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Method of producing high-purity arsenical trichloride

A high-purity arsenic trichloride and chlorine technology, applied in chemical instruments and methods, arsenic compounds, inorganic chemistry, etc., can solve the problem of arsenic trichloride gasification leakage, unsafe, and no introduction of arsenic trichloride process. and other problems, to achieve the effect of improving the utilization rate of chlorine gas, simple production operation and easy control

Active Publication Date: 2008-05-07
SHANGHAI NO 4 REAGENT & H V CHEM
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Problems solved by technology

However, the book does not describe the process of producing arsenic trichloride
[0006] In 1969, the French patent Fr 1,568,603 reported the preparation method of arsenic trichloride, which was a one-step synthesis of metal arsenic and chlorine gas at 180-200°C, with a yield of only 31%, and the high reaction temperature easily caused the gasification of arsenic trichloride leaked, unsafe

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0014] Example 1 Preparation of high-purity arsenic trichloride

[0015] In the reactor, add 100 kilograms of crushed metallic arsenic. The reaction device first passes nitrogen to replace the air, and then uses an oil pump to evacuate. The vacuum degree is controlled at 0.090-0.092Mpa, so that the reaction can be carried out under negative pressure. Control the chlorine flow rate at 2.40-2.50mol / min, the crude arsenic trichloride produced enters the collection pot, observe the sight cup on the collection pot, if there is basically no liquid drop in the sight cup, the reaction is over, and the reaction time is 10 hours.

[0016] The collected crude arsenic trichloride was distilled at 130-131° C. under normal pressure to obtain 230 kg of arsenic trichloride yellow oily liquid product with a purity of 99.8% and a yield of 94.78%.

Embodiment 2

[0017] The preparation of embodiment 2 high-purity arsenic trichloride

[0018] In the reactor, add 100 kilograms of crushed metallic arsenic. The reaction device first passes nitrogen to replace the air, and then uses an oil pump to evacuate. The vacuum degree is controlled at 0.092-0.093Mpa, so that the reaction can be carried out under negative pressure. Control the chlorine flow rate at 3.45-3.47mol / min, the crude arsenic trichloride produced enters the collection pot, observe the sight cup on the collection pot, if there is basically no liquid drop in the sight cup, the reaction is over, and the reaction time is 8.5 hours.

[0019] The collected crude arsenic trichloride was distilled at 130-131° C. under normal pressure to obtain 228 kg of arsenic trichloride yellow oily liquid product with a purity of 99.5%, with a yield of 94.13%.

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Abstract

The invention relates to a preparation method for high purity arsenic trichloride, relating to an improvement of one-step reaction synthetic method for metallic arsenic and chlorine. The reaction is carried under negative pressure, with vacuum degree of 0.085 to 0.096MPa, primary reaction temperature of 80 DEGC to 85DEG C and chlorine feeding speed of 2.0 to 5.2mol / min. with the improved technology, the yield of arsenic trichloride is increased to 94 to 95 percent (counting with As), and the purity is reached to 99.5 to 99.8 percent, the environmental pollution and the unsafe problem caused by the gasification escape of chlorine and arsenic trichloride is avoid, therefore, the invention has the advantages of easy operation, easy control, environmental pollution improvement and safe production. The invention relates to a preparation method for high purity arsenic trichloride being suitable to the industrial production.

Description

technical field [0001] The invention relates to a preparation method of inorganic compound high-purity arsenic trichloride. Background technique [0002] Arsenic trichloride belongs to inorganic salt products. High-purity arsenic trichloride can be used as semiconductor raw material, can be used in the production of arsenic-containing organic compounds and ceramic industrial products, and can also be used as a dopant gas. [0003] Regarding the preparation method of arsenic trichloride, there are not many technical reports at home and abroad, and there are mainly the following preparation methods of arsenic trichloride. [0004] The book "Chemical Product Handbook (Fourth Edition) - Inorganic Chemical Products" published by Chemical Industry Press in January 2004 introduced the hydrochloric acid method: add arsenic trioxide into the reactor, then add concentrated hydrochloric acid, slowly add concentrated sulfuric acid dropwise under stirring . Due to the dropwise addition...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G28/00
Inventor 沈忠华周琴陆鸿良
Owner SHANGHAI NO 4 REAGENT & H V CHEM
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