Glyphosate synthesis process

A synthesis process, a technology of glyphosate, which is applied in the fields of compounds of Group 5/15 elements of the periodic table, chemical instruments and methods, and organic chemistry, etc. problems, to achieve the effect of reducing side reactions, saving production costs and reducing costs

Active Publication Date: 2011-03-30
SICHUAN LESHAN FUHUA TONGDA AGRO-CHEM TECH CO LTD
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Problems solved by technology

[0005] In the above-mentioned patent, after the addition reaction is completed, dimethyl phosphite is added to carry out the condensation reaction. This step of the reaction needs to be carried out under anhydrous conditions. The anhydrous condition cannot be fully satisfied, and the control of moisture has no reduction measures in the current process, only the moisture in the raw material can be controlled to control the moisture in the reaction system. Therefore, the condensation reaction yield is affected, especially the consumption of dimethyl phosphite reacts with water to form phosphorous acid

Method used

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Experimental program
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Effect test

Embodiment 1

[0033] Take 650 grams of methanol; 198 grams of triethylamine; put it into a 3000 ml four-neck bottle, add 115 grams of paraformaldehyde under stirring, heat, control the temperature at 45 ° C, and the reaction time is 45 minutes. The reaction solution is clear and transparent; cold water bath Cool down to 38°C, add 145 grams of glycine (98.5%); the temperature rises, remove the cold water bath when it reaches 42°C, control the temperature at 42°C, and react for 21 minutes. The reaction solution is clear and transparent again. At this time, the reaction solution is transferred to Straight tube condenser equipped with potassium-type 3A molecular sieve, the lower outlet of the condenser is connected to another reaction bottle through a rubber tube, the rubber tube uses a screw clamp to control the flow rate, about 30 drops per minute, and the dripping is completed in 75 minutes. The detected moisture is 0.09% .

[0034] Add 216 grams of dimethyl phosphite through a separatory fu...

Embodiment 2

[0037] Add 6500kg of methanol to the reaction kettle; 1980kg of triethylamine, add 115g of paraformaldehyde under stirring, heat, the temperature rises to 50°C, the reaction time is 55 minutes, the reaction liquid is clear and transparent; open the coil to cool down to 40°C, add glycine (98.5%) 1450kg; the temperature rises, adjust the amount of cold water to control the temperature at 44°C, and the reaction time is 15 minutes. The reaction liquid is clear and transparent again. Open the circulation dehydration system connected with the circulation pump and the sodium-type 4A molecular sieve dehydration tower to maintain the circulation reaction for 50 Minutes, the detected moisture is 0.1%.

[0038] Add 2159.5 kg of dimethyl ester; turn on the coil for 5°C water cooling, control the temperature not to exceed 54°C, and react at 54°C for 100 minutes. The reaction liquid is clarified, the circulation pump is stopped, and the feed liquid is transferred to the hydrolysis kettle fo...

Embodiment 3

[0042] A. Depolymerization reaction: Depolymerize methanol, triethylamine and paraformaldehyde at 45°C for 45 minutes to obtain a depolymerization liquid; the molar ratio of methanol, triethylamine and paraformaldehyde is 5.0:0.5:1 ;

[0043] B. Addition reaction: After cooling down to 38°C, add glycine with a mass fraction of 98.5% to the depolymerization solution for addition reaction, and react at 42°C for 15 minutes until the addition reaction liquid is clear and the solid disappears; The addition is that the mol ratio with triethylamine in step A is 1:1;

[0044] C. Cyclic dehydration treatment and regeneration of dehydrating agent: While continuing the addition reaction of the clarified addition reaction liquid, use 3A molecular sieve to circulate dehydration treatment to obtain dehydration addition liquid; 3A molecular sieve is regenerated with nitrogen at 100°C, The treated nitrogen is condensed to recover methanol and triethylamine, and the tail gas is emptied;

[0...

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Abstract

The invention relates to a gyphosate synthesis process, which comprises the steps of depolymerization, addition, condensation, hydrolyzation, crystallization and the like. In the invention, for solving the problem that it is difficult to realize a water-free condition in the condensation for synthesizing the gyphosate, a dehydration device is used in the addition and condensation processes for dehydrating the reaction solution, reduce the water content of the reactants and the consumption of dimethyl phosphate. Thus, the reaction yield is improved, raw materials are saved and cost is reduced.

Description

technical field [0001] The present invention relates to a kind of production technique of glyphosate, more specifically, the present invention relates to a kind of synthesis technique of glyphosate. Background technique [0002] Glyphosate (glyphosate), scientific name N-(phosphonomethyl) glycine, N-(phosphonomethyl) glycine, is an organophosphorus herbicide. The herbicidal properties of glyphosate were discovered by D.D. Baird in the United States in 1971, and developed and produced by Monsanto. By the 1980s, it had become an important variety of herbicides in the world. Glyphosate is a systemic chronic broad-spectrum herbicide that mainly inhibits enolacetonyl shikimelin phosphate synthase in the body, thereby inhibiting the conversion of shikime to phenylalanine, tyrosine and tryptophan. Transformation, which interferes with protein synthesis leading to plant death. Glyphosate is absorbed by the stems and leaves and then transmitted to various parts of the plant. It can...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38
Inventor 姜永红
Owner SICHUAN LESHAN FUHUA TONGDA AGRO-CHEM TECH CO LTD
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