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Synthesis method of arsenic trichloride

A technique for the synthesis of arsenic trichloride, which is applied in the direction of chemical instruments and methods, arsenic halides, arsenic compounds, etc. It can solve the problems of low reaction efficiency, increase cost output, prolong reaction time, etc., achieve process stability and reduce waste The effect of simple processing cost and raw materials

Inactive Publication Date: 2018-04-27
清远先导材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the low reaction efficiency of chlorine gas and arsenic vapor, the process flow is longer, the reaction time is prolonged, and the cost output is increased; in addition, chlorine gas is introduced in the reaction, which requires high safety requirements for equipment and facilities

Method used

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preparation example Construction

[0012] The synthesis method of arsenic trichloride according to the present application includes steps: S1, add diarsenic trioxide into concentrated hydrochloric acid, start stirring to allow it to react, continue stirring after the reaction and add concentrated sulfuric acid until it is completely dehydrated, and then place the reaction solution in a separate Put the crude arsenic trichloride in the liquid device, then collect the lower layer liquid to obtain the crude arsenic trichloride; Clear arsenic trichloride liquid.

[0013] In the synthesis method of the present application, diarsenic trioxide is added into concentrated hydrochloric acid for reaction, then concentrated sulfuric acid is added for dehydration, and after standing for stratification, crude arsenic trichloride is taken for distillation and purification near the boiling point of arsenic trichloride. On the one hand, by controlling the concentration of concentrated hydrochloric acid, the generated arsenic tr...

Embodiment 1

[0026] Dissolve 1 kg of arsenic trioxide in 3.5 L of concentrated hydrochloric acid with a mass fraction of 32%, start stirring and let it react at 60°C for 2 hours to obtain a transparent and clear solution, then continue stirring and slowly add 1.6 L of concentrated hydrochloric acid with a mass fraction of 98%. Sulfuric acid, the dropping speed of concentrated sulfuric acid is 500mL / h, and the stirring speed is 300rpm. After the dropwise addition is completed, continue to stir for 1h, and then place the reaction solution in a liquid separation device and let it stand for 2h until the reaction solution has obvious stratification. Among them, the upper layer The clear liquid is a mixture of concentrated hydrochloric acid and concentrated sulfuric acid, and the lower layer is the oily arsenic trichloride crude product. The lower layer liquid is discharged and collected to obtain about 720ml of the arsenic trichloride crude product. After calculation, the yield of the arsenic tri...

Embodiment 2

[0029] Dissolve 1 kg of arsenic trioxide in 3.5 L of concentrated hydrochloric acid with a mass fraction of 32%, start stirring and allow it to react at 60°C for 2 hours to obtain a transparent and clear solution, then continue stirring and slowly add 2.5 L of concentrated hydrochloric acid with a mass fraction of 98%. Sulfuric acid, the dropping speed of concentrated sulfuric acid is 500mL / h, and the stirring speed is 300rpm. After the dropwise addition is completed, continue to stir for 1h, and then place the reaction solution in a liquid separation device and let it stand for 2h until the reaction solution has obvious stratification. Among them, the upper layer The clear liquid is a mixed solution of concentrated hydrochloric acid and concentrated sulfuric acid, and the lower layer is the oily crude arsenic trichloride. The lower liquid is released and collected to obtain about 780ml of the crude arsenic trichloride. The calculated yield of the crude arsenic trichloride is 94...

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Abstract

The invention provides a synthesis method of arsenic trichloride. The synthesis method of arsenic trichloride comprises the following steps: S1, adding arsenic trioxide into concentrated hydrochloricacid, starting to stir and enabling the arsenic trioxide and the concentrated hydrochloric acid to react, after reaction is finished, continuing stirring and adding the concentrated hydrochloric aciduntil completely dehydrated, placing reaction liquor in a liquor separating device and standing for layering, and then collecting liquid on the lower layer to obtain coarse arsenic trichloride; and S2, placing the coarse arsenic trichloride in a distilling device, heating for distilling and purifying, and collecting fractions at the temperature of 130-135 DEG C to obtain transparent and clear arsenic trichloride liquid. The synthesis method has the advantages of high purity of products, high synthesis yield, low cost, easiness in control of a process, stable process and low requirement for equipment, and thus, the synthesis method is suitable for large-scale industrial production.

Description

technical field [0001] The present application relates to the field of material synthesis, in particular to a method for synthesizing arsenic trichloride. Background technique [0002] Arsenic trichloride is an inorganic salt product, also known as arsenous chloride. It is a colorless or light yellow fuming oily liquid with a relative molecular weight of 181.28, a melting point of -8.5°C, and a boiling point of 130.2°C. It is soluble in ethanol, ether, and concentrated hydrochloric acid. , the relative density (water=1g / mL) is 2.16g / mL. High-purity arsenic trichloride can be used as a semiconductor material and a raw material for synthesizing arsenic-containing organic compounds, and can also be used to prepare high-purity arsenic, or in the field of pesticides, etc. [0003] At present, the methods for producing arsenic trichloride mainly include hydrochloric acid method and chlorine gas method. [0004] The process of preparing arsenic trichloride by hydrochloric acid me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G28/00
CPCC01G28/007C01P2006/80
Inventor 王春泉邵学亮王艳朱刘
Owner 清远先导材料有限公司
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