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Metal antimony purifying method and apparatus

A purification method, metal antimony technology, applied to the improvement of process efficiency, chemical instruments and methods, antimony compounds, etc., can solve the problems of difficult control of product indicators, uncontinuous production, difficult control of purification time and temperature, and achieve saving Operating procedures and equipment, improving the efficiency of equipment use, and improving the effect of product technical indicators

Inactive Publication Date: 2007-07-11
云南省通海大方科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Prior art has following shortcoming owing to technological method and the restriction of equipment: 1. production can not be continuous, can only discontinuous production, rectification product recovery rate is low, and labor intensity is big; The temperature is difficult to control, and it is impossible to form a standardized industrial production
Since the production process is operated by experience, there are many human factors, poor stability, and product indicators are difficult to control
③ During the rectification process, the phenomenon of jumping the kettle due to the metal impurity chloride is often caused, resulting in equipment damage
Therefore, it is difficult to achieve industrialization, large-scale, continuous production

Method used

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  • Metal antimony purifying method and apparatus
  • Metal antimony purifying method and apparatus
  • Metal antimony purifying method and apparatus

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Crush 1# industrial antimony ingots into irregular blocks of φ20-30φ, put 200 kg into the chlorination tower, heat the lower section of the chlorination tower to 130°C, and continuously feed chlorine gas at a rate of 0.5 cubic meters per hour to make the antimony The blocks gradually generate antimony trichloride, which flows from the outlet of the chlorination tower to the liquid storage tank, and the antimony trichloride is put into the reboiler of rectification 1 by the liquid storage tank at a rate of 5 liters per hour, and the reboiled The temperature of the device is raised to 230°C, the temperature of the lower section of the tower head is controlled at 210°C, and the temperature of the upper section of the tower head is 150°C. Under normal pressure, carry out continuous rectification, adjust the reflux valve so that the ratio of the outflow of antimony trichloride to the return flow is 5.5: 1, and the antimony trichloride distilled out passes through the liquid s...

Embodiment 2

[0039] With in embodiment 1, the antimony trichloride of rectification 2 is put into the reboiler of rectification 3 by liquid storage tank, the control condition of temperature, pressure is identical with rectification 1, continues rectification, adjusts reflux valve to make The ratio of the outflow of antimony trichloride to the return flow is 3.0:1, and the rectified antimony trichloride is put into the metering tank in the reduction system through the liquid storage tank for standby.

[0040] Use argon to drive out the air in the reduction tank, raise the temperature to 850°C, slowly introduce hydrogen, and at the same time, continuously put the antimony trichloride in the measurement tank into the reduction tank at a flow rate of 1 liter per hour, and adjust the amount of hydrogen It is 0.6 cubic meters per hour, and it is continuously fed into the reduction tank to reduce antimony trichloride to metal antimony. The material is removed every 8 hours, that is, the metal ant...

Embodiment 3

[0045] In embodiment 2, the antimony trichloride of rectification 3 is put into the reboiler of rectification 4 by liquid storage tank, the control condition of temperature, pressure is identical with rectification 1, continues rectification, adjusts reflux valve to make The ratio of the outflow of antimony trichloride to the return flow is 2.0:1, and the rectified antimony trichloride is put into the metering tank in the reduction system through the liquid storage tank for standby.

[0046] Use argon to drive out the air in the reduction tank, raise the temperature to 850°C, slowly feed hydrogen, and at the same time, put the antimony trichloride in the metering tank into the reduction tank continuously at a flow rate of 0.5 liters per hour. The amount of hydrogen is adjusted to 0.4 cubic meters per hour, and it is continuously fed into the reduction tank to reduce antimony trichloride to metal antimony. The material is removed every 8 hours to obtain 0.6 metal antimony with a...

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Abstract

This invention discloses metal antimony purifying method and its mechanism. The method is to fill the industrial antimony in the chlorination tower; lead chlorine in the middle of the tower, heat at the 1 / 3 lower part of the tower to decompose antimony pentachloride; chloride and the superfluous mental blocks in the tower react to create antimony trichloride. The antimony trichloride in the storage tank automatically flows to re-boiling equipment and steam to go into rectification 1; through reflux control valve adjust flow amount of antimony trichloride and reflux amount, and the antimony trichloride goes into the re-boiler of rectification 2; the lower output mouth of the rectification tower arch is connected by the channel with the material interface of the storage tank that has two outputting mouths connected with the computation tank of reductive tank and re-boiler of sub-grade rectification system by the tube. The upper outputting mouth is connected with the residue tank by the pipeline; orderly connect the multi-grade rectification tower and continuously bring in the superfluous hydrogen and revert it and get 99.999%, 99.9999% and 99.99999% metal antimonies.

Description

technical field [0001] The method relates to a method of hydrometallurgy, more specifically, a method for purifying metal antimony and a device for realizing the method. The method and device of the invention are particularly suitable for large-scale industrial production. Background technique [0002] In the purification process of metal antimony, due to the very strict requirements on the materials of production equipment and complicated process conditions, any method of wet purification of metal antimony so far is intermittent production, and it is difficult to form industrialized production. Therefore, the prior art has always been small-batch production through processes such as chlorination→dechlorination→rectification→reduction. Add hydrochloric acid in the rectification process to remove low-boiling impurities first, and then extract antimony trichloride through rectification. Purpose. The rectified antimony trichloride is sent to the reduction tank, and hydrogen ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B30/02C01G30/00C22B3/00C22B3/02
CPCY02P10/20
Inventor 鲁燕杰
Owner 云南省通海大方科技有限公司
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