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Method for treating glyphosate mother liquid

A technology of glyphosate mother liquor and processing method, applied in the field of glyphosate mother liquor treatment of catalyst triethylamine recovery rate, can solve the problems of rising production cost, high consumption of triethylamine, reduced possibility of industrialized production, etc. The effect of slow heat transfer efficiency, low production intensity and high energy consumption

Inactive Publication Date: 2008-06-04
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Abstract
  • Description
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Problems solved by technology

This method fundamentally eradicates the harm brought by 10% glyphosate sodium saline solution, but this invention does not make efforts in the recovery rate of triethylamine, and the recovery rate only reaches about 80%, so the consumption of triethylamine High, leading to an increase in production costs and reducing the possibility of industrialized production, it is an urgent problem to be solved for industrialized production

Method used

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  • Method for treating glyphosate mother liquid

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Experimental program
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Effect test

Embodiment 1

[0029] in the attached figure 1 In the process of glycine method synthesis, the mother liquor and ammonia gas filtered out of glyphosate crystallization are placed in the static mixer 1, and the glyphosate mother liquor is now treated with ammonia.

[0030] The flow rate of the glyphosate mother liquor is 166.7kg / h, adjust the flow rate of the ammonia gas, neutralize the two in a static mixer, and control the temperature within the range of -5°C to 15°C. The neutralization solution flowing out of the outlet of the static mixer directly enters the gravity chromatograph 2 for stratification, the amine phase of the upper layer enters the triethylamine tank 7 for dehydration treatment, and then returns to the glyphosate synthesis process, and the water phase of the lower layer enters the large mother liquor tank 3. Then the pump enters the rectification tower 4 for rectification, and the discharge from the tower kettle goes to the mother liquor concentration process. After concent...

Embodiment 2

[0034] Add 300g 99% methanol into a reactor equipped with a stirrer, first add 60g 98% triethylamine under stirring, then add 40g 93% paraformaldehyde, keep warm at 40°C for 60 minutes; add 45g 97.5% glycine, 50 Insulate at ℃ for 60 minutes; add 80g 98% dimethyl phosphite, and insulate at 65℃ for 95 minutes; cool the material to 30℃, add 200g 30% hydrochloric acid, heat up to 120℃, add 25g water when cooling to 95℃, drop Add 43g of 25% ammonia solution, so that the pH is 0.9; cool and crystallize, filter and dry to obtain 79.2g of glyphosate technical substance, the content is 95.2%, and the yield is 76.3%. The filtrate is the glyphosate mother liquor.

[0035]Take all the glyphosate mother liquor synthesized above, feed 25.2g of ammonia gas, so that the pH is 7.6, and control the process temperature between 60°C and 110°C. The mother liquor was left to stand for stratification, and 23.4g of triethylamine was obtained in the upper layer. The mother liquor in the lower layer wa...

Embodiment 5

[0037] Get all the glyphosate mother liquor prepared by the operation method in Example 2, feed 48.3g of ammonia gas, so that the pH is 10.5, and control the process temperature between 20°C and 60°C. The mother liquor was left to stand for stratification, and 44.8g of triethylamine was obtained in the upper layer. The mother liquor in the lower layer was distilled and the fraction below 110°C was collected. Ethylamine, which is equivalent to a total recovery rate of 85.9%; after the remaining mother liquor is distilled under reduced pressure, it is cooled to normal temperature, and filtered to obtain 30.4 g of ammonium chloride crystals (content 84.0%), and the concentrated mother liquor content is 3.5%.

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Abstract

The invention provides a treatment method of mother liquor of glyphosate, which is applicable in large-scale production and has low cost and can improve the recovery rate of triethylamine that is an activator and is used in the synthesis of glyphosate, wherein, in the technical process that the glyphosate mother liquor adopts a glycin method to prepare the glyphosate, the acidic hydrolysis of glyphosate is finished and the pure crystalloid of the glyphosate precipitates in the system, then the residual of the mother liquor is the mother liquor of the glyphosate. By controlling the charge-in mixture ratio and system temperature and adjusting the pH to a certain range, the method of the invention can obtain the triethylamine simply in a high recovery ratio which normally can reach over 90 percent.

Description

technical field [0001] The invention relates to a treatment method of glyphosate mother liquor, in particular to a treatment method of glyphosate mother liquor which effectively improves the recovery rate of triethylamine, a catalyst used for glyphosate synthesis. Background technique [0002] As we all know, glyphosate is a high-efficiency, broad-spectrum, low-toxicity, and safe organophosphorus herbicide, which is very effective in the control of perennial deep-rooted weeds and is widely used in agriculture, forestry, animal husbandry, and horticulture. [0003] There are many production methods of glyphosate, and currently the glycine method and the IDA method (diglyphosate oxidation method) are commonly used production processes. Glyphosate is usually produced by the glycine method in China. This method has the advantages of low raw material cost, high yield of raw powder, and high product purity. However, when glyphosate is produced by this method, a large amount of Cl-...

Claims

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Application Information

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IPC IPC(8): C07F9/38C07B63/00
Inventor 王伟周曙光邵振伟秦大伟陈静刘侠胡辉李丽娟宋学斌佘慧玲
Owner ZHEJIANG XINAN CHEM INDAL GROUP
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