High-purity arsenic preparation method

A high-purity arsenic and equipment technology, applied in the field of high-purity arsenic preparation, to achieve the effect of large solubility difference, high purity, and high product purity

Inactive Publication Date: 2013-11-13
江苏迪赛恩市政环保设计研究院有限公司
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Problems solved by technology

This method makes full use of the advantages of the liquid phase method and the sublimation method, and solves the problems existing in the process of the liquid phase method and the sublimation method. The developed process has the advantages of short process flow, simple separation and purification method, high product purity, stable quality, and process safety. Reliable, low energy consumption, small amount of three wastes, etc., it is a clean production method for the preparation of high-purity arsenic that meets the requirements of green chemical development

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Experimental program
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Effect test

Embodiment 1

[0076] Main process equipment: oxidation reactor, esterification-rectification coupling reactor, reduction reactor, adsorption impurity removal equipment and hydrolysis-crystallization equipment are stirring tanks, solid-liquid separation equipment is sedimentation solid-liquid separator, etc.

[0077] like figure 1 As shown, a method for preparing high-purity arsenic, especially a process for preparing high-purity arsenic by using the crude industrial arsenic product as a raw material using oxidation-esterification-rectification-hydrolysis-reduction coupling technology, the steps are as follows:

[0078] (1) Oxidation reaction: In the oxidation reactor, the industrial arsenic crude product is mixed with air, and the arsenic and oxygen undergo an oxidation reaction at a reaction temperature of 400°C to form arsenic oxide, and the arsenic oxide gas is condensed to 120°C to obtain arsenic oxide solid, of which arsenic trioxide The mass fraction content is higher than 99%;

[00...

Embodiment 2

[0091] Main process equipment: oxidation reactor, esterification-distillation coupling reactor, reduction reactor, adsorption impurity removal equipment and hydrolysis-crystallization equipment are stirring tanks, solid-liquid separation equipment is filter press solid-liquid separator, etc.

[0092] Proceed as follows:

[0093] (1) Oxidation reaction: In the oxidation reactor, the industrial arsenic crude product is mixed with air, and the arsenic and oxygen undergo an oxidation reaction at a reaction temperature of 600°C to form arsenic oxide, and the arsenic oxide gas is condensed to 180°C to obtain arsenic oxide solid, of which arsenic trioxide The mass fraction content is higher than 99%;

[0094] (2) Esterification reaction: in the esterification-distillation coupled reactor, add diarsenic trioxide crude product and isopropanol, the mass percent content of water in isopropanol is 20%, the molar ratio of diarsenic trioxide and alcohol is 1:24, then Heat the material to a...

Embodiment 3

[0106] Main process equipment: oxidation reactor, esterification-rectification coupling reactor, reduction reactor, adsorption impurity removal equipment and hydrolysis-crystallization equipment are stirred tanks, solid-liquid separation equipment is centrifugal solid-liquid separator, etc.

[0107] Proceed as follows:

[0108] (1) Oxidation reaction: In the oxidation reactor, the industrial arsenic crude product is mixed with air, and the arsenic and oxygen undergo an oxidation reaction at a reaction temperature of 400°C to 600°C to form arsenic oxide, and the arsenic oxide gas is condensed to 120°C to 180°C to obtain Arsenic oxide solid, wherein the mass fraction of arsenic trioxide is higher than 99%;

[0109] (2) Esterification: In the esterification-rectification coupled reactor, add the crude product of diarsenic trioxide and n-butanol, the mass percentage of water in n-butanol is 10%, and the molar ratio of diarsenic trioxide to alcohol is 1:16, Then the material is he...

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Abstract

The invention relates to a high-purity arsenic preparation method. The high-purity arsenic preparation method adopts an arsenic crude product as a raw material and orderly comprises 1, an oxidation reaction, 2, an esterification reaction, 3, solid-liquid separation, 4, adsorption purification, 5, solid-liquid separation, 6, rectification purification, 7, hydrolysis-crystallization, 8, solid-liquid separation, 9, water washing, 10, dehydration, 11, drying, and 12, a reduction reaction. The high-purity arsenic preparation method has the advantages of short process, simple separation purification processes, high product purity, stable quality, safe and reliable processes, low energy consumption and less three wastes and is a clean production method satisfying green chemical development requirements.

Description

technical field [0001] The invention relates to a method for preparing high-purity arsenic, in particular to a process for preparing high-purity arsenic by using an industrial-grade crude arsenic product as a raw material through oxidation-esterification-rectification-hydrolysis-reduction coupling technology, and belongs to the technical field of fine chemicals. Background technique [0002] 1.1 The importance of preparing high-purity arsenic [0003] Electronic information materials support modern high-tech industries such as communications, computers, networks, semiconductors, optoelectronics, new energy, micromachines, and industrial automation, and are important basic materials for the electronic information industry. High-purity arsenic (mass fraction not less than 99.999%) is an important raw material for the preparation of semiconductor materials gallium arsenide (GaAs) and indium arsenide (InAs) and other high-purity arsenic compounds (GaAlAs, GaInAsP, etc.), and hig...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B30/04
CPCY02P10/20
Inventor 许文林李树亮徐福利张小兴王雅琼
Owner 江苏迪赛恩市政环保设计研究院有限公司
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