CN102295285B - A kind of recovery method of silicon chip dicing waste mortar - Google Patents
A kind of recovery method of silicon chip dicing waste mortar Download PDFInfo
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Abstract
The invention provides a kind of recovery method of silicon chip dicing waste mortar, comprise the following steps: a. silicon chip dicing waste mortar solid-liquid separation, obtain solid sand material and liquid part; B. add discoloring agent, ion adsorbent and flocculating aids, solid-liquid separation in the liquid part obtained in step a, obtain polyoxyethylene glycol cutting Ethylene recov; C. the solid sand material obtained in step a is separated by magnetic separation and removes metal, obtains the mixture of silicon and silicon carbide; D. by mixture heating under vacuum at 1425-1550 DEG C of the silicon that obtains in step c and silicon carbide; Be cooled to screen filtration after room temperature, the material under collection screen obtains silicon carbide micro-powder, and the material on collection screen obtains silico briquette; Pulverize silico briquette and obtain silica flour.Recovery method provided by the invention very environmental protection, and comparatively thorough with being separated of silicon carbide to silicon, the purity of the polyoxyethylene glycol be recovered to, silicon carbide and silica flour is higher.
Description
Technical field
The present invention relates to a kind of recovery method of silicon chip dicing waste mortar.
Background technology
In the cutting process of single crystalline Si, polycrystalline Si, the metal powder produced after the silica flour produced when cutting silicon rod, broken silicon-carbide particle, steel wire grinding deposits in mortar, and form waste mortar, its cutting ability reduces greatly.Waste mortar is recycled, extracts silica flour, silicon carbide micro-powder and polyoxyethylene glycol wherein, recycling, object save energy can be played, cutting the waste.At present (1) centrifuging is mainly contained to the method that waste mortar reclaims: centrifugation, remove invalid silicon carbide abrasive broken in waste mortar and silica flour; (2) chemical method: adopt the silica flour in the pharmaceutical chemicals removal waste mortars such as acid/alkali and metallic impurity.
But the separation efficiency of centrifuging is lower, chemical method adopts a large amount of acid/alkali, and cost is high, has very large harm to environment; In addition, centrifuging, chemical method all can only reclaim polyoxyethylene glycol in mortar and silicon carbide micro-powder, to the high purity silicon powder energy effective recycling in waste mortar, cause great waste.The various methods seeking to reclaim silicon, carborundum powder and polyoxyethylene glycol are started in prior art.
CN101691224A discloses a kind of silicon chip cutting mortar recovery method, and (1) obtains efflux of solids and liquid stream by physics cyclonic separation; (2) liquid stream adopts by decolouring, ionic adsorption, filters, can obtain polyoxyethylene glycol; (3) efflux of solids is by gravity settling separation, obtains lighter silicon stream and heavier silicon carbide stream; (4) silicon stream washs, is drying to obtain silica flour; The macrobead screened out in silicon carbide stream obtains silicon carbide.But there is the silicon-carbide particle that particle diameter is less in waste mortar, close with silicon grain quality, cause gravity separation to reclaim the purity of silica flour and the silicon carbide micro-powder obtained lower; Especially be adsorbed on fine silica powder particle on silicon-carbide particle surface with by the silicon-carbide particle adsorbed, be often difficult to be separated completely.
CN101130237A discloses a kind of method reclaiming silica flour and carborundum powder from waste mortar, and (1) solid-liquid separation obtains mortar throw out, and add the suspension agent in acetone solution throw out and binding agent molecule, centrifugation obtains sand powder; (2) air-flow flotation, obtains silica flour and silicon carbide/metal mixed powder; (3) add the liquid of density between silicon and silicon carbide and carry out flotation, flotation thing is silica flour, and throw out is silicon carbide/metal mixed powder; (4) silica flour washing, drying obtain HIGH-PURITY SILICON particulate; Silicon carbide/metal mixed powder, isolates metal by magnetic separation, obtains carborundum powder.The method carries out flotation by selecting the liquid of density between silicon and silicon carbide, but the particle diameter of the silicon carbide be broken in waste mortar is very little, the silicon carbide micro-powder that in actual mechanical process, these particle diameters are little can be carried to float to liquid upper strata together or be dispersed in silica flour carrying process in the middle of liquid by silica flour and cause last layering not obvious, the silicon-carbide particle also containing 10-13wt% in the silica flour after adopting this method to be separated.Therefore, the purity of liquid floatation separation is still lower.Meanwhile, the various liquid costs adopted during liquid floatation are very high, and toxicity is very large, there is harm to human and environment.
Summary of the invention
The invention solves the silicon existed in prior art is separated not thorough with silicon carbide, and separating technology exists the technical problem of harm to human and environment.
The invention provides a kind of recovery method of silicon chip dicing waste mortar, comprise the following steps:
A. silicon chip dicing waste mortar solid-liquid separation, obtains solid sand material and liquid part;
B. add discoloring agent, ion adsorbent and flocculating aids, solid-liquid separation in the liquid part obtained in step a, obtain polyoxyethylene glycol cutting Ethylene recov;
C. the solid sand material obtained in step a is separated by magnetic separation and removes metal, obtains the mixture of silicon and silicon carbide;
D. by mixture heating under vacuum at 1425-1550 DEG C of the silicon that obtains in step c and silicon carbide; Be cooled to screen cloth vibration filtering after room temperature, the material under collection screen obtains silicon carbide micro-powder, and the material on collection screen obtains silico briquette; Pulverize silico briquette and obtain silica flour.
In the recovery method of silicon chip dicing waste mortar provided by the invention, first solid-liquid separation obtains solid sand material and liquid part, and liquid part obtains the higher polyoxyethylene glycol of purity by decolouring, ionic adsorption; Solid part is first separated by magnetic separation and removes metallic impurity, and then by pyroprocessing divided silicon and silicon carbide, without the need to using other pharmaceutical chemicalss, technique is simply controlled, to people, environment without harm; By selecting heating temperatures between silicon and silicon carbide fusing point to be separated, the complete vitreous clinker of silica flour, and silicon carbide is still pulverulence, thus silicon is thoroughly separated with silicon carbide, purity is very high.The present invention reclaims the polyoxyethylene glycol and silicon carbide that obtain, directly can continue on for silicon chip cutting; And the purity reclaiming the silica flour obtained is also higher, can be used as the starting material of silicon single crystal or the making of polysilicon silicon ingot.
Embodiment
The invention provides a kind of recovery method of silicon chip dicing waste mortar, comprise the following steps:
A. silicon chip dicing waste mortar solid-liquid separation, obtains solid sand material and liquid part;
B. add discoloring agent, ion adsorbent and flocculating aids, solid-liquid separation in the liquid part obtained in step a, obtain polyoxyethylene glycol cutting Ethylene recov;
C. the solid sand material obtained in step a is separated by magnetic separation and removes metal, obtains the mixture of silicon and silicon carbide;
D. by mixture heating under vacuum at 1425-1550 DEG C of the silicon that obtains in step c and silicon carbide; Be cooled to screen cloth vibration filtering after room temperature, the material under collection screen obtains silicon carbide micro-powder, and the material on collection screen obtains silico briquette; Pulverize silico briquette and obtain silica flour.
According to recovery method of the present invention, first silicon chip dicing waste mortar is carried out solid-liquid separation.Main containing silicon-carbide particle, the polyoxyethylene glycol in roughing sand slurry in the waste mortar of silicon chip cutting, the silica flour produced in working angles, broken silicon-carbide particle and metallic impurity.Solid-liquid separation can adopt plate-and-frame filter press, Membrane filtering machine or whizzer to complete.Because silicon, silicon carbide particle diameter are less, therefore the present invention preferably adopts whizzer to carry out solid-liquid separation.More preferably, in situation, during centrifugation, centrifugal rotational speed is 1000-2000rpm, centrifugation time 20-40min.
After solid-liquid separation, obtain solid sand material and liquid part, wherein main containing silica flour, silicon carbide micro-powder and metallic impurity in solid sand material, be mainly polyoxyethylene glycol in liquid part.Add discoloring agent, ion adsorbent and flocculating aids in liquid part, continue solid-liquid separation, namely obtain polyoxyethylene glycol cutting Ethylene recov, this polyoxyethylene glycol cutting Ethylene recov can continue to cut with silicon chip.
Under preferable case, the mode that discoloring agent and ion adsorbent can adopt substep to add; Such as, first in liquid part, add discoloring agent and flocculating aids, filtering centrifuge is adopted to carry out solid-liquid separation, remove filter residue, then in filtrate, ion adsorbent and flocculating aids is added, after reaction 1-10h, adopt filtering centrifuge to carry out solid-liquid separation, remove filter residue and can obtain polyoxyethylene glycol cutting Ethylene recov.Similarly, also ion adsorbent and flocculating aids can first be added, filtering separation; And then adding discoloring agent and flocculating aids, filtering separation obtains polyoxyethylene glycol.
Wherein, discoloring agent is gac and/or ammonium persulphate, and ion adsorbent is polyacrylamide or Poly Dimethyl Diallyl Ammonium Chloride, and flocculating aids is diatomite or perlite.Quality is than liquid part: discoloring agent: ion adsorbent: flocculating aids=(10-5): 1: 1: 1.
Main containing silica flour, silicon carbide micro-powder and metallic impurity in solid sand material.In the present invention, be first separated the metallic impurity removed in solid sand material by magnetic separation.Described magnetic separation is separated directly can adopt various magnetic grader in prior art.In magnetic separation separate solid sand material, obtain the mixture of silicon and silicon carbide.
In the present invention, adopt in high temperature sorting mixture silicon and silicon carbide.Silica flour fusing point is 1410 DEG C; Silicon carbide fusing point about 2700 DEG C, far above the fusing point of silica flour; Therefore when Heating temperature is between silica flour fusing point and silicon carbide fusing point, silica flour in mixture can melting be liquid-phase silicone stream, and silicon carbide is still pulverulence mutually, due to the interfacial tension of solid-liquid two-phase, the molten silicon stream aggregation closed on, to together, forms obvious separation surface with silicon carbide solid; Then mixture system is cooled to room temperature, the silicon stream caking be brought together, is formed the silico briquette that volume is relatively large, now silicon and silicon carbide can be separated by screen filtration.Be cooled in room temperature process, silico briquette surface can attach a small amount of silicon-carbide particle, the silicon-carbide particle that this attaches can be removed when screen cloth vibration filtering.
For preventing the oxygen in silica flour high temperature and air or nitrogen from reacting, described heat-processed need be carried out in a vacuum.In the present invention, heating under vacuum temperature is 1425-1550 DEG C.Under preferable case, the temperature of heating under vacuum is 1450-1480 DEG C, and vacuum tightness is not higher than-0.01MPa; The time of heating under vacuum is 3-6h.After heating under vacuum completes, to be cooledly to room temperature, discharge vacuum again, prevent silico briquette surface oxidation or nitrogenize.
In the present invention, the mixture of silicon and silicon carbide can be placed in crucible, then carry out heating under vacuum.Because heating under vacuum temperature is higher, so the present invention requires higher to crucible.Described crucible can adopt quartz crucible or alumina ceramic crucible, and crucible internal layer surface is covered with silicon nitride layer.Silicon nitride be heated in atmosphere 1450-1550 DEG C still very stable, therefore can meet the requirement of heating under vacuum of the present invention.In addition, silicon nitride layer can also prevent the bonding of mixture and crucible in high-temperature heating process.
After heating under vacuum completes, be first cooled to room temperature, then by screen cloth vibration filtering, the material on collection screen obtains the silico briquette of vitreous clinker, and the material under collection screen obtains being still the silicon carbide micro-powder of powder shaped, and this silicon carbide can continue on for silicon chip cutting.During screen cloth vibration filtering, because the particle diameter of silicon carbide micro-powder particle that adopts in roughing sand slurry is all at 100 μm and following, and the silico briquette size after melting reaches more than grade, the screen mesh size that therefore the present invention selects is 100-300 order, and screen cloth vibrational frequency is 40-80 time/min.
Sieve is collected the silico briquette obtained, various breaking method of the prior art can be adopted to pulverize, thus the silica flour be recycled, can be used as the starting material of silicon single crystal or the making of polysilicon silicon ingot.In the present invention, preferably adopt comminution by gas stream silico briquette, proceed in the mill chamber of micronizer mill by silico briquette, be crushed to required particle diameter.Stream pressure in mill chamber is 0.5-0.7MPa; The time 5-20min of comminution by gas stream.
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
By following composition preparation waste mortar: cutting liquid 44wt%, silicon carbide micro-powder 48wt%, silica flour 6.8wt%, metallic particles 1.2wt%.
(1) by 10Kg waste mortar with the rotating speed centrifugation 40min of 1400rpm, obtain liquid and solid sand material.440g polyacrylamide and 440g diatomite is added in liquid, with the rotating speed centrifuging of 1400rpm after stirring, collect filtrate to weigh 4.2kg, add the gac of 440g again as discoloring agent, with the rotating speed centrifuging of 1400rpm after stirring, collect the polyoxyethylene glycol that filtrate obtains, and weigh.
(2) with washed with de-ionized water solid sand material, and dry; By sand material by magnetic grader, except the metal in shakeout material, obtain the mixture of silicon and silicon carbide.
(3) pouring the silicon of step (2) and the mixture of silicon carbide into internal surface has in the quartz crucible of silicon nitride layer; The crucible that sand material is housed is proceeded in vacuum resistance furnace, 1450 DEG C of heating 3h; After being cooled to room temperature, crossing the screen cloth of 200 μm, sieve collects silico briquette, collects silicon carbide micro-powder under sieve, and weigh.
(4) silico briquette that sieve is collected is proceeded in micronizer mill, pulverize 5min under 0.7MPa, obtain silica flour, and weigh.
Comparative example 1
Adopt the step (1) identical with embodiment 1 and (2), obtain the mixture of silicon and silicon carbide, then proceed in settling centrifuge, pressurization 3bar, work 6h, obtain silicon and silicon carbide respectively from difference outlet, wash drying respectively and obtain silica flour, silicon carbide micro-powder, and weigh respectively.
Embodiment 2
Composition preparation waste mortar according to embodiment 1: cutting liquid 44wt%, silicon carbide micro-powder 48wt%, silica flour 6.8wt%, metallic particles 1.2wt%.
(1) by 10Kg waste mortar with the rotating speed centrifugation 30min of 2000rpm, obtain liquid and solid sand material.440g polyacrylamide and 440g diatomite is added in liquid, with the rotating speed centrifuging of 2000rpm after stirring, collect filtrate to weigh 3.9kg, add the gac of 440g again as discoloring agent, with the rotating speed centrifuging of 2000rpm after stirring, collect filtrate and obtain polyoxyethylene glycol, and weigh.
(2) with washed with de-ionized water solid sand material, and dry; By sand material by magnetic grader, except the metal in shakeout material, obtain the mixture of silicon and silicon carbide.
(3) pouring the silicon of step (2) and the mixture of silicon carbide into internal surface has in the quartz crucible of silicon nitride layer; The crucible that sand material is housed is proceeded in vacuum resistance furnace, 1500 DEG C of heating 3h; After being cooled to room temperature, crossing the screen cloth of 150 μm, sieve collects silico briquette, collects silicon carbide micro-powder under sieve, and weigh.
(4) silico briquette that sieve is collected is proceeded in micronizer mill, pulverize 5min under 0.5MPa, obtain silica flour, and weigh.
Comparative example 2
Adopt the step (1) identical with embodiment 2 and (2), obtain the mixture of silicon and silicon carbide, then proceed in methenyl bromide-alcohol mixing solutions (density is 2.75g/mL), ultrasonic oscillation 10min, leave standstill 30min, collect the floating matter on liquid, with hydrofluoric acid solution (5wt%) washing, drying, obtain silica flour, and weigh; Collect throw out in liquid, washing, drying, obtain silicon carbide micro-powder, and weigh.
The weighing results of embodiment 1-2 and comparative example 1-2 is as shown in table 1.
Table 1
| Sample | Indicated weight | S1 | DS1 | S2 | DS2 |
| Polyoxyethylene glycol (kg) | 4.4 | 3.5 | 3.5 | 3.2 | 3.2 |
| Silicon carbide (kg) | 4.8 | 3.9 | 3.5 | 4.2 | 3.9 |
| Silica flour (kg) | 0.68 | 0.6 | 0.9 | 0.65 | 0.75 |
As can be seen from the test result of upper table 1, recovery method of the present invention is all higher to the rate of recovery of polyoxyethylene glycol, silicon carbide and silica flour.Wherein the results contrast of S1 and DS1 can be found out, the silicon carbide still containing 32% in the silica flour adopting gravitational segregation to reclaim, reduces the rate of recovery of silicon carbide on the one hand, and the purity of silica flour is lower on the other hand; The results contrast of S2 and DS2 is found out, the silicon carbide also containing 10% in the silica flour of Heavy liquid floating, have impact on the purity of the silica flour of recovery.
Claims (7)
1. a recovery method for silicon chip dicing waste mortar, comprises the following steps:
A. silicon chip dicing waste mortar solid-liquid separation, obtains solid sand material and liquid part;
B. add discoloring agent, ion adsorbent and flocculating aids, solid-liquid separation in the liquid part obtained in step a, obtain polyoxyethylene glycol cutting Ethylene recov;
C. the solid sand material obtained in step a is separated by magnetic separation and removes metal, obtains the mixture of silicon and silicon carbide;
D. by mixture heating under vacuum at 1425-1550 DEG C of the silicon that obtains in step c and silicon carbide; Be cooled to screen cloth vibration filtering after room temperature, the material under collection screen obtains silicon carbide micro-powder, and the material on collection screen obtains silico briquette; Pulverize silico briquette and obtain silica flour.
2. recovery method according to claim 1, is characterized in that: in step a, and solid-liquid separation adopts centrifugation, and centrifugal rotational speed is 1000-2000rpm, centrifugation time 20-40min.
3. recovery method according to claim 1, is characterized in that: in step b, and discoloring agent is gac and/or ammonium persulphate, and ion adsorbent is polyacrylamide or Poly Dimethyl Diallyl Ammonium Chloride, and flocculating aids is diatomite or perlite; Mass ratio is liquid part: discoloring agent: ion adsorbent: flocculating aids=(10-5): 1: 1: 1.
4. recovery method according to claim 1, is characterized in that: in steps d, and the temperature of heating under vacuum is 1450-1480 DEG C, and vacuum tightness is not higher than-0.01MPa; The time of heating under vacuum is 3-6h.
5. the recovery method according to claim 1 or 4, is characterized in that: in steps d, and the heating under vacuum process of the mixture of silicon and silicon carbide is carried out in crucible; Described crucible internal layer surface is covered with silicon nitride layer, and crucible body material is quartz or alumina-ceramic.
6. the recovery method according to claim 1 or 4, is characterized in that: in steps d, and screen mesh size is 100-300 order, and screen cloth vibrational frequency is 40-80 time/min.
7. recovery method according to claim 1, is characterized in that: in steps d, and the method pulverizing silico briquette is comminution by gas stream, and stream pressure is 0.5-0.7MPa; The time of comminution by gas stream is 5-20min.
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103183349B (en) * | 2011-12-31 | 2015-03-11 | 浙江昱辉阳光能源有限公司 | Recovery method for silicon carbide and polyethyleneglycol cutting fluids in waste cutting mortar for silicon wafer |
| CN102757856B (en) * | 2012-07-30 | 2013-10-09 | 江苏阳帆机电设备制造有限公司 | Online recovery method for waste mortar produced in silicon wafer cutting |
| CN102977990B (en) * | 2012-11-16 | 2014-04-16 | 晶科能源有限公司 | Circulation process of distilled water in recycling process of silicon cutting fluids |
| CN103072988B (en) * | 2013-01-09 | 2014-07-16 | 烟台同立高科新材料股份有限公司 | Method for recycling boron carbide in sapphire grinding waste slurry |
| CN103072989B (en) * | 2013-01-09 | 2014-07-09 | 烟台同立高科新材料股份有限公司 | Method for recycling boron carbide in sapphire polishing waste slurry |
| CN104276574A (en) * | 2013-07-05 | 2015-01-14 | 河南省超贝工程设备有限公司 | Method for extraction of high-purity silicon from crystal silicon cutting waste liquid |
| CN104120026A (en) * | 2014-08-07 | 2014-10-29 | 佳明新材料科技有限公司 | Method for comprehensively recycling SiC cutting fluid waste mortar |
| CN105001969B (en) * | 2015-07-07 | 2017-12-01 | 阳光硅峰电子科技有限公司 | A kind of method for efficiently separating mortar based on temperature sensitivity |
| CN105924771A (en) * | 2016-05-12 | 2016-09-07 | 安徽理工大学 | Polypropylene material modified with photovoltaic crystal silicon processing waste and preparation method of polypropylene material |
| CN111004043A (en) * | 2019-12-16 | 2020-04-14 | 江苏诺明高温材料股份有限公司 | Method for preparing Si-Si3N4-SiC composite material by utilizing polycrystalline silicon waste material |
| CN116177552B (en) * | 2023-02-22 | 2023-11-17 | 江苏秉盛环保工程有限公司 | Silicon wafer cutting fluid silicon powder recovery system and process thereof |
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| CN1962435A (en) * | 2006-10-31 | 2007-05-16 | 锦州新世纪石英玻璃有限公司 | Production process of solar energy grade polysilicon |
| CN101691224A (en) * | 2009-09-22 | 2010-04-07 | 王勇 | Method for extracting silicon, silicon carbide and polyethylene glycol from silicon wafer slicing slurry |
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| CN1962435A (en) * | 2006-10-31 | 2007-05-16 | 锦州新世纪石英玻璃有限公司 | Production process of solar energy grade polysilicon |
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