Addition process of hydrocyanic acid

A hydrocyanic acid and addition technology, applied in chemical instruments and methods, organic chemistry, compounds of Group 5/15 elements of the periodic table, etc., can solve problems such as difficult handling, and achieve increased reaction yield, improved solubility, The effect of shortening the one-pot reaction time

Active Publication Date: 2017-12-01
SICHUAN LESHAN FUHUA TONGDA AGRO-CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that this process adds equimolar ammonium chloride. At the same time, in the water phase reaction, 5% of the ammonia gas is still taken into the next process after being recovered, and reacts with hydrochloric acid to form ammonium chloride. These ammonium chlorides are finally converted into Solid waste is separated in the form of water and organic impurities, and it is extremely difficult to deal with

Method used

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  • Addition process of hydrocyanic acid

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Effect test

Embodiment 1

[0035]A hydrocyanic acid addition process, in the cyanamide reaction kettle, put in 1,2-dichloroethane as a solvent, and then put in sodium cyanide solid, so that the input sodium cyanide solid and 1,2-dichloroethane After ethyl chloride is uniformly mixed at a molar ratio of 0.15:1, the molar ratio of sodium cyanide solid to phosphonic aldehyde is 0.98:1 and then put into the phosphonic aldehyde liquid, so that the sodium cyanide solid and phosphonic aldehyde liquid are at 1, 2 -After dissolving in ethylene dichloride, pass into ammonia gas in the suspension of this solution, control the feeding rate of ammonia gas to be 20kg / h, the feeding time is 2.5h, the solution in the still that makes becomes clear and transparent. Can.

[0036] Control the above reaction time to 4 hours, and the reaction temperature is 30°C. After the reaction is completed, carry out vacuum distillation on the materials after the reaction at -0.06Mpa and 40°C to distill out 1,2-dichloroethane and untre...

Embodiment 2

[0038] A hydrocyanic acid addition process, in the cyanamide reaction kettle, put in 1,2-dichloroethane as a solvent, and then put in sodium cyanide solid, so that the input sodium cyanide solid and 1,2-dichloroethane After ethyl chloride is evenly mixed at a molar ratio of 0.2:1, the molar ratio of sodium cyanide solid to phosphonic aldehyde is 0.98:1, and the phosphonic aldehyde solution is put into it, so that the sodium cyanide solid and phosphonic aldehyde liquid are at 1, 2 - After dissolving in ethylene dichloride, feed ammonia gas into the suspension of the solution, control the feeding rate of ammonia gas to 40kg / h, and the feeding time is 3h, so that the solution in the kettle becomes clear and transparent .

[0039] Control the above reaction time to 6 hours, and the reaction temperature is 40°C. After the reaction is completed, the material after the reaction is subjected to vacuum distillation at -0.08Mpa and 50°C to distill 1,2-dichloroethane and untreated After...

Embodiment 3

[0041] A hydrocyanic acid addition process, in the cyanamide reaction kettle, put in 1,2-dichloroethane as a solvent, and then put in sodium cyanide solid, so that the input sodium cyanide solid and 1,2-dichloroethane After ethyl chloride is uniformly mixed at a molar ratio of 0.19:1, the molar ratio of sodium cyanide solid to phosphonic aldehyde is 0.98:1, and the phosphonic aldehyde solution is put into it, so that the sodium cyanide solid and phosphonic aldehyde liquid are at 1, 2 -After dissolving in ethylene dichloride, pass into ammonia gas in the suspension of this solution, control the feeding rate of ammonia gas to be 30kg / h, and the feeding time is 2.6h, make the solution in the kettle become clear and transparent. Can.

[0042] Control the above reaction time to 5 hours, and the reaction temperature is 35°C. After the reaction is completed, carry out vacuum distillation on the materials after the reaction at -0.07Mpa and 45°C to distill out 1,2-dichloroethane and un...

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Abstract

The invention discloses an addition process of hydrocyanic acid, which includes the steps of: uniformly mixing a sodium cyanide solid with a solvent, 1,2-dichloroethane, and adding a phosphine aldehyde liquid and feeding ammonia gas; when the reaction is finished, recycling the 1,2-dichloroethane and non-reacted ammonia gas to prepare a phosphine nitrile solution. With the 1,2-dichloroethane as a solvent, the sodium cyanide solid dispersed therein is reacted with the phosphine aldehyde liquid and ammonia gas to obtain the phosphine nitrile solution. The reaction is free of addition of ammonium chloride; and ammonia in the phosphine nitrile solution, after the 1,2-dichloroethane and ammonia are recycled completely, is eliminated completely and is free from being carried into the next step, so that a glufosinate product is greatly reduced in generation quantity of ammonium chloride, which is less than that in production of 1 ton of glufosinate in a conventional process by about 700 kg.

Description

technical field [0001] The invention relates to a hydrocyanic acid addition process, specifically relates to the nitrile amination reaction process in the Strecke process for synthesizing glufosinate-ammonium, and belongs to the technical field of glufosinate-ammonium preparation. Background technique [0002] At present, the synthesis process of amino acids and their derivatives basically adopts the Strecker process. Because the reaction conditions are not high, it is suitable for industrial production. Therefore, most amino acid manufacturers use this method to synthesize, such as the herbicide glufosinate-ammonium. The process of synthesizing glufosinate-ammonium by Strecker method is to use triethyl phosphite as raw material, go through disproportionation reaction, formatting reaction, methylation reaction, addition reaction, nitrile amination reaction, acidolysis reaction, ammonization reaction and purification The eight-step reaction such as reaction obtains the origin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
CPCC07F9/301
Inventor 阮冬冬潘飞刘帆王梅
Owner SICHUAN LESHAN FUHUA TONGDA AGRO-CHEM TECH CO LTD
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