Phosphine preparation method

A technology of phosphine and yellow phosphorus, which is applied in the direction of phosphine, etc., can solve the problems of increasing production costs and large amounts of phosphoric acid, and achieve the effects of reducing waste discharge, increasing yield, and reducing raw material consumption

Inactive Publication Date: 2013-08-21
江苏先锋生物基技术研究中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method improves the yield of phosphine, but requires a large amount of phosphoric acid, whic

Method used

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Embodiment 1

[0021] 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, the pressure is slightly higher than atmospheric pressure; stir 4.0g of sodium hydroxide solution with a mass percentage concentration of 50% 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 pressure to obt...

Embodiment 2

[0023] 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

[0025] 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 Wash with a small amount of isopropanol, and evaporate the filtrate to dryness under reduced pressure to obtain 3.0 g of a viscous mixed ac...

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Abstract

The present invention relates to a phosphine preparation method, which comprises the steps that: yellow phosphorus generates phosphine, hypophosphite and phosphite under an alkali effect, an inorganic acid is adopted to treat the hypophosphite and the phosphite to obtain a mixture of hypophosphorous acid and phosphorous acid, and the obtained mixing acid is subjected to pyrolysis to produce phosphine and a by-product phosphoric acid. According to the method, the by-products of the whole process are the sodium salt and phosphoric acid so as to reduce waste emission, substantially increase the yield of phosphine, and increase the highest yield by 50-68% compared with the highest yield of the conventional alkali process.

Description

technical field [0001] The invention relates to a method for preparing phosphine from yellow phosphorus. Background technique [0002] Phosphine is an important raw material for the industrial synthesis of alkylphosphine. At the same time, phosphine is also an important N-type dopant source in the semiconductor industry. It is used in the preparation of epitaxial gallium phosphide materials in polysilicon chemical vapor deposition, ion implantation technology, and MOCVD technology. Materials such as phosphosilicate glass and passivation film. 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 generate phosphine and phosphoric acid: [0003...

Claims

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Application Information

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IPC IPC(8): C01B25/06
Inventor 周跃辉施春锦徐霞
Owner 江苏先锋生物基技术研究中心有限公司
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