CN103319433A - Production technology of CMI (cell-mediated immunity) industrial antibacterial agent - Google Patents
Production technology of CMI (cell-mediated immunity) industrial antibacterial agent Download PDFInfo
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- CN103319433A CN103319433A CN2013102840273A CN201310284027A CN103319433A CN 103319433 A CN103319433 A CN 103319433A CN 2013102840273 A CN2013102840273 A CN 2013102840273A CN 201310284027 A CN201310284027 A CN 201310284027A CN 103319433 A CN103319433 A CN 103319433A
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Abstract
The invention discloses a production technology of a CMI (cell-mediated immunity) industrial antibacterial agent. The production technology comprises the following steps of: (1) synthesizing crude ester; (2) purifying refined ester; (3) amide synthesizing/centrifuging/drying; (4) chlorination synthesis; (5) filtering hydrochloride; (6) blending and aging; and (7) filtering and packaging. Compared with the prior art, the production technology of the CMI industrial antibacterial agent disclosed by the invention is fewer in steps, simple to operate, easy to industrialize and less in pollution, has good practicability, and can generate good economic benefits and social effects.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to a kind of production technique of CMI industrial bactericide.
Background technology
The CMI industrial bactericide, is more and more used in existing Chemicals preparation as important industrial chemicals.And existing CMI industrial bactericide complicated process of preparation, energy consumption is high, and produces more pollutent and by product, can not satisfy user demand fully.
Summary of the invention
Goal of the invention: for the deficiencies in the prior art, the purpose of this invention is to provide a kind of production technique of CMI industrial bactericide, make its have simply, efficient, cost is low, pollutes the characteristics such as few.
Technical scheme: in order to realize the foregoing invention purpose, the technical solution used in the present invention is as follows:
A kind of production technique of CMI industrial bactericide, concrete steps are as follows:
(1) thick ester is synthetic
In thick ester still, add entry, start and stir and open the refrigerated brine cooling, open the liquid ammonia steel bottle ventilation line, in still, pass into ammonia; Close the liquefied ammonia ventilation line, open hydrogen sulfide steel cylinder ventilation line, the control temperature in the kettle passes into hydrogen sulfide; Led to and closed hydrogen sulfide pipeline, insulated and stirred; In still, in above-mentioned ammonium sulfide, add sulphur, in still, drip methyl acrylate, and evenly pass into hydrogen sulfide simultaneously; Standing demix after reaction finishes, blowing; Organic phase is thick ester, send smart ester purification unit; Water is ammonium sulfide solution, stays in the still and continues for the thick ester of next still is synthetic;
(2) smart ester purifying
The vulcanization unit material is sent into washing kettle, in washing kettle, add entry, start stirring, add again S-WAT, generate the dithio dipropyl dimethyl phthalate; Be incubated after 3 hours, use recirculated water to fall below the temperature in the kettle to 50 ℃, stop to stir, leave standstill 30 minutes after, the upper strata water enters the evaporation concentration still to carry out Sulfothiorine and reclaims, evaporation condensed water is back to smart ester purifying workshop section self, replenishes required process water; Lower floor's oil phase enters acid amides and synthesizes/centrifugal/drying unit;
(3) acid amides synthesizes/centrifugal/drying unit
Methyl alcohol is driven into methylamine prepares still, start stirring, open refrigerated brine and fall the still temperature, open methylamine steel cylinder pipeline, in still, pass into methylamine; Led to and closed methylamine steel cylinder pipeline, after the insulated and stirred methylamine solution that makes has been beaten to the acid amides synthesis reactor; Methylamine solution is joined in the amination still, start stirring, open refrigerated brine and fall the still temperature smart ester is joined in the still, insulated and stirred was got to whizzer with pump after 72 hours; The centrifugal solids that obtains is wet acid amides, send hydrochloride synthetic after the oven dry of drying machine; The centrifuge mother liquor main component is methylamine methyl alcohol, goes still kettle to reclaim methylamine methyl alcohol; Containing methanol waste gas and drying waste gas of volatilizing when centrifugal mixes, and reclaims methyl alcohol after water absorbs, the annual discharging of absorption liquid secondary;
(4) chlorination is synthetic
Add ethyl acetate in the chlorination reaction still, add while stirring the intermediate dithio propionic acid amide that chlorine and drying unit obtain, temperature is controlled at 20～25 ℃, adds rear insulated and stirred 1 hour, and reaction process is controlled the still temperature with refrigerated brine; After reaction finishes, arrive hydrochloride suction filtration device with pump delivery;
(5) hydrochloride suction filtration
Realize solid-liquid separation by vacuum filtration from the hydrochloride slurry that chlorination tank comes the suction filtration device, solid phase is hydrochloride, goes to allotment/aging unit; Liquid phase is the ethyl acetate of containing hydrogen chloride, goes the ethyl acetate rectification cell to reclaim ethyl acetate;
(6) allotment and aging
Water is added compounding kettle, add in proportion hydrochloride under stirring, magnesium nitrate, magnesium chloride, after control still Wen Bingyong magnesium oxide was transferred to 2 with the pH value, being warmed up to 60 ℃ carried out burin-in process 2 hours;
(7) filter and pack
Material after allocating and wearing out is removed the impurity of bringing in the raw material after filtration, obtains highly purified finished product isothiazolinone, adopts plastic tank to pack, sell.
Beneficial effect: compared with prior art, the production technique of CMI industrial bactericide of the present invention, step is few, and is simple to operate, is easy to industrialization, pollutes and lacks, and has good practicality, can produce good economic benefit and social effect.
Description of drawings
Fig. 1 is the production technological process of CMI industrial bactericide.
Embodiment
The present invention is described further below in conjunction with specific embodiment.
Embodiment 1
A kind of technological process of production of CMI industrial bactericide, as shown in Figure 1, concrete steps are as follows:
(1) thick ester is synthetic
Ammonium sulfide preparation: in thick ester still, add entry 1200kg, start and stir and open the refrigerated brine cooling, open the liquid ammonia steel bottle ventilation line, in still, pass into ammonia 90kg.Close the liquefied ammonia ventilation line, open hydrogen sulfide steel cylinder ventilation line, the control temperature in the kettle passes into hydrogen sulfide 100kg.Led to and closed hydrogen sulfide pipeline, insulated and stirred.
Thick ester is synthetic: add sulphur 500kg in above-mentioned ammonium sulfide in still, drip methyl acrylate 1600kg in still, and evenly pass into hydrogen sulfide 352kg simultaneously.Standing demix after reaction finishes, blowing.Organic phase is thick ester, send smart ester purification unit.Water is ammonium sulfide solution, stays in the still and continues for the thick ester of next still is synthetic.
Thick ester synthesis mother liquid is exactly ammonium sulfide solution, plays catalyst action in reaction, as long as strict control techniques condition in producing just can continue to use.
(2) smart ester purifying
The vulcanization unit material is sent into washing kettle, in washing kettle, add entry, start stirring, add again S-WAT (content 〉=96.0%) (temperature be controlled at 63+/-2 ℃), make trithio dipropionic acid dimethyl ester slough one " S ", generate the dithio dipropyl dimethyl phthalate.Keep this temperature after 3 hours, stopped heating uses recirculated water to fall below the temperature in the kettle to 50 ℃, stop to stir, leave standstill 30 minutes after, the upper strata water enters the evaporation concentration still to carry out Sulfothiorine and reclaims, evaporation condensed water is back to smart ester purifying workshop section self, replenishes required process water.Lower floor's oil phase enters acid amides and synthesizes/centrifugal/drying unit.
(3) acid amides synthesizes/centrifugal/drying unit
Methylamine solution preparation: 1600kg methyl alcohol is driven into methylamine prepares still, start stirring, open refrigerated brine and fall the still temperature, open methylamine steel cylinder pipeline, in still, pass into methylamine 700kg.Led to and closed methylamine steel cylinder pipeline, after the insulated and stirred methylamine solution that makes has been beaten to the acid amides synthesis reactor.
Acid amides is synthetic: methylamine solution is joined in the amination still, start stirring, open refrigerated brine and fall the still temperature 2500kg essence ester is joined in the still, insulated and stirred was got to whizzer with pump after 72 hours.
The centrifugal solids that obtains is wet acid amides, send hydrochloride synthetic after the oven dry of drying machine.
The centrifuge mother liquor main component is methylamine methyl alcohol, goes still kettle to reclaim methylamine methyl alcohol.Containing methanol waste gas and drying waste gas of volatilizing when centrifugal mixes, and reclaims methyl alcohol after water absorbs, the annual discharging of absorption liquid (water) secondary.
(4) chlorination is synthetic
Add ethyl acetate in the chlorination reaction still, add while stirring the intermediate dithio propionic acid amide (temperature is controlled at 20～25 ℃) that chlorine and drying unit obtain, add rear insulated and stirred 1 hour, reaction process is controlled the still temperature with refrigerated brine.After reaction finishes, arrive hydrochloride suction filtration device with pump delivery.
(5) hydrochloride suction filtration
Realize solid-liquid separation by vacuum filtration from the hydrochloride slurry that chlorination tank comes the suction filtration device, solid phase is hydrochloride, goes to allotment/aging unit.Liquid phase is the ethyl acetate of containing hydrogen chloride, goes the ethyl acetate rectification cell to reclaim ethyl acetate.
(6) allotment and aging
Water is added compounding kettle, add in proportion hydrochloride under stirring, magnesium nitrate, magnesium chloride after control still Wen Bingyong magnesium oxide is transferred to 2 with pH value, is warmed up to 60 ℃ and carried out burin-in process 2 hours.
(7) filter and pack
Material after allocating and wearing out is removed the impurity of bringing in the raw material after filtration, obtains highly purified finished product isothiazolinone, adopts plastic tank to pack, sell.
Claims (1)
1. the production technique of a CMI industrial bactericide is characterized in that, concrete steps are as follows:
(1) thick ester is synthetic
In thick ester still, add entry, start and stir and open the refrigerated brine cooling, open the liquid ammonia steel bottle ventilation line, in still, pass into ammonia; Close the liquefied ammonia ventilation line, open hydrogen sulfide steel cylinder ventilation line, the control temperature in the kettle passes into hydrogen sulfide; Led to and closed hydrogen sulfide pipeline, insulated and stirred; In still, in above-mentioned ammonium sulfide, add sulphur, in still, drip methyl acrylate, and evenly pass into hydrogen sulfide simultaneously; Standing demix after reaction finishes, blowing; Organic phase is thick ester, send smart ester purification unit; Water is ammonium sulfide solution, stays in the still and continues for the thick ester of next still is synthetic;
(2) smart ester purifying
The vulcanization unit material is sent into washing kettle, in washing kettle, add entry, start stirring, add again S-WAT, generate the dithio dipropyl dimethyl phthalate; Be incubated after 3 hours, use recirculated water to fall below the temperature in the kettle to 50 ℃, stop to stir, leave standstill 30 minutes after, the upper strata water enters the evaporation concentration still to carry out Sulfothiorine and reclaims, evaporation condensed water is back to smart ester purifying workshop section self, replenishes required process water; Lower floor's oil phase enters acid amides and synthesizes/centrifugal/drying unit;
(3) acid amides synthesizes/centrifugal/drying unit
Methyl alcohol is driven into methylamine prepares still, start stirring, open refrigerated brine and fall the still temperature, open methylamine steel cylinder pipeline, in still, pass into methylamine; Led to and closed methylamine steel cylinder pipeline, after the insulated and stirred methylamine solution that makes has been beaten to the acid amides synthesis reactor; Methylamine solution is joined in the amination still, start stirring, open refrigerated brine and fall the still temperature smart ester is joined in the still, insulated and stirred was got to whizzer with pump after 72 hours; The centrifugal solids that obtains is wet acid amides, send hydrochloride synthetic after the oven dry of drying machine; The centrifuge mother liquor main component is methylamine methyl alcohol, goes still kettle to reclaim methylamine methyl alcohol; Containing methanol waste gas and drying waste gas of volatilizing when centrifugal mixes, and reclaims methyl alcohol after water absorbs, the annual discharging of absorption liquid secondary;
(4) chlorination is synthetic
Add ethyl acetate in the chlorination reaction still, add while stirring the intermediate dithio propionic acid amide that chlorine and drying unit obtain, temperature is controlled at 20～25 ℃, adds rear insulated and stirred 1 hour, and reaction process is controlled the still temperature with refrigerated brine; After reaction finishes, arrive hydrochloride suction filtration device with pump delivery;
(5) hydrochloride suction filtration
Realize solid-liquid separation by vacuum filtration from the hydrochloride slurry that chlorination tank comes the suction filtration device, solid phase is hydrochloride, goes to allotment/aging unit; Liquid phase is the ethyl acetate of containing hydrogen chloride, goes the ethyl acetate rectification cell to reclaim ethyl acetate;
(6) allotment and aging
Water is added compounding kettle, add in proportion hydrochloride under stirring, magnesium nitrate, magnesium chloride, after control still Wen Bingyong magnesium oxide was transferred to 2 with the pH value, being warmed up to 60 ℃ carried out burin-in process 2 hours;
(7) filter and pack
Material after allocating and wearing out is removed the impurity of bringing in the raw material after filtration, obtains highly purified finished product isothiazolinone, adopts plastic tank to pack, sell.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110467583A (en) * | 2019-09-24 | 2019-11-19 | 山东泰和水处理科技股份有限公司 | A kind of production method of 3- isothiazolinone stability aqueous solution |
| CN113698326A (en) * | 2021-08-06 | 2021-11-26 | 唐山金硕化工有限公司 | Method and device for pipeline type continuous production of thiopropionate series compounds |
| CN113773237A (en) * | 2021-08-06 | 2021-12-10 | 唐山金硕化工有限公司 | Preparation method of dialkyl dithiodipropionate |
| CN113979965A (en) * | 2021-10-27 | 2022-01-28 | 陕西中杰科仪化学科技有限公司 | Continuous production method of 4, 5-dichloro-2-octyl-4-isothiazoline-3-ketone |
| CN114853646A (en) * | 2022-06-17 | 2022-08-05 | 山东裕滨新材料有限公司 | Method for synthesizing dimethyl dithiodipropionate based on continuous vulcanization reaction |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1671674A (en) * | 2002-05-29 | 2005-09-21 | Sk化学株式会社 | Isothiazolone composition and method for stabilizing isothiazolone |
| CN101417966A (en) * | 2007-10-25 | 2009-04-29 | 北京天擎化工有限责任公司 | Continuous production method of 3-isothiazolone derivates |
-
2013
- 2013-07-08 CN CN2013102840273A patent/CN103319433A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1671674A (en) * | 2002-05-29 | 2005-09-21 | Sk化学株式会社 | Isothiazolone composition and method for stabilizing isothiazolone |
| CN101417966A (en) * | 2007-10-25 | 2009-04-29 | 北京天擎化工有限责任公司 | Continuous production method of 3-isothiazolone derivates |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110467583A (en) * | 2019-09-24 | 2019-11-19 | 山东泰和水处理科技股份有限公司 | A kind of production method of 3- isothiazolinone stability aqueous solution |
| CN110467583B (en) * | 2019-09-24 | 2023-04-11 | 山东泰和水处理科技股份有限公司 | Production method of 3-isothiazolinone stable aqueous solution |
| CN113698326A (en) * | 2021-08-06 | 2021-11-26 | 唐山金硕化工有限公司 | Method and device for pipeline type continuous production of thiopropionate series compounds |
| CN113773237A (en) * | 2021-08-06 | 2021-12-10 | 唐山金硕化工有限公司 | Preparation method of dialkyl dithiodipropionate |
| CN113698326B (en) * | 2021-08-06 | 2024-04-09 | 唐山金硕化工有限公司 | Method and device for continuously producing thiopropionate series compounds through pipeline |
| CN113979965A (en) * | 2021-10-27 | 2022-01-28 | 陕西中杰科仪化学科技有限公司 | Continuous production method of 4, 5-dichloro-2-octyl-4-isothiazoline-3-ketone |
| CN113979965B (en) * | 2021-10-27 | 2023-07-28 | 陕西中杰科仪化学科技有限公司 | Continuous production method of 4, 5-dichloro-2-octyl-4-isothiazolin-3-ketone |
| CN114853646A (en) * | 2022-06-17 | 2022-08-05 | 山东裕滨新材料有限公司 | Method for synthesizing dimethyl dithiodipropionate based on continuous vulcanization reaction |
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Application publication date: 20130925 |