Preparation method of high-purity arsenic

A high-purity arsenic and arsenic trichloride technology, which is applied in the field of high-purity material preparation, can solve environmental pollution and other problems, and achieve the effect of low impurity content and lower requirements

Inactive Publication Date: 2013-07-03
FIRST RARE MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of preparing high-purity arsenic by this method, a large amount of highly toxic gases will be produced, su

Method used

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  • Preparation method of high-purity arsenic

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preparation example Construction

[0015] The preparation method of high-purity arsenic according to the present invention will be described in detail below.

[0016] The preparation method of high-purity arsenic according to the present invention comprises the steps of: loading the arsenic raw material into a sublimation furnace, sublimating the arsenic in the arsenic raw material at a specified vacuum degree and sublimation temperature, condensing the sublimated arsenic vapor at a specified condensation temperature, To obtain purified arsenic; put the purified arsenic into a chlorination furnace, feed chlorine gas and heat up, so that the purified arsenic reacts with chlorine gas to generate arsenic trichloride; feed arsenic trichloride into a dechlorination tower, heat up the three The arsenic chloride is steamed out, and the arsenic trichloride is steamed to obtain the impurity-removing arsenic trichloride after passing through the heat preservation section of the dechlorination tower; Evaporation, the evap...

Embodiment 1

[0028] The arsenic raw material is broken into 2~3cm, in the sublimation furnace: the specified vacuum degree is 10 -2 Pa, the sublimation temperature is 400°C, the sublimation time is 15h, and the specified condensation temperature is 200°C;

[0029] Purified arsenic is broken into small pieces of 1-3cm. In the chlorination furnace: the flow rate of chlorine gas is 800ml / min, and the heating temperature is 200°C;

[0030] In the dechlorination tower: the heating temperature is 300°C, and the temperature of the holding section is 260°C;

[0031] In the rectification kettle: the temperature of the heating is 180°C, and the temperature of the heat preservation section is 130°C;

[0032] In the reduction furnace: the flow rate of hydrogen is 500ml / min, and the heating temperature is 300°C;

[0033] In another sublimation furnace: the given vacuum is 7×10 -3 Pa, the sublimation temperature is 640°C, the sublimation time is 10h, and the given condensation temperature is 330°C. ...

Embodiment 2

[0035] The arsenic raw material is broken into 2~3cm, in the sublimation furnace: the specified vacuum degree is 1.5×10 -3 , the sublimation temperature is 450°C, the sublimation time is 14h, and the specified condensation temperature is 250°C;

[0036] The purified arsenic is broken into small pieces of 1-3cm. In the chlorination furnace: the flow rate of chlorine gas is 1200mL / min, and the heating temperature is 160°C;

[0037] In the dechlorination tower: the heating temperature is 120°C, and the temperature of the holding section is 90°C;

[0038] In the rectification kettle: the heating temperature is 120°C, and the temperature of the heat preservation section is 90°C;

[0039] In the reduction furnace: the flow rate of hydrogen is 400ml / min, and the heating temperature is 400°C;

[0040] In another sublimation furnace: Given a vacuum of 10 -2 Pa, the sublimation temperature is 700°C, the sublimation time is 5h, and the given condensation temperature is 400°C.

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Abstract

The invention provides a preparation method of high-purity arsenic. The method comprises the steps that: an arsenic raw material is placed in a sublimation furnace; under a certain vacuum degree and a certain sublimation temperature, arsenic is sublimated; the sublimated arsenic vapor is condensed under a condensation temperature, such that purified arsenic is obtained; the purified arsenic is placed into a chlorination furnace; chlorine gas is delivered in, and the temperature is increased; purified arsenic is subjected to a reaction with chlorine gas, such that arsenic trichloride is produced; arsenic trichloride is delivered into a dechlorination tower; the temperature is increased, and arsenic trichloride is evaporated; the evaporated arsenic trichloride passes through a temperature-maintaining section of the dechlorination tower, such that impurity-removed arsenic trichloride is obtained; the impurity-removed arsenic trichloride is delivered into a rectification kettle; the evaporated arsenic trichloride passes through a temperature-maintaining section of the rectification kettle, such that purified arsenic trichloride is obtained; the purified arsenic trichloride is delivered into a reduction furnace; hydrogen is delivered in and the temperature is increased by heating, such that reduced arsenic is obtained; the reduced arsenic is delivered into another sublimation furnace, and is sublimated under a given vacuum degree and a given sublimation temperature, such that reduced arsenic vapor is obtained; and the reduced arsenic vapor is then condensed under a given condensation temperature, such that high-purity arsenic is obtained.

Description

technical field [0001] The invention relates to a method for preparing high-purity materials, in particular to a method for preparing high-purity arsenic. Background technique [0002] Arsenic is a metal-like non-metallic element with a metallic luster, a melting point of 1090K (under 2.8MPa), sublimation at 898K, and a density of 5.78g / cm 3 . When arsenic is heated to 200°C in air, it will show obvious fluorescence, and it will burn at a higher temperature, showing a blue flame. Metallic arsenic is insoluble in water but soluble in nitric acid and hot sulfuric acid. [0003] Metallic arsenic is mainly used as an alloying additive. High-purity arsenic is the main raw material for the synthesis of gallium arsenide compounds, indium arsenide compounds, arsenic selenide compounds, etc. Widely used in integrated circuits, photovoltaic solar power generation technology, Hall elements and other fields. In recent years, with the development of high-tech industries, the applica...

Claims

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Application Information

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IPC IPC(8): C22B30/04
Inventor 朱刘刘留
Owner FIRST RARE MATERIALS CO LTD
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