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Method for purifying phosphine by-product and application method of phosphine by-product

A technology of phosphine and by-products, applied in the directions of phosphine, chemical instruments and methods, separation methods, etc., can solve the problems of unrealized industrialized production of trialkyl phosphine, high price, etc., achieve high value-added utilization, reduce The effect of production costs

Active Publication Date: 2010-02-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] my country has not yet realized the industrialized production of trialkylphosphine, and all the required products are imported from the above-mentioned companies, which are expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] The purification of embodiment 1 phosphine gas

[0045] The phosphine gas generated during the reaction of sodium hypophosphite is passed into the bottom of the water-sealed tank with a depth of 2m through the gas output pipe, and the phosphorus slag and other impurities brought out by the phosphine from the reactor are initially filtered, and then the gas Pass the gas outlet pipe on the top of the water seal tank into a gas purifier filled with 30% sodium hydroxide solution for further purification. The gas outlet pipe is inserted 1m below the sodium hydroxide liquid level, and the purified gas enters the gas-water separator for separation , the resulting dry gas is input into the phosphine storage tank for use.

Embodiment 2

[0046] Embodiment 2 batch method synthesizes tributylphosphine

[0047] In a 10L autoclave, add 5L of azobisisobutyronitrile xylene solution, charge 51g (1.5mol) of phosphine and 252g (4.5mol) of butene-1, the mixture of phosphine and butene-1 The ratio is 1:3, and then the reaction is carried out by raising the temperature. When the temperature in the reactor rises to 110° C. and the pressure no longer drops, the heating is stopped and cooled to room temperature. The liquid in the reaction kettle is introduced into the distillation device for whole material, and the solvent xylene and light components are removed by atmospheric distillation first. The remaining product was distilled with an oil pump under reduced pressure to obtain 275 g of a colorless liquid product, the yield was 91% based on butene-1, and mass spectrum and NMR showed that it was consistent with the title compound.

Embodiment 3

[0048] Embodiment 3 batch method synthesizes tripropylphosphine

[0049] Add 5L xylene solution of azobisisobutyronitrile in a 10L autoclave, fill with 51g (1.5mol) of phosphine and 126g (4.5mol) of propylene, then raise the temperature to start the reaction, the temperature in the autoclave will increase To 110°C, stop heating when the pressure no longer drops, cool to room temperature, discharge the material, distill off the solvent toluene under reduced pressure, and distill the remaining product under reduced pressure with an oil pump to obtain 166 g of the product colorless liquid, with a yield of 88%, as shown by mass spectrum and NMR Consistent with the title compound.

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Abstract

The invention relates to a method for purifying a phosphine by-product in a process of producing sodium hypophosphite, and a method for synthesizing trialkyl phosphine by using the phosphine by-product. The method for purifying the phosphine by-product comprises the following steps that: 1) phosphine tail gas produced in a sodium hypophosphite reactor is drawn out from a tail gas exhaust port at the upper end of the reactor, and then naturally passes through a water seal tank by means of the pressure produced by a water seal in the water seal tank; 2) the gas passing through the water seal tank enters a water seal purifier filled with sodium hydroxide aqueous solution for purification; and 3) the phosphine gas purified by the purifier enters a gas-water separator to carry out gas-water separation so as to obtain a dried gas. The method provided by the invention realizes high added value utilization of the phosphine by-product, and greatly reduces the production cost of the trialkyl phosphine.

Description

technical field [0001] The invention relates to a method for purifying by-product phosphine in the process of producing sodium hypophosphite and a method for synthesizing trialkylphosphine by using the by-product phosphine. Background technique [0002] Sodium hypophosphite is a raw material for electroplating. With the development of electroplating industry, it has become an important product of inorganic phosphorus chemical industry. In recent years, the demand in the international market has been increasing at a rate of 10% to 15% every year. In the production process of sodium hypophosphite, a large amount of highly toxic by-product - phosphine is inevitably produced, and about 20% to 25% of the yellow phosphorus used in the production is converted into phosphine. According to the current annual output of 30,000 tons of sodium hypophosphite in my country, the amount of by-product phosphine is greater than 6,000 tons. At present, in the production of sodium hypophosphite...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/06B01D53/00C23C18/00
Inventor 余伟发李本高
Owner CHINA PETROLEUM & CHEM CORP
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