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Method for preparing bensulfuron methyl

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

Active Publication Date: 2014-01-01
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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  • Method for preparing bensulfuron methyl

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Experimental program
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Effect test

Embodiment 1

[0017] Add phosgene 33 kg / h, 30% benzsulfonamide xylene suspension 127.3 kg / h and catalyst n-butyl isocyanate in a molar ratio of 40:20:1 to the photochemical kettle Ⅰ continuously for photochemical reaction. The temperature in kettle I was 105°C, and the reaction residence time was 2 hours to synthesize o-methoxycarboxybenzylsulfonamide; o-methoxycarboxybenzylsulfonamide was continuously fed into photochemical kettle II, and 8.3kg / h of phosgene was added, The molar ratio of phosgene to benzylsulfonamide xylene solution is 1:4, the temperature in photochemical kettle II is 120°C, and the reaction residence time is 1h to synthesize o-methoxycarboxybenzylsulfoisocyanate; o-methoxycarboxybenzylsulfonate The butyl isocyanate continuously enters the light removal tower, and the n-butyl isocyanate and xylene that are removed are returned to the photochemical kettle Ⅰ for recycling. The excess phosgene passes through the cooling separator, and the separated phosgene is continuously re...

Embodiment 2

[0019] Add phosgene 33kg / h, 30% benzsulfonamide xylene suspension 127.3kg / h and catalyst n-butyl isocyanate in a molar ratio of 30:10:1 to the photochemical reactor Ⅰ continuously for photochemical reaction. The temperature in I is 110°C, the reaction residence time is 2.5h, and o-methoxycarboxybenzylsulfonamide is synthesized; o-methoxycarboxybenzylsulfonamide enters photochemical kettle II continuously, and 8.3kg / h of phosgene is added, The molar ratio of phosgene to benzylsulfonamide xylene suspension is 1.2:4, the temperature in photochemical kettle II is 125°C, and the reaction residence time is 1.5h to synthesize o-methoxycarboxybenzylsulfoisocyanate; o-methoxy Carboxybenzylsulfoisocyanate continuously enters the de-lighting tower, and the desorbed n-butyl isocyanate and xylene are returned to the photochemical reactor Ⅰ for recycling, and the excess phosgene passes through the cooling separator, and the separated phosgene is continuously returned to the photochemical rea...

Embodiment 3

[0021] Add phosgene 33kg / h, 30% benzsulfonamide xylene suspension 127.3kg / h and catalyst n-butyl isocyanate in a molar ratio of 60:20:3 to the photochemical kettle Ⅰ continuously for photochemical reaction. The temperature in Ⅰ is 115°C, the reaction residence time is 3h, and the o-methoxycarboxybenzylsulfonamide is synthesized; the o-methoxycarboxybenzylsulfonamide enters the photochemical kettle II continuously, 8.3kg / h of phosgene is added, and the Gas and benzylsulfonamide xylene suspension 1.5:4, the temperature in photochemical kettle II is 127°C, the reaction residence time is 2h, and o-methoxycarboxybenzylsulfoisocyanate is synthesized; o-methoxycarboxybenzylsulfoisocyanate enters The stripping tower, the n-butyl isocyanate and xylene that are removed are returned to the photochemical kettle Ⅰ for recycling, and the excess phosgene passes through the cooling separator, and the separated phosgene is continuously returned to the photochemical kettle Ⅰ for recycling, and t...

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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 herbicide, suitable for controlling annual and perennial broad-leaved weeds and sedges in paddy 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 in the greenhouse for 8-10 hours, and steam the xylene , washed with chlorobutane and dried to obtain 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. Contents of the invention [0003] In order to solve the above problems, the present invention provides a new te...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/52
CPCC07D239/52Y02P20/584
Inventor 钱圣利韩邦友邱波朱建军康进红
Owner JIANGSU KUAIDA AGROCHEM
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