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Crystallization method for continuous desolvation production of glyphosate by using glycocoll method

A technology of glycine method and glyphosate, applied in the field of control, can solve the problems of product quality, occupational health, adverse effects of storage and transportation, low content of glyphosate dry powder, small crystal grains, etc., and achieve large crystal grains and long crystallization time The effect of short length and large stacking ratio

Active Publication Date: 2012-06-13
CAC NANTONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the traditional crystallization process method is used, the crystallization temperature is often not studied and controlled, and a slight deviation in the crystallization process will result in a low final glyphosate dry powder content (about 95% in the traditional method), small grains, and easy to raise dust. Quality, occupational health and storage have all had adverse effects

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] In the pilot scale, preheat an empty 300L crystallizer to 90°C, then fill it with glyphosate crystal liquid, keep the stirring speed at 40rpm, and raise the temperature of the crystallizer to 95°C within 20 minutes; then stir Reduce the speed to 20 rpm, control the temperature of the crystallization kettle at 100°C, and continue the reaction for 3 hours; then control the stirring speed to 30 rpm, and raise the temperature of the crystallization kettle to 110°C within 30 minutes; keep the stirring speed at 30 rpm, and control the temperature of the crystallization kettle React at 115°C for 2h; add 75kg of deionized water and 75kg of potassium hydroxide with a concentration of 20% by weight to the crystallization solution, control the stirring speed at 20rpm, and reduce the temperature of the crystallization kettle to 60°C within 3h; Keep the stirring speed at 20 rpm, and reduce the temperature of the crystallization kettle to 20°C within 3 hours. The entire process is con...

Embodiment 2

[0014] In a large production facility, the empty 10m 3 Preheat the crystallization kettle to 92℃, then fill it with glyphosate crystallization solution, keep the stirring speed at 50rpm, and raise the temperature of the crystallization kettle to 98°C within 30 minutes; then reduce the stirring speed to 20rpm to control the crystallization kettle The temperature is at 105°C and the reaction is continued for 3.5h; then, the stirring speed is controlled to 35rpm, and the temperature of the crystallization kettle is raised to 115°C within 35min; the stirring speed is maintained at 35rpm, the temperature of the crystallization kettle is controlled at 115°C, and the reaction is 3h; Add 2800kg of deionized water and 3000kg of sodium hydroxide with a concentration of 30% by weight to the crystallization solution, control the stirring speed at 20rpm, and reduce the temperature of the crystallization kettle to 65℃ within 4h; finally keep the stirring speed at 25rpm at 3.5 The temperature ...

Embodiment 3

[0016] In a large production facility, the empty 10m 3 Preheat the crystallization kettle to 95°C, then fill it with glyphosate crystallization solution, keep the stirring speed at 60rpm, and raise the temperature of the crystallization kettle to 100°C within 40 minutes; then reduce the stirring speed to 25rpm to control the crystallization kettle The temperature is 110℃, and the reaction is continued for 4h; then, the stirring speed is controlled to 40rpm, and the temperature of the crystallization kettle is raised to 117℃ within 40min; the stirring speed is maintained at 40rpm, the temperature of the crystallization kettle is controlled at 117℃, and the reaction is 4h; Add 3000kg of deionized water and 3000kg of sodium carbonate with a concentration of 40% by weight to the solution, control the stirring speed at 25rpm, and reduce the temperature of the crystallization kettle to 60℃ within 4h; finally keep the stirring speed at 25rpm, The temperature of the crystallization kett...

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Abstract

The invention relates to a crystallization method for continuous desolvation production of glyphosate by a using glycocoll method, comprising the following steps of: adding glyphosate crystalline liquid in a crystallization kettle, rising the temperature of the crystallization kettle to 95-100 DEG C within 20-40 min; controlling the stirring speed at 20-25 rpm and the temperature of the crystallization kettle at 100-110 DEG C and reacting for 3-4 h; adjusting the stirring speed to 30-40 rpm, stirring for 30-40 min, and rising the temperature of the crystallization kettle to 110-115 DEG C; then controlling the temperature of the crystallization kettle at 115-117 DEG C and reacting for 2-3 h; adding deionized water and alkali in the crystalline liquid, controlling the stirring speed at 20-25 rpm, stirring for 6-8 h and reducing the temperature of the crystallization kettle to 20-30 DEG C . The glyphosate obtained in the invention has the dry powder content of 96-98 percent and stable quality; the solid glyphosate has high yield, large crystal grain, even particle size distribution, shorter crystallization time and is beneficial to improving the output in unit time.

Description

Technical field [0001] The invention relates to a control method, in particular to a crystallization method for producing glyphosate by continuous desolvation by a glycine method. Background technique [0002] By the end of 2008, 70% of the country’s 400,000 tons of glyphosate production process used the glycine process route. The traditional process of this route is intermittent desolventization and intermittent crystallization. If the traditional crystallization process is used, the crystallization temperature is often not studied and controlled. A slight deviation in the intermediate crystallization process will result in a low content of the final dry glyphosate powder (the content of the traditional method is about 95%), small crystal grains, and easy dust generation. Quality, occupational health and storage and transportation have all brought adverse effects. In order to improve the efficiency of production equipment, major manufacturing companies have successively develo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38B01D9/02
Inventor 邵佳礼卞进平张大俊王海水田晓宏
Owner CAC NANTONG CHEM
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