CN103361485A - 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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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 of extracting rare precious metal gallium and gold and metallic aluminium from waste and old LED, belongs to waste resource comprehensive utilization technique field.
Background technology
LED is as the electricity-saving lamp of a new generation,, power consumption low, long service life little because of its volume, brightness height, energy-conserving and environment-protective, robust characteristic have obtained widely propagation and employment, 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, will further increase about the usage quantity of LED lamp.The LED quantity of China's encapsulation in 2010 reaches 1,280 hundred million, wherein contain a large amount of metals resources, such as rare precious metal gallium, gold etc., quantity is huge LED so, if if directly abandon after discarded, not only can take a large amount of land resourcess, contaminate environment, also can cause the waste of metals resources, therefore, effectively process waste and old LED lamp, realizing the recycling of valuable valuable resource, is a significant problem.At present, also the rare Patents that extracts about rare precious metal among the LED is reported.
Summary of the invention
The present patent application namely is to reclaim field above shortcomings part for present waste and old LED, and a kind of method that reclaims rare precious metal from waste and old LED is provided, and the method has simple to operate, and extraction cost is low, the characteristics that the rate of recovery is high.
Specifically, the technique of rare precious metal comprises the steps: among the waste and old LED of the described comprehensive reutilization of the present patent application
(1) coarse crushing and sorting: after getting waste and old LED wafer cleaning and drying that shell is broken, the LED wafer is partly sorted out;
(2) fragmentation: get the LED wafer in the step (1), adopt ball-milling technology, the LED wafer is milled to powder;
(3) separating gallium: the LED wafer powder in the 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 that makes catalyzer in the solution is 0.05 ~ 0.5 mol/L, then with solution constant temperature 4 ~ 12 h under 30 ~ 95 ℃ of conditions, and use the ultraviolet lamp Continuous irradiation, after reaction finishes, carry out filtering separation and wash three times, obtain filtrate and filter residue;
(4) extract gallium: with the Gallium solution that contains in the step (3), between the salt acid for adjusting pH value to 5 ~ 8 through with concentration being 0.01 ~ 0.1 mol/L, gallium is precipitated out, then the gallium throw out is joined in the concentrated alkali solution that concentration is 10 ~ 25 mol/L, adopt electrodeposition method to extract gallium;
(5) Leaching of Gold: the filter residue in the step (3) is soaked with chloroazotic acid, and solid-to-liquid ratio is 1:30 ~ 100, soaks 2 ~ 6 h under 20 ~ 50 ℃ of conditions, filters to obtain containing golden filtrate and filter residue;
(6) extract gold: the golden filtrate that contains in the step (5) is added hydrochloric acid and is heated to 90 ~ 100 ℃, drive nitrate radical out of, then adding concentration in the solution is the strong base solution of 0.01 ~ 0.1 mol/L, regulate pH value to 1.8 ~ 2.5, then in this solution, add excessive ferrous sulfate, S-WAT or sodium bisulfite, and being warming up to 90 ~ 100 ℃, reaction 1 ~ 2 h namely obtains pure golden simple substance.
Further, described method also comprises the step of extracting aluminum oxide, and is as described below:
(1) separates aluminium: the filter residue in the step in the aforesaid method (5) and the industrial alkali ratio with 1:3 ~ 10 is mixed, send in the High Temperature Furnaces Heating Apparatus, behind 400 ~ 600 ℃ of calcining at constant temperature 0.5 ~ 2 h, use deionized water dissolving, solid-to-liquid ratio is 1:20 ~ 100, then adds the sulfuric acid of 0.001 ~ 0.1 mol/L, regulator solution pH value to 1.0 ~ 3.0, the filtering separation solid-liquid namely obtains the aluminium leach liquor;
(2) extract aluminum oxide: the strong base solution that adds 0.01 ~ 0.1 mol/L in the aluminium leach liquor of step (1), regulate pH value to 4.5～6, filtering separation obtains aluminium hydroxide, then at 800 ~ 1200 ℃ temperature lower calcination 0.5～4 h, namely obtains pure aluminum oxide.
Further, the technique of rare precious metal in the waste and old LED of above-mentioned comprehensive reutilization in the step (2), is milled to 120 ~ 150 orders with the LED chip ball.
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), the electrodeposition condition is 30 ~ 60 ℃ of electrolyte temperatures, current density 100 ~ 500 A/m
2, electrodeposition time 1 ~ 5 h.
In the present patent application, as not making specified otherwise, described solid-to-liquid ratio all refers to the mass ratio of solid and liquid.
The technique of rare precious metal among the waste and old LED of the described comprehensive reutilization of the present patent application, can carry out comprehensive recycling to the rare precious metal gallium among the waste and old LED and gold and metallic aluminium, at the society of resource growing tension, have great economic worth and social value.
Description of drawings
Accompanying drawing is the process flow diagram of the technique of rare precious metal among the waste and old LED of the described comprehensive reutilization of patent application.
Embodiment
Below in conjunction with concrete embodiment the described method of the present patent application is described and illustrates that illustrated embodiment only is used for explaining the present invention, and is non-be used to limiting scope of the present invention.In fact; all improvement of described method being carried out with identical or approximate principle; comprise the concentration of used corresponding reagent, reagent, the change of reaction conditions, to realize basic identical effect as purpose, then all within the present patent application technical scheme required for protection.
Embodiment one extracts rare precious metal among the waste and old LED---the method for gallium and gold
(1) coarse crushing and sorting: after getting waste and old LED wafer cleaning and drying that shell is broken, the LED wafer is partly sorted out;
(2) fragmentation: get the LED wafer in the step (1), adopt ball-milling technology, the LED chip ball is milled to 120 orders;
(3) separating gallium: the LED wafer powder in the step (2) is joined in the KOH solution of 0.05 mol/L, and add a certain amount of Potassium Persulphate catalyzer, the concentration that makes catalyzer in the solution is 0.1 mol/L, then with solution constant temperature 12 h under 40 ℃ of conditions, and be the ultraviolet lamp Continuous irradiation of 367 nm with wavelength, after reaction finished, filtering separation obtained filtrate and filter residue;
(4) extract gallium: with the Gallium solution that contains in the step (3), through being the salt acid for adjusting pH value to 5 of 0.01 mol/L with concentration, gallium is precipitated out, then the gallium throw out is joined in the NaOH solution that concentration is 10 mol/L, adopt electrodeposition method to extract gallium, the electrodeposition condition is 35 ℃ of electrolyte temperatures, current density 500 A/m
2, electrodeposition time 0.5 h;
(5) Leaching of Gold: filter residue in the step (3) is soaked with chloroazotic acid, and solid-to-liquid ratio is 1:60, soaks 3 h under 40 ℃ of conditions, filters and obtains containing golden filtrate and filter residue;
(6) extract gold: add hydrochloric acid and be heated to 90 ℃ containing golden filtrate in the step (5), drive nitrate radical out of, then in solution, add an amount of sodium hydroxide, regulate pH value to 2.5, then in this solution, add excessive FeSO
4Be warming up to 95 ℃, react 1.5 h, namely obtain pure golden simple substance.
Embodiment two further extracts the method for aluminum oxide on the basis of embodiment one
On the basis of embodiment one, further extract aluminum oxide, comprise following step:
(1) separates aluminium: filter residue in the step in the aforesaid method (5) and NaOH are mixed with the ratio of 1:5, send in the High Temperature Furnaces Heating Apparatus, behind 550 ℃ of calcining at constant temperature 1 h, use water dissolution, solid-to-liquid ratio is about 1:50, then the sulfuric acid that adds 0.005 mol/L, regulator solution pH value to 2, the filtering separation solid-liquid namely obtains the aluminium leach liquor;
(2) extract aluminum oxide: add the NaOH solution of 0. 05 mol/L in the above-mentioned aluminium leach liquor, regulate pH value to 5, filtering separation obtains aluminium hydroxide, then calcines 1 h at 900 ℃ and namely obtains pure aluminum oxide.
Embodiment three extracts rare precious metal---the method for gallium and gold and aluminum oxide among the waste and old LED
(1) coarse crushing and sorting: after getting waste and old LED wafer cleaning and drying that shell is broken, the LED wafer is partly sorted out;
(2) fragmentation: get the LED wafer in the step (1), adopt ball-milling technology, the LED wafer is milled to 150 purpose powder;
(3) separating gallium: the LED wafer powder in the 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 that makes catalyzer in the solution is 0.05 mol/L, then with solution constant temperature 4 h under 95 ℃ of conditions, and be the ultraviolet lamp Continuous irradiation of 254 nm with wavelength, after reaction finished, the use Medium speed filter paper carried out filtering separation and washes three times, obtains filtrate and filter residue;
(4) extract gallium: with the Gallium solution that contains in the step (3), through being the salt acid for adjusting pH value to 8 of 0.01 mol/L with concentration, gallium is precipitated out, then the gallium throw out is joined in the KOH solution that concentration is 25 mol/L, adopt electrodeposition method to extract gallium, the electrodeposition condition is 60 ℃ of electrolyte temperatures, current density 100 A/m
2, electrodeposition times 5 h;
(5) Leaching of Gold: the filter residue in the step (3) is soaked with chloroazotic acid, and solid-to-liquid ratio is 1:30, soaks 6 h under 20 ℃ of conditions, filters and obtains containing golden filtrate and filter residue;
(6) extract gold: the golden filtrate that contains in the step (5) is added hydrochloric acid and is heated to 95 ℃, drive nitrate radical out of, then adding concentration in the solution is the strong base solution of 0.01 mol/L, regulate pH value to 1.8, then in this solution, add excessive S-WAT, and be warming up to 90 ℃, react 1 h and namely obtain pure golden simple substance;
(7) separate aluminium: filter residue in the step (5) and the industrial alkali ratio with 1:3 is mixed, send in the High Temperature Furnaces Heating Apparatus, behind 400 ℃ of calcining at constant temperature 2 h, use deionized water dissolving, solid-to-liquid ratio is 1:20, then the sulfuric acid that adds 0.1 mol/L, regulator solution pH value to 3.0, the filtering separation solid-liquid namely obtains the aluminium leach liquor;
(8) extract aluminum oxide: add the strong base solution of 0.01 mol/L in the aluminium leach liquor of step (7), regulate pH value to 4.5, filtering separation obtains aluminium hydroxide, then at 800 ℃ temperature lower calcination 0.5 h, namely obtains pure aluminum oxide.
Embodiment four extracts rare precious metal---the method for gallium and gold and aluminum oxide among the waste and old LED
Specifically, the technique of rare precious metal comprises the steps: among the waste and old LED of the described comprehensive reutilization of the present patent application
(1) coarse crushing and sorting: after getting waste and old LED wafer cleaning and drying that shell is broken, the LED wafer is partly sorted out;
(2) fragmentation: get the LED wafer in the step (1), adopt ball-milling technology, the LED wafer is milled to 130 purpose powder;
(3) separating gallium: the LED wafer powder in the 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 that makes catalyzer in the solution is 0.5 mol/L, then with solution constant temperature 12 h under 30 ℃ of conditions, and use the ultraviolet lamp Continuous irradiation, after reaction finishes, carry out filtering separation and wash three times, obtain filtrate and filter residue;
(4) extract gallium: with the Gallium solution that contains in the step (3), through being the salt acid for adjusting pH value to 6 of 0.1 mol/L with concentration, gallium is precipitated out, then the gallium throw out is joined in the concentrated alkali solution that concentration is 10 mol/L, adopt electrodeposition method to extract gallium, the electrodeposition condition is 45 ℃ of electrolyte temperatures, current density 300 A/m
2, electrodeposition times 3 h;
(5) Leaching of Gold: the filter residue in the step (3) is soaked with chloroazotic acid, and solid-to-liquid ratio is 1:100, soaks 2 h under 50 ℃ of conditions, filters and obtains containing golden filtrate and filter residue;
(6) extract gold: the golden filtrate that contains in the step (5) is added hydrochloric acid and is heated to 100 ℃, drive nitrate radical out of, then adding concentration in the solution is the strong base solution of 0.1 mol/L, regulate pH value to 2.5, then in this solution, add excessive sodium bisulfite, and be warming up to 100 ℃, react 1 h and namely obtain pure golden simple substance;
(7) separate aluminium: filter residue in the step (5) and the industrial alkali ratio with 1:10 is mixed, send in the High Temperature Furnaces Heating Apparatus, behind 600 ℃ of calcining at constant temperature 0.5 h, use deionized water dissolving, solid-to-liquid ratio is 1:100, then the sulfuric acid that adds 0.001 mol/L, regulator solution pH value to 1.0, the filtering separation solid-liquid namely obtains the aluminium leach liquor;
(8) extract aluminum oxide: add the strong base solution of 0.1 mol/L in the aluminium leach liquor of step (7), regulate pH value to 6, filtering separation obtains aluminium hydroxide, then at 1200 ℃ temperature lower calcination 4 h, namely obtains pure aluminum oxide.
Claims (6)
1. the technique of rare precious metal among the waste and old LED of comprehensive reutilization is characterized in that: comprise the steps:
(1) coarse crushing and sorting: after getting waste and old LED wafer cleaning and drying that shell is broken, the LED wafer is partly sorted out;
(2) fragmentation: get the LED wafer in the step (1), adopt ball-milling technology, the LED wafer is milled to powder;
(3) separating gallium: the LED wafer powder in the 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 that makes catalyzer in the solution is 0.05 ~ 0.5 mol/L, then with solution constant temperature 4 ~ 12 h under 30 ~ 95 ℃ of conditions, and use the ultraviolet lamp Continuous irradiation, after reaction finishes, carry out filtering separation and wash three times, obtain filtrate and filter residue;
(4) extract gallium: with the Gallium solution that contains in the step (3), between the salt acid for adjusting pH value to 5 ~ 8 through with concentration being 0.01 ~ 0.1 mol/L, gallium is precipitated out, then the gallium throw out is joined in the concentrated alkali solution that concentration is 10 ~ 25 mol/L, adopt electrodeposition method to extract gallium;
(5) Leaching of Gold: the filter residue in the step (3) is soaked with chloroazotic acid, and solid-to-liquid ratio is 1:30 ~ 100, soaks 2 ~ 6 h under 20 ~ 50 ℃ of conditions, filters to obtain containing golden filtrate and filter residue;
(6) extract gold: the golden filtrate that contains in the step (5) is added hydrochloric acid and is heated to 90 ~ 100 ℃, drive nitrate radical out of, then adding concentration in the solution is the strong base solution of 0.01 ~ 0.1 mol/L, regulate pH value to 1.8 ~ 2.5, then in this solution, add excessive ferrous sulfate, S-WAT or sodium bisulfite, and being warming up to 90 ~ 100 ℃, reaction 1 ~ 2 h namely obtains pure golden simple substance.
2. method according to claim 1 is characterized in that, described method also comprises the step of extracting aluminum oxide,
(1) separates aluminium: the filter residue in claim 1 step (5) and the industrial alkali ratio with 1:3 ~ 10 is mixed, send in the High Temperature Furnaces Heating Apparatus, behind 400 ~ 600 ℃ of calcining at constant temperature 0.5 ~ 2 h, use deionized water dissolving, solid-to-liquid ratio is 1:20 ~ 100, then the sulfuric acid that adds 0.001 ~ 0.1 mol/L, regulator solution pH value to 1.0 ~ 3.0, the filtering separation solid-liquid namely obtains the aluminium leach liquor;
(2) extract aluminum oxide: the strong base solution that adds 0.01 ~ 0.1 mol/L in the aluminium leach liquor of step (1), regulate pH value to 4.5～6, filtering separation obtains aluminium hydroxide, then at 800 ~ 1200 ℃ temperature lower calcination 0.5～4 h, namely obtains pure aluminum oxide.
3. method according to claim 1 is characterized in that: in step (2), the LED chip ball is milled to 120 ~ 150 orders.
4. method according to claim 1, it is characterized in that: in step (3), the wavelength of ultra violet lamp is 254 ~ 367 nm.
5. method according to claim 1 is characterized in that: in step (3), adopt Medium speed filter paper to carry out filtering separation.
6. method according to claim 1, it is characterized in that: in step (4), the electrodeposition condition is 30 ~ 60 ℃ of electrolyte temperatures, current density 100 ~ 500 A/m
2, electrodeposition time 1 ~ 5 h.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104726894A (en) * | 2015-03-30 | 2015-06-24 | 北京化工大学 | Gallium recycling method |
| CN106381390A (en) * | 2016-09-14 | 2017-02-08 | 南昌大学 | Waste LED lighting bulb recycling method |
| CN109055782A (en) * | 2018-08-24 | 2018-12-21 | 华南理工大学 | The leaching method of gallium in a kind of useless light emitting diode |
| CN109112546A (en) * | 2018-07-27 | 2019-01-01 | 佛山市三水雄鹰铝表面技术创新中心有限公司 | Stew the oxidation line configuration and technique of mould liquid recycling aluminium hydroxide and sodium sulphate |
| CN109112537A (en) * | 2018-07-27 | 2019-01-01 | 佛山市三水雄鹰铝表面技术创新中心有限公司 | Configuration and technique of the oxidation solution for oil removing neutralizer recycling aluminium hydroxide and sodium sulphate |
| 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 |
| 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 |
| CN112264037A (en) * | 2020-10-21 | 2021-01-26 | 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 |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104726894A (en) * | 2015-03-30 | 2015-06-24 | 北京化工大学 | Gallium recycling method |
| CN104726894B (en) * | 2015-03-30 | 2018-07-27 | 北京化工大学 | The method for recycling gallium |
| CN106381390A (en) * | 2016-09-14 | 2017-02-08 | 南昌大学 | Waste LED lighting bulb recycling method |
| CN109112546A (en) * | 2018-07-27 | 2019-01-01 | 佛山市三水雄鹰铝表面技术创新中心有限公司 | Stew the oxidation line configuration and technique of mould liquid recycling aluminium hydroxide and sodium sulphate |
| CN109112537A (en) * | 2018-07-27 | 2019-01-01 | 佛山市三水雄鹰铝表面技术创新中心有限公司 | Configuration and technique of the oxidation solution for oil removing neutralizer recycling aluminium hydroxide and sodium sulphate |
| 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 |
| CN109055782A (en) * | 2018-08-24 | 2018-12-21 | 华南理工大学 | The leaching method of gallium in a kind of useless 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 |
| CN112264037A (en) * | 2020-10-21 | 2021-01-26 | 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 |
| 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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