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Metal antimony purifying method and apparatus

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

Inactive Publication Date: 2005-10-05
云南省通海大方科技有限公司
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  • 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 in the chlorination tower, heat the lower section of the chlorination tower to 130°C, and continuously introduce chlorine gas at a rate of 0.5 cubic meters per hour to make the antimony The block gradually generates antimony trichloride, which flows from the outlet of the chlorination tower to the liquid storage tank, and puts the antimony trichloride into the reboiler of rectification 1 from the liquid storage tank at a speed of 5 liters per hour, and the reboiler The temperature of the lower part of the tower head is controlled to be 210°C, and the temperature of the upper part of the tower head is 150°C. Under normal pressure conditions, carry out continuous rectification, adjust the reflux valve so that the ratio of antimony trichloride outflow to reflux is 5.5:1. The flow goes to the reboiler of rectification 2. Continue rectification under the same temperature and pressure conditions ...

Embodiment 2

[0038] In Example 1, the antimony trichloride of rectification 2 was put into the reboiler of rectification 3 by the liquid storage tank, and the control conditions of temperature and pressure were the same as those of rectification 1, and continued rectification, adjusting the reflux valve to make The ratio of antimony trichloride outflow to reflux is 3.0:1, and the rectified antimony trichloride is put into the measuring tank in the reduction system through the liquid storage tank for standby use.

[0039] 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, at a flow rate of 1 liter per hour, put the antimony trichloride in the metering tank into the reduction tank continuously, and adjust the amount of hydrogen. For 0.6 cubic meters per hour, continuously pass into the reduction tank to reduce antimony trichloride to metal antimony, and remove the material every 8 hours, that is, metal antimon...

Embodiment 3

[0043] In Example 2, the antimony trichloride of rectification 3 was put into the reboiler of rectification 4 by the liquid storage tank, and the control conditions of temperature and pressure were the same as rectification 1, and continued rectification, and the reflux valve was adjusted to make The ratio of antimony trichloride outflow to reflux is 2.0:1, and the rectified antimony trichloride is put into the measuring tank in the reduction system through the liquid storage tank for standby use.

[0044] The air in the reduction tank was purged with argon gas, and the temperature was raised to 850°C, and hydrogen was slowly introduced into the reduction tank. The amount of hydrogen was adjusted to 0.4 cubic meters per hour, and it was continuously fed into the reduction tank to reduce antimony trichloride to metal antimony, and the material was removed every 8 hours to obtain metal antimony 0.6, with a purity of more than 99.99999%, using a glow discharge mass spectrometer. ...

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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 present method relates to a method of hydrometallurgy, more particularly, to a method for purifying antimony metal and a device for realizing the method. The method and apparatus of the present invention are particularly suitable for large-scale industrial production. Background technique [0002] In the purification process of metal antimony, due to the strict material requirements of production equipment and complex process conditions, any method of wet purification of metal antimony so far is intermittent production, and it is difficult to form an industrialized production. Therefore, in the prior art, it has been produced in small batches through processes such as chlorination→dechlorination→rectification→reduction. In the rectification process, add hydrochloric acid to remove low-boiling impurities first, and then extract antimony trichloride through rectification. Purpose. The rectified antimony trichloride is sen...

Claims

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Application Information

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