of reaction in step (1) in reactor is 58 ℃, 60 ℃, 62 ℃; The addition of refining hydrochloric acid is respectively 9.5 equivalents, 10 equivalents, 10.5 equivalents.

When in step (3), the drying temperature of drying machine is 78 ℃, be 4.2 hours corresponding time of drying; Be 4 hours time of drying that is 80 ℃ of correspondences; When being 82 ℃, be 3.8 hours corresponding time of drying.

The invention has the beneficial effects as follows: a kind of method of producing Carbocisteine in batches is provided, this production method have technique simple, use general-purpose equipment and number of devices is few, three-waste free discharge, without high-temperature high-voltage reaction, be easy to production operation, the series of advantages such as production cost is low and productive rate is high, good product quality, can be mass, can produce high-quality Carbocisteine.

Embodiment

Below in conjunction with specific embodiment, the present invention is described in further detail.

Embodiment 1

send into after the assay was approved 300 kilograms of cysteine hydrochloride monohydrates in ceramic reactor, add 1000 liters of Mono Chloro Acetic Acids, start agitator, rotating speed is 20 rev/mins, cysteine hydrochloride monohydrate and Mono Chloro Acetic Acid are mixed into thick liquid, add appropriate liquefied ammonia, adjust pH reaches between 9.5-10.5, stirring reaction adds the gac of 6 kilograms after 2 hours, simultaneously sending into steam to the reactor interlayer heats, transfer reactor temperature to 58 ℃, reaction decolouring 0.5 hour, then reactant being sent into filter filters, after filtering, filtrate is sent into ceramic reactor again, the refining hydrochloric acid that adds 9.5 equivalents, adjust pH is 3.2, then the stirred crystallization while lowering the temperature, obtain the Carbocisteine solid, Carbocisteine solid body is sent into whizzer carry out solid-liquid separation, obtain the Carbocisteine xln, the Carbocisteine xln is sent into Vacuumdrier carry out drying, drying is 4.2 hours under 78 ℃, the parallel operation dry blending that can sieve, and the packing warehouse-in namely obtains the Carbocisteine finished product.

Embodiment 2

send into after the assay was approved 300 kilograms of cysteine hydrochloride monohydrates in ceramic reactor, add 1000 liters of Mono Chloro Acetic Acids, start agitator, rotating speed is 20 rev/mins, cysteine hydrochloride monohydrate and Mono Chloro Acetic Acid are mixed into thick liquid, add appropriate liquefied ammonia, adjust pH reaches between 9.5-10.5, stirring reaction adds the gac of 6 kilograms after 2 hours, simultaneously sending into steam to the reactor interlayer heats, transfer reactor temperature to 60 ℃, reaction decolouring 0.5 hour, then reactant being sent into filter filters, after filtering, filtrate is sent into ceramic reactor again, the refining hydrochloric acid that adds 10 equivalents, adjust pH is 3, then the stirred crystallization while lowering the temperature, obtain the Carbocisteine solid, Carbocisteine solid body is sent into whizzer carry out solid-liquid separation, obtain the Carbocisteine xln, the Carbocisteine xln is sent into Vacuumdrier carry out drying, drying is 4 hours under 80 ℃, the parallel operation dry blending that can sieve, and the packing warehouse-in namely obtains the Carbocisteine finished product.

Embodiment 3

send into after the assay was approved 300 kilograms of cysteine hydrochloride monohydrates in ceramic reactor, add 1000 liters of Mono Chloro Acetic Acids, start agitator, rotating speed is 20 rev/mins, cysteine hydrochloride monohydrate and Mono Chloro Acetic Acid are mixed into thick liquid, add appropriate liquefied ammonia, adjust pH reaches between 9.5-10.5, stirring reaction adds the gac of 6 kilograms after 2 hours, simultaneously sending into steam to the reactor interlayer heats, transfer reactor temperature to 62 ℃, reaction decolouring 0.5 hour, then reactant being sent into filter filters, after filtering, filtrate is sent into ceramic reactor again, the refining hydrochloric acid that adds 10.5 equivalents, adjust pH is 2.8, then the stirred crystallization while lowering the temperature, obtain the Carbocisteine solid, Carbocisteine solid body is sent into whizzer carry out solid-liquid separation, obtain the Carbocisteine xln, the Carbocisteine xln is sent into Vacuumdrier carry out drying, drying is 3.8 hours under 82 ℃, the parallel operation dry blending that can sieve, and the packing warehouse-in namely obtains the Carbocisteine finished product.

Claims

1. the production method of a Carbocisteine, the proportioning raw materials of using is: 300 kilograms of cysteine hydrochloride monohydrates, 1000 liters of Mono Chloro Acetic Acids, liquefied ammonia are appropriate, 6 kilograms of gacs, refining hydrochloric acid 9.5-10.5 equivalent, and the equipment of use is 2 tons of ceramic reactors, strainer, whizzer, Vacuumdrier, it is characterized in that: step (1) is sent into 300 kilograms of cysteine hydrochloride monohydrates in ceramic reactor after the assay was approved, add 1000 liters of Mono Chloro Acetic Acids, start agitator, rotating speed is 20 rev/mins, cysteine hydrochloride monohydrate and Mono Chloro Acetic Acid are mixed into thick liquid, add appropriate liquefied ammonia, adjust pH reaches between 9.5-10.5, stirring reaction adds the gac of 6 kilograms after 2 hours, simultaneously sending into steam to the reactor interlayer heats, transfer reactor temperature to 58 ℃-62 ℃, reaction decolouring 0.5 hour, then reactant being sent into filter filters, after filtering, filtrate is sent into ceramic reactor again, the refining hydrochloric acid that adds the 9.5-10.5 equivalent, adjust pH is 2.8-3.2, then the stirred crystallization while lowering the temperature, obtain the Carbocisteine solid, step (2) is sent the Carbocisteine solid into whizzer and is carried out solid-liquid separation, obtains the Carbocisteine xln, step (3) is sent the Carbocisteine xln into Vacuumdrier and is carried out drying, and under 78 ℃-82 ℃ dry 3.8-4.2 hour, the parallel operation dry blending that can sieve, the packing warehouse-in namely obtains the Carbocisteine finished product.

2. the production method of a kind of Carbocisteine according to claim 1, the feature of its step (1) is: the temperature of reaction in described reactor is 58 ℃, 60 ℃, 62 ℃; The addition of refining hydrochloric acid is respectively 9.5 equivalents, 10 equivalents, 10.5 equivalents.

3. the production method of a kind of Carbocisteine according to claim 1, the feature of its step (3) is: the drying temperature in described drying machine when being 78 ℃ corresponding time of drying be 4.2 hours; Be 4 hours time of drying that is 80 ℃ of correspondences; When being 82 ℃, be 3.8 hours corresponding time of drying.