CN107758672A - The recovery method of silica flour in crystalline silicon cutting waste material - Google Patents
The recovery method of silica flour in crystalline silicon cutting waste material Download PDFInfo
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- CN107758672A CN107758672A CN201711260184.5A CN201711260184A CN107758672A CN 107758672 A CN107758672 A CN 107758672A CN 201711260184 A CN201711260184 A CN 201711260184A CN 107758672 A CN107758672 A CN 107758672A
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- waste material
- silica flour
- cutting waste
- crystalline silicon
- rotary drum
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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
Abstract
The invention discloses a kind of recovery method of silica flour in crystalline silicon cutting waste material, the recovery method of silica flour includes in crystalline silicon cutting waste material：Step S1, crystalline silicon cutting waste material are pre-processed to obtain the mixed powder of silicon and carborundum；Solvent is added in the mixed powder of step S2, silicon and carborundum and is adjusted to the mixed solution that pH value is 6~9；Step S3, mixed solution, which is inserted in hypergravity grading plant, carries out isolated Si-rich phase solution and rich depositing SiC phase；Step S4, Si-rich phase solution adjust pH value to 1~3, silica flour are obtained after filtering drying.According to the recovery method of silica flour in the crystalline silicon cutting waste material of the present invention, by means of the difference of two kinds of particulates of silicon and carborundum, the relation of mating surface current potential and pH value, the big multipotency of the silicon powder in mixed solution is set to be in suspended state by hypergravity grading plant, and granularity silicon-carbide particle bigger than normal then can rapid precipitation in bottom, so as to realize the separation of carborundum and silicon, it is easy to the recycling of silica flour.
Description
Technical field
The present invention relates to chemical technology field, more particularly to a kind of recovery method of silica flour in crystalline silicon cutting waste material.
Background technology
In correlation technique, when making silicon chip of solar cell, it will first be cut into slices again after high-purity crystal silicon ingot casting.Cutting into slices
In process, Si powder waste material that the part that accounts for silicon ingot weight more than 30% can be by multi-wire saw into fine sizes, with cutting
Metal fillings caused by skiving material silicon carbide powder, grinding and the polyethylene glycol mixing shape used as cutting abrasive suspension
Into sticky slug.In this slug, value highest composition is silicon, however, the recycling of silicon is difficult, resource
Utilization rate is low and pollutes environment.
The content of the invention
It is contemplated that at least solves one of technical problem present in prior art.Therefore, the present invention proposes a kind of crystalline substance
The recovery method of silica flour in body silicon cutting waste material, the recovery method of silica flour is easily operated in the crystalline silicon cutting waste material and ring
Protect.
The recovery method of silica flour in crystalline silicon cutting waste material according to embodiments of the present invention, including：Step S1, crystalline silicon are cut
Waste material is cut to be pre-processed to obtain the mixed powder of silicon and carborundum；Added in the mixed powder of step S2, silicon and carborundum
Solvent is simultaneously adjusted to the mixed solution that pH value is 6~9；Step S3, mixed solution are inserted in hypergravity grading plant and separated
Obtain Si-rich phase solution and rich depositing SiC phase；Step S4, Si-rich phase solution adjust pH value to 1~3, obtained after filtering drying
Silica flour.
The recovery method of silica flour in crystalline silicon cutting waste material according to embodiments of the present invention, by means of two kinds of silicon and carborundum
The relation of the difference of particulate, mating surface current potential and pH value, make the silicon powder in mixed solution big by hypergravity grading plant
Multipotency is in suspended state, and granularity silicon-carbide particle bigger than normal then can rapid precipitation in bottom, so as to realize carborundum and silicon
Separation, be easy to the recycling of silica flour, it is easy to operate and be advantageous to reduce the pollution to environment.
In addition, the recovery method of silica flour is also with following attached in crystalline silicon cutting waste material according to the above embodiment of the present invention
The technical characteristic added：
According to some embodiments of the present invention, the preprocessing process includes：In crystalline silicon cutting waste material add water and
Acid after stirring the scheduled time, is filtered, dried and grind to obtain the mixed-powder of silicon and carborundum to remove polyethylene glycol.
Further, in the preprocessing process, stirred 3 to 4 hours after water and acid are added in crystalline silicon cutting waste material,
Then dried using cake filtration and to filter cake, be put into ball mill and grind 10~30 minutes after filter cake drying, obtain silicon and carbon
SiClx mixed-powder.
Specifically, the acid added in crystalline silicon cutting waste material is included in hydrochloric acid, nitric acid, sulfuric acid, citric acid, oxalic acid at least
It is a kind of.
According to some embodiments of the present invention, the mixed-powder of silicon and carborundum is according to liquid-solid ratio 3 in the step S2：1
~5:1 addition water simultaneously stirs to form the mixed solution.
Further, the solvent added in the step S2 includes water and sodium hydroxide, potassium hydroxide, ammonium carbonate, carbon
At least one of sour hydrogen ammonium and ammoniacal liquor alkali.
According to some embodiments of the present invention, the hypergravity grading plant includes：Fixed support；Cylinder, the cylinder
It is located on the fixed support, the cylinder has the slurry outlet for connecting its inner chamber；Rotary drum, the rotary drum are arranged on the cylinder
In vivo；Rotary drum motor, the rotary drum motor are located at the outer bottom of the cylinder and are connected with the rotary drum for driving described turn
Drum rotation；Input and output material pipeline, the lower end of the input and output material pipeline are adapted to extend into the rotary drum；Lowering or hoisting gear, the lifting dress
It is set in the outer top of the cylinder and is connected with the input and output material pipeline, the lowering or hoisting gear is connected with lifting motor to drive
The input and output material pipeline raising and lowering.
Further, the mixed solution obtained in step S2 is inserted in hypergravity grading plant, and passes through slurry outlet
Collect the silica flour solution that overflow goes out.
Specifically, the rotary drum motor is variable-frequency motor.
Alternatively, the rotating speed of the rotary drum is 50~200 revs/min, and processing time is 10~30 minutes, after separation terminates
Rinse the silicon carbide powder collected and deposited on drum inner wall.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description
Obtain substantially, or recognized by the practice of the present invention.
Brief description of the drawings
The above-mentioned and/or additional aspect and advantage of the present invention will become in the description from combination accompanying drawings below to embodiment
Substantially and it is readily appreciated that, wherein：
Fig. 1 is a flow chart of the recovery method of silica flour in crystalline silicon cutting waste material according to embodiments of the present invention；
Fig. 2 is a schematic diagram of hypergravity grading plant according to embodiments of the present invention.
Reference：
Hypergravity grading plant 100, cylinder 1, slurry outlet 11, baffle ring 12, rotary drum 2, rotary drum motor 3, input and output material pipeline
4, main line 41, bye-pass 42, lowering or hoisting gear 5, lifting motor 6, fixed support 7.
Embodiment
Embodiments of the invention are described below in detail, the example of the embodiment is shown in the drawings, wherein from beginning to end
Same or similar label represents same or similar element or the element with same or like function.Below with reference to attached
The embodiment of figure description is exemplary, it is intended to for explaining the present invention, and is not considered as limiting the invention.
In the description of the invention, it is to be understood that the instruction such as term " on ", " under ", " top ", " bottom " " interior ", " outer "
Orientation or position relationship be based on orientation shown in the drawings or position relationship, be for only for ease of the description present invention and simplification retouched
State, rather than instruction or imply signified device or element there must be specific orientation, with specific azimuth configuration and operation,
Therefore it is not considered as limiting the invention.In the description of the invention, unless otherwise indicated, " multiple " are meant that two
Or two or more.
In the description of the invention, it is necessary to illustrate, unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " should be interpreted broadly, for example, it may be being fixedly connected or being detachably connected, or be integrally connected；Can
To be mechanical connection or electrical connection；Can be joined directly together, can also be indirectly connected by intermediary, Ke Yishi
The connection of two element internals.For the ordinary skill in the art, with concrete condition above-mentioned term can be understood at this
Concrete meaning in invention.
In correlation technique, Solar use has become the important directions of new energy development, various solar photocells
Research and development are just among mushroom development, wherein the solar cell for having more than 80% is all using based on high purity polycrystalline silicon
Raw material makes, in current all kinds of photocell products in occupation of absolute leading position.
Production silicon chip mainly uses multifibres line cutting technology, and caused slug main component (mass fraction) has：20%
The metal impurities such as the HIGH-PURITY SILICON of left and right, 40% or so carborundum, 30% or so polyethylene glycol and water, 5% or so iron.It is single
For silica flour sheet in the cutting waste material of crystal silicon and polysilicon as high-purity crystalline silicon, impurity content is few, and it is high to recycle value.
The recovery of carborundum and polyethylene glycol in being starched in correlation technique primarily directed to cutting waste material, is reclaimed on HIGH-PURITY SILICON
It is less.If the silicon in separation and recovery slug, which re-works, is made solar silicon wafers, resource utilization can be both improved, is reduced
Environmental hazard, the manufacturing cost of solar energy polycrystal silion cell can be reduced again.
Method on reclaiming HIGH-PURITY SILICON has：A kind of scheme is, first by slug removal suspending agent and binding agent, then will
To solid Si and SiC mixed powder are obtained by flotation, then carry out gravity with heavy-fluid of the density between Si and SiC
Or centrifugal sedimentation separation, obtain purer SiC and Si micro mists finally by iron removal by magnetic separation.
Another scheme is to handle monocrystalline silicon cutting waste liquor with watery hydrochloric acid, and be stirred into runny compound；
Mixed material heating is subjected to separation of solid and liquid again, water and polyethylene glycol steam, condensed, being dehydrated, reclaiming and to obtain polyethylene glycol together, separation
Obtained solid is the mixture of carborundum and silicon；Then clean the mixture twice with water, formed with nitric acid and hydrofluoric acid
Silicon therein is dissolved in mix acid liquor processing, and final recovery obtains carborundum.
However, certain deficiency be present in the technical scheme of above-mentioned separation and recovery silicon：Such as technological process it is universal longer and
Silicon is even converted into compound by complex operation, some methods by simple substance, and further also principle is more difficult.It is in addition, big
More separation methods have all used that some are poisonous, have the reagent of pollution.Although silicon is in monocrystalline silicon and polysilicon lines cutting waste material slurry
Most there is the part of recovery value, but can realize that its is industrialized there is presently no a kind of simple ripe isolation technics and regenerate
Circulation turns into high purity polycrystalline silicon, remanufactures as solar-grade polysilicon.
It is to be solved by this invention to be given up it is a key issue that being cut using gravity Method separation and recovery monocrystalline silicon and polysilicon lines
Silica fume and carborundum powder in material.
It was found from after the sample test that domestic multiple producers fetch, in cutting on line slug, the average grain diameter of silicon is about 1
μm, the average grain diameter of carborundum is about 10 μm, differs ten times or so, and the density of silicon is 2.4g/cm3, the density of carborundum
For 3.2g/cm3 or so, therefore, the two granularity, volume and mass discrepancy are quite big.By means of the above difference of two kinds of particulates,
The present invention proposes the method for efficiently separating two kinds of particulates.In view of in surface potential-pH value relation, when pH value is 6~9,
The big multipotency of silicon powder in mixed solution is in suspended state, and granularity silicon-carbide particle bigger than normal then can rapid precipitation the bottom of at
Layer, so as to realize the separation with silicon.
The recovery method of silica flour in crystalline silicon cutting waste material according to embodiments of the present invention is described below in conjunction with the accompanying drawings.Its
In, crystalline silicon can be monocrystalline silicon or polysilicon.
Specifically, as Figure 1-Figure 2, in crystalline silicon cutting waste material according to embodiments of the present invention silica flour recovery side
Method, including：Step S1, crystalline silicon cutting waste material are pre-processed to obtain the mixed powder of silicon and carborundum.By to crystal
Silicon cutting waste material, which carries out pretreatment, can remove the impurity such as polyglycol solution and iron in cutting waste material, pure so as to obtain
The mixed powder of the higher silicon of degree and carborundum, is advantageously implemented the recovery of silica flour.
Solvent (such as water etc.) is added in the mixed powder of step S2, silicon and carborundum and be adjusted to pH value be 6~9 it is mixed
Close solution.In the relation of surface potential and pH value, when pH value is 6~9, the big multipotency of silicon powder in mixed solution is in outstanding
Floating state, and granularity silicon-carbide particle bigger than normal then can rapid precipitation in bottom, be easy to implement the separation of carborundum and silicon.
Step S3, mixed solution, which is inserted in hypergravity grading plant, carries out isolated Si-rich phase solution (rich carborundum phase
Silicon carbide powder is obtained after drying) and rich depositing SiC phase.Rotated, can produced super by the high speed of hypergravity grading plant
Gravity, it is easy to be classified mixed solution to obtain Si-rich phase solution and rich depositing SiC phase.
Step S4, Si-rich phase solution adjust pH value to 1~3, silica flour are obtained after filtering drying.For example, by Si-rich phase solution
Dilute acid for adjusting pH value is added to 1~3, silicon particle is agglomerated into larger particles and settled rapidly, and silica flour is obtained after filtering drying, realizes
The recycling of silica flour.
The recovery method of silica flour in crystalline silicon cutting waste material according to embodiments of the present invention, by means of two kinds of silicon and carborundum
The relation of the difference of particulate, mating surface current potential and pH value, make the silicon powder in mixed solution big by hypergravity grading plant
Multipotency is in suspended state, and granularity silicon-carbide particle bigger than normal then can rapid precipitation in bottom, so as to realize carborundum and silicon
Separation, be easy to the recycling of silica flour, it is easy to operate and be advantageous to reduce the pollution to environment.
According to some embodiments of the present invention, the preprocessing process includes：In crystalline silicon cutting waste material add water and
Acid after stirring the scheduled time, is filtered, dried and grind to obtain the mixed-powder of silicon and carborundum to remove polyethylene glycol.It is logical
Cross and pre-process the impurity such as the polyethylene glycol that can be removed in crystalline silicon cutting waste material, iron, be easy to obtain purity higher silicon and carbon
The mixed-powder of SiClx.
Wherein, the acid added in crystalline silicon cutting waste material can be such as diluted acid, and concentration is 2mol/L etc., and diluted acid is a kind of
Liquid acid, it is divided into sulfuric acid, nitric acid, hydrochloric acid in inorganic acid.Described diluted acid refers to the solution more than the few solvent of solute in sour solution.
Further, in preprocessing process, stir 3 to 4 hours, stir after water and acid are added in crystalline silicon cutting waste material
It can at normal temperatures carry out, by stirring, reaction can be made more abundant, so as to by impurity removal as much as possible；So
Dried afterwards using cake filtration and to filter cake, be put into ball mill and grind 10~30 minutes after filter cake drying, obtain silicon and carbonization
Silicon mixed-powder.It is easy to further reclaim silica flour.
Specifically, the acid added in crystalline silicon cutting waste material is included in hydrochloric acid, nitric acid, sulfuric acid, citric acid, oxalic acid at least
It is a kind of.Conveniently select and easily operated.
According to some embodiments of the present invention, the mixed-powder of silicon and carborundum is according to liquid-solid ratio 3 in step S2：1~5:1
Add water and stir to form mixed solution.Further, reference picture 1, the solvent added in step S2 include water and
At least one of sodium hydroxide, potassium hydroxide, ammonium carbonate, ammonium hydrogen carbonate and ammoniacal liquor alkali.It is easy to regulate and control mixed powder solution
PH value, preferably separate silica flour.
For example, in the relation of surface potential and pH value, when pH value is 6~9, the big multipotency of silicon powder in mixed solution
In suspended state, and granularity silicon-carbide particle bigger than normal then can rapid precipitation in bottom, so as to realize point of carborundum and silicon
From.
The recovery method of silica flour in crystalline silicon cutting waste material according to embodiments of the present invention, including：
Cutting waste material pre-processes：Water, liquid-solid ratio 3 are added in monocrystalline silicon and polysilicon lines cutting waste material:1.Stir on side
Side adds a small amount of sour (can use hydrochloric acid, nitric acid, sulfuric acid and citric acid, oxalic acid etc.) to remove polyethylene glycol and iron and other impurities
Element, after stirring 3~4 hours (process can be carried out at normal temperatures), filtered, filter cake is dried.Filter cake after drying is put
Enter in ball mill and grind 10~30 minutes, obtain silicon and carborundum mixed-powder.
Adjust the pH value of mixed-powder aqueous suspension：Powder after grinding is put into container, adds a certain amount of water,
Liquid-solid ratio is 3:1, then add alkali (sodium hydroxide, potassium hydroxide, ammonium carbonate, ammonium hydrogen carbonate, ammoniacal liquor etc. can be used) regulation pH value
To 6~9.Now the surface potential of silicon is much larger than carborundum, and interparticle mutually electrostatic repulsion effect is maximum in the solution, super
The tiny silicon powder particle of granularity can be made to keep suspended state in gravity based separation process.
Gravity Method separation process：The above-mentioned adjusted slurry for certain ph is continuously injected into certain flow velocity overweight
In power grading plant 100, and the silica flour solution gone out by the collection overflow of slurry outlet 11, equipment rotating speed are 50~200 revs/min
Clock, processing time are 10~30 minutes, and separation rinses the silicon carbide powder for collecting deposition after terminating.
Adjust the pH value of Si-rich phase solution：The Si-rich phase solution obtained after separation, adding diluted acid (can use watery hydrochloric acid, dilute nitre
Acid, acetic acid etc.) for regulation pH value to 1~3, now the mutual electrostatic repulsion effect between silicon particle is smaller, can be rolled into a ball rapidly between particle
Be polymerized to larger particles and rapid subsidence, obtain silica flour after filtering drying.
Present invention beneficial effect possessed compared with prior art is：
First, the technological process of the present invention is simple, technological parameter is stable, is separated with hypergravity grading plant, lock out operation
Time is short, and power consumption is low, and semicontinuous operation can be achieved.
Second, the present invention realizes separation according to granularity (the volume, quality) difference of silicon and carborundum, and by different pH
It is different to be worth lower surface current potential, silica flour is fully suspended and is not easy to deposit to barrel in super gravity field, so that the two is separated.
Third, the main separating medium used in the present invention is water, the change of micro mist surface potential in the regulation aqueous solution used
It is all common common acid or alkali to learn reagent, belongs to nontoxic reagent, therefore pollution is small, and water can recycle, basic to realize
Zero-emission.
Fourth, the technological process being related in the present invention can be carried out at normal temperatures.
According to some embodiments of the present invention, as shown in Fig. 2 hypergravity grading plant 100 according to embodiments of the present invention,
Including：Fixed support 7, cylinder 1, rotary drum 2, rotary drum motor 3, input and output material pipeline 4 and lowering or hoisting gear 5.
Specifically, cylinder 1 is located on fixed support 7 (such as welding etc.), and there is cylinder 1 slurry for connecting its inner chamber to go out
Mouth 11, can further be discharged the slurry in cylinder 1 by slurry outlet 11.
Rotary drum 2 is arranged in cylinder 1.The material of cylinder 1 can be stainless steel, titanium etc., and cylinder 1 can not only protect rotary drum
2, moreover it is possible to prevent overflow slurry from splashing.
For example, rotary drum 2 can be located at the bottom in cylinder 1, and the relative position of rotary drum 2 and cylinder 1 is fixed, rotary drum 2
Top can open wide, or on rotary drum 2 formed with connection cylinder 1 inner chamber feed inlet and outlet.
Rotary drum motor 3 is located at outside cylinder 1, and rotary drum motor 3 is connected with rotary drum 2 to drive rotary drum 2 to rotate.Rotary drum 2 can
To be made up of stainless steel or titanium etc., rotary drum motor 3 can be located at the lower section of rotary drum 2, and rotary drum 2 can be driven by rotary drum motor 3
Rotation produces hypergravity at a high speed, is advantageous to the separation of slurry.
Here hypergravity refer to rotary drum 2 rotate at a high speed caused by centrifugal force, rotary drum 2 rotate acceleration be more than gravity
Acceleration.
The lower end of input and output material pipeline 4 is adapted to extend into rotary drum 2.By the way that input and output material pipeline 4 is stretched into rotary drum 2, be easy to
Addition slurry in rotary drum 2, or extract slurry out from rotary drum 2, it is easily operated.
Lowering or hoisting gear 5 is located at outside cylinder 1, and lowering or hoisting gear 5 is connected with input and output material pipeline 4, and lowering or hoisting gear 5 is connected with liter
Motor 6 drops to be driven in and out the raising and lowering of pipe material 4.By lowering or hoisting gear 5 and lifting motor 6, can automatic lifting or under
Input and output material pipeline 4 drops, and it is easy to operate.
Wherein, slurry can be injected in rotary drum 2 via input and output material pipeline 4, drive rotary drum 2 to revolve at a high speed by rotary drum motor 3
Change the line of production raw hypergravity, the slurry of different specific weight can be layered, so as to be advantageous to the separation of slurry, easily operated and separative efficiency
It is high.
Hypergravity grading plant 100 according to embodiments of the present invention, slurry can be injected in rotary drum 2 by input and output material pipeline 4,
Drive rotary drum 2 to rotate at a high speed by rotary drum motor 3 and produce hypergravity, the slurry of different specific weight can be layered, so as to be advantageous to
The separation of slurry, easily operated and separative efficiency are high.
Further, the mixed solution obtained in step S2 is inserted in hypergravity grading plant 100, and gone out by slurry
Mouth 11 collects the silica flour solution that overflows go out.By the way that the slurry for being adjusted to certain ph is continuously injected into hypergravity with certain flow velocity
In grading plant 100, the recovery of silica flour can be further realized, it is easily operated.
Specifically, rotary drum motor 3 is variable-frequency motor, and the frequency of rotary drum motor 3 is 0-50Hz.Thus, rotary drum motor 3 connects
Stepless time adjustment function can be realized after frequency converter, controls rotary drum rotating speed, preferably drives rotary drum 2 to rotate, realizes the separation of slurry.
In addition, can preferably drive rotary drum 2 to rotate at a high speed by rotary drum motor 3 produces hypergravity, so that will not be year-on-year
The slurry layering of weight, is easy to the separation of slurry.
Alternatively, the rotating speed of rotary drum 2 is 50~200 revs/min, and processing time is 10~30 minutes, and separation terminates backlash
Wash the silicon carbide powder collected and deposited on the inwall of rotary drum 2.
Wherein, the rotating speed of rotary drum 2 can be 50rpm, 80rpm, 100rpm, 120rpm, 140rpm or 200rpm etc..
Referring to Figures 1 and 2, according to some embodiments of the present invention, rotary drum motor 3 is located at the bottom outside cylinder 1, rotary drum electricity
Machine 3 is connected (such as gear drive, V belt translation etc.) with rotary drum 2, by rotary drum motor 3 rotary drum 2 can be driven to rotate at a high speed,
Be advantageous to the further separation of slurry.
Lowering or hoisting gear 5 is located at the top outside cylinder 1.It is easy to the installation of lowering or hoisting gear 5, and is advantageous to improve hypergravity classification
The automaticity of device 100, improve efficiency.
According to some embodiments of the present invention, formed with extending downwardly and relative with the output shaft of rotary drum motor 3 on rotary drum 2
Axle portion, rotary drum 2 is connected by shaft coupling with rotary drum motor 3.In other words, on rotary drum 2 formed with axle portion, axle portion can be to downward
Stretch, and axle portion can be relative with the output shaft of rotary drum motor 3, thus, is easy to realize rotary drum 2 and rotary drum motor by shaft coupling
Being reliably connected between 3.
As shown in Fig. 2 according to some embodiments of the present invention, input and output material pipeline 4 includes：Main line 41 and bye-pass 42,
(above-below direction shown in reference picture 2) extends main line 41 along the vertical direction；Bye-pass 42 is located at the lower end of main line 41, and
And bye-pass 42 connects with main line 41, bye-pass 42 can include the multiple of one or circumferentially spaced arrangement.Thus, to
In input and output material pipeline 4 during injection slurry, slurry can pass through bye-pass 42 and inject rotary drum 2 first via main line 41
It is interior, be advantageous to slurry and be uniformly distributed in rotary drum 2.
In addition, input and output material pipeline 4 can make slurry enter rotary drum 2 in, input and output material pipeline 4 can also be by rotary drum 2 from inside to outside
Discharge, flushing water can also be injected into rotary drum 2 by input and output material pipeline 4.
Reference picture 2, according to some embodiments of the present invention, the bottom of cylinder 1 is in the taper to contract from top to bottom.Turn
The slurry that drum 2 overflows during high speed rotates, which is easy to slide downwards via cylinder 1, to be built up, and is easy to further leading for slurry
Go out.
Further, can be formed on the bottom wall of cylinder 1 with reference to Fig. 2, slurry outlet 11.So that it is accumulated to the bottom of cylinder 1
The slurry in portion can discharge via slurry outlet 11.
Further, reference picture 2, the inner bottom surface of cylinder 1 is formed with upwardly extending and be spaced apart with the exterior bottom wall of rotary drum 2
Baffle ring 12.That is, the inner bottom surface of cylinder 1 can upwardly extend formed with baffle ring 12, baffle ring 12, and baffle ring 12 and rotary drum
2 exterior bottom wall can be spaced apart.By setting baffle ring 12, it can prevent slurry from flowing into rotary drum motor 3 and rotary drum motor 3 with turning
The junction of drum 2, fault rate is advantageously reduced, ensure the use reliability of hypergravity grading plant 100.
Further, stagger in the vertical direction with slurry outlet 11 with reference to Fig. 1, baffle ring 12, slurry outlet 11 can be with
Positioned at the outside of baffle ring 12.Preferably, baffle ring 12 is coaxial with rotary drum motor 3.As a result, the structure of hypergravity grading plant 100
Compact and reasonable.
According to some embodiments of the present invention, rotary drum motor 3 is variable-frequency motor, and the frequency of rotary drum motor 3 is 0-50Hz.By
This, rotary drum motor 3 can realize stepless time adjustment function after connecting frequency converter, control rotary drum rotating speed, preferably drive rotary drum 2 to revolve
Turn, realize the separation of slurry.
Hypergravity grading plant 100 according to embodiments of the present invention, rotary drum 2 is driven to rotate production at a high speed using rotary drum motor 3
Raw hypergravity so that the material of different grain size or proportion is layered in hypergravity grading plant 100 in waste residue slurry, and continuously
Fine grained overflow is exported, coarse granule is periodically taken away, and impurity content is extremely low in fine grained valuable material, and coarse granule volume is few.
Several specific embodiments of the recovery method of silica flour in crystalline silicon cutting waste material according to the present invention are described below.
Embodiment one：
It is 4 that the mixed-powder of polyethylene glycol, which will be got rid of, according to liquid-solid ratio：1 adds water, and pH is adjusted with sodium hydroxide solution
It is worth for 7, then the mixed solution is continuously injected into hypergravity grading plant 100 with certain flow velocity, and passes through slurry outlet 11
The silica flour solution that overflow goes out is collected, processing time is 20 minutes, 100 revs/min of rotating speed.Separation is rinsed after terminating and collects rotary drum 2
The silicon carbide powder deposited on inwall, filtering drying recovery；After the regulation pH value sedimentation of Si-rich phase solution, silicon is obtained after filtering drying
Powder, silica flour purity is 81.5% after testing, carborundum powder 93.8%.
Embodiment two：
It is 3 that the mixed-powder of polyethylene glycol, which will be got rid of, according to liquid-solid ratio：1 adds water, and pH is adjusted with sodium hydroxide solution
It is worth for 8, then the mixed solution is continuously injected into hypergravity grading plant 100 with certain flow velocity, and passes through slurry outlet 11
The silica flour solution that overflow goes out is collected, processing time is 30 minutes, 80 revs/min of rotating speed.Separation is rinsed after terminating and collected in rotary drum 2
The silicon carbide powder deposited on wall, filtering drying recovery；After the regulation pH value sedimentation of Si-rich phase solution, silicon is obtained after filtering drying
Powder, silica flour purity is 82.7% after testing, carborundum powder 91.2%.
Embodiment three：
It is 5 that the mixed-powder of polyethylene glycol, which will be got rid of, according to liquid-solid ratio：1 adds water, and pH is adjusted with sodium hydroxide solution
It is worth for 8.5, then the mixed solution is continuously injected into hypergravity grading plant 100 with certain flow velocity, and passes through slurry outlet
The silica flour solution that 11 collection overflows go out, processing time are 15 minutes, 150 revs/min of rotating speed.Separation is rinsed after terminating and collects rotary drum
The silicon carbide powder deposited on 2 inwalls, filtering drying recovery；After the regulation pH value sedimentation of Si-rich phase solution, obtained after filtering drying
Silica flour, silica flour purity is 83.6% after testing, carborundum powder 94.3%.
The recovery of silica flour in crystalline silicon cutting waste material according to embodiments of the present invention is described in detail with reference to Fig. 1 to Fig. 2
The course of work of method.
Specifically, cutting waste material is pre-processed first, removes the impurity such as polyglycol solution and iron, after drying
To silicon and the mixed-powder of carborundum；The mixed-powder is added water to stir and adjusts pH value to 6~9 with alkali, then by the mixing slurry
Material is inserted in hypergravity grading plant 100, after separation, you can be collected into silica flour and carborundum powder, wherein silica flour purity can
Reach more than 80%, while the purity of carborundum powder is up to more than 90%.
Wherein, cutting waste material pretreatment includes：Water is added in monocrystalline silicon and polycrystalline silicon cut waste, and is added a small amount of
Acid, after stirring 3~4 hours, filtered, dry the simultaneously mixed-powder of grinding distribution silicon and carborundum；
The pH value of regulation and control mixed-powder solution includes：By the mixed-powder of silicon and carborundum according to certain liquid-solid ratio 3~
5：1 adds water, and acid adding or alkali regulation pH value are 6~9, are stirred；
Hypergravity separation process includes：Mixing liquid is inserted in hypergravity grading plant 100, passes through the separation of the device
It can obtain Si-rich phase solution and rich depositing SiC phase；
Filtering drying process includes：Si-rich phase solution is added into dilute acid for adjusting pH value to 1~3, silicon particle is agglomerated into larger
Particle and settle rapidly, silica flour is obtained after filtering drying；Silicon carbide powder is obtained after rich carborundum phase drying.So far basis is completed
The course of work of the recovery method of silica flour in the crystalline silicon cutting waste material of the embodiment of the present invention.
Other configuration examples of the recovery method of silica flour and operation in crystalline silicon cutting waste material according to embodiments of the present invention
All it is for those of ordinary skills known, is not detailed herein.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or the feature for combining the embodiment or example description
It is contained at least one embodiment or example of the present invention.In this manual, need not to the schematic representation of above-mentioned term
Identical embodiment or example must be directed to.Moreover, specific features, structure, material or the feature of description can be any
Combined in an appropriate manner in individual or multiple embodiments or example.In addition, in the case of not conflicting, the technology of this area
Different embodiments or example and the feature of different embodiments or example described in this specification can be combined by personnel
And combination.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changed, replacing and modification.
Claims (10)
- A kind of 1. recovery method of silica flour in crystalline silicon cutting waste material, it is characterised in that including：Step S1, crystalline silicon cutting waste material are pre-processed to obtain the mixed powder of silicon and carborundum；Solvent is added in the mixed powder of step S2, silicon and carborundum and is adjusted to the mixed solution that pH value is 6~9；Step S3, mixed solution, which is inserted in hypergravity grading plant, carries out isolated Si-rich phase solution and rich depositing SiC Phase；Step S4, Si-rich phase solution adjust pH value to 1~3, silica flour are obtained after filtering drying.
- 2. the recovery method of silica flour in crystalline silicon cutting waste material according to claim 1, it is characterised in that the pretreatment Process includes：Water and acid are added in crystalline silicon cutting waste material to remove polyethylene glycol, after stirring the scheduled time, filters, dry and grind To obtain the mixed-powder of silicon and carborundum.
- 3. the recovery method of silica flour in crystalline silicon cutting waste material according to claim 2, it is characterised in that the pretreatment During, stir 3 to 4 hours after water and acid are added in crystalline silicon cutting waste material, then dried using cake filtration and to filter cake It is dry, it is put into ball mill and grinds 10~30 minutes after filter cake drying, obtains silicon and carborundum mixed-powder.
- 4. the recovery method of silica flour in crystalline silicon cutting waste material according to claim 2, it is characterised in that crystalline silicon is cut The acid added in waste material includes at least one of hydrochloric acid, nitric acid, sulfuric acid, citric acid, oxalic acid.
- 5. the recovery method of silica flour in crystalline silicon cutting waste material according to claim 1, it is characterised in that the step S2 The mixed-powder of middle silicon and carborundum is according to liquid-solid ratio 3：1~5:1 addition water simultaneously stirs to form the mixed solution.
- 6. the recovery method of silica flour in crystalline silicon cutting waste material according to claim 5, it is characterised in that the step S2 The solvent of middle addition includes at least one of water and sodium hydroxide, potassium hydroxide, ammonium carbonate, ammonium hydrogen carbonate and ammoniacal liquor Alkali.
- 7. the recovery method of silica flour in the crystalline silicon cutting waste material according to any one of claim 1-6, it is characterised in that The hypergravity grading plant includes：Fixed support；Cylinder, the cylinder are located on the fixed support, and the cylinder has the slurry outlet for connecting its inner chamber；Rotary drum, the rotary drum are arranged in the cylinder；Rotary drum motor, the rotary drum motor are located at the outer bottom of the cylinder and are connected with the rotary drum for driving the rotary drum Rotation；Input and output material pipeline, the lower end of the input and output material pipeline are adapted to extend into the rotary drum；Lowering or hoisting gear, the lowering or hoisting gear are located at the outer top of the cylinder and are connected with the input and output material pipeline, the lifting Device is connected with lifting motor to drive the input and output material pipeline raising and lowering.
- 8. the recovery method of silica flour in crystalline silicon cutting waste material according to claim 7, it is characterised in that by step S2 Obtained mixed solution is inserted in hypergravity grading plant, and the silica flour solution gone out by slurry outlet collection overflow.
- 9. the recovery method of silica flour in crystalline silicon cutting waste material according to claim 7, it is characterised in that the rotary drum electricity Machine is variable-frequency motor.
- 10. the recovery method of silica flour in crystalline silicon cutting waste material according to claim 8, it is characterised in that the rotary drum Rotating speed be 50~200 revs/min, processing time be 10~30 minutes, separation terminate after rinse collect drum inner wall on deposits Silicon carbide powder.
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| CN112441588A (en) * | 2020-12-31 | 2021-03-05 | 重庆大学 | Deoxidation method for diamond wire cutting silicon waste |
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