Preparation method of phosphine

A technology of phosphine and yellow phosphorus, applied in the direction of phosphine, phosphoric acid, phosphorus oxyacid, etc., can solve the problems of increasing production cost and a large amount of phosphoric acid, reducing waste discharge, improving yield, and reducing raw material consumption effect of dosage

Inactive Publication Date: 2013-10-09
南京宏福高端膦技术研发中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method improves the yield of phosphine, but requires a large amount of phosphoric acid, which increases the production cost, and the treatment of the pyrolysis product is also a big problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 2.0g of yellow phosphorus and 20g of methanol into the reaction flask, replace the air in the reaction flask with nitrogen and maintain the nitrogen flow, and the pressure is slightly higher than atmospheric pressure; 4.0g of sodium hydroxide solution with a mass percentage concentration of 50% is stirred at 25°C While slowly dropping into the reaction flask, slowly raise the temperature to 60°C, the color of the reaction solution turns reddish brown, and phosphine is released. After the sodium hydroxide solution is added dropwise, continue to stir for 5 hours, and the reaction mixture changes from reddish brown to Earthy yellow, pH 9; add 5.2g of 36% hydrochloric acid to make the pH of the mixture 2; add 15g of absolute ethanol, stir at 50°C for 1 hour to obtain a beige liquid-solid mixture; filter the solid mixture at room temperature , the filter cake was washed with a small amount of absolute ethanol, and the filtrate was evaporated to dryness under reduced press...

Embodiment 2

[0025] Add 2.0g of yellow phosphorus and 20g of ethanol into the reaction flask, replace the air in the reaction flask with nitrogen and maintain the nitrogen flow; slowly drop 4.0g of sodium hydroxide solution with a mass percentage concentration of 50% into the reaction flask while stirring at 25°C In the flask, slowly increase the temperature to 50°C, the color of the reaction solution turns reddish brown, phosphine is released, and after the sodium hydroxide solution is added dropwise, continue to stir for 4 hours, the reaction mixture changes from reddish brown to khaki, and the pH is 8 Add 2.6g of sulfuric acid with a concentration of 98% to make the pH of the mixture 1; add 15g of isopropanol and stir for 0.5 hours at 40°C to obtain a beige liquid-solid mixture; filter the solid mixture at room temperature, and filter the cake with a small amount of isopropanol Wash with propanol, and evaporate the filtrate to ethanol under reduced pressure to obtain 2.7 g of a viscous m...

Embodiment 3

[0027] Add 2.0g of yellow phosphorus and 20g of isopropanol into the reaction flask, replace the air in the reaction flask with nitrogen and maintain the nitrogen flow; slowly drop 4.0g of sodium hydroxide solution with a mass percentage concentration of 50% at 30°C while stirring Put it into the reaction flask, slowly increase the temperature to 60 ° C, the color of the reaction solution turns reddish brown, phosphine is released, and after the sodium hydroxide solution is added dropwise, continue to stir for 6 hours, the reaction mixture changes from reddish brown to khaki, and the pH 9; add 4.0 g of phosphoric acid with a concentration of 85% to make the pH of the mixture 1; add 15 g of isopropanol and stir at 50°C for 0.5 hours to obtain a beige liquid-solid mixture; filter the solid mixture at room temperature, and filter the cake with A small amount of isopropanol was washed, and the filtrate was evaporated to dryness under reduced pressure to obtain 3.0 g of a viscous mi...

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PUM

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Abstract

The invention relates to a preparation method of phosphine. The preparation method comprises the following steps of: generating phosphine, hypophosphite and phosphite from yellow phosphorus under the action of a base, processing the hypophosphite and the phosphite by using an inorganic acid to obtain a mixture of hypophosphorous acid and phosphorous acid, and performing pyrolysis on the mixed acid to generate the phosphine and a byproduct, namely phosphoric acid. During the whole technological process of the preparation method, the byproducts, namely a sodium salt and the phosphoric acid are produced, the emission of wastes is reduced, and the yield of the phosphine is greatly improved by 50-68.3% in comparison with the highest yield of a traditional base method process.

Description

technical field [0001] The invention relates to a method for preparing phosphine, in particular to a method for preparing phosphine by using yellow phosphorus as a raw material. Background technique [0002] Phosphine is an important raw material for the industrial synthesis of alkylphosphines. At the same time, phosphine is also an important N-type dopant source in the semiconductor industry. It is used in polysilicon chemical vapor deposition, ion implantation technology and MOCVD technology to prepare epitaxial gallium phosphide. materials, phosphosilicate glass, and passivation films. Bottled mixed gas of phosphine and carbon dioxide is gradually replacing aluminum phosphide as a fumigant for grain warehouses. Phosphine is currently produced in industry by two main processes, one is the acid process and the other is the alkali process. In the acid process, yellow phosphorus undergoes disproportionation under the action of acid and at a temperature as high as 280°C to g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/06C01B25/20
Inventor 张雅琴王瑞敏江卓贤
Owner 南京宏福高端膦技术研发中心有限公司
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