CN103361485B - Technology for comprehensively recycling rare noble metals in waste LED (light-emitting diode) - Google Patents
Technology for comprehensively recycling rare noble metals in waste LED (light-emitting diode) Download PDFInfo
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- CN103361485B CN103361485B CN201210100653.8A CN201210100653A CN103361485B CN 103361485 B CN103361485 B CN 103361485B CN 201210100653 A CN201210100653 A CN 201210100653A CN 103361485 B CN103361485 B CN 103361485B
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Abstract
The application of the invention provides a technology for comprehensively recycling rare noble metals in a waste LED (light-emitting diode). The technology comprises the following steps of: carrying out coarse crushing, sorting and crush on a waste LED wafer, squashing the waste LED wafer into powder, adding the powder into a strong base solution, adding a certain amount of potassium peroxodisulfate as a catalyst,, continuously irradiating the powder through an ultraviolet lamp, and filtering and separating the powder, thereby obtaining a gallium containing filter liquor and a primary filter residue; depositing out gallium in the gallium-containing filter liquor, extracting metal gallium through an electrodeposition method, soaking the primary filter residue with chloroazotic acid, and filtering to obtain a gold-containing filter liquor and a secondary filter residue; extracting pure gold simple substances from the gold-containing filter liquor, uniformly mixing the secondary filter residue with industrial alkali so as to enter into a high temperature furnace, thereby obtaining an aluminum leach liquor after reaction; adding an alkali solution in the leach liquor, regulating the pH value, and filtering and separating to obtain aluminium hydroxide; and calcinating to obtain the pure aluminium oxide. The method is capable of comprehensively recycling rare noble metals and gold as well as metallic aluminium in the waste LED, and the method has the important economic values.
Description
Technical field
The present patent application relates to a kind of processing method extracting rare precious metal gallium and gold and metallic aluminium from waste and old LED, belongs to waste resource technical field of comprehensive utilization.
Background technology
LED is as the electricity-saving lamp of a new generation, because its volume is little, it is low to consume energy, high, the energy-conserving and environment-protective of long service life, brightness, robust characteristic obtain propagation and employment widely, its output also grows with each passing day, along with the development of science and technology and the raising of living standards of the people, the usage quantity about LED will increase further.The LED quantity of China's encapsulation in 2010 reaches 1,280 hundred million, wherein containing a large amount of metals resources, as rare precious metal gallium, gold etc., the LED that quantity is so huge, if if directly abandon after discarded, not only can take a large amount of land resources, contaminate environment, also can cause the waste of metals resources, therefore, the effectively waste and old LED of process, realizing the recycling of valuable valuable resource, is a significant problem.At present, also the rare Patents extracted about rare precious metal in LED is reported.
Summary of the invention
Namely the present patent application is reclaim field above shortcomings part for current waste and old LED, and provide a kind of method reclaiming rare precious metal from waste and old LED, the method has simple to operate, and extraction cost is low, the feature that the rate of recovery is high.
Specifically, in the waste and old LED of the comprehensive reutilization described in the present patent application, the technique of rare precious metal, comprises the following steps:
(1) coarse crushing and sorting: get waste and old LED wafer and clean and after drying, by shell fragmentation, LED wafer part sorted out;
(2) broken: to get the LED wafer in step (1), adopt ball-milling technology, LED wafer is milled to powder;
(3) separating gallium: the LED wafer powder in step (2) is joined in the strong base solution of 0.05 ~ 0.5 mol/L, and add a certain amount of Potassium Persulphate as catalyzer, the concentration of catalyzer in solution is made to be 0.05 ~ 0.5 mol/L, then by solution constant temperature 4 ~ 12 h under 30 ~ 95 DEG C of conditions, and use ultraviolet lamp Continuous irradiation, after reaction terminates, carry out filtering separation and wash three times, obtaining filtrate and filter residue;
(4) extract gallium: by step (3) containing Gallium solution, between salt acid for adjusting pH value to 5 ~ 8 through by concentration being 0.01 ~ 0.1 mol/L, gallium is precipitated out, and then gallium throw out being joined concentration is in the concentrated alkali solution of 10 ~ 25 mol/L, adopts electrodeposition method to extract gallium;
(5) Leaching of Gold: the filter residue chloroazotic acid in step (3) is soaked, solid-to-liquid ratio is 1:30 ~ 100, under 20 ~ 50 DEG C of conditions, soak 2 ~ 6 h, filters and obtains containing golden filtrate and filter residue;
(6) gold is extracted: by adding hydrochloric acid containing golden filtrate and being heated to 90 ~ 100 DEG C in step (5), drive nitrate radical out of, then in solution, the strong base solution that concentration is 0.01 ~ 0.1 mol/L is added, adjust ph is to 1.8 ~ 2.5, then in this solution, excessive ferrous sulfate, S-WAT or sodium bisulfite is added, and being warming up to 90 ~ 100 DEG C, namely reaction 1 ~ 2 h obtains pure golden simple substance.
Further, described method also comprises the step extracting aluminum oxide, as described below:
(1) aluminium is separated: mixed with the ratio of 1:3 ~ 10 with industrial alkali by the filter residue in step in aforesaid method (5), send in High Temperature Furnaces Heating Apparatus, after 400 ~ 600 DEG C of calcining at constant temperature 0.5 ~ 2 h, with deionized water dissolving, solid-to-liquid ratio is 1:20 ~ 100, then adds the sulfuric acid of 0.001 ~ 0.1 mol/L, and regulator solution pH value is to 1.0 ~ 3.0, filtering separation solid-liquid, namely obtains aluminium leach liquor;
(2) aluminum oxide is extracted: the strong base solution adding 0.01 ~ 0.1 mol/L in the aluminium leach liquor of step (1), adjust ph to 4.5 ~ 6, filtering separation obtains aluminium hydroxide, then at temperature lower calcination 0.5 ~ 4 h of 800 ~ 1200 DEG C, namely obtains pure aluminum oxide.
Further, the technique of rare precious metal in the waste and old LED of above-mentioned comprehensive reutilization, in step (2), is milled to 120 ~ 150 orders by LED wafer.
Further, the technique of rare precious metal in the waste and old LED of above-mentioned comprehensive reutilization, in step (3), the wavelength of ultra violet lamp is 254 ~ 367 nm.
Further, the technique of rare precious metal in the waste and old LED of above-mentioned comprehensive reutilization, in step (3), adopts Medium speed filter paper to carry out filtering separation.
Further, the technique of rare precious metal in the waste and old LED of above-mentioned comprehensive reutilization, in step (4), electrodeposition condition is, electrolyte temperature 30 ~ 60 DEG C, current density 100 ~ 500 A/m
2, electrodeposition time 1 ~ 5 h.
In the present patent application, if do not made specified otherwise, described solid-to-liquid ratio all refers to the mass ratio of solid and liquid.
The technique of rare precious metal in the waste and old LED of comprehensive reutilization described in the present patent application, comprehensive recycling can be carried out to the rare precious metal gallium in waste and old LED and gold and metallic aluminium, at the society of resource growing tension, there is great economic worth and social value.
Accompanying drawing explanation
Accompanying drawing is the process flow diagram of the technique of rare precious metal in the waste and old LED of comprehensive reutilization described in patent application.
Embodiment
Be described below in conjunction with concrete embodiment the method described in the present patent application and illustrate, illustrated embodiment is only for explaining the present invention, non-for limiting scope of the present invention.In fact; all improvement described method carried out with identical or approximate principle; comprise corresponding reagent used, the concentration of reagent, the change of reaction conditions, to realize for the purpose of basic same effect, then all within the present patent application technical scheme required for protection.
embodiment one extracts rare precious metal in waste and old LED---the method for gallium and gold
(1) coarse crushing and sorting: get waste and old LED wafer and clean and after drying, by shell fragmentation, LED wafer part sorted out;
(2) broken: to get the LED wafer in step (1), adopt ball-milling technology, LED chip ball is milled to 120 orders;
(3) separating gallium: the LED wafer powder in step (2) is joined in the KOH solution of 0.05 mol/L, and add a certain amount of potassium persulphate catalyst, the concentration of catalyzer in solution is made to be 0.1 mol/L, then by solution constant temperature 12 h under 40 DEG C of conditions, and be the ultraviolet lamp Continuous irradiation of 367 nm with wavelength, after reaction terminates, filtering separation, obtains filtrate and filter residue;
(4) extract gallium: by step (3) containing Gallium solution, through by concentration being the salt acid for adjusting pH value to 5 of 0.01 mol/L, gallium is precipitated out, then gallium throw out being joined concentration is in the NaOH solution of 10 mol/L, electrodeposition method is adopted to extract gallium, electrodeposition condition is, electrolyte temperature 35 DEG C, current density 500 A/m
2, electrodeposition time 0.5 h;
(5) Leaching of Gold: soaked by filter residue chloroazotic acid in step (3), solid-to-liquid ratio is 1:60, soaks 3 h under 40 DEG C of conditions, filters and obtains containing golden filtrate and filter residue;
(6) gold is extracted: add hydrochloric acid by step (5) containing golden filtrate and be heated to 90 DEG C, drive nitrate radical out of, then in solution, add appropriate sodium hydroxide, adjust ph, to 2.5, then adds excessive FeSO in this solution
4be warming up to 95 DEG C, react 1.5 h, namely obtain pure golden simple substance.
embodiment two, on the basis of embodiment one, extracts the method for aluminum oxide further
On the basis of embodiment one, extract aluminum oxide further, comprise following step:
(1) aluminium is separated: mixed with the ratio of 1:5 with NaOH by filter residue in step in aforesaid method (5), send in High Temperature Furnaces Heating Apparatus, by water dissolution after 550 DEG C of calcining at constant temperature 1 h, solid-to-liquid ratio is about 1:50, then the sulfuric acid of 0.005 mol/L is added, regulator solution pH value is to 2, and filtering separation solid-liquid, namely obtains aluminium leach liquor;
(2) extract aluminum oxide: the NaOH solution adding 0. 05 mol/L in above-mentioned aluminium leach liquor, adjust ph to 5, filtering separation obtains aluminium hydroxide, then namely obtains pure aluminum oxide at 900 DEG C of calcining 1 h.
embodiment three extracts rare precious metal in waste and old LED---the method for gallium and gold and aluminum oxide
(1) coarse crushing and sorting: get waste and old LED wafer and clean and after drying, by shell fragmentation, LED wafer part sorted out;
(2) broken: to get the LED wafer in step (1), adopt ball-milling technology, LED wafer is milled to 150 object powder;
(3) separating gallium: the LED wafer powder in step (2) is joined in the NaOH solution of 0.05 mol/L, and add a certain amount of Potassium Persulphate as catalyzer, the concentration of catalyzer in solution is made to be 0.05 mol/L, then by solution constant temperature 4 h under 95 DEG C of conditions, and be the ultraviolet lamp Continuous irradiation of 254 nm with wavelength, after reaction terminates, use Medium speed filter paper carry out filtering separation and wash three times, obtain filtrate and filter residue;
(4) extract gallium: by step (3) containing Gallium solution, through by concentration being the salt acid for adjusting pH value to 8 of 0.01 mol/L, gallium is precipitated out, then gallium throw out being joined concentration is in the KOH solution of 25 mol/L, electrodeposition method is adopted to extract gallium, electrodeposition condition is, electrolyte temperature 60 DEG C, current density 100 A/m
2, electrodeposition time 5 h;
(5) Leaching of Gold: the filter residue chloroazotic acid in step (3) is soaked, solid-to-liquid ratio is 1:30, soaks 6 h under 20 DEG C of conditions, filters and obtains containing golden filtrate and filter residue;
(6) gold is extracted: by adding hydrochloric acid containing golden filtrate and being heated to 95 DEG C in step (5), drive nitrate radical out of, then in solution, the strong base solution that concentration is 0.01 mol/L is added, adjust ph is to 1.8, then in this solution, excessive S-WAT is added, and be warming up to 90 DEG C, react 1 h and namely obtain pure golden simple substance;
(7) aluminium is separated: mixed with the ratio of 1:3 with industrial alkali by filter residue in step (5), send in High Temperature Furnaces Heating Apparatus, with deionized water dissolving after 400 DEG C of calcining at constant temperature 2 h, solid-to-liquid ratio is 1:20, then the sulfuric acid of 0.1 mol/L is added, regulator solution pH value is to 3.0, and filtering separation solid-liquid, namely obtains aluminium leach liquor;
(8) aluminum oxide is extracted: the strong base solution adding 0.01 mol/L in the aluminium leach liquor of step (7), adjust ph to 4.5, filtering separation obtains aluminium hydroxide, then at temperature lower calcination 0.5 h of 800 DEG C, namely obtains pure aluminum oxide.
embodiment four extracts rare precious metal in waste and old LED---the method for gallium and gold and aluminum oxide
Specifically, in the waste and old LED of the comprehensive reutilization described in the present patent application, the technique of rare precious metal, comprises the following steps:
(1) coarse crushing and sorting: get waste and old LED wafer and clean and after drying, by shell fragmentation, LED wafer part sorted out;
(2) broken: to get the LED wafer in step (1), adopt ball-milling technology, LED wafer is milled to 130 object powder;
(3) separating gallium: the LED wafer powder in step (2) is joined in the KOH solution of 0.5 mol/L, and add a certain amount of Potassium Persulphate as catalyzer, the concentration of catalyzer in solution is made to be 0.5 mol/L, then by solution constant temperature 12 h under 30 DEG C of conditions, and use ultraviolet lamp Continuous irradiation, after reaction terminates, carry out filtering separation and wash three times, obtaining filtrate and filter residue;
(4) extract gallium: by step (3) containing Gallium solution, through by concentration being the salt acid for adjusting pH value to 6 of 0.1 mol/L, gallium is precipitated out, then gallium throw out being joined concentration is in the concentrated alkali solution of 10 mol/L, electrodeposition method is adopted to extract gallium, electrodeposition condition is, electrolyte temperature 45 DEG C, current density 300 A/m
2, electrodeposition time 3 h;
(5) Leaching of Gold: the filter residue chloroazotic acid in step (3) is soaked, solid-to-liquid ratio is 1:100, soaks 2 h under 50 DEG C of conditions, filters and obtains containing golden filtrate and filter residue;
(6) gold is extracted: by adding hydrochloric acid containing golden filtrate and being heated to 100 DEG C in step (5), drive nitrate radical out of, then in solution, the strong base solution that concentration is 0.1 mol/L is added, adjust ph is to 2.5, then in this solution, excessive sodium bisulfite is added, and be warming up to 100 DEG C, react 1 h and namely obtain pure golden simple substance;
(7) aluminium is separated: mixed with the ratio of 1:10 with industrial alkali by filter residue in step (5), send in High Temperature Furnaces Heating Apparatus, with deionized water dissolving after 600 DEG C of calcining at constant temperature 0.5 h, solid-to-liquid ratio is 1:100, then the sulfuric acid of 0.001 mol/L is added, regulator solution pH value is to 1.0, and filtering separation solid-liquid, namely obtains aluminium leach liquor;
(8) aluminum oxide is extracted: the strong base solution adding 0.1 mol/L in the aluminium leach liquor of step (7), adjust ph to 6, filtering separation obtains aluminium hydroxide, then at temperature lower calcination 4 h of 1200 DEG C, namely obtains pure aluminum oxide.
Claims (6)
1. the technique of rare precious metal in the waste and old LED of comprehensive reutilization, is characterized in that: comprise the following steps:
(1) coarse crushing and sorting: get waste and old LED wafer and clean and after drying, by shell fragmentation, LED wafer part sorted out;
(2) broken: to get the LED wafer in step (1), adopt ball-milling technology, LED wafer is milled to powder;
(3) separating gallium: the LED wafer powder in step (2) is joined in the strong base solution of 0.05 ~ 0.5 mol/L, and add a certain amount of Potassium Persulphate as catalyzer, the concentration of catalyzer in solution is made to be 0.05 ~ 0.5 mol/L, then by solution constant temperature 4 ~ 12 h under 30 ~ 95 DEG C of conditions, and use ultraviolet lamp Continuous irradiation, after reaction terminates, carry out filtering separation and wash three times, obtaining filtrate and filter residue;
(4) extract gallium: by step (3) containing gallium filtrate, between salt acid for adjusting pH value to 5 ~ 8 through by concentration being 0.01 ~ 0.1 mol/L, gallium is precipitated out, and then gallium throw out being joined concentration is in the concentrated alkali solution of 10 ~ 25 mol/L, adopts electrodeposition method to extract gallium;
(5) Leaching of Gold: the filter residue chloroazotic acid in step (3) is soaked, solid-to-liquid ratio is 1:30 ~ 100, under 20 ~ 50 DEG C of conditions, soak 2 ~ 6 h, filters and obtains containing golden filtrate and filter residue;
(6) gold is extracted: by adding hydrochloric acid containing golden filtrate and being heated to 90 ~ 100 DEG C in step (5), drive nitrate radical out of, then in solution, the strong base solution that concentration is 0.01 ~ 0.1 mol/L is added, adjust ph is to 1.8 ~ 2.5, then in this solution, excessive ferrous sulfate, S-WAT or sodium bisulfite is added, and being warming up to 90 ~ 100 DEG C, namely reaction 1 ~ 2 h obtains pure golden simple substance.
2. technique according to claim 1, is characterized in that, described technique also comprises the step extracting aluminum oxide,
(1) aluminium is separated: mixed with the ratio of 1:3 ~ 10 with industrial alkali by the filter residue in claim 1 step (5), send in High Temperature Furnaces Heating Apparatus, with deionized water dissolving after 400 ~ 600 DEG C of calcining at constant temperature 0.5 ~ 2 h, solid-to-liquid ratio is 1:20 ~ 100, then the sulfuric acid of 0.001 ~ 0.1 mol/L is added, regulator solution pH value is to 1.0 ~ 3.0, and filtering separation solid-liquid, namely obtains aluminium leach liquor;
(2) aluminum oxide is extracted: the strong base solution adding 0.01 ~ 0.1 mol/L in the aluminium leach liquor of step (1), adjust ph to 4.5 ~ 6, filtering separation obtains aluminium hydroxide, then at temperature lower calcination 0.5 ~ 4 h of 800 ~ 1200 DEG C, namely obtains pure aluminum oxide.
3. technique according to claim 1, is characterized in that: in step (2), LED wafer is milled to 120 ~ 150 orders.
4. technique according to claim 1, is characterized in that: in step (3), and the wavelength of ultra violet lamp is 254 ~ 367 nm.
5. technique according to claim 1, is characterized in that: in step (3), adopts Medium speed filter paper to carry out filtering separation.
6. technique according to claim 1, is characterized in that: in step (4), and electrodeposition condition is, electrolyte temperature 30 ~ 60 DEG C, current density 100 ~ 500 A/ ㎡, electrodeposition time 1 ~ 5 h.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103740940A (en) * | 2013-12-14 | 2014-04-23 | 中国铝业股份有限公司 | Processing method for lime slag generated during purifying process of gallium pregnant solution |
| CN104726894B (en) * | 2015-03-30 | 2018-07-27 | 北京化工大学 | The method for recycling gallium |
| CN106381390B (en) * | 2016-09-14 | 2018-07-20 | 南昌大学 | A kind of waste and old LED illumination light bulb recovery method |
| CN109112546B (en) * | 2018-07-27 | 2021-04-20 | 佛山市三水雄鹰铝表面技术创新中心有限公司 | Oxidation line system and process for recovering aluminum hydroxide and sodium sulfate from mold-stewing liquid |
| CN109112537B (en) * | 2018-07-27 | 2021-08-03 | 佛山市三水雄鹰铝表面技术创新中心有限公司 | Device and process for recovering aluminum hydroxide and sodium sulfate from oxidation liquid and deoiling neutralization liquid |
| CN109055782B (en) * | 2018-08-24 | 2020-12-22 | 华南理工大学 | Leaching method of gallium in waste light-emitting diode |
| DE102018222185A1 (en) * | 2018-12-18 | 2020-06-18 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Method and device for recycling LED components from old lamp mixtures and use of the device |
| CN109468471A (en) * | 2018-12-28 | 2019-03-15 | 山东金艺珠宝有限公司 | Purifying technique is concentrated for precious metal solution in one kind |
| CN112264037B (en) * | 2020-10-21 | 2023-04-07 | 优赛环保工程(天津)有限公司 | Method for preparing ozonolysis catalyst by using waste LED lamp beads, ozonolysis catalyst prepared by method and application of ozonolysis catalyst |
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| CN101857918A (en) * | 2009-04-07 | 2010-10-13 | 国立云林科技大学 | Method for purifying and recycling gallium and arsenic in waste gallium arsenide |
| CN102251098A (en) * | 2011-07-04 | 2011-11-23 | 沈少波 | Method for extracting rare noble metals |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101857918A (en) * | 2009-04-07 | 2010-10-13 | 国立云林科技大学 | Method for purifying and recycling gallium and arsenic in waste gallium arsenide |
| CN102251098A (en) * | 2011-07-04 | 2011-11-23 | 沈少波 | Method for extracting rare noble metals |
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