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Amination process for preparing butralin as chemical herbicide

A preparation process, a technology of chlorbutin, which is applied in the chemical industry, can solve the problems of low yield of chlorbutin and reduced purity, and achieve the effects of reducing the waste water treatment load, reducing the amount of CODcr, and reducing operating costs.

Inactive Publication Date: 2007-11-07
易文中
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention aims at 2,6-dinitro-p-tert-butyl chlorobenzene under strongly alkaline conditions, easily replaced by OH to generate 2,6-dinitro-p-tert-butyl phenol sodium, which is soluble in water and is Loss, so that the yield of Zhongbuling is low, the purity is reduced and other unfavorable factors

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] Embodiment 1: small test: take the input 246g99 p-tert-butylchlorobenzene processing technology as example:

[0009] Nitrification reaction: weigh 98% HNO 3 (Industrial) 396g, put in 98% H 2 SO 4 926g, in a 2000ml four-necked glass reaction bottle, cool it with Cacl refrigerant outside; continue to stir, so that the temperature of the mixed acid drops to between 0-10°C; accurately weigh 246g99 p-tert-butylchlorobenzene and start dropping for nitration Reaction, control the reaction temperature below 20°C; when the dropwise addition of pate is completed, continue to react within 25°C for 15 minutes, replace the frozen brine with a heating electric furnace, start heating, and stop stirring when the temperature rises to 95°C , static layering; take out the four-necked reaction bottle, pour the hot 2,6-dinitro-p-tert-butylchlorobenzene and mixed acid into a 2000ml separating funnel, and separate the mixed acid in the lower layer.

[0010] The treatment process for 2,6-di...

Embodiment 2

[0015] Embodiment 2: industrialized production: take input 99% 380kg p-tert-butyl chlorobenzene processing technology as example, after the nitration reaction, the processing technology to 2,6-dinitro p-tert-butyl chlorobenzene is: in 2000 liters In the amination kettle, add 800 liters of clear water, and heat to 95-100°C, continue to stir, put about 560kg of molten 2,6-dinitro-p-tert-butylchlorobenzene with mixed acid in the nitration kettle, in Put into boiling water within 5 minutes, wash with hot water for 5 minutes, then add 30% NaOH solution dropwise for neutralization; when red appears, test with pH test paper, control to PH 7-8, stop adding caustic soda dropwise; continue to stir, cool rapidly, Make 2,6-dinitro-p-tert-butylchlorobenzene into granules; stop stirring, and vacuum the upper layer of waste water; at this time, the discharged waste water is light red, has no pungent smell, and has a pH of 7-8.

[0016] The amination reaction process is: one-time input of 40k...

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PUM

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Abstract

The present invention relates to amination process for preparing butralin as chemical herbicide, and belongs to the field of chemical industry technology. The present invention includes a process of treating 2, 6-dinitro-p-tert-butyl chlorobenzene through heating in water at 85-100 deg.c, washing in boiling water, neutralizing with 30 % concentration NaOH solution to pH 7-8, cooling and other steps; and an amination process with NaHCO3 as buffering agent. The present invention can reach chemical content of 89-91 % and nitrated amine yield of 79-82 %, higher than available technology, and has less waste water treating load.

Description

technical field [0001] The invention relates to an amination process in the preparation process of the chemical herbicide secbutamyl, which belongs to the field of chemical industry. Background technique [0002] Butylline belongs to dinitroaniline chemical herbicides. In 1972, it was developed and registered by American Amchen Company. The current industrial production process of Zhongbuling generally includes: alkylation reaction, nitration reaction and amination reaction. At present, there are still two low technical indicators in the production process of Zhongbuling. One, the content of the original drug produced is on the low side, generally only between 85-86%, which affects its efficacy and safety in use. Second, the yield of Zhongbuling is low, generally between 72-73%, which affects its economic benefits and application range. In order to solve the existing problems, in the prior art, toluene is used as a solvent in the amination reaction, and progress has been...

Claims

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Application Information

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IPC IPC(8): C07C211/52C07C209/10
Inventor 易文中
Owner 易文中
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