CN107162937A - A kind of synthesis technique of high-quality diuron - Google Patents
A kind of synthesis technique of high-quality diuron Download PDFInfo
- Publication number
- CN107162937A CN107162937A CN201710567385.3A CN201710567385A CN107162937A CN 107162937 A CN107162937 A CN 107162937A CN 201710567385 A CN201710567385 A CN 201710567385A CN 107162937 A CN107162937 A CN 107162937A
- Authority
- CN
- China
- Prior art keywords
- diuron
- quality
- dimethylamine
- toluene
- synthesis technique
- 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
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of synthesis technique of high-quality diuron, its step is as follows:Toluene and 40% dimethylamine are added in cold synthesis reactor, 3.4 dichloro phenylisocyanates are added dropwise at 25 DEG C or so, Bi Baowen half an hour is added dropwise, is put into heat seal kettle and is warming up to 85 DEG C, react to obtain diuron, dried by centrifuge washing.Invention consumption of raw materials, cost are low, and no waste water is produced, and is conducive to environmental protection, while the conversion ratio of product improves more than 98.5%, the purity of product also reaches more than 99.3%.
Description
Technical field
The present invention relates to pesticide processing field, and in particular to a kind of synthesis technique of high-quality diuron.
Background technology
Diuron, chemical entitled 3- (3,4- dichlorophenyl) -1,1- dimethyl ureas, molecular weight:233.1, sterling is colourless
Crystalline solid, 158~159 DEG C of fusing point is soluble in hot alcohol, and solubility is 5.3% in acetone at 27 DEG C, is slightly dissolved in acetic acid second
Ester, ethanol and hot benzene.It is water insoluble, 42ppm when solubility in water is 25 DEG C, solubility is low in hydro carbons, to oxidation and
Hydrolysis-stable, the general weeds for preventing and kill off noncrop area, anti-weeds spread again, be also used for asparagus, citrus, cotton, pineapple,
The weeding of sugarcane, temperate zone trees and shrub fruit.Its structural formula is:
At present, the synthetic method of diuron mainly includes two-step reaction:
(1) photochemical reaction generation 3,4- dichlorophenyl isocyanates occur for 3,4- dichloroanilines and phosgene;(2) 3,4- dichloros
With dimethylamine aminating reaction generation diuron occurs for phenyl isocyanate.(1) step reaction generation 3,4- dichlorophenyl isocyanic acids
The method of ester mainly has two kinds, and one kind is, first by 3,4-DCA and hydrogen chloride into after salt, then to carry out high temperature photochemical reaction, should
Method occupancy equipment is more, and seriously corroded, and hydrogen chloride gas are produced in addition and know from experience the substantial amounts of spent acid of generation.Will during another method
Between 3,4-DCA be dissolved in organic solvent, then first low temperature is passed through phosgene and carries out luminescence reaction, then the hot light of progress that heats up
Change temperature in reaction, this method production process to be difficult to control to, easily caking parcel, yield is low, and content is low.
Because although existing cold conjunction technique solve above mentioned problem, but still do not reach in environmental protection and yield and purity
It is required that, therefore the present invention further provides a kind of cold conjunction work of higher quality on the basis of the cold conjunction technique productions of existing our factory
Skill.
The content of the invention
It is an object of the invention to provide a kind of synthesis technique of high-quality diuron, the purity of product is improved.
To achieve these goals, the technical solution adopted by the present invention is:
A kind of synthesis technique of high-quality diuron, it is characterised in that its step is as follows:
1) toluene and 40% dimethylamine are added in cold synthesis reactor;
2) 3,4 dichloro phenylisocyanates, completion of dropping insulation half an hour are added dropwise at 20-28 DEG C;
3) shift in above-mentioned material to heat seal kettle and be warming up to 80-95 DEG C, react to obtain diuron;
4) above-mentioned product is drying to obtain to the diuron of high-quality by centrifuge washing.
Further, step 1 carries out the preparation of dimethylamine solution first:First toluene solution is added in dissolution kettle, so
The dimethylamine for adding liquid afterwards is stirred uniformly, and well mixed mixture is transferred to by the dimethylamine solution of formation 40%
It is stand-by in aniline toluene tank.
Further, it is negative pressure that the pressure in cold light kettle is kept in step 2, and temperature is stirred 15 minutes at 20-28 DEG C, drop
Add and stirred 20-30 minutes while insulation after finishing.
Further, step 3 is deviate from for product is transferred into heat seal kettle after being to slowly warm up to 80-95 DEG C, sampling clear
Dimethylamine solution;By greenhouse cooling to 20-25 DEG C, diuron raw material tank is transferred to after sampling analysis qualified products, now product is supplied
Rectifying section is used.
Further, the diuron raw material generated step 3 in step 4 is added to essence with 1000-1500 kilograms per hour
Evaporate section, under vacuum by an overhead extraction per hour 700-800 kilograms of toluene solvant to toluene groove;Then concentrate
350-400 kilograms produces the kettle liquid groove entered in a tower from bottom of towe per hour, then by a tower reactor liquid pump with per hour
350-400 kilograms is transported in two towers, further sloughs 50-100 kilograms per hour of solvent toluene from tower top under vacuum;
Then 260-300 kilograms of concentrate is produced by tower reactor, is entered in three towers, under vacuum, from side take-off diuron into
200-250 kilograms per hour of product;The diuron of high-quality is drying to obtain by centrifuge washing, carries out being transferred to finished product after analysis is qualified
In storage tank.
Further, 40% dimethylamine in step 1 is 40% dimethylamine agueous solution.
Further, toluene and 3 in step 1 and 2, the amount ratio of the material of 4 dichloro phenylisocyanates is (10.0-11.1):
1。
Further, temperature when being added dropwise in step 2 is 25 DEG C.
Further, the temperature heated up in step 3 is 92 DEG C.
Further, the amount ratio of the material of 3,4 dichloro phenylisocyanates and dimethylamine is (1-1.1):1.
Advantage of the present invention is:Cold conjunction is first carried out using above-mentioned technique and then heat seal reaction is carried out both having avoided 3,4- dichloros
Decomposition of the phenyl isocyanate in aqueous phase, also solves and is asked using addition late phase reaction is slow during dimethylamine gas
Topic, while it also avoid the problem of existing use phosgene produces accessory substance, the simpler process of production process is also relatively easy to control,
It is high amount of liquid diformazan that the dimethylamine used in product quality and yield, the present invention is further improved on the basis of existing
Amine, it is easy to store, transport, the process of dimethylamine vaporization is also reduced compared with using gas dimethylamine, dimethylamine is reduced and disappears
Consumption.Consumption of raw materials of the present invention, cost are low, and no waste water is produced, and is conducive to environmental protection, while the conversion ratio of product improves 98.5%
More than, the purity of product also reaches more than 99.3%.
Embodiment
The present invention is described in further details below in conjunction with embodiment.
Embodiment 1
The preparation of dimethylamine solution is carried out first:First toluene solution is added in dissolution kettle, the two of liquid is then added
Methylamine is stirred uniformly, the dimethylamine solution of formation 40%, and well mixed mixture is transferred in aniline toluene tank
It is stand-by, 28.2Kg toluene and 40% dimethylamine 16.8Kg are added in cold synthesis reactor, 138Kg 3.4 dichloros are added dropwise at 20 DEG C
Phenylisocyanate, it is negative pressure to hold the pressure in cold light kettle, is stirred 15 minutes, 20-30 points of stirring while insulation after completion of dropping
Clock, is added dropwise Bi Baowen half an hour;Product is transferred to heat seal kettle, dimethylamine is deviate from after being to slowly warm up to 80 DEG C, sampling clear
Solution;By greenhouse cooling to 20-25 DEG C, diuron raw material tank is transferred to after sampling analysis qualified products, now product supplies rectifying section
Use, react to obtain diuron, the diuron raw material of generation is added to rectifying section with 1000-1500 kilograms per hour, in vacuum bar
Under part by an overhead extraction per hour 700-800 kilograms of toluene solvant to toluene groove;Then concentrate 350-400 per hour
Kilogram the kettle liquid groove that enters in a tower is produced from bottom of towe, then by a tower reactor liquid pump with 350-400 kilograms per hour conveying
Into two towers, further 50-100 kilograms per hour of solvent toluene is sloughed from tower top under vacuum;Then concentrate 260-
300 kilograms are produced by tower reactor, are entered in three towers, under vacuum, from side take-off diuron finished product 200-250 per hour
Kilogram;High-quality 34.887Kg diuron is drying to obtain by centrifuge washing, be transferred to after analysis is qualified in finished product storage tank.
The present invention first carries out cold conjunction using above-mentioned technique and then carries out heat seal reaction both to have avoided 3,4- dichlorophenyls different
Decomposition of the cyanate in aqueous phase, also solves addition late phase reaction slow problem when using dimethylamine gas, simultaneously
The problem of existing use phosgene produces accessory substance is it also avoid, the simpler process of production process is also relatively easy to control, in existing base
It is high amount of liquid dimethylamine that the dimethylamine used in product quality and yield, the present invention is further improved on plinth, easily
In storage, transport, the process of dimethylamine vaporization is also reduced compared with using gas dimethylamine, dimethylamine consumption is reduced.This
Invention consumption of raw materials, cost are low, and no waste water is produced, and is conducive to environmental protection, while the conversion ratio of product improves more than 98.5%,
The purity of product also reaches more than 99.3%.
Embodiment 2
The preparation of dimethylamine solution is carried out first:First toluene solution is added in dissolution kettle, the two of liquid is then added
Methylamine is stirred uniformly, the dimethylamine solution of formation 40%, and well mixed mixture is transferred in aniline toluene tank
It is stand-by, 28.2Kg toluene and 40% dimethylamine 17.2Kg are added in cold synthesis reactor, the 3.4 2 of 140.5Kg is added dropwise at 20 DEG C
Chlorobenzene isocyanates, it is negative pressure to hold the pressure in cold light kettle, is stirred 15 minutes, and 20-30 is stirred while insulation after completion of dropping
Minute, Bi Baowen half an hour is added dropwise;Product is transferred to heat seal kettle, diformazan is deviate from after being to slowly warm up to 85 DEG C, sampling clear
Amine aqueous solution;By greenhouse cooling to 20-25 DEG C, diuron raw material tank is transferred to after sampling analysis qualified products, now product supplies rectifying
Section is used, and reacts to obtain diuron, the diuron raw material of generation is added to rectifying section with 1000-1500 kilograms per hour, in vacuum
Under the conditions of by an overhead extraction per hour 700-800 kilograms of toluene solvant to toluene groove;Then concentrate 350- per hour
400 kilograms produce the kettle liquid groove entered in a tower from bottom of towe, then defeated with 350-400 kilograms per hour by a tower reactor liquid pump
It is sent in two towers, further sloughs 50-100 kilograms per hour of solvent toluene from tower top under vacuum;Then concentrate
260-300 kilograms is produced by tower reactor, is entered in three towers, under vacuum, from side take-off diuron finished product per hour
200-250 kilograms;High-quality 34.913Kg diuron is drying to obtain by centrifuge washing, carries out being transferred to finished product after analysis is qualified
In storage tank.
The present invention first carries out cold conjunction using above-mentioned technique and then carries out heat seal reaction both to have avoided 3,4- dichlorophenyls different
Decomposition of the cyanate in aqueous phase, also solves addition late phase reaction slow problem when using dimethylamine gas, simultaneously
The problem of existing use phosgene produces accessory substance is it also avoid, the simpler process of production process is also relatively easy to control, in existing base
It is high amount of liquid dimethylamine that the dimethylamine used in product quality and yield, the present invention is further improved on plinth, easily
In storage, transport, the process of dimethylamine vaporization is also reduced compared with using gas dimethylamine, dimethylamine consumption is reduced.This
Invention consumption of raw materials, cost are low, and no waste water is produced, and is conducive to environmental protection, while the conversion ratio of product improves more than 98.5%,
The purity of product also reaches more than 99.3%.
Embodiment 3
The preparation of dimethylamine solution is carried out first:First toluene solution is added in dissolution kettle, the two of liquid is then added
Methylamine is stirred uniformly, the dimethylamine solution of formation 40%, and well mixed mixture is transferred in aniline toluene tank
It is stand-by, 28.7Kg toluene and 40% dimethylamine 17.88Kg are added in cold synthesis reactor, the 3.4 2 of 143.2Kg is added dropwise at 20 DEG C
Chlorobenzene isocyanates, it is negative pressure to hold the pressure in cold light kettle, is stirred 15 minutes, and 20-30 is stirred while insulation after completion of dropping
Minute, Bi Baowen half an hour is added dropwise;Product is transferred to heat seal kettle, diformazan is deviate from after being to slowly warm up to 88 DEG C, sampling clear
Amine aqueous solution;By greenhouse cooling to 20-25 DEG C, diuron raw material tank is transferred to after sampling analysis qualified products, now product supplies rectifying
Section is used, and reacts to obtain diuron, the diuron raw material of generation is added to rectifying section with 1000-1500 kilograms per hour, in vacuum
Under the conditions of by an overhead extraction per hour 700-800 kilograms of toluene solvant to toluene groove;Then concentrate 350- per hour
400 kilograms produce the kettle liquid groove entered in a tower from bottom of towe, then defeated with 350-400 kilograms per hour by a tower reactor liquid pump
It is sent in two towers, further sloughs 50-100 kilograms per hour of solvent toluene from tower top under vacuum;Then concentrate
260-300 kilograms is produced by tower reactor, is entered in three towers, under vacuum, from side take-off diuron finished product per hour
200-250 kilograms;High-quality 34.899Kg diuron is drying to obtain by centrifuge washing, carries out being transferred to finished product after analysis is qualified
In storage tank.
The present invention first carries out cold conjunction using above-mentioned technique and then carries out heat seal reaction both to have avoided 3,4- dichlorophenyls different
Decomposition of the cyanate in aqueous phase, also solves addition late phase reaction slow problem when using dimethylamine gas, simultaneously
The problem of existing use phosgene produces accessory substance is it also avoid, the simpler process of production process is also relatively easy to control, in existing base
It is high amount of liquid dimethylamine that the dimethylamine used in product quality and yield, the present invention is further improved on plinth, easily
In storage, transport, the process of dimethylamine vaporization is also reduced compared with using gas dimethylamine, dimethylamine consumption is reduced.This
Invention consumption of raw materials, cost are low, and no waste water is produced, and is conducive to environmental protection, while the conversion ratio of product improves more than 98.5%,
The purity of product also reaches more than 99.3%.
Embodiment 4
The preparation of dimethylamine solution is carried out first:First toluene solution is added in dissolution kettle, the two of liquid is then added
Methylamine is stirred uniformly, the dimethylamine solution of formation 40%, and well mixed mixture is transferred in aniline toluene tank
It is stand-by, 28.7Kg toluene and 40% dimethylamine 18.2Kg are added in cold synthesis reactor, the 3.4 2 of 148.8Kg is added dropwise at 20 DEG C
Chlorobenzene isocyanates, it is negative pressure to hold the pressure in cold light kettle, is stirred 15 minutes, and 20-30 is stirred while insulation after completion of dropping
Minute, Bi Baowen half an hour is added dropwise;Product is transferred to heat seal kettle, diformazan is deviate from after being to slowly warm up to 92 DEG C, sampling clear
Amine aqueous solution;By greenhouse cooling to 20-25 DEG C, diuron raw material tank is transferred to after sampling analysis qualified products, now product supplies rectifying
Section is used, and reacts to obtain diuron, the diuron raw material of generation is added to rectifying section with 1000-1500 kilograms per hour, in vacuum
Under the conditions of by an overhead extraction per hour 700-800 kilograms of toluene solvant to toluene groove;Then concentrate 350- per hour
400 kilograms produce the kettle liquid groove entered in a tower from bottom of towe, then defeated with 350-400 kilograms per hour by a tower reactor liquid pump
It is sent in two towers, further sloughs 50-100 kilograms per hour of solvent toluene from tower top under vacuum;Then concentrate
260-300 kilograms is produced by tower reactor, is entered in three towers, under vacuum, from side take-off diuron finished product per hour
200-250 kilograms;High-quality 34.938Kg diuron is drying to obtain by centrifuge washing, carries out being transferred to finished product after analysis is qualified
In storage tank.
The present invention first carries out cold conjunction using above-mentioned technique and then carries out heat seal reaction both to have avoided 3,4- dichlorophenyls different
Decomposition of the cyanate in aqueous phase, also solves addition late phase reaction slow problem when using dimethylamine gas, simultaneously
The problem of existing use phosgene produces accessory substance is it also avoid, the simpler process of production process is also relatively easy to control, in existing base
It is high amount of liquid dimethylamine that the dimethylamine used in product quality and yield, the present invention is further improved on plinth, easily
In storage, transport, the process of dimethylamine vaporization is also reduced compared with using gas dimethylamine, dimethylamine consumption is reduced.This
Invention consumption of raw materials, cost are low, and no waste water is produced, and is conducive to environmental protection, while the conversion ratio of product improves more than 98.5%,
The purity of product also reaches more than 99.3%.
Embodiment 5
The preparation of dimethylamine solution is carried out first:First toluene solution is added in dissolution kettle, the two of liquid is then added
Methylamine is stirred uniformly, the dimethylamine solution of formation 40%, and well mixed mixture is transferred in aniline toluene tank
It is stand-by, 28.2Kg toluene and 40% dimethylamine 18.30Kg are added in cold synthesis reactor, the 3.4 2 of 151.0Kg is added dropwise at 20 DEG C
Chlorobenzene isocyanates, it is negative pressure to hold the pressure in cold light kettle, is stirred 15 minutes, and 20-30 is stirred while insulation after completion of dropping
Minute, Bi Baowen half an hour is added dropwise;Product is transferred to heat seal kettle, diformazan is deviate from after being to slowly warm up to 95 DEG C, sampling clear
Amine aqueous solution;By greenhouse cooling to 20-25 DEG C, diuron raw material tank is transferred to after sampling analysis qualified products, now product supplies rectifying
Section is used, and reacts to obtain diuron, the diuron raw material of generation is added to rectifying section with 1000-1500 kilograms per hour, in vacuum
Under the conditions of by an overhead extraction per hour 700-800 kilograms of toluene solvant to toluene groove;Then concentrate 350- per hour
400 kilograms produce the kettle liquid groove entered in a tower from bottom of towe, then defeated with 350-400 kilograms per hour by a tower reactor liquid pump
It is sent in two towers, further sloughs 50-100 kilograms per hour of solvent toluene from tower top under vacuum;Then concentrate
260-300 kilograms is produced by tower reactor, is entered in three towers, under vacuum, from side take-off diuron finished product per hour
200-250 kilograms;High-quality 34.930Kg diuron is drying to obtain by centrifuge washing, carries out being transferred to finished product after analysis is qualified
In storage tank.
The present invention first carries out cold conjunction using above-mentioned technique and then carries out heat seal reaction both to have avoided 3,4- dichlorophenyls different
Decomposition of the cyanate in aqueous phase, also solves addition late phase reaction slow problem when using dimethylamine gas, simultaneously
The problem of existing use phosgene produces accessory substance is it also avoid, the simpler process of production process is also relatively easy to control, in existing base
It is high amount of liquid dimethylamine that the dimethylamine used in product quality and yield, the present invention is further improved on plinth, easily
In storage, transport, the process of dimethylamine vaporization is also reduced compared with using gas dimethylamine, dimethylamine consumption is reduced.This
Invention consumption of raw materials, cost are low, and no waste water is produced, and is conducive to environmental protection, while the conversion ratio of product improves more than 98.5%,
The purity of product also reaches more than 99.3%.
Claims (10)
1. a kind of synthesis technique of high-quality diuron, it is characterised in that its step is as follows:
1) toluene and 40% dimethylamine are added in cold synthesis reactor;
2) 3,4 dichloro phenylisocyanates, completion of dropping insulation half an hour are added dropwise at 20-28 DEG C;
3) shift in above-mentioned material to heat seal kettle and be warming up to 80-95 DEG C, react to obtain diuron;
4) above-mentioned product is drying to obtain to the diuron of high-quality by centrifuge washing.
2. a kind of synthesis technique of high-quality diuron according to claim 1, it is characterised in that:Step 1 is carried out first
The preparation of dimethylamine solution:First toluene solution is added in dissolution kettle, the dimethylamine for then adding liquid is stirred uniformly,
The dimethylamine solution of formation 40%, well mixed mixture is transferred to stand-by in aniline toluene tank.
3. a kind of synthesis technique of high-quality diuron according to claim 1, it is characterised in that:Kept in step 2 cold
Pressure in light kettle is negative pressure, and temperature is stirred 15 minutes at 20-28 DEG C, 20-30 points of stirring while insulation after completion of dropping
Clock.
4. a kind of synthesis technique of high-quality diuron according to claim 1, it is characterised in that:Step 3 is by product
Heat seal kettle is transferred to, dimethylamine solution is deviate from after being to slowly warm up to 80-95 DEG C, sampling clear;By greenhouse cooling to 20-25
DEG C, diuron raw material tank is transferred to after sampling analysis qualified products, now product is used for rectifying section.
5. a kind of synthesis technique of high-quality diuron according to claim 1, it is characterised in that:By step 3 in step 4
The diuron raw material of generation is added to rectifying section with 1000-1500 kilograms per hour, passes through an overhead extraction under vacuum
700-800 kilograms of toluene solvant is to toluene groove per hour;Then concentrate produces entrance for 350-400 kilograms from bottom of towe per hour
To the kettle liquid groove in a tower, then it is transported to by a tower reactor liquid pump with 350-400 kilograms per hour in two towers, in vacuum condition
Under further slough 50-100 kilograms per hour of solvent toluene from tower top;Then 260-300 kilograms of concentrate is produced by tower reactor, is entered
Enter into three towers, under vacuum, from 200-250 kilograms per hour of side take-off diuron finished product;It is dry by centrifuge washing
The dry diuron for producing high-quality, be transferred to after analysis is qualified in finished product storage tank.
6. a kind of synthesis technique of high-quality diuron according to claim 1, it is characterised in that:40% in step 1
Dimethylamine be 40% dimethylamine agueous solution.
7. a kind of synthesis technique of high-quality diuron according to claim 1, it is characterised in that:Toluene in step 1 and 2
With 3, the amount ratio of the material of 4 dichloro phenylisocyanates is (10.0-11.1):1.
8. a kind of synthesis technique of high-quality diuron according to claim 1, it is characterised in that:When being added dropwise in step 2
Temperature be 25 DEG C.
9. a kind of synthesis technique of high-quality diuron according to claim 1 or 4, it is characterised in that:Risen in step 3
The temperature of temperature is 92 DEG C.
10. a kind of synthesis technique of high-quality diuron according to claim 1, it is characterised in that:3,4 dichloro-benzenes isocyanides
The amount ratio of the material of acid esters and dimethylamine is (1-1.1):1.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710567385.3A CN107162937A (en) | 2017-07-12 | 2017-07-12 | A kind of synthesis technique of high-quality diuron |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710567385.3A CN107162937A (en) | 2017-07-12 | 2017-07-12 | A kind of synthesis technique of high-quality diuron |
Publications (1)
Publication Number | Publication Date |
---|---|
CN107162937A true CN107162937A (en) | 2017-09-15 |
Family
ID=59824058
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201710567385.3A Pending CN107162937A (en) | 2017-07-12 | 2017-07-12 | A kind of synthesis technique of high-quality diuron |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN107162937A (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 |
Citations (3)
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 |
CN103739520A (en) * | 2013-12-26 | 2014-04-23 | 安徽广信农化股份有限公司 | Refining method of 3,4-dichlorobenzene isocyanate |
CN105037214A (en) * | 2015-06-29 | 2015-11-11 | 安徽广信农化股份有限公司 | Esterification synthesis technology of diuron |
-
2017
- 2017-07-12 CN CN201710567385.3A patent/CN107162937A/en active Pending
Patent Citations (3)
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 |
CN103739520A (en) * | 2013-12-26 | 2014-04-23 | 安徽广信农化股份有限公司 | Refining method of 3,4-dichlorobenzene isocyanate |
CN105037214A (en) * | 2015-06-29 | 2015-11-11 | 安徽广信农化股份有限公司 | Esterification synthesis technology of diuron |
Non-Patent Citations (1)
Title |
---|
任嘉敏 等: "《通用化工产品分析方法手册》", 31 January 1999 * |
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 |
---|---|---|
CN106278953B (en) | A kind of production method for improving Metformin hydrochloride purity | |
CN105837563A (en) | Production method of flumioxazin | |
CN103539704A (en) | Method for preparing diuron | |
CN112358419B (en) | Synthesis process of 3, 4-dichlorophenyl isocyanate | |
CN101376627B (en) | Preparation of 4-hydroxybenzoyl chloride | |
CN107162937A (en) | A kind of synthesis technique of high-quality diuron | |
CN103739520A (en) | Refining method of 3,4-dichlorobenzene isocyanate | |
CN111217765A (en) | Synthesis process of 3-methyl-4-nitroiminoperhydro-1,3,5-oxadiazine | |
CN101274904B (en) | Preparation for 3, 4-dichloro phenyl isocyanate | |
CN107445869A (en) | A kind of synthetic method of Metformin hydrochloride | |
CN107473927B (en) | Preparation process of biphenyl dichlorobenzyl | |
CN104628670A (en) | 6-nitro-1,2-diazoxynaphthalene-4-sulfonic acid and preparation method thereof | |
CA2118378C (en) | Preparation of 5-acetoacetylamino-2-benzimidazolone | |
CN110437078A (en) | The preparation method of bis- [4- aminophenyl] fluorene derivatives of 9,9- | |
CN102267706B (en) | Method for preparing potassium nitrate | |
CN111825120A (en) | Method for preparing battery-grade manganese sulfate from manganese metal | |
CN105622408B (en) | The preparation method of double (2 acetoxy-benzoic acid) calcium carbamide compounds | |
CN108546248B (en) | Preparation method of 1, 2-dihydro-3, 6-pyridazine dione | |
CN102746238A (en) | Preparation method of pyrimethanil | |
CN106518687A (en) | Efficient preparation method of high-purity tetraethyl ammonium chloride | |
CN111410614A (en) | Full-synthesis environment-friendly process of D-calcium pantothenate | |
CN101747281B (en) | Method for preparing 2-nitroimidazole | |
CN104072379B (en) | A kind of preparation method of 2,6 dichloro-4,4 5-trifluoromethylaniline | |
CN102643208B (en) | Preparation method of agomelatine I crystal form | |
CN102702030A (en) | Method for synthesizing diuron original drug |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170915 |
|
WD01 | Invention patent application deemed withdrawn after publication |