Method for separating antimony and arsenic from antimony and arsenic-containing ash through oxidation and alkaline leaching

A technology of oxidizing alkali leaching and soot, which is applied in the field of smelting special metals antimony and arsenic, which can solve the problems of extremely high operating process requirements, secondary pollution, and poor operating process conditions, and achieve simple process, high-efficiency separation, and easy operation Effect

Inactive Publication Date: 2016-06-08
INST OF PROCESS ENG CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN102233229A discloses a fire separation method, which uses the difference in volatilization temperature of arsenic trioxide and antimony trioxide to realize step-by-step volatilization, specifically volatilizing arsenic trioxide at 680°C, and then raising the temperature to 850°C to volatilize antimony trioxide ; However, the pyrotechnic process has high energy consumption, the separation of antimony and arsenic is not complete, and there are problems such as arsenic-containing dust pollution
CN1312392 discloses a kind of method of wet separation, and this method adopts Na 2 The mixed alkali solution of S and NaOH leaches antimony and arsenic synchronously, and then 2 o 2 Oxidize the sulfur immersion solution to obtain crude sodium antimonate precipitation and oxidation solution containing sodium arsenate; pickle the crude sodium antimonate precipitation with HCl and neutralize it with NaOH to obtain sodium pyroantimonate, and obtain the oxidation solution containing sodium arsenate by heating Sodium arsenate i

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  • Method for separating antimony and arsenic from antimony and arsenic-containing ash through oxidation and alkaline leaching

Examples

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Embodiment 1

[0014] The method for separating the arsenic of antimony in the soot of antimony and arsenic by oxidation alkali leaching of the present embodiment comprises the following steps:

[0015] (1) Prepare a NaOH solution with an alkali concentration of 400g / L, mix the antimony-arsenic soot (including Sb32.23%, As36.22%) and NaOH solution according to the liquid-solid ratio of 9:1, and place it in an alkali-resistant high-pressure reaction Heat and stir in the kettle; when the temperature of the slurry reaches 250°C, inject 1.0MPa of oxygen into the reaction kettle, and start timing. After reacting for 2 hours, cool the slurry to below 90°C to obtain the reaction-completed slurry;

[0016] (2) The slurry is filtered and separated after the reaction is completed, and the filtrate is returned to the pressurized alkaline leaching process for the next batch of antimony-arsenic soot;

[0017] (3) Wash the filter cake obtained in step (2) with multi-stage countercurrent washing with hot w...

Embodiment 2

[0021] The method for separating the arsenic of antimony in the soot of antimony and arsenic by oxidation alkali leaching of the present embodiment comprises the following steps:

[0022] (1) Prepare a NaOH solution with an alkali concentration of 480g / L, mix the antimony-arsenic soot (including Sb43.66%, As21.97%) and NaOH solution according to the liquid-solid ratio of 5:1, and place it in an alkali-resistant high-pressure reaction Heat and stir in the kettle; when the temperature of the slurry reaches 90°C, feed 1.8MPa oxygen into the reaction kettle, and start timing. After 3 hours of reaction, the reaction-completed slurry is obtained;

[0023] (2) The slurry is filtered and separated after the reaction is completed, and the filtrate is returned to the pressurized alkaline leaching process for the next batch of antimony-arsenic soot;

[0024] (3) The filter cake obtained in step (2) is subjected to multistage countercurrent washing with hot water at 80 to 90° C., and filt...

Embodiment 3

[0028] The method for separating the arsenic of antimony in the soot of antimony and arsenic by oxidation alkali leaching of the present embodiment comprises the following steps:

[0029] (1) Prepare a NaOH solution with an alkali concentration of 600g / L, mix the antimony-arsenic soot (including Sb15.16%, As46.29%) and NaOH solution according to the liquid-solid ratio of 3:1, and place it in an alkali-resistant high-pressure reaction Heat and stir in the kettle; when the temperature of the slurry reaches 150°C, inject 1.5MPa of oxygen into the reaction kettle, and start timing. After reacting for 1 hour, cool the slurry to below 90°C to obtain the reaction-completed slurry;

[0030] (2) The slurry is filtered and separated after the reaction is completed, and the filtrate is returned to the pressurized alkaline leaching process for the next batch of antimony-arsenic soot;

[0031] (3) Wash the filter cake obtained in step (2) with multi-stage countercurrent washing with hot wa...

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Abstract

The invention relates to a method for separating antimony and arsenic from antimony and arsenic-containing ash through an oxidation and alkaline leaching process. The method comprises the specific steps that the antimony and arsenic-containing ash and an alkaline solution with a certain concentration are mixed and then placed in an alkali-resisting and pressure-resisting reaction kettle, and a gaseous oxidizing agent of a certain pressure is introduced into the reaction kettle to conduct a reaction at a certain temperature; after the reaction is completed, liquid-solid separation is carried out when slurry is cooled to the temperature below 90 DEG C, and a liquid phase is returned to the pressure alkaline leaching procedure; a filter cake is subjected to multistage countercurrent washing and filtering with hot water, and arsenic-enriched washing liquid and an antimonite filter cake are obtained; the antimonite filter cake can serve as an antimony concentrate for preparation of antimony oxide powder; and the arsenic-enriched washing liquid is evaporated, then cooled and crystallized, the crystallization end-point temperature and the crystallization time are controlled, arsenate crystals can be obtained after liquid-solid separation, and crystallization mother liquor is alkaline liquor containing a little amount of arsenic and is returned for the leaching process of the antimony and arsenic-containing ash. By means of the method, the process is simple, antimony and arsenic are separated thoroughly, harm caused by arsenic volatilization during the roasting process and arsenic hydride gas produced through the acid leaching process can be avoided, and environmental friendliness is achieved.

Description

technical field [0001] The invention belongs to the technical field of smelting special metal antimony and arsenic. Background technique [0002] In some pyrometallurgical processes, soot containing a certain amount of antimony and arsenic (such as copper blast furnace soot, etc.) is often produced, which has a certain recovery value. Since antimony, arsenic and their oxides are extremely volatile, antimony and arsenic are generally recovered by volatile roasting. For example, using a reverberatory furnace to reduce and volatilize copper blast furnace soot or other slag containing antimony and arsenic can obtain soot with high antimony and arsenic content, in which the content of antimony can reach 10% to 40% (mass fraction), and the content of arsenic can reach 10%. ~60% (mass fraction), with significant enrichment effect. However, due to the ineffective separation of antimony and arsenic in the obtained soot, it is not conducive to the further utilization of antimony and...

Claims

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Application Information

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IPC IPC(8): C22B7/02C22B30/02C22B30/04
CPCY02P10/20
Inventor 郑诗礼王晓辉张盈乔珊王辉刘朗明苗华磊林文军
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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