CN109265372A - The synthetic method of diuron - Google Patents
The synthetic method of diuron Download PDFInfo
- Publication number
- CN109265372A CN109265372A CN201811325502.6A CN201811325502A CN109265372A CN 109265372 A CN109265372 A CN 109265372A CN 201811325502 A CN201811325502 A CN 201811325502A CN 109265372 A CN109265372 A CN 109265372A
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- CN
- China
- Prior art keywords
- diuron
- thermal synthesis
- synthesis kettle
- synthetic method
- kettle
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
- C07C273/18—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of substituted ureas
- C07C273/1809—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of substituted ureas with formation of the N-C(O)-N moiety
- C07C273/1818—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of substituted ureas with formation of the N-C(O)-N moiety from -N=C=O and XNR'R"
- C07C273/1827—X being H
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of synthetic methods of diuron, are included in cold synthesis reactor and 3,4- dichlorophenyl isocyanate is added；Toluene is added into 3,4- dichlorophenyl isocyanate in the agitating device for starting cold synthesis reactor；Mixing liquid is transferred in the thermal synthesis kettle for being warming up to 65 degrees Celsius ~ 75 degrees Celsius；Start the agitating device of thermal synthesis kettle, and is passed through dimethylamine gas to thermal synthesis kettle；Continue stirring a period of time after ventilation, obtains diuron.The present invention has abandoned traditional water hair addition, but is passed directly into dimethylamine gas, effectively prevents 3,4- dichlorophenyl isocyanate and decomposes in water phase, convenient for improving the yield of product, while can also improve the purity of product.
Description
Technical field
The present invention relates to a kind of synthetic methods of diuron, belong to pesticide processing field.
Background technique
Diuron is colorless crystalline solid, 158~159 DEG C of fusing point, is soluble in hot alcohol, solubility in acetone at 27 DEG C
It is 5.3%, is slightly dissolved in ethyl acetate, ethyl alcohol and hot benzene, not soluble in water, 42 ppm when solubility in water is 25 DEG C, in hydro carbons
Middle solubility is low, to oxidation and hydrolysis-stable.Diuron is a kind of good herbicide, and traditional diuron sends out addition using water
Dimethylamine agueous solution, i.e., be added in the organic solution of 3,4- dichlorophenyl isocyanate and reacted by preparation, 3,4- dichloro-benzenes
Based isocyanate easily decomposes in water phase, influences the yield of preparation.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of synthetic methods of diuron.
In order to achieve the above object, the technical scheme adopted by the invention is that:
The synthetic method of diuron, includes the following steps,
3,4- dichlorophenyl isocyanate is added in cold synthesis reactor；
Toluene is added into 3,4- dichlorophenyl isocyanate in the agitating device for starting cold synthesis reactor；
Mixing liquid is transferred in the thermal synthesis kettle for being warming up to 65 degrees Celsius ~ 75 degrees Celsius；
Start the agitating device of thermal synthesis kettle, and is passed through dimethylamine gas to thermal synthesis kettle；
Continue stirring a period of time after ventilation, obtains diuron.
Mixed liquor standing in cold synthesis reactor is transferred to thermal synthesis kettle after ten minutes.
The temperature of thermal synthesis kettle is 70 degrees Celsius.
Continue to stir half an hour after ventilating in thermal synthesis kettle.
Obtained diuron also needs that finished product to the end could be obtained after centrifuge washing, drying.
In thermal synthesis kettle, the pipeline of logical dimethylamine gas protrudes into thermal synthesis kettle intracavity bottom.
Advantageous effects of the invention: the present invention has abandoned traditional water hair addition, but it is passed directly into dimethylamine
Gas effectively prevents 3,4- dichlorophenyl isocyanate and decomposes in water phase, convenient for improving the yield of product, while can also mention
The purity of high product.
Specific embodiment
The following examples are only intended to illustrate the technical solution of the present invention more clearly, and cannot be used as a limitation the limitation present invention
Protection scope.
The synthetic method of diuron, comprising the following steps:
Step 1,3,4- dichlorophenyl isocyanate is added in cold synthesis reactor.
Step 2, toluene is added into 3,4- dichlorophenyl isocyanate in the agitating device for starting cold synthesis reactor.
Step 3, mixed liquor is stood after ten minutes, is transferred in the thermal synthesis kettle for being warming up to 65 degrees Celsius ~ 75 degrees Celsius, heat
The Optimal Temperature of synthesis reactor is 70 degrees Celsius.
Step 4, start the agitating device of thermal synthesis kettle, and be passed through dimethylamine gas to thermal synthesis kettle；In thermal synthesis kettle, lead to
The pipeline of dimethylamine gas protrudes into thermal synthesis kettle intracavity bottom.
Step 5, continue to stir half an hour after ventilation, obtain diuron.
Step 6, the diuron obtained also needs that finished product to the end could be obtained after centrifuge washing, drying.
The present invention has abandoned traditional water hair addition, but is passed directly into dimethylamine gas, effectively prevents 3,4- dichloro
Phenyl isocyanate is decomposed in water phase, convenient for improving the yield of product, while can also improve the purity of product.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvement and deformations can also be made, these improvement and deformations
Also it should be regarded as protection scope of the present invention.
Claims (6)
1. the synthetic method of diuron, it is characterised in that: include the following steps,
3,4- dichlorophenyl isocyanate is added in cold synthesis reactor；
Toluene is added into 3,4- dichlorophenyl isocyanate in the agitating device for starting cold synthesis reactor；
Mixing liquid is transferred in the thermal synthesis kettle for being warming up to 65 degrees Celsius ~ 75 degrees Celsius；
Start the agitating device of thermal synthesis kettle, and is passed through dimethylamine gas to thermal synthesis kettle；
Continue stirring a period of time after ventilation, obtains diuron.
2. the synthetic method of diuron according to claim 1, it is characterised in that: the mixed liquor in cold synthesis reactor stands 10
Thermal synthesis kettle is transferred to after minute.
3. the synthetic method of diuron according to claim 1, it is characterised in that: the temperature of thermal synthesis kettle is 70 Celsius
Degree.
4. the synthetic method of diuron according to claim 1, it is characterised in that: continue after ventilating in thermal synthesis kettle
Stir half an hour.
5. the synthetic method of diuron according to claim 1, it is characterised in that: obtained diuron is also needed by centrifugation
Finished product to the end could be obtained after washing, drying.
6. the synthetic method of diuron according to claim 1, it is characterised in that: in thermal synthesis kettle, lead to dimethylamine gas
Pipeline protrude into thermal synthesis kettle intracavity bottom.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811325502.6A CN109265372A (en) | 2018-11-08 | 2018-11-08 | The synthetic method of diuron |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811325502.6A CN109265372A (en) | 2018-11-08 | 2018-11-08 | The synthetic method of diuron |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109265372A true CN109265372A (en) | 2019-01-25 |
Family
ID=65192585
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811325502.6A Pending CN109265372A (en) | 2018-11-08 | 2018-11-08 | The synthetic method of diuron |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109265372A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101709041A (en) * | 2009-11-13 | 2010-05-19 | 安徽广信集团铜陵化工有限公司 | Process for producing diuron |
| CN103539704A (en) * | 2013-11-08 | 2014-01-29 | 江苏安邦电化有限公司 | Method for preparing diuron |
| CN104496855A (en) * | 2015-01-05 | 2015-04-08 | 山东润博生物科技有限公司 | Method for preparing diuron |
| CN105017088A (en) * | 2015-06-29 | 2015-11-04 | 安徽广信农化股份有限公司 | Production process of diuron |
| CN105294504A (en) * | 2015-10-20 | 2016-02-03 | 安徽广信农化股份有限公司 | Method for synthesizing diuron |
-
2018
- 2018-11-08 CN CN201811325502.6A patent/CN109265372A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101709041A (en) * | 2009-11-13 | 2010-05-19 | 安徽广信集团铜陵化工有限公司 | Process for producing diuron |
| CN103539704A (en) * | 2013-11-08 | 2014-01-29 | 江苏安邦电化有限公司 | Method for preparing diuron |
| CN104496855A (en) * | 2015-01-05 | 2015-04-08 | 山东润博生物科技有限公司 | Method for preparing diuron |
| CN105017088A (en) * | 2015-06-29 | 2015-11-04 | 安徽广信农化股份有限公司 | Production process of diuron |
| CN105294504A (en) * | 2015-10-20 | 2016-02-03 | 安徽广信农化股份有限公司 | Method for synthesizing diuron |
Non-Patent Citations (2)
| Title |
|---|
| "敌草隆合成新工艺通过鉴定 ", 《山东农药信息》 * |
| 于春红等: "敌草隆的合成方法改进 ", 《现代农药》 * |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190125 |
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| RJ01 | Rejection of invention patent application after publication |