A kind of method for preparing bensulfuron-methyl

A technology of bensulfuron-methyl and benzsulfonyl isocyanate, which is applied in the field of preparation of bensulfuron-methyl, can solve the problems of many raw materials of bensulfuron-methyl, unsafe operation, high risk of chlorobutane, etc., so as to improve the synthesis yield and The effect of product quality, improvement of conversion rate and reduction of product cost

Active Publication Date: 2016-03-09
JIANGSU KUAIDA AGROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using this method to prepare bensulfuron-methyl consumes a lot of raw materials, while chlorobutane is highly dangerous and unsafe to operate. Therefore, in order to solve the above problems, the present invention provides a new technical solution

Method used

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  • A kind of method for preparing bensulfuron-methyl

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Embodiment 2

[0018] 33kg / h of phosgene, 127.3kg / h of 30% benzylsulfonamide xylene suspension and catalyst n-butyl isocyanate at a molar ratio of 30:10:1 were continuously added to photochemical reactor I for photochemical reaction. The temperature in Ⅰ is 110℃, the reaction residence time is 2.5h, the synthesis of o-methoxycarboxybenzyl sulfoisocyanate; the reaction containing o-methoxycarboxybenzyl sulfoisocyanate and unreacted phosgene and the catalyst n-butyl isocyanate The mixture was continuously fed into photochemical reactor II, 8.3kg / h of phosgene was added, the molar ratio of phosgene to the benzylsulfonamide xylene suspension was 1.2:4, the temperature in photochemical reactor II was 125℃, and the reaction residence time was 1.5 h, synthesize o-methoxycarboxybenzyl sulfoisocyanate; o-methoxycarboxybenzyl sulfoisocyanate continuously enters the delustering tower, and the extracted n-butyl isocyanate and xylene are returned to the photochemical reactor I for recycling, and the excess...

Embodiment 3

[0020] 33kg / h of phosgene, 127.3kg / h of 30% benzylsulfonamide xylene suspension and catalyst n-butyl isocyanate at a molar ratio of 60:20:3 were continuously added to the photochemical reactor I for photochemical reaction. The temperature in Ⅰ is 115℃, the reaction residence time is 3h, the synthesis of o-methoxycarboxybenzyl sulfoisocyanate; the reaction mixture containing o-methoxycarboxybenzyl sulfoisocyanate and unreacted phosgene and catalyst n-butyl isocyanate Enter the photochemical kettle II continuously, add 8.3kg / h of phosgene, 1.5:4 phosgene and benzylsulfonamide xylene suspension, the temperature in the photochemical kettle II is 127℃, the reaction residence time is 2h, and o-methoxy is synthesized. Benzyl carboxyl benzyl sulfo isocyanate; o-methoxy carboxyl benzyl sulfo isocyanate enters the delustering tower, and the removed n-butyl isocyanate and xylene are returned to the photochemical reactor I for recycling. The excess phosgene is passed through a cooling separ...

Embodiment 4

[0022] 33kg / h of phosgene, 127.3kg / h of 30% benzylsulfonamide xylene suspension and catalyst n-butyl isocyanate at a molar ratio of 20:5:1 were continuously added to photochemical reactor I for photochemical reaction. The temperature in Ⅰ is 120℃, the reaction residence time is 4h, the synthesis of o-methoxycarboxybenzyl sulfoisocyanate; a reaction mixture containing o-methoxycarboxybenzyl sulfoisocyanate and unreacted phosgene and catalyst n-butyl isocyanate Continuously enter the photochemical reactor II, add 8.3kg / h of phosgene, the molar ratio of phosgene to the benzylsulfonamide xylene solution is 2:4, the temperature in the photochemical reactor II is 130℃, the reaction residence time is 3h, and the ortho Methoxy carboxyl benzyl sulfo isocyanate; o-methoxy carboxyl benzyl sulfo isocyanate enters the delustering tower, and the removed n-butyl isocyanate and xylene are returned to the photochemical reactor I for recycling. The excess phosgene is separated by a cooling separa...

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Abstract

The invention discloses a method for preparing bensulfuron methyl. The method comprises the following steps: adding phosgene, benzylsulfamide xylene and normal-butyl isocyanate into a photochemical kettle I to synthesize o-methoxy carboxyl benzyl sulfamide; after the o-methoxy carboxyl benzyl sulfamide enters a photochemical kettle II, adding phosgene to synthesize o-methoxy carboxyl benzylsulfo isocyanate; enabling o-methoxy carboxyl benzylsulfo isocyanate to enter a stripping tower to strip normal-butyl isocyanate, dimethyl benzene and phosgene; adding o-methoxy carboxyl benzylsulfo isocyanate subjected to gas stripping and 2-amino-4,6-dimethoxy pyrimidine into a synthesis kettle; after the material enters an automatic centrifuger, performing centrifugal separation to obtain the product bensulfuron methyl. The method has the benefits that a catalyst is recycled in the photochemical process, so that the consumption is reduced, and the cost and the treatment cost are both lowered; the stripping tower is adopted to remove phosgene in a dimethyl benzene solution, so that the consumption of dimethyl benzene is reduced; when the method provided by the invention is adopted for synthesis, the synthesis yield and the product quality are improved and the synthesis yield can be up to 98%.

Description

Technical field [0001] The invention relates to a method for preparing herbicides, in particular to a method for preparing bensulfuron-methyl. Background technique [0002] Bensulfuron-methyl is a selective systemic and conductive herbicide, suitable for controlling one-year and perennial broad-leaved weeds and sedges in rice fields. The general preparation method of bensulfuron-methyl is to stir the xylene solution of 2-amino-4,6-dimethoxypyrimidine and methyl o-formate benzylsulfonyl isocyanate for 8-10h in the greenhouse, and then distill the xylene. , Washed with chlorobutane and dried to prepare bensulfuron-methyl. Using this method to prepare bensulfuron-methyl consumes a lot of raw materials, and at the same time chlorobutane is highly dangerous and unsafe to operate. Therefore, in order to solve the above problems, the present invention provides a new technical solution. Summary of the invention [0003] In order to solve the above problems, the present invention provide...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/52
CPCY02P20/584
Inventor 钱圣利韩邦友邱波朱建军康进红
Owner JIANGSU KUAIDA AGROCHEM
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