CN103102295A - Production method of acetylcysteine - Google Patents
Production method of acetylcysteine Download PDFInfo
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- CN103102295A CN103102295A CN2012100842782A CN201210084278A CN103102295A CN 103102295 A CN103102295 A CN 103102295A CN 2012100842782 A CN2012100842782 A CN 2012100842782A CN 201210084278 A CN201210084278 A CN 201210084278A CN 103102295 A CN103102295 A CN 103102295A
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Abstract
The invention discloses a production method of acetylcysteine, belonging to the field of manufacturing amino acid. In the method, cysteine hydrochloride monohydrate is taken as main raw materials, and anhydride, 20% liquid caustic soda and water are take as auxiliary materials. The production method comprises the steps: conducting an acylation reaction, cooling and crystallization, centrifugal separation, drying and other procedures through devices of a ceramic reaction kettle, a cooling reaction kettle, a centrifugal machine and a vacuum drier to obtain finished product. Compared with the prior art, the production method has a series of advantages of being simple in technique, capable of using universal equipment, free from emission of three wastes, free from 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, is capable of conducting batch production and producing high-quality acetylcysteine.
Description
Technical field
The invention belongs to amino acid and make the field, relate in particular to a kind of method of producing acetylcysteine take cysteine hydrochloride monohydrate as raw material in batches.
Background technology
Acetylcysteine, have another name called N-acetyl-L-cysteine, N-acetylcystein, Fluimucil, acetylcystein, mucofilin, muco-sof powder etc., molecular formula is C5H9NO3S, molecular weight is 163.20, and outward appearance is white crystalline powder, 101 ℃ of fusing points--107 ℃, soluble in water and ethanol, the foul smell that similar garlic is arranged, flavor acid has water absorbability.acetylcysteine is mucolytic agent, because containing sulfydryl in its molecular formula, can make the cystine linkage fracture in polypeptide chain, reduce the viscosity of phlegm, and make it to liquefy, acetylcysteine can also make the DNA fiber fracture in purulent sputum, therefore can not only dissolve the sticking phlegm of white and can dissolve purulent sputum, reduce the viscosity of phlegm, phlegm is easily discharged, be applicable to glue in a large number the phlegm resistance and cause expiratory dyspnea, and the illness of the difficulty of coughing up phlegm, the respiratory system infection for the treatment of take dense pituita excess secretion as feature, as acute bronchitis, chronic bronchitis, chronic obstructive pulmonary disease, pulmonary emphysema, bronchiectasis and glue consistence mucus disease, the cough up phlegm treatment of difficult person and idiopathic interstitial lung also has good effect for postoperative, this product also can be used for poisoning by paracetamol patient's detoxifcation and children's's non-suppurative otitis media, in case deaf.Using method is: 1. spraying, make it to be dissolved into 10% solution with sodium chloride injection, and spraying sucks, and a 1-3 milliliter 2-3 time on the one, uses under nonemergency; 2. tracheae splashes into, during first aid with 5% solution through tracheae or directly splash in tracheae, each 1-2 milliliter, 2-6 time on the 1st; 3. tracheae injects, during first aid with 5% solution with syringe in tracheae ring-type cartilaginous ring first film injected gas tube chamber, 0.5-2 milliliter at every turn; 4. oral, each 300 milligrams, every day 3 times.the technique of producing acetylcysteine is more, the present invention is produce this Product Process a kind of, take cysteine hydrochloride monohydrate as main raw material, with acid anhydrides, 20% liquid caustic soda, hydrochloric acid, water is auxiliary material, with ceramic reactor, cooling reactor, whizzer, Vacuumdrier is equipment, pass through acylation reaction, crystallisation by cooling, centrifugation, the operations such as oven dry make finished product, this production method compared to the prior art, has 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 acetylcysteine.
Summary of the invention
The problem that the present invention mainly solves is to provide a kind of production method of acetylcysteine; the method is take cysteine hydrochloride monohydrate as main raw material; take acid anhydrides, 20% liquid caustic soda, hydrochloric acid, water as auxiliary material; make finished product by operations such as acylation reaction, crystallisation by cooling, centrifugation, oven dry; the proportioning raw materials that the present invention uses is: 300 kilograms of cysteine hydrochloride monohydrates, 1650 kilograms, water, 1 cubic metre, acid anhydrides, 20% liquid caustic soda is appropriate, hydrochloric acid is appropriate, and the equipment of use is 2 tons of ceramic reactors, 2 tons of cooling reactors, whizzer, Vacuumdrier.
The present invention can be achieved through the following technical solutions:
A kind of production method of acetylcysteine is characterized in that being made of following steps:
(1) with 300 kilograms of cysteine hydrochloride monohydrates in sending into after the assay was approved 2 tons of ceramic reactors; and add 1650 kilograms of stirrings of water and become liquid state; reactor is sealed; pass into successively 1 cubic metre, acid anhydrides; then adding while stirring appropriate concentration is 20% liquid caustic soda; recording the pH value reaches at 12 o'clock and stops adding alkali; pressurization begins to heat; pressure regulation power is 0.4Mpa; temperature is 125 ℃-135 ℃, and insulation was carried out acylation reaction 1.8-2.2 hour, then added appropriate hydrochloric acid; measure the pH value and reach at 3 o'clock, stop stirring.
(2) material in 2 tons of ceramic reactors is transferred to 2 tons of cooling reactors while hot, uses while stirring circulating brine that material in still is cooled to rapidly below 3 ℃, obtain the acetylcysteine xln.
(3) the acetylcysteine xln is sent into whizzer and carry out solid-liquid separation, to remove and obtain the acetylcysteine solid after moisture and send into Vacuumdrier and carry out drying, under 75 ℃-85 ℃ dry 11-13 hour, can fragmentation sieve after drying is completed, then packing namely obtains the acetylcysteine finished product.
Temperature of reaction in step (1) is 125 ℃, 130 ℃, 135 ℃.
When in step (3), the drying temperature of drying machine is 75 ℃, be 13 hours corresponding time of drying; Be 12 hours time of drying that is 80 ℃ of correspondences; When being 85 ℃, be 11 hours corresponding time of drying.
The invention has the beneficial effects as follows: a kind of method of producing acetylcysteine in batches is provided, this production method have technique simple, use general-purpose equipment, 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 acetylcysteine.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
300 kilograms of cysteine hydrochloride monohydrates in sending into after the assay was approved 2 tons of ceramic reactors, and are added 1650 kilograms of stirrings of water and become liquid state, reactor is sealed, pass into successively 1 cubic metre, acid anhydrides, then adding while stirring appropriate concentration is 20% liquid caustic soda, records the pH value and reaches at 12 o'clock and stop adding alkali, and pressurization begins to heat, pressure regulation power is 0.4Mpa, temperature is 125 ℃, and insulation was carried out acylation reaction 2.2 hours, then added appropriate hydrochloric acid, measure the pH value and reach at 3 o'clock, stop stirring; Material in 2 tons of ceramic reactors is transferred to 2 tons of cooling reactors while hot, uses while stirring circulating brine that material in still is cooled to rapidly below 3 ℃, obtain the acetylcysteine xln; The acetylcysteine xln is sent into whizzer carry out solid-liquid separation, to remove and obtain the acetylcysteine solid after moisture and send into Vacuumdrier and carry out drying, drying is 13 hours under 75 ℃, can fragmentation sieve after drying is completed, and then the packing warehouse-in namely obtains the acetylcysteine finished product.
Embodiment 2
300 kilograms of cysteine hydrochloride monohydrates in sending into after the assay was approved 2 tons of ceramic reactors, and are added 1650 kilograms of stirrings of water and become liquid state, reactor is sealed, pass into successively 1 cubic metre, acid anhydrides, then adding while stirring appropriate concentration is 20% liquid caustic soda, records the pH value and reaches at 12 o'clock and stop adding alkali, and pressurization begins to heat, pressure regulation power is 0.4Mpa, temperature is 130 ℃, and insulation was carried out acylation reaction 2 hours, then added appropriate hydrochloric acid, measure the pH value and reach at 3 o'clock, stop stirring; Material in 2 tons of ceramic reactors is transferred to 2 tons of cooling reactors while hot, uses while stirring circulating brine that material in still is cooled to rapidly below 3 ℃, obtain the acetylcysteine xln; The acetylcysteine xln is sent into whizzer carry out solid-liquid separation, to remove and obtain the acetylcysteine solid after moisture and send into Vacuumdrier and carry out drying, drying is 12 hours under 80 ℃, can fragmentation sieve after drying is completed, and then the packing warehouse-in namely obtains the acetylcysteine finished product.
Embodiment 3
300 kilograms of cysteine hydrochloride monohydrates in sending into after the assay was approved 2 tons of ceramic reactors, and are added 1650 kilograms of stirrings of water and become liquid state, reactor is sealed, pass into successively 1 cubic metre, acid anhydrides, then adding while stirring appropriate concentration is 20% liquid caustic soda, records the pH value and reaches at 12 o'clock and stop adding alkali, and pressurization begins to heat, pressure regulation power is 0.4Mpa, temperature is 135 ℃, and insulation was carried out acylation reaction 1.8 hours, then added appropriate hydrochloric acid, measure the pH value and reach at 3 o'clock, stop stirring; Material in 2 tons of ceramic reactors is transferred to 2 tons of cooling reactors while hot, uses while stirring circulating brine that material in still is cooled to rapidly below 3 ℃, obtain the acetylcysteine xln; The acetylcysteine xln is sent into whizzer carry out solid-liquid separation, to remove and obtain the acetylcysteine solid after moisture and send into Vacuumdrier and carry out drying, drying is 11 hours under 85 ℃, can fragmentation sieve after drying is completed, and then the packing warehouse-in namely obtains the acetylcysteine finished product.
Claims (3)
1. the production method of an acetylcysteine, the proportioning raw materials of using is: 300 kilograms of cysteine hydrochloride monohydrates, 1650 kilograms, water, 1 cubic metre, acid anhydrides, 20% liquid caustic soda is appropriate, hydrochloric acid is appropriate, and the equipment of use is 2 tons of ceramic reactors, 2 tons of cooling reactors, whizzer, Vacuumdrier; It is characterized in that: step (1) with 300 kilograms of cysteine hydrochloride monohydrates in sending into after the assay was approved 2 tons of ceramic reactors, and add 1650 kilograms of stirrings of water and become liquid state, reactor is sealed, pass into successively 1 cubic metre, acid anhydrides, then adding while stirring appropriate concentration is 20% liquid caustic soda, recording the pH value reaches at 12 o'clock and stops adding alkali, pressurization begins to heat, pressure regulation power is 0.4Mpa, temperature is 125 ℃-135 ℃, and insulation was carried out acylation reaction 1.8-2.2 hour, then added appropriate hydrochloric acid, measure the pH value and reach at 3 o'clock, stop stirring; Step (2) is transferred to 2 tons of cooling reactors while hot with material in 2 tons of ceramic reactors, uses while stirring circulating brine that material in still is cooled to rapidly below 3 ℃, obtains the acetylcysteine xln; Step (3) is sent the acetylcysteine xln into whizzer and is carried out solid-liquid separation, to remove and obtain the acetylcysteine solid after moisture and send into Vacuumdrier and carry out drying, under 75 ℃-85 ℃ dry 11-13 hour, can fragmentation sieve after drying is completed, then packing namely obtains the acetylcysteine finished product.
2. the production method of a kind of acetylcysteine according to claim 1, the feature of its step (1) is: described temperature of reaction is 125 ℃, 130 ℃, 135 ℃.
3. the production method of a kind of acetylcysteine according to claim 1, the feature of its step (4) is: the drying temperature in described drying machine when being 75 ℃ corresponding time of drying be 13 hours; Be 12 hours time of drying that is 80 ℃ of correspondences; When being 85 ℃, be 11 hours corresponding time of drying.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100842782A CN103102295A (en) | 2012-03-28 | 2012-03-28 | Production method of acetylcysteine |
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| CN2012100842782A CN103102295A (en) | 2012-03-28 | 2012-03-28 | Production method of acetylcysteine |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104098491A (en) * | 2014-07-17 | 2014-10-15 | 蒋银妹 | Acetylcysteine compound and acetylcysteine solution being used for inhalation and containing same |
| CN104844488A (en) * | 2015-03-25 | 2015-08-19 | 武汉远大弘元股份有限公司 | Production method of N-acetyl-L-cysteine |
| CN109096161A (en) * | 2018-08-24 | 2018-12-28 | 武汉远大弘元股份有限公司 | A kind of preparation method of N-acetylcystein |
-
2012
- 2012-03-28 CN CN2012100842782A patent/CN103102295A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104098491A (en) * | 2014-07-17 | 2014-10-15 | 蒋银妹 | Acetylcysteine compound and acetylcysteine solution being used for inhalation and containing same |
| CN104098491B (en) * | 2014-07-17 | 2016-08-17 | 蒋银妹 | A kind of mucolyticum acid compound and the suction acetylcysteine solution containing this compound |
| CN104844488A (en) * | 2015-03-25 | 2015-08-19 | 武汉远大弘元股份有限公司 | Production method of N-acetyl-L-cysteine |
| CN104844488B (en) * | 2015-03-25 | 2016-08-24 | 武汉远大弘元股份有限公司 | A kind of production method of N-acetyl-L-cysteine |
| CN109096161A (en) * | 2018-08-24 | 2018-12-28 | 武汉远大弘元股份有限公司 | A kind of preparation method of N-acetylcystein |
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Application publication date: 20130515 |