A kind of continuous production process for preparing glufosinate-ammonium

A production process and glufosinate-ammonium technology are applied in the production process field of continuous preparation of glufosinate-ammonium, which can solve the problem of not involving glufosinate-ammonium synthesis process operation flow and process equipment, difficult recycling of by-products, and inconcentration of recovered hydrochloric acid. and other problems, to achieve the effect of continuous production of by-products, saving equipment investment, and small one-time investment in equipment

Active Publication Date: 2019-04-26
SICHUAN LESHAN FUHUA TONGDA AGRO-CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The operation time of the process is long, the equipment investment is high, the utilization rate is low, and the by-products are not easy to recycle. Since the evaporation is carried out in a single tank, the energy consumption is large, and the recovery of hydrochloric acid is not concentrated, and only less than 20% of dilute acid can be recovered. Environmental pressure Large, high cost and many other problems
[0004] In the existing patent documents related to the synthesis of glufosinate by Strecker method, such as the publication number is CN1267305, the patent name is "method and intermediate for preparing glufosinate" and the publication number is CN103374030A, and the patent name is "a method for preparing glufosinate The invention patent application for the method of ammonium phosphine and the preparation method of its intermediate” only discloses the synthesis process route of glufosinate-ammonium, and does not involve the specific operation process and process equipment of the synthesis process of glufosinate-ammonium. Therefore, based on The present situation of domestic process operation, the present invention proposes a kind of production technique based on the continuous preparation of glufosinate-ammonium of Strecker method

Method used

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  • A kind of continuous production process for preparing glufosinate-ammonium

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Experimental program
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Effect test

Embodiment 1

[0028] A production process for continuously preparing glufosinate-ammonium, comprising the following steps:

[0029] A. After mixing the phosphazene liquid with hydrochloric acid, send it to the hydrolysis tower 1, the low boiler obtained by hydrolysis completes step B, and the kettle liquid obtained by hydrolysis completes step C;

[0030] B, low boilers obtain recovery ethanol through condenser 2;

[0031] C, still liquid is sent into hydrochloric acid flasher 3, and the hydrochloric acid that removes is sent into hydrochloric acid absorber 4, and concentrated solution is sent into crystallization kettle 5;

[0032] D. The crystallization material in the crystallization tank 5 is sent into the centrifuge 6 to obtain the crude product of glufosinate-ammonium, and the centrifuged mother liquor is returned to the hydrochloric acid flasher 3.

Embodiment 2

[0034] In this embodiment, on the basis of Example 1, the temperature in the hydrolysis tower 1 in step A is limited, the temperature should be controlled at 100° C., and the pressure should be controlled at 0.02 MPa.

Embodiment 3

[0036] In this example, on the basis of Example 1, the temperature of the condenser 2 in step B is limited, and the temperature should be controlled at 40°C.

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Abstract

The invention discloses a continuous production process for preparing glufosinate, which includes the following steps: 1) mixing a phosphonitrilic liquid and hydrochloric acid and feeding the mixture into a hydrolysis column, hydrolyzing the mixture to obtain a low-boiling-point substance, and condensing the low-boiling-point substance through a condenser to recycle ethanol; 2) feeding a kettle liquid generated in the hydrolysis into a hydrochloric acid flash evaporator to separate hydrochloric acid, feeding the hydrochloric acid into a hydrochloric acid absorber and a concentrate into a crystallization kettle, and feeding a crystallized material in the crystallization kettle into a centrifuge to prepare a glufosinate crude product; 3) feeding a centrifugal mother liquid back to the hydrochloric acid flash evaporator. The continuous acidolysis method solves the defects in an acidolysis reaction in a Strecker method in our country due to intermittent production, is short in production time and high in production efficiency, is low in environment-protection load, and is low in production cost.

Description

technical field [0001] The invention relates to a continuous production process for preparing glufosinate-ammonium, specifically relates to a process system for synthesizing glufosinate-ammonium by using a continuous Strecker method, and belongs to the technical field of glufosinate-ammonium preparation. Background technique [0002] At present, the synthesis techniques of glufosinate-ammonium mainly include Abzov synthesis method, high-pressure catalytic synthesis method, Gabriel synthesis method and Strecker synthesis method, etc. Because the first three synthesis processes require expensive raw materials and harsh reaction conditions, while the Strecker method is mature, the reaction conditions are not high, and the yield can reach about 35%, which is suitable for industrial production. Therefore, most manufacturers in the world use This method synthesizes glufosinate-ammonium. [0003] The process of synthesizing glufosinate-ammonium by Strecker method is to use triethy...

Claims

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Application Information

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Patent Type & Authority Patents(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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