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A method for preparing low-arsenic yellow phosphorus using a microchannel reactor

A microchannel reactor and low-arsenic yellow phosphorus technology, applied in the chemical industry, can solve the problems of low arsenic removal efficiency, complicated process, and low yield of yellow phosphorus

Active Publication Date: 2020-10-27
GUIZHOU MICRO CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Existing documents such as Japanese Patent Laid-Open No. 5-116916, Japanese Showa 54-93692, WO99 / 62819, CN1257040, CN102107859A, CN1311756A, etc. have reported some methods for removing arsenic by aqueous phase oxidation, but there are some or low arsenic removal efficiency in the implementation process , or low yield of yellow phosphorus, or low safety, or complex process, or high production cost, poor economy and other defects

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A kind of method utilizing microchannel reactor to prepare low-arsenic yellow phosphorus, comprises the steps:

[0019] (1) Melting: heating and melting 910g (arsenic content 191ppm) industrial yellow phosphorus;

[0020] (2) Preparation of oxidant solution: nitric acid is prepared with ultrapure water to form a nitric acid solution with a mass concentration of 5%;

[0021] (3) Arsenic removal: Nitric acid solution and molten industrial yellow phosphorus have a volumetric flow ratio of 3:1, and are transported to T-shaped microchannel reactor Ⅰ through metering pumps respectively, and react at 50°C for 60 seconds to obtain arsenic removal yellow phosphorus;

[0022] (4) Washing: The volume flow ratio of ultrapure water and dersensic yellow phosphorus is 3:1, respectively pumped into the channel form S-type microchannel reactor II through a metering pump, and countercurrent washed at a temperature of 50°C for 60s to obtain yellow phosphorus 874.51g, the measured arseni...

Embodiment 2

[0024] A kind of method utilizing microchannel reactor to prepare low-arsenic yellow phosphorus, comprises the steps:

[0025] (1) Melting: heating and melting 910g (arsenic content 191ppm) industrial yellow phosphorus;

[0026] (2) Preparation of oxidant solution: nitric acid is prepared with ultrapure water to form a nitric acid solution with a mass concentration of 10%;

[0027] (3) Arsenic removal: Nitric acid solution and molten industrial yellow phosphorus have a volume flow ratio of 5:1, and are transported to Y-shaped microchannel reactor Ⅰ through metering pumps respectively, and react at 65°C for 15 seconds to obtain arsenic removal yellow phosphorus;

[0028] (4) Washing: The volume flow ratio of ultrapure water and dersenicized yellow phosphorus is 5:1, respectively pumped into the channel form Z-shaped microchannel reactor II through a metering pump, and countercurrent washed at a temperature of 65°C for 36s to obtain yellow phosphorus 841.30g, the measured arse...

Embodiment 3

[0030] A kind of method utilizing microchannel reactor to prepare low-arsenic yellow phosphorus, comprises the steps:

[0031] (1) Melting: heating and melting 910g (arsenic content 191ppm) industrial yellow phosphorus;

[0032] (2) Preparation of oxidant solution: nitric acid is prepared with ultrapure water to form a nitric acid solution with a mass concentration of 18%;

[0033] (3) Removal of arsenic: Nitric acid solution and molten industrial yellow phosphorus have a volume flow ratio of 7:1, respectively transported to the collision flow microchannel reactor Ⅰ through a metering pump, and react at 80°C for 5 seconds to obtain arsenic-removed yellow phosphorus ;

[0034] (4) Washing: The volume flow ratio of ultrapure water and dearsenic yellow phosphorus is 7:1, respectively pumped into H-type and L-type combined microchannel reactor II through metering pumps, and countercurrent washed at 80°C for 24s to obtain Yellow phosphorus is 783.51g, and the measured arsenic con...

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PUM

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Abstract

The invention discloses a method for preparing low arsenic yellow phosphorus by using a microchannel reactor, comprising the following steps: heating and melting industrial yellow phosphorus; using ultrapure water to prepare an oxidizing agent into an oxidant solution with the mass concentration of 5% to 20%; conveying the oxidant solution and the molten industrial yellow phosphorus at a volume flow ratio of (1 to 9):1 to the microchannel reactor I by a metering pump, and reacting at 50 to 90 DEG C for 5s to 60s to obtain the arsenic-removed yellow phosphorus; respectively pumping ultrapure water and the arsenic-removed yellow phosphorus at a volume flow ratio of (1-9):1 into the microchannel reactor II through a metering pump, and performing countercurrent washing at a temperature of 50 to 90 DEG C for 5s to 60s to obtain the low arsenic yellow phosphorus, wherein the oxidizing agent is nitric acid, hydrogen peroxide or hypochlorous acid. The method has the advantages of high arsenicremoval rate, high phosphorus yield and good safety.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and specifically relates to a method for preparing low-arsenic yellow phosphorus by using a microchannel reactor. Background technique [0002] Yellow phosphorus is an important chemical raw material. In some specific application fields (such as electronic materials such as pharmaceutical intermediates indium phosphide and gallium phosphide), the purity requirements for yellow phosphorus are high, and strict requirements are put forward for the impurity content in yellow phosphorus. requirements, wherein the arsenic content must be less than 20ppm. Arsenic mainly exists in phosphate rock in the form of arsenate. Since phosphorus and arsenic belong to two adjacent elements of the same main group, many physical and chemical properties are similar. Reduction, the two are condensed in the yellow phosphorus product at the same time, arsenic exists in the eutectic form of arsenic phosphide, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/047B01J19/00
CPCB01J19/0093C01B25/047C01P2006/80
Inventor 禹志宏伍廷鑫王贵城卫炎勋
Owner GUIZHOU MICRO CHEM TECH CO LTD
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