- Preparation method of phenoxycarboxylate herbicide
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The invention provides a preparation method of a phenoxycarboxylate herbicide, wherein the preparation method includes the steps: S1, carrying out condensation reaction of phenol or o-cresol with chlorocarboxylic ester under the action of alkaline substances to obtain phenoxycarboxylic ester, wherein chlorocarboxylic ester has the general formula of ClR1COOR, R1 is C1-3 alkylene or alkylidene, R is C1-10 alkyl of or C3-10 cycloalkyl; and S2, under the action of a first catalyst and a second catalyst, carrying out selective chlorination of the phenoxycarboxylic ester with a chlorinating agent to obtain the chlorophenoxycarboxylic ester represented by the formula I, R3 is H, Cl or CH3, the first catalyst is selected from Lewis acid, and the second catalyst is selected from C5-22 thioether, thiazole, isothiazole or thiophene compounds; and S3, mixing chlorophenoxycarboxylic ester with an alkaline compound, and carrying out alkaline hydrolysis to obtain the phenoxycarboxylate herbicide. The preparation method can improve the product quality and production operation environment, and has low quantity of three wastes.
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Paragraph 0075; 0077
(2019/01/08)
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- A phenoxy carboxylic acid herbicide preparation method (by machine translation)
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The invention provides a phenoxy carboxylic acid herbicide preparation method, including: S1, will be [...], alkaline substance mixed with the chlorinated carboxylic acid ester, in the one-pot condensation reaction in anhydrous system, phenoxy carboxylic acid ester obtained; the ClR states the chloro- carboxylic acid ester of the formula is1 COOR, R1 Is C1 - 3 alkylene or alkylidene, R is C1 - 10 alkyl or C3 - 10 cycloalkyl; S2, the [...] ester in the 1st and 2nd catalyst under the action of a catalyst, with the chlorinating agent to carry out the selective chlorination of, get [...] ester; the Lewis acid catalyst is selected from 1st, 2nd catalyst is C5 - 22 of the thioether compound, thiazole compound, isothiazole compound or thiophene compound; S3, will the [...] ester to acid hydrolysis reaction, as shown in formula I phenoxy carboxylic acid herbicide, R3 Is H, Cl or CH3 . This invention can improve the quality of the products and the operating environment of production, three waste low. (by machine translation)
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Paragraph 0081; 0083; 0118; 0120
(2019/01/08)
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- Preparation method of phenoxycarboxylic acid herbicide
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The invention provides a preparation method of a phenoxycarboxylic acid herbicide, wherein the preparation method includes the steps: S1, carrying out reaction of anhydrous phenol with an active metalto form phenoxide, and carrying out condensation reaction of the phenoxide with chlorocarboxylic ester to obtain phenoxycarboxylic ester, wherein the chlorocarboxylic ester has the general formula ofClR1COOR, R1 is C1-3 alkylene or alkylidene, and R is C1-10 alkyl or C3-10 of cycloalkyl; S2, carrying out selective chlorination of the phenoxycarboxylic ester with a chlorinating agent in the presence of a first catalyst and a second catalyst to obtain chlorobenzoxycarboxylic ester, wherein the first catalyst is selected from Lewis acid, and the second catalyst is C5-22 thioether, thiazole, isothiazole or thiophene compounds; and S3, carrying out acidolysis reaction of chlorobenzoxycarboxylic ester to obtain the phenoxycarboxylic acid herbicide represented by the formula I, wherein R3 is H,Cl or CH3. The preparation method can improve the product quality and the operation environment of the production site, and has low quantity of three wastes.
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Paragraph 0081; 0083
(2019/01/08)
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- Preparation method of phenoxy carboxylic acid herbicide
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The invention provides a preparation method of a phenoxy carboxylic acid herbicide, comprising the following steps: S1, carrying out a condensation reaction between a phenolic compound and hydroxycarboxylic ester under the action of a catalyst so as to obtain phenoxycarboxylic ester, wherein the catalyst is one or more of protonic acid, solid acid and a supported catalyst; S2, carrying out 2- and/or 4- selecting chlorination reaction between phenoxycarboxylic ester and a chloridizing agent in the presence of a first catalyst and a second catalyst, so as to obtain chlorinated phenoxycarboxylicester, wherein the first catalyst is selected from Lewis acid, and the second catalyst is selected from a C5-C22 thioether compound, a C5-C22 thiazole compound, a C5-C22 isothiazole compound or a C5-C22 thiophene compound; and S3, carrying out an acidolysis reaction on chlorinated phenoxycarboxylic ester so as to obtain the phenoxy carboxylic acid herbicide. By the method, product quality and thelive environment of production can be improved, and ''three wastes (waste gas, waste water and industrial residue)'' are minimized.
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Paragraph 0087; 0089
(2019/01/08)
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- Preparation method of phenoxycarboxylic acid herbicide
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The invention provides a preparation method of a phenoxycarboxylic acid herbicide, wherein the preparation method includes the steps: S1, carrying out condensation reaction of phenol or o-cresol withchlorocarboxylic ester under the action of an alkaline substance to obtain phenoxycarboxylic ester, wherein the chlorocarboxylic ester has the general formula of ClR1COOR, R1 is C1-3 alkylene or alkylidene, and R is C1-10 alkyl or C3-10 cycloalkyl; S2, carrying out selective chlorination of phenoxycarboxylic ester with a chlorinating agent under the action of a first catalyst and a second catalyst, to obtain chlorobenzoxycarboxylic ester, wherein the first catalyst is selected from Lewis acid, the second catalyst is C5-22 thioether compounds, thiazole compounds, isothiazole compounds or thiophene compounds; and S3, carrying out acidolysis reaction of chlorobenzoxycarboxylic ester, to obtain the phenoxycarboxylic acid herbicide represented by the formula I, wherein R3 is H, Cl or CH3. The preparation method can improve the product quality and the operation environment of a production site, and has low quantity of three wastes.
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Paragraph 0082; 0084
(2019/01/08)
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- Preparation method of chlorophenoxycarboxylic ester
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The invention provides a preparation method of chlorophenoxycarboxylic ester, wherein the preparation method includes the following steps: S1) carrying out 2-site and/or 4-site selective chlorinationreaction of phenoxycarboxylic ester with a chlorinating agent under the action of a catalyst A and a catalyst B to obtain chlorophenoxycarboxylic ester, wherein the catalyst A is Lewis acid, the catalyst B has the following structural formula of R1'-S-R2', and the phenoxycarboxylic ester has any structure represented by the formulas I-IV; and S2) carrying out transesterification reaction of chlorophenoxycarboxylic ester and alcohol under the action of a catalyst to obtain long-chain chlorophenoxycarboxylic ester, wherein the alcohol has the molecular formula of R2OH, and R2 is C4-20 alkyl or cycloalkyl. The method improves the yield and purity of chlorophenoxycarboxylic ester by redesigning of the process route and fine screening of the catalysts and the chlorinating agent. The content ofthe obtained chlorophenoxycarboxylic ester can reach 98.5% or more and the yield can reach 98.5% or more.
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Paragraph 0103; 0105; 0109; 0111
(2019/01/08)
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- A phenoxy carboxylic acid ester herbicide preparation method (by machine translation)
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The invention provides a phenoxy carboxylic acid ester herbicide preparation method, including: S1, phenol in the presence of alkaline substance with the chlorinated carboxylic acid ester condensation reaction, phenoxy carboxylic acid ester obtained; the ClR states the chloro- carboxylic acid ester of the general formula1 COOR, R1 Is C1 - 3 alkylene or alkylidene, R is C1 - 10 alkyl or C3 - 10 cycloalkyl; S2, the [...] ester in the 1st and 2nd catalyst the presence of a catalyst, with the chlorinating agent to carry out the selective chlorination of, get [...] ester; the Lewis acid catalyst is selected from the 1st, the 2nd catalyst is C5 - 22 of the thioether, thiazole, thiophene compounds or different benzisothiazoles; S3, will the [...] ester with an alcohol reaction, as shown in formula I phenoxy carboxylic acid ester herbicide; R3 Is H, Cl or CH3 , R ' is a C4 - 20 alkyl or cycloalkyl. This invention can improve the product quality and the production environment, three waste low. (by machine translation)
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Paragraph 0082; 0085
(2019/01/08)
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- Preparation method of chlorophenoxycarboxylic ester
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The invention provides a preparation method of chlorophenoxycarboxylic ester, wherein the preparation method includes the following steps: S1) carrying out 2-site and/or 4-site selective chlorinationreaction of phenoxycarboxylic ester with a chlorinating agent under the action of a catalyst A and a catalyst B to obtain chlorophenoxycarboxylic ester, wherein the catalyst A is Lewis acid, the catalyst B is C5-22 thiazoles, isothiazoles and thiophenes or halogenated derivatives thereof, and the phenoxycarboxylic ester has any structure represented by the formulas I-IV; and S2) carrying out transesterification reaction of chlorophenoxycarboxylic ester and alcohol under the action of a catalyst to obtain long-chain chlorophenoxycarboxylic ester, wherein the alcohol has the molecular formula ofR2OH, and R2 is C4-20 alkyl or cycloalkyl. The method improves the yield and purity of chlorophenoxycarboxylic ester by redesigning of the process route and fine screening of the catalysts and the chlorinating agent. The content of the obtained chlorophenoxycarboxylic ester can reach 98.5% or more and the yield can reach 98.5% or more.
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Paragraph 0092; 0094
(2019/01/08)
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