Method for reclaiming metal stibium from waste fluorination catalyst antimony pentachloride

A fluorination catalyst, antimony pentachloride technology, applied in the direction of improving process efficiency, etc., can solve the problems such as no technical inspiration for recovering simple metal antimony, achieve the effect of simple and easy treatment process, and reduce the impact on the environment

Inactive Publication Date: 2008-06-25
CHANGSHU 3F ZHONGHAO NEW CHEM MATERIALS
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  • Abstract
  • Description
  • Claims
  • Application Information

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  • Method for reclaiming metal stibium from waste fluorination catalyst antimony pentachloride

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Embodiment 1

[0018] According to the technological process shown in the accompanying drawing, metal elemental antimony was recovered from 402.4 g of spent fluorination catalyst antimony pentachloride.

[0019] A), extraction, get 402.4g spent fluorination catalyst antimony pentachloride, wherein SbCl 5-m f m (m is 0~5), SbCl 3-n f n (n is 0 to 3) and hydrogen fluoride and a variety of organic substances with different boiling points are extracted with 24% hydrochloric acid at a ratio of 1:1 by volume. Carbon organic phase, the upper layer is an inorganic phase containing antimony ions, the separated organic phase is then extracted according to the above ratio, after layering, the organic phase is incinerated, and the inorganic phase is mixed with the previous inorganic phase to obtain antimony ion-containing Inorganic phase extract;

[0020] B), reduction, adding aluminum to the inorganic phase extract containing antimony ions in a weight ratio of 1:5 (aluminum: inorganic phase extract...

Embodiment 2

[0022] According to the process flow of the accompanying drawing, metal elemental antimony is recovered from the spent fluorination catalyst antimony pentachloride from the same spent catalyst as in Example 1.

[0023] A), extraction, take 400.3g spent fluorination catalyst antimony pentachloride, extract with 6% hydrochloric acid according to the ratio of volume ratio 3:1, after stirring and mixing evenly, static layering, the lower layer is dichloromethane, polychlorofluoro Carbon organic phase, the upper layer is an inorganic phase containing antimony ions, the separated organic phase is then extracted according to the above ratio, after layering, the organic phase is incinerated, and the inorganic phase is mixed with the previous inorganic phase to obtain antimony ion-containing Inorganic phase extract;

[0024] B), reduction, adding aluminum to the inorganic phase extract containing antimony ions in a weight ratio of 1: 13 (aluminum: inorganic phase extract), during which...

Embodiment 3

[0026] According to the process flow of the accompanying drawing, metal elemental antimony is recovered from the spent fluorination catalyst antimony pentachloride from the same spent catalyst as in Example 1.

[0027] A), extraction, take 403.6g of spent fluorination catalyst antimony pentachloride, extract with 6% hydrochloric acid according to the ratio of volume ratio 5.8:1, after stirring and mixing evenly, static layering, the lower layer is dichloromethane, polychlorofluoro Carbon organic phase, the upper layer is an inorganic phase containing antimony ions, the separated organic phase is then extracted according to the above ratio, after layering, the organic phase is incinerated, and the inorganic phase is mixed with the previous inorganic phase to obtain antimony ion-containing Inorganic phase extract;

[0028] B), reduction, adding aluminum to the inorganic phase extract containing antimony ions in a weight ratio of 1: 15.7 (aluminum: inorganic phase extract), durin...

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Abstract

A method of recovering metallic elemental antimony from waste fluorination catalyst antimony pentachloride belongs to the waste catalyst recovery technical field, and comprises the following steps of extraction and reduction, wherein, the extraction comprises the steps of using extractant to extract waste fluorination catalyst antimony pentachloride so as to obtain inorganic phase extract containing antimony ions; the reduction comprises the steps of using reducing agent to reduce the inorganic phase extract containing antimony ions to obtain mud containing antimony powder, washing, filtering and drying the mud to obtain metallic antimony. The present invention has the advantages that: the treatment process is simple and easy to implement; the influence on the environment can be decreased; the antimony powder obtained by using the method can be used to react with chlorine to generate antimony pentachloride for recycling.

Description

technical field [0001] The invention relates to a method for recovering elemental metal antimony from spent fluorination catalyst antimony pentachloride, and belongs to the technical field of recovery of spent catalysts. Background technique [0002] As known in the industry, antimony pentachloride is a commonly used reactive fluorination catalyst in the production of chlorofluorocarbons (CFCs), hydrochlorofluorocarbons (HCFCs) and hydrofluorocarbons (HFCs). During use, it will be poisoned and ineffective due to the gradual accumulation of some impurities generated during the reaction process. The components present in the spent catalyst are very complex, including SbCl 5-m f m (m is 0~5), SbCl 3-n (n is 0 to 3) and hydrogen fluoride and various organic substances with different boiling points such as methylene chloride, polychlorofluorocarbon organic substances, etc. The inorganic antimony mentioned above is an example. It is very toxic. If it is released into the envir...

Claims

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Application Information

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IPC IPC(8): C22B30/02C22B3/10
CPCY02P10/20
Inventor 王其明
Owner CHANGSHU 3F ZHONGHAO NEW CHEM MATERIALS
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