Method for separating antimony from arsenic in antimony-arsenic soot

An antimony arsenic soot and antimonate technology is applied in the field of arsenic and smelting special metal antimony, which can solve the problems of high reagent consumption, volatile antimony and arsenic, and secondary pollution.

Inactive Publication Date: 2016-06-08
INST OF PROCESS ENG CHINESE ACAD OF SCI +1
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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 is obtained by evaporation; the consumption of vulcanizing agent, oxidizing agent and other reagents in this method is large, which makes the process economical of this method not good
CN103757424A discloses a process for selectively leaching antimony-arsenic fumes, that is, first mixing antimony-arsenic fumes with sodium nitrate and alkali, calcining at 400-680°C, and immersing and filtering in water after calcining to obtain sodium metaantimonate filter cake and arsenic sodium antimonate solution, and then dry the sodium antimonate filter cake and the concentrated sodium arsenate solution to obtain sodium antimonate and sodium arsenate products respectively; The operating conditions are poor, and antimony and arsenic are volatile, which can easily cause secondary pollution
In addition, there is also a process using acid leaching, but because highly toxic arsine gas is easily generated during the acid leaching process, the requirements for the operation process are extremely high, and the environment is not friendly

Method used

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  • Method for separating antimony from arsenic in antimony-arsenic soot

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Experimental program
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Effect test

Embodiment 1

[0012] Prepare a NaOH solution with an alkali concentration of 200g / L, mix the antimony-arsenic soot (including Sb30.25%, As34.20%) and NaOH solution according to the liquid-solid ratio of 9:1, and heat in an alkali-resistant autoclave Stir; when the temperature of the feed liquid reaches 200°C, feed 1.0MPa air into the reactor, and start timing. After reacting for 2 hours, cool the slurry to below 90°C to obtain the reaction-completed slurry; dilute the reaction-completed slurry to The NaOH concentration is 150g / L, filter, and wash the filter residue with hot water at 80-90°C to obtain sodium antimonate slag (in which Sb36.94%), the arsenic content in sodium antimonate slag is reduced to 0.01%, which can be used as antimony concentrate Prepare antimony oxide powder; evaporate the filtrate to a NaOH concentration of 220g / L, add 0.1% sodium arsenate seed crystals to the evaporated lye, stir and gradually cool to 35°C, crystallize for 2 hours and then filter and separate, the sol...

Embodiment 2

[0015] Prepare a NaOH solution with an alkali concentration of 380g / L, mix the antimony-arsenic soot (including Sb41.66%, As20.97%) and NaOH solution according to the liquid-solid ratio of 2.5:1, and heat in an alkali-resistant autoclave Stir; when the temperature of the feed liquid reaches 280°C, feed 0.2MPa of oxygen into the reactor, and start timing. After reacting for 1 hour, cool the slurry to below 90°C to obtain the reaction-completed slurry; dilute the reaction-completed slurry to The NaOH concentration is 100g / L, filter, and wash the filter residue with hot water at 80-90°C to obtain sodium antimonate slag (Sb37.52%). The arsenic content in sodium antimonate slag is reduced to 0.03%, which can be used as antimony concentrate Prepare antimony oxide powder; evaporate the filtrate to a NaOH concentration of 380g / L, add 2% sodium arsenate seed crystals to the evaporated lye, stir and gradually cool to 45°C, crystallize for 12 hours and then filter and separate, the solid ...

Embodiment 3

[0018] Prepare a NaOH solution with an alkali concentration of 80g / L, mix the antimony-arsenic soot (including Sb16.16%, As45.29%) and NaOH solution according to the liquid-solid ratio of 5:1, and heat in an alkali-resistant autoclave Stir; when the temperature of the feed liquid reaches 90°C, feed 1.8MPa oxygen-enriched gas into the reactor, and start timing. After 3.5 hours of reaction, the reaction complete slurry is obtained; Washing with hot water obtains sodium antimonate slag (wherein Sb28.36%), and the arsenic rate in the sodium antimonate slag drops to 0.14%, which can be used as antimony concentrate to prepare antimony oxide powder; the filtrate is evaporated to a NaOH concentration of 250g / L , add 5% sodium arsenate seed crystals to the evaporated lye, stir and gradually cool to 55 ° C, filter and separate after crystallization for 8 hours, the solid phase is sodium arsenate crystals (wherein Sb0.05%), and the liquid phase is The NaOH solution containing a small amo...

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Abstract

The invention relates to a method for separating antimony from arsenic in antimony-arsenic soot through oxidation alkaline leaching. The method specifically includes the steps that the antimony-arsenic soot and an alkali solution of a certain concentration are mixed and placed in an alkali-resisting and pressure-resisting reaction still, a gas oxidizing agent of certain pressure is introduced, and a reaction is carried out at a certain temperature; after the reaction, the alkali concentration is adjusted to be below 150 g/L with water or dilute alkali, liquid and solid are separated, an arsenic-rich leaching solution and antimonate slags are obtained, and the antimonate slags can be used for preparation of antimonious oxide powder as antimony concentrate; the arsenic-rich leaching solution is evaporated and added with little seed crystals for cooling crystallization, arsenate crystal products are obtained, and crystallization mother liquor returns to the leaching process of the antimony-arsenic soot. The method is simple in process, capable of separating antimony and arsenic thoroughly and short in flow path; and the method can also avoid arsenic volatilization of the roasting process and harm caused by arsenic hydride gas of the acid leaching process, thereby being environmentally friendly.

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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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/02C22B30/04C22B30/02
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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