CN106587067A - Method for recycling silicon powder from silicon-containing waste residues - Google Patents
Method for recycling silicon powder from silicon-containing waste residues Download PDFInfo
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- CN106587067A CN106587067A CN201611064181.XA CN201611064181A CN106587067A CN 106587067 A CN106587067 A CN 106587067A CN 201611064181 A CN201611064181 A CN 201611064181A CN 106587067 A CN106587067 A CN 106587067A
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- silicon
- containing waste
- silica flour
- ball milling
- waste residue
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to the technical field of silicon powder preparing, in particular to a method for recycling silicon powder from silicon-containing waste residues. The method includes the specific following steps that the silicon-containing waste residues are taken, water, an oxidizing agent and hydrochloric acid are added for washing, then the mixture is transferred into a vacuum filtration tank, clear water is added for washing, the filtered precipitate enters a stirring tank, clear water is added, the mixture is stirred to be even, then the stirred product is subjected to ball milling for 1 h to 2 h through a ball milling machine, centrifugal separation is carried out, decarbonization and dehydration are carried out, and the silicon powder is obtained. The method is high in silicon-dioxide recycling rate, low in treating cost, simple in technology step, easy to operate and suitable for industrialization, it is achieved that the silicon-containing waste residues are reasonably used, environment pollution is reduced, and economic benefits are increased.
Description
（One）Technical field
The present invention relates to silica flour preparing technical field, more particularly to a kind of method that silica flour is reclaimed from silicon-containing waste residue.
（Two）Background technology
The compound such as organosilicon and trichlorosilane is the usual products in Chemical Manufacture, is widely used in electric, building, fortune
The industries such as defeated, chemical industry, weaving, medical treatment, it is of many uses.
Discarded silica flour is inevitably produced in organosilicon or trichlorosilane preparation process, is reaction aborning
The mixture of silica flour and other impurities is referred to as waste residue.If these waste residues are directly buried, serious environmental pollution is not only caused, and
And can large losses silicon, cause the significant wastage of resource, so silica flour is recycled from waste residue necessary.
The Chinese patent document of Publication No. CN1760124A discloses a kind of catalyst and silicon for based on copper
The waste silicon powder produced during powder hybrid reaction production organosilicon carries out resurrection regeneration method.Its step is：First washed with organic solvent
The organic pollution on waste silicon powder surface is removed, adds sulphuric acid to remove reactive metal oxide complete solvent, then with sulfuric acid scrubbing, controlled
Reaction temperature processed is 75-80 DEG C, insulated and stirred 24 hours, makes metal copper dissolution in waste silicon powder completely, and pickle repetition makes
With reclaiming to pH value to when 1-1.5, solid portion is the silica flour for bringing back to life, and is dried when being washed to pH value about 7.But, the method
In targeted waste silicon powder predominantly because of floating, sedimentation and react the waste silicon powder that the reason such as not exclusively is produced, impurity kind therein
Class is less, therefore the method narrow application range, and during need to use organic solvent, the method not to enter organic solvent
Row recycling, economic benefit and environmental protection effect it is not obvious enough.
（Three）The content of the invention
The present invention is in order to make up the deficiencies in the prior art, there is provided a kind of process is simple, low production cost from silicon-containing waste residue
The method for reclaiming silica flour.
For achieving the above object, the present invention is achieved through the following technical solutions：One kind reclaims silicon from silicon-containing waste residue
The method of powder, it is characterised in that including step in detail below：
（1）Solvent clean：Take silicon-containing waste residue to pour in the first agitator tank, add water, oxidant and hydrochloric acid to be cleaned, it is siliceous useless
The mass ratio of slag, water, oxidant and hydrochloric acid is（95-105）:（180-200）:（0.5-1.5）:1；
（2）Washing：By step（1）Mixture proceed in vacuum filtration tank, add clear water wash 2-3 time, then sucking filtration obtain
Precipitate enter the second agitator tank, add clear water stir；
（3）Ball milling：Step（2）The product for obtaining passes through ball mill ball milling 1-2h；
（4）Centrifugation：Step（3）The product that ball milling is obtained by the 3rd agitator tank stirring after, into horizontal type screw settling centrifuge
In, it is centrifuged, after dehydration, obtains product silica flour.
Further, the oxidant is hydrogen peroxide or sodium peroxide solution.
Further, step（2）The condition of middle vacuum filtration is -0.1MPa.
Further, step（3）After middle ball milling, the fineness of products therefrom is 100-150 mesh.
Further, step（4）The rotating speed of horizontal type screw settling centrifuge is 1200-1300r/min.
The invention has the beneficial effects as follows：
（1）The response rate of silica flour is higher than 80%, and silica flour content of monomer is higher than 98%, and processing cost is low；
（2）Processing step is simple, easy to operate, is suitable to industrialization；
（3）The reasonable utilization to silicon-containing waste residue is realized, environmental pollution is not only reduced, and be increased economic benefit.
（Four）Specific embodiment
The invention will be further described with reference to embodiments, but the invention is not limited in these embodiments.
Embodiment one
A kind of method that silicon dioxide is reclaimed from silicon-containing waste residue, including step in detail below：
（1）Solvent clean：Take 95 parts of silicon-containing waste residues to pour in the first agitator tank, add 180 portions of water, 0.5 part of hydrogen peroxide and 1 portion of salt
Acid is cleaned；
（2）Washing：By step（1）Mixture proceed in vacuum filtration tank, in room temperature（25℃）, under the conditions of pressure -0.1MPa,
Washed with clear water 2 times, the precipitate that then sucking filtration is obtained enters the second agitator tank, add clear water to stir；
（3）Ball milling：Step（2）The product for obtaining obtains fineness for 100-150 purpose products by ball mill ball milling 1h；
（4）Centrifugation：Step（3）The product that ball milling is obtained by the 3rd agitator tank stirring after, into horizontal type screw settling centrifuge
In, it is centrifuged under the conditions of 1200r/min, after dehydration, obtains product silica flour.
Embodiment two
A kind of method that silicon dioxide is reclaimed from silicon-containing waste residue, including step in detail below：
（1）Solvent clean：Take 100 parts of silicon-containing waste residues to pour in the first agitator tank, add 190 portions of water, 1 part of hydrogen peroxide and 1 portion of salt
Acid is cleaned；
（2）Washing：By step（1）Mixture proceed in vacuum filtration tank, in room temperature（25℃）, under the conditions of pressure -0.1MPa,
Washed with clear water 3 times, the precipitate that then sucking filtration is obtained enters the second agitator tank, add clear water to stir；
（3）Ball milling：Step（2）The product for obtaining obtains fineness for 100-150 purpose products by ball mill ball milling 2h；
（4）Centrifugation：Step（3）The product that ball milling is obtained by the 3rd agitator tank stirring after, into horizontal type screw settling centrifuge
In, it is centrifuged under the conditions of 1200r/min, after dehydration, obtains product silica flour.
Embodiment three
A kind of method that silicon dioxide is reclaimed from silicon-containing waste residue, including step in detail below：
（1）Solvent clean：Take 105 parts of silicon-containing waste residues to pour in the first agitator tank, add 200 parts of water, 1.5 parts of sodium peroxide solution
Cleaned with 1 part of hydrochloric acid；
（2）Washing：By step（1）Mixture proceed in vacuum filtration tank, in room temperature（25℃）, under the conditions of pressure -0.1MPa,
Washed with clear water 2 times, the precipitate that then sucking filtration is obtained enters the second agitator tank, add clear water to stir；
（3）Ball milling：Step（2）The product for obtaining obtains fineness for 100-150 purpose products by ball mill ball milling 2h；
（4）Centrifugation：Step（3）The product that ball milling is obtained by the 3rd agitator tank stirring after, into horizontal type screw settling centrifuge
In, it is centrifuged under the conditions of 1300r/min, after dehydration, obtains product silica flour.
Embodiment described above, simply several, the those skilled in the art of the present invention more preferably specific embodiment
The usual variations and alternatives that member is carried out in the range of technical solution of the present invention all should be comprising within the scope of the present invention.
Claims (5)
1. it is a kind of from silicon-containing waste residue reclaim silica flour method, it is characterised in that including step in detail below：
（1）Solvent clean：Take silicon-containing waste residue to pour in the first agitator tank, add water, oxidant and hydrochloric acid to be cleaned, it is siliceous useless
The mass ratio of slag, water, oxidant and hydrochloric acid is（95-105）:（180-200）:（0.5-1.5）:1；
（2）Washing：By step（1）Mixture proceed in vacuum filtration tank, add clear water wash 2-3 time, then sucking filtration obtain
Precipitate enter the second agitator tank, add clear water stir；
（3）Ball milling：Step（2）The product for obtaining passes through ball mill ball milling 1-2h；
（4）Centrifugation：Step（3）The product that ball milling is obtained by the 3rd agitator tank stirring after, into horizontal type screw settling centrifuge
In, it is centrifuged, after dehydration, obtains product silica flour.
2. it is according to claim 1 from silicon-containing waste residue reclaim silica flour method, it is characterised in that：The oxidant is double
Oxygen water or sodium peroxide solution.
3. it is according to claim 1 from silicon-containing waste residue reclaim silica flour method, it is characterised in that：Step（2）Middle vacuum
The condition of sucking filtration is -0.1MPa.
4. it is according to claim 1 from silicon-containing waste residue reclaim silica flour method, it is characterised in that：Step（3）Middle ball milling
The fineness of products therefrom is 100-150 mesh afterwards.
5. it is according to claim 1 from silicon-containing waste residue reclaim silica flour method, it is characterised in that：Step（4）Horizontal spiral shell
The rotating speed of rotation sedimentation centrifuge is 1200-1300r/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611064181.XA CN106587067A (en) | 2016-11-28 | 2016-11-28 | Method for recycling silicon powder from silicon-containing waste residues |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611064181.XA CN106587067A (en) | 2016-11-28 | 2016-11-28 | Method for recycling silicon powder from silicon-containing waste residues |
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| Publication Number | Publication Date |
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| CN106587067A true CN106587067A (en) | 2017-04-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201611064181.XA Pending CN106587067A (en) | 2016-11-28 | 2016-11-28 | Method for recycling silicon powder from silicon-containing waste residues |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109319795A (en) * | 2018-10-18 | 2019-02-12 | 江西星火狮达科技有限公司 | The method of recycling purification silicon powder production silica solution from organosilicon slag |
| CN113699378A (en) * | 2021-08-26 | 2021-11-26 | 枣阳市一鸣化工有限公司 | Treatment method and treatment system for organic silicon waste residues |
-
2016
- 2016-11-28 CN CN201611064181.XA patent/CN106587067A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109319795A (en) * | 2018-10-18 | 2019-02-12 | 江西星火狮达科技有限公司 | The method of recycling purification silicon powder production silica solution from organosilicon slag |
| CN109319795B (en) * | 2018-10-18 | 2020-07-31 | 江西星火狮达科技有限公司 | Method for producing silica sol by recovering and purifying silicon powder from organic silicon slag |
| CN113699378A (en) * | 2021-08-26 | 2021-11-26 | 枣阳市一鸣化工有限公司 | Treatment method and treatment system for organic silicon waste residues |
| CN113699378B (en) * | 2021-08-26 | 2023-09-15 | 枣阳市一鸣化工有限公司 | Method and system for treating organic silicon waste residues |
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Application publication date: 20170426 |
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