Separation and refining method of arsenic trioxide

A technology of arsenic trioxide and refining method, applied in chemical instruments and methods, arsenic compounds, inorganic chemistry and other directions, can solve the problems of low heat and mass transfer rate, unstable product quality, low energy utilization rate, etc. The effect of high yield and fast reaction rate

Active Publication Date: 2013-09-25
哈尔滨医大药业股份有限公司
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AI Technical Summary

Problems solved by technology

[0016] (1) High impurity content and unstable product quality: the material processed by sublimation method in the whole production process is solid phase or gas-solid material, and the obtained arsenic trioxide product usually has high impurity content and unstable product quality
[0017] (2) Low production efficiency: the sublimation method utilizes the easy sublimation characteristics of solid diarsenic trioxide to remove impurities in diarsenic trioxide
Affected by the sublimation area, the heat and mass transfer rate of solid phase materials or gas-solid phase materials is small, so the production efficiency is low
[0018] (3) Large energy consumption: In the separation and refining process of the sublimation method, in order to increase the sublimation rate, it needs to be carried out at a high temperature, and the gas phase material after sublimation must be cooled to increase the yield of the product, so the material must be heated and must be heated. Cool down, resulting in large energy consumption and low energy utilization
[0019] (4) Large amount of waste gas treatment: In the separation and refining process of the sublimation method, in order to increase the sublimation rate and protect the product, it is usually necessary to complete the sublimation and sublimation material collection process under certain atmospheric conditions, and a large amount of waste gas must be treated for recycling. or standard discharge

Method used

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  • Separation and refining method of arsenic trioxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Main process equipment: The esterification reactor is an esterification-rectification coupled reactor, the adsorption and impurity removal equipment and the hydrolysis-crystallization equipment are stirred tanks, and the solid-liquid separation equipment is a sedimentation solid-liquid separator.

[0060] Such as figure 1 As shown, a method for separating and refining diarsenic trioxide is to prepare high-purity diarsenic trioxide by separating and refining the crude product of diarsenic trioxide as raw material by alcohol esterification, and the steps are as follows:

[0061] (1) Esterification reaction: In the esterification-rectification coupling reactor, add diarsenic trioxide crude product and n-propanol, the mass percent content of water in n-propanol is 20%, the molar ratio of diarsenic trioxide and alcohol is 1:8, Then the material is heated to a boiling state, the arsenic trioxide is the solid phase, and the alcohol is the liquid phase. The alkoxy arsenic is fo...

Embodiment 2

[0072] Main process equipment: The esterification reactor is an esterification-distillation coupling reactor, the adsorption and impurity removal equipment and the hydrolysis-crystallization equipment are stirred tanks, and the solid-liquid separation equipment is a filter-press solid-liquid separator, etc.

[0073] Proceed as follows:

[0074] (1) 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 boiling state, arsenic trioxide is the solid phase, and alcohol is the liquid phase. The alkoxy arsenic is formed through solid-liquid esterification and enters the liquid phase. The alcohol forms an azeotrope with the by-product water generated during the reaction and enters through evaporation. Gas phase, the gas phase material is condensed to recover alcohol; ...

Embodiment 3

[0085] Main process equipment: The esterification reactor is an esterification-rectification coupling reactor, the adsorption and impurity removal equipment and the hydrolysis-crystallization equipment are stirred tanks, and the solid-liquid separation equipment is a centrifugal solid-liquid separator, etc.

[0086] Proceed as follows:

[0087] (1) Esterification: In the esterification reactor of the esterification-rectification coupled reactor, add diarsenic trioxide crude product 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, and then heat the material to boiling state, diarsenic trioxide is the solid phase, alcohol is the liquid phase, alkoxy arsenic is formed by solid-liquid esterification reaction and enters the liquid phase, alcohol and the by-product water generated in the reaction process form a co- The boiled matter enters the gas phase through evaporation, and the gas phase material is co...

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Abstract

The invention relates to a separation and refining method of arsenic trioxide. According to the method, a arsenic trioxide crude product is used as raw material and undergoes the following steps: (1) esterification reaction; (2) solid-liquid separation; (3) adsorption and impurity removal; (4) solid-liquid separation; (5) rectification and impurity removal; (6) hydrolysis-crystallization; (7) solid-liquid separation; (8) washing; (9) dehydration; and (10) drying. Thus, high-purity arsenic trioxide is obtained. The separation and refining method has the following advantages: process flow is short; the separation and refining method is simple; product purity is high; quality is stable; the process is safe and reliable; energy consumption is low; the amount of ''three wastes (waste gas, waste water and industrial residue)'' is small; and the separation and refining method is a clean production method which is adopted for the preparation of high-purity arsenic trioxide and accords with development requirements of the green chemical industry.

Description

technical field [0001] The invention relates to a method for separating and refining diarsenic trioxide, in particular to a method for obtaining a high-purity arsenic trioxide product by separating and refining crude diarsenic trioxide as a raw material through esterification-rectification-hydrolysis-crystallization coupling technology, belonging to the technical field of fine chemicals. Background technique [0002] 1.1 Properties and uses of arsenic trioxide [0003] Arsenic trioxide, commonly known as arsenic, also known as anhydrous arsenic acid, arsenic, white arsenic, arsenous anhydride; English name is arsenic trioxide; arsenous acid anhydride; molecular formula As 2 o 3 , white powder or crystal. There are three crystal forms: monoclinic crystal with a relative density of 4.15 and sublimation at 193°C; cubic crystal with a relative density of 3.865; amorphous body with a relative density of 3.738 and a melting point of 312.3°C. Arsenic trioxide is slightly soluble...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G28/00
Inventor 许文林徐福利李树亮张小兴王雅琼
Owner 哈尔滨医大药业股份有限公司
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