CN104561558A - Method for treating selenium-containing mercury acid mud - Google Patents
Method for treating selenium-containing mercury acid mud Download PDFInfo
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- CN104561558A CN104561558A CN201510025970.1A CN201510025970A CN104561558A CN 104561558 A CN104561558 A CN 104561558A CN 201510025970 A CN201510025970 A CN 201510025970A CN 104561558 A CN104561558 A CN 104561558A
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Abstract
The invention discloses a method for treating mercury selenide acid mud, which comprises the steps of adding mercury selenide acid mud into a sodium chloride or calcium chloride solution, and filtering and separating to obtain lead leaching liquid and lead leaching residues; adding sodium hydroxide or calcium oxide neutralizer into the obtained lead dipping liquid, filtering to obtain lead hydroxide slag and neutralized liquid, and returning the lead hydroxide slag to a lead smelting system to recover lead; adding the lead-leaching residues into hydrochloric acid, slowly adding an oxidant, and filtering and separating to obtain mercury-leaching residues and a mercury-leaching solution; adding a neutralizing agent into the mercury soaking solution to precipitate mercury, filtering and separating to obtain mercury oxide and a selenium-containing solution, adding the mercury oxide into the diluted reducing agent solution, reducing the mercury, distilling and purifying to obtain metallic mercury, adding a reducing agent into the selenium-containing solution, and filtering to obtain crude selenium and a reduced solution. The treatment method has the advantages of simple process, less equipment investment, no pollution and good economic benefit, and can recover lead while realizing the recovery of selenium and mercury.
Description
Technical field
The present invention relates to metallurgical technology field, particularly relate to a kind for the treatment of process containing selenium mercury acid mud.
Background technology
At present, in the fusion process of lead ore concentrate, because handled lead ore concentrate raw material is comparatively complicated, the valuable element such as trace selenium, mercury contained in lead ore concentrate with fume, enters towerman's sequence in smelting process after purification; Be enriched in due to reasons such as dust collection effects in relieving haperacidity cleaning section in relieving haperacidity acid mud.
And this generation containing selenium mercury acid mud due to complicated component, intractability is relatively large, in prior art, a lot of factory does not all process or reclaims the part metals in slag after only doing simple process, lack effective processing scheme, so just cause the very large wasting of resources, bring serious environmental problem simultaneously.
Summary of the invention
The object of this invention is to provide a kind for the treatment of process containing selenium mercury acid mud, the method can solve environmental pollution and the not high problem of valuable metal recovery utilization ratio, and technique is simple, facility investment is few, pollution-free, good in economic efficiency, while selenium and mercury are reclaimed in realization, can also lead be reclaimed.
Containing a treatment process for selenium mercury acid mud, described method comprises:
Step 1, by containing in the selenium mercury acid mud sodium-chlor that adds 200 ~ 350g/L or calcium chloride solution, then add hydrochloride adjusted solution pH value to 1 ~ 2, at 60 ~ 95 DEG C after agitation leach 1 ~ 4h, filtering separation obtains soaking plumbous liquid and leaching lead skim;
Step 2, in the plumbous liquid of obtained leaching, add sodium hydroxide or calcium oxide neutralization agent, adjustment solution ph to 7 ~ 9, reaction 1-4h, obtains hydroxide lead skim and the rear liquid of neutralization after filtration, described hydroxide lead skim returns plumbous smelting system and reclaims plumbous, and after described neutralization, liquid returns step 1 continuation leaching lead;
Step 3, leaching lead skim step 1 obtained add in 50 ~ 100g/L hydrochloric acid, and liquid-solid ratio is 5 ~ 15, at 40 ~ 80 DEG C, slowly add oxygenant, the consumption of described oxygenant is 1.0 ~ 2.0 times of described leaching lead skim, agitation leach 1 ~ 3h, obtains leaching mercury slag and leaching mercury solution after filtering separation;
Step 4, the leaching mercury slag obtained is returned step 3 carry out secondary leaching, described leaching mercury solution adopts neutralizing agent regulator solution pH value to 12 ~ 14 of 20 ~ 40% mass concentrations, and neutralization reaction 2 ~ 4h, obtain red precipitate and Se solution after filtering separation;
Step 5, red precipitate step 4 obtained add in the reductant solution after dilution, and distilation after mercury reduction is obtained mercury metal;
Step 6, Se solution salt acid for adjusting pH value to 0.1 ~ 2.0 step 4 obtained, and the reductive agent adding reduction selenium theoretical amount 1.0 ~ 2.0 times, reduction reaction 2 ~ 5h at 60 ~ 95 DEG C, filters and obtains thick selenium and the rear liquid of reduction.
As seen from the above technical solution provided by the invention, this treatment process technique is simple, facility investment is few, pollution-free, good in economic efficiency, while selenium and mercury are reclaimed in realization, can also reclaim lead.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme of the embodiment of the present invention, below the accompanying drawing used required in describing embodiment is briefly described, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 provides by the embodiment of the present invention process flow schematic diagram containing selenium mercury acid mud.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on embodiments of the invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to protection scope of the present invention.
Below in conjunction with accompanying drawing, the embodiment of the present invention is described in further detail, be illustrated in figure 1 the embodiment of the present invention provide containing selenium mercury acid mud process flow schematic diagram, the treating method comprises:
Step 1, by containing in the selenium mercury acid mud sodium-chlor that adds 200 ~ 350g/L or calcium chloride solution, then add hydrochloride adjusted solution pH value to 1 ~ 2, at 60 ~ 95 DEG C after agitation leach 1 ~ 4h, filtering separation obtains soaking plumbous liquid and leaching lead skim;
In this step, described sodium-chlor or calcium chloride solution and the described liquid-solid ratio (ie in solution volume/material dry weight) containing selenium mercury acid mud are 8 ~ 25:1, and preferably liquid-solid ratio is 10 ~ 20;
And described sodium-chlor or calcium chloride solution are preferably 300 ~ 350g/L, adjustment solution ph preferably to 1.0 ~ 1.5, the plumbous temperature of preferred leaching is 80 ~ 95 DEG C.
Step 2, in the plumbous liquid of obtained leaching, add sodium hydroxide or calcium oxide neutralization agent, adjustment solution ph to 7 ~ 9, reaction 1-4h, obtains hydroxide lead skim and the rear liquid of neutralization after filtration, described hydroxide lead skim returns plumbous smelting system and reclaims plumbous, and after described neutralization, liquid returns step 1 continuation leaching lead;
In this step, add sodium hydroxide or calcium oxide neutralization agent, adjustment solution ph is preferably 7 ~ 8.
Step 3, leaching lead skim step 1 obtained add in 50 ~ 100g/L hydrochloric acid, and liquid-solid ratio is 5 ~ 15, at 40 ~ 80 DEG C, slowly add oxygenant, the consumption of described oxygenant is 1.0 ~ 2.0 times of described leaching lead skim, agitation leach 1 ~ 3h, and filtering separation obtains leaching mercury slag and leaching mercury solution;
In this step, the concentration of hydrochloric acid added in described leaching lead skim is preferably 70 ~ 100g/L, and preferred liquid-solid ratio is 5 ~ 10, and preferred extraction temperature is 50 ~ 80 DEG C;
The oxygenant added can comprise sodium chlorate, hydrogen peroxide, hypochlorous acid or clorox, is preferably sodium chlorate or hydrogen peroxide;
And the consumption of described oxygenant is preferably 1.0 ~ 1.5 times of described leaching lead skim, the preferred agitation leach time is 1 ~ 2h.
Step 4, the leaching mercury slag obtained is returned step 3 carry out secondary leaching, described leaching mercury solution adopts neutralizing agent regulator solution pH value to 12 ~ 14 of 20 ~ 40% mass concentrations, and neutralization reaction 2 ~ 4h, obtain red precipitate and Se solution after filtering separation;
In this step, the neutralizing agent adopted is sodium hydroxide, and preferred mass concentration is 30 ~ 40%, and regulator solution pH value preferably to 13 ~ 14, the neutralization reaction time is preferably 2 ~ 3h.
Step 5, red precipitate step 4 obtained add in the reductant solution after dilution, and distilation after mercury reduction is obtained mercury metal;
In this step, the reductant solution adopted is hydrazine hydrate solution, and the consumption of hydrazine hydrate is 1.0 ~ 1.5 times of reduction-oxidation mercury theoretical amount, is preferably 1.0 ~ 1.2 times;
The distillation temperature of distilation is 150 ~ 300 DEG C, is preferably 200 ~ 300 DEG C; Distillation time is 2 ~ 5h, is preferably 2 ~ 4h.
Step 6, Se solution salt acid for adjusting pH value to 0.1 ~ 2.0 step 4 obtained, and the reductive agent adding reduction selenium theoretical amount 1.0 ~ 2.0 times, reduction reaction 2 ~ 5h at 60 ~ 95 DEG C, filters and obtains thick selenium and the rear liquid of reduction.
In this step, with salt acid for adjusting pH value preferably to 0.1 ~ 0.5;
The reductive agent added can be S-WAT or sulfurous gas, and preferable amount is 1.0 ~ 1.5 times of reduction selenium theoretical amount;
The temperature of above-mentioned reduction reaction is preferably 80 ~ 90 DEG C, and the time of reduction reaction is preferably 3 ~ 4h.
In addition, after described step 6 obtains described reduction after liquid, further liquid after described reduction is obtained sodium-chlor after evaporative crystallization, the partial oxidation sodium obtained can return described step 1 to be continued to recycle.
Below in conjunction with specific examples, treatment process of the present invention is described further:
Embodiment 1,
1. get containing selenium mercury acid mud 50g, analyzing main chemical compositions is: Se 32.85%, Hg 35.44%, Pb 15.12%.Sour mud is added in 500ml 300g/L sodium chloride solution, add hydrochloric acid and adjust pH ~ 1,90 DEG C, reaction 2h; After filtering, filtrate adds sodium hydroxide tune pH ~ 8, reaction 2h, and heavy lead skim, containing Pb 79.85%, is returned pyrometallurgical smelting of lead system recoveries plumbous by heavy lead skim.
2. added by leaching lead skim in 80g/L HCl solution, under liquid-solid ratio 10:1, the condition of 80 DEG C, add 16.82g sodium chlorate, reaction 2h, leached mud is containing Se 3.03%, Hg 0.64%, and leached mud returns Oxidation Leaching and carries out secondary leaching; Leach liquor adds 40%NaOH and adjusts pH value of solution to 13.5, and reaction 2h, obtains rich mercury slag, mercurous 90.74%; Rich mercury slag adds in hydrazine hydrate solution and reduces, and after reduction, slag distills 2h at 240 DEG C, obtains mercury metal.
3. after heavy mercury, liquid acid adding adjusts pH to 0.5, and add 18g S-WAT reduction selenium at 80 DEG C, reaction 3h, obtains the thick selenium of grey black, containing selenium 98.86%.
4. according to prior art evaporative crystallization sodium-chlor liquid after reduction selenium, the partial oxidation sodium obtained can continue to recycle.
Embodiment 2,
1. get containing selenium mercury acid mud 100g, analyzing main component is: Se 32.85%, Hg 35.44%, Pb 15.12%.Added by sour mud in 1500ml 350g/L calcium chloride solution, acid adding adjusts pH ~ 1.5,90 DEG C, reaction 2h; After filtering, filtrate adds calcium oxide tune pH ~ 8.5, reaction 3h, and heavy lead skim, containing Pb 81.63%, is returned pyrometallurgical smelting of lead system recoveries plumbous by heavy lead skim.
2. added by leaching lead skim in 100g/L HCl solution, under liquid-solid ratio 8:1, the condition of 60 DEG C, add 100ml hydrogen peroxide, reaction 3h, leached mud is containing Se2.73%, Hg 0.41%, and leached mud returns Oxidation Leaching and carries out secondary leaching; Leach liquor adds 30%NaOH and adjusts pH value of solution to 13.0, and reaction 2h, obtains rich mercury slag, mercurous 86.32%; Rich mercury slag adds in hydrazine hydrate solution and reduces, and after reduction, slag distills 4h at 200 DEG C, obtains mercury metal.
3. after heavy mercury, liquid acid adding adjusts pH to 0.2, and add 27g S-WAT reduction selenium at 90 DEG C, reaction 2h, obtains the thick selenium of grey black, containing selenium 97.91%.
4. according to prior art from reduction selenium after liquid evaporative crystallization sodium-chlor, the partial oxidation sodium obtained can continue to recycle.
Embodiment 3,
1. get containing selenium mercury acid mud 50g, analyzing main component is: Se26.44%, Hg 26.68%, Pb 24.61%.Added by sour mud in 600ml 280g/L sodium chloride solution, acid adding adjusts pH ~ 1,85 DEG C, reaction 2h; After filtering, filtrate adds sodium hydroxide tune pH ~ 8, reaction 2h, and heavy lead skim, containing Pb80.23%, is returned pyrometallurgical smelting of lead system recoveries plumbous by heavy lead skim.
2. added by leaching lead skim in 100g/L HCl solution, under liquid-solid ratio 10:1, the condition of 70 DEG C, add 50ml hydrogen peroxide, reaction 2h, leached mud is containing Se 2.44%, Hg 0.27%, and leached mud returns Oxidation Leaching and carries out secondary leaching; Leach liquor adds 40%NaOH and adjusts pH value of solution to 14, and reaction 2h, obtains rich mercury slag, mercurous 89.13%; Rich mercury slag adds in hydrazine hydrate solution and reduces, and after reduction, slag distills 2h at 240 DEG C, obtains mercury metal.
3. after heavy mercury, liquid acid adding adjusts pH to 0.5, and add 13.6g S-WAT reduction selenium at 90 DEG C, reaction 2h, obtains the thick selenium of grey black, containing selenium 98.67%.
4. according to prior art from reduction selenium after liquid evaporative crystallization sodium-chlor, the partial oxidation sodium obtained can continue to recycle.
In sum, the treatment process that the embodiment of the present invention provides adopts wet processing flow process, and solution circulated utilizes, without outer row, environmentally friendly, belongs to clean metallurgical technology; Flow process is short simultaneously, simple to operate, containing the rate of recovery of valuable metal elemental selenium, mercury and lead in selenium mercury acid mud up to more than 96%, and obtain byproduct sodium-chlor, solve the problem of complex utilization of sour mud valuable element well, greatly reduce selenium and mercury in sour mud and, to the pollution of environment, efficiently utilize secondary resource.
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (7)
1., containing a treatment process for selenium mercury acid mud, it is characterized in that, described method comprises:
Step 1, by containing in the selenium mercury acid mud sodium-chlor that adds 200 ~ 350g/L or calcium chloride solution, then add hydrochloride adjusted solution pH value to 1 ~ 2, at 60 ~ 95 DEG C after agitation leach 1 ~ 4h, filtering separation obtains soaking plumbous liquid and leaching lead skim;
Step 2, in the plumbous liquid of obtained leaching, add sodium hydroxide or calcium oxide neutralization agent, adjustment solution ph to 7 ~ 9, reaction 1-4h, obtains hydroxide lead skim and the rear liquid of neutralization after filtration, described hydroxide lead skim returns plumbous smelting system and reclaims plumbous, and after described neutralization, liquid returns step 1 continuation leaching lead;
Step 3, leaching lead skim step 1 obtained add in 50 ~ 100g/L hydrochloric acid, and liquid-solid ratio is 5 ~ 15, at 40 ~ 80 DEG C, slowly add oxygenant, the consumption of described oxygenant is 1.0 ~ 2.0 times of described leaching lead skim, agitation leach 1 ~ 3h, obtains leaching mercury slag and leaching mercury solution after filtering separation;
Step 4, the leaching mercury slag obtained is returned step 3 carry out secondary leaching, described leaching mercury solution adopts neutralizing agent regulator solution pH value to 12 ~ 14 of 20 ~ 40% mass concentrations, and neutralization reaction 2 ~ 4h, obtain red precipitate and Se solution after filtering separation;
Step 5, red precipitate step 4 obtained add in the reductant solution after dilution, and distilation after mercury reduction is obtained mercury metal;
Step 6, Se solution salt acid for adjusting pH value to 0.1 ~ 2.0 step 4 obtained, and the reductive agent adding reduction selenium theoretical amount 1.0 ~ 2.0 times, reduction reaction 2 ~ 5h at 60 ~ 95 DEG C, filters and obtains thick selenium and the rear liquid of reduction.
2., according to claim 1 containing the treatment process of selenium mercury acid mud, it is characterized in that, in described step 1:
Described sodium-chlor or calcium chloride solution and the described liquid-solid ratio containing selenium mercury acid mud are 8 ~ 25, and preferably liquid-solid ratio is 10 ~ 20;
And described sodium-chlor or calcium chloride solution are preferably 300 ~ 350g/L, adjustment solution ph preferably to 1.0 ~ 1.5, soak plumbous temperature and are preferably 80 ~ 95 DEG C.
3., according to claim 1 containing the treatment process of selenium mercury acid mud, it is characterized in that, in step 3:
The concentration of hydrochloric acid added in described leaching lead skim is preferably 70 ~ 100g/L, and liquid-solid ratio is preferably 5 ~ 10, and extraction temperature is preferably 50 ~ 80 DEG C;
The oxygenant added comprises sodium chlorate, hydrogen peroxide, hypochlorous acid or clorox, is preferably sodium chlorate or hydrogen peroxide;
And the consumption of described oxygenant is preferably 1.0 ~ 1.5 times of described leaching lead skim, the agitation leach time is preferably 1 ~ 2h.
4., according to claim 1 containing the treatment process of selenium mercury acid mud, it is characterized in that, in described step 4:
The neutralizing agent adopted is sodium hydroxide, and mass concentration is preferably 30 ~ 40%, regulator solution pH value preferably to 13 ~ 14, and the neutralization reaction time is preferably 2 ~ 3h.
5., according to claim 1 containing the treatment process of selenium mercury acid mud, it is characterized in that, in described step 5:
The reductant solution adopted is hydrazine hydrate solution, and the consumption of hydrazine hydrate is 1.0 ~ 1.5 times of reduction-oxidation mercury theoretical amount, is preferably 1.0 ~ 1.2 times;
The distillation temperature of distilation is 150 ~ 300 DEG C, is preferably 200 ~ 300 DEG C; Distillation time is 2 ~ 5h, is preferably 2 ~ 4h.
6., according to claim 1 containing the treatment process of selenium mercury acid mud, it is characterized in that, in described step 6:
With salt acid for adjusting pH value preferably to 0.1 ~ 0.5;
The reductive agent added is S-WAT or sulfurous gas, and consumption is preferably 1.0 ~ 1.5 times of reduction selenium theoretical amount;
The temperature of reduction reaction is preferably 80 ~ 90 DEG C, and the time of reduction reaction is preferably 3 ~ 4h.
7., according to claim 1 containing the treatment process of selenium mercury acid mud, it is characterized in that, after described step 6 obtains described reduction after liquid, described method also comprises:
Liquid after described reduction is obtained sodium-chlor after evaporative crystallization, and the sodium-chlor obtained can return described step 1 to be continued to recycle.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106542507A (en) * | 2016-12-08 | 2017-03-29 | 湖南水口山有色金属集团有限公司 | A kind of method for producing low impurity impure selenium with mercurous sour mud oxygen pressure alkali immersion liquid |
| CN106756038A (en) * | 2016-12-08 | 2017-05-31 | 湖南水口山有色金属集团有限公司 | A kind of method that selenium mercury is separated in the acid mud from copper-lead-zinc smelting sulfate system |
| CN106893865A (en) * | 2017-04-01 | 2017-06-27 | 湖南省环境保护科学研究院 | The method that mercury is extracted from weight acid mud is related to |
| CN108004408A (en) * | 2017-12-13 | 2018-05-08 | 江西理工大学 | Separating hydrargyrum, selenium, the method for lead in a kind of acid mud from nonferrous smelting |
| CN108179290A (en) * | 2017-12-21 | 2018-06-19 | 昆明寰世科技开发有限公司 | A kind of method that mercury is enriched with from sour mud |
| CN108220606A (en) * | 2018-02-07 | 2018-06-29 | 云南省固体废物管理中心 | A kind of method of lead, mercury, selenium synthetical recovery in Copper making acid mud |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106542507A (en) * | 2016-12-08 | 2017-03-29 | 湖南水口山有色金属集团有限公司 | A kind of method for producing low impurity impure selenium with mercurous sour mud oxygen pressure alkali immersion liquid |
| CN106756038A (en) * | 2016-12-08 | 2017-05-31 | 湖南水口山有色金属集团有限公司 | A kind of method that selenium mercury is separated in the acid mud from copper-lead-zinc smelting sulfate system |
| CN106893865A (en) * | 2017-04-01 | 2017-06-27 | 湖南省环境保护科学研究院 | The method that mercury is extracted from weight acid mud is related to |
| CN108004408A (en) * | 2017-12-13 | 2018-05-08 | 江西理工大学 | Separating hydrargyrum, selenium, the method for lead in a kind of acid mud from nonferrous smelting |
| CN108179290A (en) * | 2017-12-21 | 2018-06-19 | 昆明寰世科技开发有限公司 | A kind of method that mercury is enriched with from sour mud |
| CN108179290B (en) * | 2017-12-21 | 2019-09-24 | 昆明寰世科技开发有限公司 | A method of it being enriched with mercury from sour mud |
| CN108220606A (en) * | 2018-02-07 | 2018-06-29 | 云南省固体废物管理中心 | A kind of method of lead, mercury, selenium synthetical recovery in Copper making acid mud |
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