CN101899574A - Method for comprehensively reclaiming arsenic caustic dross and sulfur dioxide flue gas in antimony pyrometallurgical smelting - Google Patents

Method for comprehensively reclaiming arsenic caustic dross and sulfur dioxide flue gas in antimony pyrometallurgical smelting Download PDF

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CN101899574A
CN101899574A CN2010102441814A CN201010244181A CN101899574A CN 101899574 A CN101899574 A CN 101899574A CN 2010102441814 A CN2010102441814 A CN 2010102441814A CN 201010244181 A CN201010244181 A CN 201010244181A CN 101899574 A CN101899574 A CN 101899574A
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arsenic
antimony
sulfur dioxide
slag
solution
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CN101899574B (en
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单桃云
刘鹊鸣
谈应顺
戴永俊
李志强
邓卫华
姚兴娜
曾雁
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TINNERY SHANXING ANTIMONY INDUSTRY LLC
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Abstract

The invention discloses a method for comprehensively reclaiming arsenic caustic dross and sulfur dioxide flue gas in antimony pyrometallurgical smelting. The method comprises the following steps: arsenic containing caustic dross in the antimony smelting process is leached; waste gas sulfur dioxide in the antimony-containing alkaline solution is absorbed; vulcanizer is used for dearsenizing; ferric sulfate is used for further dearsenizing; and purification, concentration and drying are performed; and the like. Therefore, the hard treated arsenic caustic dross and low content sulfur dioxide of the waste gas, which are generated in the antimony smelting process, can be treated completely, wherein the antimony reclaiming rate reaches 99 percent, arsenic removal rate is over 90 percent, sulfur dioxide removal rate is over 95 percent through absorption, so that the gas reaches emission standard, and alkali is transformed into sodium sulfite. The method has the advantages of simple technical process, small equipment investment, remarkable economic benefit and environmental benefit, completely solves the arsenic caustic dross and waste gas sulfur dioxide in the antimony smelting process, and cleans the antimony smelting process. Water solution in the whole process is circulated in a closed loop without wastewater discharge, and the waste gas is qualified to be exhausted to air, so the method is a clean and environment-friendly process.

Description

The method of comprehensively reclaiming arsenic caustic dross and sulfur dioxide flue gas in a kind of antimony pyrometallurgical smelting
Technical field
The present invention relates to the method for comprehensively reclaiming arsenic caustic dross and sulfur dioxide flue gas in a kind of antimony pyrometallurgical smelting.
Background technology
At present, the antimony production technique adopts pyrometallurgical smelting process more than 90% both at home and abroad, and pyrometallurgical smelting process is again based on antimony concentrate blast furnace volatile smelting---the technical process of antimony reverberatory furnace retailoring purified.Stibium blast furnace is with its siege processing power height, strong to adaptability to raw material, characteristics such as metal recovery rate height, be subjected to the generally favor of antimony smelting enterprise, but stibium blast furnace produces antimony sulfonium, needle antimony output capacity height (about 20～30%), foreign matter content height (about 15～30%), can only enter stibium blast furnace once more as the product that return handles, not only consume a large amount of energy consumptions, and influence a series of technico-economical comparisones such as processed in units amount of stibium blast furnace, thereby production cost is raise.
CN200410023055.0 discloses " pollution-free arsenic alkali slag treatment process ", adopts the carbon dioxide dealkalize, and the carbonate that filters the back output returns antimony and smelts, and waste water returns use.There is long flow path in this method; Contain a certain amount of sodium sulfate etc. in the carbonate of output, return the antimony smelting and will reduce result of use; Need to use more hydrated barta sulfate precipitate sodium, produce the more high barium sulfate slag of arsenic that contains simultaneously.CN03118325.5 discloses " treatment process of arsenic-containing material ", this method adopt water logging, in and after the ammonia still process, the carbonization of suction ammonia, arsenic removal process, obtain the antimony slag and return antimony regulus, obtain red arsenic and be used to refine arsenic, and obtain containing the high sodium salt of arsenic.This method adopts adds more ammonium sulfate or sulfuric acid or hydrochloric acid, and liquor sodii arsenatis is dried to anhydrous arsenic acid sodium cost height, the while inconvenient operation, and the SO 2 from fume that produces in the antimony regulus process is not fully used.
The waste gas that produces in the antimony metallurgical process concentration that not only contains sulfurous gas has only 0.6～1.0% in addition, economic utilization concentration well below sulfurous gas, but also contain lower concentration and ultra-fine grain contain antimony powder dirt, the antimony powder dust concentration has only 10 mg/L～30mg/L, granularity is less than 2 microns, and routine techniques is difficult to economy and catches.Low concentration sulphur dioxide flue gas in the antimony metallurgical process never finds effective improvement technology at present, have only a few big factory to adopt lime method desulfurization technology to carry out desulfurization, but this technology exists that desulfuration efficiency is low, desulphurization cost is high (product per ton increases by 500 yuan of desulphurization costs), in the waste gas contain antimony powder dirt can not comprehensive reutilization, desulfurization slag can only store up and exist secondary pollution problem.The waste gas of other small businesss substantially all is direct discharging, and sulfur dioxide gas and contain antimony powder dirt and all can cause huge pollution to surface soil and surface water also can directly influence people's drinking water safety.
Summary of the invention
The object of the present invention is to provide the method for a kind of comprehensively reclaiming arsenic caustic dross and sulfur dioxide flue gas.Sulfurous gas with low levels in reluctant arsenic alkali slag that the antimony regulus process is produced and the waste gas is thoroughly handled and comprehensive the recovery, can changing waste into valuables; Simultaneously can realize not causing pollution again to environment.
Technical scheme of the present invention may further comprise the steps:
(1) leaching of arsenic alkali slag: the water that in arsenic alkali slag, adds 2 times of arsenic alkali slag quality; Feeding is steam heated to 90-100 ℃, agitation leach 30-60 minute; Repeat once, filter;
(2) sulfurous gas neutralization: in leach liquor, feed form waste gas of sulfur dioxide, at 20-50 ℃ of neutralization reaction 10-20 hour, reduction high price antimony and high price arsenic; When the pH of solution value reaches 3-6, stop ventilation;
(3) sulfuration dearsenification: at 20～40 ℃ of temperature, the dropping chemistry amount 1.0-2.0 vulcanizing agent aqueous solution doubly; Reacting 1-2 hour, is 6.0～7.0 with the sulphur acid for adjusting pH value, static 2-6 hour, and filtering separation arsenic sulfide slag and low arsenic sodium sulfite solution; The stink damp body and function that produces contains returns dearsenification after arsenic alkali solution water absorbs;
(4) deeply removing arsenic: in low arsenic sodium sulfite solution, slowly add the ferric sulfate of As content mol ratio in the solution, reacted 1 hour, to the pH value be 6-9; Static 4 hours, filter out and contain the arsenic scum, repeat again 1 time;
(5) the comprehensive recovery:
(A) sodium sulfite solution after the secondary deep arsenic removal is regulated pH value to 11～12 after condensing crystal, drying obtain S-WAT;
(B) reclaim antimony, arsenic: two kinds of scums that the antimony slag in the leached mud in the process, the antimony slag that absorbs the sulfurous gas after-filtration and deeply removing arsenic obtain are all concentrated and are entered blast furnace, be used to reclaim antimony, the rate of recovery of antimony reaches more than 99%, and wherein arsenic returns antimony system about 9%; The slag major ingredient of sulfuration dearsenification is red arsenic, is sold to refining arsenic enterprise as the raw material that refines arsenic.This part arsenic is that arsenic in the arsenic alkali slag is more than 90%.
Its chemical equation is as follows:
2NaOH+SO 2=Na 2SO 3+H 2O
Na 2CO 3+SO 2=Na 2SO 3+CO 2↑
Na 3AsO 4+SO 2+H 2O=Na 3AsO 3+H 2SO 4
2?Na 3AsO 3+3SO 2+H 2O=3Na 2SO 3+HAsO 2
2H 3AsO 3+Na 2S=As 2S 3↓+6NaOH
2H 3AsO 3+Fe 2（SO 4） 3=FeAsO 3↓+3?H 2SO 4
Side reaction mainly contains: Na 2S+H 2SO 3=H 2S ↑+Na 2SO 3
Described vulcanizing agent is sodium sulphite, hydrogen sulfide, Iron sulfuret.
The present invention is thoroughly handled the reluctant arsenic alkali slag of antimony regulus process generation and the sulfurous gas of waste gas low levels, and antimony recovery reaches 99%; Arsenic open circuit rate surpasses 90%, and the sulfur in smoke specific absorption surpasses 95%, makes gas reach emission standard; Alkali is converted into S-WAT.Technical process is simple, and facility investment is few; Economic benefit and environmental benefit highly significant, one action has solved and has contained arsenic alkali slag and waste gas sulfurous gas in the antimony regulus process, has cleaned the antimony regulus process.Aqueous solution closed cycle in the whole process does not have waste water to efflux, and exhaust gas emission is up to standard.The present invention has reached the purpose of waste recycling, is the technology of a clean environment firendly.
Embodiment
Below in conjunction with example the present invention is further specified.
Embodiment 1
1, water logging: in 500 liters stainless steel reaction jar, add antimony smelting arsenic alkali slag and (contain antimony 21.55%, arsenic 6.06%, yellow soda ash and sodium hydroxide 60%) 300 liters in 150kg and water, stir down with being steam heated to 95 ℃, 40 minutes reaction times, filter for the first time, filter residue adds 100 liters in water again, reacts 60 minutes down at 90 ℃, carry out the second time and filter, its input-output situation is as follows:
Drop into:
Arsenic alkali slag weight 150kg, grade is: Sb 21.55%, and As 6.06%; (wherein: Sb 100%, and As 100%).
Output:
(1), antimony slag dry weight 77.88kg, grade is: Sb 37.37%, As 0.85%; (wherein the shared per-cent of Sb, As is: Sb 90.03%, and As 7.28%).
(2), a leach liquor 205L, concentration is: Sb 11.79g/L, As 33.92g/L; (wherein the shared per-cent of Sb, As is: Sb 7.48%, and As 76.50%).
(3), secondary leach liquor 141L, concentration is: Sb 5.71g/L, As 10.46g/L; (wherein the shared per-cent of Sb, As is: Sb 2.49%, and As 16.22%).
2, absorb sulfurous gas
Get a leach liquor 50L in the plastics steel basin, under 20-35 ℃ of stirring, feed sulfur dioxide flue gas in the antimony regulus process (SO wherein 2Concentration is: 16000～29000mg/m 3, antimony content is seldom), after 15 hours, the pH value of solution is 3.5～4.5, stops ventilation, and static 10 hours after-filtration obtain dried antimony slag 1.03kg, and composition is: Sb 52.81%, and As 0.49%; Solution becomes reducing solution, and its composition is: Sb 0.91g/L, As 33.81g/L; After SO 2 tail gas absorbed through a leach liquor foam, content was 700mg/m 3Directly (standard of emptying is 800mg/m in emptying 3), the specific absorption of sulfurous gas is 96%.
3, sulfuration dearsenification
20～40 ℃, sodium sulphite 8.45kg is made into 16L solution and under agitation slowly adds in the reduced liquid in 2,1.5 hours time, control pH value is 6.0～7.0, static 2-6 hour after-filtration, obtain arsenic sulfide slag dry weight 5.37kg, composition is: Sb0.62%, and As 30.99%; Liquor capacity 66L, composition is: Sb 0.15g/L, As 0.4g/L.
4, deeply removing arsenic
20～30 ℃, in sulfuration dearsenification solution, slowly add 1.5kg ferric sulfate under stirring, carry out deeply removing arsenic first time, 1 hour time, control pH value 6-9.Static 4 hours, filter and obtain dried scum 2.08kg, composition is: Sb 0.57%, and Fe 13.00%, and As 1.21%; As 15mg/L in the solution, volume 65L.
20～30 ℃, in the solution of the deeply removing arsenic first time, slowly add 0.52kg ferric sulfate, 1 hour time, control pH value 6.9 under stirring.Static 4 hours, filter and obtain dried scum 0.32kg, composition is: Fe 28.56%, and As 0.30%; As 0.25mg/L in the solution, volume 65L.
5, the comprehensive recovery:
A produces S-WAT:
To carry out condensing crystal behind the adjusting of the sodium sulfite solution after secondary deep deironing pH value to 11～12, the pneumatic dryer drying after the centrifuge dehydration under 250～300 ℃ obtains dried S-WAT 29kg, analyzes composition to be: Na 2SO 3Content 76%, Fe content 25ppm, As content 1ppm.(S-WAT more than 60% can be used as industry and uses).
The recovery of B antimony:
Antimony slag dry weight 77.88kg in the leached mud in the process, grade is: Sb 37.37%, the antimony slag antimony slag 1.03kg behind As 0.85%, the absorption sulfurous gas, composition is: Sb 52.81%, and As 0.49%; And the scum 2.08kg first time that obtains of deeply removing arsenic, composition is: Sb 0.57%, and Fe 13.00%, As 1.21% and scum 0.32kg for the second time, composition is: Fe 28.56%, and As 0.30% all mixes with other high-grade antimony concentrate again and takes raw material as stibium blast furnace, reclaims antimony.Iron level wherein can be used for slag making in the stove.The antimony that enters blast furnace is the antimony 99.2% in the arsenic alkali slag.
The slag that sulfuration dearsenification in the process produces is 5.37kg, and composition is: Sb0.62%, and As 30.99%, and this part slag is sold to refining arsenic factory as the raw material of carrying arsenic, is open circuit arsenic.This part arsenic is 91.5% of input amount.Therefore, dark open circuit rate is 91.5%.
Embodiment 2
1, absorbs sulfurous gas
Other gets a leach liquor 50L in the plastics steel basin, feeds sulfur dioxide flue gas in the antimony regulus process (SO wherein under 30-45 ℃ of stirring 2Concentration is: 16000～29000mg/m 3, antimony content is seldom), after 13 hours, the pH value of solution is 4.0～5.5, stops ventilation, and static 8 hours after-filtration obtain dried antimony slag 1.10kg, and composition is: Sb 50.87%, and As 0.15%; Solution becomes reducing solution, and its composition is: Sb 0.87g/L, As 33.88g/L; After SO 2 tail gas absorbed through a leach liquor foam, content was 710mg/m 3Directly (standard of emptying is 800mg/m in emptying 3), the specific absorption of sulfurous gas is 95.5%.
2, sulfuration dearsenification
20～40 ℃, sodium sulphite 8.00kg is made into 16L solution and under agitation slowly adds in the reduced liquid in 1,1.0 hours time, control pH value is 6.0～7.0, static 6 hours after-filtration, obtain arsenic sulfide slag dry weight 5.56kg, composition is: Sb 0.40%, and As 29.72%; Liquor capacity 65L, composition is: Sb 0.10g/L, As 0.5g/L.
3, deeply removing arsenic
20～30 ℃, in sulfuration dearsenification solution, slowly add 3.0kg ferric sulfate under stirring, carry out deeply removing arsenic first time, 2 hours time, control pH value 6-9.Static 4 hours, filter and obtain dried scum 2.16kg, composition is: Sb 0.35%, and Fe 25.00%, and As 1.47%; As 10mg/L in the solution, volume 63L.
20～30 ℃, in the solution of the deeply removing arsenic first time, slowly add 0.50kg ferric sulfate, 1 hour time, control pH value 6～9 under stirring.Static 4 hours, filter and obtain dried scum 0.30kg, composition is: Fe 30.00%, and As 0.20%; As 0.30mg/L in the solution, volume 62L.
4, produce S-WAT
After the adjusting of the sodium sulfite solution after secondary deep deironing pH value to 11～12, purification, carry out condensing crystal, the pneumatic dryer drying after the centrifuge dehydration under 250～300 ℃ obtains dried S-WAT 21kg, analyzes composition to be: Na 2SO 3Content 93%, Fe content 20ppm, As content 1ppm.
In the whole process, the rate of recovery of antimony is 99.1%, and arsenic is 91.4% by red arsenic open circuit rate.
Embodiment 3
1, absorbs sulfurous gas
Get a leach liquor 50L in the plastics steel basin, under 40-50 ℃ of stirring, feed sulfur dioxide flue gas in the antimony regulus process (SO wherein 2Concentration is: 16000～29000mg/m 3, antimony content is seldom), after 18 hours, the pH value of solution is 3.5～4.5, stops ventilation, and static 8 hours after-filtration obtain dried antimony slag 0.52kg, and composition is: Sb 51.67%, and As 0.60%; Solution becomes reducing solution, and its composition is: Sb 0.33g/L, As 10.38g/L; After SO 2 tail gas absorbed through a leach liquor foam, content was 720mg/m 3Directly (standard of emptying is 800mg/m in emptying 3), the specific absorption of sulfurous gas is 95%.
2, sulfuration dearsenification
20～40 ℃, sodium sulphite 2.6kg is made into 6L solution and under agitation slowly adds in the reduced liquid in 1,1.0 hours time, control pH value is 6.0～7.0, static 8 hours after-filtration, obtain arsenic sulfide slag dry weight 1.42kg, composition is: Sb 0.60%, and As 33.93%; Liquor capacity 53L, composition is: Sb 0.76g/L, As 0.7g/L.
3, deeply removing arsenic
20～30 ℃, in sulfuration dearsenification solution, slowly add 2.6kg ferric sulfate under stirring, carry out deeply removing arsenic first time, 2 hours time, control pH value 6-9.Static 4 hours, filter and obtain dried scum 2.03kg, composition is: Fe 23.15%, and As 1.72%; As 20mg/L in the solution, volume 50L.
20～30 ℃, in the solution of the deeply removing arsenic first time, slowly add 0.6kg ferric sulfate, 1 hour time, control pH value 6～9 under stirring.Static 4 hours, filter and obtain dried scum 0.35kg, composition is: Fe30.76%, As0.28%; As0.13mg/L in the solution, volume 48L.
4, produce S-WAT
To carry out condensing crystal behind the adjusting of the sodium sulfite solution after secondary deep deironing pH value to 11～12, the pneumatic dryer drying after the centrifuge dehydration under 250～300 ℃ obtains dried S-WAT 5kg, analyzes composition to be: Na 2SO 3Content 65%, Fe content 25ppm, As content 1ppm.
In the whole process, the rate of recovery of antimony is 99.2%, and arsenic is 91.3% by red arsenic open circuit rate.

Claims (4)

1. the method for comprehensively reclaiming arsenic caustic dross and sulfur dioxide flue gas in the antimony pyrometallurgical smelting is characterized in that, may further comprise the steps:
(1) leaching of arsenic alkali slag: the water that in arsenic alkali slag, adds 2 times of arsenic alkali slag quality; Feeding is steam heated to 90-100 ℃, agitation leach 30-60 minute; Repeat once, filter;
(2) sulfurous gas neutralization: in leach liquor, feed form waste gas of sulfur dioxide, at 20-50 ℃ of neutralization reaction 10-20 hour, reduction high price antimony and high price arsenic; When the pH of solution value reaches 3-6, stop ventilation;
(3) sulfuration dearsenification: at 20～40 ℃ of temperature, the dropping chemistry amount 1.0-2.0 vulcanizing agent aqueous solution doubly; Reacting 1-2 hour, is 6.0～7.0 with the sulphur acid for adjusting pH value, static 2-6 hour, and filtering separation arsenic sulfide slag and low arsenic sodium sulfite solution; The stink damp body and function that produces contains returns dearsenification after arsenic alkali solution water absorbs;
(4) deeply removing arsenic: in low arsenic sodium sulfite solution, slowly add the ferric sulfate of As content mol ratio in the solution, reacted 1 hour, to the pH value be 6-9; Static 4 hours, filter out and contain the arsenic scum, repeat again 1 time;
(5) the comprehensive recovery:
(A) sodium sulfite solution after the secondary deep arsenic removal is regulated pH value to 11～12 after condensing crystal, drying obtain S-WAT;
(B) reclaim antimony, arsenic: two kinds of scums that the antimony slag in the leached mud in the process, the antimony slag that absorbs the sulfurous gas after-filtration and deeply removing arsenic obtain are all concentrated and are entered blast furnace, be used to reclaim antimony, the rate of recovery of antimony reaches more than 99%, and wherein arsenic returns antimony system about 9%; The slag major ingredient of sulfuration dearsenification is red arsenic, is sold to refining arsenic enterprise as the raw material that refines arsenic, and this part arsenic is that arsenic in the arsenic alkali slag is more than 90%.
2. method according to claim 1 is characterized in that, described vulcanizing agent is sodium sulphite, hydrogen sulfide, Iron sulfuret.
3. method according to claim 1 is characterized in that, described ferric sulfate is the bodied ferric sulfate of technical grade.
4. deeply removing arsenic according to claim 2 is characterized in that, the solution arsenic content after the processing is less than 0.5mg/L, contains that iron level is more than 20% in the arsenic scum.
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CN102286665A (en) * 2011-09-05 2011-12-21 耒阳市焱鑫有色金属有限公司 Comprehensive recovery method for complicated materials containing arsenic and valuable metal slag dust
CN102351360A (en) * 2011-07-04 2012-02-15 锡矿山闪星锑业有限责任公司 Method for comprehensive recovery of arsenic-containing alkaline liquid and waste gas of sulfur dioxide
CN102560132A (en) * 2012-02-03 2012-07-11 锡矿山闪星锑业有限责任公司 Method for treating selenium alkali residues in antimony pyro-refining
CN103551025A (en) * 2013-08-27 2014-02-05 昆明理工大学 Harmless treatment method of arsenic-containing flue dust
CN104085903A (en) * 2014-06-27 2014-10-08 锡矿山闪星锑业有限责任公司 Method for separating and purifying sodium hydroxide from arsenic-containing sodium hydroxide solution
CN106480319A (en) * 2016-10-26 2017-03-08 山东国大黄金股份有限公司 A kind of method of the immersion cleaning treatment hydrogen containing tail gas synthetical recovery antimony of alkali containing antimony
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CN109876630A (en) * 2019-03-06 2019-06-14 株洲三特环保节能股份有限公司 A method of sulfur dioxide flue gas is administered with alkaline scrap material and recycles tin antimony metal and sodium sulfite crystal
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WO2019127305A1 (en) * 2017-12-29 2019-07-04 焱鑫环保科技有限公司 Processing method for producing sodium sulfite product by so2 flue gas absorption and arsenic-removal purification using leaching solution of arsenic-containing industrial alkaline residue
WO2020133210A1 (en) * 2018-12-28 2020-07-02 焱鑫环保科技有限公司 Method for producing sodium sulfite by removing sulfur from sulfur-containing flue gas using industrial alkali residue containing arsenic
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CN112961987A (en) * 2021-02-01 2021-06-15 中国科学院沈阳应用生态研究所 Harmless and recycling treatment method for arsenic alkali slag
CN113443690A (en) * 2021-07-05 2021-09-28 上海交通大学 Method for enhancing sulfuration treatment of arsenic-containing wastewater by using sulfur dioxide

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CN102351360A (en) * 2011-07-04 2012-02-15 锡矿山闪星锑业有限责任公司 Method for comprehensive recovery of arsenic-containing alkaline liquid and waste gas of sulfur dioxide
CN102286665A (en) * 2011-09-05 2011-12-21 耒阳市焱鑫有色金属有限公司 Comprehensive recovery method for complicated materials containing arsenic and valuable metal slag dust
CN102286665B (en) * 2011-09-05 2012-10-31 耒阳市焱鑫有色金属有限公司 Comprehensive recovery method for complicated materials containing arsenic and valuable metal slag dust
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