CN102304093A - Process for producing sulfadimidine - Google Patents
Process for producing sulfadimidine Download PDFInfo
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- CN102304093A CN102304093A CN201110110245A CN201110110245A CN102304093A CN 102304093 A CN102304093 A CN 102304093A CN 201110110245 A CN201110110245 A CN 201110110245A CN 201110110245 A CN201110110245 A CN 201110110245A CN 102304093 A CN102304093 A CN 102304093A
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- sulphamethazine
- neutralization
- sulfadimidine
- hydrochloric acid
- solvent
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Abstract
The invention relates to a process for producing sulfadimidine. Sulfaguanidine and acetylacetone are taken as raw materials; and the process comprises the following steps of: 1, performing condensation reaction to obtain a wet product of sulfadimidine; 2, washing with hot water to obtain a wet product of sulfadimidine, and removing other inclusions in a reaction solvent; 3, adding active carbon and caustic soda liquid into the washed sulfadimidine and performing alkali dissolution decoloration; 4, neutralizing caustic soda liquid brought by the decolored sulfadimidine by using an acid solvent, and crystallizing; and 5, separating out crystallized sulfadimidine by adopting a centrifugal analysis method, and drying to obtain a finished product. The process is characterized in that: in the neutralizing and crystallizing step, the acid solvent neutralization is hydrochloric acid neutralization. In the whole chemical production, hydrochloric acid is taken as a byproduct and can be recycled massively; and the hydrochloric acid replaces the conventional acetic acid neutralization solvent, which is more economic, and the quality of the obtained product is improved.
Description
Technical field
The present invention relates in a kind of sulfamido product the sulphamethazine production technique.
Background technology
Sulphamethazine is a kind of water, ether of being insoluble in, and has treatment hemolytic coccus, meningococcus and pneumococcal effect.In the technological process of preparation sulphamethazine, adopt acetic acid to go up residual liquid caustic soda in the single step reaction as neutralization in neutralization, the crystallisation process.From integration factory, consider that the employing of acetic acid needs outsourcing, and has the hydrochloric acid of same neutralizing effect, is to produce as the tail gas hydrogen chloride gas in process of production in the technological process of these classification soups of production; If only adopt acetic acid as in and medicament, the market value of acetic acid is higher than hydrochloric acid, has not only increased raw materials cost greatly, and the tail gas hydrogenchloride of yet having wasted in chemical process is not really recycled, and is a kind of wastage of material yet.
Summary of the invention
Technical problem to be solved by this invention provides a kind of sulphamethazine production technique that reduces cost, increases economic efficiency.
The present invention solves the technical scheme that its technical problem takes: a kind of sulphamethazine production technique; With sulfanilylguanidine and methyl ethyl diketone is raw material; Carry out condensation reaction in the first step; Make wet article sulphamethazine after the condensation; Second step made wet article sulphamethazine with hot wash; Remove other spin offs in the reaction solvent; The 3rd step; Add gac and liquid caustic soda in the sulphamethazine after washing and carry out the processing of alkali solution-off look; In the 4th step, adopt acid solvent to neutralize crystallization afterwards for the liquid caustic soda of taking out of in the sulphamethazine after the decolouring; The 5th step; Adopt the centrifugal analysis method to separate out for the sulphamethazine after the crystallization, carry out drying, make finished product; It is characterized in that: said neutralization; In the crystallisation step, the neutralization of the acid solvent of employing is the hydrochloric acid neutralization.
In order when increasing economic efficiency, to guarantee the quality of product sulphamethazine product, in said neutralization, crystallisation step, neutral temperature remains between 90 ℃ to 100 ℃, and the concentration of said hydrochloric acid is 6%～12%.
For the residual alkali lye of more effective neutralization, in said neutralization, the crystallisation step, when neutral temperature was controlled at 92 ℃ to 94 ℃, the concentration of hydrochloric acid of employing was 11%.
In order to remain in the alkali lye in the sulphamethazine solution in reaching effectively with in the alkali lye decoloring reaction, in said neutralization, the crystallisation step, when neutral temperature was controlled at 96 ℃ to 98 ℃, the concentration of hydrochloric acid of employing was 7%.
The invention has the beneficial effects as follows: neutralize with salt acid substitution acetic acid originally, not only reach neutralization, in having reduced and cost; In neutralization.In the crystallisation process, make the process condition of reaction obtain optimization, the concentration of hydrochloric acid of employing has ensured the crystallization quality product.
Description of drawings:
Fig. 1 is a production technique synoptic diagram of the present invention.
Embodiment
A kind of sulphamethazine production technique shown in Fig. 1; With sulfanilylguanidine and methyl ethyl diketone is raw material; Carry out condensation reaction in the first step; Make wet article sulphamethazine after the condensation; Second step made wet article sulphamethazine with hot wash; Remove other spin offs in the reaction solvent; The 3rd step; Add gac and liquid caustic soda in the sulphamethazine after washing and carry out the processing of alkali solution-off look; In the 4th step, adopt acid solvent to neutralize crystallization afterwards for the liquid caustic soda of taking out of in the sulphamethazine after the decolouring; The 5th step; Adopt the centrifugal analysis method to separate out for the sulphamethazine after the crystallization, carry out drying, make finished product; It is characterized in that: said neutralization; In the crystallisation step, the neutralization of the acid solvent of employing is the hydrochloric acid neutralization.
In order when increasing economic efficiency, to guarantee the quality of product sulphamethazine product; In said neutralization, crystallisation step; Neutral temperature remains between 90 ℃ to 100 ℃, and the concentration of said hydrochloric acid is 6%～12%, in the time of between the pH value of solution arrives 6.4～6.7 be in and terminal point.
For the residual alkali lye of more effective neutralization, in said neutralization, the crystallisation step, when neutral temperature was controlled at 92 ℃ to 94 ℃, the concentration of hydrochloric acid of employing was 11%, in the time of between the pH value of solution arrives 6.4～6.7 be in and terminal point.
In order to remain in the alkali lye in the sulphamethazine solution in reaching effectively with in the alkali lye decoloring reaction; In said neutralization, the crystallisation step; When neutral temperature was controlled at 96 ℃ to 98 ℃, the concentration of hydrochloric acid of employing was 7%, in the time of between the pH value of solution arrives 6.4～6.7 be in and terminal point.
The present invention neutralizes with salt acid substitution acetic acid originally; Not only reach neutralization; Cost as far as product; Adopt 1.44 yuan/kilogram of acetic acid; And adopt hydrochloric acid is 0.3 yuan/kilogram, and every kilogram finished product can be saved 1.14 yuan; Annual economical savings is just up to a million, in greatly reducing and cost; In neutralization.In the crystallisation process, make the process condition of reaction obtain optimization, under this temperature of reaction, the concentration of hydrochloric acid of employing has ensured the crystallization quality product.
Claims (4)
1. sulphamethazine production technique; With sulfanilylguanidine and methyl ethyl diketone is raw material; Carry out condensation reaction in the first step; Make wet article sulphamethazine after the condensation; Second step made wet article sulphamethazine with hot wash; Remove other spin offs in the reaction solvent; The 3rd step; Add gac and liquid caustic soda in the sulphamethazine after washing and carry out the processing of alkali solution-off look; In the 4th step, adopt acid solvent to neutralize crystallization afterwards for the liquid caustic soda of taking out of in the sulphamethazine after the decolouring; The 5th step; Adopt the centrifugal analysis method to separate out for the sulphamethazine after the crystallization, carry out drying, make finished product; It is characterized in that: said neutralization; In the crystallisation step, the neutralization of the acid solvent of employing is the hydrochloric acid neutralization.
2. sulphamethazine production technique according to claim 1 is characterized in that: in said neutralization, crystallisation step, neutral temperature remains between 90 ℃ to 100 ℃, and the concentration of said hydrochloric acid is 6%～12%.
3. sulphamethazine production technique according to claim 2 is characterized in that: in said neutralization, the crystallisation step, when neutral temperature was controlled at 92 ℃ to 94 ℃, the concentration of hydrochloric acid of employing was 11%.
4. sulphamethazine production technique according to claim 2 is characterized in that: in said neutralization, the crystallisation step, when neutral temperature was controlled at 96 ℃ to 98 ℃, the concentration of hydrochloric acid of employing was 7%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110110245A CN102304093A (en) | 2011-04-29 | 2011-04-29 | Process for producing sulfadimidine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110110245A CN102304093A (en) | 2011-04-29 | 2011-04-29 | Process for producing sulfadimidine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102304093A true CN102304093A (en) | 2012-01-04 |
Family
ID=45378031
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110110245A Pending CN102304093A (en) | 2011-04-29 | 2011-04-29 | Process for producing sulfadimidine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102304093A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709109A (en) * | 2013-12-24 | 2014-04-09 | 福建省福抗药业股份有限公司 | Preparation method of sulfadimidine hydrosulfate |
| RU2657241C2 (en) * | 2016-05-23 | 2018-06-09 | Открытое акционерное общество "Ирбитский химико-фармацевтический завод" | Method for preparation of sulfadimezine (variants) |
| CN111269187A (en) * | 2020-03-18 | 2020-06-12 | 湖南吴赣药业有限公司 | Environment-friendly synthesis method of sulfadiazine |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2429184A (en) * | 1942-03-05 | 1947-10-14 | Ciba Pharm Prod Inc | Process of making rho-aminobenzenesulphonamidopyrimidines |
| US2631147A (en) * | 1951-08-28 | 1953-03-10 | Us Rubber Co | Preparation of medicinal grade sulfamethazine |
| US3395141A (en) * | 1966-04-29 | 1968-07-30 | American Cyanamid Co | Preparation of sulfamethazine and acetyl sulfamethazine |
-
2011
- 2011-04-29 CN CN201110110245A patent/CN102304093A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2429184A (en) * | 1942-03-05 | 1947-10-14 | Ciba Pharm Prod Inc | Process of making rho-aminobenzenesulphonamidopyrimidines |
| US2631147A (en) * | 1951-08-28 | 1953-03-10 | Us Rubber Co | Preparation of medicinal grade sulfamethazine |
| US3395141A (en) * | 1966-04-29 | 1968-07-30 | American Cyanamid Co | Preparation of sulfamethazine and acetyl sulfamethazine |
Non-Patent Citations (1)
| Title |
|---|
| 徐开堃等: "《合成药物》", 30 November 1959, 上海科学技术出版社, article "磺胺二甲嘧啶", pages: 22-24 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709109A (en) * | 2013-12-24 | 2014-04-09 | 福建省福抗药业股份有限公司 | Preparation method of sulfadimidine hydrosulfate |
| CN103709109B (en) * | 2013-12-24 | 2016-08-17 | 福建省福抗药业股份有限公司 | A kind of preparation method of sulfadimidine hydrosulfate |
| RU2657241C2 (en) * | 2016-05-23 | 2018-06-09 | Открытое акционерное общество "Ирбитский химико-фармацевтический завод" | Method for preparation of sulfadimezine (variants) |
| CN111269187A (en) * | 2020-03-18 | 2020-06-12 | 湖南吴赣药业有限公司 | Environment-friendly synthesis method of sulfadiazine |
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| PB01 | Publication | ||
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120104 |