CN106115716B - The method that silica flour is purified from sintering scrap silicon - Google Patents
The method that silica flour is purified from sintering scrap silicon Download PDFInfo
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- CN106115716B CN106115716B CN201610476582.XA CN201610476582A CN106115716B CN 106115716 B CN106115716 B CN 106115716B CN 201610476582 A CN201610476582 A CN 201610476582A CN 106115716 B CN106115716 B CN 106115716B
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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 methods that silica flour is purified in scrap silicon from sintering, it is intended to which formation package solid solution influences silicon purification and pollution environment after solving the problems, such as existing scrap silicon sintering.Include the following steps：Sintering scrap silicon is subjected to two-stage successively and is crushed and vacuumizes grinding, it is mixed in a kettle in proportion with water again, and a certain amount of dispersant is added into reaction kettle and antioxidant is carried out at the same time ultrasonic disperse and its mixing is made to be uniformly dispersed, then sulfuric acid and nitric acid is added and resulting material is subjected to three-level vacuumizing filtration processing, then resulting material is sieved into pine processing in high frequency shale shaker.The silicon mass percentage being sintered in scrap silicon can be increased to 70% ~ 90%, and gained silica flour good dispersion by this method by 20% ~ 30%, be not easy to reunite, sinterable silicon waste entrainment environment, strong operability of the present invention is avoided to be highly suitable for industrial application.
Description
Technical field
The present invention relates to purifying silicon powder technical fields, and in particular to a method of purifying silica flour from sintering scrap silicon.
Background technology
Crystal silicon wafer cutting edge material is granularity generally between 5~15 μm of relatively fine silicon carbide solid micro-powder particle, quality
It is hard and have sharp corner angle, be used as cutting solar energy crystal silicon chip cell piece sword material, monocrystalline silicon and polysilicon are cut into
Piece.In cutting process, silicon bits are constantly cut and are mixed into cutting blade material, and with the accumulation that silicon is considered to be worth doing, are cut to silicon chip
Quality is cut to impact.It is main by the way of online recycling at present, the silicon cut bits are separated from cutting blade material.Separation
The mode that generally use centrifuges considers silicon by silicon crumble waste is separated and formed in cutting blade material to be worth doing.The silicon crumble is discarded
For object granularity generally between 2~100 μm, particle size range is wide, and fine grained accounting of the granularity less than 10 μm is more than more than half.
It since particle is tiny, causes its reactivity higher, concurrent biochemical reaction is easily contacted with the oxygen in air and releases heat
Amount, and the heat released promotes more silicon bits to free exothermic reaction in turn so that the silicon after centrifugation considers waste to be worth doing
Become to be sintered scrap silicon.If the sintering scrap silicon as solid waste without processing, will be to soil, water resource and air
It causes damages, pollutes environment.Silicon is as a kind of metal material and semi-conducting material that added value is high, at present to the place of the waste
Reason is concentrated mainly on the processing of the silica flour to being wherein rich in.After ingredient in the sintering scrap silicon includes unreacted silicon, reaction
The metal impurities that silica, the mixed silicon carbide micro-powder of centrifugation and the wire rod abrasion of generation introduce.However in sintering process
In, tiny silicon bits micro powder granule fuses into one silicon carbide micro-powder, bulky grain silicon powder, metal impurities etc. as melt,
So-called package is formed, the presence for being sintered package causes obstacle to the purification of silicon.How to take measures in the sintering scrap silicon
Silicon carry out further purification processes, become technical barrier urgently to be resolved hurrily at present.
Invention content
The present invention provides a kind of method from sinterable silicon purifying scrap silica flour, solves the melt of sintering package and influences silicon purification
The problem of.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：
It designs a kind of from the method for being sintered purification silica flour in scrap silicon, which is characterized in that include the following steps：
（1）Pending sintering scrap silicon is subjected to coarse crushing and fine crushing two via jaw crusher and double-roll crusher respectively
Grade is broken；Then it reuses ball mill and carries out vacuum grinding processing under conditions of vacuumizing, obtain the powder that granularity is less than 100 μm
Body material；
（2）By step（1）The material of gained presses 1 with water:5~20 mass ratio is mixed and stirred in a kettle,
Form slurry；
（3）To step（2）Dispersant and antioxidant are added in the slurry of gained, while slurry is carried out at sonic oscillation
Reason, and continuing stirring makes its mixing be uniformly dispersed；
（4）Again to step（3）The mass ratio of addition sulfuric acid and nitric acid in gained slurry, added sulfuric acid and nitric acid is 1:1~
2, the sulfuric acid of addition and the total amount of nitric acid are be sintered scrap silicon quality 5%~10%；
（5）By step（4）Gained slurry carries out vacuumizing filtration；
（6）By step（5）The material of gained carries out sieving loose processing in high frequency shale shaker.
Preferably, in the step（1）In, the breaking strength of jaw crusher is 250MPa~300MPa；Roller pair breaking
The breaking strength of machine is 200MPa~250MPa.
Preferably, in the step（1）In, ball mill carries out vacuum under conditions of vacuum degree is 10000~50000Pa
Grinding processing.
Preferably, in the step（2）Used in water be deionized water, the μ s/cm of conductivity≤1；The reaction kettle
For stainless steel cauldron.
Preferably, the step（3）In dispersant be calgon, sodium metnylene bis-naphthalene sulfonate, in maleic anhydride
At least one, total amount of adding be sintered scrap silicon quality 0.1%~0.2%；Antioxidant be disodium ethylene diamine tetraacetate,
At least one of sodium hypophosphite, oxamides, additive amount are be sintered scrap silicon quality 0.05%~0.1%.
Preferably, dispersant used is the mixture of calgon, sodium metnylene bis-naphthalene sulfonate and maleic anhydride, and six partially
Sodium phosphate：Sodium metnylene bis-naphthalene sulfonate：The mass ratio of maleic anhydride is 1~10：1~5：1；Antioxidant used is ethylenediamine tetraacetic
The mixture of acetic acid disodium, sodium hypophosphite, oxamides, disodium ethylene diamine tetraacetate：Sodium hypophosphite：The mass ratio of oxamides
For 1~5：1~3：1.
Preferably, the step（4）In, the mass percent concentration of the sulfuric acid of addition is 95%~100%, the quality of nitric acid
Percent concentration is 65%~70%.
Preferably, the step（5）In to slurry carry out vacuumizing filtration by the way of continous way three-stage filtration：
First order filtration stage is：It only vacuumizes, the filtrate in slurry is filtered out, filtered subsequently into the second level；
Second level filtration stage is：Shower water washing is carried out while vacuumizing, by the material of first order filtering gained
It is further washed, and adjusts its pH value between 6.5~7.5, subsequently into third pole filtration stage；
Third pole filtration stage is：Stop shower water washing only to keep vacuumizing, the material solid content of gained is made to reach 90%
More than.
Preferably, the step（5）It is middle that the vacuumizing filtration process is carried out using crawler type filter cloth vacuum filter, it takes out
The vacuum degree of vacuum filter is 1 × 10-3~1 × 10-4Pa；The spray pressure of shower water used in second filtration stage be 50000~
100000Pa。
Preferably, in the step（6）In, the vibration frequency of high frequency shale shaker is 3000~5000 beats/min；Sieve mesh
Number is 100~300 mesh.
In the above-mentioned technical solutions, step（1）First in such a way that two-stage is crushed step by step, i.e., first use the huge of jaw crusher
Bulk is sintered package scrap silicon and 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 by the way of vacuumizing negative pressure grinding, ensures grinding normal
Temperature is lower to be carried out, and avoids the tiny silicon powder particle of grinding is heated from chemically reacting, and ensures that original materialization of the silicon materials of grinding is special
Property is constant.Step（2）Make the dispersion of grinding resulting material in the liquid phase, and in step（3）Under the action of the dispersant of addition, more
It is evenly dispersed in liquid phase.Oxidation reaction occurs for the silicon powder particle that the addition of antioxidant can inhibit tiny, divides being added
Ultrasonic disperse is carried out while powder in a kettle, the fine particle being wrapped in further is broken up to realize, accelerates particle
The effect of rate of dispersion.
Step（4）Sulfuric acid and nitric acid is added, makes it that chemical oxidation reaction occur with the metal impurities in sintering scrap silicon, and
Further pass through step（5）Vacuum filter filters off filtrate, the solvable residue of washing removal, adjusts pH value and improves it to realize
The effect of solid content.Step（6）High frequency shale shaker step will be passed through（5）Treated, and silicon powder sieve is loose, avoids it that group occurs
It is poly- hardened.
The beneficial technical effect of the present invention lies in：
1. the present invention can solve sintering package there is technical issues that purifying silicon powder, conveniently and efficiently will be sintered
Scrap silicon carries out purification processes, the silicon mass percentage in the sintering scrap silicon can be increased to 70% by 20%~30%~
90%, and gained silica flour good dispersion, it is not easy to reunite, while avoiding the presence pollution environment of sintering scrap silicon.
2. the present invention provides from sintering scrap silicon in purify silica flour method and technique, to package sintering scrap silicon into
Row silicon purification processes are suitable for purifying silicon powder technical field, avoid sinterable silicon waste entrainment environment, and the silica flour for purifying gained is not easy
In reunion, good dispersion；And this method strong operability, convenient and efficient are highly suitable for industrial application.
Specific implementation mode
Illustrate the specific implementation mode of the present invention with reference to embodiment, but following embodiment is used only to be described in detail
The present invention does not limit the scope of the invention in any way.Involved production equipment or detection device in following embodiment,
Unless otherwise instructed, then it is conventional equipment, involved source chemicals are then commercial product unless otherwise instructed.
Embodiment 1：The method that silica flour is purified from sintering scrap silicon, includes the following steps：
（1）Pending sintering scrap silicon is subjected to coarse crushing and fine crushing two via jaw crusher and double-roll crusher respectively
Grade is broken；Then it reuses ball mill and carries out vacuum grinding processing under conditions of vacuumizing, obtain the powder that granularity is less than 100 μm
Body material；Wherein, the breaking strength of jaw crusher is 300MPa；The breaking strength of double-roll crusher is 250MPa.Ball mill
Vacuum grinding processing is carried out under conditions of vacuum degree is 50000Pa, the position that ball mill vacuumizes is located at ball mill grinding bucket
End center.
（2）By step（1）The deionized water of the μ s/cm of the material of gained and conductivity≤1 presses 1:20 mass ratioes are in reaction kettle
In be mixed and stirred for, formed slurry.
（3）To step（2）Sodium hexametaphosphate dispersant and antioxidant ethylenediamine tetra-acetic acid two are added in the slurry of gained
Sodium, additive amount are respectively the ultrasonic wave hair for being sintered the 0.2% and 0.1% of scrap silicon quality, while opening the installation of reaction kettle kettle wall
Raw device carries out sonic oscillation processing to slurry, and continuing stirring makes its mixing be uniformly dispersed.
（4）Again to step（3）The mass ratio of addition sulfuric acid and nitric acid in gained slurry, added sulfuric acid and nitric acid is 1:1~
2, the sulfuric acid of addition and the total amount of nitric acid are be sintered scrap silicon quality 10%；Wherein the mass percent concentration of sulfuric acid is 98%,
The mass percent concentration of nitric acid is 67%.
（5）Using crawler type filter cloth vacuum filter by step（4）Gained slurry carries out vacuumizing filtration, vacuumizing filtration
It is 1 × 10 in vacuum degree-4It is carried out under conditions of Pa；And the vacuumizing filtration is by the way of continous way three-stage filtration：
First order filtration stage is：It only vacuumizes, the filtrate in slurry is filtered out, filtered subsequently into the second level；
Second level filtration stage is：Shower water washing is carried out while vacuumizing, the spray pressure of shower water is
100000Pa further washs the material of first order filtering gained, and adjusts its pH value between 6.5~7.5, then
Into third pole filtration stage；
Third pole filtration stage is：Stop shower water washing only to keep vacuumizing, the material solid content of gained is made to reach 90%
More than.
In step（5）It is sprayed while middle vacuumizing filtration, can realize that washing removes solvable residue and adjusts
Material pH value can reduce the usage amount of chemical regulator in production, can further decrease production cost.
（6）By step（5）The material of gained is in the high frequency that vibration frequency is 5000 beats/min, sieve mesh number is 300 mesh
It carries out sieving loose processing in vibrating screen.
Embodiment 2：Silica flour is purified from sintering scrap silicon according to the same manner as in Example 1, the difference is that, step
（1）The breaking strength of jaw crusher and double-roll crusher is respectively 280MPa and 230MPa, and ball mill is in vacuum degree
Vacuum grinding processing is carried out under conditions of 20000Pa.Step（2）The mass ratio of middle material and water is 1:10, step（3）In it is used
Dispersant and antioxidant are respectively sodium metnylene bis-naphthalene sulfonate and sodium hypophosphite, and additive amount is respectively scrap silicon quality
0.15% and 0.08%, step（5）The vacuum degree of middle vacuumizing filtration is 0.5 × 10-4Pa；Shower water used in second filtration stage
Spray pressure be 80000Pa.Step（6）In high frequency shale shaker vibration frequency be 4000 beats/min, sieve mesh number is
200 mesh.
Embodiment 3：Silica flour is purified from sintering scrap silicon according to the same manner as in Example 2, the difference is that, step
（3）Dispersant and antioxidant used is respectively maleic anhydride and oxamides, and additive amount is respectively scrap silicon quality
0.12% and 0.07%.
Embodiment 4：Silica flour is purified from sintering scrap silicon according to the same manner as in Example 1, the difference is that, step
（3）Dispersant and antioxidant used is respectively calgon and sodium hypophosphite, and additive amount is respectively scrap silicon matter
The 0.13% and 0.09% of amount.
Embodiment 5：Silica flour is purified from sintering scrap silicon according to the same manner as in Example 1, the difference is that, step
（3）Dispersant and antioxidant used is respectively calgon and oxamides, and additive amount is respectively scrap silicon quality
0.12% and 0.08%.
Embodiment 6：Silica flour is purified from sintering scrap silicon according to the same manner as in Example 2, the difference is that, step
（3）Dispersant and antioxidant used is respectively sodium metnylene bis-naphthalene sulfonate and disodium ethylene diamine tetraacetate, additive amount point
Not Wei scrap silicon quality 0.14% and 0.09%.
Embodiment 7：Silica flour is purified from sintering scrap silicon according to the same manner as in Example 2, the difference is that, step
（3）Dispersant and antioxidant used is respectively sodium metnylene bis-naphthalene sulfonate and oxamides, and additive amount is respectively scrap silicon
The 0.11% of quality and 0.06%.
Embodiment 8：Silica flour is purified from sintering scrap silicon according to the same manner as in Example 2, the difference is that, step
（3）Dispersant and antioxidant used is respectively maleic anhydride and disodium ethylene diamine tetraacetate, and additive amount is respectively that silicon is useless
Expect the 0.13% and 0.08% of quality.
Embodiment 9：Silica flour is purified from sintering scrap silicon according to the same manner as in Example 2, the difference is that, step
（3）Dispersant and antioxidant used is respectively maleic anhydride and sodium hypophosphite, and additive amount is respectively scrap silicon quality
0.12% and 0.09%.
Embodiment 10：Silica flour is purified from sintering scrap silicon according to the same manner as in Example 2, the difference is that, step
Suddenly（3）Dispersant used is the mixture of calgon, sodium metnylene bis-naphthalene sulfonate, maleic anhydride, the mass ratio of three
It is 8：5：1；Antioxidant be disodium ethylene diamine tetraacetate, sodium hypophosphite, oxamides mixture, the mass ratio of three is 3：
2：1, mixture dispersant and the additive amount of mixture antioxidant are respectively the 0.2% and 0.07% of scrap silicon quality.
Purifying silicon powder is carried out from sintering scrap silicon by the method in the present invention, the presence of sintering package can be solved to silicon
Sintering scrap silicon is conveniently and efficiently carried out purification processes by the technical issues of powder purification influences, can will be in the sintering scrap silicon
Silicon mass percentage is increased to 70%~90% by 20%~30%, and solid content reaches 90% or more, and gained silica flour dispersibility
It is good, it is not easy to reunite, while avoiding the presence pollution environment of sintering scrap silicon, and strong operability of the present invention, is highly suitable for work
Industryization promotes and applies.
The present invention can realize the effective recycling to being sintered scrap silicon, can scrap silicon be wrapped up in reluctant sintering
It carries out purification processes, and the particularly relevant performance indicator data of material before and after the processing are as shown in table 1 below.
The present invention is described in detail above in conjunction with embodiment, still, person of ordinary skill in the field can
Understand, without departing from the purpose of the present invention, each design parameter in above-described embodiment can also be changed, shape
At multiple specific embodiments, it is the common variation range of the present invention, is no longer described in detail one by one herein.
Claims (10)
1. a kind of method for purifying silica flour in scrap silicon from sintering, which is characterized in that include the following steps：
（1）Pending sintering scrap silicon is subjected to coarse crushing via jaw crusher and double-roll crusher respectively and two-stage fine crushing is broken
It is broken；Then it reuses ball mill and carries out vacuum grinding processing under conditions of vacuumizing, obtain the powder thing that granularity is less than 100 μm
Material；
（2）By step（1）The material of gained presses 1 with water:5~20 mass ratio is mixed and stirred in a kettle, is formed
Slurry；
（3）To step（2）Dispersant and antioxidant are added in the slurry of gained, while sonic oscillation processing is carried out to slurry,
And continuing stirring makes its mixing be uniformly dispersed；
（4）Again to step（3）The mass ratio of addition sulfuric acid and nitric acid in gained slurry, added sulfuric acid and nitric acid is 1:1~2, add
The total amount of the sulfuric acid and nitric acid that add is be sintered scrap silicon quality 5%~10%；
（5）By step（4）Gained slurry carries out vacuumizing filtration；
（6）By step（5）The material of gained carries out sieving loose processing in high frequency shale shaker.
2. the method for purifying silica flour in the scrap silicon according to claim 1 from sintering, which is characterized in that in the step
（1）In, the breaking strength of jaw crusher is 250MPa~300MPa；The breaking strength of double-roll crusher be 200MPa~
250MPa。
3. the method for purifying silica flour in the scrap silicon according to claim 1 from sintering, which is characterized in that in the step
（1）In, ball mill carries out vacuum grinding processing under conditions of vacuum degree is 10000~50000Pa.
4. the method for purifying silica flour in the scrap silicon according to claim 1 from sintering, which is characterized in that in the step
（2）Used in water be deionized water, the μ s/cm of conductivity≤1；The reaction kettle is stainless steel cauldron.
5. the method for purifying silica flour in the scrap silicon according to claim 1 from sintering, which is characterized in that the step（3）
In dispersant be calgon, sodium metnylene bis-naphthalene sulfonate, at least one of maleic anhydride, total amount of adding is sintering
The 0.1%~0.2% of scrap silicon quality；Antioxidant is at least one in disodium ethylene diamine tetraacetate, sodium hypophosphite, oxamides
Kind, additive amount is be sintered scrap silicon quality 0.05%~0.1%.
6. the method for purifying silica flour in the scrap silicon according to claim 5 from sintering, which is characterized in that dispersant used is
The mass ratio of the mixture of calgon, sodium metnylene bis-naphthalene sulfonate and maleic anhydride, three is 1~10：1~5：1；It is used
Antioxidant be disodium ethylene diamine tetraacetate, sodium hypophosphite, oxamides mixture, the mass ratio of three be 1~5：1~
3：1.
7. the method for purifying silica flour in the scrap silicon according to claim 1 from sintering, which is characterized in that the step（4）
In, the mass percent concentration of the sulfuric acid of addition is 95%~100%, and the mass percent concentration of nitric acid is 65%~70%.
8. the method for purifying silica flour in the scrap silicon according to claim 1 from sintering, which is characterized in that the step（5）
In to slurry carry out vacuumizing filtration by the way of continous way three-stage filtration：
First order filtration stage is：It only vacuumizes, the filtrate in slurry is filtered out, filtered subsequently into the second level；
Second level filtration stage is：Shower water washing is carried out while vacuumizing, by the material of first order filtering gained into one
Step is washed, and adjusts its pH value between 6.5~7.5, subsequently into third level filtration stage；
Third level filtration stage is：Stop shower water washing only keep vacuumize, make gained material solid content reach 90% with
On.
9. the method for purifying silica flour in the scrap silicon according to claim 8 from sintering, which is characterized in that the step（5）
Middle to carry out the vacuumizing filtration process using crawler type filter cloth vacuum filter, the vacuum degree of vacuumizing filtration is 1 × 10-3~
1×10-4Pa；The spray pressure of shower water used in the filtration stage of the second level is 50000~100000Pa.
10. the method for purifying silica flour in the scrap silicon according to claim 1 from sintering, which is characterized in that in the step
（6）In, the vibration frequency of high frequency shale shaker is 3000~5000 beats/min；Sieve mesh number is 100~300 mesh.
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| 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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| 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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