CN106115716A - The method purifying silica flour from sinterable silicon waste material - Google Patents
The method purifying silica flour from sinterable silicon waste material Download PDFInfo
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- CN106115716A CN106115716A CN201610476582.XA CN201610476582A CN106115716A CN 106115716 A CN106115716 A CN 106115716A CN 201610476582 A CN201610476582 A CN 201610476582A CN 106115716 A CN106115716 A CN 106115716A
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- waste material
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- silica flour
- sinterable silicon
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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
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a kind of method purifying silica flour from sinterable silicon waste material, it is intended to forming parcel solid solution after solving existing scrap silicon sintering affects the problem that silicon purifies and pollutes environment.Comprise the following steps: that sinterable silicon waste material carries out two-stage successively to be crushed and evacuation grinding, again it is mixed the most in a kettle. with water, and in reactor, add a certain amount of dispersant and antioxidant carries out ultrasonic disperse simultaneously and makes it mix to be uniformly dispersed, it is subsequently adding sulphuric acid and nitric acid and gained material is carried out three grades of vacuumizing filtration process, then gained material is processed high frequency shale shaker sieve pine.Silicon weight/mass percentage composition in sinterable silicon waste material can be brought up to 70% ~ 90%, and gained silica flour good dispersion by 20% ~ 30% by the method, is difficult to reunite, it is to avoid sinterable silicon waste entrainment environment, strong operability of the present invention, is highly suitable for industrial application.
Description
Technical field
The present invention relates to purifying silicon powder technical field, be specifically related to a kind of method purifying silica flour from sinterable silicon waste material.
Background technology
Crystal silicon wafer cutting edge material is the granularity relatively fine carborundum solid micro-powder granule generally between 5～15 μm, quality
Hard and there are sharp corner angle, it is used as the sword material of cutting solar energy crystal silicon chip cell piece, monocrystal silicon and polysilicon are cut into
Sheet.In cutting process, silicon bits are the most cut and are mixed in cutting blade material, and along with the accumulation of silicon bits, cut silicon chip
Cut quality to impact.Currently mainly use the mode of online recycling, the silicon cut bits are separated from cutting blade material.Separate
Silicon is considered to be worth doing by separating and formed silicon crumble garbage in cutting blade material by the mode generally using centrifugation.This silicon crumble is discarded
Between thing granularity is generally between 2～100 μm, particle size range width, and granularity exceedes more than half less than the fine grained accounting of 10 μm.
Owing to granule is tiny, cause its reactivity higher, easily contact concurrent biochemical reaction with the oxygen in air and release heat
Amount, and liberated heat promotes more silicon bits to free exothermic reaction in turn so that the silicon bits garbage after centrifugation
Become sinterable silicon waste material.If this sinterable silicon waste material does not processes as solid waste, will be to soil, water resource and air
Work the mischief, pollute environment.Silicon is as the high metal material of a kind of added value and semi-conducting material, the place to this garbage at present
Reason be concentrated mainly on to wherein rich in the process of silica flour.After composition in this sinterable silicon waste material includes unreacted silicon, reaction
The metal impurities that the silicon dioxide generated, the centrifugal silicon carbide micro-powder being mixed into and wire rod abrasion introduce.But in sintering process
In, silicon carbide micro-powder, bulky grain silicon powder, metal impurities etc. are all fused into one by tiny silicon bits micro powder granule as melt,
Forming so-called parcel, the purification of silicon is caused obstacle by the existence of sintering parcel.How to take measures in this sinterable silicon waste material
Silicon carry out further purification processes, become technical barrier the most urgently to be resolved hurrily.
Summary of the invention
The present invention provides a kind of method from sinterable silicon purifying scrap silica flour, and the melt solving sintering parcel affects silicon purification
Problem.
For solving above-mentioned technical problem, the present invention adopts the following technical scheme that
Design a kind of method purifying silica flour from sinterable silicon waste material, it is characterised in that comprise the following steps:
(1) pending sinterable silicon waste material is carried out coarse crushing via jaw crusher and double-roll crusher respectively and two-stage in small, broken bits is broken
Broken；Then re-use ball mill under conditions of evacuation, carry out vacuum grinding process, obtain the granularity powder body thing less than 100 μm
Material；
(2) material of step (1) gained is mixed and stirred for by the mass ratio of 1:5～20 in a kettle. with water, is formed
Slip；
(3) in the slip of step (2) gained, add dispersant and antioxidant, slip carried out sonic oscillation process simultaneously,
And continue stirring and make it mix to be uniformly dispersed；
(4) adding sulphuric acid and nitric acid again in step (3) gained slip, the mass ratio of added sulphuric acid and nitric acid is 1:1～2, adds
The sulphuric acid added and the total amount of nitric acid are the 5%～10% of sinterable silicon waste material quality；
(5) step (4) gained slip is carried out vacuumizing filtration；
(6) carry out the material of step (5) gained in high frequency shale shaker sieving pine process.
Preferably, in described step (1), the crushing strength of jaw crusher is 250MPa～300MPa；Roller pair breaking
The crushing strength of machine is 200MPa～250MPa.
Preferably, in described step (1), ball mill carries out vacuum under conditions of vacuum is 10000～50000Pa
Grinding processes.
Preferably, water used in described step (2) is deionized water, its electrical conductivity≤1 μ s/cm；Described reactor
For stainless steel cauldron.
Preferably, the dispersant in described step (3) is in sodium hexameta phosphate, sodium metnylene bis-naphthalene sulfonate, maleic anhydride
At least one, its add total amount be the 0.1%～0.2% of sinterable silicon waste material quality；Antioxidant be disodiumedetate,
At least one in sodium hypophosphite, oxamides, its addition is the 0.05%～0.1% of sinterable silicon waste material quality.
Preferably, dispersant used is the mixture of sodium hexameta phosphate, sodium metnylene bis-naphthalene sulfonate and maleic anhydride, and six is inclined
Sodium phosphate: sodium metnylene bis-naphthalene sulfonate: the mass ratio of maleic anhydride is 1～10:1～5:1；Antioxidant used is ethylenediamine tetraacetic
Acetic acid disodium, sodium hypophosphite, the mixture of oxamides, disodiumedetate: sodium hypophosphite: the mass ratio of oxamides
For 1～5:1～3:1.
Preferably, in described step (4), the mass percent concentration of the sulphuric acid of addition is 95%～100%, the quality of nitric acid
Percent concentration is 65%～70%.
Preferably, slip is carried out by described step (5) vacuumizing filtration use continuous way three-stage filtration mode:
First order filtration stage is: only evacuation, the filtrate in slip is filtered, and filters subsequently into the second level；
Second level filtration stage is: carry out shower water washing while evacuation, and the material that the first order filters gained enters one
Step is washed, and regulates its pH value between 6.5～7.5, subsequently into the 3rd pole filtration stage；
3rd pole filtration stage is: stop shower water washing only keep evacuation, make the material solid content of gained reach 90% with
On.
Preferably, described step (5) uses crawler type filter cloth vacuum filter carry out described vacuumizing filtration process, take out
The vacuum that vacuum filters is 1 × 10-3～1 × 10-4Pa；The spray pressure of shower water used by second filtration stage be 50000～
100000Pa。
Preferably, in described step (6), the frequency of vibration of high frequency shale shaker is 3000～5000 beats/min；Sieve mesh
Number is 100～300 mesh.
In technique scheme, step (1) first uses the mode that two-stage crushes step by step, the most first uses the huge of jaw crusher
Bulk sintering parcel scrap silicon is broken into middle piece and fritter by big shear extrusion power, then is broken into fritter by double-roll crusher.
Then the sinterable silicon waste powder of fritter is worn into fine grained, and use the mode of evacuation negative pressure grinding, it is ensured that grinding is often
Carry out under temperature, it is to avoid the tiny silicon powder particle of grinding is heated generation chemical reaction, it is ensured that original materialization of the silicon materials of grinding is special
Property is constant.Step (2) makes grinding gained material be dispersed in liquid phase, and under the effect of the dispersant added in step (3), more
It is evenly dispersed in liquid phase.The addition of antioxidant can suppress tiny silicon powder particle generation oxidation reaction, divides adding
Carry out ultrasonic disperse while powder in a kettle., to realize breaing up further the fine particle being wrapped in, accelerate granule
The effect of rate of dispersion.
Step (4) adds sulphuric acid and nitric acid so that it is with the metal impurities generation chemical oxidation reaction in sinterable silicon waste material, and
Filtered by step (5) vacuum further and realize filtering off filtrate, the washing solvable residue of removal, regulation pH value and improving it
The effect of solid content.Silicon powder sieve after step (6) will be processed by high frequency shale shaker step (5) is loose, it is to avoid it occurs group
Gather and harden.
The Advantageous Effects of the present invention is:
1. the present invention can solve the technical problem that purifying silicon powder is affected by the existence of sintering parcel, is given up by sinterable silicon conveniently and efficiently
Material carries out purification processes, by 20%～30% the silicon weight/mass percentage composition in this sinterable silicon waste material can be brought up to 70%～90%, and
And gained silica flour good dispersion, it is difficult to reunite, avoids the existence of sinterable silicon waste material to pollute environment simultaneously.
2. the invention provides method and the technique purifying silica flour from sinterable silicon waste material, the scrap silicon of parcel sintering is entered
Row silicon purification processes, it is adaptable to purifying silicon powder technical field, it is to avoid sinterable silicon waste entrainment environment, the silica flour purifying gained is difficult to
In reunion, good dispersion；And the method strong operability, convenient and efficient, it is highly suitable for industrial application.
Detailed description of the invention
The detailed description of the invention of the present invention is described below in conjunction with embodiment, but following example are used only to describe in detail
The present invention, and limit the scope of the present invention never in any form.Production equipment involved in following example or detection equipment,
If no special instructions, then it is conventional equipment, involved source chemicals, is the most then commercially available prod.
Embodiment 1: the method purifying silica flour from sinterable silicon waste material, comprises the steps:
(1) pending sinterable silicon waste material is carried out coarse crushing via jaw crusher and double-roll crusher respectively and two-stage in small, broken bits is broken
Broken；Then re-use ball mill under conditions of evacuation, carry out vacuum grinding process, obtain the granularity powder body thing less than 100 μm
Material；Wherein, the crushing strength of jaw crusher is 300MPa；The crushing strength of double-roll crusher is 250MPa.Ball mill is very
Reciprocal of duty cycle is to carry out vacuum grinding process under conditions of 50000Pa, and the position of ball mill evacuation is positioned at the end of ball mill grinding bucket
Center, portion.
(2) deionized water of the material of step (1) gained Yu electrical conductivity≤1 μ s/cm is pressed 1:20 mass ratio at reactor
In be mixed and stirred for, formed slip.
(3) in the slip of step (2) gained, sodium hexametaphosphate dispersant and antioxidant ethylenediaminetetraacetic acid two are added
Sodium, its addition is respectively the 0.2% and 0.1% of sinterable silicon waste material quality, and the ultrasound wave simultaneously opening the installation of reactor still wall is sent out
Raw device, carries out sonic oscillation process to slip, and continues stirring and make it mix to be uniformly dispersed.
(4) in step (3) gained slip, add sulphuric acid and nitric acid again, the mass ratio of added sulphuric acid and nitric acid be 1:1～
2, the sulphuric acid of interpolation and the total amount of nitric acid are the 10% of sinterable silicon waste material quality；Wherein the mass percent concentration of sulphuric acid is 98%,
The mass percent concentration of nitric acid is 67%.
(5) use crawler type filter cloth vacuum filter that step (4) gained slip is carried out vacuumizing filtration, vacuumizing filtration
It is 1 × 10 in vacuum-4Carry out under conditions of Pa；And the mode of described vacuumizing filtration employing continuous way three-stage filtration:
First order filtration stage is: only evacuation, the filtrate in slip is filtered, and filters subsequently into the second level；
Second level filtration stage is: carry out shower water washing while evacuation, and the spray pressure of shower water is 100000Pa,
The material that the first order filters gained washs further, and regulates its pH value between 6.5～7.5, subsequently into the 3rd
Pole filtration stage；
3rd pole filtration stage is: stop shower water washing only keep evacuation, make the material solid content of gained reach 90% with
On.
Step (5) sprays while vacuumizing filtration, it is possible to realize washing and remove solvable residue and regulate
Material pH value, can reduce the usage amount of chemical regulator in production, it is possible to reduce production cost further.
(6) by the material of step (5) gained be 5000 beats/min at frequency of vibration, sieve number be the high frequency of 300 mesh
Vibrosieve is carried out sieve pine process.
Embodiment 2: purifying silica flour according to the same manner as in Example 1 from sinterable silicon waste material, difference is, step
(1) crushing strength of jaw crusher and double-roll crusher is respectively 280MPa and 230MPa, and ball mill in vacuum is
Vacuum grinding process is carried out under conditions of 20000Pa.In step (2), material is 1:10 with the mass ratio of water, used in step (3)
Dispersant and antioxidant are respectively sodium metnylene bis-naphthalene sulfonate and sodium hypophosphite, and its addition is respectively scrap silicon quality
0.15% and 0.08%, in step (5), the vacuum of vacuumizing filtration is 0.5 × 10-4Pa；Shower water used by second filtration stage
Spray pressure be 80000Pa.The frequency of vibration of the high frequency shale shaker in step (6) is 4000 beats/min, sieve number is
200 mesh.
Embodiment 3: purifying silica flour according to the same manner as in Example 2 from sinterable silicon waste material, difference is, step
(3) dispersant and antioxidant used by are respectively maleic anhydride and oxamides, and its addition is respectively scrap silicon quality
0.12% and 0.07%.
Embodiment 4: purifying silica flour according to the same manner as in Example 1 from sinterable silicon waste material, difference is, step
(3) dispersant and antioxidant used by are respectively sodium hexameta phosphate and sodium hypophosphite, and its addition is respectively scrap silicon matter
The 0.13% and 0.09% of amount.
Embodiment 5: purifying silica flour according to the same manner as in Example 1 from sinterable silicon waste material, difference is, step
(3) dispersant and antioxidant used by are respectively sodium hexameta phosphate and oxamides, and its addition is respectively scrap silicon quality
0.12% and 0.08%.
Embodiment 6: purifying silica flour according to the same manner as in Example 2 from sinterable silicon waste material, difference is, step
(3) dispersant and antioxidant used by are respectively sodium metnylene bis-naphthalene sulfonate and disodiumedetate, and its addition divides
Not Wei scrap silicon quality 0.14% and 0.09%.
Embodiment 7: purifying silica flour according to the same manner as in Example 2 from sinterable silicon waste material, difference is, step
(3) dispersant and antioxidant used by are respectively sodium metnylene bis-naphthalene sulfonate and oxamides, and its addition is respectively scrap silicon
The 0.11% and 0.06% of quality.
Embodiment 8: purifying silica flour according to the same manner as in Example 2 from sinterable silicon waste material, difference is, step
(3) dispersant and antioxidant used by are respectively maleic anhydride and disodiumedetate, and its addition is respectively silicon and gives up
The 0.13% and 0.08% of material quality.
Embodiment 9: purifying silica flour according to the same manner as in Example 2 from sinterable silicon waste material, difference is, step
(3) dispersant and antioxidant used by are respectively maleic anhydride and sodium hypophosphite, and its addition is respectively scrap silicon quality
0.12% and 0.09%.
Embodiment 10: purifying silica flour according to the same manner as in Example 2 from sinterable silicon waste material, difference is, step
Suddenly the dispersant used by (3) is the mixture of sodium hexameta phosphate, sodium metnylene bis-naphthalene sulfonate, maleic anhydride, the mass ratio of three
For 8:5:1；Antioxidant is the mixture of disodiumedetate, sodium hypophosphite, oxamides, and the mass ratio of three is 3:
2:1, mixture dispersant is respectively the 0.2% and 0.07% of scrap silicon quality with the addition of mixture antioxidant.
Method in the present invention carries out purifying silicon powder from sinterable silicon waste material, it is possible to resolve the existence of sintering parcel is to silicon
Powder purifies the technical problem of impact, conveniently and efficiently sinterable silicon waste material is carried out purification processes, can be by this sinterable silicon waste material
Silicon weight/mass percentage composition is brought up to 70%～90% by 20%～30%, and its solid content reaches more than 90%, and gained silica flour dispersibility
Good, it is difficult to reunite, avoids the existence of sinterable silicon waste material to pollute environment simultaneously, and strong operability of the present invention, it is highly suitable for work
Industry popularization and application.
The present invention is capable of the effective recycling to sinterable silicon waste material, can be by reluctant sintering parcel scrap silicon
It carries out purification processes, and the material particularly relevant performance indications data before and after process are as shown in table 1 below.
Above in conjunction with embodiment, the present invention is described in detail, but, person of ordinary skill in the field can
Understand, on the premise of without departing from present inventive concept, it is also possible to each design parameter in above-described embodiment is changed, shape
Become multiple specific embodiment, be the common excursion of the present invention, describe in detail the most one by one at this.
Claims (10)
1. the method purifying silica flour from sinterable silicon waste material, it is characterised in that comprise the following steps:
(1) pending sinterable silicon waste material is carried out coarse crushing via jaw crusher and double-roll crusher respectively and two-stage in small, broken bits is broken
Broken；Then re-use ball mill under conditions of evacuation, carry out vacuum grinding process, obtain the granularity powder body thing less than 100 μm
Material；
(2) material of step (1) gained is mixed and stirred for by the mass ratio of 1:5～20 in a kettle. with water, is formed
Slip；
(3) in the slip of step (2) gained, add dispersant and antioxidant, slip carried out sonic oscillation process simultaneously,
And continue stirring and make it mix to be uniformly dispersed；
(4) adding sulphuric acid and nitric acid again in step (3) gained slip, the mass ratio of added sulphuric acid and nitric acid is 1:1～2, adds
The sulphuric acid added and the total amount of nitric acid are the 5%～10% of sinterable silicon waste material quality；
(5) step (4) gained slip is carried out vacuumizing filtration；
(6) carry out the material of step (5) gained in high frequency shale shaker sieving pine process.
The method purifying silica flour from sinterable silicon waste material the most according to claim 1, it is characterised in that in described step
(1), in, the crushing strength of jaw crusher is 250MPa～300MPa；The crushing strength of double-roll crusher be 200MPa～
250MPa。
The method purifying silica flour from sinterable silicon waste material the most according to claim 1, it is characterised in that in described step
(1), in, ball mill carries out vacuum grinding process under conditions of vacuum is 10000～50000Pa.
The method purifying silica flour from sinterable silicon waste material the most according to claim 1, it is characterised in that in described step
(2) water used in is deionized water, its electrical conductivity≤1 μ s/cm；Described reactor is stainless steel cauldron.
The method purifying silica flour from sinterable silicon waste material the most according to claim 1, it is characterised in that described step (3)
In dispersant be at least one in sodium hexameta phosphate, sodium metnylene bis-naphthalene sulfonate, maleic anhydride, its add total amount for sintering
The 0.1%～0.2% of scrap silicon quality；Antioxidant is at least in disodiumedetate, sodium hypophosphite, oxamides
Kind, its addition is the 0.05%～0.1% of sinterable silicon waste material quality.
The method purifying silica flour from sinterable silicon waste material the most according to claim 5, it is characterised in that dispersant used is
The mixture of sodium hexameta phosphate, sodium metnylene bis-naphthalene sulfonate and maleic anhydride, the mass ratio of three is 1～10:1～5:1；Used
Antioxidant is the mixture of disodiumedetate, sodium hypophosphite, oxamides, the mass ratio of three be 1～5:1～
3:1.
The method purifying silica flour from sinterable silicon waste material the most according to claim 1, it is characterised in that described step (4)
In, the mass percent concentration of the sulphuric acid of addition is 95%～100%, and the mass percent concentration of nitric acid is 65%～70%.
The method purifying silica flour from sinterable silicon waste material the most according to claim 1, it is characterised in that described step (5)
In slip carried out vacuumizing filtration use the mode of continuous way three-stage filtration:
First order filtration stage is: only evacuation, the filtrate in slip is filtered, and filters subsequently into the second level；
Second level filtration stage is: carry out shower water washing while evacuation, and the material that the first order filters gained enters one
Step is washed, and regulates its pH value between 6.5～7.5, subsequently into the 3rd pole filtration stage；
3rd pole filtration stage is: stop shower water washing only keep evacuation, make the material solid content of gained reach 90% with
On.
The method purifying silica flour from sinterable silicon waste material the most according to claim 8, it is characterised in that described step (5)
Middle employing crawler type filter cloth vacuum filter carries out described vacuumizing filtration process, and the vacuum of vacuumizing filtration is 1 × 10-3~
1×10-4Pa；The spray pressure of shower water used by second filtration stage is 50000～100000Pa.
The method purifying silica flour from sinterable silicon waste material the most according to claim 1, it is characterised in that in described step
(6), in, the frequency of vibration of high frequency shale shaker is 3000～5000 beats/min；Sieve number is 100～300 mesh.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108675305A (en) * | 2018-05-26 | 2018-10-19 | 河南易成新能源股份有限公司 | A method of preparing HIGH-PURITY SILICON with silicon carbide sliced crystal silicon waste mortar |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104512894A (en) * | 2013-09-27 | 2015-04-15 | 东莞市长安东阳光铝业研发有限公司 | Treatment method of silicon block |
| CN105523557A (en) * | 2016-02-14 | 2016-04-27 | 东北大学 | Method for recycling waste slurry produced during diamond wire cutting of crystalline silicon |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104512894A (en) * | 2013-09-27 | 2015-04-15 | 东莞市长安东阳光铝业研发有限公司 | Treatment method of silicon block |
| CN105523557A (en) * | 2016-02-14 | 2016-04-27 | 东北大学 | Method for recycling waste slurry produced during diamond wire cutting of crystalline silicon |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108675305A (en) * | 2018-05-26 | 2018-10-19 | 河南易成新能源股份有限公司 | A method of preparing HIGH-PURITY SILICON with silicon carbide sliced crystal silicon waste mortar |
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