CN105039703A - Method for recycling manganese and lead in electrolytic manganese anode mud - Google Patents

Method for recycling manganese and lead in electrolytic manganese anode mud Download PDF

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Publication number
CN105039703A
CN105039703A CN201510396827.3A CN201510396827A CN105039703A CN 105039703 A CN105039703 A CN 105039703A CN 201510396827 A CN201510396827 A CN 201510396827A CN 105039703 A CN105039703 A CN 105039703A
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China
Prior art keywords
electrolytic manganese
anode mud
mud
manganese anode
lead
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Application number
CN201510396827.3A
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Chinese (zh)
Inventor
杨勇
秦旭芝
黄冠汉
刘栋柱
邓永光
明宪权
韦旭甜
严超
梁敏
吴晓丹
何溯结
刘登祥
Original Assignee
中信大锰矿业有限责任公司大新锰矿分公司
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Priority to CN201510396827.3A priority Critical patent/CN105039703A/en
Publication of CN105039703A publication Critical patent/CN105039703A/en

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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention discloses a method for recycling manganese and lead in electrolytic manganese anode mud. The method is characterized by comprising the following steps that (1) the electrolytic manganese anode mud is subjected to reduction leaching, anode liquor, reducing agents and a concentrated sulfuric acid solution are sequentially added into the electrolytic manganese anode mud to be subjected to a reduction reaction for 6-10 h, then filter pressing is conducted, and leaching residues containing PbSO4 and leaching liquor containing MnSO4 are obtained; (2) the leaching residues are processed, the obtained leaching residues are aired at the temperature of 30-35 DEG C until the moisture content is smaller than or equal to 5%, and then a lead concentrate product can be obtained; and (3) the leaching liquor is processed, the leaching liquor obtained in the step (1) is collected and then is reused as anode liquor to be recycled according to the step (1). The problem of stacking pollution of the electrolytic manganese anode mud is solved, separation of manganese and lead can be achieved, valuable lead is recycled, and economic value is created. The method is easy to operate, has feasibility and has certain popularization value in the production of the field.

Description

Manganese and plumbous method is reclaimed in electrolytic manganese anode mud
Technical field
The invention belongs to field of metallurgy, particularly in a kind of electrolytic manganese anode mud, reclaim manganese and plumbous method.
Background technology
Electrolytic manganese anode mud is by product when producing electrolytic metal Mn, positive plate produced, because wherein containing the plurality of impurities such as Pb, Se, Co, Ni, main pollution element is Pb, Se, the mineral composition of electrolytic manganese anode mud and complex structure, the hydrous oxide symbiotic relationship of lead wherein and manganese is very close, most of manganese oxide jelly becomes with gluey zonal structure, and crystalline form grows imperfection, adopts mechanical sorting method can not to purify manganese and reclaim plumbous.At present, the anode sludge except minute quantity is used as except chemical fertilizer raw material and cement adjustable solidification agent, and heap is abandoned mostly, or as Mn series alloy raw material, directly uses simply.The former causes the wasting of resources, greatly reduces Business Economic Benefit, and land occupation, causes heavy metal contamination, and the latter causes lead volatility, and the anode sludge per ton will volatilize nearly 50 kilograms of lead metal, not only waste lead resource, the more important thing is serious environment pollution.According to analytical test, in anode slag, Mn content is 40% ~ 50%, is more than 4% containing Pb, is a kind of well manganese lead resource.Owing to containing a certain amount of Pb in the anode sludge, electrolytic manganese anode slag has clearly been listed in the useless management of danger by current country, and the treatment processs such as conventional stacking can bring the rising of cost.Therefore, how economic environmental protection ground recycles electrolytic manganese anode mud is very significant.
Summary of the invention
Goal of the invention of the present invention is to provide in a kind of electrolytic manganese anode mud and reclaims manganese and plumbous method, electrolytic manganese anode mud resource utilization can not only be recycled, solve electrolytic manganese anode mud and stack pollution problem, and the separation of manganese lead can be realized, reclaim valuable lead, create economic worth.
To achieve these goals, the present invention is achieved through the following technical solutions:
Reclaim manganese and plumbous method in electrolytic manganese anode mud, comprise the following steps:
(1) electrolytic manganese anode mud reducing leaching: successively adding anolyte, reductive agent and concentrated sulfuric acid solution carries out reduction reaction to electrolytic manganese anode mud, and the reaction times is 6-10h, then carries out press filtration, obtains containing PbSO 4leached mud and containing MnSO 4leach liquor;
(2) process of leached mud: leached mud obtained above airing at 30 DEG C-35 DEG C, to water ratio≤5%, is namely obtained lead ore concentrate product;
(3) process of leach liquor: leach liquor step (1) obtained is collected rear resume at step (1) and continued to recycle as anolyte.
In the present invention, as further illustrating, the mass ratio of described electrolytic manganese anode mud and anolyte is 1:2-6.
In the present invention, as further illustrating, the solid-liquid mass ratio of described electrolytic manganese anode mud and reductive agent is 8-20:1.
In the present invention, as further illustrating, described reductive agent is waste molasses or industrial glucose.
In the present invention, as further illustrating, the mass ratio of described electrolytic manganese anode mud and the vitriol oil is 1-8:1.
Raw of the present invention all can on the market buying arrive.
Reaction formula of the present invention is as follows:
C 6H 12O 6+12MnO 2+12H 2SO 4=12MnSO 4+6CO 2+18H 2O
Beneficial effect of the present invention is:
1. the present invention using electrolytic manganese anode mud directly as reactant, do not need to carry out playing any process such as powder to electrolytic manganese anode mud, reaction process does not need heating, reaction process is thermopositive reaction, temperature of reaction system can be climbed to more than 80 DEG C, the object of simple flow step can be realized, and then reduce production cost.
2. the invention provides the new road of the recycling of an electrolytic manganese anode mud environmental protection, solve electrolytic manganese anode mud and stack pollution problem, and realize manganese, plumbous separation, reclaim valuable lead, create economic worth.
3. the anolyte that the present invention adopts is the waste liquid produced in manganese metal production process, mn ion content in anolyte is low, after anode sludge reducing leaching, in waste liquid, mn ion content raises, following cycle is made to produce in leach liquor process, do not need to add a large amount of breezes, realize the object economized in raw materials.
4. the leach liquor of the present invention to electrolytic manganese anode mud reducing leaching returns to production system after collecting and continues to put into production as anolyte, reduces needed for cyclic production and adds a large amount of breeze, be rich in MnSO in leach liquor 4, thus improve Mn 2+the rate of recovery, manganese recovery ratio reaches more than 95%, and acid also can return systemic circulation utilize, in the process of electrolytic manganese anode mud reducing leaching, initial spent acid>=200g/L, spent acid>=30g/L after reducing leaching, saved resource.
5. lead tolerance > 30% in leached mud of the present invention, < 1% is measured containing Mn, lead recovery reaches more than 96%, can be used as lead ore concentrate after carrying out airing to water ratio≤5% to leached mud to sell, bring certain economic benefit, under 30 DEG C of-35 DEG C of conditions, airing is carried out to leached mud, the airing time can be shortened, prevent when water ratio is larger oxidized.
6. the present invention adopts specific solid-to-liquid ratio to design, the rate of recovery that is plumbous, manganese can be improved, use waste molasses and industrial glucose as reductive agent, cheap, can production cost be reduced, the new road of waste molasses and industrial glucose environmental protection treatment is also provided, the inventive method is simple to operate, there is feasibility, in this area produces, there is certain promotional value.
Accompanying drawing explanation
Fig. 1 is schema of the present invention.
Embodiment
Below by way of specific embodiment, the invention will be further described.The present invention is not limited to following embodiment.
embodiment 1:
Reclaim manganese and plumbous method in electrolytic manganese anode mud, comprise the following steps:
(1) electrolytic manganese anode mud reducing leaching: successively adding anolyte, waste molasses and concentrated sulfuric acid solution carries out reduction reaction to electrolytic manganese anode mud, the mass ratio of electrolytic manganese anode mud and anolyte is 1:2, the solid-liquid mass ratio of electrolytic manganese anode mud and reductive agent is 8:1, the mass ratio of electrolytic manganese anode mud and the vitriol oil is 1:1, reaction times is 6h, then carry out press filtration, obtain the leached mud containing PbSO4 and the leach liquor containing MnSO4;
(2) process of leached mud: be 5% by leached mud obtained above airing to water ratio at 30 DEG C, namely obtains lead ore concentrate product;
(3) process of leach liquor: leach liquor step (1) obtained is collected rear resume at step (1) and continued to recycle as anolyte.
embodiment 2:
Reclaim manganese and plumbous method in electrolytic manganese anode mud, comprise the following steps:
(1) electrolytic manganese anode mud reducing leaching: successively adding anolyte, industrial glucose and concentrated sulfuric acid solution carries out reduction reaction to electrolytic manganese anode mud, the mass ratio of electrolytic manganese anode mud and anolyte is 1:6, the solid-liquid mass ratio of electrolytic manganese anode mud and reductive agent is 20:1, the mass ratio of electrolytic manganese anode mud and the vitriol oil is 8:1, reaction times is 10h, then carry out press filtration, obtain the leached mud containing PbSO4 and the leach liquor containing MnSO4;
(2) process of leached mud: leached mud obtained above airing at 35 DEG C, to water ratio to 4%, is namely obtained lead ore concentrate product;
(3) process of leach liquor: leach liquor step (1) obtained is collected rear resume at step (1) and continued to recycle as anolyte.
embodiment 3:
Reclaim manganese and plumbous method in electrolytic manganese anode mud, comprise the following steps:
(1) electrolytic manganese anode mud reducing leaching: successively adding anolyte, waste molasses and concentrated sulfuric acid solution carries out reduction reaction to electrolytic manganese anode mud, the mass ratio of electrolytic manganese anode mud and anolyte is 1:3, the solid-liquid mass ratio of electrolytic manganese anode mud and reductive agent is 10:1, the mass ratio of electrolytic manganese anode mud and the vitriol oil is the 2:1 reaction times is 8h, then carry out press filtration, obtain the leached mud containing PbSO4 and the leach liquor containing MnSO4;
(2) process of leached mud: leached mud obtained above airing at 32 DEG C, to water ratio to 3%, is namely obtained lead ore concentrate product;
(3) process of leach liquor: leach liquor step (1) obtained is collected rear resume at step (1) and continued to recycle as anolyte.
embodiment 4:
Reclaim manganese and plumbous method in electrolytic manganese anode mud, comprise the following steps:
(1) electrolytic manganese anode mud reducing leaching: successively adding anolyte, waste molasses and concentrated sulfuric acid solution carries out reduction reaction to electrolytic manganese anode mud, the mass ratio of electrolytic manganese anode mud and anolyte is 1:4, the solid-liquid mass ratio of electrolytic manganese anode mud and reductive agent is 15:1, the mass ratio of electrolytic manganese anode mud and the vitriol oil is the 4:1 reaction times is 8h, then carry out press filtration, obtain the leached mud containing PbSO4 and the leach liquor containing MnSO4;
(2) process of leached mud: leached mud obtained above airing at 33 DEG C, to water ratio to 2%, is namely obtained lead ore concentrate product;
(3) process of leach liquor: leach liquor step (1) obtained is collected rear resume at step (1) and continued to recycle as anolyte.
embodiment 5:
Reclaim manganese and plumbous method in electrolytic manganese anode mud, comprise the following steps:
(1) electrolytic manganese anode mud reducing leaching: successively adding anolyte, waste molasses and concentrated sulfuric acid solution carries out reduction reaction to electrolytic manganese anode mud, the mass ratio of electrolytic manganese anode mud and anolyte is 1:5, the solid-liquid mass ratio of electrolytic manganese anode mud and reductive agent is 18:1, the mass ratio of electrolytic manganese anode mud and the vitriol oil is 6:1, reaction times is 8h, then carry out press filtration, obtain the leached mud containing PbSO4 and the leach liquor containing MnSO4;
(2) process of leached mud: leached mud obtained above airing at 34 DEG C, to water ratio to 4%, is namely obtained lead ore concentrate product;
(3) process of leach liquor: leach liquor step (1) obtained is collected rear resume at step (1) and continued to recycle as anolyte.
Carry out the detection as following table to embodiment 1-5, detection case is in table 1:
Table 1 detection case table
As seen from the above table, after the inventive method process, lead tolerance > 30% in leached mud, manganese content < 1%, manganese recovery ratio reaches more than 95%.
Test with embodiment 1, with reference to recent market price, calculate the ton amount of metal consuming cost of anode sludge leaching method of the present invention and carbonic acid ore deposit extract technology, result is as shown in table 2:
Cost comparisons is leached in table 2 anode sludge leaching method of the present invention and carbonic acid ore deposit
Note: consume the sulfuric acid amount that sulfuric acid refers to reaction process actual consumption in table;
Carbonic acid ore deposit extract technology consumes sulfuric acid amount=the add sulfuric acid amount in the vitriol oil+anolyte;
Wherein add the vitriol oil by producing actual 2.1 tons of sulfuric acid/ton product at present, anolyte consumes 45m 3, sulfuric acid presses 33.3g/L densitometer, amounts to 1.5 tons of acid, and carbonic acid ore deposit extract technology consumes sulfuric acid amount and amounts to 3.6 tons;
Anode sludge leaching method of the present invention consumes sulfuric acid amount=actual consumption sulfuric acid amount;
Raw material calculates by market price, anode sludge unit price 1200 yuan/t, the 427 yuan/t in carbonic acid ore deposit, glucose 3500 yuan/t, the vitriol oil 270 yuan/t.
Embodiment 1 and carbonic acid ore deposit extract technology advantage contrast situation are in table 3:
Table 3 anode sludge leaching method of the present invention and carbonic acid ore deposit extract technology advantage contrast
Note: raw material calculates by market price, and lead skim presses amount of metal 8000 yuan/t;
Real cost=liquid cost-cost recovery processed.
As can be seen from Table 3, anode sludge leaching method of the present invention just can complete reaction owing to can utilize the acid in the anolyte of equivalent, has saved and has used sour cost, simultaneous reactions achieves plumbous manganese and is separated, lead is recycled, and creates part and is worth, make real cost lower than the liquid cost processed in carbonic acid ore deposit.

Claims (5)

1. reclaim manganese and plumbous method in electrolytic manganese anode mud, it is characterized in that, comprise the following steps:
(1) electrolytic manganese anode mud reducing leaching: successively adding anolyte, reductive agent and concentrated sulfuric acid solution carries out reduction reaction to electrolytic manganese anode mud, and the reaction times is 6-10h, then carries out press filtration, obtains containing PbSO 4leached mud and containing MnSO 4leach liquor;
(2) process of leached mud: leached mud obtained above airing at 30 DEG C-35 DEG C, to water ratio≤5%, is namely obtained lead ore concentrate product;
(3) process of leach liquor: leach liquor step (1) obtained is collected rear resume at step (1) and continued to recycle as anolyte.
2. reclaim manganese and plumbous method in electrolytic manganese anode mud according to claim 1, it is characterized in that: the mass ratio of described electrolytic manganese anode mud and anolyte is 1:2-6.
3. reclaim manganese and plumbous method in electrolytic manganese anode mud according to claim 2, it is characterized in that: the mass ratio of described electrolytic manganese anode mud and reductive agent is 8-20:1.
4. reclaim manganese and plumbous method in the electrolytic manganese anode mud according to claim 1 or 2 or 3, it is characterized in that: described reductive agent is waste molasses or industrial glucose.
5. reclaim manganese and plumbous method in electrolytic manganese anode mud according to claim 4, it is characterized in that: the mass ratio of described electrolytic manganese anode mud and the vitriol oil is 1-8:1.
CN201510396827.3A 2015-07-08 2015-07-08 Method for recycling manganese and lead in electrolytic manganese anode mud CN105039703A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106048236A (en) * 2016-08-16 2016-10-26 贵州铜仁金瑞锰业有限责任公司 Comprehensive recovery treatment process for electrolytic manganese anode slime
CN106834754A (en) * 2016-12-29 2017-06-13 宁夏天元锰业有限公司 A kind of method that manganese is reclaimed in electrolytic manganese anode slag
CN108118156A (en) * 2018-01-10 2018-06-05 中信大锰矿业有限责任公司 A kind of electrolytic manganese anode mud separation production electrolytic manganese metal and the method for recycling lead
CN108754145A (en) * 2018-05-30 2018-11-06 宁夏天元锰业有限公司 The technique of valuable metal in a kind of recycling electrolytic manganese anode mud
CN108823410A (en) * 2018-06-01 2018-11-16 青海华信环保科技有限公司 A method of feed grade manganese sulfate and recycling lead are prepared with electrolytic zinc anode mud
CN109457110A (en) * 2018-11-27 2019-03-12 中信大锰矿业有限责任公司 A kind of acids reduction leaching method of Gabon's manganese oxide ore
CN109468458A (en) * 2018-11-27 2019-03-15 中信大锰矿业有限责任公司 A kind of method that Gabon's manganese oxide ore leaches and recycles iron
CN110218860A (en) * 2019-05-30 2019-09-10 贵州大学 A kind of method that anode slag low-temperature reduction roasted-prepared manganese sulfate solution recycling lead
CN110358916A (en) * 2019-07-12 2019-10-22 重庆大学 A kind of electric field-enhanced method for recycling manganese and lead in electrolytic manganese anode mud
CN110408786A (en) * 2019-08-29 2019-11-05 贵州大学 A kind of method that the catalysis of electrolytic manganese anode slag prepares manganese sulfate solution and recycles lead

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CN103789551A (en) * 2014-02-18 2014-05-14 广西大学 Method for preparing manganese sulfate electrolyte and recycling lead by using electrolytic manganese anode mud

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106048236A (en) * 2016-08-16 2016-10-26 贵州铜仁金瑞锰业有限责任公司 Comprehensive recovery treatment process for electrolytic manganese anode slime
CN106048236B (en) * 2016-08-16 2018-09-25 贵州铜仁金瑞锰业有限责任公司 A kind of electrolytic manganese anode mud synthetical recovery treatment process
CN106834754A (en) * 2016-12-29 2017-06-13 宁夏天元锰业有限公司 A kind of method that manganese is reclaimed in electrolytic manganese anode slag
CN108118156A (en) * 2018-01-10 2018-06-05 中信大锰矿业有限责任公司 A kind of electrolytic manganese anode mud separation production electrolytic manganese metal and the method for recycling lead
CN108118156B (en) * 2018-01-10 2019-11-26 中信大锰矿业有限责任公司 A kind of method that electrolytic manganese anode mud separation produces electrolytic manganese metal and recycles lead
CN108754145A (en) * 2018-05-30 2018-11-06 宁夏天元锰业有限公司 The technique of valuable metal in a kind of recycling electrolytic manganese anode mud
CN108754145B (en) * 2018-05-30 2019-09-17 宁夏天元锰业有限公司 The technique of valuable metal in a kind of recycling electrolytic manganese anode mud
CN108823410A (en) * 2018-06-01 2018-11-16 青海华信环保科技有限公司 A method of feed grade manganese sulfate and recycling lead are prepared with electrolytic zinc anode mud
CN109468458A (en) * 2018-11-27 2019-03-15 中信大锰矿业有限责任公司 A kind of method that Gabon's manganese oxide ore leaches and recycles iron
CN109457110A (en) * 2018-11-27 2019-03-12 中信大锰矿业有限责任公司 A kind of acids reduction leaching method of Gabon's manganese oxide ore
CN110218860A (en) * 2019-05-30 2019-09-10 贵州大学 A kind of method that anode slag low-temperature reduction roasted-prepared manganese sulfate solution recycling lead
CN110358916A (en) * 2019-07-12 2019-10-22 重庆大学 A kind of electric field-enhanced method for recycling manganese and lead in electrolytic manganese anode mud
CN110408786A (en) * 2019-08-29 2019-11-05 贵州大学 A kind of method that the catalysis of electrolytic manganese anode slag prepares manganese sulfate solution and recycles lead

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