CN105254536A - Diuron esterification synthesis process - Google Patents
Diuron esterification synthesis process Download PDFInfo
- Publication number
- CN105254536A CN105254536A CN201510692499.1A CN201510692499A CN105254536A CN 105254536 A CN105254536 A CN 105254536A CN 201510692499 A CN201510692499 A CN 201510692499A CN 105254536 A CN105254536 A CN 105254536A
- Authority
- CN
- China
- Prior art keywords
- aniline
- toluene
- phosgene
- still
- toluene solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- NWXBVNPCVMVNRI-OOOIMJHGSA-N CC(C(/C=C/N[C@@H](N(C)C)O)Cl)C=C Chemical compound CC(C(/C=C/N[C@@H](N(C)C)O)Cl)C=C NWXBVNPCVMVNRI-OOOIMJHGSA-N 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a diuron esterification synthesis process which comprises the following steps: a toluene solution is fed into a dissolving dehydration kettle, liquid aniline is fed into a metering tank from an aniline storage tank, aniline is added and dissolved into toluene, and the mixture is fed into an aniline toluene storage tank to obtain a 3,4-dichloroaniline toluene solution; the toluene is fed into a cold light kettle for absorbing phosgene, after the aniline is analyzed to be up to standard, the 3,4-dichloroaniline toluene solution is dropwisely added while light is fed; light is continuously fed into the cold light kettle for reaction, phosgene is continuously fed, and stirring is stopped; under the condition that the negative pressure is kept for the material subjected to the light feeding reaction, the material is transferred to a hot light kettle, the hot light kettle is heated slowly, and the mixture is sampled and clarified to be transparent; the material is transferred to a solvent removal kettle, a phosgene toluene solution in the material is removed, meanwhile nitrogen is fed for exhausting, sampling analysis is performed, and a qualified product is transferred to an iso ester raw material tank, so that diuron is obtained. With the adoption of the production process, the process is simple and easy to operate, and the reaction condition is easy to control.
Description
Technical field
The present invention relates to plastics fine chemistry industry production field, be specifically related to a kind of lactate synthesis technique of Diuron Tech.
Background technology
Diuron Tech is colorless crystalline solid, and fusing point 158 ~ 159 DEG C, is soluble in hot alcohol, and when 27 DEG C, solubleness is 5.3% in acetone, is slightly dissolved in vinyl acetic monomer, ethanol and hot benzene.Water insoluble, the 42ppm when solubleness in water is 25 DEG C.In hydro carbons, solubleness is low.To oxidation and hydrolysis-stable.Another name N-(3,4-dichlorophenyl)-N', N'-dimethyl urea N'-(3,4-dichlorophenyl)-N, N-dimethyl urea; 3-(3,4-dichlorophenyl)-1,1-dimethyl urea; For preventing and kill off the general weeds in noncrop area, anti-weeds spread again.These product are also for the weeding of asparagus, citrus, cotton, pineapple, sugarcane, temperate zone trees and shrub fruit, and its structural formula is:
Diuron Tech is produced due to esterification technique stage more complicated, and reaction conditions is difficult to control, and therefore side reaction is more, and esterification finished product purity is not high.
Summary of the invention
For above problems of the prior art, the invention provides a kind of lactate synthesis technique of Diuron Tech, the time of esterification can be shortened, improve the purity of esterification product.
The present invention is achieved by the following technical solutions:
A lactate synthesis technique for Diuron Tech, its step is as follows:
1) first the toluene solution measured is squeezed in dissolving dehydrating kettle, again the aniline of liquid state is squeezed into scale tank from aniline storage tank, quantitative aniline is put into afterwards according to Weighing module, and aniline is dissolved in toluene by stirring, squeeze in aniline toluene tank that to obtain 3,4-DCA toluene solution stand-by;
2) quantitative toluene is squeezed in cold light still absorb a certain amount of phosgene, after up to standard by analysis, while lead to the 3,4-DCA toluene solution that plain edge drips metering in step 1, and keep pressure in cold light still all the time under negative pressure, temperature 70-75 DEG C;
3) logical photoresponse will be continued in the cold light still in step 2, and the time of continuing logical phosgene is 1.5-2h, stops stirring;
4) material of the logical photoresponse of step 3 is being kept, under negative pressure, proceeding to thermo-optical still, and thermo-optical still being slowly warming up to 80-90 DEG C, rear sampling clear;
5) material in step 4 is transferred in desolventizing still, and deviates from the phosgene toluene liquid in material, catching up with gas with passing into nitrogen, catching up with gas, catching up with the gas time to be 1-1.5h, and sampling analysis, qualified product proceed to different ester raw material tank.
Further, its step is as follows:
1) first the toluene solution measured is squeezed in dissolving dehydrating kettle, again the aniline of liquid state is squeezed into scale tank from aniline storage tank, quantitative aniline is put into afterwards according to Weighing module, and aniline is dissolved in toluene by stirring, squeeze in aniline toluene tank that to obtain 3,4-DCA toluene solution stand-by;
2) quantitative toluene is squeezed in cold light still absorb a certain amount of phosgene, after up to standard by analysis, while lead to the 3,4-DCA toluene solution that plain edge drips metering in step 1, and keep pressure in cold light still all the time under negative pressure, temperature 70 C;
3) logical photoresponse will be continued in the cold light still in step 2, and the time of continuing logical phosgene is 1.5h, stops stirring;
4) material of the logical photoresponse of step 3 is being kept, under negative pressure, proceeding to thermo-optical still, and thermo-optical still being slowly warming up to 80 DEG C, rear sampling clear;
5) material in step 4 is transferred in desolventizing still, and deviates from the phosgene toluene liquid in material, catching up with gas with passing into nitrogen, catching up with gas, catching up with the gas time to be 1h, and sampling analysis, qualified product proceed to different ester raw material tank.
Beneficial effect of the present invention is: the present invention adopts above-mentioned production technique, can by simple for Diuron Tech esterification technique easy handling, and reaction conditions also easily controls, and therefore by product is less, and esterification finished product purity is higher, improves the efficiency of later stage synthesis Diuron Tech.
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 the toluene solution measured is squeezed into and dissolve in dehydrating kettle, again the aniline of liquid state is squeezed into scale tank from aniline storage tank, quantitative aniline is put into afterwards according to Weighing module, and aniline is dissolved in toluene by stirring, squeeze in aniline toluene tank and obtain 3,4-dichlorphenamide bulk powder toluene solution is stand-by, can obtain the 3,4-DCA toluene solution of higher degree;
Again quantitative toluene is squeezed in cold light still and absorb a certain amount of phosgene, after up to standard by analysis, while lead to 3 of the aforementioned middle metering of plain edge dropping, 4-dichlorphenamide bulk powder toluene solution, and the pressure in maintenance cold light still is all the time under negative pressure, temperature 70 C, and the by product of reaction is less, improves the efficiency of reaction;
To continue logical photoresponse in aforesaid cold light still again, and the time of continuing logical phosgene is 1.5h, stops stirring, can reduce the generation of by product, make reactant reaction more complete;
Again by the material of aforesaid logical photoresponse under maintenance negative pressure, proceed to thermo-optical still, and thermo-optical still be slowly warming up to 80 DEG C, rear sampling clear, be easy to control the condition of reactant;
Finally the material in aforementioned is transferred in desolventizing still, and the phosgene toluene liquid deviate from material, catching up with gas with passing into nitrogen, catching up with gas, the gas time is caught up with to be 1h, and sampling analysis, qualified product proceed to different ester raw material tank, therefore integrated artistic list easy handling, reaction conditions also easily controls, therefore by product is less, and esterification finished product purity is higher, improves the efficiency of later stage synthesis Diuron Tech.
Therefore above-mentioned production technique is adopted, can by simple for Diuron Tech esterification technique easy handling, reaction conditions also easily controls, and therefore by product is less, and esterification finished product purity is higher, improves the efficiency of later stage synthesis Diuron Tech.
Embodiment 2
First the toluene solution measured is squeezed into and dissolve in dehydrating kettle, again the aniline of liquid state is squeezed into scale tank from aniline storage tank, quantitative aniline is put into afterwards according to Weighing module, and aniline is dissolved in toluene by stirring, squeeze in aniline toluene tank and obtain 3,4-dichlorphenamide bulk powder toluene solution is stand-by, can obtain the 3,4-DCA toluene solution of higher degree;
Again quantitative toluene is squeezed in cold light still and absorb a certain amount of phosgene, after up to standard by analysis, while lead to 3 of the aforementioned middle metering of plain edge dropping, 4-dichlorphenamide bulk powder toluene solution, and the pressure in maintenance cold light still is all the time under negative pressure, temperature 71 DEG C, and the by product of reaction is less, improves the efficiency of reaction;
To continue logical photoresponse in aforesaid cold light still again, and the time of continuing logical phosgene is 2h, stops stirring, can reduce the generation of by product, make reactant reaction more complete;
Again by the material of aforesaid logical photoresponse under maintenance negative pressure, proceed to thermo-optical still, and thermo-optical still be slowly warming up to 83 DEG C, rear sampling clear, be easy to control the condition of reactant;
Finally the material in aforementioned is transferred in desolventizing still, and the phosgene toluene liquid deviate from material, catching up with gas with passing into nitrogen, catching up with gas, the gas time is caught up with to be 1.2h, and sampling analysis, qualified product proceed to different ester raw material tank, therefore integrated artistic list easy handling, reaction conditions also easily controls, therefore by product is less, and esterification finished product purity is higher, improves the efficiency of later stage synthesis Diuron Tech.
Therefore above-mentioned production technique is adopted, can by simple for Diuron Tech esterification technique easy handling, reaction conditions also easily controls, and therefore by product is less, and esterification finished product purity is higher, improves the efficiency of later stage synthesis Diuron Tech.
Embodiment 3
First the toluene solution measured is squeezed into and dissolve in dehydrating kettle, again the aniline of liquid state is squeezed into scale tank from aniline storage tank, quantitative aniline is put into afterwards according to Weighing module, and aniline is dissolved in toluene by stirring, squeeze in aniline toluene tank and obtain 3,4-dichlorphenamide bulk powder toluene solution is stand-by, can obtain the 3,4-DCA toluene solution of higher degree;
Again quantitative toluene is squeezed in cold light still and absorb a certain amount of phosgene, after up to standard by analysis, while lead to 3 of the aforementioned middle metering of plain edge dropping, 4-dichlorphenamide bulk powder toluene solution, and the pressure in maintenance cold light still is all the time under negative pressure, temperature 73 DEG C, and the by product of reaction is less, improves the efficiency of reaction;
To continue logical photoresponse in aforesaid cold light still again, and the time of continuing logical phosgene is 1.8h, stops stirring, can reduce the generation of by product, make reactant reaction more complete;
Again by the material of aforesaid logical photoresponse under maintenance negative pressure, proceed to thermo-optical still, and thermo-optical still be slowly warming up to 85 DEG C, rear sampling clear, be easy to control the condition of reactant;
Finally the material in aforementioned is transferred in desolventizing still, and the phosgene toluene liquid deviate from material, catching up with gas with passing into nitrogen, catching up with gas, the gas time is caught up with to be 1.3h, and sampling analysis, qualified product proceed to different ester raw material tank, therefore integrated artistic list easy handling, reaction conditions also easily controls, therefore by product is less, and esterification finished product purity is higher, improves the efficiency of later stage synthesis Diuron Tech.
Therefore above-mentioned production technique is adopted, can by simple for Diuron Tech esterification technique easy handling, reaction conditions also easily controls, and therefore by product is less, and esterification finished product purity is higher, improves the efficiency of later stage synthesis Diuron Tech.
Embodiment 4
First the toluene solution measured is squeezed into and dissolve in dehydrating kettle, again the aniline of liquid state is squeezed into scale tank from aniline storage tank, quantitative aniline is put into afterwards according to Weighing module, and aniline is dissolved in toluene by stirring, squeeze in aniline toluene tank and obtain 3,4-dichlorphenamide bulk powder toluene solution is stand-by, can obtain the 3,4-DCA toluene solution of higher degree;
Again quantitative toluene is squeezed in cold light still and absorb a certain amount of phosgene, after up to standard by analysis, while lead to 3 of the aforementioned middle metering of plain edge dropping, 4-dichlorphenamide bulk powder toluene solution, and the pressure in maintenance cold light still is all the time under negative pressure, temperature 74 DEG C, and the by product of reaction is less, improves the efficiency of reaction;
To continue logical photoresponse in aforesaid cold light still again, and the time of continuing logical phosgene is 1.5h, stops stirring, can reduce the generation of by product, make reactant reaction more complete;
Again by the material of aforesaid logical photoresponse under maintenance negative pressure, proceed to thermo-optical still, and thermo-optical still be slowly warming up to 87 DEG C, rear sampling clear, be easy to control the condition of reactant;
Finally the material in aforementioned is transferred in desolventizing still, and the phosgene toluene liquid deviate from material, catching up with gas with passing into nitrogen, catching up with gas, the gas time is caught up with to be 1.4h, and sampling analysis, qualified product proceed to different ester raw material tank, therefore integrated artistic list easy handling, reaction conditions also easily controls, therefore by product is less, and esterification finished product purity is higher, improves the efficiency of later stage synthesis Diuron Tech.
Therefore above-mentioned production technique is adopted, can by simple for Diuron Tech esterification technique easy handling, reaction conditions also easily controls, and therefore by product is less, and esterification finished product purity is higher, improves the efficiency of later stage synthesis Diuron Tech.
Embodiment 5
First the toluene solution measured is squeezed into and dissolve in dehydrating kettle, again the aniline of liquid state is squeezed into scale tank from aniline storage tank, quantitative aniline is put into afterwards according to Weighing module, and aniline is dissolved in toluene by stirring, squeeze in aniline toluene tank and obtain 3,4-dichlorphenamide bulk powder toluene solution is stand-by, can obtain the 3,4-DCA toluene solution of higher degree;
Again quantitative toluene is squeezed in cold light still and absorb a certain amount of phosgene, after up to standard by analysis, while lead to 3 of the aforementioned middle metering of plain edge dropping, 4-dichlorphenamide bulk powder toluene solution, and the pressure in maintenance cold light still is all the time under negative pressure, temperature 75 DEG C, and the by product of reaction is less, improves the efficiency of reaction;
To continue logical photoresponse in aforesaid cold light still again, and the time of continuing logical phosgene is 2.0h, stops stirring, can reduce the generation of by product, make reactant reaction more complete;
Again by the material of aforesaid logical photoresponse under maintenance negative pressure, proceed to thermo-optical still, and thermo-optical still be slowly warming up to 90 DEG C, rear sampling clear, be easy to control the condition of reactant;
Finally the material in aforementioned is transferred in desolventizing still, and the phosgene toluene liquid deviate from material, catching up with gas with passing into nitrogen, catching up with gas, the gas time is caught up with to be 1.5h, and sampling analysis, qualified product proceed to different ester raw material tank, therefore integrated artistic list easy handling, reaction conditions also easily controls, therefore by product is less, and esterification finished product purity is higher, improves the efficiency of later stage synthesis Diuron Tech.
Therefore above-mentioned production technique is adopted, can by simple for Diuron Tech esterification technique easy handling, reaction conditions also easily controls, and therefore by product is less, and esterification finished product purity is higher, improves the efficiency of later stage synthesis Diuron Tech.
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. a lactate synthesis technique for Diuron Tech, is characterized in that: its step is as follows:
1) first the toluene solution measured is squeezed in dissolving dehydrating kettle, again the aniline of liquid state is squeezed into scale tank from aniline storage tank, quantitative aniline is put into afterwards according to Weighing module, and aniline is dissolved in toluene by stirring, squeeze in aniline toluene tank that to obtain 3,4-DCA toluene solution stand-by;
2) quantitative toluene is squeezed in cold light still absorb a certain amount of phosgene, after up to standard by analysis, while lead to the 3,4-DCA toluene solution that plain edge drips metering in step 1, and keep pressure in cold light still all the time under negative pressure, temperature 70-75 DEG C;
3) logical photoresponse will be continued in the cold light still in step 2, and the time of continuing logical phosgene is 1.5-2h, stops stirring;
4) material of the logical photoresponse of step 3 is being kept, under negative pressure, proceeding to thermo-optical still, and thermo-optical still being slowly warming up to 80-90 DEG C, rear sampling clear;
5) material in step 4 is transferred in desolventizing still, and deviates from the phosgene toluene liquid in material, catching up with gas with passing into nitrogen, catching up with gas, catching up with the gas time to be 1-1.5h, and sampling analysis, qualified product proceed to different ester raw material tank.
2. the lactate synthesis technique of a kind of Diuron Tech according to claim 1, is characterized in that: its step is as follows:
1) first the toluene solution measured is squeezed in dissolving dehydrating kettle, again the aniline of liquid state is squeezed into scale tank from aniline storage tank, quantitative aniline is put into afterwards according to Weighing module, and aniline is dissolved in toluene by stirring, squeeze in aniline toluene tank that to obtain 3,4-DCA toluene solution stand-by;
2) quantitative toluene is squeezed in cold light still absorb a certain amount of phosgene, after up to standard by analysis, while lead to the 3,4-DCA toluene solution that plain edge drips metering in step 1, and keep pressure in cold light still all the time under negative pressure, temperature 70 C;
3) logical photoresponse will be continued in the cold light still in step 2, and the time of continuing logical phosgene is 1.5h, stops stirring;
4) material of the logical photoresponse of step 3 is being kept, under negative pressure, proceeding to thermo-optical still, and thermo-optical still being slowly warming up to 80 DEG C, rear sampling clear;
5) material in step 4 is transferred in desolventizing still, and deviates from the phosgene toluene liquid in material, catching up with gas with passing into nitrogen, catching up with gas, catching up with the gas time to be 1h, and sampling analysis, qualified product proceed to different ester raw material tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510692499.1A CN105254536A (en) | 2015-10-20 | 2015-10-20 | Diuron esterification synthesis process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510692499.1A CN105254536A (en) | 2015-10-20 | 2015-10-20 | Diuron esterification synthesis process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105254536A true CN105254536A (en) | 2016-01-20 |
Family
ID=55094533
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510692499.1A Pending CN105254536A (en) | 2015-10-20 | 2015-10-20 | Diuron esterification synthesis process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105254536A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112521312A (en) * | 2020-12-03 | 2021-03-19 | 安徽广信农化股份有限公司 | Synthesis method of isoproturon herbicide |
-
2015
- 2015-10-20 CN CN201510692499.1A patent/CN105254536A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 于春红等: "敌草隆的合成方法改进", 《现代农药》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112521312A (en) * | 2020-12-03 | 2021-03-19 | 安徽广信农化股份有限公司 | Synthesis method of isoproturon herbicide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101709041A (en) | Process for producing diuron | |
| CN103539704A (en) | Method for preparing diuron | |
| CA3186770C (en) | Method for preparing crystalline d-psicose | |
| CN104530053A (en) | Preparation method of medicinal crystal form tofacitinib citrate | |
| CN104479257A (en) | Application of uracil compound as organic thermal stabilizer of transparent polyester product | |
| CN101704766B (en) | Preparation method of arginine aspirin and powder-injection of arginine aspirin | |
| CN103420891B (en) | The synthetic method of type II diabetes medicine glimepiride intermediate benzene sulfanilamide (SN) triphosgene | |
| CN105254536A (en) | Diuron esterification synthesis process | |
| CN102617374B (en) | Method for preparing betaine hydrochloride | |
| CN103626654B (en) | One prepares the method for 2,4-D dimethylamine salt raw pesticide | |
| CN107383418B (en) | A kind of uvioresistant plastic additive and preparation method thereof | |
| CN104926692A (en) | Preparation process for bromoxynil octanoate | |
| CN102432625A (en) | Crystallization method for preparing high-purity I-type clopidogrel hydrogen sulfate | |
| CN105001123A (en) | Cold synthesis technology of diuron | |
| CN102234239A (en) | Optimization process of glycine ethyl ester hydrochloride | |
| CN104447289A (en) | Preparation method of 2, 4-D dimethylamine salt and water-soluble granules thereof | |
| CN105017088A (en) | Production process of diuron | |
| CN105037214A (en) | Esterification synthesis technology of diuron | |
| CN103980185A (en) | Preparation method of hindered amine light stabilizer 770 | |
| CN105294503B (en) | A kind of purifying technique of diuron | |
| CN105439846A (en) | Purification method for natural abscisic acid | |
| CN203264720U (en) | Reaction kettle with mixed feeding device for chemical reaction process | |
| CN104496855A (en) | Method for preparing diuron | |
| CN103922366B (en) | A kind of Delan of utilization produces the method for mother liquor extracting sulfuric acid sodium | |
| CN105017087A (en) | Pretreatment technology for diuron recovered solvent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160120 |
|
| RJ01 | Rejection of invention patent application after publication |