CN108285147A - The method that high-purity silicon powder is extracted from crystalline silicon mortar cutting waste material - Google Patents
The method that high-purity silicon powder is extracted from crystalline silicon mortar cutting waste material Download PDFInfo
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- CN108285147A CN108285147A CN201810247293.1A CN201810247293A CN108285147A CN 108285147 A CN108285147 A CN 108285147A CN 201810247293 A CN201810247293 A CN 201810247293A CN 108285147 A CN108285147 A CN 108285147A
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- waste material
- cutting waste
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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
- C01B33/037—Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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Abstract
The invention discloses a kind of methods that high-purity silicon powder is extracted in mortar cutting waste material from crystalline silicon.It the described method comprises the following steps：Nitration mixture medium is added into crystalline silicon mortar cutting waste material, is stirred, then heats to 50 DEG C~70 DEG C and continue to stir, carries out solid-liquor separation, obtained solid part is dried, solid material is obtained；Aqueous dispersion medium is added into the solid material, is stirred, obtains slurry；The slurry is sent into cyclone and carries out cyclonic separation, solid-liquor separation is carried out to the product that overflow goes out, solids is obtained, the solids is dried；Dense media is added in products therefrom after to drying, is made into dense media slurry；The dense media slurry is sent into cyclone and carry out cyclonic separation, the part gone out to overflow carries out solid-liquor separation, by obtained solid be dried to get.Easy to operate, good separating effect of the invention, can continuous production, production efficiency is high, and extracted silica flour purity height.
Description
Technical field
The present invention relates to crystalline silicon mortar cutting waste material recovery technology fields, and in particular to a kind of to be cut from crystalline silicon mortar
The method that high-purity silicon powder is extracted in waste material.
Background technology
With the increasingly reduction of the non-renewable energy resources such as coal, oil, reproducible solar energy is increasingly becoming a kind of important
The energy, wherein for crystalline silicon as the most important photoelectric material of solar cell is prepared, strategic resource status is increasingly apparent.With
When crystalline silicon prepares solar cell, needs crystalline silicon ingot casting, cuts into silicon chip.Crystalline silicon cutting mainly have mortar cutting and
Buddha's warrior attendant wire cutting two ways will produce a large amount of crystal silicon cutting waste materials in cutting process.Wherein mortar cutting is mainly using by carbon
The mortar of SiClx micro mist and polyethylene glycol composition carries out steel wire cutting, and there are about 40%~50% crystalline silicons to enter sand in cutting process
It starches in cutting waste material.There are silica flour, polyethylene glycol and silicon carbide with recovery value in the mortar cutting waste material, at present from mortar
Polyethylene glycol is recycled in cutting waste material and the technology of silicon carbide is ripe, and it is useless that the country there are many enterprises that mortar cutting may be implemented
The regeneration of polyethylene glycol and silicon carbide in material.However, for the silica flour in mortar cutting waste material or mortar regeneration tailing still without having
The recovery method of effect.
With the improvement of cutting technique, mortar cutting is gradually replaced by Buddha's warrior attendant wire cutting.However, being cut by mortar
And the waste material generated has had accumulated nearly million tons in the whole nation, causes hundred billion yuan of HIGH-PURITY SILICON economic loss；In addition, what a large amount of heaps were abandoned
Crystal silicon cutting waste material also occupies a large amount of soil money and polluted environment.Therefore, recycling profit is carried out to crystal silicon cutting waste material
With and recycling HIGH-PURITY SILICON have huge economy and environmental benefit.
Chinese patent CN201110041395.6 is disclosed a kind of detaching the silicon in crystal silicon cutting waste material by electrophoresis
With silicon carbide, the difference of silicon and silicon carbide isoelectric point is utilized in the patent, controls silica flour under electric field environment and carborundum powder exists
It floats or sinks in heavy-fluid suspension, and silica flour and carborundum powder are collected in electrophoresis slot tail different zones.But due to silicon and
Silicon carbide isoelectric point is close, therefore the method action pane in the technical solution is relatively narrow and uncontrollable.
Chinese patent CN201210060027.0 discloses one kind and is detached in crystal silicon cutting waste material by foam flotation method
Silicon and silicon carbide, wherein using lipid nonionic collecting agent, using lauryl sodium sulfate or neopelex
For foaming agent.Since silica flour and carborundum powder surface physico-chemical property are close, and silicon particle size is too thin, therefore foam in separation process
Entrainment phenomenon is serious, and separating effect is general.
Patent document TW1392647B1 disclose a kind of method by phase separation detach silicon in crystal silicon cutting waste material with
Silicon carbide, this method are filled using the hydrophily of the hydrophobicity and silica flour of carborundum powder in oil water mixture and crystal silicon cutting waste material
After touch, silica flour enters water phase to tap, carborundum powder enters oil phase and silicon and silicon carbide is made to detach.However this method needs very
Big liquid-solid ratio, and be intermittently operated, therefore production efficiency and production capacity are all very low.
Cyclone is a kind of continuous separation device, and production capacity is big, is suitable for industrial production.However, the present inventor studies
It was found that since the grain size of a large amount of SiC in cutting waste material and the grain size of Si are close, cannot get using conventional hydraulic cyclone
High-purity silicon powder；Although a kind of silicon carbide micro-powder eddy flow method of purification, Yi Jizhong disclosed in Chinese patent CN201410101220.3
A kind of silicon chip waste mortar for wire cutting separation combined-type cyclone, all uses disclosed in state patent document CN201520572495.5
Si and SiC in hydrocyclone separation technology crystal silicon cutting waste material, but can only isolate the larger SiC micro mists of granularity, and SiC
Impurity content is high, further cannot obtain HIGH-PURITY SILICON by refining.
Invention content
It is easily manipulated the technical problem to be solved in the present invention is to provide a kind of, can continuously detach the crystal silica sand of silicon carbide
The method that high-purity silicon powder is extracted in cutting waste material is starched, to solve the separating effect of silicon carbide and silicon in current crystal silicon cutting waste material
Difference, low production efficiency and it is complicated for operation the problems such as.
Inventor the study found that from crystal silicon cutting waste material recycling prepare HIGH-PURITY SILICON key be to be sufficiently separated silica flour and
Carborundum powder obtains high-purity silicon powder, however, since a large amount of carborundum powders in crystal silicon cutting waste material are close with the granularity of silica flour,
And chemical property is stablized than silicon, therefore separation silicon carbide is extremely difficult from crystal silicon cutting waste material.
The present invention uses dense media eddy flow, by inhibiting silica flour sedimentation to be imitated to further increase the separation of silicon and silicon carbide
Rate can effectively obtain the high-purity silicon powder that SiC content is less than 3 wt%, meanwhile, pass through the recycling such as solid-liquor separation, rectifying, evaporative crystallization
Dense media is suitble to industrial mass production recycling.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：
A kind of method for extracting high-purity silicon powder in the mortar cutting waste material from crystalline silicon is designed, is included the following steps：
（1）Nitration mixture medium is added into crystalline silicon mortar cutting waste material, is stirred, then heats to 50 DEG C~70 DEG C and continue to stir
It mixes, carries out solid-liquor separation, obtained solid part is dried, solid material is obtained；
（2）To step（1）Aqueous dispersion medium is added in middle obtained solid material, is stirred, obtains slurry；
（3）By step（2）Middle gained slurry is sent into cyclone and carries out cyclonic separation, and carry out liquid to the product that overflow goes out divides admittedly
From obtaining solids, the solids be dried；
（4）To step（3）Dense media is added in products therefrom after middle drying, is made into dense media slurry；
（5）By step（4）Middle gained dense media slurry is sent into cyclone and carries out cyclonic separation, and liquid is carried out to the part that overflow goes out
Gu separation, by obtained solid be dried to get.
Preferably, in the step（1）In, the nitration mixture medium is hydrofluoric acid and at least one in hydrochloric acid, sulfuric acid, nitric acid
Kind, wherein a concentration of wt% of 0 wt%~5 of the hydrofluoric acid；The wt% of a concentration of 5wt%~20 of hydrochloric acid；Sulfuric acid it is a concentration of
The wt% of 20 wt%~65；A concentration of wt% of 15 wt%~70 of nitric acid.
Preferably, in the step（1）In, in the stirring at 50 DEG C~70 DEG C, mixing time is 2~5 h.
Preferably, in the step（2）In, the aqueous dispersion medium is waterglass, calgon, sodium tripolyphosphate
At least one of with sodium pyrophosphate, wherein ‰~1 wt ‰ of a concentration of 0.05 wt of the waterglass；Calgon
‰~1 wt ‰ of a concentration of 0.1 wt；‰~1 wt ‰ of a concentration of 0.05 wt of sodium tripolyphosphate；Sodium pyrophosphate it is a concentration of
0.1 wt, ‰~0.5 wt ‰.
Preferably, in the step（2）In, the rate of the stirring is 300~1000r/min, and the mixing time is
10~30 minutes.
Preferably, in the step（2）In, the mass ratio of the solid material and slurry is 4%~15%.
Preferably, in the step（3）In, the inlet pressure of the cyclone is 0.4~0.6 MPa, cyclone diameter
For 10~25mm.
Preferably, in the step（4）In, the dense media be bromoform, tetrabromoethane, more sodium tungstates, zinc chloride,
At least one of calcium chloride, potassium iodide, mercuric iodixde.
Preferably, in the step（5）In, the partition size d of the cyclone95Control is 3~5 microns.
Compared with prior art, the beneficial technical effect of the present invention lies in：
1. the silica flour purity that the method for the present invention to the good separating effect of silicon carbide and silica flour, is extracted is high.
2. the method for the present invention is easy to operate, can continuous production, and production efficiency is high.
3. dense media used, can be through modes such as pervaporation, rectifying, crystallizations again after solid-liquor separation in the method for the present invention
It is raw, further save production cost.
Description of the drawings
Fig. 1 is a kind of XRD diagram of the extracted high-purity silicon powder of specific embodiment of the present invention.
Specific implementation mode
Illustrate the specific implementation mode of the present invention with reference to the accompanying drawings and examples, but following embodiment is used only in detail
It describes the bright present invention in detail, does not limit the scope of the invention in any way.
Involved instrument and equipment is routine instrument device unless otherwise instructed in the examples below；Involved
Material and reagent are purchased from conventional chemical reagent shop unless otherwise instructed；Involved test, preparation method, such as without especially
Illustrate, is conventional method.
The method that high-purity silicon powder is extracted in a kind of mortar cutting waste material from crystalline silicon of embodiment 1, specially：
（1）50 L of hydrochloric acid of mortar cutting waste material 10 kg and 10 wt% are mixed, stirred under the mixing speed of 300 r/min
30 min；Then temperature is risen to 50 DEG C, continues to stir 3h, solid-liquor separation is then carried out by plate and frame filter press, drying obtains
6.2 kg of solid material, wherein SiC content are 54 wt%.
（2）To step（1）Tap water 80 L, calgon 20g are added in obtained solid material, in 300 r/
30 min are stirred under the mixing speed of min, the slurry after being disperseed.
（3）By step（2）Obtained slurry, which is driven into cyclone, carries out hydrocyclone separation technology, the cyclone inlets
Pressure is 0.6 MPa, cyclone diameter 25mm；The product that overflow is gone out carries out solid-liquor separation by plate and frame filter press, by liquid
Gu obtained solid is dried after separation, 2.7 kg of solid material is obtained；Wherein SiC content is 18 wt%.
（4）To step（3）Bromoform 39kg, ethyl alcohol 19kg are added in obtained solid material, carries out ball milling to fill
Dispersion, obtains dense media slurry；
（5）By step（4）Obtained dense media slurry, which is driven into cyclone, carries out hydrocyclone separation technology, cyclone inlets pressure
Power is 0.3 MPa, cyclone partition size d95It is 5 microns；The product that overflow is gone out carries out solid-liquor separation, by institute after solid-liquor separation
It obtains solid to be dried, obtains 1.8 kg of high-purity silicon powder that purity is 97.7%, wherein SiC content is 2.2 wt%.
The method that high-purity silicon powder is extracted in a kind of mortar cutting waste material from crystalline silicon of embodiment 2, detailed step are as follows：
（1）40 L of sulfuric acid of mortar cutting waste material 10 kg and 20 wt% are mixed, stirred under the mixing speed of 300 r/min
30 min；Then temperature is risen to 65 DEG C, continues to stir 4h, solid-liquor separation is then carried out by plate and frame filter press, drying obtains
7.8 kg of solid material, wherein SiC content are 28 wt%.
（2）To step（1）Tap water 100 L, waterglass 30g are added in obtained solid material, in 1000 r/min
Mixing speed under stir 30 min, the slurry after being disperseed.
（3）By step（2）Obtained slurry, which is driven into cyclone, carries out hydrocyclone separation technology, the cyclone inlets
Pressure is 0.45 MPa, cyclone diameter 10mm；The product that overflow is gone out carries out solid-liquor separation by plate and frame filter press, by liquid
Gu obtained solid is dried after separation, 3.7 kg of solid material is obtained；Wherein SiC content is 9 wt%.
（4）To step（3）A concentration of 80% 80 kg of poly- sodium tungstate solution is added in obtained solid material, using height
After fast dispersion machine progress is fully dispersed, dense media slurry is obtained；
（5）By step（4）Obtained dense media slurry, which is driven into cyclone, carries out hydrocyclone separation technology, cyclone inlets pressure
Power is 0.3 MPa, cyclone partition size d95It is 3 microns；The product that overflow is gone out carries out solid-liquor separation, by institute after solid-liquor separation
It obtains solid to be dried, obtains 2.6 kg of high-purity silicon powder that purity is 98%, wherein SiC content is 1.9 wt%.
The present invention is described in detail above in conjunction with drawings and examples, still, those of skill in the art
Member is it is understood that without departing from the purpose of the present invention, can also carry out each design parameter in above-described embodiment
Change, forms multiple specific embodiments, is the common variation range of the present invention, is no longer described in detail one by one herein.
Claims (9)
1. a kind of method for extracting high-purity silicon powder in mortar cutting waste material from crystalline silicon, which is characterized in that include the following steps：
（1）Nitration mixture medium is added into crystalline silicon mortar cutting waste material, is stirred, then heats to 50 DEG C~70 DEG C and continue to stir
It mixes, carries out solid-liquor separation, obtained solid part is dried, solid material is obtained；
（2）To step（1）Aqueous dispersion medium is added in middle obtained solid material, slurry is obtained after stirring evenly；
（3）By step（2）Middle gained slurry is sent into cyclone and carries out cyclonic separation, and carry out liquid to the product that overflow goes out divides admittedly
From obtaining solids, the solids be dried；
（4）To step（3）Dense media is added in products therefrom after middle drying, is made into dense media slurry；
（5）By step（4）Middle gained dense media slurry is sent into cyclone and carries out cyclonic separation, and liquid is carried out to the part that overflow goes out
Gu separation, by obtained solid be dried to get.
2. the method for extracting high-purity silicon powder in the mortar cutting waste material according to claim 1 from crystalline silicon, feature exist
In in the step（1）In, the nitration mixture medium is at least one of hydrofluoric acid and hydrochloric acid, sulfuric acid, nitric acid, wherein described
A concentration of wt% of 0.5 wt%~5 of hydrofluoric acid；The wt% of a concentration of 5wt%~20 of hydrochloric acid；A concentration of 20 wt%~65 of sulfuric acid
wt%；A concentration of wt% of 15 wt%~70 of nitric acid.
3. the method for extracting high-purity silicon powder in the mortar cutting waste material according to claim 1 from crystalline silicon, feature exist
In in the step（1）In, 2~5 h are stirred at 50 DEG C~70 DEG C.
4. the method for extracting high-purity silicon powder in the mortar cutting waste material according to claim 1 from crystalline silicon, feature exist
In in the step（2）In, the aqueous dispersion medium is in waterglass, calgon, sodium tripolyphosphate and sodium pyrophosphate
At least one, wherein ‰~1 wt ‰ of a concentration of 0.05 wt of the waterglass；A concentration of the 0.1 of calgon
‰~1 wt ‰ of wt；‰~1 wt ‰ of a concentration of 0.05 wt of sodium tripolyphosphate；A concentration of 0.1 wt ‰ of sodium pyrophosphate~
0.5 wt‰。
5. the method for extracting high-purity silicon powder in the mortar cutting waste material according to claim 1 from crystalline silicon, which is characterized in that
In the step（2）In, the rate of the stirring is 300~1000r/min, and the mixing time is 10~30 minutes.
6. the method for extracting high-purity silicon powder in the mortar cutting waste material according to claim 1 from crystalline silicon, which is characterized in that
In the step（2）In, the mass ratio of the solid material and slurry is 4%~15%.
7. the method for extracting high-purity silicon powder in the mortar cutting waste material according to claim 1 from crystalline silicon, feature exist
In in the step（3）In, the inlet pressure of the cyclone is 0.4~0.6 MPa, and cyclone diameter is 10~25mm.
8. the method for extracting high-purity silicon powder in the mortar cutting waste material according to claim 1 from crystalline silicon, which is characterized in that
In the step（4）In, the dense media be bromoform, tetrabromoethane, more sodium tungstates, zinc chloride, calcium chloride, potassium iodide,
At least one of mercuric iodixde.
9. the method for extracting high-purity silicon powder in the mortar cutting waste material according to claim 1 from crystalline silicon, which is characterized in that
In the step（5）In, the partition size d of the cyclone95Control is 3~5 microns.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108298545A (en) * | 2017-01-11 | 2018-07-20 | 中国科学院过程工程研究所 | Utilize the method for sulfuric acid and metal chloride medium de_ironing refinement quartz sand |
| CN111822154A (en) * | 2020-07-30 | 2020-10-27 | 济南大学 | Method for floating silicon from silicon slag |
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| CN101792142A (en) * | 2009-12-31 | 2010-08-04 | 唐康宁 | Method for recovering polysilicon ingots, carborundum powder and polyethylene glycol from cutting waste mortar |
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| CN108298545A (en) * | 2017-01-11 | 2018-07-20 | 中国科学院过程工程研究所 | Utilize the method for sulfuric acid and metal chloride medium de_ironing refinement quartz sand |
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| CN111822154B (en) * | 2020-07-30 | 2023-10-13 | 济南大学 | Method for floating silicon from silicon slag |
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Application publication date: 20180717 |