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Method for preparing bis(2,4,4-trimethylpentyl)phosphinic acid from by-product phosphine in sodium hypophosphite production process

A technology of trimethylpentyl and phosphinic acid, applied in chemical instruments and methods, organic chemistry, compounds of elements of Group 5/15 of the periodic table, etc., can solve problems such as pollution and waste

Active Publication Date: 2016-03-16
CHANGSHU NEW TECH CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the phosphorus trichloride route can produce a large number of organophosphorus products, this route causes a lot of pollution and waste during production due to the introduction and removal of chlorine atoms
However, this method is only used for the synthesis of a small number of trialkylphosphorus

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 7000 grams of diisobutene (75% 2,4,4-trimethyl-1-pentene, 25% 2,4,4-trimethyl-2-pentene) was sucked into a stainless steel high-pressure reaction kettle. The by-product crude phosphine (hereinafter referred to as crude phosphine) from the production of sodium hypophosphite is washed with 30% NaOH solution and then enters the freeze dryer, freeze-dried at 0-3°C to remove water, and then enters the high-pressure reaction pot through the compressor . The temperature in the pot is kept at -30~-20°C. When the pressure in the kettle rose to 50 atmospheres, the vent valve was opened to keep the 50 atmospheres in the kettle. The temperature of the solution in the high-pressure reaction kettle is maintained below -20°C. After maintaining this process for 1.5 hours, the input of crude phosphine gas was stopped. The pressure was released to 40 atmospheres, and 900 grams of phosphine was absorbed in the high-pressure reaction kettle (the input total gas flow rate was 2090 grams)...

Embodiment 2

[0027] Dissolve 50 g of benzoyl peroxide in 7000 g of diisobutylene (75% 2,4,4-trimethyl-1-pentene, 25% 2,4,4-trimethyl-2-pentene). The resulting solution is sucked into a stainless steel high-pressure reaction kettle. Crude phosphine is washed with 50% NaOH solution, and then enters the freeze dryer, freeze-dried at 0-3°C to remove water, and then enters the high-pressure reaction pot through the compressor. The temperature in the kettle is maintained at -15°C~-20°C. When the pressure in the kettle rose to 60 atmospheres, the vent valve was opened to keep the 60 atmospheres in the kettle. This process was maintained for 2 hours, and the input of crude phosphine gas was stopped. The pressure in the high-pressure reaction kettle is released to 40 atmospheres, and 1361 grams of phosphine are absorbed in the high-pressure reaction kettle (3404 grams of total gas flow input). When the high-pressure reaction pot is heated to 80°C, the pressure inside the pot rises to 60-70 atmos...

Embodiment 3

[0029] Dissolve 136 g of benzoyl peroxide in 7000 g of diisobutylene (75% 2,4,4-trimethyl-1-pentene, 25% 2,4,4-trimethyl-2-pentene). The resulting solution is sucked into a stainless steel high-pressure reaction kettle. Crude phosphine is washed with 40% NaOH solution and then enters the freeze dryer, freeze-dried at 0-3°C to remove water, and then enters the high-pressure reaction pot through the compressor. The temperature in the pot is kept at -15~-20°C. When the pressure in the kettle rose to 70 atmospheres, open the vent valve to keep the pressure in the kettle. This process was maintained for 2 hours, and the input of crude phosphine gas was stopped. The pressure in the high-pressure reaction kettle is released to 40 atmospheres, and 1603 grams of phosphine are absorbed in the high-pressure reaction kettle (3730 grams of total gas flow input). Heat the high-pressure reaction kettle and keep the temperature at 80-85°C, and the pressure in the kettle rises to 60-70 atmo...

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Abstract

The invention discloses a method for preparing bis(2,4,4-trimethylpentyl) phosphinic acid from hydrogen phosphide as a byproduct in a sodium hypophosphite production process. The bis(2,4,4-trimethylpentyl) phosphinic acid is prepared by the steps of implementing alkaline cleaning to hydrogen phosphide which is a byproduct in sodium hypophosphite production and freeze-drying the hydrogen phosphide to remove water; pumping the such processed hydrogen phosphide into a high-pressure reaction kettle containing diisobutylene and an initiator through a compressor, wherein the hydrogen phosphide is absorbed by the diisobutylene while hydrogen and little nitrogen in the hydrogen phosphide, instead of being absorbed, enter a combustion furnace along with tail gas, and the purified hydrogen phosphide is subjected to free radical addition reaction with the diisobutylene in the presence of the initiator to generate bis(2,4,4-trimethylpentyl) phosphine; evaporating out residual diisobutylene and monoalkyl substitute; and oxidizing rest materials through hydrogen peroxide to obtain the bis(2,4,4-trimethylpentyl) phosphinic acid.

Description

technical field [0001] The present invention relates to the purification of sodium hypophosphite by-product phosphine and the synthesis of organic phosphorus products, in particular to the preparation of bis(2,4,4-trimethylpentyl)times from by-product phosphine in the production process of sodium hypophosphite Phosphonic acid method. Background technique [0002] Organophosphorus products containing carbon-phosphorus bonds are widely used in industry. There are two main routes for the synthesis of organophosphorus products. One is to start from phosphorus trichloride through Hooke reaction, Grignard reaction or Arbuzov reaction to generate organic phosphorus products containing carbon and phosphorus bonds. Another route is the free radical addition of phosphine or hypophosphorous acid to alkenes to generate organophosphorus products containing carbon-phosphorus bonds. Although the phosphorus trichloride route can produce a large number of organophosphorus products, this r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/30
Inventor 周跃辉叶志松傅益民
Owner CHANGSHU NEW TECH CHEM