CN105883823A - Method for preparing silica sol from silica powder in silicon wafer cutting waste mortar by utilizing slurry reactor - Google Patents
Method for preparing silica sol from silica powder in silicon wafer cutting waste mortar by utilizing slurry reactor Download PDFInfo
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- CN105883823A CN105883823A CN201410784447.2A CN201410784447A CN105883823A CN 105883823 A CN105883823 A CN 105883823A CN 201410784447 A CN201410784447 A CN 201410784447A CN 105883823 A CN105883823 A CN 105883823A
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- silica flour
- waste mortar
- slurry
- phase reactor
- ludox
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Abstract
The invention discloses a method for preparing silica sol from silica powder in silicon wafer cutting waste mortar by utilizing a slurry reactor. The method has the advantages that silica powder recovered from the silicon wafer cutting waste mortar is used as a silicon source and is hydrolyzed to prepare silica sol; by recovering the waste mortar, the problem nagging the high-purity silicon industry is solved, the resource is effectively utilized and the product added value is increased while pollution is reduced; the adopted shell and tube slurry reactor can take full advantage of the impacting and supporting and floating effects of H2 released in the silica powder hydrolysis process on silica powder in the free ascending process in the tube and combine with the pushing effect of alkali liquor on the silica powder by entering from bottom to top to achieve homogenization in a reactant and dispenses with power consumption, so the shell and tube slurry reactor is more energy-saving and environment-friendly; the generated gas has the characteristics of small volume, uniform size and uniform distribution, so that the gas has a favourable effect of stirring a system.
Description
Technical field
The present invention relates to the preparation method of a kind of Ludox, be specifically related to a kind of reclaim the method that Ludox is prepared in simple substance silica flour hydrolysis.
Background technology
Silicon chip cutting process uses with carborundum (SiC) as abrasive material, and Polyethylene Glycol (PEG) is dispersant, and water is that the aqueous of solvent is cut
Cutting liquid, under tinsel drives, abrasive material particles is ground cutting Si.The crystal silicon of 44% is had in theory with powder in cutting process
End form is mixed into cutting slurry, actually this numerical value and is up to more than 50%.Discarded silica flour enters in cutting liquid in the way of dropping,
Adhering to and be enclosed in abrasive sand, making silicon carbide abrasive in mortar skid along material surface before cutting, cutting power declines, altogether
With forming discarded mortar.Waste mortar produced by silicon chip producer of annual China has hundreds of thousands ton, not only cause the wasting of resources but also
Bring huge environmental pollution.The problem recycling always puzzlement HIGH-PURITY SILICON industry of waste mortar.
CN103058154A discloses a kind of crystalline silicon processing waste mortar recovery silica flour and prepares the air flow bed reaction of beta-silicon nitride powder
Device, with crystalline silicon processing waste mortar reclaim silica flour as raw material, nitrogen as while unstripped gas be also silica flour and heat conveying
Carrier.Under stream condition, silicon powder nitride generates silicon nitride, and owing to reclaiming, silica flour particle diameter is less, generated time is shorter, and gained produces
Product are nanoscale.Specification in terms of emphasis elaborates reactor in this patent, and operating process is not discussed in detail.
CN102787011A discloses a kind of crystalline silicon processing waste mortar comprehensive treatment technique discharged without sewage and solid waste, will remove
Silicon after de-iron and Polyethylene Glycol, carborundum binary mortar, through dehydration, can proceed as follows: via nitride sinters carbon into respectively
SiClx-silicon nitride composite ceramics material；Nitridation or carbonization treatment, make silicon be converted into silicon nitride or carborundum.Regardless of which kind of operation side
Formula, is required for the high temperature of more than 1000 DEG C, although production process is discharged without sewage and solid waste, but the requirement to device is higher.
CN102557053A discloses a kind of method that washes utilizing crystalline silicon cutting waste mortar to reclaim prepares Ludox, is illustrated
Waste water be waste mortar waste water after first alkali cleaning, after i.e. alkali cleaning removing silicon powder obtains carborundum produce waste water.This waste water through from
Son exchange, regulation pH and decompression distillation obtain 15～the Ludox product of 35% (wt).Although the utilization to alkali Shen waste water is direct
Convenient, but ion exchange process can produce a large amount of waste water.CN103601191A discloses one and recycles silicon chip continuously
The method of silica flour in cutting processing waste mortar.Remove the binary mortar after cutting liquid, in conjunction with physics and chemical method, rely on carbonization
Gas (the H of silicon gravitational settling effect, silica flour hydrolysis and generation2) agitaion, it is achieved the recycling of mortar.This is special
The focusing on separation method of profit and to the quality of Ludox product without illustrating.
Summary of the invention
It is an object of the invention to make up the deficiency that prior art exists, it is provided that one utilizes slurry-phase reactor to be cut antiquated sand by silicon chip
The method that in slurry, Ludox prepared by silica flour.The method is so that in silicon chip dicing waste mortar, the silica flour of recovery is for silicon source, by the water of silica flour
Solution prepares Ludox.Recycling to waste mortar, solves a difficult problem for puzzlement HIGH-PURITY SILICON industry, makes resource obtain effective profit
With, reduce and improve added value of product while polluting.The shell and tube slurry-phase reactor used can make full use of and hydrolyze at silica flour
H released in process2, the process that freely rises in pipe is to the shock of silica flour and supporting effect, and combines alkali liquor by lower
On enter the impetus of silica flour realized the homogenization in reactant, non-power consumption, more energy efficient environmental protection.The gas produced
Body has that volume is little, size uniformly and the feature that is evenly distributed so that gas is to the stirring action of system advantageously.The present invention
Advantage be with silicon chip dicing waste mortar reclaim silica flour prepare Ludox for silicon source.Meanwhile, make full use of in silica flour hydrolytic process
Released in H2, the process that freely rises in pipe is to the shock of silica flour and supporting effect, and combines alkali liquor from bottom to top
Enter the impetus to silica flour and realize the homogenization in reactant.
The technical scheme provided according to the present invention, one utilizes slurry-phase reactor to be prepared Ludox by silica flour in silicon chip dicing waste mortar
Method, it is characterised in that said method comprising the steps of, its component according to the mass fraction:
A. gas-liquid-solid three-phase slurry-phase reactor based on accompanying drawing, alkali liquor is added by the alkali liquor mouth (1) of bottom, to reactor 1/5～1/2
After height, charge door (5) it is dividedly in some parts silica flour, adds thermal medium and entered by (4), (6) discharge, control anti-
Answering temperature is 50～90 DEG C；
B. silica flour reacts with water under base catalysis, generates silicic acid monomer and hydrogen, obtains silicon dioxide after silicic acid monomer polymerization
The hydrosol, hydrogen floats and forms bubbling stirring, and silicon powder particle relies on hydrogen to hold up in alkali liquor in suspended state；
C., after alkali liquor is full of reactor, close (3) place valve and stop being passed through alkali liquor, continue reaction 2～12 hours；
D. feed liquid is discharged by bottom discharge mouth (2), filter and get rid of unreacted silica flour, obtain product single dispersing Ludox.
Optimum, described slurry-phase reactor is shell and tube slurry-phase reactor；
Optimum, described silica flour is that silicon chip dicing waste mortar is treated to be obtained, and particle diameter is 100～600 mesh, and purity is 85～99%.
Optimum, it is 3～6 times that described silica flour is dividedly in some parts number of times, every minor tick 20～120 minutes.
Optimum, described aqueous slkali is NaOH, KOH, NH4The aqueous solution of one or more in OH, LiOH, its
Mass concentration is 0.05～2.5%.
Optimum, the addition speed of described aqueous slkali is 0.5mL/min～5mL/min.
Optimum, described silica flour is 50: 1～10: 1 with the mass ratio of alkali.
Optimum, the particle diameter of gained Ludox product is 10～45nm.
Accompanying drawing explanation
Fig. 1 is shell and tube slurry-phase reactor device schematic diagram
Fig. 2 is the scanning electron microscope (SEM) photograph of particle diameter 18nm Ludox
Fig. 3 is the grain size distribution of particle diameter 20nm Ludox
Fig. 4 is the scanning electron microscope (SEM) photograph of particle diameter 44nm Ludox
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
A kind of method utilizing slurry-phase reactor to be prepared Ludox by silica flour in silicon chip dicing waste mortar, its component according to the mass fraction,
Comprise the following steps that:
Silica flour particle diameter is 100 mesh, and purity is 85%, and addition is 10 parts, point 3 additions, every minor tick 60 minutes；Alkali
Liquid is made up of 0.05 part of NaOH and 99.95 parts of water, and feed liquor speed is 0.5mL/min；Silica flour is 50: 1 with the mass ratio of alkali,
Reaction temperature 75 DEG C, reacts 2 hours after stopping being passed through alkali liquor.The Ludox particle diameter obtained is 18nm.Fig. 2 is the present embodiment
Under obtain the scanning electron microscope (SEM) photograph of Ludox.
Embodiment 2
A kind of method utilizing slurry-phase reactor to be prepared Ludox by silica flour in silicon chip dicing waste mortar, its component according to the mass fraction,
Comprise the following steps that:
Silica flour particle diameter is 200 mesh, and purity is 90%, and addition is 100 parts, point 4 additions, every minor tick 20 minutes；Alkali
Liquid is made up of 0.5 part of NaOH, 0.5 part of KOH and 99 parts of water, and feed liquor speed is 1mL/min；Silica flour with the mass ratio of alkali is
20: 1, reaction temperature 50 DEG C, react 8 hours after stopping being passed through alkali liquor.The Ludox particle diameter obtained is about 20nm.Fig. 3
For obtaining the grain size distribution of Ludox under the present embodiment.
Embodiment 3
A kind of method utilizing slurry-phase reactor to be prepared Ludox by silica flour in silicon chip dicing waste mortar, its component according to the mass fraction,
Comprise the following steps that:
Silica flour particle diameter is 600 mesh, and purity is 99%, and addition is 120 parts, point 6 additions, every minor tick 120 minutes；
Alkali liquor is by 1 part of NaOH, 0.5 part of KOH, 1 part of NH4OH and 97.5 parts of water are constituted, and feed liquor speed is 5mL/min；Silica flour
It is 10: 1 with the mass ratio of alkali, reaction temperature 90 DEG C, react 12 hours after stopping being passed through alkali liquor.The Ludox particle diameter obtained is
About 44nm.Fig. 4 is the scanning electron microscope (SEM) photograph obtaining Ludox under the present embodiment.
The description of above-described embodiment should be considered explanation, it is easy to is understood by, can be without departing from illustrating the most in detail in the claims
The present invention in the case of use many changes and the combination of feature described above, this kind of change has been not to be regarded as a departure from this
Bright spirit and scope, and all such change be included in the range of claims below.
Claims (8)
1. utilize the method that slurry-phase reactor is prepared Ludox by silica flour in silicon chip dicing waste mortar, it is characterised in that preparation process comprises the steps:
A. gas-liquid-solid three-phase slurry-phase reactor based on accompanying drawing, alkali liquor is added by the alkali liquor mouth (1) of bottom, to reactor 1/5～1/2 height, it is dividedly in some parts silica flour by charge door (5), add thermal medium to be entered by (4), being discharged by (6), controlling reaction temperature is 50～90 DEG C；
B. silica flour reacts with water under base catalysis, generates silicic acid monomer and hydrogen, obtains silica hydrosol after silicic acid monomer polymerization, and hydrogen floats and forms bubbling stirring, and silicon powder particle relies on hydrogen to hold up in alkali liquor in suspended state；
C., after alkali liquor is full of reactor, close (3) place valve and stop being passed through alkali liquor, continue reaction 2～12 hours；
D. feed liquid is discharged by bottom discharge mouth (2), filter and get rid of unreacted silica flour, obtain product single dispersing Ludox.
2. according to utilizing, described in claims 1, the method that slurry-phase reactor prepared Ludox by silica flour in silicon chip dicing waste mortar, it is characterised in that described slurry-phase reactor is shell and tube slurry-phase reactor.
3. according to utilizing, described in claims 1, the method that slurry-phase reactor prepared Ludox by silica flour in silicon chip dicing waste mortar, it is characterised in that described silica flour is that silicon chip dicing waste mortar is treated to be obtained, and particle diameter is 100～600 mesh, and purity is 85～99%.
4. according to utilizing, described in claims 1, the method that slurry-phase reactor prepared Ludox by silica flour in silicon chip dicing waste mortar, it is characterised in that it is 3～6 times that silica flour is dividedly in some parts number of times, every minor tick 20～120 minutes.
5. according to utilizing, described in claims 1, the method that slurry-phase reactor prepared Ludox by silica flour in silicon chip dicing waste mortar, it is characterised in that described aqueous slkali is NaOH, KOH, NH4The aqueous solution of one or more in OH, LiOH, its mass concentration is 0.05～2.5%.
6. according to utilizing, described in claims 1, the method that slurry-phase reactor prepared Ludox by silica flour in silicon chip dicing waste mortar, it is characterised in that the addition speed of aqueous slkali is 0.5mL/min～5mL/min.
7. according to utilizing, described in claims 1, the method that slurry-phase reactor prepared Ludox by silica flour in silicon chip dicing waste mortar, it is characterised in that silica flour is 50: 1～10: 1 with the mass ratio of alkali.
8. according to utilizing, described in claims 1, the method that slurry-phase reactor prepared Ludox by silica flour in silicon chip dicing waste mortar, it is characterised in that the particle diameter of gained Ludox product is 10～45nm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410784447.2A CN105883823B (en) | 2014-12-16 | 2014-12-16 | The method that silica solution is prepared by silicon powder in silicon chip dicing waste mortar using slurry-phase reactor |
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| CN201410784447.2A CN105883823B (en) | 2014-12-16 | 2014-12-16 | The method that silica solution is prepared by silicon powder in silicon chip dicing waste mortar using slurry-phase reactor |
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| CN105883823B CN105883823B (en) | 2019-03-29 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1830777A (en) * | 2005-03-07 | 2006-09-13 | 中国科学院上海应用物理研究所 | Manufacturing method of silica sol and obtained silica sol |
| CN1974385A (en) * | 2006-12-08 | 2007-06-06 | 中国科学院宁波材料技术与工程研究所 | Prepn process of monodispersive silica sol |
| CN102173426A (en) * | 2011-01-06 | 2011-09-07 | 清华大学 | Preparation method for SiO2 sol with high evenness degree |
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2014
- 2014-12-16 CN CN201410784447.2A patent/CN105883823B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1830777A (en) * | 2005-03-07 | 2006-09-13 | 中国科学院上海应用物理研究所 | Manufacturing method of silica sol and obtained silica sol |
| CN1974385A (en) * | 2006-12-08 | 2007-06-06 | 中国科学院宁波材料技术与工程研究所 | Prepn process of monodispersive silica sol |
| CN102173426A (en) * | 2011-01-06 | 2011-09-07 | 清华大学 | Preparation method for SiO2 sol with high evenness degree |
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