CN104961685A - Method for reducing carbendazim impurity DAP in production process of carbendazim - Google Patents
Method for reducing carbendazim impurity DAP in production process of carbendazim Download PDFInfo
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- CN104961685A CN104961685A CN201510324761.7A CN201510324761A CN104961685A CN 104961685 A CN104961685 A CN 104961685A CN 201510324761 A CN201510324761 A CN 201510324761A CN 104961685 A CN104961685 A CN 104961685A
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- dap
- carbendazim
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- derosal
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D235/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings
- C07D235/02—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings condensed with carbocyclic rings or ring systems
- C07D235/04—Benzimidazoles; Hydrogenated benzimidazoles
- C07D235/24—Benzimidazoles; Hydrogenated benzimidazoles with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached in position 2
- C07D235/30—Nitrogen atoms not forming part of a nitro radical
- C07D235/32—Benzimidazole-2-carbamic acids, unsubstituted or substituted; Esters thereof; Thio-analogues thereof
Abstract
The invention provides a method for reducing a carbendazim impurity DAP in the production process of carbendazim. The method includes: synthesizing o-phenylenediamie; synthesizing cyanamide based methyl formate; synthesizing carbendazim, namely transferring o-phenylenediamie and cyanamide based methyl formate into a reaction kettle for complexation, dropwise adding hydrochloric acid during complexation, adding an additive into the reaction kettle after dropwise condensation adding of hydrochloric acid is finished, starting a reaction kettle stirring device for sufficient stirring, maintaining temperature, filtering, using water for washing, swabbing-off and drying. The additive is added after condensation is finished on the basis of controlling DAP content, the DAP content can reach level A+ after material drying, the DAP content reaches about 0.5ppm after testing and rectification, DAP does not rebound after overnight placement, production requirements can be met better, and content of the impurity in the carbendazim is lowered. Consequently, through testing, the DAP content of carbendazim raw materials is lowered to be about 0.2ppm, so that quality is improved, carbendazim content is improved from 95% to 96.3%, and DAP+HAP is smaller than or equal to 1.5mg/kg.
Description
Technical field
The present invention relates to derosal production field, be specifically related to a kind of method reducing derosal impurity DAP in derosal production process.
Background technology
2,3 diaminophenol piperazines (DAP) are an important impurity in derosal finished product, how many direct qualities affecting derosal of its foreign matter content; By adding complexing agent, the content of derosal impurity is reduced greatly.
Traditional DAP control method is mainly controlled by rectifying tower effect in early stage, but when rectification effect is bad in derosal product DAP comparision contents high, after rectifying, content is higher.
Summary of the invention
For above problems of the prior art, the invention provides a kind of method reducing derosal impurity DAP in derosal production process, reduce the content of impurity in product.
The present invention is achieved by the following technical solutions:
Reduce a method of derosal impurity DAP in derosal production process, described method comprises, and first carries out the synthesis of O-Phenylene Diamine, carrying out the synthesis of cyanamide base methyl-formiate, then the synthesis of derosal is carried out: O-Phenylene Diamine and cyanamide base methyl-formiate are transferred in reactor and carried out complex reaction, and drip hydrochloric acid while complex reaction, drip hydrochloric acid in condensation to terminate, now in reactor PH at 4.2-4.7, and it is more stable, the additive of 1.8-2.5kg is added again in reactor, open stirring apparatus for reaction kettle fully to stir, insulation, and temperature is 90-98 DEG C, soaking time is 30-60min, again the material in reactor is filtered, material after filtering is washed, again the material after washing is drained, finally the material after draining is dried, .
Further, described additive is paraformaldehyde, and paraformaldehyde is solid.
Wherein the synthesis of O-Phenylene Diamine is as follows
The synthesis of cyanamide base methyl-formiate is as follows
CaCN
2+H
2O→HCN
2+Ca(OH)
2
The synthesis of derosal is as follows
intermediate O-Phenylene Diamine and cyanamide base methyl-formiate are condensed into derosal in acid condition
Beneficial effect of the present invention is: have employed doping again after condensation completes on original control DAP content basis, after making drying materials, DAP content can reach A
+rank, after inspection rectifying, DAP content reaches about 0.5ppm, places DAP after spending the night and does not rebound, can better meet the requirement of production; Simultaneously, additive is added separately after condensation completes, carry out complexing by DAP and additive, DAP is deviate from from product, reduce the content of impurity in product, therefore, through inspection, the DAP content achieving derosal raw material can be reduced to about 0.2ppm, thus improves quality, therefore derosal content has brought up to about 96.3%, DAP+HAP≤1.5mg/kg from 95%.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiment 1
First carry out the synthesis of O-Phenylene Diamine, carrying out the synthesis of cyanamide base methyl-formiate, then the synthesis of derosal is carried out: O-Phenylene Diamine and cyanamide base methyl-formiate are transferred in reactor and carried out complex reaction, and drip hydrochloric acid while complex reaction, drip hydrochloric acid in condensation to terminate, now in reactor PH 4.2, and it is more stable, the additive paraformaldehyde of 2.5kg is added again in reactor, open stirring apparatus for reaction kettle fully to stir, insulation, and temperature is 98 DEG C, soaking time is 60min, again the material in reactor is filtered, material after filtering is washed, again the material after washing is drained, finally the material after draining is dried, , after rectifying, DAP content reaches about 0.5ppm, placement spend the night after DAP do not rebound, the requirement of production can be better met, namely after condensation completes, additive is added separately, complexing is carried out by DAP and additive, DAP is deviate from from product, reduce the content of impurity in product, therefore, through inspection, the DAP content achieving derosal raw material can be reduced to about 0.2ppm, thus improve quality, therefore derosal content has brought up to 96.2% from 95%, DAP+HAP≤1.5mg/kg.
Embodiment 2
First carry out the synthesis of O-Phenylene Diamine, carrying out the synthesis of cyanamide base methyl-formiate, then the synthesis of derosal is carried out: O-Phenylene Diamine and cyanamide base methyl-formiate are transferred in reactor and carried out complex reaction, and drip hydrochloric acid while complex reaction, drip hydrochloric acid in condensation to terminate, now in reactor PH 4.3, and it is more stable, the additive paraformaldehyde of 2.4kg is added again in reactor, open stirring apparatus for reaction kettle fully to stir, insulation, and temperature is 96 DEG C, soaking time is 40min, again the material in reactor is filtered, material after filtering is washed, again the material after washing is drained, finally the material after draining is dried, namely rectifiable rear DAP content reaches about 0.5ppm, placement spend the night after DAP do not rebound, the requirement of production can be better met, namely after condensation completes, additive is added separately, complexing is carried out by DAP and additive, DAP is deviate from from product, reduce the content of impurity in product, therefore, through inspection, the DAP content achieving derosal raw material can be reduced to about 0.2ppm, thus improve quality, therefore derosal content has brought up to 96.3% from 95%, DAP+HAP≤1.5mg/kg.
Embodiment 3
First carry out the synthesis of O-Phenylene Diamine, carrying out the synthesis of cyanamide base methyl-formiate, then the synthesis of derosal is carried out: O-Phenylene Diamine and cyanamide base methyl-formiate are transferred in reactor and carried out complex reaction, and drip hydrochloric acid while complex reaction, drip hydrochloric acid in condensation to terminate, now in reactor PH 4.4, and it is more stable, the additive paraformaldehyde of 2.3kg is added again in reactor, open stirring apparatus for reaction kettle fully to stir, insulation, and temperature is 95 DEG C, soaking time is 30min, again the material in reactor is filtered, material after filtering is washed, again the material after washing is drained, finally the material after draining is dried, , after rectifying, DAP content reaches about 0.5ppm, placement spend the night after DAP do not rebound, the requirement of production can be better met, namely after condensation completes, additive is added separately, complexing is carried out by DAP and additive, DAP is deviate from from product, reduce the content of impurity in product, therefore, through inspection, the DAP content achieving derosal raw material can be reduced to about 0.2ppm, thus improve quality, therefore derosal content has brought up to 96.5% from 95%, DAP+HAP≤1.5mg/kg.
Embodiment 4
First carry out the synthesis of O-Phenylene Diamine, carrying out the synthesis of cyanamide base methyl-formiate, then the synthesis of derosal is carried out: O-Phenylene Diamine and cyanamide base methyl-formiate are transferred in reactor and carried out complex reaction, and drip hydrochloric acid while complex reaction, drip hydrochloric acid in condensation to terminate, now in reactor PH 4.5, and it is more stable, the additive paraformaldehyde of 2.0kg is added again in reactor, open stirring apparatus for reaction kettle fully to stir, insulation, and temperature is 92 DEG C, soaking time is 45min, again the material in reactor is filtered, material after filtering is washed, again the material after washing is drained, finally the material after draining is dried, , after rectifying, DAP content reaches about 0.5ppm, placement spend the night after DAP do not rebound, the requirement of production can be better met, namely after condensation completes, additive is added separately, complexing is carried out by DAP and additive, DAP is deviate from from product, reduce the content of impurity in product, therefore, through inspection, the DAP content achieving derosal raw material can be reduced to about 0.2ppm, thus improve quality, therefore derosal content has brought up to 96.6% from 95%, DAP+HAP≤1.5mg/kg.
Embodiment 5
First carry out the synthesis of O-Phenylene Diamine, carrying out the synthesis of cyanamide base methyl-formiate, then the synthesis of derosal is carried out: O-Phenylene Diamine and cyanamide base methyl-formiate are transferred in reactor and carried out complex reaction, and drip hydrochloric acid while complex reaction, drip hydrochloric acid in condensation to terminate, now in reactor PH 4.6, and it is more stable, the additive paraformaldehyde of 1.9kg is added again in reactor, open stirring apparatus for reaction kettle fully to stir, insulation, and temperature is 91 DEG C, soaking time is 30min, again the material in reactor is filtered, material after filtering is washed, again the material after washing is drained, finally the material after draining is dried, , after rectifying, DAP content reaches about 0.5ppm, placement spend the night after DAP do not rebound, the requirement of production can be better met, namely after condensation completes, additive is added separately, complexing is carried out by DAP and additive, DAP is deviate from from product, reduce the content of impurity in product, therefore, through inspection, the DAP content achieving derosal raw material can be reduced to about 0.2ppm, thus improve quality, therefore derosal content has brought up to 96.1% from 95%, DAP+HAP≤1.5mg/kg.
Embodiment 6
First carry out the synthesis of O-Phenylene Diamine, carrying out the synthesis of cyanamide base methyl-formiate, then the synthesis of derosal is carried out: O-Phenylene Diamine and cyanamide base methyl-formiate are transferred in reactor and carried out complex reaction, and drip hydrochloric acid while complex reaction, drip hydrochloric acid in condensation to terminate, now in reactor PH 4.7, and it is more stable, the additive paraformaldehyde of 1.8kg is added again in reactor, open stirring apparatus for reaction kettle fully to stir, insulation, and temperature is 90 DEG C, soaking time is 30min, again the material in reactor is filtered, material after filtering is washed, again the material after washing is drained, finally the material after draining is dried, , after rectifying, DAP content reaches about 0.5ppm, placement spend the night after DAP do not rebound, the requirement of production can be better met, namely after condensation completes, additive is added separately, complexing is carried out by DAP and additive, DAP is deviate from from product, reduce the content of impurity in product, therefore, through inspection, the DAP content achieving derosal raw material can be reduced to about 0.2ppm, thus improve quality, therefore derosal content has brought up to 96.45% from 95%, DAP+HAP≤1.5mg/kg.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. reduce a method of derosal impurity DAP in derosal production process, described method comprises, and first carries out the synthesis of O-Phenylene Diamine, carrying out the synthesis of cyanamide base methyl-formiate, then the synthesis of derosal is carried out: O-Phenylene Diamine and cyanamide base methyl-formiate are transferred in reactor and carried out complex reaction, and drip hydrochloric acid while complex reaction, it is characterized in that: drip hydrochloric acid in condensation and terminate, now in reactor PH at 4.2-4.7, and it is more stable, the additive of 1.8-2.5kg is added again in reactor, open stirring apparatus for reaction kettle fully to stir, insulation, and temperature is 90-98 DEG C, soaking time is 30-60min, again the material in reactor is filtered, material after filtering is washed, again the material after washing is drained, finally the material after draining is dried, .
2. reduce the method for derosal impurity DAP in a kind of derosal production process according to claim 1, it is characterized in that: described additive is paraformaldehyde, and paraformaldehyde is solid.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106316961A (en) * | 2016-08-13 | 2017-01-11 | 安徽东至广信农化有限公司 | Processing device for reducing DAP impurities through carbendazim production |
| CN107188854A (en) * | 2017-07-12 | 2017-09-22 | 安徽广信农化股份有限公司 | A kind of synthesis technique for improving carbendazim quality |
| CN107778253A (en) * | 2017-11-08 | 2018-03-09 | 安徽东至广信农化有限公司 | A kind of technique of hydrogen chloride synthesis carbendazim |
| CN108558772A (en) * | 2018-06-14 | 2018-09-21 | 安徽广信农化股份有限公司 | A kind of manufacturing technique method improving carbendazim quality |
| CN109053586A (en) * | 2018-09-11 | 2018-12-21 | 安徽东至广信农化有限公司 | A kind of production method of carbendazim |
| CN113698354A (en) * | 2021-08-06 | 2021-11-26 | 安徽东至广信农化有限公司 | Method for reducing carbendazim impurity DAP |
| CN114014813A (en) * | 2021-11-08 | 2022-02-08 | 安徽东至广信农化有限公司 | Production process for synthesizing carbendazim by hydrogen chloride method |
| CN114539160A (en) * | 2022-02-10 | 2022-05-27 | 安徽东至广信农化有限公司 | Production process for synthesizing carbendazim by acidic photocatalysis method |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106316961A (en) * | 2016-08-13 | 2017-01-11 | 安徽东至广信农化有限公司 | Processing device for reducing DAP impurities through carbendazim production |
| CN107188854A (en) * | 2017-07-12 | 2017-09-22 | 安徽广信农化股份有限公司 | A kind of synthesis technique for improving carbendazim quality |
| CN107778253A (en) * | 2017-11-08 | 2018-03-09 | 安徽东至广信农化有限公司 | A kind of technique of hydrogen chloride synthesis carbendazim |
| CN108558772A (en) * | 2018-06-14 | 2018-09-21 | 安徽广信农化股份有限公司 | A kind of manufacturing technique method improving carbendazim quality |
| CN109053586A (en) * | 2018-09-11 | 2018-12-21 | 安徽东至广信农化有限公司 | A kind of production method of carbendazim |
| CN109053586B (en) * | 2018-09-11 | 2022-01-07 | 安徽东至广信农化有限公司 | Production method of carbendazim |
| CN113698354A (en) * | 2021-08-06 | 2021-11-26 | 安徽东至广信农化有限公司 | Method for reducing carbendazim impurity DAP |
| CN114014813A (en) * | 2021-11-08 | 2022-02-08 | 安徽东至广信农化有限公司 | Production process for synthesizing carbendazim by hydrogen chloride method |
| CN114539160A (en) * | 2022-02-10 | 2022-05-27 | 安徽东至广信农化有限公司 | Production process for synthesizing carbendazim by acidic photocatalysis method |
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Application publication date: 20151007 |