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Production method of high-purity spermine and co-production of high-purity trimethyl thiophosphate by-product

A technology of pure trimethyl thiophosphate and trimethyl thiophosphate, which is applied in the production field of high-purity spermine and co-production of high-purity trimethyl thiophosphate by-product, and can solve the problem of difficult removal of spermine, etc. problems, to achieve the effect of simple equipment and simplified process flow

Pending Publication Date: 2021-03-26
安道麦股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to solve the problem that the by-product trimethylphosphorothioate is contained in the crude amine of the existing product after alcoholysis of thionium trichloride, which causes the subsequent isomerization reaction of spermine to be inhibited and the product acephate contained in To solve the problem of difficult removal of the by-product trimethyl thiophosphate, provide a production method with a simpler process, environmental protection, and the ability to obtain high-purity spermine and co-produce high-purity trimethyl thiophosphate as a by-product

Method used

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  • Production method of high-purity spermine and co-production of high-purity trimethyl thiophosphate by-product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 1) After preheating the product crude amine from the trichloride to 0.2 times the heat exchanger to 40 ° C, the reduced pressure rectification column is entered from the middle of the reduced pressure rectification column. Among them, the composition of the crude amine is: 80 ~ 90% by weight of the aminethromine (O, O-dimethylthiometryamide), 5 to 10% by weight of trimethyl ester and 2 to 5 wt% water, wherein Trimethyl phosphate is by-product. The amine is then produced by ammonia, catalyzed isomer, acylated, and has the final product acetamin phosphorus.

[0018] 2) Set the top of the rectification tower to -0.009MPa, the top temperature of the tower is 30 ° C, the gas phase of the reduced pressure distillation is discharged from the top of the tower, and the colored condenser is condensed, and the condensate enters the die. After the moisture was separated, the upper separated water phase was used to obtain a top-level oil phase thiophosphate trimethyl ester content was 9...

Embodiment 2

[0021] 1) After preheating the product crude amine from the trichloride and 0.2 times the water to 50 ° C, the reduced pressure rectification column is entered from the middle of the reduced pressure rectification column. The composition of the crude amine is: 80 ~ 90 wt% of the amtroine (O, O-dimethylthylphopphipamide), 5 to 10% by weight of trimethyl phthalate and 2 to 5 wt% water;

[0022] 2) Set the rectification tower top pressure to -0.010 MPa, the top temperature of the tower is 40 ° C, the gas phase of the reduced pressure distillation is discharged from the top of the tower, and the colored condenser is condensed, and the condensate enters the water supply. After the moisture was separated, the upper separated water phase was used to recover, the above the lower oil phase phosphoric acid trimethyl ester was 97.6%, and the trimethyl phthalate recovery of thiophosphate was 78%;

[0023] 3) The liquid phase of the reduced pressure distillation is discharged from the bottom o...

Embodiment 3

[0025] 1) After preheating the product crude amine from the trichloride to 0.4 times the water through the heat exchanger to 50 ° C, the reduced pressure rectification column is entered from the middle of the reduced pressure rectification column. The composition of the crude amine is: 80 ~ 90 wt% of the amtroine (O, O-dimethylthylphopphipamide), 5 to 10% by weight of trimethyl phthalate and 2 to 5 wt% water;

[0026] 2) Set the top of the rectification tower to -0.015 MPa, the top temperature of the tower is 40 ° C, the gas phase of the reduced pressure distillation is discharged from the top of the tower, and the condensate is condensed, and the condensate enters the water supply. After the moisture was separated, the upper separated water phase recovery sleeve, the above-yielded lower oil phase thiophosphate is 97.6%, and the trimethyl phthalate recovery of thiophosphate is 80%;

[0027] 3) The liquid phase of the reduced pressure distillation is discharged from the bottom of t...

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Abstract

The invention discloses a production method of high-purity spermine and co-production of a high-purity trimethyl thiophosphate byproduct. The production method comprises the following steps: mixing crude amine obtained after alcoholysis of thiophosphoryl chloride with water, preheating by a heat exchanger, and separating in a vacuum distillation tower; a gas phase is discharged from the tower topand enters a tower top condenser to be condensed, condensate enters a water segregator, a water phase separated from the upper layer is recycled and reused, and an oil phase at the lower layer is trimethyl thiophosphate with the content larger than 98%; discharging the liquid phase from the bottom of the tower, dehydrating the water-containing spermine at the bottom of the tower through a film evaporator to obtain spermine of which the content is greater than 97%, and directly recycling the gas-phase condensed water of the film evaporator. According to the production method, the marketable high-purity by-product trimethyl thiophosphate is obtained, the subsequent reaction of spermine can be normally carried out, and in addition, the trouble of removing the by-product trimethyl thiophosphate from the final product acephate of the subsequent reaction and the environmental pollution caused by removing the by-product trimethyl thiophosphate are avoided; and the method is an environment-friendly and economic production process.

Description

Technical field [0001] The present invention relates to the field of chemical synthesis, and specifically, a method for producing a high-purity amine amine and a trimethyl ester by high purity thiophosphate. Background technique [0002] Acetaninophosamine is a widely used organophosphorus insecticide at home and abroad, and is also one of the largest production tons of production in my country. At present, most of the domestic trichloroalkaliodide is more alcohol, ammonia, catalyzed isomer, and recrystis, produce product acetaminophosphorus. After the trichlorohydric phosphorus, the end-stage intermediate of its tandem reaction is a crude amine. The composition of the crude amine is: 80-90 wt% O, O-dimethylthiometryramide (commonly known as steriline), 5-10% by weight O, O, O-phosphomethane (hereinafter referred to as three Esterium and 2-5 wt% of water, wherein trimethyl phthalate is by-product. The spermine is reactes ammonia, catalyzed isomer, and acylated, the final product ...

Claims

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Application Information

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IPC IPC(8): C07F9/17C07F9/24
CPCC07F9/2408C07F9/17
Inventor 范锦龙王现刚陈艳李卫陈建国薛光才周用义孙梅
Owner 安道麦股份有限公司
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