CN104561558B - Method for treating selenium-containing mercury acid mud - Google Patents
Method for treating selenium-containing mercury acid mud Download PDFInfo
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- CN104561558B CN104561558B CN201510025970.1A CN201510025970A CN104561558B CN 104561558 B CN104561558 B CN 104561558B CN 201510025970 A CN201510025970 A CN 201510025970A CN 104561558 B CN104561558 B CN 104561558B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P10/20—Recycling
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 the processing method of metallurgical technology field, more particularly to a kind of sour mud of mercury containing selenium.
Background technology
At present, it is contained in lead concentrate because handled lead concentrate raw material is complex in the fusion process of lead concentrate
The valuable element such as trace selenium, mercury in smelting process with fume, it is purified after enter towerman's sequence；Work is purified in relieving haperacidity
It is enriched in sequence due to reasons such as dust collection effects in the sour mud of relieving haperacidity.
And the sour mud of mercury containing selenium of the generation is due to complicated component, intractability is relatively large, in the prior art many factories
The part metals reclaimed after simple process in slag are not all processed or only done, are lacked effective processing scheme, are thus caused very
The big wasting of resources, while bringing serious environmental problem.
The content of the invention
It is an object of the invention to provide a kind of processing method of the sour mud of mercury containing selenium, this method can solve the problem that environmental pollution and
The problem of valuable metal recovery utilization rate is not high, and technique is simple, equipment investment is few, pollution-free, good in economic efficiency, is realizing back
While receiving selenium and mercury, moreover it is possible to reclaim lead.
A kind of processing method of the sour mud of mercury containing selenium, methods described includes：
Step 1, the sour mud of mercury containing selenium added in 200~350g/L sodium chloride or calcium chloride solution, add hydrochloric acid tune
Whole solution ph is to 1~2, at 60~95 DEG C after 1~4h of leaching, is separated by filtration and obtains leaching lead liquid and leaching lead skim；
Step 2, addition sodium hydroxide or calcium oxide nertralizer in resulting leaching lead liquid, adjustment solution ph to 7~
9,1-4h is reacted, liquid after hydroxide lead skim is obtained after filtering and is neutralized, the hydroxide lead skim returns to lead smelting system and reclaims lead,
Liquid return to step 1 continues to soak lead after the neutralization；
Step 3, the leaching lead skim for obtaining step 1 are added in 50~100g/L hydrochloric acid, and liquid-solid ratio is 5~15,40~80
At DEG C, oxidant is slowly added to, the consumption of the oxidant is 1.0~2.0 times of the leaching lead skim, 1~3h of leaching, mistake
Leaching mercury slag is obtained after filter separation and mercury solution is soaked；
Step 4, obtained leaching mercury slag return to step 3 carries out to secondary leaching, the leaching mercury solution uses 20~40% mass
The nertralizer of concentration adjusts solution ph to 12~14, and 2~4h of neutralization reaction, mercury oxide is obtained after being separated by filtration and molten containing selenium
Liquid；
Step 5, the mercury oxide for obtaining step 4 are added in the reductant solution after dilution, distilation after mercury is reduced
Obtain mercury metal；
Step 6, the Se solution for obtaining step 4 are with salt acid for adjusting pH value to 0.1~2.0, and it is theoretical to add reduction selenium
The reducing agent of 1.0~2.0 times of amount, 2~5h of reduction reaction at 60~95 DEG C is filtrated to get liquid after impure selenium and reduction.
As seen from the above technical solution provided by the invention, the processing method technique is simple, equipment investment is few, without dirt
It is dye, good in economic efficiency, reclaim selenium and while mercury realizing, moreover it is possible to reclaim lead.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, being used required in being described below to embodiment
Accompanying drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this
For the those of ordinary skill in field, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings
Accompanying drawing.
Fig. 1 is provided the process flow schematic diagram of the sour mud of mercury containing selenium by the embodiment of the present invention.
Embodiment
With reference to the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Ground is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on this
The embodiment of invention, the every other implementation that those of ordinary skill in the art are obtained under the premise of creative work is not made
Example, belongs to protection scope of the present invention.
The embodiment of the present invention is described in further detail below in conjunction with accompanying drawing, is as shown in Figure 1 present invention implementation
Example provides the process flow schematic diagram of the sour mud of mercury containing selenium, the treating method comprises：
Step 1, the sour mud of mercury containing selenium added in 200~350g/L sodium chloride or calcium chloride solution, add hydrochloric acid tune
Whole solution ph is to 1~2, at 60~95 DEG C after 1~4h of leaching, is separated by filtration and obtains leaching lead liquid and leaching lead skim；
In this step, the sour mud of the sodium chloride or calcium chloride solution and the mercury containing selenium liquid-solid ratio (ie in solution volume/
Material dry weight) it is 8~25：1, and preferably liquid-solid ratio is 10~20；
And the sodium chloride or calcium chloride solution are preferably 300~350g/L, solution ph is adjusted preferably to 1.0~1.5,
It is preferred that leaching lead temperature be 80~95 DEG C.
Step 2, addition sodium hydroxide or calcium oxide nertralizer in resulting leaching lead liquid, adjustment solution ph to 7~
9,1-4h is reacted, liquid after hydroxide lead skim is obtained after filtering and is neutralized, the hydroxide lead skim returns to lead smelting system and reclaims lead,
Liquid return to step 1 continues to soak lead after the neutralization；
In this step, sodium hydroxide or calcium oxide nertralizer are added, adjustment solution ph is preferably 7~8.
Step 3, the leaching lead skim for obtaining step 1 are added in 50~100g/L hydrochloric acid, and liquid-solid ratio is 5~15,40~80
At DEG C, oxidant is slowly added to, the consumption of the oxidant is 1.0~2.0 times of the leaching lead skim, 1~3h of leaching, mistake
The isolated leaching mercury slag of filter and leaching mercury solution；
In this step, the concentration of hydrochloric acid added in the leaching lead skim is preferably 70~100g/L, liquid-solid ratio preferably
For 5~10, extraction temperature preferably is 50~80 DEG C；
The oxidant added can include sodium chlorate, hydrogen peroxide, hypochlorous acid or sodium hypochlorite, preferably sodium chlorate or double
Oxygen water；
And the consumption of the oxidant is preferably the leaching 1.0~1.5 times of lead skim, preferably the leaching time be 1~
2h。
Step 4, obtained leaching mercury slag return to step 3 carries out to secondary leaching, the leaching mercury solution uses 20~40% mass
The nertralizer of concentration adjusts solution ph to 12~14, and 2~4h of neutralization reaction, mercury oxide is obtained after being separated by filtration and molten containing selenium
Liquid；
In this step, the nertralizer used is sodium hydroxide, and preferred mass concentration is 30~40%, adjusts solution
PH value is preferably to 13~14, and the neutralization reaction time is preferably 2~3h.
Step 5, the mercury oxide for obtaining step 4 are added in the reductant solution after dilution, distilation after mercury is reduced
Obtain mercury metal；
In this step, the reductant solution used is hydrazine hydrate solution, and the consumption of hydrazine hydrate is reduction-oxidation mercury
1.0~1.5 times of theoretical amount, preferably 1.0~1.2 times；
The vapo(u)rizing temperature of distilation is 150~300 DEG C, preferably 200~300 DEG C；Distillation time is 2~5h, preferably
For 2~4h.
Step 6, the Se solution for obtaining step 4 are with salt acid for adjusting pH value to 0.1~2.0, and it is theoretical to add reduction selenium
The reducing agent of 1.0~2.0 times of amount, 2~5h of reduction reaction at 60~95 DEG C is filtrated to get liquid after impure selenium and reduction.
In this step, with salt acid for adjusting pH value preferably to 0.1~0.5；
The reducing agent added can be sodium sulfite or sulfur dioxide, and preferable amount is the 1.0 of reduction selenium theoretical amount
~1.5 times；
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, being obtained in the step 6 after the reduction after liquid, further by liquid after the reduction after evaporative crystallization
Obtain sodium chloride, resulting partial oxidation sodium, which can return to the step 1 and continue cycling through, to be used.
Processing method of the present invention is described further with reference to instantiation：
Embodiment 1,
1. the sour mud 50g of mercury containing selenium is taken, analysis main chemical compositions are：Se 32.85%, Hg 35.44%, Pb
15.12%.Sour mud is added in 500ml 300g/L sodium chloride solutions, plus hydrochloric acid adjusts pH~1,90 DEG C, reacts 2h；Filtered after filtering
Liquid adds sodium hydroxide and adjusts pH~8, reacts 2h, and the lead skim that sinks contains Pb 79.85%, and heavy lead skim is returned into pyrometallurgical smelting of lead system and reclaims lead.
2. leaching lead skim is added in 80g/L HCl solutions, in liquid-solid ratio 10:1st, under conditions of 80 DEG C, 16.82g chlorine is added
Sour sodium, reacts 2h, and leached mud contains Se 3.03%, Hg 0.64%, and leached mud returns to Oxidation Leaching and carries out secondary leach；Leachate
Adding 40%NaOH adjusts pH value of solution to 13.5, reacts 2h, obtains rich mercury slag, mercurous 90.74%；Rich mercury slag adds hydrazine hydrate solution
Middle reduction, slag obtains mercury metal in distilling 2h at 240 DEG C after reduction.
3. liquid acid adding is adjusted and 18g sodium sulfites reduction selenium is added at pH to 0.5,80 DEG C after heavy mercury, reacts 3h, obtains grey black
Impure selenium, containing selenium 98.86%.
4. according to prior art after reduction selenium evaporative crystallization sodium chloride in liquid, resulting partial oxidation sodium can continue
Recycle.
Embodiment 2,
1. the sour mud 100g of mercury containing selenium is taken, analysis main component is：Se 32.85%, Hg 35.44%, Pb 15.12%.Will
Sour mud is added in 1500ml 350g/L calcium chloride solutions, and acid adding adjusts pH~1.5,90 DEG C, reacts 2h；Filtrate adds oxygen after filtering
Change calcium and adjust pH~8.5, react 3h, the lead skim that sinks contains Pb 81.63%, heavy lead skim is returned into pyrometallurgical smelting of lead system and reclaims lead.
2. leaching lead skim is added in 100g/L HCl solutions, in liquid-solid ratio 8:1st, under conditions of 60 DEG C, 100ml dioxygens are added
Water, reacts 3h, and leached mud contains Se2.73%, Hg 0.41%, and leached mud returns to Oxidation Leaching and carries out secondary leach；Leachate adds
Entering 30%NaOH adjusts pH value of solution to 13.0, reacts 2h, obtains rich mercury slag, mercurous 86.32%；Rich mercury slag is added in hydrazine hydrate solution
Reduction, slag obtains mercury metal in distilling 4h at 200 DEG C after reduction.
3. liquid acid adding is adjusted and 27g sodium sulfites reduction selenium is added at pH to 0.2,90 DEG C after heavy mercury, reacts 2h, obtains grey black
Impure selenium, containing selenium 97.91%.
4. according to prior art from liquid evaporative crystallization sodium chloride after reduction selenium, resulting partial oxidation sodium can continue to follow
Ring is used.
Embodiment 3,
1. the sour mud 50g of mercury containing selenium is taken, analysis main component is：Se26.44%, Hg 26.68%, Pb 24.61%.By acid
Mud is added in 600ml 280g/L sodium chloride solutions, and acid adding adjusts pH~1,85 DEG C, reacts 2h；Filtrate adds sodium hydroxide after filtering
PH~8 are adjusted, 2h is reacted, the lead skim that sinks contains Pb80.23%, heavy lead skim is returned into pyrometallurgical smelting of lead system and reclaims lead.
2. leaching lead skim is added in 100g/L HCl solutions, in liquid-solid ratio 10:1st, under conditions of 70 DEG C, 50ml dioxygens are added
Water, reacts 2h, and leached mud contains Se 2.44%, Hg 0.27%, and leached mud returns to Oxidation Leaching and carries out secondary leach；Leachate adds
Entering 40%NaOH adjusts pH value of solution to 14, reacts 2h, obtains rich mercury slag, mercurous 89.13%；Rich mercury slag is added in hydrazine hydrate solution also
Slag obtains mercury metal in distilling 2h at 240 DEG C after original, reduction.
3. liquid acid adding is adjusted and 13.6g sodium sulfites reduction selenium is added at pH to 0.5,90 DEG C after heavy mercury, reacts 2h, obtains greyish black
Color impure selenium, containing selenium 98.67%.
4. according to prior art from liquid evaporative crystallization sodium chloride after reduction selenium, resulting partial oxidation sodium can continue to follow
Ring is used.
In summary, the processing method that the embodiment of the present invention is provided uses wet processing flow, and solution is recycled, nothing
Outer row, it is environmentally friendly, belong to clean metallurgical technology；Flow is short simultaneously, simple to operate, the valuable metal element in the acid mud of mercury containing selenium
The rate of recovery of selenium, mercury and lead is up to more than 96%, and has obtained byproduct sodium chloride, and sour mud valuable element is solved well
Problem of complex utilization, greatly reduce the pollution of selenium and mercury to environment in sour mud, efficiently utilize secondary resource.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art is in the technical scope of present disclosure, the change or replacement that can be readily occurred in,
It should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Enclose and be defined.
Claims (5)
1. the processing method of the sour mud of a kind of mercury containing selenium, it is characterised in that methods described includes：
Step 1, the sour mud of mercury containing selenium added in 200~350g/L sodium chloride or calcium chloride solution, add hydrochloric acid adjustment molten
Liquid pH value is to 1~2, at 60~95 DEG C after 1~4h of leaching, is separated by filtration and obtains leaching lead liquid and leaching lead skim；
Step 2, addition sodium hydroxide or calcium oxide nertralizer in resulting leaching lead liquid, adjustment solution ph to 7~9, instead
Liquid after hydroxide lead skim is obtained after 1-4h, filtering and is neutralized is answered, the hydroxide lead skim returns to lead smelting system and reclaims lead, described
Liquid return to step 1 continues to soak lead after neutralization；
Step 3, the leaching lead skim for obtaining step 1 are added in 50~100g/L hydrochloric acid, and liquid-solid ratio is 5~15, at 40~80 DEG C,
Oxidant is slowly added to, the consumption of the oxidant is 1.0~2.0 times of the leaching lead skim, 1~3h of leaching, filtering point
Leaching mercury slag is obtained from after and mercury solution is soaked；
Step 4, obtained leaching mercury slag return to step 3 carries out to secondary leaching, the leaching mercury solution uses 20~40% mass concentrations
Nertralizer adjust solution ph to 12~14, and 2~4h of neutralization reaction obtains mercury oxide and Se solution after being separated by filtration；
Wherein, the nertralizer used is sodium hydroxide；
Step 5, the mercury oxide for obtaining step 4 are added in the reductant solution after dilution, and distilation is obtained after mercury is reduced
Mercury metal；Wherein, the reductant solution used is hydrazine hydrate solution, and the consumption of hydrazine hydrate is reduction-oxidation mercury theoretical amount
1.0~1.5 times；The vapo(u)rizing temperature of distilation is 150~300 DEG C；Distillation time is 2~5h；
Step 6, the Se solution for obtaining step 4, to 0.1~2.0, and add reduction selenium theoretical amount 1.0 with salt acid for adjusting pH value
~2.0 times of reducing agent, 2~5h of reduction reaction at 60~95 DEG C is filtrated to get liquid after impure selenium and reduction.
2. the processing method of the sour mud of mercury containing selenium according to claim 1, it is characterised in that in the step 1：
The liquid-solid ratio of the sodium chloride or calcium chloride solution and the sour mud of the mercury containing selenium is 8~25；
And the sodium chloride or calcium chloride solution are specially 300~350g/L, adjustment solution ph is specific to 1.0~1.5, soaks lead
Temperature is specially 80~95 DEG C.
3. the processing method of the sour mud of mercury containing selenium according to claim 1, it is characterised in that in step 3：
The concentration of hydrochloric acid added in the leaching lead skim is specially 70~100g/L, and liquid-solid ratio is specially 5~10, extraction temperature tool
Body is 50~80 DEG C；
The oxidant added includes sodium chlorate, hydrogen peroxide, hypochlorous acid or sodium hypochlorite；
And the consumption of the oxidant is specially 1.0~1.5 times of the leaching lead skim, the leaching time is specially 1~2h.
4. the processing method of the sour mud of mercury containing selenium according to claim 1, it is characterised in that in the step 6：
It is specific to 0.1~0.5 with salt acid for adjusting pH value；
The reducing agent added is sodium sulfite or sulfur dioxide, and consumption is specially reduce selenium theoretical amount 1.0~1.5 times；
The temperature of reduction reaction is specially 80~90 DEG C, and the time of reduction reaction is specially 3~4h.
5. the processing method of the sour mud of mercury containing selenium according to claim 1, it is characterised in that the step 6 obtain it is described also
After original after liquid, methods described also includes：
Liquid after the reduction is obtained into sodium chloride after evaporative crystallization, resulting sodium chloride, which can return to the step 1, to be continued to follow
Ring is used.
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| CN106542507B (en) * | 2016-12-08 | 2019-06-18 | 湖南水口山有色金属集团有限公司 | A method of low impurity impure selenium is produced with mercurous sour mud oxygen pressure alkali immersion liquid |
| CN106756038B (en) * | 2016-12-08 | 2018-09-25 | 湖南水口山有色金属集团有限公司 | A method of detaching selenium mercury from copper-lead-zinc smelting sulfate system acid mud |
| CN106893865B (en) * | 2017-04-01 | 2018-10-30 | 湖南省环境保护科学研究院 | From the method for relating to extraction mercury in the sour mud of weight |
| CN108004408B (en) * | 2017-12-13 | 2019-06-21 | 江西理工大学 | A method of separating hydrargyrum, selenium, lead from nonferrous smelting acid 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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