CN104131312A - Method utilizing eutectic solvent to carry out in-situ reduction on lead oxide to produce lead - Google Patents
Method utilizing eutectic solvent to carry out in-situ reduction on lead oxide to produce lead Download PDFInfo
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- CN104131312A CN104131312A CN201410321997.0A CN201410321997A CN104131312A CN 104131312 A CN104131312 A CN 104131312A CN 201410321997 A CN201410321997 A CN 201410321997A CN 104131312 A CN104131312 A CN 104131312A
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- eutectic solvent
- plumbous
- plumbous oxide
- lead
- lead oxide
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- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 239000002904 solvent Substances 0.000 title claims abstract description 36
- 230000005496 eutectics Effects 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 18
- 229910000464 lead oxide Inorganic materials 0.000 title abstract 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 13
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 13
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 9
- 239000003792 electrolyte Substances 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012153 distilled water Substances 0.000 claims abstract description 7
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 7
- 239000010439 graphite Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 4
- YADSGOSSYOOKMP-UHFFFAOYSA-N dioxolead Chemical compound O=[Pb]=O YADSGOSSYOOKMP-UHFFFAOYSA-N 0.000 claims description 24
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000008151 electrolyte solution Substances 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 6
- 238000011010 flushing procedure Methods 0.000 claims description 6
- NHGXDBSUJJNIRV-UHFFFAOYSA-M tetrabutylammonium chloride Chemical compound [Cl-].CCCC[N+](CCCC)(CCCC)CCCC NHGXDBSUJJNIRV-UHFFFAOYSA-M 0.000 claims description 6
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 claims description 4
- 235000019743 Choline chloride Nutrition 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims description 4
- 229960003178 choline chloride Drugs 0.000 claims description 4
- MEIRRNXMZYDVDW-MQQKCMAXSA-N (2E,4E)-2,4-hexadien-1-ol Chemical compound C\C=C\C=C\CO MEIRRNXMZYDVDW-MQQKCMAXSA-N 0.000 claims description 3
- OKIZCWYLBDKLSU-UHFFFAOYSA-M N,N,N-Trimethylmethanaminium chloride Chemical compound [Cl-].C[N+](C)(C)C OKIZCWYLBDKLSU-UHFFFAOYSA-M 0.000 claims description 3
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims description 3
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims description 3
- 239000000811 xylitol Substances 0.000 claims description 3
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims description 3
- 229960002675 xylitol Drugs 0.000 claims description 3
- 235000010447 xylitol Nutrition 0.000 claims description 3
- 239000002184 metal Substances 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000012300 argon atmosphere Substances 0.000 abstract 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 abstract 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 abstract 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract 1
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 239000001099 ammonium carbonate Substances 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000005272 metallurgy Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 229920005862 polyol Polymers 0.000 abstract 1
- 150000003077 polyols Chemical class 0.000 abstract 1
- 239000011148 porous material Substances 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000897 Babbitt (metal) Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000000374 eutectic mixture Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011244 liquid electrolyte Substances 0.000 description 1
- 238000009856 non-ferrous metallurgy Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention relates to a method utilizing a eutectic solvent to carry out in-situ reduction on lead oxide to produce lead, and belongs to the technical field of non-ferrous metal metallurgy. The method comprises the following steps: taking lead oxide as the raw material, ammonium bicarbonate as the pore forming agent, and polyvinyl alcohol as the adhesive, evenly mixing three materials together, pressing the mixture into a lead oxide block, burning the lead oxide at an argon atmosphere so as to produce a lead oxide electrode; evenly mixing quaternary ammonium salts and polyol at an argon atmosphere to form a eutectic solvent electrolyte, carrying out electrolysis in the eutectic solvent electrolyte prepared in the previous step by taking graphite as the positive electrode and the lead oxide electrode as the negative electrode, washing the reduced negative electrode by acetone and distilled water, and finally drying so as to obtain high-purity metal lead. The technology is simple, the requirement on the equipment material is low, the energy consumption is low, and the method is economic and environment-friendly.
Description
Technical field
The present invention relates to a kind of eutectic solvent in-situ reducing plumbous oxide and produce plumbous method, belong to non-ferrous metallurgy technology field.
Background technology
Metallic lead is a kind of important industrial chemicals, because it has lower fusing point, good ductility and erosion resistance, can be used as the starting material of manufacturing store battery, gasoline dope and cable, the liner of chemical industry equipment and metallurgical works electrolyzer, also be the main raw of radioactive ray protective shield in nuclear industry and medical science, also can be used for the fields such as pantograph device of bearing metal, scolder, sintered wear-resistant part and electric car simultaneously.In recent years, rapidly, refining splicer skill is also along with the development of industry presents diversified trend in the plumbous smelting industry development of China.At present, plumbous production method is mainly pyrogenic process, generally adopts traditional baking with agglomeration-retailoring of blast furnace flow process, and this technique accounts for 85% left and right of International Lead output, has the features such as technical maturity, stable operation.But still there are some problems in this method, as the SO after sintering
2flue gas concentration is on the low side, is difficult to reach the requirement of conventional relieving haperacidity, and sintering process long flow path, and equipment is many, and returning charge amount is large, is difficult to realize cleaner production.Therefore, be necessary to study that a kind of technique is simple, energy-conservation, cost is low and environment amenable novel method, metallic lead can be applied in more field.
The eutectic mixture that eutectic solvent is normally combined by quaternary ammonium salt and the hydrogen-bond donor (as compounds such as acid amides, carboxylic acid and polyvalent alcohols) of certain stoichiometric ratio.Eutectic solvent has that electrochemical window is wide, good conductivity, steam forces down and the good advantages such as physical and chemical stability, is a kind of novel green solvent.Aspect in-situ metal electrolytic reduction, eutectic solvent is a kind of desirable room temperature liquid electrolyte, it has merged the advantage of high-temperature molten salt and the aqueous solution: have wider electrochemical window, at room temperature can obtain ability electrolysis obtains in high-temperature molten salt metal and alloy, and there is no the such severe corrosive of high-temperature molten salt.The above-mentioned characteristic of eutectic solvent and easy preparation process thereof and cheap cost of material make it to become the brand-new liquid medium in metal and alloy electrolysis research thereof.Therefore, the preparation by eutectic solvent for metallic lead, can solve the problems that conventional production methods exists technically, realizes the greenization of producing, and is the very wide electrochemistry metallurgical of a kind of application prospect.
Summary of the invention
It is long that the present invention is intended to solve the Production Flow Chart existing in existing metallic lead production method, use equipment is many, returning charge amount is large, be difficult to realize the problems such as cleaner production, provide a kind of eutectic solvent in-situ reducing plumbous oxide that adopts environmental protection to produce the method for metallic lead, the present invention is achieved through the following technical solutions.
Eutectic solvent in-situ reducing plumbous oxide is produced a plumbous method, and its concrete steps are as follows:
(1) take plumbous oxide as raw material, bicarbonate of ammonia is pore-forming material, and polyvinyl alcohol is binding agent, and above-mentioned three kinds of mixing of materials are pressed into block plumbous oxide after evenly, is incubated 1 ~ 4h and makes lead dioxide electrode in argon gas atmosphere at 600 ~ 1000 ℃;
(2) under ar gas environment, by quaternary ammonium salt and polyvalent alcohol according to mol ratio (1 ~ 3): (2 ~ 5) are uniformly mixed to form eutectic solvent electrolytic solution;
(3) take graphite as anode, the lead dioxide electrode that step (1) prepares is negative electrode, controlling electrolyte temperature, be that 40 ~ 100 ℃, bath voltage are under 1.8 ~ 2.5V, the anode and cathode pole span condition that is 0.5 ~ 2cm, electrolysis 3 ~ 10h in the eutectic solvent electrolytic solution preparing in step (2), then take out negative electrode through acetone, distilled water flushing, after being dried, obtain metallic lead.
The add-on of the bicarbonate of ammonia in described step (1) is 5 ~ 30% of plumbous oxide quality.
The add-on of the polyvinyl alcohol in described step (1) is 1 ~ 2% of plumbous oxide quality.
The quality of the block plumbous oxide in described step (1) is 0.5 ~ 5g.
Quaternary ammonium salt in described step (2) is choline chloride 60, tetramethyl ammonium chloride or tetrabutylammonium chloride.
Polyvalent alcohol in described step (2) is ethylene glycol, glycerol, Xylitol or sorbyl alcohol.
The invention has the beneficial effects as follows: adopting the method can be directly highly purified metallic lead by plumbous oxide in-situ reducing, and technique is simple, low to the material requirement of equipment, energy consumption is less, economic environmental protection.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
This eutectic solvent in-situ reducing plumbous oxide is produced the method for metallic lead, and its concrete steps are as follows:
(1) take plumbous oxide as raw material, bicarbonate of ammonia is pore-forming material, polyvinyl alcohol is binding agent, plumbous oxide, the polyvinyl alcohol that accounts for the bicarbonate of ammonia of plumbous oxide quality 5% and account for plumbous oxide quality 1% are mixed evenly, be pressed into quality and be and in argon gas atmosphere, at 600 ℃, be incubated 1h after the block plumbous oxide of 0.5g and be fired into lead dioxide electrode;
(2), under ar gas environment, by choline chloride 60 and ethylene glycol, according to mol ratio, be that 1:2 is uniformly mixed to form eutectic solvent electrolytic solution;
(3) take graphite as anode, the lead dioxide electrode that step (1) prepares is negative electrode, controlling electrolyte temperature, be that 40 ℃, bath voltage are under 1.8V, the anode and cathode pole span condition that is 0.5cm, electrolysis 3h in the eutectic solvent electrolytic solution preparing in step (2), then take out negative electrode through acetone, distilled water flushing, after being dried, obtain metallic lead.Adopting Shimadzu XRF-1800 type Xray fluorescence spectrometer to detect product lead content is 99.99wt%.
Embodiment 2
This eutectic solvent in-situ reducing plumbous oxide is produced the method for metallic lead, and its concrete steps are as follows:
(1) take plumbous oxide as raw material, bicarbonate of ammonia is pore-forming material, polyvinyl alcohol is binding agent, plumbous oxide, the polyvinyl alcohol that accounts for the bicarbonate of ammonia of plumbous oxide quality 30% and account for plumbous oxide quality 2% are mixed evenly, be pressed into quality and be and in argon gas atmosphere, at 1000 ℃, be incubated 4h after the block plumbous oxide of 5g and be fired into lead dioxide electrode;
(2), under ar gas environment, by tetramethyl ammonium chloride and glycerol, according to mol ratio, be that 3:5 is uniformly mixed to form eutectic solvent electrolytic solution;
(3) take graphite as anode, the lead dioxide electrode that step (1) prepares is negative electrode, controlling electrolyte temperature, be that 100 ℃, bath voltage are under 2.5V, the anode and cathode pole span condition that is 2cm, electrolysis 10h in the eutectic solvent electrolytic solution preparing in step (2), then take out negative electrode through acetone, distilled water flushing, after being dried, obtain metallic lead.Adopting Shimadzu XRF-1800 type Xray fluorescence spectrometer to detect product lead content is 99.99wt%.
Embodiment 3
This eutectic solvent in-situ reducing plumbous oxide is produced the method for metallic lead, and its concrete steps are as follows:
(1) take plumbous oxide as raw material, bicarbonate of ammonia is pore-forming material, polyvinyl alcohol is binding agent, plumbous oxide, the polyvinyl alcohol that accounts for the bicarbonate of ammonia of plumbous oxide quality 15% and account for plumbous oxide quality 1.5% are mixed evenly, be pressed into quality and be and in argon gas atmosphere, at 800 ℃, be incubated 2h after the block plumbous oxide of 3g and be fired into lead dioxide electrode;
(2), under ar gas environment, by tetrabutylammonium chloride and Xylitol, according to mol ratio, be that 2:3 is uniformly mixed to form eutectic solvent electrolytic solution;
(3) take graphite as anode, the lead dioxide electrode that step (1) prepares is negative electrode, controlling electrolyte temperature, be that 60 ℃, bath voltage are under 2.3V, the anode and cathode pole span condition that is 1cm, electrolysis 6h in the eutectic solvent electrolytic solution preparing in step (2), then take out negative electrode through acetone, distilled water flushing, after being dried, obtain metallic lead.Adopting Shimadzu XRF-1800 type Xray fluorescence spectrometer to detect product lead content is 99.99wt%.
Embodiment 4
This eutectic solvent in-situ reducing plumbous oxide is produced the method for metallic lead, and its concrete steps are as follows:
(1) take plumbous oxide as raw material, bicarbonate of ammonia is pore-forming material, polyvinyl alcohol is binding agent, plumbous oxide, the polyvinyl alcohol that accounts for the bicarbonate of ammonia of plumbous oxide quality 10% and account for plumbous oxide quality 1% are mixed evenly, be pressed into quality and be and in argon gas atmosphere, at 850 ℃, be incubated 3h after the block plumbous oxide of 1g and be fired into lead dioxide electrode;
(2), under ar gas environment, by choline chloride 60 and sorbyl alcohol, according to mol ratio, be that 1:2 is uniformly mixed to form eutectic solvent electrolytic solution;
(3) take graphite as anode, the lead dioxide electrode that step (1) prepares is negative electrode, controlling electrolyte temperature, be that 80 ℃, bath voltage are under 2.0V, the anode and cathode pole span condition that is 1cm, electrolysis 7h in the eutectic solvent electrolytic solution preparing in step (2), then take out negative electrode through acetone, distilled water flushing, after being dried, obtain metallic lead.Adopting Shimadzu XRF-1800 type Xray fluorescence spectrometer to detect product lead content is 99.99wt%.
Claims (6)
1. eutectic solvent in-situ reducing plumbous oxide is produced a plumbous method, it is characterized in that concrete steps are as follows:
(1) take plumbous oxide as raw material, bicarbonate of ammonia is pore-forming material, and polyvinyl alcohol is binding agent, and above-mentioned three kinds of mixing of materials are pressed into block plumbous oxide after evenly, is incubated 1 ~ 4h and makes lead dioxide electrode in argon gas atmosphere at 600 ~ 1000 ℃;
(2) under ar gas environment, by quaternary ammonium salt and polyvalent alcohol according to mol ratio (1 ~ 3): (2 ~ 5) are uniformly mixed to form eutectic solvent electrolytic solution;
(3) take graphite as anode, the lead dioxide electrode that step (1) prepares is negative electrode, controlling electrolyte temperature, be that 40 ~ 100 ℃, bath voltage are under 1.8 ~ 2.5V, the anode and cathode pole span condition that is 0.5 ~ 2cm, electrolysis 3 ~ 10h in the eutectic solvent electrolytic solution preparing in step (2), then take out negative electrode through acetone, distilled water flushing, after being dried, obtain metallic lead.
2. eutectic solvent in-situ reducing plumbous oxide according to claim 1 is produced plumbous method, it is characterized in that: the add-on of the bicarbonate of ammonia in described step (1) is 5 ~ 30% of plumbous oxide quality.
3. eutectic solvent in-situ reducing plumbous oxide according to claim 1 is produced plumbous method, it is characterized in that: the add-on of the polyvinyl alcohol in described step (1) is 1 ~ 2% of plumbous oxide quality.
4. eutectic solvent in-situ reducing plumbous oxide according to claim 1 is produced plumbous method, it is characterized in that: the quality of the block plumbous oxide in described step (1) is 0.5 ~ 5g.
5. eutectic solvent in-situ reducing plumbous oxide according to claim 1 is produced plumbous method, it is characterized in that: the quaternary ammonium salt in described step (2) is choline chloride 60, tetramethyl ammonium chloride or tetrabutylammonium chloride.
6. eutectic solvent in-situ reducing plumbous oxide according to claim 1 is produced plumbous method, it is characterized in that: the polyvalent alcohol in described step (2) is ethylene glycol, glycerol, Xylitol or sorbyl alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410321997.0A CN104131312A (en) | 2014-07-08 | 2014-07-08 | Method utilizing eutectic solvent to carry out in-situ reduction on lead oxide to produce lead |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410321997.0A CN104131312A (en) | 2014-07-08 | 2014-07-08 | Method utilizing eutectic solvent to carry out in-situ reduction on lead oxide to produce lead |
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Cited By (4)
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| CN104499002A (en) * | 2014-12-10 | 2015-04-08 | 上海大学 | Method for preparing copper-iron nano plated layer from low-grade sulfide ore through direct electro-deposition |
| CN105908219A (en) * | 2016-04-27 | 2016-08-31 | 昆明理工大学 | Method for extracting metallic lead by electrolytically reducing galena with ionic liquid |
| WO2016198872A1 (en) * | 2015-06-12 | 2016-12-15 | Imperial Innovations Limited | Electrochemical recycling of lead-based materials |
| US11427478B2 (en) | 2018-08-03 | 2022-08-30 | Imperial College Innovations Limited | Recycling of lead- and tin-based materials |
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| US11427478B2 (en) | 2018-08-03 | 2022-08-30 | Imperial College Innovations Limited | Recycling of lead- and tin-based materials |
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