CN105177297A - Method for leaching waste lead-acid accumulator paste by utilizing oxidation-reduction characteristic of raw materials - Google Patents
Method for leaching waste lead-acid accumulator paste by utilizing oxidation-reduction characteristic of raw materials Download PDFInfo
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- CN105177297A CN105177297A CN201510665494.XA CN201510665494A CN105177297A CN 105177297 A CN105177297 A CN 105177297A CN 201510665494 A CN201510665494 A CN 201510665494A CN 105177297 A CN105177297 A CN 105177297A
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- lead
- leaching
- magnesium chloride
- concentrate
- sulfide ore
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for conducting wet processing on waste lead paste by utilizing an oxidation-reduction characteristic of raw materials. The method is composed of the following steps that (1) the waste lead-acid accumulator paste and lead sulfide concentrate are added to a proportioned hydrochloric solution for leaching at the mass ratio of 3:1, magnesium chloride is added after a period of reaction, the temperature is adjusted to 80 DEG C-95 DEG C, and the reaction time is 60 min-120 min; (2) after leaching is finished, immediate filtration is conducted with the residual heat, leached residues can be subjected to flotation to extract element sulfur, leachate is subjected to cooling and crystallization to obtain solid lead chloride and crystallization mother liquor which contains MgSO4 and MgCl2; and (3) after being subjected to regeneration through magnesium chloride and purification treatment, the crystallization mother liquor is returned to the waste lead paste and leached with the lead sulfide concentrate simultaneously, excessive calcium chloride is added to the crystallization mother liquor to regenerate the leaching agent magnesium chloride, a byproduct gypsum is produced simultaneously, and after SO42- is removed, the crystallization mother liquor is returned to the waste lead paste and leached with the lead sulfide concentrate simultaneously after being subjected to purification treatment.
Description
Technical field
The present invention relates to a kind of method of lead-acid accumulator cream mud wet-leaching, particularly relate to a kind of method utilizing material oxidation-reduction characteristic simultaneously to leach lead-acid accumulator cream mud and concentrate of lead sulfide ore in hydrochloric acid and magnesium chloride solution, belong to plumbous and secondary lead metallurgical technology field.
Background technology
Mainly contain two kinds of refining leady raw materialses in the world: one is concentrate of lead sulfide ore, and one is lead-acid accumulator.At present, countries in the world all adopt pyrometallurgy technology to extract metallic lead from concentrate of lead sulfide ore.From lead-acid accumulator, reclaim plumbous method is generally first adopt fragmentation-sorting technology refuse battery to be resolved into spent acid, plastic waste, useless grid and scrap lead cream mud four kinds of products.Useless grid can through low smelting heat output lead alloy; Plastic waste and spent acid can be transformed into byproduct through simple process; Scrap lead cream mud needs to produce lead bullion by pyrometallurgy technology.China's pyrometallurgical smelting of lead Technical comparing is advanced, and dust collection device and device are comparatively perfect, and the discharge of sulfurous gas and leaded flue dust all can be up to state standards.But China's pyrometallurgical smelting of lead number of the enterprise is many, industrial scale is large, and the environmental pollution that long-term operation causes is still very important.For this problem, people are seeking always and are developing wet method refining lead in recent decades.It is few that wet method refining lead has greenhouse gas emissions, and energy consumption is low and do not produce pyrogenic process waste residue, the useless advantage such as dirt, sulfur dioxide flue gas.Wet method refining sheath draws together two portions: one is plumbous leaching process, is intended to that the lead in raw material is dissolved and enters leach liquor; Two is reclaim lead from plumbous leach liquor.Plumbous leaching process is the gordian technique in wet method refining splicer skill, is also the popular research topic of current field of hydrometallurgy.
The main chemical compositions of lead-acid accumulator cream mud comprises PbSO
4, PbO
2, PbO and a small amount of Pb, be the part of the most difficult recycling of lead-acid accumulator.The leaching method of scrap lead cream mud mainly comprises.
(1) chlorination leaching process.
With Pb powder or H
2o
2under making the condition of reductive agent, with hydrochloric acid-sodium chloride solution by the lead in scrap lead cream mud with solvable plumbous chloro-complex (Na
2pbCl
4) form leaching.
(2) silicofluoric acid and boron fluoric acid lixiviation process.
First with sodium hydroxide or sodium carbonate, lead sulfate is changed into Pb (OH)
2or PbCO
3, then at Pb powder or H
2o
2under making the condition of reductive agent, with silicofluoric acid or boron fluoric acid by the lead in material with Pb (BF
4)
2or PbSiF
6form leaches.
(3) citric acid lixiviation process.
Scrap lead cream mud citric acid leaching method is achievement in research in recent years.Its process uses H
2o
2make reductive agent, in citric acid solution, the lead in scrap lead cream mud is changed into lead citrate, lead citrate makes it resolve into plumbous oxide through low temperature calcination.
In the above-mentioned leaching method of lead-acid accumulator cream mud, also have the following disadvantages: (1) four kind of leaching method all needs to adopt Pb powder or H
2o
2pbO in reduction scrap lead cream mud
2, cause leaching high cost.(2) silicofluoric acid leaching and boron fluoric acid leach needs to adopt NaOH, Na
2cO
3or (NH
4)
2cO
3by PbSO
4change into Pb (OH)
2or PbCO
3and Na
2sO
4, sweetening process running cost is too high, and output byproduct Na
2sO
4economic worth not high.(3) citric acid leaching process speed of response is comparatively slow, leaches filtrate (comprising there being Na
2sO
4, Na
3c
6h
5o
72H
2o and C
6h
8o
7h
2o) separation and reclaim more difficult; The structure of output lead citrate is comparatively complicated, PbSO in useless cream mud
4leach the lead citrate (Pb obtained
3(C
6h
5o
7)
23H
2o) with PbO and PbO
2leach the lead citrate (Pb(C obtained
6h
6o
7) H
2o) structure is different.
In recent decades, various countries metallargist has carried out large quantifier elimination to the hydrometallurgy of concentrate of lead sulfide ore.Lead in concentrate of lead sulfide ore exists with PbS form, and the concentrate of lead sulfide ore leaching method of exploitation mainly comprises potassium cloride, silicofluoric acid leaches and boron fluoric acid leaches.Three kinds of leaching methods all need to adopt oxygenant by the PbS oxidation in concentrate of lead sulfide ore, and make lead enter solution with plumbous Chloro complex, fluosilicic lead plumbate or boron fluoric acid Lead speciation, sulphur is converted into elementary sulfur and enters in leached mud.
In the hydrometallurgical processes of the concentrate of lead sulfide ore of early development, the negative divalent sulfur in PbS must be oxidized to elementary sulfur by oxygenant by the leaching of concentrate of lead sulfide ore, and then makes divalence lead enter solution.Leach the Cl adopted
2, O
2, Fe
3+(FeCl
3, Fe
2(SiF
6)
3, Fe (BF
4)
3and H
2o
2all have the following disadvantages in oxygenant: (1) four kind of oxygenant price all costly, and then causes leaching process running cost too high; (2) Fe is used
3+make oxygenant and iron can be introduced Leaching Systems; (3) Cl is used
2make oxygenant and can cause the bad control of leaching process, Cl
2easy effusion.
Just because of the deficiency of above-mentioned lead-acid accumulator cream mud and concentrate of lead sulfide ore leaching-out technique, people are seeking the method for the green wet processing scrap lead cream mud of a kind of low cost and concentrate of lead sulfide ore always.
Applicant has developed one HCl-O
2-NaCl system is from the method (patent No.: ZL200910044022.7) of concentrate of lead sulfide ore leaching lead; it is characterized in that concrete technology method is: first granularity is that the concentrate of lead sulfide ore that-200 orders account for 80%-90% is inserted in reactive tank by solid-to-liquid ratio=1:2.5 ~ 5 by (1); solid phase transformation reaction is carried out under copper ion catalysts, oxygen and hydrochloric acid effect; wherein catalyst levels controls at 1g/L ~ 1.5g/L; temperature of reaction is 40 DEG C ~ 75 DEG C; the pH value of solution controls 0.5 ~ 1; oxygen flow is 200ml/min, and the reaction times is not less than 4h; (2) after reaction terminates, solution is cooled to room temperature, then, carries out solid-liquid separation, obtain conversion fluid and solid phase transformation slag, conversion fluid is pending, and conversion slag proceeds to next procedure and leaches; (3) inserted in leaching vat by solid-to-liquid ratio=1:4 ~ 8 by solid phase transformation slag and carry out Leaching of sodium chloride, sodium chloride concentration 4.5-5mol/L, extraction temperature 90 DEG C-95 DEG C, extraction time is 3 ~ 6h; (4) after Leaching reaction terminates, carry out solid-liquid separation, obtain leach liquor and leached mud, leached mud is pending, and leach liquor is plumbous through crystallisation by cooling output solid chlorine.
On the basis of hydrochloric acid-oxygen-Leaching of sodium chloride system, the applicant substitutes sodium-chlor as solubilising complexing agent with magnesium chloride, also been proposed the new system (publication number CN102560108A) that a kind of hydrochloric acid-oxygen-magnesium chloride leaches concentrate of lead sulfide ore.Adopt hydrochloric acid-oxygen-sodium-chlor (or magnesium chloride) system to leach concentrate of lead sulfide ore, leaching yield plumbous in mineral and sulphur to enter slag rate all higher.Deficiency is the oxygenant that leaching process needs to be transformed into as the negative divalent sulfur in PbS with oxygen elementary sulfur, and accelerates oxidizing reaction speed by catalyzer.
Present applicant has proposed the method (patent No.: ZL200910013549.3) of a kind of magnesium chloride desulfurization from lead-acid accumulator cream mud, its technique is carried out as follows: (1) decomposes falling the waste lead accumulator after acid, obtain cream mud, it is pending to enter next procedure; (2) cream mud magnesium chloride solution leaches, and the lead sulfate in cream mud changes into lead chloride and enters solution, and other plumbous oxide compound is stayed in leached mud, and reaction equation is: PbSO
4+ MgCl
2→ PbCl
2+ MgSO
4, the technical qualification that the desulfurization of cream mud is leached are: liquid-solid ratio 3-6:1, density of magnesium chloride 2.5mol/L-5.5mol/L, extraction temperature 80 DEG C-95 DEG C, extraction time 60-120 minute; Leach and completely carry out solid-liquor separation, leached mud is through low smelting heat output lead bullion, and leach liquor crystallisation by cooling, obtain the plumbous and crystalline mother solution of solid chlorine, solid chlorine is plumbous through low smelting heat output lead bullion, and crystalline mother solution returns the desulfurization of cream mud and leaches after magnesium chloride manipulation of regeneration.(3) crystalline mother solution adds calcium chloride sweetening agent magnesium chloride is regenerated, simultaneously output byproduct calcium sulfate, calcium chloride from the leaching process of lead chloride low smelting heat slag, the chemical equation of wherein sweetening agent magnesium chloride regeneration: MgSO
4+ CaCl
2→ MgCl
2+ CaSO
4↓, MgCl
2technical qualification in regenerative process are: temperature of reaction is 40 DEG C-90 DEG C, reaction times 60-120 minute.The method adopts the sweetening agent of magnesium chloride calcellation lead plaster mud, and sweetening effectiveness is good, and desulphurization cost is low.Deficiency is PbO, PbO in scrap lead cream mud
2and a small amount of metallic lead, non-desulfurization conversion PbSO
4in lead need be reclaimed by pyrometallurgical smelting.
Summary of the invention
Object of the present invention is just the deficiency overcoming prior art existence, and for existing lead-acid accumulator cream mud wet processing process Problems existing, propose one and utilize material oxidation-reduction characteristic, leach the novel method of lead-acid accumulator cream mud and concentrate of lead sulfide ore with hydrochloric acid and magnesium chloride solution simultaneously.
The technical solution that the present invention provides is: this method utilizing material oxidation-reduction characteristic wet processing scrap lead cream mud, its feature is made up of following steps.
(1) granularity-200 order is accounted for 80% ~ 90% lead-acid accumulator cream mud and concentrate of lead sulfide ore in mass ratio 3:1 be added in the hydrochloric acid soln prepared and leach; The technical qualification that scrap lead cream mud and concentrate of lead sulfide ore leach simultaneously are: liquid-solid ratio 4 ~ 8:1, temperature of reaction 50 DEG C ~ 80 DEG C, reaction times 60min ~ 120min, and leaching process pH value controls 2 ~ 3; Add magnesium chloride after reaction for some time, Chlorine in Solution magnesium density is 3mol/L ~ 5.5mol/L; After adding magnesium chloride, temperature is transferred to 80 DEG C ~ 95 DEG C, reaction times 60min ~ 120min.The main chemical reactions that scrap lead cream mud and concentrate of lead sulfide ore leach in hydrochloric acid-magnesium chloride solution is simultaneously:
PbO
2+PbS+4HCl→2PbCl
2↓+S↓+2H
2O
Pb+2HCl→PbCl
2↓+H
2↑
PbO+2HCl→PbCl
2↓+H
2O
PbSO
4+MgCl
2→PbCl
2↓+MgSO
4
PbCl
2+MgCl
2→MgPbCl
4。
(2) leaching terminates rear filtered while hot, and leached mud can extract elementary sulfur through flotation; Leach liquor crystallisation by cooling, obtains solid chlorine lead and contains MgSO
4, MgCl
2crystalline mother solution.The reaction equation of leach liquor crystallisation by cooling lead chloride:
MgPbCl
4→PbCl
2↓+MgCl
2。
(3) crystalline mother solution leaches return scrap lead cream mud and concentrate of lead sulfide ore after magnesium chloride regeneration and purifying treatment while.Crystalline mother solution adds excessive calcium chloride makes leaching agent magnesium chloride regenerate, and the chemical equation of output by-produced gypsum is simultaneously:
MgSO
4+CaCl
2+2H
2O→MgCl
2+CaSO
4·2H
2O↓。
Remove SO
4 2-after crystalline mother solution after purifying treatment, return scrap lead cream mud and concentrate of lead sulfide ore while leach operation.
Compared with prior art, the invention has the beneficial effects as follows.
(1) the oxidation-reduction characteristic of lead-acid accumulator cream mud and concentrate of lead sulfide ore is utilized, using hydrochloric acid and magnesium chloride solution as Leaching Systems, can avoid using sodium hydroxide, sodium carbonate or volatile salt as the desulfurization conversion agent of lead-acid accumulator cream mud, significantly can reduce the running cost of lead-acid accumulator cream mud desulfurization conversion process.
(2) PbO in scrap lead cream mud is utilized
2with the oxidation-reduction characteristic each other of the PbS in concentrate of lead sulfide ore, make whole leaching process neither need additional oxidizer, also do not need additional reducing agent, and then cause leaching process running cost significantly to reduce.
(3) leaching agent magnesium chloride not only can reprocessing cycle use, and produces by-produced gypsum simultaneously.
The present invention can carry out hydrometallurgic recovery to the lead in lead-acid accumulator cream mud and concentrate of lead sulfide ore simultaneously, and whole technological process is carried out all in aqueous, can not produce lead dust and SO
2pollution; Leaching liquid recoverable, and form closed cycle, realize no effuent discharge, produce without leaded waste liquid; Obtained intermediates lead chloride can be used as Chemicals and sells, also can through pyrogenic process or the further Footwall drift lead of wet processing.
Leach separately research approach with lead-acid accumulator cream mud and concentrate of lead sulfide ore to compare, in chloride system, the while of two kinds of refining leady raw materialses, the running cost of leaching method can reduce by more than 50%; The leached mud of leaching process output is leaded lower than 2%; Plumbous leaching yield reaches more than 98%.
Accompanying drawing explanation
Accompanying drawing 1 is process flow sheet of the present invention.
Specific embodiments
Now in conjunction with case study on implementation, technical scheme of the present invention is described in detail.
Embodiment 1.
Granularity-200 order is accounted for 80% ~ 90% lead-acid accumulator cream mud and concentrate of lead sulfide ore in mass ratio 3:1 be added in the hydrochloric acid soln prepared and leach, leach liquid-solid ratio 4:1, Leaching reaction temperature 50 C, leaching process pH value controls 2 ~ 3, add magnesium chloride after reaction 60min, density of magnesium chloride is 3mol/L, after adding magnesium chloride, temperature is transferred to 80 DEG C, reaction 60min; Leaching terminates rear filtered while hot, obtains leaded leach liquor and the leached mud containing elemental sulfur.
Result:
Plumbous leaching yield 98.13%
Leached mud leaded 1.97%
Sulphur enters slag rate (sulphur in concentrate of lead sulfide ore) 74.7%.
Embodiment 2.
First-200 orders are accounted for 85% scrap lead cream mud and concentrate of lead sulfide ore in mass ratio 3:1 be added in the hydrochloric acid soln prepared and leach, leaching liquid-solid ratio is 5:1, Leaching reaction temperature 60 C, leaching process pH value controls 2 ~ 3, add magnesium chloride after reaction 90min, density of magnesium chloride is 4mol/L, after adding magnesium chloride, temperature is transferred to 85 DEG C, reaction 60min; Leaching terminates rear filtered while hot, obtains leaded leach liquor and the leached mud containing elemental sulfur.
Result:
Plumbous leaching yield 98.83%
Leached mud leaded 1.91%
Sulphur enters slag rate (sulphur in concentrate of lead sulfide ore) 73.5%.
Embodiment 3.
First-200 orders are accounted for 85% scrap lead cream mud and concentrate of lead sulfide ore in mass ratio 3:1 be added in the hydrochloric acid soln prepared and leach, leaching liquid-solid ratio is 5:1, Leaching reaction temperature 65 DEG C, leaching process pH value controls 2 ~ 3, add magnesium chloride after reaction 120min, density of magnesium chloride is 4.5mol/L, after adding magnesium chloride, temperature is transferred to 90 DEG C, reaction 90min; Leaching terminates rear filtered while hot, obtains leaded leach liquor and the leached mud containing elemental sulfur.
Result:
Plumbous leaching yield 99.04%
Leached mud leaded 1.52%
Sulphur enters slag rate (sulphur in concentrate of lead sulfide ore) 72%.
Embodiment 4.
First-200 orders are accounted for 85% scrap lead cream mud and concentrate of lead sulfide ore in mass ratio 3:1 be added to and prepare
Hydrochloric acid soln in leach, leaching liquid-solid ratio is 6:1, Leaching reaction temperature 70 C, and leaching process pH value controls 2 ~ 3, reaction 120min after add magnesium chloride, density of magnesium chloride is 5mol/L, after adding magnesium chloride, temperature is transferred to 90 DEG C, reaction 90min; Leaching terminates rear filtered while hot, obtains leaded leach liquor and the leached mud containing elemental sulfur.
Result:
Plumbous leaching yield 99.47%
Leached mud leaded 1.48%
Sulphur enters slag rate (sulphur in concentrate of lead sulfide ore) 71.8%.
Embodiment 5.
First-200 orders are accounted for 85% scrap lead cream mud and concentrate of lead sulfide ore in mass ratio 3:1 be added in the hydrochloric acid soln prepared and leach, leaching liquid-solid ratio is 8:1, Leaching reaction temperature 70 C, leaching process pH value controls 2 ~ 3, add magnesium chloride after reaction 120min, density of magnesium chloride is 5.5mol/L, after adding magnesium chloride, temperature is transferred to 95 DEG C, reaction 120min; Leaching terminates rear filtered while hot, obtains leaded leach liquor and the leached mud containing elemental sulfur.
Result:
Plumbous leaching yield 99.77%
Leached mud leaded 1.39%
Sulphur enters slag rate (sulphur in concentrate of lead sulfide ore) 70.7%.
These are only the preferred embodiments of the present invention.All any amendments done within the spirit and principles in the present invention scope, equivalent replacement, improvement etc., all should be included in protection scope of the present invention.
Claims (1)
1. utilize the method for material oxidation-reduction characteristic wet processing scrap lead cream mud, it is characterized in that being made up of following steps:
(1) granularity-200 order is accounted for 80% ~ 90% lead-acid accumulator cream mud and concentrate of lead sulfide ore in mass ratio 3:1 be added in the hydrochloric acid soln prepared and leach; The technical qualification that scrap lead cream mud and concentrate of lead sulfide ore leach simultaneously are: liquid-solid ratio 4 ~ 8:1, temperature of reaction 50 DEG C ~ 80 DEG C, reaction times 60min ~ 120min, and leaching process pH value controls 2 ~ 3; Add magnesium chloride after reaction for some time, Chlorine in Solution magnesium density is 3mol/L ~ 5.5mol/L; After adding magnesium chloride, temperature is transferred to 80 DEG C ~ 95 DEG C, reaction times 60min ~ 120min;
(2) leaching terminates rear filtered while hot, and leached mud can extract elementary sulfur through flotation; Leach liquor crystallisation by cooling, obtains solid chlorine lead and contains MgSO
4, MgCl
2crystalline mother solution;
(3) crystalline mother solution leaches return scrap lead cream mud and concentrate of lead sulfide ore after magnesium chloride regeneration and purifying treatment while, and crystalline mother solution adds excessive calcium chloride makes leaching agent magnesium chloride regenerate, and output by-produced gypsum, removes SO simultaneously
4 2-after crystalline mother solution after purifying treatment, return scrap lead cream mud and concentrate of lead sulfide ore while leach operation.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105755290A (en) * | 2016-05-12 | 2016-07-13 | 南通职业大学 | Waste lead acid accumulator lead paste reduction method |
| CN105936979A (en) * | 2016-07-06 | 2016-09-14 | 广东新生环保科技股份有限公司 | Lead recovery agent for lead-containing wastes and application method thereof |
| CN106517318A (en) * | 2016-09-30 | 2017-03-22 | 华东师范大学 | Method for preparation of lead sulfide ultrafine powder from waste lead-acid battery lead paste |
| CN106676270A (en) * | 2017-01-05 | 2017-05-17 | 中南大学 | All-wet method for extracting lead from lead plaster and lead sulfide concentrate |
| CN107658519A (en) * | 2017-09-13 | 2018-02-02 | 华中科技大学 | A kind of method of recycling waste lead acid battery lead plaster |
| CN107674977A (en) * | 2017-10-11 | 2018-02-09 | 北京科技大学 | A kind of method of hydrometallurgic recovery lead in cream from waste lead acid battery lead |
| CN111172395A (en) * | 2019-10-23 | 2020-05-19 | 超威电源集团有限公司 | Method for preparing lead oxide from waste lead paste |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105755290A (en) * | 2016-05-12 | 2016-07-13 | 南通职业大学 | Waste lead acid accumulator lead paste reduction method |
| CN105936979A (en) * | 2016-07-06 | 2016-09-14 | 广东新生环保科技股份有限公司 | Lead recovery agent for lead-containing wastes and application method thereof |
| CN105936979B (en) * | 2016-07-06 | 2019-06-07 | 广东新生环保科技股份有限公司 | A kind of lead recovery catalyst and its application method for leaded waste |
| CN106517318A (en) * | 2016-09-30 | 2017-03-22 | 华东师范大学 | Method for preparation of lead sulfide ultrafine powder from waste lead-acid battery lead paste |
| CN106676270A (en) * | 2017-01-05 | 2017-05-17 | 中南大学 | All-wet method for extracting lead from lead plaster and lead sulfide concentrate |
| CN106676270B (en) * | 2017-01-05 | 2018-07-31 | 中南大学 | A method of Whote-wet method extracts lead from lead plaster and concentrate of lead sulfide ore |
| CN107658519A (en) * | 2017-09-13 | 2018-02-02 | 华中科技大学 | A kind of method of recycling waste lead acid battery lead plaster |
| CN107674977A (en) * | 2017-10-11 | 2018-02-09 | 北京科技大学 | A kind of method of hydrometallurgic recovery lead in cream from waste lead acid battery lead |
| CN111172395A (en) * | 2019-10-23 | 2020-05-19 | 超威电源集团有限公司 | Method for preparing lead oxide from waste lead paste |
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|---|---|
| CN105177297B (en) | 2017-08-01 |
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