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PMIDA preparation method

A technology of bisglyphosate and Celsius, which is applied in the field of preparation of bisglyphosate, can solve the problems of high environmental protection pressure and low production efficiency, and achieve the effects of reducing labor costs, high production efficiency and increasing yield

Inactive Publication Date: 2017-06-23
威海韩孚生化药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims to solve the problems of high environmental protection pressure and low production efficiency in the prior art, and provides a continuous industrial preparation method of diglyphosate with high production efficiency and no environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) At first, drop into 320 kilograms of waters and start stirring in the dissolving tank, then drop into weighed iminodiacetonitrile 200kg. Control the temperature at 40°C, stir for 30 minutes, and then transfer to the high level tank of iminodiacetonitrile solution.

[0025] (2) drop into the liquid caustic soda of the mass percentage concentration 32% of 534kg in liquid caustic soda metering tank.

[0026] (3) Firstly, the above two materials are put into the continuous reactor according to the molar ratio of iminodiacetonitrile: sodium hydroxide = 1:2.2 for continuous reaction.

[0027] (4) The reaction solution continuously enters the receiving tank, and the ammonia gas produced by the reaction enters the absorption device, and the reaction is completed and the heat preservation reaction is carried out for 2 hours.

[0028] (5) be warming up to 80 degrees centigrade, decompression distillation ammonia, steam 150 kilograms of ammoniacal liquor.

[0029] (6) Cool d...

Embodiment 2

[0033] (1) At first, drop into 320 kilograms of waters and start stirring in the dissolving tank, then drop into weighed iminodiacetonitrile 200kg. Control the temperature at 50°C, stir for 30 minutes, and then transfer to the high level tank of iminodiacetonitrile solution.

[0034] (2) Drop into 538kg mass percentage concentration 32% liquid caustic soda in liquid caustic soda metering tank.

[0035] (3) First, the above two materials are put into the continuous reactor according to the molar ratio of iminodiacetonitrile: sodium hydroxide = 1:2.2 for continuous reaction, and the temperature of the heat exchanger is controlled at 50 degrees Celsius.

[0036] (4) The reaction liquid enters the receiving kettle continuously, the ammonia gas enters the absorption device, and the reaction is completed and the heat preservation reaction is carried out for 2 hours.

[0037] (5) be warming up to 80 degrees centigrade negative pressure distillation ammonia, steam 150 kilograms of am...

Embodiment 3

[0042] (1) At first, drop into 320 kilograms of waters and start stirring in the dissolving tank, then drop into weighed iminodiacetonitrile 200kg. Control the temperature at 60°C, stir for 30 minutes, and then transfer to the high tank of iminodiacetonitrile solution.

[0043] (2) drop into 530kg mass percentage concentration 32% liquid caustic soda in liquid caustic soda metering tank.

[0044] (3) First put the above two materials in a molar ratio of 1:2.2 into the continuous reactor for continuous reaction, and the temperature of the heat exchanger is controlled at 40-50 degrees Celsius.

[0045] (4) The reaction liquid enters the receiving kettle continuously, the ammonia gas enters the absorption device, and the reaction is completed and the heat preservation reaction is carried out for 2 hours.

[0046] (5) be warming up to 80 degrees centigrade negative pressure distillation ammonia, steam 150 kilograms of ammoniacal liquor.

[0047] (6) Cool down to 65 degrees Celsi...

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Abstract

The invention relates to a PMIDA preparation method, and solves the problems of high environmental protection pressure and low production efficiency in the prior art. The PMIDA preparation method comprises the following steps: taking iminodiacetonitrile as a raw material, performing continuous alkaline hydrolysis on the raw material by use of a tubular reactor to prepare iminodiacetic acid disodium salt, and collecting the reaction liquid in a receiving kettle; adding phosphorous acid, hydrochloric acid and formaldehyde into the receiving kettle of the first-step reaction liquid, controlling the temperature to be 100-180 DEG C to prepare PMIDA, and maintaining 120 DEG C backflow of the receiving kettle; cooling the reaction liquid to 80 DEG C, and adjusting the pH value to be 0-1 to obtain the final product. The PMIDA preparation method can be widely applied to the field of PMIDA preparation.

Description

technical field [0001] The invention relates to the technical field of pesticide synthesis, in particular to a preparation method of bisglyphosate. Background technique [0002] Diglyphosate is called PMIDA for short, with a molecular formula of C5H10NO7P and a molecular weight of 227.1. PMIDA is mainly used as an intermediate raw material for a series of herbicides and other chemical products, especially as an important intermediate for the large-tonnage pesticide herbicide glyphosate at home and abroad, and glyphosate is a systemic, low-toxic, low-residue , efficient, broad-spectrum herbicide, safer than other pesticides, widely used in corn, cotton, soybean, wheat and many other crops and other plants. [0003] For many years, glyphosate has always occupied the first place in the sales of pesticides in the world. The most common synthesis methods of glyphosate are the glycine method and the IAD method. The glycine method produces more waste water, and the pressure on en...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38
CPCC07F9/3808
Inventor 王玉亭刘文波董继波张玉超陈磊刘凯丁金鹏李帅
Owner 威海韩孚生化药业有限公司