CN107188831A - A kind of carbendazim intermediate cyanamide base methyl formate synthesis technique - Google Patents
A kind of carbendazim intermediate cyanamide base methyl formate synthesis technique Download PDFInfo
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- CN107188831A CN107188831A CN201710566927.5A CN201710566927A CN107188831A CN 107188831 A CN107188831 A CN 107188831A CN 201710566927 A CN201710566927 A CN 201710566927A CN 107188831 A CN107188831 A CN 107188831A
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- Prior art keywords
- lime
- methyl formate
- base methyl
- synthesis technique
- carbendazim
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C269/00—Preparation of derivatives of carbamic acid, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups
- C07C269/06—Preparation of derivatives of carbamic acid, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups by reactions not involving the formation of carbamate groups
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Removal Of Specific Substances (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The present invention relates to a kind of carbendazim intermediate cyanamide base methyl formate synthesis technique, following step is specifically included：1) after quick lime and ammoniacal liquor being put into hydrolysis kettle by a certain percentage, the temperature 1h in rise hydrolysis kettle；2) lime ammonia water mixture is carried out filtering to obtain filtered fluid, then the filtered fluid is put into synthesis reactor, lime nitrogen is added, albendazole insulation 1h is then added dropwise；3) cyanamide base methyl formate of the generation with accessory substance calcium salt after pH adjusting agent regulation pH is added dropwise；4) the light room of electric dialyzator will be introduced after the lime ammoniacal liquor solution esterifying liquid cooling after acidifying, ethanol is introduced to the dense room of electric dialyzator, opens and adjusts dc source so that electric dialyzator work obtains final products；Phosgene is replaced with lime ammoniacal liquor in the cyanamide base methyl formate synthesis technique of the present invention, the pollution to environment and the injury to human body is not only reduced, and the purity of product is improved to more than 99%.
Description
Technical field
The present invention relates to carbendazim synthesis technique field, especially a kind of carbendazim intermediate cyanamide base methyl formate synthesis work
Skill.
Background technology
Cyanamide base methyl formate is colourless or has a little light blue aqueous solution, in alkalescent, there is stink, is also many bacterium of synthesis
The important intermediate of spirit, it is existing in the technique of synthesis cyanamide base methyl formate, often utilize relatedization such as phosgene and methanol
Material is learned to be synthesized, but phosgene has high toxicity, environment can be polluted, human body is damaged.
The content of the invention
The problem of purpose of the present invention exists aiming at above-mentioned prior art is simple there is provided a kind of technique, environmental protection and production
Product have the carbendazim intermediate cyanamide base methyl formate synthesis technique of high-purity.
The technical solution adopted in the present invention is：A kind of carbendazim intermediate cyanamide base methyl formate synthesis technique, it is described
Synthesis technique comprises the steps：
1) by quick lime：Ammoniacal liquor presses 0.5-0.9:After in 1.1-1.5 ratio input hydrolysis kettle, raise in the hydrolysis kettle
Temperature to 30-50 DEG C insulation 1h after lime ammonia water mixture, it is standby；
2) obtained lime ammonia water mixture is carried out filtering to obtain filtered fluid, the filtered fluid is then put into synthesis reactor
In, the lime nitrogen of addition 0.7-1.2 parts by weight is then added dropwise albendazole after pH is equal to 7, lime ammonia is obtained after insulation 1h
Esterifying liquid is hydrolyzed, it is standby；
3) obtained lime ammoniacal liquor solution esterifying liquid is added after pH adjusting agent, regulation pH to 1-4, generation carries accessory substance calcium
The cyanamide base methyl formate of salt；
4) the lime ammoniacal liquor solution esterifying liquid after acidifying is cooled to the light room that electric dialyzator is introduced after 5-15 DEG C, ethanol is drawn
Enter the dense room of electric dialyzator, circulated respectively in electric dialyzator, open and adjust dc source so that electric dialyzator works；
5) after calcium ion content is down to 500-1500ppm in light room esterifying liquid, final cyanamide base methyl formate is obtained.
Further, first submersible agitator stirring reaction liquid is used before insulation in the step 2 until reaction solution is without heavy
Starch.
Further, the pH adjusting agent is the supernatant after the film process of industrial wastewater synthetic resin, the industry
The pH value of waste water is 2-5.
Further, the temperature of the industrial wastewater is 10 DEG C -50 DEG C, and COD content is below 16000mg/L,
Suspension content is below 350mg/L.
Further, in the step 1 quick lime and the ratio of ammoniacal liquor is 0.62:1.34.
Further, the temperature in hydrolysis kettle is raised in the step 1 to 45 DEG C.
Further, the lime nitrogen in the step 2 is 0.96 parts by weight.
The beneficial effect for the carbendazim intermediate cyanamide base methyl formate synthesis technique that the present invention is provided is：The cyanogen of the present invention
Phosgene is replaced with lime ammoniacal liquor in amidocarbonic acid methyl esters synthesis technique, the pollution to environment and the wound to human body is not only reduced
Evil, and the purity of product is improved to more than 99%.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Embodiment 1
A kind of carbendazim intermediate cyanamide base methyl formate synthesis technique, is by quick lime：Ammoniacal liquor presses 0.62:1.34 ratio
After in example input hydrolysis kettle, raise the temperature in the hydrolysis kettle to 45 DEG C, then with submersible agitator stirring reaction liquid until
1h is incubated after reaction solution deposit-free, lime ammonia water mixture is obtained, it is standby；Then obtained lime ammonia water mixture was carried out
Filtered fluid is filtered to obtain, then puts into the filtered fluid in synthesis reactor, the lime nitrogen of 0.96 parts by weight is added, ammonia formic acid is then added dropwise
Methyl esters obtains lime ammoniacal liquor solution esterifying liquid after pH is equal to 7 after insulation 1h, standby；Then obtained lime ammoniacal liquor solution is esterified
Liquid is added after pH adjusting agent, regulation pH to 2, cyanamide base methyl formate of the generation with accessory substance calcium salt；Then by after acidifying
Lime ammoniacal liquor solution esterifying liquid is cooled to the light room that electric dialyzator is introduced after 11 DEG C, ethanol is introduced to the dense room of electric dialyzator, respectively
Circulated in electric dialyzator, open and adjust dc source so that electric dialyzator works；Finally when calcium ion in light room esterifying liquid
Content is down to after 1000ppm, obtains final cyanamide base methyl formate.
The pH adjusting agent is the supernatant after the film process of industrial wastewater synthetic resin, the pH value of the industrial wastewater
For 3, and the temperature of the industrial wastewater is 30 DEG C, and COD content is below 16000mg/L, and suspension content is
Below 350mg/L.
Phosgene is replaced with lime ammoniacal liquor in the cyanamide base methyl formate synthesis technique of the present invention, is not only reduced to environment
Pollution and the injury to human body, and the purity of product is improved to more than 99%.
Embodiment 2
A kind of carbendazim intermediate cyanamide base methyl formate synthesis technique, is by quick lime：Ammoniacal liquor presses 0.5:1.1 ratio
After putting into hydrolysis kettle, the temperature in the hydrolysis kettle is raised to 30 DEG C, then with submersible agitator stirring reaction liquid until anti-
1h is incubated after answering liquid deposit-free, lime ammonia water mixture is obtained, it is standby；Then obtained lime ammonia water mixture is filtered
Filtered fluid is obtained, then puts into the filtered fluid in synthesis reactor, the lime nitrogen of 0.7 parts by weight is added, ammonia formic acid first is then added dropwise
Ester obtains lime ammoniacal liquor solution esterifying liquid after pH is equal to 7 after insulation 1h, standby；Then by obtained lime ammoniacal liquor solution esterifying liquid
Add after pH adjusting agent, regulation pH to 1, cyanamide base methyl formate of the generation with accessory substance calcium salt；Then by the stone after acidifying
Grey ammoniacal liquor solution esterifying liquid is cooled to the light room that electric dialyzator is introduced after 5 DEG C, ethanol is introduced to the dense room of electric dialyzator, respectively in electricity
Circulated in dialyzer, open and adjust dc source so that electric dialyzator works；Finally when calcium ion content in light room esterifying liquid
It is down to after 500ppm, obtains final cyanamide base methyl formate.
The pH adjusting agent is the supernatant after the film process of industrial wastewater synthetic resin, the pH value of the industrial wastewater
For 2, and the temperature of the industrial wastewater is 10 DEG C, and COD content is below 16000mg/L, and suspension content is
Below 350mg/L.
Phosgene is replaced with lime ammoniacal liquor in the cyanamide base methyl formate synthesis technique of the present invention, is not only reduced to environment
Pollution and the injury to human body, and the purity of product is improved to more than 99%.
Embodiment 3
A kind of carbendazim intermediate cyanamide base methyl formate synthesis technique, is by quick lime：Ammoniacal liquor presses 0.9:1.5 ratio
After putting into hydrolysis kettle, the temperature in the hydrolysis kettle is raised to 50 DEG C, then with submersible agitator stirring reaction liquid until anti-
1h is incubated after answering liquid deposit-free, lime ammonia water mixture is obtained, it is standby；Then obtained lime ammonia water mixture is filtered
Filtered fluid is obtained, then puts into the filtered fluid in synthesis reactor, the lime nitrogen of 1.2 parts by weight is added, ammonia formic acid first is then added dropwise
Ester obtains lime ammoniacal liquor solution esterifying liquid after pH is equal to 7 after insulation 1h, standby；Then by obtained lime ammoniacal liquor solution esterifying liquid
Add after pH adjusting agent, regulation pH to 4, cyanamide base methyl formate of the generation with accessory substance calcium salt；Then by the stone after acidifying
Grey ammoniacal liquor solution esterifying liquid is cooled to the light room that electric dialyzator is introduced after 15 DEG C, and ethanol is introduced to the dense room of electric dialyzator, existed respectively
Circulated in electric dialyzator, open and adjust dc source so that electric dialyzator works；Finally when in light room esterifying liquid calcium ion contain
Amount is down to after 1500ppm, obtains final cyanamide base methyl formate.
The pH adjusting agent is the supernatant after the film process of industrial wastewater synthetic resin, the pH value of the industrial wastewater
For 5, and the temperature of the industrial wastewater is 50 DEG C, and COD content is below 16000mg/L, and suspension content is
Below 350mg/L.
Phosgene is replaced with lime ammoniacal liquor in the cyanamide base methyl formate synthesis technique of the present invention, is not only reduced to environment
Pollution and the injury to human body, and the purity of product is improved to more than 99%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modifications, equivalent substitutions and improvements made within refreshing and principle etc., should be included in the scope of the protection.
Claims (7)
1. a kind of carbendazim intermediate cyanamide base methyl formate synthesis technique, it is characterised in that the synthesis technique includes following
Step：
1) by quick lime：Ammoniacal liquor presses 0.5-0.9:After in 1.1-1.5 ratio input hydrolysis kettle, the temperature in the hydrolysis kettle is raised
Degree is incubated after 1h to 30-50 DEG C and obtains lime ammonia water mixture, standby；
2) obtained lime ammonia water mixture is carried out filtering to obtain filtered fluid, then put into the filtered fluid in synthesis reactor, plus
Enter the lime nitrogen of 0.7-1.2 parts by weight, albendazole is then added dropwise after pH is equal to 7, lime ammoniacal liquor solution is obtained after insulation 1h
Esterifying liquid, it is standby；
3) obtained lime ammoniacal liquor solution esterifying liquid is added after pH adjusting agent, regulation pH to 1-4, generation carries accessory substance calcium salt
Cyanamide base methyl formate；
4) the lime ammoniacal liquor solution esterifying liquid after acidifying is cooled to the light room that electric dialyzator is introduced after 5-15 DEG C, ethanol is introduced into electricity
The dense room of dialyzer, circulates in electric dialyzator, opens and adjust dc source respectively so that electric dialyzator works；
5) after calcium ion content is down to 500-1500ppm in light room esterifying liquid, final cyanamide base methyl formate is obtained.
2. carbendazim intermediate cyanamide base methyl formate synthesis technique according to claim 1, it is characterised in that the step
First with submersible agitator stirring reaction liquid until reaction solution deposit-free before insulation in rapid 2.
3. carbendazim intermediate cyanamide base methyl formate synthesis technique according to claim 1, it is characterised in that the pH
Conditioning agent is the supernatant after the film process of industrial wastewater synthetic resin, and the pH value of the industrial wastewater is 2-5.
4. carbendazim intermediate cyanamide base methyl formate synthesis technique according to claim 3, it is characterised in that the work
The temperature of industry waste water be 10 DEG C -50 DEG C, COD content be below 16000mg/L, suspension content be 350mg/L with
Under.
5. carbendazim intermediate cyanamide base methyl formate synthesis technique according to claim 1, it is characterised in that the step
The ratio of quick lime and ammoniacal liquor in rapid 1 is 0.62:1.34.
6. carbendazim intermediate cyanamide base methyl formate synthesis technique according to claim 1, it is characterised in that the step
The temperature in hydrolysis kettle is raised in rapid 1 to 45 DEG C.
7. carbendazim intermediate cyanamide base methyl formate synthesis technique according to claim 1, it is characterised in that the step
The parts by weight that lime nitrogen in rapid 2 is 0.96.
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| CN201710566927.5A CN107188831A (en) | 2017-07-12 | 2017-07-12 | A kind of carbendazim intermediate cyanamide base methyl formate synthesis technique |
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| CN201710566927.5A CN107188831A (en) | 2017-07-12 | 2017-07-12 | A kind of carbendazim intermediate cyanamide base methyl formate synthesis technique |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111718283A (en) * | 2020-07-28 | 2020-09-29 | 安徽东至广信农化有限公司 | Production method of medicine intermediate methyl cyanamide formate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3897448A (en) * | 1972-11-30 | 1975-07-29 | Rhone Progil | Process for the manufacture of alkyl benzimidazolylcarbamates |
| CN106565609A (en) * | 2016-09-28 | 2017-04-19 | 江苏扬农化工集团有限公司 | Preparation method of carbendazim |
-
2017
- 2017-07-12 CN CN201710566927.5A patent/CN107188831A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3897448A (en) * | 1972-11-30 | 1975-07-29 | Rhone Progil | Process for the manufacture of alkyl benzimidazolylcarbamates |
| CN106565609A (en) * | 2016-09-28 | 2017-04-19 | 江苏扬农化工集团有限公司 | Preparation method of carbendazim |
Non-Patent Citations (1)
| Title |
|---|
| 庄海燕: "多菌灵的合成研究", 《中国优秀博硕士学位论文全文数据库（硕士）工程科技I辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111718283A (en) * | 2020-07-28 | 2020-09-29 | 安徽东至广信农化有限公司 | Production method of medicine intermediate methyl cyanamide formate |
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Application publication date: 20170922 |
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