Method for recovering and making antimony oxide from antimony pentachloride solution

A technology of antimony pentachloride and antimony oxide, applied in chemical instruments and methods, liquid solution solvent extraction, inorganic chemistry and other directions, can solve the problems of reducing hydrolysis rate, large consumption of sodium hydroxide and hydrochloric acid, environmental and human harm, etc. To achieve the effect of easy control of process conditions, low cost input, and low consumption of raw materials

Inactive Publication Date: 2008-04-23
JUHUA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The components present in the expired catalyst are quite complex, including pentavalent antimony, trivalent antimony and antimony fluoride chloride (SbCl 5 -nFn, where n=1~5) and a variety of organic substances with high content of hydrogen fluoride and different boiling points, which are extremely toxic
If it is not treated and regenerated, it will cause great harm to the environment and human beings.
[0003] "Study on the process of preparing antimony white from antimony-containing industrial waste residues" in the third issue of "Liaoning Chemical Industry" in 1996 disclosed the production process of using hydrochloric acid to dissolve waste residues to prepare antimony white (antimony oxide). The solid precipitate after sodium neutralization of the spent catalyst is used as the raw material, and the secondary dissolution of hydrochloric acid is used for pretreatment, reduction, hydrolysis, filtration, pickling, neutralization, filtration and drying processes. The disadvantage is that sodium hydroxide and hydrochloric acid consume a lot , high cost, hydrogen fluoride is not thorough in pretreatment, the existence of hydrogen fluoride seriously affects the treatment of subsequent processes, especially the formation of complexes between fluoride ions and antimony ions reduces the hydrolysis rate and the recovery rate of antimony oxide

Method used

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  • Method for recovering and making antimony oxide from antimony pentachloride solution

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Embodiment 1: the present embodiment reclaims antimony oxide from 250ml antimony pentachloride waste liquid, combines figure 1 As shown in the process block diagram, proceed as follows:

[0020] Step 1: get the antimony pentachloride waste liquid of 250ml, wherein there are pentavalent antimony, trivalent antimony and antimony fluoride chloride (SbCl 5 -nFn, where n=1~5) and various organic substances with higher content of hydrogen fluoride and different boiling points, undergo vacuum distillation, the temperature during distillation is controlled at 20°C to 30°C, until no white smoke comes out, The distillate is directly absorbed with lye.

[0021] Step 2: After distillation, slowly add to 2.0mol / L hydrochloric acid. After cooling to room temperature, the solution is layered. After standing for 1.0 hour, separate with a separatory funnel and wash with 2.0mol / L hydrochloric acid. The organic phase. The ratio of the organic phase to the water phase is 1:2.5 (volume r...

Embodiment 2

[0027] according to figure 1 , follow the steps below:

[0028] In the step 1, the distillation temperature is changed to be controlled between 35° C. to 45° C., and the rest are the same as in Example 1. Step 3 and step 4 are the same as embodiment 1.

[0029] Step 2: Distillation is completed, slowly added to dilute hydrochloric acid, after cooling to room temperature, the solution is layered, separated with a separatory funnel after standing for 1.0 hour, and the organic phase is washed with hydrochloric acid with a concentration of 2.0mol / L. The amount of hydrochloric acid provided is insufficient, and the antimony salt in the spent catalyst is easily hydrolyzed, which makes it difficult to separate the antimony from the organic phase. Too much dilute hydrochloric acid will increase the amount of wastewater in the subsequent hydrolysis process, so the ratio of the aqueous phase to the organic phase is 3.2: 1 (volume ratio ).

[0030] Step 5: The neutralization process i...

Embodiment 3

[0032] according to figure 1 , follow the steps below:

[0033] In the step 1, the distillation temperature is changed to be controlled between 50° C. and 60° C., and the rest are the same as in Example 1. Step 3 and step 4 are the same as embodiment 1.

[0034] Step 2: Distillation is completed, slowly added to dilute hydrochloric acid, after cooling to room temperature, the solution is layered, separated with a separatory funnel after standing for 1.0 hour, and the organic phase is washed with hydrochloric acid with a concentration of 2.0mol / L. The amount of hydrochloric acid provided is insufficient, and the antimony salt in the spent catalyst is easily hydrolyzed, which makes it difficult to separate the antimony from the organic phase. Too much hydrochloric acid will increase the amount of wastewater in the subsequent hydrolysis process, so the ratio of the aqueous phase to the organic phase is 3.8:1 (volume ratio) .

[0035] Step 5: The neutralization process is to dr...

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Abstract

The invention relates to a method for recovering and making antimony oxide from antimony pentachloride solution which comprises the steps of pretreatment, reduction, hydrolytic decomposition, drying and neutralization, wherein the pretreatment consists of antimony pentachloride effluent liquor vacuum distillation, inorganic acid abstraction and organic solvent extraction.

Description

technical field [0001] The invention relates to a method for recovering metals and oxides thereof, in particular to a method for recovering and preparing antimony oxide from antimony pentachloride solution. Background technique [0002] In the production of fluororefrigerant-12, fluororefrigerant-22, etc., antimony pentachloride is used as the reaction catalyst. During continuous use, the catalyst will gradually accumulate due to the impurities mixed in the raw materials and the by-products generated during the reaction. and fail. The components present in the expired catalyst are quite complex, including pentavalent antimony, trivalent antimony and antimony fluoride chloride (SbCl 5 -nFn, where n=1 to 5) and various organic substances with higher content of hydrogen fluoride and different boiling points are extremely toxic. If it is not treated and regenerated, it will cause great harm to the environment and human beings. [0003] "Study on the process of preparing antim...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G30/00B01D11/04
Inventor 郑林树郑苏云姜志田宣晓君
Owner JUHUA GRP
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