Preparation technology and equipment for sulfur-free arsenious oxide

A technology of arsenic sulfur oxide and equipment, which is applied in the field of preparation technology and equipment of sulfur-free arsenic oxide, which can solve the problems of harmfulness and difficulty in controlling the stability of sulfur removal, and achieve the effects of convenient use, easy operation, and simple equipment structure

Inactive Publication Date: 2013-08-28
JIANGXI HAICHEN OPTOELECTRONICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] When preparing the compound electronic material gallium arsenide, the impurity element sulfur in the raw material high-purity elemental arsenic is a very harmful element. When preparing high-purity elemental arsenic, the concentration of sulfur element must be controlled below 10PPb. The classic process is to use oxidation Arsenic or elemental arsenic is converted into arsenic trichloride, and then let arsenic trichloride flow through a packing column filled with elemental arsenic to remove sulfur to obtain arsenic trichloride with very low sulfur content. The disadvantage of this process is that the arsenic i

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1: Throw 50kg of granular material into the high-level material box at a time, and the reaction temperature of each section follows the set temperature. After the temperature reaches the set temperature, start feeding. The continuous feeding rate is 200g / min. The oxygen flow rate is adjusted to the tail gas to observe the bubbles in the jar. It can be counted, the continuous working time is about 4 hours, the material level of the high-level silo is alarmed, the power of the feeding system is turned off to stop the feeding, the outlet of the material box is opened, and the material in the material box is taken out to obtain 39kg of arsenic oxide. After reduction, only one element of sulfur is detected by GDMS, and the test result shows that the sulfur content is below 10PPb.

Embodiment 2

[0030] Example 2: Throw 500kg of granular material into the high-level material box at a time, and the reaction temperature of each section follows the set temperature. After the temperature reaches the set temperature, start feeding. The continuous feeding rate is 100g / min. The oxygen flow rate is adjusted to the tail gas to observe the bubbles in the jar. It can be counted, the contact working time is 80 hours, the material level of the high-level silo is alarmed, the power of the feeding system is turned off to stop the feeding, the outlet of the material box is opened, and the material in the material box is taken out to obtain 633kg of arsenic oxide, which is reduced with hydrogen Finally, only one element of sulfur is detected by GDMS, and the test result shows that the sulfur content is below 10PPb.

Embodiment 3

[0031] Embodiment 3: The A and C sections of the reaction furnace are heated up according to the set temperature. After the temperature reaches the set temperature, put the E tube of 15kg particles of 1 ~ 30mm material and cover the lid F, and put the E tube into the A section reaction tube. Cover the flange cover of section A, tighten the flange bolts and connect the oxygen hose to the ventilation joint of the flange cover of section A at the same time, open the oxygen flow meter in the pipeline to 3L / min of oxygen in advance, and ensure that the flange cover of section A is covered At the same time, oxygen is input into the reaction furnace. Set the temperature in section A from the initial temperature to 800~850℃ for a total time of 10-12 hours. The staff is on duty in front of the flowmeter and adjusts the flowmeter as the temperature in section A rises. Oxygen flow, always keep the bubbles in the jar continuously and countable. When the temperature of section A reaches 800...

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PUM

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Abstract

The invention relates to a preparation technology and equipment for sulfur-free arsenious oxide. A special horizontal ceramic tubular reformer is adopted, and the technology is characterized in that the simple substance arsenic is oxidized at high temperature in an oxygen enrichment condition so as to remove sulfur to obtain the sulfur-free arsenious oxide. The equipment comprises a tubular structure A, a tubular structure B and a tubular structure C, wherein the tubular structure A is taken as a material section, the tubular structure B is taken as a reaction section, the tubular structure C is taken as a transition section, the diameters of the tubular structure A, the tubular structure B and tubular structure C are identical, and the preparation technology comprises two forms of interrupted feeding or uninterrupted feeding. The equipment has a simple structure, is convenient to use and easy to operate, has short processes, can be used for rapidly and effectively preparing plenty of arsenious oxide products with sulfur content less than 50PPb, and provides raw materials with low sulfur content for preparation of high purity arsenic by adopting arsenic trichloride through rectification or arsenic trioxide through distillation.

Description

technical field [0001] The present invention relates to the removal of elements that are easily oxidized into gaseous oxides that are not easy to condense in simple oxygen by oxidation reaction, so as to achieve the purpose of completely removing impurities. In particular, it relates to the sulfur-free oxidation of elemental arsenic through high-temperature oxidation under oxygen-enriched conditions to remove sulfur. Arsenic process. Background technique [0002] When preparing the compound electronic material gallium arsenide, the impurity sulfur element in the high-purity elemental arsenic raw material is a very harmful element. When preparing high-purity elemental arsenic, the concentration of sulfur element must be controlled below 10PPb. The classic process is to use oxidation Arsenic or elemental arsenic is converted into arsenic trichloride, and then let arsenic trichloride flow through a packing column filled with elemental arsenic to remove sulfur to obtain arsenic ...

Claims

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Application Information

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IPC IPC(8): C01G28/00
Inventor 周斌金杰罗学文罗亮
Owner JIANGXI HAICHEN OPTOELECTRONICS
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