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Method for producing hydrogen phosphide by utilizing phosphorous acid pyrolysis

A technology of phosphine and phosphorous acid, applied in phosphine and other directions, can solve problems such as strong corrosion of reaction equipment, and achieve the effects of low reaction temperature, high product recovery rate and low energy consumption

Active Publication Date: 2013-09-25
南京韦福化工技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] However, this method requires a higher temperature, which usually needs to reach about 350°C. At this high temperature, the concentrated acid is also very corrosive to the reaction equipment. For this reason, the patented technology uses a graphite reactor.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Preparation of Platinum Carbon Catalyst

[0023] 1) Preparation of activated carbon support

[0024] Sieve 200-300 mesh activated carbon, add 5g of activated carbon and 45ml17%HNO into a three-necked flask 3 The solution (solid-liquid mass ratio is 1:10) was stirred and refluxed at 90-100°C for 3 hours, washed with distilled water until neutral, filtered, and dried at 110°C to obtain the activated carbon carrier.

[0025] 2) Preparation of platinum-carbon catalyst

[0026] Add 0.12g of carrier and 1.8ml of distilled water into a 50ml three-necked flask, add 0.19ml of chloroplatinic acid solution (31.65mg / ml (c=0.0772mol / l) equivalent to 5%Pt / Ac) under stirring, and heat up to 80°C Stir for 2 hours, then cool down to 40°C, add 0.2ml of formic acid, stir for 0.5h; dropwise add NaOH solution (0.1ml / L) to pH=8~9, raise the temperature to 80°C to promote the reduction; until Pt (IV ) was completely reduced; the reducing solution was filtered and washed several times with ...

Embodiment 2

[0028] In a 250ml three-necked flask, add 200g of phosphorous acid raw material (1mol) with a purity of 93%, and add 0.372g of a platinum carbon catalyst with a platinum content of 5w / w% prepared in Example 1. The weight ratio of platinum and phosphorous acid is 1 / 10,000 one. After purging the reaction system thoroughly with nitrogen, maintain a small nitrogen flow rate, and raise the temperature to 200 °C under stirring. Phosphine begins to be produced and enters the collection bottle along with the nitrogen flow. The collection bottle is filled with 1000ml of absorption solution (composed of 37w / w% formaldehyde and 10w / w% hydrochloric acid). After the collection bottle absorbs all the phosphine produced, its total phosphorus content is determined to be 5.1 g of phosphorus. In theory, 1 mol of phosphorous acid can generate 0.25 mol of phosphine, containing 7.75 g of phosphorus, which indicates that the yield of phosphine is 65.8%.

Embodiment 3

[0030] In a 250ml three-necked flask, add 84g of phosphorous acid raw material (1mol) with a purity of 98%, and add 1.64g of the platinum carbon catalyst with a platinum content of 5w / w% prepared in Example 1. The weight ratio of platinum and phosphorous acid is 1 / 1000 one. After purging the reaction system thoroughly with nitrogen, maintain a small nitrogen flow rate, and raise the temperature to 160°C under stirring. Phosphine begins to be produced and enters the collection bottle along with the nitrogen flow. The collection bottle is filled with 1000ml of absorption solution (composed of 37w / w% formaldehyde and 10w / w% hydrochloric acid). After the collection bottle absorbed all the phosphine produced, its total phosphorus content was determined to be 6.3g phosphorus. In theory, 1 mol of phosphorous acid can generate 0.25 mol of phosphine, containing 7.75 g of phosphorus, which indicates that the yield of phosphine is 81.3%.

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Abstract

The invention discloses a method for producing hydrogen phosphide by utilizing phosphorous acid pyrolysis. A platinum-carbon catalyst is utilized for pyrolyzing phosphorous acid at 150 DEG C-200 DEG C, so that high-purity hydrogen phosphide is obtained. The method for producing hydrogen phosphide by utilizing phosphorous acid pyrolysis disclosed by the invention is low in reaction temperature, small in energy consumption, high in product yield and lower in corrosion to the device.

Description

technical field [0001] The invention relates to a method for preparing phosphine, in particular to a method for producing phosphine by pyrolysis of phosphorous acid. 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 generate phos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/06
Inventor 王瑞敏张雅琴江卓贤
Owner 南京韦福化工技术有限公司
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