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Method for recycling gallium from indissolvable gallium compounds and gallium recycled by virtue of method

A compound, insoluble technology, applied in the field of gallium recovery, can solve the problems of difficult separation, consumption of large oxides, harsh conditions, etc., to achieve the effect of simple process flow, improved leaching rate, and less time consumption

Active Publication Date: 2018-08-07
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the good thermal and chemical stability of gallium nitride, insoluble in inorganic acids such as sulfuric acid and hydrochloric acid, and low-concentration alkalis, there are few studies on the recovery of gallium from waste materials containing gallium nitride, and the existing technologies usually have their own defects. , not conducive to industrial application
[0004] CN 102951618 A discloses a method for recovering germanium, gallium, indium, and selenium from waste diodes. By crushing waste diodes, separating plastic powder and metal powder, oxidizing and roasting the metal powder, adding zinc powder after dissolving the product with acid, Substitution to obtain germanium, gallium, and indium elemental substances, and then roasting the elemental substances in an atmosphere of chlorine or hydrogen chloride, and separating germanium, gallium, and indium elements according to the different condensation temperatures of the chlorination products, but the final product of this method does not obtain metal elemental substances, and consumes The energy is huge, chlorine gas is needed in the recycling process, waste gas and dust are likely to cause environmental pollution, and are not suitable for industrial production
CN 105567982 A discloses a method for recovering gallium metal from gallium nitride waste. Gallium nitride is placed in a reaction vessel, and then sodium hydroxide, hydrogen peroxide, sodium peroxide and other oxidants are added dropwise into the reaction vessel. Until gallium nitride is completely dissolved, finally the reaction solution is passed through electrowinning to recover metal gallium, but this method needs to consume a large amount of oxide and produce a large amount of alkaline solution, and the high concentration of alkaline solution makes separation difficult, which is not conducive to wide application
CN 104532012 A discloses a method for recovering gallium and gold from gallium nitride chip production waste, and CN 104576848 A discloses a method for recovering gallium from waste gallium nitride-based light-emitting diodes, both of which contain nitrogen The particles after crushing gallium chloride waste are separated by high-temperature vacuum metallurgy, and metal elements are recovered. However, this method requires harsh conditions of high temperature and high vacuum, and the waste gas generated needs special treatment before it can be discharged.

Method used

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  • Method for recycling gallium from indissolvable gallium compounds and gallium recycled by virtue of method

Examples

Experimental program
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Effect test

Embodiment 1

[0056] This embodiment provides a method for recovering gallium from waste materials containing insoluble gallium compounds, the method comprising the following steps:

[0057] (1) Take 100g of powder produced when the MOCVD method is used to produce gallium nitride, wherein the gallium content is 75wt%, and the main form of gallium is GaN, and then 200g of ammonium chloride is mixed with the powder, at a speed of 200r / min Ball milling treatment for 30 minutes, and then roasting treatment, the roasting treatment temperature is 300 ° C, and the roasting treatment time is 2 hours;

[0058] (2) leaching the roasted product of step (1) with deionized water, the leaching temperature is 50° C., leaching for 60 min at a rotating speed of 300 r / min, and filtering to obtain a gallium-rich solution, which is passed through an inductively coupled plasma emission spectrometer ( ICP-OES) test, the gallium-rich solution contains 24.98g / L gallium, the gallium-rich solution is kept at a const...

Embodiment 2

[0061] This embodiment provides a method for reclaiming gallium from waste materials containing insoluble gallium compounds, the process flow diagram of the method is as follows figure 1 shown, including the following steps:

[0062] (1) Take 100g of waste LED lamp bead chips as the waste material containing indium gallium nitride, wherein the gallium content is 6.05wt%, after the waste material is crushed, it is sieved through a sieve with a sieve diameter of 0.149mm, and after soaking in water Filtrate to obtain the powder containing indium gallium nitride, then take 200g of magnesium chloride and mix it with the powder, rod mill for 40min at a speed of 300r / min, and then perform roasting treatment, the roasting treatment temperature is 400°C, and the roasting treatment time is 1.5 h;

[0063] (2) The product roasted in step (1) is leached with 0.5mol / L hydrochloric acid, the leaching temperature is 60°C, and the leaching is performed at a speed of 300r / min for 60min, filte...

Embodiment 3

[0066] This embodiment provides a method for reclaiming gallium from waste materials containing insoluble gallium compounds. The method is referred to the method in Example 1, the difference is only that the chlorination agent used in step (1) is sodium chloride and Potassium chloride, the mass ratio of gallium nitride powder to chlorinating agent is 1:5.

[0067] In this example, 73.90 g of gallium metal was obtained by electrolysis, with a yield of 98.53% and a purity of 99.9 wt%.

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Abstract

The invention provides a method for recycling gallium from indissolvable gallium compounds and gallium recycled by virtue of the method. The method comprises the steps of mixing waste containing the indissolvable gallium compounds with a chlorinating agent, sintering, leaching a sintered product, and carrying out electrolysis, so as to obtain metal gallium. According to the method, the waste containing the indissolvable gallium compounds is mixed with the chlorinating agent and is sintered, and the difficulty-leached gallium compounds are converted into easily-leached gallium chloride, so thatthe leaching rate of gallium is greatly increased, the recycling rate of gallium reaches 98% or above, and the purity of metal gallium can reach 99.9wt%. The process flow is simple, the consumed timeis relatively short, the waste gas and the dust which are harmful to the environment are not discharged, and the method has wide industrial application prospects.

Description

technical field [0001] The invention belongs to the technical field of recycling semiconductor waste materials, and relates to a method for recovering gallium from waste materials containing insoluble gallium compounds and the gallium obtained by the method. Background technique [0002] Gallium nitride (GaN) is widely used in solid-state light sources, electronic power and microwave radio frequency devices due to its superior properties such as large band gap, high breakdown electric field, high thermal conductivity, high electron saturation drift rate and strong radiation resistance. Wide range of applications, its products cover semiconductor lighting, mobile communications, energy Internet, high-speed rail transit, new energy vehicles and consumer electronics and other fields. With the upgrading of products, the amount of waste slag containing gallium nitride in my country is also increasing rapidly year by year. Since gallium is a scattered metal, the annual output is l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B58/00C25C1/22C22B1/02
CPCC22B1/02C22B7/001C22B7/007C22B58/00C25C1/22Y02P10/20
Inventor 孙峙方升曹宏斌
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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