CN106995254A - A kind of method that polyethylene glycol and silicon-carbide particle are reclaimed in silicon wafer cutting waste liquor - Google Patents
A kind of method that polyethylene glycol and silicon-carbide particle are reclaimed in silicon wafer cutting waste liquor Download PDFInfo
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- CN106995254A CN106995254A CN201710350921.4A CN201710350921A CN106995254A CN 106995254 A CN106995254 A CN 106995254A CN 201710350921 A CN201710350921 A CN 201710350921A CN 106995254 A CN106995254 A CN 106995254A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/34—Treatment of water, waste water, or sewage with mechanical oscillations
- C02F1/36—Treatment of water, waste water, or sewage with mechanical oscillations ultrasonic vibrations
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
- C02F1/488—Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2371/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2371/02—Polyalkylene oxides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
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Abstract
The invention discloses a kind of method that polyethylene glycol and silicon-carbide particle are reclaimed in silicon wafer cutting waste liquor, step is as follows：Step（1）Distilled water diluting, stirring are added in silicon wafer cutting waste liquor and is made into compound, is then soaked, same sex electrode slice is passed through to compound and ultrasonication is carried out, then the metal iron filings in compound are suctioned out with magnet；Step（2）Flocculant is added in compound, is stirred and isolated solids one, solids two and liquid；Step（3）Add distilled water diluting into carborundum suspension in solids one, then pass to same sex electrode slice, add sodium hydroxide and obtain carborundum crude product；Step（4）Silicon-carbide particle crude product is centrifuged, silicon-carbide particle finished product is obtained after drying；Step（5）To step（2）Obtained liquid filtered and heating evaporation dehydration after obtain polyethylene glycol finished product.Preparation technology flow of the present invention is relatively simple, reasonable and environmental protection, efficiently separates the silicon grain in cutting waste liquor, meets actual operation requirements.
Description
Technical field
The present invention relates to a kind of method that polyethylene glycol and silicon-carbide particle are reclaimed in silicon wafer cutting waste liquor, belong to waste liquid and return
Receive technical field.
Background technology
In Multi-wire wafer cutting process, cutting liquid, which is acted on, mainly to be disperseed, suspends, lubricating, cooling down, improving and cut effect
Rate, reduction cutting consumption etc..Existing silicon chip cutting fluid main component is polyethylene glycol and carborundum, therefore cuts production in silicon chip
Main component is polyethylene glycol and carborundum in raw cutting waste liquor, while also including a small amount of silicon bits or silicon grain（Generally
2%-5%）With micro metallic iron.Often there is the rate of recovery not in the existing recovery to polyethylene glycol in silicon crystal cutting fluid and carborundum
Height, the polyethylene glycol of recovery, the problems such as carborundum purity is not high.
As disclosed in 30 days January in 2008 of State Intellectual Property Office " the processing recovery method of monocrystalline silicon cutting waste liquor "（It is public
The number of opening：CN101113029）.This method comprises the following steps：（1）The waste liquid is handled with watery hydrochloric acid, and stirring is mixed into easy stream
Dynamic compound；（2）Mixed material heating carries out separation of solid and liquid, and water and polyethylene glycol are steamed, condensed, being dehydrated, reclaiming and must gather together
Ethylene glycol, the solid separated is the thick solid mixture of carborundum and silicon；（3）The thick solid mixture is carried out with water secondary
After cleaning, the secondary cleaning solid mixture of carborundum and silicon is obtained；（4）Then the mix acid liquor processing constituted with HNO3+HF, can
Reclaim to obtain silicon and carborundum.This method is easy to control, and equipment is simple, and cost is relatively low, but it is the problem of exist：One is pair
Carborundum and silicon grain can not be efficiently separated；Two be the mix acid liquor processing method constituted with HNO3+HF, easily causes fluorine dirty
Dye.Above-mentioned technique is further improved, such as to steam polyethylene glycol under vacuum temperature will to 200 degree or so, and this
When polyethylene glycol gone bad rubescent, lose use value.For this reason, it may be necessary to a kind of new technical scheme is designed, can be comprehensively
Overcome above-mentioned the deficiencies in the prior art.
The content of the invention
The present invention exactly in view of the deficienciess of the prior art, provide in a kind of silicon wafer cutting waste liquor reclaim polyethylene glycol and
The method of silicon-carbide particle, this method preparation technology flow is relatively simple, reasonable and environmental protection, efficiently separates the silicon in cutting waste liquor
Particle, meets actual operation requirements.
To solve the above problems, the technical solution used in the present invention is as follows：
A kind of method that polyethylene glycol and silicon-carbide particle are reclaimed in silicon wafer cutting waste liquor, it comprises the following steps：
Step（1）Quantitative distilled water diluting, stirring are added in silicon wafer cutting waste liquor, compound is made into, 10-20 points are then soaked
Clock, then the progress electrode effect of same sex electrode slice is passed through to the compound after immersion and ultrasonication is carried out, then suctioned out with magnet
Metal iron filings in compound；
Step（2）Flocculant is added in compound, is separated after stirring using centrifugal separator, obtain be with carborundum
The solids one of main component, the solids two by main component of silicon and using polyethylene glycol as the liquid of main component, wherein,
The addition of the flocculant is the 0.04-0.1% of cutting waste liquor quality；
Step（3）Quantitative distilled water diluting is added in solids one into carborundum suspension, then carborundum suspension is entered
Row is passed through same sex electrode slice and carries out electrode effect, then it is 11.5-13.5 to add sodium hydroxide to pH value in carborundum suspension,
It is heated to 65-90 DEG C to be reacted, reaction is cleaned to pH value to 7.5-8.5 after terminating with water, it is 1.5- to add acid to pH value
3.5, cleaned with water to pH value to 6.6-7, obtain carborundum crude product；
Step（4）Silicon-carbide particle crude product is centrifuged, and obtain silicon-carbide particle finished product after drying；
Step（5）To step（2）Obtained liquid is filtered, to obtaining poly- second two after the liquid heating evaporation dehydration after filtering
Alcohol finished product.
It is used as the improvement of above-mentioned technical proposal, step（2）Described in flocculant be polyacrylamide with diatomite with 1:5-
The mixture of 15 mass ratioes.
It is used as the improvement of above-mentioned technical proposal, step（5）Described in after filtering liquid heating evaporation dehydration be -
Under 0.05-0.1MPa pressure environment, 50-150 DEG C of completion is heated to.
It is used as the improvement of above-mentioned technical proposal, step（4）Resulting silicon-carbide particle finished product is carried out always according to its particle diameter
Classification is handled, and the classification processing is classified using gas flow sizing machine；Step（4）In centrifugation to carborundum crude product
It is to be separated using scraper type centrifuge.
It is used as the improvement of above-mentioned technical proposal, step（3）The sodium hydroxide of middle addition is sodium hydrate aqueous solution, the acid
It is aqueous sulfuric acid or aqueous hydrochloric acid solution.
Compared with prior art, implementation result of the invention is as follows by the present invention：
The method that polyethylene glycol and silicon-carbide particle are reclaimed in a kind of silicon wafer cutting waste liquor of the present invention, the present invention passes through to mixed
Compound carries out electrode and corresponding ultrasonication, the silicon bits sticked on silicon-carbide particles can be loosened to the full extent, in wadding
In centrifugation after solidifying agent flocculation, because silicon is different from the density of carborundum, a part of silicon can be separated in carborundum, institute
The silicon purity of separation is higher, on the one hand improves added value of product；On the other hand, step is reduced（3）The addition of middle sodium hydroxide,
Beneficial to reduction environmental protection treatment cost and saving water for cleaning；Metal iron filings in waste liquid are suctioned out with magnet, step is reduced（3）In acid
Addition, further beneficial to reduction environmental protection treatment cost and saving water for cleaning.
In addition, the technical program is first diluted using compound, the polyethylene glycol that carborundum is taken away when reducing separation of solid and liquid,
So as to improve the rate of recovery of polyethylene glycol；
Because compound is first through electrode and ultrasonication and except iron, the content of silicon and iron in carborundum crude product is reduced, is improved
The purity of carborundum, also reduces acid, the consumption of alkali.
Summary, the technical program has does not result in fluoride pollution in process of production, reclaims polyethylene glycol and carbonization
The efficiency and purity of silicon are high, and the features such as rational technology, environmental protection.
Embodiment
Illustrate present disclosure below in conjunction with specific embodiments.
First, flocculant is configured
With polyacrylamide and diatomite with 1:5 or 1:8 or 1:10 or 1:15 mass ratio mixing.
2nd, it is passed through same sex electrode
The principle mutually repelled according to same sex electrode, loosens silicon bits and the silicon grain sticked on silicon-carbide particles to the full extent.
3rd, ultrasonication, except iron
It is diluted with water, stirs in silicon wafer cutting waste liquor, be made into compound, compound carries out same sex electrode and ultrasonically treated, can
Mixture flow is passed through to the container for involving device equipped with same sex electrode and ultrasound, to loosen the silicon sticked on carborundum microparticle
Bits, then suction out the iron filings in compound with magnet.
4th, flocculation, separation of solid and liquid
Remix in material and add flocculant, after the completion of reaction, separation of solid and liquid is carried out using centrifugal separator, due to centrifugal separator
Solid-liquid can not only be separated, the solid of different densities can also be separated, therefore obtain using carborundum as main component
Solids one, the solids two by main component of silicon and using polyethylene glycol as the liquid of main component；Because solids two is led
It is silicon to want composition, and its impurity is mainly carborundum, therefore solids two can sell.
5th, carborundum is refined
Carborundum suspension is diluted with water into the solids one that separation of solid and liquid is obtained, the addition of water is solids quality
0.5-1.5 times, it is 11-13 that sodium hydroxide is added in carborundum suspension to pH, is heated to 60-90 DEG C and is reacted, this is anti-
The silicon in suspension should be mainly removed, after reaction terminates, is cleaned with water to pH to 7-8, it is 1-4 to add acid to pH value, uses water
Cleaning obtains carborundum crude product to pH value to 6.5-7；The purpose for adding acid is to remove the metal such as iron, copper in suspension.
6th, polyethylene glycol is refined
The liquid that separation of solid and liquid is obtained is filtered, to after filtering liquid heating evaporation dehydration after obtain polyethylene glycol into
Product, are under 0.05-0.1MPa pressure environment, to be heated to 50-150 DEG C of completion to the liquid heating evaporation dehydration after filtering.
7th, improvement project
Because the particle diameter of carborundum obtained above is mainly distributed on 1-25 microns of region, therefore as an improvement, to refining carbon
The finished silicon carbide product that SiClx is obtained carries out classification processing always according to its particle diameter.
Specific embodiment 1
A kind of method that polyethylene glycol and silicon-carbide particle are reclaimed in silicon wafer cutting waste liquor, it comprises the following steps：
Step（1）：Quantitative distilled water diluting, stirring are added in silicon wafer cutting waste liquor, compound is made into, 10 points are then soaked
Clock, then the progress electrode effect of same sex electrode slice is passed through to the compound after immersion and ultrasonication is carried out, then suctioned out with magnet
Metal iron filings in compound；
Step（2）：Flocculant is added in compound, is separated, obtained with carborundum using centrifugal separator after stirring
For the solids one of main component, the solids two by main component of silicon and using polyethylene glycol as the liquid of main component, its
In, the addition of the flocculant is the 0.04% of cutting waste liquor quality；
Step（3）：Quantitative distilled water diluting is added in solids one into carborundum suspension, then carborundum suspension is entered
Row is passed through same sex electrode slice and carries out electrode effect, then it is 11.5 to add sodium hydroxide to pH value in carborundum suspension, heating
Reacted to 65 DEG C, reaction is cleaned to pH value to 7.5 after terminating with water, it is 1.5 to add acid to pH value, is cleaned with water to pH
It is worth 6.6, obtains carborundum crude product；
Step（4）：Silicon-carbide particle crude product is centrifuged, and obtain silicon-carbide particle finished product after drying；
Step（5）：To step（2）Obtained liquid is filtered, to obtaining poly- second after the liquid heating evaporation dehydration after filtering
Glycol finished product.
Specifically, step（2）Described in flocculant be polyacrylamide with diatomite with 1：The mixture of 15 mass ratioes；Step
Suddenly（5）Described in after filtering liquid heating evaporation dehydration be under -0.05MPa pressure environment, be heated to 50 DEG C completion；
Step（4）Resulting silicon-carbide particle finished product carries out classification processing always according to its particle diameter, and the classification processing is to use air-flow
Grader is classified；Step（4）In to the centrifugation of carborundum crude product separated using scraper type centrifuge；Step
（3）The sodium hydroxide of middle addition is sodium hydrate aqueous solution, and the acid is aqueous sulfuric acid or aqueous hydrochloric acid solution.
The present invention can to the full extent loosen by carrying out electrode and corresponding ultrasonication to mixture and stick to carbon
Silicon bits on SiClx particulate,, can be by one because silicon is different from the density of carborundum in the centrifugation after flocculant flocculation
Divide silicon to be separated in carborundum, separated silicon purity is higher, on the one hand improve added value of product；On the other hand, step is reduced
（3）The addition of middle sodium hydroxide, beneficial to reduction environmental protection treatment cost and saving water for cleaning；Metal in waste liquid is suctioned out with magnet
Iron filings, reduce step（3）In the addition of acid, further beneficial to reduction environmental protection treatment cost and saving water for cleaning.
In addition, the technical program is first diluted using compound, the polyethylene glycol that carborundum is taken away when reducing separation of solid and liquid,
So as to improve the rate of recovery of polyethylene glycol；
Because compound is first through electrode and ultrasonication and except iron, the content of silicon and iron in carborundum crude product is reduced, is improved
The purity of carborundum, also reduces acid, the consumption of alkali.
Summary, the technical program has does not result in fluoride pollution in process of production, reclaims polyethylene glycol and carbonization
The efficiency and purity of silicon are high, and the features such as rational technology, environmental protection.
Specific embodiment 2
A kind of method that polyethylene glycol and silicon-carbide particle are reclaimed in silicon wafer cutting waste liquor, it comprises the following steps：
Step（1）：Quantitative distilled water diluting, stirring are added in silicon wafer cutting waste liquor, compound is made into, 15 points are then soaked
Clock, then the progress electrode effect of same sex electrode slice is passed through to the compound after immersion and ultrasonication is carried out, then suctioned out with magnet
Metal iron filings in compound；
Step（2）：Flocculant is added in compound, is separated, obtained with carborundum using centrifugal separator after stirring
For the solids one of main component, the solids two by main component of silicon and using polyethylene glycol as the liquid of main component, its
In, the addition of the flocculant is the 0.07% of cutting waste liquor quality；
Step（3）：Quantitative distilled water diluting is added in solids one into carborundum suspension, then carborundum suspension is entered
Row is passed through same sex electrode slice and carries out electrode effect, then it is 12.5 to add sodium hydroxide to pH value in carborundum suspension, heating
Reacted to 77.5 DEG C, reaction is cleaned to pH value to 8 after terminating with water, it is 2.5 to add acid to pH value, is cleaned with water to pH
It is worth 6.8, obtains carborundum crude product；
Step（4）：Silicon-carbide particle crude product is centrifuged, and obtain silicon-carbide particle finished product after drying；
Step（5）：To step（2）Obtained liquid is filtered, to obtaining poly- second after the liquid heating evaporation dehydration after filtering
Glycol finished product.
Specifically, step（2）Described in flocculant be polyacrylamide with diatomite with the mixture of 2.5-15 mass ratioes；
Step（5）Described in after filtering liquid heating evaporation dehydration be under 0.025MPa pressure environment, be heated to 100 DEG C it is complete
Into；Step（4）Resulting silicon-carbide particle finished product carries out classification processing always according to its particle diameter, and the classification processing is to use gas
Current classifier is classified；Step（4）In to the centrifugation of carborundum crude product separated using scraper type centrifuge；Step
Suddenly（3）The sodium hydroxide of middle addition is sodium hydrate aqueous solution, and the acid is aqueous sulfuric acid or aqueous hydrochloric acid solution.
The present invention can to the full extent loosen by carrying out electrode and corresponding ultrasonication to mixture and stick to carbon
Silicon bits on SiClx particulate,, can be by one because silicon is different from the density of carborundum in the centrifugation after flocculant flocculation
Divide silicon to be separated in carborundum, separated silicon purity is higher, on the one hand improve added value of product；On the other hand, step is reduced
（3）The addition of middle sodium hydroxide, beneficial to reduction environmental protection treatment cost and saving water for cleaning；Metal in waste liquid is suctioned out with magnet
Iron filings, reduce step（3）In the addition of acid, further beneficial to reduction environmental protection treatment cost and saving water for cleaning.
In addition, the technical program is first diluted using compound, the polyethylene glycol that carborundum is taken away when reducing separation of solid and liquid,
So as to improve the rate of recovery of polyethylene glycol；
Because compound is first through electrode and ultrasonication and except iron, the content of silicon and iron in carborundum crude product is reduced, is improved
The purity of carborundum, also reduces acid, the consumption of alkali.
Summary, the technical program has does not result in fluoride pollution in process of production, reclaims polyethylene glycol and carbonization
The efficiency and purity of silicon are high, and the features such as rational technology, environmental protection.
Specific embodiment 3
A kind of method that polyethylene glycol and silicon-carbide particle are reclaimed in silicon wafer cutting waste liquor, it comprises the following steps：
Step（1）：Quantitative distilled water diluting, stirring are added in silicon wafer cutting waste liquor, compound is made into, 20 points are then soaked
Clock, then the progress electrode effect of same sex electrode slice is passed through to the compound after immersion and ultrasonication is carried out, then suctioned out with magnet
Metal iron filings in compound；
Step（2）：Flocculant is added in compound, is separated, obtained with carborundum using centrifugal separator after stirring
For the solids one of main component, the solids two by main component of silicon and using polyethylene glycol as the liquid of main component, its
In, the addition of the flocculant is the 0.1% of cutting waste liquor quality；
Step（3）：Quantitative distilled water diluting is added in solids one into carborundum suspension, then carborundum suspension is entered
Row is passed through same sex electrode slice and carries out electrode effect, then it is 13.5 to add sodium hydroxide to pH value in carborundum suspension, heating
Reacted to 90 DEG C, reaction is cleaned to pH value to 8.5 after terminating with water, it is 3.5 to add acid to pH value, is cleaned with water to pH
It is worth 7, obtains carborundum crude product；
Step（4）：Silicon-carbide particle crude product is centrifuged, and obtain silicon-carbide particle finished product after drying；
Step（5）：To step（2）Obtained liquid is filtered, to obtaining poly- second after the liquid heating evaporation dehydration after filtering
Glycol finished product.
Specifically, step（2）Described in flocculant be polyacrylamide with diatomite with the mixture of 5-15 mass ratioes；Step
Suddenly（5）Described in after filtering liquid heating evaporation dehydration be under 0.1MPa pressure environment, be heated to 150 DEG C completion；
Step（4）Resulting silicon-carbide particle finished product carries out classification processing always according to its particle diameter, and the classification processing is to use air-flow
Grader is classified；Step（4）In to the centrifugation of carborundum crude product separated using scraper type centrifuge；Step
（3）The sodium hydroxide of middle addition is sodium hydrate aqueous solution, and the acid is aqueous sulfuric acid or aqueous hydrochloric acid solution.
The present invention can to the full extent loosen by carrying out electrode and corresponding ultrasonication to mixture and stick to carbon
Silicon bits on SiClx particulate,, can be by one because silicon is different from the density of carborundum in the centrifugation after flocculant flocculation
Divide silicon to be separated in carborundum, separated silicon purity is higher, on the one hand improve added value of product；On the other hand, step is reduced
（3）The addition of middle sodium hydroxide, beneficial to reduction environmental protection treatment cost and saving water for cleaning；Metal in waste liquid is suctioned out with magnet
Iron filings, reduce step（3）In the addition of acid, further beneficial to reduction environmental protection treatment cost and saving water for cleaning.
In addition, the technical program is first diluted using compound, the polyethylene glycol that carborundum is taken away when reducing separation of solid and liquid,
So as to improve the rate of recovery of polyethylene glycol；
Because compound is first through electrode and ultrasonication and except iron, the content of silicon and iron in carborundum crude product is reduced, is improved
The purity of carborundum, also reduces acid, the consumption of alkali.
Summary, the technical program has does not result in fluoride pollution in process of production, reclaims polyethylene glycol and carbonization
The efficiency and purity of silicon are high, and the features such as rational technology, environmental protection.
Above content is made for the present invention in conjunction with specific embodiments describes in detail, it is impossible to assert that the present invention is specific real
Apply and be only limitted to these explanations.For those skilled in the art, before present inventive concept is not departed from
Put, some simple deduction or replace can also be made, the scope of protection of the invention should be all considered as belonging to.
Claims (5)
1. the method for polyethylene glycol and silicon-carbide particle is reclaimed in a kind of silicon wafer cutting waste liquor, it is characterised in that：It includes following
Step：
Step（1）：Quantitative distilled water diluting, stirring are added in silicon wafer cutting waste liquor, compound is made into, then soaks 10-20
Minute, then the progress electrode effect of same sex electrode slice is passed through to the compound after immersion and ultrasonication is carried out, then inhaled with magnet
The metal iron filings gone out in compound；
Step（2）：Flocculant is added in compound, is separated, obtained with carborundum using centrifugal separator after stirring
For the solids one of main component, the solids two by main component of silicon and using polyethylene glycol as the liquid of main component, its
In, the addition of the flocculant is the 0.04-0.1% of cutting waste liquor quality；
Step（3）：Quantitative distilled water diluting is added in solids one into carborundum suspension, then carborundum suspension is entered
Row is passed through same sex electrode slice and carries out electrode effect, then it is 11.5-13.5 to add sodium hydroxide to pH value in carborundum suspension,
It is heated to 65-90 DEG C to be reacted, reaction is cleaned to pH value to 7.5-8.5 after terminating with water, it is 1.5- to add acid to pH value
3.5, cleaned with water to pH value to 6.6-7, obtain carborundum crude product；
Step（4）：Silicon-carbide particle crude product is centrifuged, and obtain silicon-carbide particle finished product after drying；
Step（5）：To step（2）Obtained liquid is filtered, to obtaining poly- second after the liquid heating evaporation dehydration after filtering
Glycol finished product.
2. reclaiming the method for polyethylene glycol and silicon-carbide particle in a kind of silicon wafer cutting waste liquor according to claim 1, it is special
Levy and be：Step（2）Described in flocculant be polyacrylamide with diatomite with 1:The mixture of 5-15 mass ratioes.
3. reclaiming the method for polyethylene glycol and silicon-carbide particle in a kind of silicon wafer cutting waste liquor according to claim 1, it is special
Levy and be：Step（5）Described in after filtering liquid heating evaporation dehydration be under -0.05-0.1MPa pressure environment, plus
Hot to 50-150 DEG C completion.
4. reclaiming the method for polyethylene glycol and silicon-carbide particle in a kind of silicon wafer cutting waste liquor according to claim 1, it is special
Levy and be：Step（4）Resulting silicon-carbide particle finished product carries out classification processing always according to its particle diameter, and the classification processing is to adopt
It is classified with gas flow sizing machine；Step（4）In to the centrifugation of carborundum crude product divided using scraper type centrifuge
From.
5. reclaiming the method for polyethylene glycol and silicon-carbide particle in a kind of silicon wafer cutting waste liquor according to claim 1, it is special
Levy and be：Step（3）The sodium hydroxide of middle addition is sodium hydrate aqueous solution, and the acid is that aqueous sulfuric acid or hydrochloric acid are water-soluble
Liquid.
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