CN103387237A - Method for recycling optical fiber wastes - Google Patents
Method for recycling optical fiber wastes Download PDFInfo
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- CN103387237A CN103387237A CN201210142853XA CN201210142853A CN103387237A CN 103387237 A CN103387237 A CN 103387237A CN 201210142853X A CN201210142853X A CN 201210142853XA CN 201210142853 A CN201210142853 A CN 201210142853A CN 103387237 A CN103387237 A CN 103387237A
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- optical fiber
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- resource recovery
- fiber waste
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Abstract
The invention relates to the treatment of electronic waste materials, and particularly relates to a method for recycling optical fiber wastes. The scheme of the method for recycling the optical fiber wastes includes the following steps: (1) crushing the optical fiber wastes into optical fiber powder; (2) cleaning the optical fiber powder and drying; (3) mixing the optical fiber powder and carbon powder evenly; (4) reacting mixed powder in chlorine gas flow conditions at the temperature of 980-1200 DEG C for 1-4 h; and (5) condensing a mixed gas obtained by the reaction, and then obtaining silicon tetrachloride and germanium tetrachloride through fractional distillation of a liquid obtained by the condensation. The method for recycling the optical fiber wastes has the features of short technological process, high product purity, environmental friendliness and the like.
Description
Technical field
The present invention relates to the processing to the electronics waste and scrap, be specifically related to a kind of method of optical fiber waste resource recovery.
Background technology
Development along with information technology and optic fibre manufacturing technology, whole world optical fiber demand is just with annual 10% speed increase, optical fiber is popularized on a large scale in global information communication, when giving a large amount of high transfer rates of the mankind, annual a large amount of optical fiber waste material to the environment band huge negative impact.At present the resource utilization of optical fiber waste material mainly concentrates on the germanium that extracts wherein, and the technique of using has: 1. hydrofluoric acid lixiviation process, the method adopts the main substance SiO of hydrofluoric acid dissolution optical fiber waste material
2Produce H
-2SiF
6, GeO wherein
2Generate H with HF
-2GeF
6Enter solution, adopt the heavy germanium of tannic acid after neutralization, carry out finally chlorinated distillation and obtain thick GeCl
4, the shortcoming of the method is that HF is large to equipment corrosion, equipment cost is large; 2. high-temperature roasting after alkali fusion, the method mix with alkali and optical fiber waste material, make SiO
2Change Na into
2SiO
4Destroy SiO
2, to the parcel of germanium, make simultaneously GeO
2Be converted into germanate, then through chlorinated distillation, obtain thick GeCl
4, the shortcoming of the method is to need to consume a large amount of alkali and acid.Above two kinds of techniques, due to himself shortcoming, make it outside obtaining the germanium of high added value, and are also quite serious on the impact of environment.
Summary of the invention
The invention provides a kind of method of optical fiber waste resource recovery, is a kind of novel process of optical fiber comprehensive utilization of waste material, and this technique has the characteristics such as technical process is short, products obtained therefrom purity is high, environmental friendliness.
The method of a kind of optical fiber waste resource recovery of the present invention, its scheme comprises the following steps:
(1) the optical fiber waste material is made the fine powder of 80～200 sight through fragmentation;
(2) clean the optical fiber powder, and dry to constant weight under 100～200 ℃;
(3) the optical fiber powder is mixed with 80～200 purpose carbon dusts, the mass ratio of optical fiber powder and carbon dust is 1:0.1～0.8;
(4) with mixed powder under the cl gas flow condition of 180～300Nl/h, react 1～4h at 980～1200 ℃ of temperature;
(5) Mixed Gas Condensation to 20 that reaction is obtained～40 ℃, and then the liquid fractionation that condensation is obtained, 60～75 ℃ of collections obtain silicon tetrachloride, and 85～95 ℃ of collections obtain germanium tetrachloride.
Preferably,
In step (1), optical fiber is crushed to 120～150 order powder;
Step (2) washed with de-ionized water optical fiber powder, and dry to constant weight under 150～180 ℃;
The mass ratio of step (3) optical fiber powder and carbon dust is 1:0.5;
Step (4) is heated to 1050～1100 ℃;
Cardinal principle of the present invention is, obtain the powder of certain particle size after the fragmentation of optical fiber waste material, adopt the carbon thermal chlorination to obtain silicon tetrachloride and germanium tetrachloride mixed gas, then through fractionation, silicon tetrachloride is separated with germanium tetrachloride, silicon tetrachloride directly reclaims, and obtains germanium dioxide after the germanium tetrachloride hydrolysis.
SiO
2+2C+2Cl
2→SiCl
4+2CO
GeO
2+2C+2Cl
2→GeCl
4+2CO
The method of optical fiber waste resource recovery of the present invention has the characteristics such as technical process is short, products obtained therefrom purity is high, environmental friendliness.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment, but protection scope of the present invention is not limited to these embodiment.
Embodiment one
The method of optical fiber waste resource recovery, concrete steps are as follows:
(1) the optical fiber waste material makes the fine powder of 120 sight through fragmentation;
(2) dry to constant weight with washed with de-ionized water optical fiber powder and under 150 ℃;
(3) the optical fiber powder mixes with 150 purpose carbon dusts, and the mass ratio of optical fiber powder and carbon dust is 1:0.5;
(4) mixed powder, as in silica tube, passes into the cl gas flow (nitrogen dilution) of 240Nl/h, is heated to 1050 ℃, reaction 2h;
(5) reacting the mixed gas that obtains is transported in condenser and is condensed to 30 ℃ with nitrogen;
(6) liquid that obtains fractionation again, collect the silicon tetrachloride cut under 70 ℃, collect the germanium tetrachloride cut under 90 ℃;
The silicon tetrachloride purity that obtains is 99%, directly as production marketing;
Obtain purity after the hydrolysis of the germanium tetrachloride that obtains and be the germanium dioxide more than 99%.
Embodiment two
The method of optical fiber waste resource recovery, concrete steps are as follows:
(1) the optical fiber waste material makes the fine powder of 150 sight through fragmentation;
(2) dry to constant weight with washed with de-ionized water optical fiber powder and under 180 ℃;
(3) the optical fiber powder mixes with 150 purpose carbon dusts, and the mass ratio of optical fiber powder and carbon dust is 1:0.1;
(4) mixed powder, as in silica tube, passes into the cl gas flow (nitrogen dilution) of 180Nl/h, is heated to 980 ℃, reaction 4h;
(5) reacting the mixed gas that obtains is transported in condenser and is condensed to 30 ℃ with nitrogen;
(6) liquid that obtains fractionation again, collect the silicon tetrachloride cut under 68 ℃, collect the germanium tetrachloride cut under 85 ℃;
The silicon tetrachloride purity that obtains is 98.5%, directly as production marketing;
Obtain purity after the hydrolysis of the germanium tetrachloride that obtains and be the germanium dioxide more than 99%.
Embodiment three
The method of optical fiber waste resource recovery, concrete steps are as follows:
(1) the optical fiber waste material makes the fine powder of 130 sight through fragmentation;
(2) dry to constant weight with washed with de-ionized water optical fiber powder and under 100 ℃;
(3) the optical fiber powder mixes with 130 purpose carbon dusts, and the mass ratio of optical fiber powder and carbon dust is 1:0.8;
(4) mixed powder, as in silica tube, passes into the cl gas flow (nitrogen dilution) of 300Nl/h, is heated to 1200 ℃, reaction 2h;
(5) reacting the mixed gas that obtains is transported in condenser and is condensed to 40 ℃ with nitrogen;
(6) liquid that obtains fractionation again, collect the silicon tetrachloride cut under 75 ℃, collect the germanium tetrachloride cut under 90 ℃;
The silicon tetrachloride purity that obtains is 98%, directly as production marketing;
Obtain purity after the hydrolysis of the germanium tetrachloride that obtains and be the germanium dioxide more than 99%.
Embodiment four
The method of optical fiber waste resource recovery, concrete steps are as follows:
(1) the optical fiber waste material makes the fine powder of 80 sight through fragmentation;
(2) dry to constant weight with washed with de-ionized water optical fiber powder and under 200 ℃;
(3) the optical fiber powder mixes with 200 purpose carbon dusts, and the mass ratio of optical fiber powder and carbon dust is 1:0.4;
(4) mixed powder, as in silica tube, passes into the cl gas flow (nitrogen dilution) of 220Nl/h, is heated to 1100 ℃, reaction 3h;
(5) reacting the mixed gas that obtains is transported in condenser and is condensed to 35 ℃ with nitrogen;
(6) liquid that obtains fractionation again, collect the silicon tetrachloride cut under 70 ℃, collect the germanium tetrachloride cut under 95 ℃;
The silicon tetrachloride purity that obtains is 99%, directly as production marketing;
Obtain purity after the hydrolysis of the germanium tetrachloride that obtains and be the germanium dioxide more than 99%.
Embodiment five
The method of optical fiber waste resource recovery, concrete steps are as follows:
(1) the optical fiber waste material makes the fine powder of 200 sight through fragmentation;
(2) dry to constant weight with washed with de-ionized water optical fiber powder and under 160 ℃;
(3) the optical fiber powder mixes with 80-200 purpose carbon dust, and the mass ratio of optical fiber powder and carbon dust is 1:0.7;
(4) mixed powder, as in silica tube, passes into the cl gas flow (nitrogen dilution) of 200Nl/h, is heated to 1070 ℃, reaction 2.5h;
(5) reacting the mixed gas that obtains is transported in condenser and is condensed to 25 ℃ with nitrogen;
(6) liquid that obtains fractionation again, collect the silicon tetrachloride cut under 75 ℃, collect the germanium tetrachloride cut under 95 ℃;
The silicon tetrachloride purity that obtains is 97.5%, directly as production marketing;
Obtain purity after the hydrolysis of the germanium tetrachloride that obtains and be the germanium dioxide more than 99%.
Embodiment six
The method of optical fiber waste resource recovery, concrete steps are as follows:
(1) the optical fiber waste material makes the fine powder of 140 sight through fragmentation;
(2) dry to constant weight with washed with de-ionized water optical fiber powder and under 180 ℃;
(3) the optical fiber powder mixes with 140 purpose carbon dusts, and the mass ratio of optical fiber powder and carbon dust is 1:0.2;
(4) mixed powder, as in silica tube, passes into the cl gas flow (nitrogen dilution) of 280Nl/h, is heated to 1180 ℃, reacts 1.5 hours;
(5) reacting the mixed gas that obtains is transported in condenser and is condensed to 20 ℃ with nitrogen;
(6) liquid that obtains fractionation again, collect the silicon tetrachloride cut under 75 ℃, collect the germanium tetrachloride cut under 85 ℃;
The silicon tetrachloride purity that obtains is 97%, directly as production marketing;
Obtain purity after the hydrolysis of the germanium tetrachloride that obtains and be the germanium dioxide more than 99%.
Above-described embodiment is the better embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (5)
1. the method for an optical fiber waste resource recovery, is characterized in that, comprises the following steps:
(1) the optical fiber waste material is made the fine powder of 80～200 sight through fragmentation;
(2) clean the optical fiber powder, and dry to constant weight under 100～200 ℃;
(3) the optical fiber powder is mixed with 80～200 purpose carbon dusts, the mass ratio of optical fiber powder and carbon dust is 1:0.1～0.8;
(4) with mixed powder under the cl gas flow condition of 180～300Nl/h, react 1～4h at 980～1200 ℃ of temperature;
(5) Mixed Gas Condensation that reaction is obtained, and then the liquid fractionation that condensation obtains is obtained silicon tetrachloride and germanium tetrachloride.
2. the method for optical fiber waste resource recovery according to claim 1, is characterized in that, in step (1), optical fiber is crushed to 120～150 order powder.
3. the method for optical fiber waste resource recovery according to claim 1, is characterized in that, step (2) washed with de-ionized water optical fiber powder, and dry to constant weight under 150～180 ℃.
4. the method for optical fiber waste resource recovery according to claim 1, is characterized in that, the mass ratio of step (3) optical fiber powder and carbon dust is 1:0.5.
5. the method for optical fiber waste resource recovery according to claim 1, is characterized in that, step (4) is heated to 1050～1100 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210142853XA CN103387237A (en) | 2012-05-10 | 2012-05-10 | Method for recycling optical fiber wastes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210142853XA CN103387237A (en) | 2012-05-10 | 2012-05-10 | Method for recycling optical fiber wastes |
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| Publication Number | Publication Date |
|---|---|
| CN103387237A true CN103387237A (en) | 2013-11-13 |
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ID=49531672
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210142853XA Pending CN103387237A (en) | 2012-05-10 | 2012-05-10 | Method for recycling optical fiber wastes |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110079686A (en) * | 2018-11-20 | 2019-08-02 | 云南驰宏国际锗业有限公司 | A kind of germanium scrap metal processing method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1597533A (en) * | 2004-07-27 | 2005-03-23 | 南京大学 | Production technology of optical fiber grade high purity ger manium tetrachloride |
| CN1842491A (en) * | 2004-08-04 | 2006-10-04 | 德古萨公司 | Method and device for purifying silicon tetrachloride or germanium tetrachloride containing hydride |
| CN101925537A (en) * | 2007-12-05 | 2010-12-22 | 国家科学研究学院 | From optical fiber or glass slag, reclaim GeCl 4And/or SiCl 4Method and by being rich in SiO 2Material make SiCl 4Method |
-
2012
- 2012-05-10 CN CN201210142853XA patent/CN103387237A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1597533A (en) * | 2004-07-27 | 2005-03-23 | 南京大学 | Production technology of optical fiber grade high purity ger manium tetrachloride |
| CN1842491A (en) * | 2004-08-04 | 2006-10-04 | 德古萨公司 | Method and device for purifying silicon tetrachloride or germanium tetrachloride containing hydride |
| CN101925537A (en) * | 2007-12-05 | 2010-12-22 | 国家科学研究学院 | From optical fiber or glass slag, reclaim GeCl 4And/or SiCl 4Method and by being rich in SiO 2Material make SiCl 4Method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110079686A (en) * | 2018-11-20 | 2019-08-02 | 云南驰宏国际锗业有限公司 | A kind of germanium scrap metal processing method |
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Application publication date: 20131113 |