CN105648226A - Method for separating antimony from arsenic in antimony-arsenic soot - Google Patents
Method for separating antimony from arsenic in antimony-arsenic soot Download PDFInfo
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- CN105648226A CN105648226A CN201410648127.4A CN201410648127A CN105648226A CN 105648226 A CN105648226 A CN 105648226A CN 201410648127 A CN201410648127 A CN 201410648127A CN 105648226 A CN105648226 A CN 105648226A
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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
The invention belongs to a kind of method smelting specialty metal antimony, arsenic technical field.
Background technology
In some pyrometallurgical smelting processes, normal generation, containing the cigarette ash (such as copper blast-furnace cigarette ash etc.) of a certain amount of antimony and arsenic, has certain recovery value. Due to antimony, arsenic and oxide compound highly volatile thereof, general method recovery antimony and the arsenic adopting volatilization roasting. Reverberatory furnace reduction volatilization is such as adopted to process the copper blast-furnace cigarette ash containing antimony, arsenic or other slag material, the cigarette ash of high antimony, arsenic can be obtained, wherein antimony content can reach 10%��40% (massfraction), arsenic content can reach 10%��60% (massfraction), has significant concentration effect. But owing to antimony, arsenic fail effectively to be separated in the cigarette ash of acquisition, it is unfavorable for the further utilization of antimony and arsenic resource. Therefore, it is achieved in antimony arsenic smoke dust, the high efficiency separation of antimony and arsenic needs the technical problem of solution badly.
It is reported, for the cigarette ash of this kind high antimony arsenic, the current main fire method of employing further realizes antimony with the method for wet method, arsenic is separated. CN102233229A discloses a kind of method of fire concentrate, the method utilizes the difference of white arsenic and antimonous oxide volatilization temperature and realizes substep volatilization, it is specially the white arsenic that first volatilizees at 680 DEG C, then it is warming up to 850 DEG C of volatilization antimonous oxides; But, thermal process energy consumption height, the separation of antimony, arsenic is not thorough, and exists containing problems such as arsenic powder dust pollutions. CN1312392 discloses a kind of method of wet separation, and this method adopts Na2S and NaOH mixed ammonium/alkali solutions leaching simultaneously antimony and arsenic, then use H2O2Oxide treatment sulphur immersion liquid, obtains thick sodium antimonate precipitation and the oxidation solution containing sodium arseniate; With in NaOH and obtain sodium pyroantimoniate after thick sodium antimonate precipitation HCl pickling, containing the oxidation solution of sodium arseniate by the obtained sodium arseniate of heating evaporation; The reagent consumption such as this method vulcanizing agent, oxygenant are big, cause this method process economy not good enough. CN103757424A discloses the technique of a kind of Selectively leaching process antimony arsenic flue dust, namely first antimony arsenic flue dust is mixed with SODIUMNITRATE, alkali, 400��680 DEG C of calcinings, after calcining, water logging is filtered, obtain sodium antimoniate filter cake and sodium arseniate solution, again sodium antimoniate filter cake and concentrated sodium arseniate solution are dried, obtain sodium antimoniate and sodium arseniate product respectively;This method technical process is simple, easily realizes antimony, arsenic separation, but due to roasting process operating procedure condition poor, and antimony, arsenic easily volatilizees, and very easily causes secondary pollution. In addition, also having the technique adopting acid method to leach, but owing to very easily generating the arsine gas of severe toxicity in acidleach process, require extremely high to operating process, environment is unfriendly.
Summary of the invention
Technical problem to be solved by this invention overcomes the deficiencies in the prior art, it is provided that a kind of fast, efficient, cost is low, flow process is simple, the method for antimony, arsenic separation in eco-friendly high antimony arsenic smoke dust, it is achieved the synthetical recovery of antimony and arsenic resource. The present invention, by leaching system being adjusted, changes the atmosphere of leaching system, makes the arsenic clean conversion in antimony arsenic smoke dust be the water-soluble arsenate of high-valence state, and antimony is converted into the very little stibnate of solubleness, thus realizes the high efficiency separation of arsenic and antimony.
It is an object of the invention to be achieved through the following technical solutions. Antimony and arsenic in antimony arsenic smoke dust mainly exist with the form of antimonous oxide and white arsenic. Owing to arsenic is amphoteric metal, for avoiding the generation of severe toxicity arsine gas, adopt sodium hydroxide or potassium hydroxide solution as the Selectively leaching agent of arsenic. Owing to sodium hydroxide and potassium hydroxide solution itself do not have oxidisability, need additional oxidizer to realize the oxidation of arsenic component, wherein the oxidizing potential of oxygen is higher, oxidisability induces one more by force and not other impurity, therefore select oxygen as oxygenant, adopt alkaline media pressure oxidation technology to leach the arsenic in antimony arsenic smoke dust. Antimony is then converted into the very little stibnate of solubleness in the basic solution of oxidizing atmosphere and enters slag phase, thus can realize being separated of antimony and arsenic. Adopt certain density NaOH or KOH solution when leading to the oxygenant of certain oxygen pressure, the antimony in antimony arsenic smoke dust and arsenic are separately converted to insoluble stibnate and solubility sodium arseniate, utilize the difference of the two solubleness can realize being separated of antimony and arsenic; Based on the dissolubility property of arsenic in alkaline medium, adopt evaporation to increase and dense prepares arsenate crystal with cooling crystallization technology; The alkaline media leaching process for antimony arsenic smoke dust capable of circulation after separation arsenic; Stibnate slag after separation arsenic can be used as the preparation of antimony ore raw material for antimony oxygen powder. The operating process of the method comprises:
(1) being the NaOH of 80��380g/L or KOH solution by antimony arsenic smoke dust and alkali concn is mixed to join in alkaline-resisting autoclave by liquid-solid ratio (volume mass than) 2.5:1��9:1, heating to temperature of reaction 90��280 DEG C, to lead to into oxygen pressure be the oxygen of 0.2��1.8MPa, air or oxygen rich gas, after reaction 1��3.5h, cooling slip to 90 DEG C, with bottom discharge, obtains reaction and completes slip;
(2) reaction obtained according to step (1) completes the alkali concn of slip, with water or low-concentration alkali liquor adjustment slip alkali concn at below 150g/L, filtering separation, filtrate is the rich arsenic leach liquor containing a large amount of arsenate, filter residue is mainly the very low stibnate of solubleness, removing arsenate subsidiary in stibnate slag with hot wash, can obtain stibnate slag, stibnate slag can be used as the preparation of antimony concentrate for antimony oxygen powder;
(3) the rich arsenic leach liquor that step (2) obtains being evaporated to alkali concn is 220��380g/L, and add the arsenate crystal seed of 0.1%��5%, carry out crystallisation by cooling, crystallization control terminal temperature is 35��55 DEG C, crystallization 2��12h, then carries out solid-liquor separation, and solid phase is arsenate crystal product, liquid phase is the crystalline mother solution containing a small amount of arsenic, and mother liquor is back to the alkaline pressure of oxygen leaching process of step (1).
Accompanying drawing explanation
Fig. 1 is the process diagram of the present invention.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but the technical scheme of the present invention is not limited to described scope.
Embodiment 1
Configuration alkali concn is the NaOH solution of 200g/L, antimony arsenic smoke dust (wherein Sb30.25%, As34.20%) and NaOH solution is mixed according to liquid-solid ratio 9:1, and is placed in alkaline-resisting autoclave heated and stirred; After feed temperature reaches 200 DEG C, in reactor, lead to the air into 1.0MPa, and start timing, after reaction 2h, below cooling slurry to 90 DEG C, obtain reaction and complete slip; It is 150g/L that diluting reaction completes slip to NaOH concentration, filters, and filter residue obtains sodium antimonate slag (wherein Sb36.94%) with 80��90 DEG C of hot washes, and the arsenic rate that contains in sodium antimonate slag is down to 0.01%, can be used as antimony concentrate and prepares antimony oxygen powder; It is 220g/L that filtrate is evaporated to NaOH concentration, the sodium arseniate crystal seed of 0.1% is added in the alkali lye of inspissation, stir and progressively it is cooled to 35 DEG C, filtering separation after crystallization 2h, solid phase is sodium arseniate crystal (wherein Sb0.18%), liquid phase is the NaOH solution containing a small amount of arsenic, returns the alkaline pressure of oxygen leaching process for next batch antimony arsenic smoke dust.
In the present embodiment, antimony recovery is 98.07%, and the arsenic rate of recovery is 98.70%.
Embodiment 2
Configuration alkali concn is the NaOH solution of 380g/L, antimony arsenic smoke dust (wherein Sb41.66%, As20.97%) and NaOH solution is mixed according to liquid-solid ratio 2.5:1, and is placed in alkaline-resisting autoclave heated and stirred; After feed temperature reaches 280 DEG C, in reactor, lead to the oxygen into 0.2MPa, and start timing, after reaction 1h, below cooling slurry to 90 DEG C, obtain reaction and complete slip; It is 100g/L that diluting reaction completes slip to NaOH concentration, filters, and filter residue obtains sodium antimonate slag (wherein Sb37.52%) with 80��90 DEG C of hot washes, and the arsenic rate that contains in sodium antimonate slag is down to 0.03%, can be used as antimony concentrate and prepares antimony oxygen powder; It is 380g/L that filtrate is evaporated to NaOH concentration, the sodium arseniate crystal seed of 2% is added in the alkali lye of inspissation, stir and progressively it is cooled to 45 DEG C, filtering separation after crystallization 12h, solid phase is sodium arseniate crystal (wherein Sb0.12%), liquid phase is the NaOH solution containing a small amount of arsenic, returns the alkaline pressure of oxygen leaching process for next batch antimony arsenic smoke dust.
In the present embodiment, antimony recovery is 99.07%, and the arsenic rate of recovery is 99.70%.
Embodiment 3
Configuration alkali concn is the NaOH solution of 80g/L, antimony arsenic smoke dust (wherein Sb16.16%, As45.29%) and NaOH solution is mixed according to liquid-solid ratio 5:1, and is placed in alkaline-resisting autoclave heated and stirred; After feed temperature reaches 90 DEG C, in reactor, lead to the oxygen rich gas into 1.8MPa, and start timing, after reaction 3.5h, obtain reaction and complete slip; Then solid-liquor separation, filter residue obtains sodium antimonate slag (wherein Sb28.36%) with 80��90 DEG C of hot washes, and the arsenic rate that contains in sodium antimonate slag is down to 0.14%, can be used as antimony concentrate and prepares antimony oxygen powder; It is 250g/L that filtrate is evaporated to NaOH concentration, the sodium arseniate crystal seed of 5% is added in the alkali lye of inspissation, stir and progressively it is cooled to 55 DEG C, filtering separation after crystallization 8h, solid phase is sodium arseniate crystal (wherein Sb0.05%), liquid phase is the NaOH solution containing a small amount of arsenic, returns the alkaline pressure of oxygen leaching process for next batch antimony arsenic smoke dust.
In the present embodiment, antimony recovery is 98.48%, and the arsenic rate of recovery is 98.73%.
Embodiment 4
Configuration alkali concn is the KOH solution of 80g/L, antimony arsenic smoke dust (wherein Sb21.80%, As37.44%) and KOH solution is mixed according to liquid-solid ratio 6:1, and is placed in alkaline-resisting autoclave heated and stirred; After feed temperature reaches 150 DEG C, in reactor, lead to the air into 1.5MPa, and start timing, after reaction 3h, below cooling slurry to 90 DEG C, obtain reaction and complete slip; Then solid-liquor separation, filter residue obtains potassium antimonate slag (wherein Sb29.67%) with 80��90 DEG C of hot washes, and the arsenic rate that contains in potassium antimonate slag is down to 0.06%, can be used as antimony concentrate and prepares antimony oxygen powder; It is 240g/L that filtrate is evaporated to KOH concentration, the potassium dihydrogen arsenate crystal seed of 0.5% is added in the alkali lye of inspissation, stir and progressively it is cooled to 40 DEG C, filtering separation after crystallization 4h, solid phase is potassium dihydrogen arsenate crystal (wherein Sb0.02%), liquid phase is the KOH solution containing a small amount of arsenic, returns the alkaline pressure of oxygen leaching process for next batch antimony arsenic smoke dust.
In the present embodiment, antimony recovery is 99.29%, and the arsenic rate of recovery is 99.60%.
Embodiment 5
Configuration alkali concn is the KOH solution of 380g/L, antimony arsenic smoke dust (wherein Sb26.09%, As51.24%) and KOH solution is mixed according to liquid-solid ratio 9:1, and is placed in alkaline-resisting autoclave heated and stirred; After feed temperature reaches 90 DEG C, in reactor, lead to the oxygen into 0.6MPa, and start timing, after reaction 2.5h, obtain reaction and complete slip. It is 150g/L that diluting reaction completes slip to KOH concentration, filters, and filter residue obtains potassium antimonate slag (wherein Sb43.95%) with 80��90 DEG C of hot washes, and the arsenic rate that contains in potassium antimonate slag is down to 0.12%, can be used as antimony concentrate and prepares antimony oxygen powder; It is 350g/L that filtrate is evaporated to KOH concentration, the potassium dihydrogen arsenate crystal seed of 0.4% is added in the alkali lye of inspissation, stir and progressively it is cooled to 50 DEG C, filtering separation after crystallization 10h, solid phase is potassium dihydrogen arsenate crystal (wherein Sb0.16%), liquid phase is the KOH solution containing a small amount of arsenic, returns the alkaline pressure of oxygen leaching process for next batch antimony arsenic smoke dust.
In the present embodiment, antimony recovery is 98.97%, and the arsenic rate of recovery is 99.10%.
Embodiment 6
Configuration alkali concn is the KOH solution of 300g/L, antimony arsenic smoke dust (wherein Sb24.15%, As12.53%) and KOH solution is mixed according to liquid-solid ratio 2.5:1, and is placed in alkaline-resisting autoclave heated and stirred; After feed temperature reaches 280 DEG C, in reactor, lead to the oxygen rich gas into 1.2MPa, and start timing, after reaction 2h, below cooling slurry to 90 DEG C, obtain reaction and complete slip; It is 150g/L that diluting reaction completes slip to KOH concentration, filters, and filter residue obtains potassium antimonate slag (wherein Sb21.61%) with 80��90 DEG C of hot washes, and the arsenic rate that contains in potassium antimonate slag is down to 0.02%, can be used as antimony concentrate and prepares antimony oxygen powder; It is 300g/L that filtrate is evaporated to KOH concentration, the sodium arseniate crystal seed of 1.5% is added in the alkali lye of inspissation, stir and progressively it is cooled to 35 DEG C, filtering separation after crystallization 3h, solid phase is potassium dihydrogen arsenate crystal (wherein Sb0.06%), liquid phase is the KOH solution containing a small amount of arsenic, returns the alkaline pressure of oxygen leaching process for next batch antimony arsenic smoke dust.
In the present embodiment, antimony recovery is 99.86%, and the arsenic rate of recovery is 99.30%.
Claims (4)
1. in antimony arsenic smoke dust, antimony soaks the method being separated with arsenic alkali oxide, and the method comprises the following steps:
1) alkaline solution of antimony arsenic smoke dust and alkali concn 80��380g/L is mixed to join in alkaline-resisting autoclave by liquid-solid ratio (volume mass than) 2.5:1��9:1, lead to the gaseous oxidant into certain pressure, react 1��3.5h at a certain temperature, slip is cooled to 90 DEG C with bottom discharge after terminating by reaction, obtains reaction and completes slip;
2) by step 1) reaction that obtains completes the alkali concn water of slip or low-concentration alkali liquor is adjusted to below alkali concn 150g/L, then filtering separation is carried out, filtrate is rich arsenic leach liquor, filter residue is mainly stibnate, filter residue is with 80��90 DEG C of hot washes, obtained stibnate slag, can be used as the preparation of antimony concentrate for antimony oxygen powder;
3) by step 2) to be evaporated to alkali concn be 220��380g/L for the rich arsenic leach liquor that obtains, and add the arsenate crystal seed of 0.1%��5%, carry out crystallisation by cooling, crystallization control terminal temperature is 35��55 DEG C, crystallization 2��12h, then carries out solid-liquor separation, and solid phase is arsenate crystal, liquid phase is the crystalline mother solution containing a small amount of arsenic, and mother liquor is back to step 1) alkaline pressure of oxygen leaching process.
2. the method for claim 1, is characterized in that: described step 1) in alkaline solution be sodium hydroxide or potassium hydroxide solution.
3. the method for claim 1, is characterized in that: described step 1) in gaseous oxidant be oxygen, air or oxygen level be the oxygen rich gas of 21��100%.
4. the method for claim 1, is characterized in that: described step 1) in temperature of reaction be 90��280 DEG C, the oxygen partial pressure of gaseous oxidant is 0.2��1.8MPa.
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Cited By (7)
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| CN106756031A (en) * | 2016-11-23 | 2017-05-31 | 昆明理工大学 | A kind of method that lead antimony and arsenic are separated in the alkaline leaching solution from the earth of positive pole |
| CN107326188A (en) * | 2017-06-29 | 2017-11-07 | 郴州市金贵银业股份有限公司 | A kind of method for preparing sodium pyroantimonate with leaded silver-colored arsenic antimony cigarette ash |
| CN107858521A (en) * | 2017-12-07 | 2018-03-30 | 郴州市金贵银业股份有限公司 | The method that cigarette ash containing antimony prepares sodium pyroantimonate |
| CN111135674A (en) * | 2020-01-07 | 2020-05-12 | 华北电力大学（保定） | Absorption liquid for collecting gas-phase arsenic with different valence states |
| CN113174479A (en) * | 2021-04-28 | 2021-07-27 | 中南大学 | Antimony sulfide concentrate volatilizing roasting process |
| CN113699380A (en) * | 2021-07-15 | 2021-11-26 | 湖南有色金属研究院有限责任公司 | Arsenic-antimony smoke treatment method |
| CN115044782A (en) * | 2022-06-23 | 2022-09-13 | 江西理工大学 | Method for deeply removing arsenic from arsenic-antimony secondary material and preparing sodium antimonate |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106756031A (en) * | 2016-11-23 | 2017-05-31 | 昆明理工大学 | A kind of method that lead antimony and arsenic are separated in the alkaline leaching solution from the earth of positive pole |
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| CN107326188A (en) * | 2017-06-29 | 2017-11-07 | 郴州市金贵银业股份有限公司 | A kind of method for preparing sodium pyroantimonate with leaded silver-colored arsenic antimony cigarette ash |
| CN107326188B (en) * | 2017-06-29 | 2019-03-08 | 郴州市金贵银业股份有限公司 | A method of sodium pyroantimonate is prepared with leaded silver-colored arsenic antimony cigarette ash |
| CN107858521A (en) * | 2017-12-07 | 2018-03-30 | 郴州市金贵银业股份有限公司 | The method that cigarette ash containing antimony prepares sodium pyroantimonate |
| CN111135674A (en) * | 2020-01-07 | 2020-05-12 | 华北电力大学（保定） | Absorption liquid for collecting gas-phase arsenic with different valence states |
| CN113174479A (en) * | 2021-04-28 | 2021-07-27 | 中南大学 | Antimony sulfide concentrate volatilizing roasting process |
| CN113174479B (en) * | 2021-04-28 | 2022-06-07 | 中南大学 | Antimony sulfide concentrate volatilizing roasting process |
| CN113699380A (en) * | 2021-07-15 | 2021-11-26 | 湖南有色金属研究院有限责任公司 | Arsenic-antimony smoke treatment method |
| CN115044782A (en) * | 2022-06-23 | 2022-09-13 | 江西理工大学 | Method for deeply removing arsenic from arsenic-antimony secondary material and preparing sodium antimonate |
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Application publication date: 20160608 |