CN1559885A - Technology of extracting fine sulphur from produced antimonic white slag by wet process production - Google Patents
Technology of extracting fine sulphur from produced antimonic white slag by wet process production Download PDFInfo
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- CN1559885A CN1559885A CNA2004100229290A CN200410022929A CN1559885A CN 1559885 A CN1559885 A CN 1559885A CN A2004100229290 A CNA2004100229290 A CN A2004100229290A CN 200410022929 A CN200410022929 A CN 200410022929A CN 1559885 A CN1559885 A CN 1559885A
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Abstract
The invention discloses a technique of extracting refined sulfur from stibium trioxide slags of wet production, and its technical steps: (1) fully stirring and mixing stibium trioxide slags with extractant in weight ratio of 1 to 7-8, heating to 140 deg.C-160 deg.C, preserving heat for 15-20 minutes and continuously vibrating and stirring; (2) fast filtering, and making solid-liquid separation, where the filtering time is 30-35 minutes; (3) heating the obtained mixed filtrate in a heater to 130 deg.C-140 deg.C, then placing in cooling water of 0 deg.C-10 deg.C to shake and cool, and simultaneously continuously stirring until the temperature of the mixed filtrate is lowered to under 4 deg.C; (4) making the mixed filtrate static, depositing for 20-22 minutes, and then filtering and separating to obtain extractant and refined sulfur.
Description
Technical field
The invention belongs to the smelting technology field, be specifically related to extract in a kind of wet production stibium trioxide slag the novel process of refined sulfur.
Background technology
China is one of country that the antimony ore resource is the abundantest in the world, and reserves, output all occupy first place in the world.Exploitation, sorting, smelting ability that antimony ore is produced are big, and raw material type kind amounts such as the antimony concentrate of production, star metal, thick weisspiessglanz, antimony sulfide breeze, lead antimony alloy are of fine quality greatly, created good condition for developing the deep processing of antimony product.Antimony pyrometallurgical smelting is the domestic and international production technique that adopts of tradition, but because in smelting process, and arsenic, sulphur pollution environment are serious, so wet production stibium trioxide technology becomes the main flow that present antimony product is produced.But, in wet processing, produced a large amount of slags, in the middle of contain a certain amount of simple substance sulphur, most of slags are stacked everywhere and are not dealt with and administer.For the recovery sulphur resource, adopt traditional local method (distillation method) to extract sulphur technology at present, what local method was extracted the sulphur most critical is three parts: the one, scoriaceous roasting, the 2nd, the condensation of sulfur vapor and collection, the 3rd, treatment of waste gas is (if any foreign gas H
2S etc. will suitably handle).This several sections is not only independent but also interrelated, is directly connected to the rate of recovery, laid down cost, production cost, energy conservation and the environmental protection problem of sulphur.How they being connected is a very crucial problem, and never finds one well to be connected point at present.The control difficulty is bigger, seriously polluted in actually operating simultaneously, and the equipment cost height.So local method is extracted sulphur and had shortcomings such as investment is high, the cycle is long, danger is high, operation inconvenience, the feasibility of suitability for industrialized production is not strong.In order to handle and solve slag and the recycling sulphur resource that the wet production stibium trioxide produces, constantly exploring and study new technological method has become the problem that needs to be resolved hurrily.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, provide a kind of less investment, production unit simple, pollute little, easy to operate, as the to be convenient to suitability for industrialized production technology of from wet production stibium trioxide slag, extracting refined sulfur.
The technical scheme that the present invention solves the problems of the technologies described above employing is: the technology of from wet production stibium trioxide slag, extracting refined sulfur of the present invention, and its processing step is:
(1) stibium trioxide slag and leaching agent 1: 7 by weight percentage～8 are fully mixed in mixing tank, be heated to 140～160 ℃, kept 15～20 minutes, and constantly vibrate and stir;
(2) quick suction filtration carries out solid-liquid separation, and the suction filtration time was 30～35 seconds;
The filtration mixed solution that (3) will obtain is in well heater internal heating to 130～140 ℃, and placing temperature then is 0～10 ℃ water coolant, rocks cooling, constantly stirs simultaneously, reduces to below 4 ℃ until filtering mixeding liquid temperature.
(4) above-mentioned mixed solution is static, sedimentation is 20～22 minutes, and suction filtration separates then, obtains leaching agent and refined sulfur respectively.
Leaching agent of the present invention can be whiteruss.
The present invention adopts leaching and crystallization processes to extract refined sulfur from wet production stibium trioxide slag.Owing to have great difference on sulphur and the solubleness of other composition in organic solvent in the stibium trioxide slag, select for use the method for leaching can easier separate sulphur and slag; And leaching can be carried out under usual condition, does not need the processing condition of excessive demand, does not also need undue complicated laboratory apparatus, and production unit is simple, pollutes for a short time, is convenient to operate the suitability for industrialized production of being more convenient for.Sulphur after separating simultaneously adopts the method for quick cooling crystallization to be easy to separate with leaching agent solution.
The key of leaching is the selection of extracting solvent, and according to the character of sulphur, sulphur is water insoluble, is slightly soluble in alcohol, very easily is dissolved in organic solvents such as dithiocarbonic anhydride, so select for use organic solvent as leaching agent.Common alternative leaching agent has benzene,toluene,xylene, dithiocarbonic anhydride, tetracol phenixin etc., benzene,toluene,xylene and dithiocarbonic anhydride have high volatile volatile and toxicity, especially poisonous, the dithiocarbonic anhydride of long-term contact low concentration, generation is based on the clinical manifestation of maincenter and peripheral nervous system infringement, and other organs also can be got involved.Therefore, consider from the aspects such as ease for operation of safety, economy, feasibility and suitability for industrialized production, the present invention selects whiteruss as leaching agent, and it is the leaching agent that a kind of efficient cheapness has safety, feasibility again, has economy, nontoxic, characteristics such as saturation solubility is big.
The rate of recovery and the leaching agent rate of recovery height that refined sulfur is extracted in crystallization leached in the present invention; Product refined sulfur purity is big, and the median size size is about 5 microns.Experimental study through multilevel leaching shows: multilevel leaching does not have any influence basically for the leaching agent recovering effect, can recycle; Purity and granularity through measuring sulphur do not have any variation basically yet simultaneously.
Be described in further detail the present invention below in conjunction with embodiment.
Embodiment:
Embodiment 1: get stibium trioxide slag 45kg, whiteruss 450l fully mixes both in mixing tank as leaching agent, is heated to 150 ℃, and constant temperature kept 15 minutes, and constantly vibrates and stirs, is dissolved in the leaching agent to greatest extent with assurance sulphur.Then this mixed solution is poured into rapidly in the large-scale suction filtration device, suction filtration carries out quick solid-liquid separation fast, and the suction filtration time is 30 seconds.The filtration mixed solution that then will obtain places in the well heater, is heated rapidly to 140 ℃, and placing temperature then is 0 ℃ water coolant, and cooling is rapidly constantly stirred simultaneously, reduces to about 0 ℃ until mixeding liquid temperature.Made the mixed solution quiescent settling 20 minutes this moment, and suction filtration separates then, until cooled whiteruss is drained, obtains leaching agent whiteruss and sulphur respectively.The quality that obtains refined sulfur is 23.6kg, and its granularity can reach about 5 microns, and purity is 99.1%; The whiteruss that reclaims is 415.6l.Extract the refined sulfur rate of recovery and can reach 96.6%, the leaching agent rate of recovery is 92.4%.
Embodiment 2: get stibium trioxide slag 15kg, whiteruss 135l fully mixes both in mixing tank as leaching agent, is heated to 150 ℃, and constant temperature kept 20 minutes, and constantly vibrates and stirs, is dissolved in the leaching agent to greatest extent with assurance sulphur.Then this mixed solution is poured into rapidly in the large-scale suction filtration device, suction filtration carries out quick solid-liquid separation fast, and the suction filtration time is 30 seconds.The filtration mixed solution that then will obtain places in the well heater, is heated to 130 ℃, and placing temperature then is 0 ℃ water coolant, and cooling is rapidly constantly stirred simultaneously, reduces to about 0 ℃ until mixeding liquid temperature.Made the mixed solution quiescent settling 20 minutes this moment, and suction filtration separates then, until cooled whiteruss is drained, obtains leaching agent whiteruss and sulphur respectively.The quality that obtains refined sulfur is 14.4kg, and its granularity can reach about 5 microns, and purity is 99.0%; The whiteruss that reclaims is 124.3l.The leaching refined sulfur rate of recovery can reach 95.7%, and the leaching agent rate of recovery is 92.1%.
Claims (2)
1, a kind of technology of from wet production stibium trioxide slag, extracting refined sulfur, its processing step is:
(1) stibium trioxide slag and leaching agent 1: 7 by weight percentage～8 are fully mixed in mixing tank, be heated to 140～160 ℃, kept 15～20 minutes, and constantly vibrate and stir;
(2) quick suction filtration carries out solid-liquid separation, and the suction filtration time was 30～35 seconds;
The filtration mixed solution that (3) will obtain is in well heater internal heating to 130～140 ℃, and placing temperature then is 0～10 ℃ water coolant, rocks cooling, constantly stirs simultaneously, reduces to below 4 ℃ until filtering mixeding liquid temperature;
(4) above-mentioned mixed solution is static, sedimentation is 20～22 minutes, and suction filtration separates then, obtains leaching agent and refined sulfur respectively.
2, the technology of extracting refined sulfur from wet production stibium trioxide slag according to claim 1 is characterized in that described leaching agent is a whiteruss.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410022929 CN1267337C (en) | 2004-02-26 | 2004-02-26 | Technology of extracting fine sulphur from produced antimonic white slag by wet process production |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410022929 CN1267337C (en) | 2004-02-26 | 2004-02-26 | Technology of extracting fine sulphur from produced antimonic white slag by wet process production |
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| CN1559885A true CN1559885A (en) | 2005-01-05 |
| CN1267337C CN1267337C (en) | 2006-08-02 |
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| CN 200410022929 Expired - Fee Related CN1267337C (en) | 2004-02-26 | 2004-02-26 | Technology of extracting fine sulphur from produced antimonic white slag by wet process production |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104195345A (en) * | 2014-09-01 | 2014-12-10 | 株洲起源科技有限责任公司 | Process for recovering sulfur, lead, zinc and silver from oxygen-enriched directly leached residues of zinc concentrates or lead-zinc mixed ores |
| CN109835873A (en) * | 2019-03-27 | 2019-06-04 | 淮北师范大学 | The device and method for producing sulphur from sulfur-bearing waste residue |
-
2004
- 2004-02-26 CN CN 200410022929 patent/CN1267337C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104195345A (en) * | 2014-09-01 | 2014-12-10 | 株洲起源科技有限责任公司 | Process for recovering sulfur, lead, zinc and silver from oxygen-enriched directly leached residues of zinc concentrates or lead-zinc mixed ores |
| CN104195345B (en) * | 2014-09-01 | 2017-03-15 | 株洲起源科技有限责任公司 | Recovered sulphur and lead, zinc, the technique of silver in a kind of oxygen-enriched direct leached mud from zinc concentrate or lead and zinc industry |
| CN109835873A (en) * | 2019-03-27 | 2019-06-04 | 淮北师范大学 | The device and method for producing sulphur from sulfur-bearing waste residue |
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| Publication number | Publication date |
|---|---|
| CN1267337C (en) | 2006-08-02 |
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