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Loaded type catalyst for preparing elemental phosphorus and preparation method thereof

A supported catalyst, elemental phosphorus technology, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of easy crystallization catalytic activity, low conversion rate, complex process, etc. Effects of activity and selectivity, large aspect ratio, and low thermal decomposition temperature

Inactive Publication Date: 2009-09-09
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Decomposing phosphine under catalytic conditions to prepare high-purity phosphorus is the most commonly used method. The catalysts currently used generally have disadvantages such as complicated processes, low conversion rates, high energy consumption, and poor stability.
[0003] As a new type of catalytic material, amorphous alloy is favored by catalytic workers. It will be an ideal choice if amorphous alloy is used as a catalyst carrier for decomposing phosphine to prepare high-purity phosphorus, but amorphous alloy In a metastable state, it is easy to accumulate and crystallize at high temperature to reduce its catalytic activity

Method used

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  • Loaded type catalyst for preparing elemental phosphorus and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Dissolve 0.048mol of cobalt sulfate and 0.070mol of sodium citrate in deionized water, then add 0.384mol of sodium hypophosphite, 0.136mol of ammonium sulfate and 1.0g of treated CNTS, and then dilute the reaction solution with deionized water to 200mL, in the reaction solution, Co 2+ The concentrations of ions, sodium citrate, sodium hypophosphite and ammonium sulfate are 0.24mol / L, 0.35mol / L, 1.92mol / L and 0.68mol / L respectively; the pH of the reaction solution is adjusted to 9.0 with concentration of 25% ammonia water Around, at a temperature of 90°C, fully stir to form a black powder precipitate; separate the precipitate and wash it with deionized water until the supernatant reaches neutrality, and finally wash twice with absolute ethanol and place the precipitate in Preserved in absolute ethanol, the precipitate is fresh Co-P / CNTS amorphous alloy. It has been detected that the mass percent of Co and P in the product is Co 38.9 P 5.8 / CNTS, the specific surface a...

Embodiment 2

[0024] Change the sodium hypophosphite addition in Example 1 to 0.240mol, and the concentration in the reaction solution is 1.20mol / L, and all the other steps and conditions are the same as in Example 1. The resulting product has been tested and shown that the mass percentages of Co and P are: Co 41.3 P 4.7 / CNTS, the specific surface area is 72.32m 2 / g.

Embodiment 3

[0026] Change the sodium hypophosphite addition in Example 1 to 0.624mol, and the concentration in the reaction solution is 3.12mol / L, and all the other steps and conditions are the same as in Example 1. The resulting product has been tested and shown that its Co, P mass percent composition is: Co 37.5 P 6.8 / CNTS, the specific surface area is 79.52m 2 / g.

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Abstract

The invention discloses a loaded type catalyst for catalyzing and decomposing phosphine to prepare elemental phosphorus, which takes a carbon nano tube as carrier and forms Co-P / CNTs amorphous alloy together with Co and P. A method for preparing the loaded type catalyst comprises: water-soluble cobalt salt, sodium citrate, sodium hypophosphite and ammonium sulphate are dissolved in de-ionized water and then added with the carbon nano tube which is purified and functionalized, and is steeped by the cobalt salt; the pH of the reaction liquid is adjusted to be about 9 by using ammonia water; under the condition of 80-90 DEG C, the reaction liquid is added with potassium borohydride for initiation and then fully stirred, so that black precipitate is produced in the reaction; after being separated, the precipitate is respectively washed by the de-ionized water and absolute ethyl alcohol, and then put into the absolute ethyl alcohol to be saved. The invention has the advantages that the carbon nano tube (CNTs) is adopted as the carrier to prepare the Co-P / CNTs amorphous alloy which is taken as catalyst for pyrolyzing the phosphine, decomposition temperature is low, and the catalytic activity and the thermal stability are good.

Description

technical field [0001] The invention relates to a catalyst and its preparation technology, in particular to a supported catalyst for preparing elemental phosphorus and its preparation method. Background technique [0002] High-purity phosphorus is a prerequisite for fine phosphorus chemical industry. The development of electronic-grade phosphorus with high added value has good economic value and social benefits. Decomposing phosphine under catalytic conditions to prepare high-purity phosphorus is the most commonly used method. The catalysts currently used generally have disadvantages such as complex processes, low conversion rates, high energy consumption, and poor stability. [0003] As a new type of catalytic material, amorphous alloy is favored by catalytic workers. It will be an ideal choice if amorphous alloy is used as a catalyst carrier for decomposing phosphine to prepare high-purity phosphorus, but amorphous alloy In a metastable state, it is easy to accumulate and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185B01J21/18B01J37/03C01B25/02
Inventor 张宝贵李俐俐韩长秀韩新宇王晓英
Owner NANKAI UNIV
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