CN104032139B - The method reclaiming mercury from mercurous tailings is decomposed in a kind of complexation leaching-strengthening - Google Patents
The method reclaiming mercury from mercurous tailings is decomposed in a kind of complexation leaching-strengthening Download PDFInfo
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- CN104032139B CN104032139B CN201410247462.3A CN201410247462A CN104032139B CN 104032139 B CN104032139 B CN 104032139B CN 201410247462 A CN201410247462 A CN 201410247462A CN 104032139 B CN104032139 B CN 104032139B
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Abstract
The invention belongs to field of environment protection; mercurous tailings amount for nonferrous metal mine and non-ferrous smelt enterprise output is in process of production large, complicated component, at present without the problem of suitable art breading, the present invention disclose the method that mercury is reclaimed in a kind of complexation leaching strengthening decomposition from mercurous tailings.The method is: adopt the mixing solutions of thiosulphate and selenosulfate to carry out complexation leaching mercurous tailings, transportable state mercury in mercurous tailings is made to be transferred to leach liquor, by the complex compound that the mercury in leach liquor and thiosulfate anion, seleno sulfate radical are formed, add and carry out strengthening decomposition by heat and the method blasting carbon dioxide, make mercury finally be converted into stable zunsober/mercury selenide form precipitation.Present method is simple to operate, and the transportable state mercury in mercurous tailings is converted into the zunsober and/or mercury selenide precipitation forms that solubleness is low, stability is high, toxicity is little, to contribute to reducing in mercurous tailings mercury to the pollution hazard of environment.
Description
Technical field
The invention belongs to field of environment protection, relate to a kind of complexation leaching that adopts and strengthen the method for decomposing and reclaiming mercury from mercurous tailings.
Background technology
Mercury is the heavy metal contaminants that in environment, a kind of bio-toxicity is extremely strong, and it is difficult to be discharged after entering organism, serious threat human health.Between the more than ten years in the past, in world wide environment, the concentration of mercury continues to rise, and has caused the very big concern of national governments and environmental protection organization, has become another Global Environmental Problems after climate change problem.
At present, domestic purification mercuryvapour commonly uses absorption process, absorption method, gas-phase reaction method, method of cooling and combined purifying method etc.Wherein the many employings of absorption process have the material of higher oxygen reduction potential, as potassium permanganate (KMnO
4), chlorine bleach liquor etc., features such as there is speed of response fast when they and mercuryvapour effect, purification efficiency is high, strength of solution is low, not volatile, throw out is few.Processing the how chlorinating gac of secondary purification of the mercurous waste gas of lower concentration and the mercurous waste gas of high density, but in mercury smelting or other high densitys or the mercurous waste gas pollution control and treatment of atm number, consider the factor of Financial cost, also adopt the coke of sodium polysulphide process to make sorbent material.Modal in gas-phase reaction method is iodine complexometry, and this method utilizes containing iodine gas and mercurous waste gas generation chemical reaction, reaches the mercury eliminated in waste gas.The mercurous tail gas of high density, as the tail gas of the processes such as mercury smelting, waste slag containing mercury pyrogenic attack, often to adopt the scavenging process ability qualified discharge of more than secondary, common are: condensation-absorption process, clorox absorption-active carbon adsorption, liquid-absorbent-fill chlorine active carbon adsorption etc.
The treatment process relating to mercury-containing waste water has iron filings or aluminium bits reduction method, chemical precipitation method, ion exchange method and active carbon adsorption etc.
For mercurous solid waste, more various mercurous product uses the waste of rear output, as PVC industry creates a large amount of useless mercury catalysts, mercurous gac in process of production, medical industry still partly uses mercurous thermometer, sphygmomanometer etc. at present, and the luminescent lamp that the widely used mercury line of electric light source industry excites is all containing mercury.For this type of mercury-containing wastes, after in category set, roasting-condensation method can be adopted to reclaim mercury.As the patent No. Chinese patent that is 200420082423.4 provides a kind for the treatment of unit of waste slag containing mercury, mercurous waste fluorescent light tube is heated in Sealing Arrangement, makes mercury be evaporated to mercury vapour, then condensation Footwall drift mercury.The patent No. be 200420082125.5 Chinese patent provide a kind of process furnace for waste slag containing mercury process, adopt a kind of airtight process furnace, waste slag containing mercury removed mercury through heating evaporation.Application number be 201310671649 Chinese patent disclose a kind of useless mercury catalyst mercury chloride recovery process, in gas retort by heating, condensation to reclaim mercury chloride and gac simultaneously.
And for the mercurous tailings of nonferrous metal mine and non-ferrous smelt enterprise output in process of production, because its amount is large, complicated component, than its complex treatment process of mercurous solid waste such as useless mercury catalyst, mercurous thermometers.As the mercurous tailings of output in gold mining and smelting process, at present without suitable art breading, simply store up after only doing antiseepage, or spray liming simple process on tailings top.
Summary of the invention
The present invention seeks to the mercurous tailings for nonferrous metal mine and non-ferrous smelt enterprise output in process of production, because its amount is large, complicated component, the current problem without suitable art breading, thering is provided a kind of adopts complexation leaching-strengthening to decompose the method reclaiming mercury from mercurous tailings, present method is simple to operate, transportable state mercury in mercurous tailings is converted into the zunsober that solubleness is low, stability is high, toxicity is little and/or mercury selenide precipitation forms to reclaim, contributes to reducing in mercurous tailings mercury to the pollution hazard of environment.
For achieving the above object, the technical solution used in the present invention is:
Adopt complexation leaching-strengthening to decompose the method reclaiming mercury from mercurous tailings, comprise following steps:
1, concentration is adopted to be the thiosulphate of 10 ~ 30g/L and concentration to be the mixing solutions of the selenosulfate of 0 ~ 0.3g/L to carry out agitation leach to mercurous tailings, mixing solutions add-on is that the mercurous tailings of per kilogram adds 3 ~ 10L, the Leaching reaction time is 1.0 ~ 5.0h, through solid-liquor separation after reaction, obtain leached mud, leach liquor and washings;
Described thiosulphate is Sulfothiorine; Described selenosulfate is sodium thiosulfate;
2, the leached mud obtained is stored up, merge leach liquor and washings, obtain the solution containing soluble mercury complex compound;
3, the solution containing soluble mercury complex compound obtained is heated to 60 ~ 85 DEG C, blast carbon dioxide, the gas amount of blasting is that every cubic metre of solution per minute blasts 0 ~ 0.05 cubic metre, by soluble mercury complex compound Mandatory Decomposition 1 ~ 12h simultaneously; After reaction, in solution, add flocculation agent, its concentration is 1 ~ 2g/L, and add-on is that every cubic metre of solution adds 10 ~ 20L flocculation agent, through solid-liquor separation, obtains decomposed solution and zunsober and/or mercury selenide and precipitates;
Wherein, described flocculation agent is polyacrylamide slurries;
4, the mercurous mercury product being precipitated as recovery, decomposed solution returns step 1 after supplying thiosulphate and selenosulfate and recycles, for mercurous tailings agitation leach.
Principle of the present invention is: mercury contained in mercurous tailings, and part exists with stable residual form zunsober form, and part exists with water miscible mercury chloride and rare acid soluble red precipitate and Mercury bisulfate form.With the mercury that zunsober form exists, because its solubleness is low, stability is strong, and toxicity is low, generally less to environmental hazard.And the mercury of transportable state is belonged to the mercury that mercury chloride, red precipitate and Mercury bisulfate form exist, and easily move at occurring in nature, larger to the pollution hazard of environment.Due to, thiosulphate and selenosulfate can form the very large complexing ion of stability constant with mercury, thiosulphate and selenosulfate is adopted to leach mercurous tailings, the stability of the complexing ion that can be formed by mercury and thiosulphate and selenosulfate, pulls the strong forward of Leaching reaction to carry out, namely greatly promotes the Leaching reaction of mercury in mercurous tailings, wherein, the ability of the formation complex compound of mercury and selenosulfate is stronger, and leaching effect is better, but the cost of selenosulfate is higher.Therefore, the present invention adopts the mixing solutions of thiosulfate solution or thiosulphate and selenosulfate to leach mercurous tailings, and the mercurous tailings through leaching, after washing, substantially not containing the mercury of transportable state, follow-uply greatly to reduce the harm of environment when storing up.For mercurous leach liquor, the present invention proposes to strengthen the method for decomposing, adopt heated solution, blast the measure of carbonic acid gas, make the complex decomposes of mercury and thiosulfate anion and seleno sulfate radical be that solubleness is low, stability is high, toxicity is little zunsober and/or mercury selenide precipitation forms are to reclaim.
Advantage of the present invention:
1, present method is simple to operate, leaching process does not need boosting, at normal temperatures, transportable state mercury in mercurous tailings is leached by thiosulphate and selenosulfate, after agitation leach process, transportable state mercury leaching yield is 99%, and the transportable state mercury in mercurous tailings is almost all removed, and to greatly reduce in mercurous tailings mercury to the pollution hazard of environment.
2, the thiosulphate of the mercury of leaching and selenosulfate are adopted heated solution, blast the measure of carbonic acid gas by present method, strengthening is decomposed, decomposition course is simple to operate, react completely, removing carbon dioxide is outer without the need to adding other chemical reagent, after strengthening is decomposed, the thiosulphate of mercury and selenosulfate are converted into the zunsober and/or mercury selenide precipitation forms that solubleness is low, stability is high, toxicity is little, to eliminate in mercurous tailings mercury to the pollution hazard of environment.
3, present method safety and environmental protection, the infusion solution used at the mercurous tailings of process is reusable, and whole process is without mercurous waste gas and mercury-containing waste water discharge.
Specific implementation method
Following embodiment only in order to further illustrate the present invention, but does not limit the scope of the invention.
Mercurous tailings is gold mine cyanidation tailings, and wherein total mercury is 1570mg/kg, and adopting 1mol/L sodium acetate solution (adding glacial acetic acid adjustment pH is 5) to leach and measuring transportable state mercury in this cyanidation tailings is 706.5mg/kg.
Agents useful for same is industrial goods.
Embodiment 1
Get the mercurous tailings of 1kg, add the mixing solutions that 3L concentration is 30g/L Sulfothiorine and 0.3g/L sodium thiosulfate, at room temperature agitation leach 1.0h, after solid-liquor separation, obtain leached tailings, leach liquor and washings; Sampling analysis, in leached tailings, the leaching yield of transportable state mercury is 99%, is stored up by the leached tailings after being separated;
Leach liquor and washings are merged, obtain the solution of 4L containing soluble mercury complex compound, solution is heated to 85 DEG C, after Mandatory Decomposition 12h, add 1g/L polyacrylamide slurries 0.04L again, carry out solid-liquor separation, obtain decomposed solution and mercury selenide precipitation, in solution, the mercury of 99.98% is converted into mercurous precipitation.
Embodiment 2
Get the mercurous tailings of 1kg, adding 10L concentration is 30g/L hypo solution, and at room temperature agitation leach 3.0h, obtains leached tailings, leach liquor and washings after solid-liquor separation; Sampling analysis, in leached tailings, the leaching yield of transportable state mercury is 99%, is stored up by the leached tailings after being separated;
Leach liquor and washings are merged, obtain the solution of 11L containing soluble mercury complex compound, solution is heated to 60 DEG C, carbon dioxide is blasted with the tolerance of per minute 0.5L, Mandatory Decomposition 10h, then add 2g/L polyacrylamide slurries 0.2L, carry out solid-liquor separation, obtain decomposed solution and zunsober precipitation, in solution, the mercury of 99.96% is converted into mercurous precipitation;
The decomposed solution obtained adds Sulfothiorine, makes its concentration be after 30g/L, returns agitation leach step cycle for mercurous tailings agitation leach.
Embodiment 3
Get the mercurous tailings of 1kg, add the mixing solutions that 10L concentration is 10g/L Sulfothiorine and 0.15g/L sodium thiosulfate, at room temperature agitation leach 5.0h, after solid-liquor separation, obtain leached tailings, leach liquor and washings; Sampling analysis, in leached tailings, the leaching yield of transportable state mercury is 99%, is stored up by the leached tailings after being separated;
Leach liquor and washings are merged, obtain the solution of 11L containing soluble mercury complex compound, solution is heated to 75 DEG C, carbon dioxide is blasted with the tolerance of per minute 0.25L, Mandatory Decomposition 4h, then add 2g/L polyacrylamide slurries 0.15L, carry out solid-liquor separation, obtain decomposed solution and mercury selenide precipitation, in solution, the mercury of 99.97% is converted into mercurous precipitation.
Embodiment 4
Get the mercurous tailings of 1kg, add the mixing solutions that 6L concentration is 20g/L Sulfothiorine and 0.1g/L sodium thiosulfate, at room temperature agitation leach 4.0h, after solid-liquor separation, obtain leached tailings, leach liquor and washings; Sampling analysis, in leached tailings, the leaching yield of transportable state mercury is 99%, is stored up by the leached tailings after being separated;
Leach liquor and washings are merged, obtain the solution of 7L containing soluble mercury complex compound, solution is heated to 60 DEG C, carbon dioxide is blasted with the tolerance of per minute 0.35L, Mandatory Decomposition 5h, then add 1.5g/L polyacrylamide slurries 0.14L, carry out solid-liquor separation, obtain decomposed solution and zunsober and mercury selenide mixed precipitation, in solution, the mercury of 99.97% is converted into mercurous precipitation.
Embodiment 5
Get the mercurous tailings of 1kg, add the mixing solutions that 10L concentration is 30g/L Sulfothiorine and 0.3g/L sodium thiosulfate, at room temperature agitation leach 1.0h, after solid-liquor separation, obtain leached tailings, leach liquor and washings; Sampling analysis, in leached tailings, the leaching yield of transportable state mercury is 99%, is stored up by the leached tailings after being separated;
Leach liquor and washings are merged, obtain the solution of 11L containing soluble mercury complex compound, solution is heated to 85 DEG C, carbon dioxide is blasted with the tolerance of per minute 0.55L, Mandatory Decomposition 1h, then add 2g/L polyacrylamide slurries 0.22L, carry out solid-liquor separation, obtain decomposed solution and mercury selenide precipitation, in solution, the mercury of 99.99% is converted into mercurous precipitation;
The decomposed solution obtained adds Sulfothiorine and sodium thiosulfate, after making its concentration be respectively 30g/L and 0.3g/L, returns agitation leach step cycle for mercurous tailings agitation leach.
Claims (6)
1. adopt complexation leaching-strengthening to decompose the method reclaiming mercury from mercurous tailings, it is characterized in that, comprise following steps:
(1) adopt thiosulphate and selenosulfate mixing solutions to carry out agitation leach to mercurous tailings, through solid-liquor separation after reaction, obtain leached mud, leach liquor and washings;
Wherein, described thiosulphate is Sulfothiorine, and concentration is 10 ~ 30g/L;
Described selenosulfate is sodium thiosulfate, and concentration is 0 ~ 0.3g/L;
(2) leached mud obtained is stored up, merge leach liquor and washings, obtain the solution containing soluble mercury complex compound;
(3) blast carbon dioxide to what obtain containing in the solution of soluble mercury complex compound, by soluble mercury complex compound Mandatory Decomposition, after decomposition reaction, through solid-liquor separation, obtain decomposed solution and zunsober and/or mercury selenide and precipitate, be precipitated as the mercury product of recovery;
Wherein, the carbon dioxide amount of blasting is: every cubic metre of solution per minute blasts 0 ~ 0.05 cubic metre.
2. a kind of method adopting complexation leaching-strengthening decomposition to reclaim mercury from mercurous tailings according to claim 1, it is characterized in that, in described step (1), thiosulphate and selenosulfate mixing solutions add-on are: the mercurous tailings of per kilogram adds 3 ~ 10L.
3. a kind of method adopting complexation leaching-strengthening decomposition to reclaim mercury from mercurous tailings according to claim 1, it is characterized in that, in described step (1), the agitation leach reaction times is 1.0 ~ 5.0h.
4. a kind of method adopting complexation leaching-strengthening decomposition to reclaim mercury from mercurous tailings according to claim 1, it is characterized in that, in described step (3), decomposition reaction condition is: solution is heated to 60 ~ 85 DEG C, and the reaction times is 1 ~ 12h.
5. a kind of method adopting complexation leaching-strengthening decomposition to reclaim mercury from mercurous tailings according to claim 1, is characterized in that, in described step (3), after decomposition reaction, in solution, add flocculation agent, then carry out solid-liquor separation;
Described flocculation agent is polyacrylamide slurries, and its concentration is 1 ~ 2g/L, and add-on is that every cubic metre of solution adds 10 ~ 20L.
6. a kind of method adopting complexation leaching-strengthening decomposition to reclaim mercury from mercurous tailings according to claim 1, it is characterized in that, the decomposed solution that described step (3) obtains, after supplying thiosulphate and selenosulfate, return step (1) recycle, for mercurous tailings agitation leach.
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| CN104438285B (en) * | 2014-11-06 | 2019-12-24 | 中国科学院生态环境研究中心 | Method for innocent treatment of waste mercury catalyst by mechanical ball milling with sulfur as additive |
| CN104805297B (en) * | 2015-05-20 | 2017-04-26 | 西安西北有色地质研究院有限公司 | Method for recovering selenium, mercury, gold and silver from acid sludge |
| CN107973335A (en) * | 2017-11-24 | 2018-05-01 | 江苏盐城环保科技城重金属防治研究中心 | A kind of method of useless mercury catalyst alkaline wet recycling mercury |
| CN108395020B (en) * | 2018-04-10 | 2021-02-19 | 北京科技大学 | Universal harmless disposal method for mercury overproof wastewater |
| CN113894135B (en) * | 2020-06-22 | 2023-10-24 | 内蒙古岱海发电有限责任公司 | Method for removing mercury from fly ash and purifying mercury-removing liquid |
| CN112063840A (en) * | 2020-09-21 | 2020-12-11 | 河南科技大学 | Harmless treatment method for mercury-containing thiosulfate leachate |
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| GB1121845A (en) * | 1964-10-27 | 1968-07-31 | Huels Chemische Werke Ag | Process and apparatus for recovering mercury or mercury(ii) chloride from catalysts containing mercury |
| CN101130833A (en) * | 2007-10-12 | 2008-02-27 | 紫金矿业集团股份有限公司 | Demercuration method for active gold-carrying carbon containing mercury |
| CN102247685A (en) * | 2010-05-18 | 2011-11-23 | 上海复拓环境技术有限公司 | Harmless treatment process for mercury-containing waste dangerous chemicals |
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| GB1121845A (en) * | 1964-10-27 | 1968-07-31 | Huels Chemische Werke Ag | Process and apparatus for recovering mercury or mercury(ii) chloride from catalysts containing mercury |
| CN101130833A (en) * | 2007-10-12 | 2008-02-27 | 紫金矿业集团股份有限公司 | Demercuration method for active gold-carrying carbon containing mercury |
| CN102247685A (en) * | 2010-05-18 | 2011-11-23 | 上海复拓环境技术有限公司 | Harmless treatment process for mercury-containing waste dangerous chemicals |
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