CN101899574B - 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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CN101899574B
CN101899574B CN2010102441814A CN201010244181A CN101899574B CN 101899574 B CN101899574 B CN 101899574B CN 2010102441814 A CN2010102441814 A CN 2010102441814A CN 201010244181 A CN201010244181 A CN 201010244181A CN 101899574 B CN101899574 B CN 101899574B
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arsenic
antimony
sulfur dioxide
solution
slag
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CN101899574A (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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锡矿山闪星锑业有限责任公司
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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, sulfurdioxide 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 technicalprocess, 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 themethod 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 with antimony concentrate blast furnace volatile smelting---and the technical process of antimony reverberatory furnace retailoring purified is main.Stibium blast furnace is high with its siege processing power, and is strong to adaptability to raw material, characteristics such as metal recovery rate height; Receive the generally favor of antimony smelting enterprise, but stibium blast furnace produces antimony sulfonium, needle antimony output capacity high (about 20~30%), foreign matter content high (about 15~30%); Can only get into stibium blast furnace once more as the article 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 dioxide gas 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 permanent white 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 it is high that liquor sodii arsenatis is dried to anhydrous arsenic acid sodium cost, the while inconvenient operation, and the SO 2 from fume that produces in the antimony regulus process is not fully used.

The concentration that the waste gas that produces in the antimony metallurgical process in addition not only contains sulfurous gas has only 0.6~1.0%; 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, and 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 peanuts basically all is direct discharging, sulfur dioxide gas with contain antimony powder dirt and all can cause huge pollution 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.Thoroughly handled with comprehensive with the sulfurous gas of low levels in reluctant arsenic alkali slag that the antimony regulus process is produced and the waste gas and to be reclaimed the ability 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; Reacted 1-2 hour, using the sulphur acid for adjusting pH value is 6.0~7.0, 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 of absorbing sulfur dioxide after-filtration and deeply removing arsenic obtain are all concentrated and are got into blast furnace; Be used to reclaim antimony; The 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 reaction formula is following:

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 43=FeAsO 3↓+3?H 2SO 4

Side reaction mainly contains: Na 2S+H 2SO 3=H 2S ↑+Na 2SO 3

Said 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 instance 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 following:

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 Sb, the shared per-cent of As are: Sb 90.03%, and As 7.28%).

(2), a leach liquor 205L, concentration is: Sb 11.79g/L, As 33.92g/L; (wherein Sb, the shared per-cent of As are: Sb 7.48%, and As 76.50%).

(3), secondary leach liquor 141L, concentration is: Sb 5.71g/L, As 10.46g/L; (wherein Sb, the shared per-cent of As are: Sb 2.49%, and As 16.22%).

2, absorbing sulfur dioxide

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 be made into 16L solution under agitation slowly add 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 ℃, stir down and in sulfuration dearsenification solution, slowly add 1.5kg ferric sulfate, carry out the 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 ℃, stir down and in the solution of the deeply removing arsenic first time, slowly add 0.52kg ferric sulfate, 1 hour time, control pH value 6.9.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:

With carrying out condensing crystal behind the adjusting of the sodium sulfite solution after secondary deep deironing pH value to 11~12, the pneumatic dryer after the centrifuge dehydration under 250~300 ℃ is dry, 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 after As 0.85%, the absorbing sulfur dioxide, 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 mixing takes the raw material as stibium blast furnace with other high-grade antimony concentrate again, reclaims antimony.Iron level wherein can be used for slag making in the stove.The antimony that gets into 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, absorbing sulfur dioxide

Other gets a leach liquor 50L in the plastics steel basin, under 30-45 ℃ of stirring, feeds sulfur dioxide flue gas in the antimony regulus process (SO wherein 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 be made into 16L solution under agitation slowly add 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 ℃, stir down and in sulfuration dearsenification solution, slowly add 3.0kg ferric sulfate, carry out the 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 ℃, stir down and in the solution of the deeply removing arsenic first time, slowly add 0.50kg ferric sulfate, 1 hour time, control pH value 6~9.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 after the centrifuge dehydration under 250~300 ℃ is dry, obtains dried S-WAT 21kg, analyzes composition to be: Na 2SO 3Content 93%, Fe content 20ppm, As content 1ppm.

In the whole process, the recovery of antimony is 99.1%, and arsenic is 91.4% through red arsenic open circuit rate.

Embodiment 3

1, absorbing sulfur dioxide

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 be made into 6L solution under agitation slowly add 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 ℃, stir down and in sulfuration dearsenification solution, slowly add 2.6kg ferric sulfate, carry out the 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 ℃, stir down and in the solution of the deeply removing arsenic first time, slowly add 0.6kg ferric sulfate, 1 hour time, control pH value 6~9.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

With carrying out condensing crystal behind the adjusting of the sodium sulfite solution after secondary deep deironing pH value to 11~12, the pneumatic dryer after the centrifuge dehydration under 250~300 ℃ is dry, obtains dried S-WAT 5kg, analyzes composition to be: Na 2SO 3Content 65%, Fe content 25ppm, As content 1ppm.

In the whole process, the recovery of antimony is 99.2%, and arsenic is 91.3% through red arsenic open circuit rate.

Claims (3)

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, the said vulcanizing agent aqueous solution is sodium sulphite, hydrogen sulfide or the Iron sulfuret aqueous solution; Reacted 1-2 hour, using the sulphur acid for adjusting pH value is 6.0~7.0, 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 of absorbing sulfur dioxide after-filtration and deeply removing arsenic obtain are all concentrated and are got into blast furnace, are used to reclaim antimony, and the recovery of antimony reaches more than 99%; The slag major ingredient of sulfuration dearsenification is red 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, said ferric sulfate is the bodied ferric sulfate of technical grade.
3. method according to claim 1 is characterized in that, the arsenic content in the solution after the deeply removing arsenic in said (4) step is handled is less than 0.5mg/L, contains that iron level is more than 20% in the arsenic scum.
CN2010102441814A 2010-08-04 2010-08-04 Method for comprehensively reclaiming arsenic caustic dross and sulfur dioxide flue gas in antimony pyrometallurgical smelting CN101899574B (en)

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CN102351360B (en) * 2011-07-04 2013-05-01 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
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
CN102560132B (en) * 2012-02-03 2013-06-12 锡矿山闪星锑业有限责任公司 Method for treating selenium alkali residues in antimony pyro-refining
CN103551025B (en) * 2013-08-27 2015-06-03 昆明理工大学 Harmless treatment method of arsenic-containing flue dust
CN104085903B (en) * 2014-06-27 2015-12-09 锡矿山闪星锑业有限责任公司 A kind of from the method containing separating-purifying sodium hydroxide arsenic 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
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
CN107963642A (en) * 2017-12-29 2018-04-27 焱鑫环保科技有限公司 SO is absorbed using the water logging of industrial caustic containing arsenic lye2The process of flue gas, dearsenification purification production sodium sulfite product
CN109439911A (en) * 2019-01-02 2019-03-08 湖南省环境保护科学研究院 Arsenic alkaline slag disposal system and the method for handling arsenic alkaline slag using it
CN109913659A (en) * 2019-02-27 2019-06-21 郴州钖涛环保科技有限公司 A kind of method of antimony smelting arsenic alkali slag and flue gas during smelting comprehensive treatment

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