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Method for recycling germanium from high-silicon-content optical fiber production waste

A technology for producing waste and optical fibers, applied in the direction of improving process efficiency, can solve the problems of inability to leaching, high silicon content in the leaching solution, and high production costs, and achieve the effects of avoiding hazards, high-efficiency recycling, and low-cost

Pending Publication Date: 2019-03-08
六盘水中联工贸实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high silicon content, it is not possible to directly chlorinate and distill germanium tetrachloride with hydrochloric acid, because silicon will also be distilled as silicon tetrachloride and mixed with germanium tetrachloride. During hydrolysis, germanium dioxide and silicon dioxide will be precipitated at the same time, which cannot be separated. germanium and silicon
Direct use of sulfuric acid leaching or sulfuric acid oxidation leaching, germanium cannot be leached because silicon dioxide wraps germanium
Using sodium hydroxide or fluoride leaching, the obtained leaching solution contains a lot of silicon, which cannot be successfully separated from germanium and silicon.
At the same time, sodium hydroxide or fluoride consumes a lot, and the production cost is very high, which is unacceptable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0017] Embodiment: A method for recovering germanium from waste material of high-silicon-containing optical fiber production, including the following steps:

[0018] Step 1. Grind the high-silicon fiber production waste (bottom slag and scum) to more than 100 meshes, destroying the crystalline silicon structure and the phenomenon of silicon-coated germanium;

[0019] Step 2. Add sodium sulfide or sulfur powder to the grinding material of step 1 according to S / Ge=1.2-1.3, mix evenly, and granulate into a diameter of 1-5mm;

[0020] Step 3. Add the granular raw material of step 2 to a microwave oven, a fuming furnace, a rotary kiln, and other sulfidation volatilization furnaces, and control the sulfidation volatilization temperature of 800-1000°C for germanium sulfidation volatilization;

[0021] Step 4. Perform oxidation roasting of the sulfide volatilized fume in step 3, and control the oxidation roasting temperature to be 300-500°C. In this step, care should be taken to prevent german...

example 1

[0024] Example 1. The furnace bottom slag produced by an enterprise producing optical fiber contains 96.5% silica and 2.78% germanium. It is ground to 120 mesh first, and then sodium sulfide is added according to S / Ge=1.2, mixed uniformly and granulated into diameter 2mm. Put it in a microwave oven for vulcanization and volatilization. The operating conditions of the microwave oven are microwave radiation frequency 2.4GHz, power 500W, furnace temperature 850℃, time 20 minutes, and vulcanized volatile fumes mainly contain 29.1% germanium, 18.3% sulfur, 9.2% silica, and volatile residue contains dioxide Silicon is 94.5%, germanium is 0.18%, and germanium volatilization rate is 92.3%.

example 2

[0025] Example 2. The bottom slag and scum mixture of an optical fiber production furnace contains 95.2% silicon dioxide and 3.1% germanium. After grinding to 250 mesh, add sulfur powder according to S / Ge=1.25, mix and granulate to a diameter of 3.5mm. The sulfide volatilization furnace in the laboratory uses electric heating to perform vulcanization and volatilization. The temperature in the furnace is controlled to 1000°C for 2 hours. The sulfurized dust contains 27.8% germanium, 16.5% sulfur, 15.8% silica, and 0.31 germanium in the slag. %. The germanium volatilization rate is 90%.

[0026] Example 3. Use the sulfurized volatile fumes of Example 1 to oxidize and roast in a microwave oven, add an oxidizer (hydrogen peroxide) to 110% of the oxygen required for the total sulfur content in the raw materials, mix uniformly, and place in a microwave oven to control the microwave power 300-500W, temperature 350℃± 10°C, time 10 minutes. The sulfur content in the roasted product is r...

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PUM

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Abstract

The invention discloses a method for recycling germanium from high-silicon-content optical fiber production waste. The method comprises the following steps that (1) the high-silicon-content and germanium-containing optical fiber production waste is ground till the number of holes is 100 or above,, and then a vulcanizing agent is added and uniformly mixed to prepare particles with the diameters of1-5 mm; (2) sulfidingvolatilization is carried out on the germanium, and the germanium sulfide volatilization smoke dust is collected, or the mixed volatilization smoke dust of the germanium sulfide and germanium dioxide is collected; (3) the obtained germanium-containing smoke dust is subjected to microwave oxidation roasting or oxidation roasting in other forms, or is subjected to sulfuric acidoxidation leaching directly; (4) the high-germanium-content microwave oxidation roasting product is directly subjected to hydrochloric acid chlorination distillation so as to obtain germanium tetrachloride to be subjected to hydrolyzation, and thus a germanium dioxide concentrate is obtained; and (5) sulfuric acid oxidation leaching is carried out on the low-germanium-content materials in the step(2) and the step (3), wherein a leaching solution adopts tannin or an organic solvent to precipitate or extract the enriched germanium and to produce the germanium concentrate. The method can be usedfor extracting and separating the germanium and the silicon from the materials containing 95% or above of the silicon at high efficiency and low cost.

Description

Technical field [0001] The invention relates to a furnace bottom slag or scum with high silicon and germanium content produced in the production of germanium-doped optical fiber, and a technology for recovering germanium from the middle, low cost and high efficiency, belonging to the field of comprehensive recovery of rare and rare metals. Background technique [0002] Optical fiber communication has replaced the traditional wired cable communication, and the production of optical fiber must be doped with germanium to have communication advantages. At present, the consumption of germanium in optical fiber communication has reached more than 30% of the total germanium consumption. Germanium is a kind of rare and rare metal with limited geological reserves, wide use and high value. Therefore, recovery of germanium from various renewable resources has important social and economic benefits. The production of germanium-doped fiber will produce about 5% of the bottom dross and scum....

Claims

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Application Information

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IPC IPC(8): C22B7/00C22B1/00C22B1/02C22B41/00
CPCC22B1/02C22B7/007C22B41/00Y02P10/20
Inventor 李世平钟波
Owner 六盘水中联工贸实业有限公司
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