CN101130237A - Method for recycling silica powder and carborundum powder from cut waste mortar - Google Patents
Method for recycling silica powder and carborundum powder from cut waste mortar Download PDFInfo
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- CN101130237A CN101130237A CNA2007100186369A CN200710018636A CN101130237A CN 101130237 A CN101130237 A CN 101130237A CN A2007100186369 A CNA2007100186369 A CN A2007100186369A CN 200710018636 A CN200710018636 A CN 200710018636A CN 101130237 A CN101130237 A CN 101130237A
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Abstract
The invention discloses an extracting method of high-purity silicon powder and carborundum powder from waste slurry of monocrystalline silicon cutting or grinding course, which comprises the following steps: separating solid from liquid for the waste slurry; using organic solvent to remove suspending agent and adhesive; doing gas float for solid sand; obtaining certain purity silicon powder; doing liquid float and gravity sorting for the silicon powder further; acidifying the silicon powder through acid; obtaining high-purity silicon powder; doing magnetic float for the composite powder of carborundum-metal through gravity; obtaining the pure carborundum powder. The invention can recycle high-purity silicon from waste slurry in the silicon bar cutting manufacturing course effectively, which changes waste into value with high receiving rate to solve the problem of resource shortage of high-purity silicon.
Description
Technical field
The present invention relates to a kind of method of from the waste mortar that the cutting or the grinding silicon wafer of monocrystalline silicon or polycrystalline silicon rod produce, extracting high-purity silicon powder and carborundum powder.
Background technology
Integrated circuit adopts multi-thread incision principle with the cutting preparation of the thin sheet products of substrate, solar cell substrate, drives the mortar that is made of silicon carbide abrasive with steel wire highly purified monocrystalline silicon or polycrystalline silicon rod are cut.Though this mortar can recycle,, sneak into the steel wire smear metal of silicon bits and trace in the mortar along with the carrying out of cutting process, the mortar cutting ability is reduced, the silicon wafer precision that causes obtaining worsens, and therefore needs constantly to discharge old mortar in working angles, and replenishes new mortar.These old mortars are generally taked the way of waste treatment.But valuable high-purity silicon powder also can lose along with the discarded of grinding mortar.As strategic resource, need import at 95% of China's high purity silicon, its main cause is that high-purity polycrystalline also can't scale be processed into industrial silicon in China.And useless cutting mortar the inside is mixed with the HIGH-PURITY SILICON powder of 6-7 weight %, and the cutting loss late of high purity silicon rods is up to 40 weight % in silicon rod cutting processing process.Therefore the high-purity silicon powder that will cut in the mortar extracts, and is further used for preparing the raw material of monocrystalline silicon or polysilicon, will be an important contribution for the resources effective utilization, can also solve the shortage of resources problem of high purity silicon.Silicon carbide micro-powder as abrasive passes through to extract recycling, also can play energy savings, the purpose that cuts the waste.The Japan Patent spy opens the recovery method that 2001-278612 discloses a silicon, the technology that is adopted is with after the waste mortar dehydration, remove dispersant and binding agent with organic solvent, carry out pickling again and remove metal and silica, adopt the way divided silicon of flow separation and carborundum to obtain silica flour at last.The pneumatic separation technology that adopts in the technology, the terminal velocity of particle are the principal elements that influences pneumatic separation, in stable upwelling, can't realize the separation that particle is taken as the leading factor by density in theory.Therefore the silica flour purity that reclaims of this invention has only 98 weight %, is mixed with the carborundum of 2 weight %, and the silica flour of acquisition can't reach the purity requirement that is used for preparing monocrystalline silicon or polysilicon block material, has reduced the ability of utilizing of recovery silica flour.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of process of separating and reclaim high-purity silica flour and carborundum powder from the waste mortar that the cutting or the grinding of monocrystalline or polycrystalline silicon rod produce.
For reaching above purpose, the present invention takes following technical scheme to be achieved:
A kind of method that reclaims silica flour and carborundum powder from the cutting waste mortar is characterized in that, comprises the steps:
A. earlier waste mortar is carried out Separation of Solid and Liquid and obtain the mortar sediment;
B. in resultant sediment, add suspending agent and binding agent molecule in the acetone solution mortar sediment, clean then and remove suspending agent and binding agent molecule,, obtain the sand powder again by centrifugation;
C. the sand powder is carried out the air-flow flotation, obtain low pure silicon powder and carborundum/metal mixed powder;
D. to the low pure silicon powder among the step c, add the liquid of density between Si and SiC and carry out flotation and gravity separation, silica flour is separated with carborundum/metal mixed powder, gained flotation thing is a silica flour, sediment is carborundum/metal mixed powder, again silica flour is carried out pickling, drying, promptly obtain the HIGH-PURITY SILICON particulate; Described liquid can be selected one or more mixed solutions of methylene bromide alcoholic solution, bromoform alcoholic solution, solution of calcium bromide in water, the zinc bromide aqueous solution and the calcium iodide aqueous solution for use;
E. with above-mentioned steps d gained carborundum/metal mixed powder. carry out magnetic separation after the drying and isolate metal, obtain carborundum powder.
In the such scheme, described liquid floatation and gravity separation are to leave standstill 5-30 minute after adopting supersonic oscillations, reclaim floating thing and sediment, then washing; Described pickling is that to add weight concentration in the flotation thing after washing be that 2～10% hydrofluoric acid stirs, and places 5-20 minute post rinse; Described density of liquid is 2.40-3.10g/cm
3
The present invention's method compared to existing technology, because the proportion of carborundum and steel is bigger in the waste mortar, in the silica flour after carrying out the air-flow flotation, silicon monomer and carborundum and powdered steel are separated fully, the purity of the silica flour that obtains also is not very high, can be mingled with the silicon-carbide particle of 2-10 weight %.Further adopt density between Si (2.33g/cm to this low pure silicon powder
3) and SiC (3.21g/cm
3) solution carry out liquid floatation and gravity separation because the difference of specific gravity of silicon and carborundum, Si powder come-up that density is lower and the higher SiC powder of density sink, and can sub-elect highly purified silica flour.Because the silicon monomer surface is oxidized easily, form silica, therefore use hydrofluoric acid to carry out pickling the silica flour that obtains again, finally can obtain highly purified silica flour.Simultaneously the carborundum of acquisition and the mixed powder of metal are used the magnetic force sorting, finally can obtain the silicon carbide powder of certain purity.
The process of from waste mortar, extracting separating high-purity silica flour and silicon carbide powder provided by the present invention, its advantage is, its yield is higher, the purity of the silicon monomer that reclaims can be greater than 98 weight %, identical with mother metal, highly purified silicon powder can be further as the raw material of preparation monocrystalline silicon or polysilicon bar, and silicon carbide powder can be prepared into slurry and be reused for the cutting of silicon rod or be used as other purposes.
The specific embodiment
Embodiment 1
The silicon chip that solar energy and integrated circuit are used is made in multi-thread cutting, and the dispersant in the abrasive material mortar that uses is oiliness, waste mortar consist of dispersion liquid 44 weight %, silicon carbide abrasive particles 48 weight %, silicon 6.4 weight %, metal 1.6 weight %.Get 1 ton of useless slicing slurry, earlier waste mortar is carried out centrifugation, the sediment 550kg that obtains is put into container, use acetone soaks and cleans, and by centrifugation, obtains the 540kg powder.The powder that obtains is carried out backing, feed in the air-flow flotation device, obtain silica flour 63kg and carborundum-metal mixed powder 470kg.Silica flour is further put into container, and (density is 2.40g/cm to add methylene bromide-alcohol mixed solution
3), and used supersonic oscillations 10 minutes, and left standstill 20 minutes, the floating thing above reclaiming, and wash, separate.The silica flour that obtains is put into container, adds hydrofluoric acid solution [2 weight % concentration], stirs, and places 5 minutes post rinses, drying, acquisition high-purity (carborundum＜200ppm, the silicon particle 60kg of metal＜100ppm).The mixed powder of the carbonization silicon-metal that obtains fed in the magnetic grader separate, obtain carborundum powder 450kg.
Embodiment 2
The silicon chip that solar energy and integrated circuit are used is made in multi-thread cutting, and the dispersant in the abrasive material mortar that uses is oiliness, waste mortar consist of dispersion liquid 44 weight %, silicon carbide abrasive particles 48 weight %, silicon 6.4 weight %, metal 1.6 weight %.Get 1 ton of useless cutting slurry, earlier waste material is carried out centrifugation, the sediment 550kg that obtains is put into container, use acetone soaks and cleans, and by centrifugation, obtains the 540kg powder.The powder that obtains is carried out backing, feed in the air-flow flotation device, obtain silica flour 63kg and carborundum-metal mixed powder 470kg.Silica flour is further put into container, and (density is adjusted into 2.40g/cm to add solution of calcium bromide in water
3), and used supersonic oscillations 10 minutes, and left standstill 15 minutes, the floating thing above reclaiming, and wash, separate.The silica flour that obtains is put into container, adds hydrofluoric acid [5 weight % concentration], stirs, and places 20 minutes post rinses, drying, acquisition high-purity (carborundum＜200ppm, the silicon particle 60kg of metal＜100ppm).The mixed powder of the carbonization silicon-metal that obtains fed in the magnetic grader separate, obtain carborundum powder 450kg.
Embodiment 3
The silicon chip that solar energy and integrated circuit are used is made in multi-thread cutting, and the dispersant in the abrasive material mortar that uses is oiliness, waste mortar consist of dispersion liquid 44 weight %, silicon carbide abrasive particles 48 weight %, silicon 6.4 weight %, metal 1.6 weight %.Get 1 ton of useless cutting slurry, earlier waste material is carried out centrifugation, the sediment 540kg that obtains is put into container, use acetone soaks and cleans, and by centrifugation, obtains the 530kg powder.The powder that obtains is carried out backing, feed in the air-flow flotation device, obtain silica flour 62kg and carborundum-metal mixed powder 460kg.Silica flour is further put into container, and bromoform-(density is adjusted into 2.45g/cm to the alcohol mixed solution in adding
3), and used supersonic oscillations 10 minutes, and left standstill 30 minutes, the floating thing above reclaiming, and wash, separate.The silica flour that obtains is put into container, adds hydrofluoric acid solution [5 weight % concentration], stirs, and places 15 minutes post rinses, drying, acquisition high-purity (carborundum＜180ppm, the silicon particle 58kg of metal＜100ppm).The mixed powder of the carbonization silicon-metal that obtains fed in the magnetic grader separate, obtain carborundum powder 440kg.
Embodiment 4
The silicon chip that solar energy and integrated circuit are used is made in multi-thread cutting, and the dispersant in the slip that uses is oiliness, waste mortar consist of dispersion liquid 42 weight %, silicon carbide abrasive particles 50 weight %, silicon 6.4 weight %, metal 1.6 weight %.Get 1 ton of useless cutting slurry, earlier waste material is carried out centrifugation, the sediment 540kg that obtains is put into container, use acetone soaks and cleans, and by centrifugation, obtains the 530kg powder.The powder that obtains is carried out backing, feed in the air-flow flotation device, obtain silica flour 62kg and carborundum-metal mixed powder 465kg.Silica flour is further put into container, and (density is adjusted into 3.10g/cm to add the calcium iodide aqueous solution
3), and used supersonic oscillations 10 minutes, and left standstill 10 minutes, the floating thing above reclaiming, and wash, separate.The silica flour that obtains is put into container, adds hydrogen fluorine solution [8 weight % concentration], stirs, and places 10 minutes post rinses, drying, acquisition high-purity (carborundum＜200ppm, the silicon particle 58kg of metal＜100ppm).The mixed powder of the carbonization silicon-metal that obtains fed in the magnetic grader separate, obtain carborundum powder 445kg.
Embodiment 5
The silicon chip that solar energy and integrated circuit are used is made in multi-thread cutting, and the dispersant in the slip that uses is oiliness, waste mortar consist of dispersion liquid 42 weight %, silicon carbide abrasive particles 48.4 weight %, silicon 8 weight %, metal 1.6 weight %.Get 1 ton of useless cutting slurry, earlier waste material is carried out centrifugation, the sediment 560kg that obtains is put into container, use acetone soaks and cleans, and by centrifugation, obtains the 530kg powder.The powder that obtains is carried out backing, feed in the air-flow flotation device, obtain silica flour 75kg and carborundum-metal mixed powder 475kg.Silica flour is further put into container, and (density is adjusted into 2.42g/cm to add the zinc bromide aqueous solution
3), and used supersonic oscillations 10 minutes, and left standstill 5 minutes, the floating thing above reclaiming, and wash, separate.The silica flour that obtains is put into container, adds hydrofluoric acid solution [10 weight %], stirs, and places 20 minutes post rinses, drying, acquisition high-purity (carborundum＜180ppm, the silicon particle 70kg of metal＜100ppm).The mixed powder of the carbonization silicon-metal that obtains fed in the magnetic grader separate, obtain carborundum powder 465kg.
Claims (4)
1. a method that reclaims silica flour and carborundum powder from the cutting waste mortar is characterized in that, comprises the steps:
A. earlier waste mortar is carried out Separation of Solid and Liquid and obtain the mortar sediment;
B. in resultant sediment, add suspending agent and binding agent molecule in the acetone solution mortar sediment, clean then and remove suspending agent and binding agent molecule,, obtain the sand powder again by centrifugation;
C. the sand powder is carried out the air-flow flotation, obtain low pure silicon powder and carborundum/metal mixed powder;
D. to the low pure silicon powder among the step c, add the liquid of density between Si and SiC and carry out flotation and gravity separation, silica flour is separated with carborundum/metal mixed powder, gained flotation thing is a silica flour, sediment is carborundum/metal mixed powder, again silica flour is carried out pickling, drying, promptly obtain the HIGH-PURITY SILICON particulate; Described liquid is selected one or more mixed solutions of methylene bromide alcoholic solution, bromoform alcoholic solution, solution of calcium bromide in water, the zinc bromide aqueous solution and the calcium iodide aqueous solution for use;
E. with above-mentioned steps d gained carborundum/metal mixed powder. carry out magnetic separation after the drying and isolate metal, obtain carborundum powder.
2. the method that reclaims silica flour and carborundum powder from the cutting waste mortar according to claim 1 is characterized in that, described liquid floatation and gravity separation are to leave standstill 5-30 minute after adopting supersonic oscillations, reclaim floating thing and sediment, then washing.
3. the method that from the cutting waste mortar, reclaims silica flour and carborundum powder according to claim 1, it is characterized in that, described pickling is that to add weight concentration in the flotation thing after washing be that 2～10% hydrofluoric acid solution stirs, and places rinsing again after 5-20 minute.
4. according to claim 1 or the 2 or 3 described methods that from the cutting waste mortar, reclaim silica flour and carborundum powder, it is characterized in that described density of liquid is 2.40-3.10g/cm
3
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| CNB2007100186369A CN100528488C (en) | 2007-09-11 | 2007-09-11 | Method for recycling silica powder and carborundum powder from cut waste mortar |
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| CN101130237A true CN101130237A (en) | 2008-02-27 |
| CN100528488C CN100528488C (en) | 2009-08-19 |
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| CN101792141A (en) * | 2010-04-06 | 2010-08-04 | 西安交通大学 | Treatment process of waste mortar in the processing course of silicon crystal |
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| CN104211064A (en) * | 2014-08-29 | 2014-12-17 | 平顶山易成新材料有限公司 | Impurity removing process for enhancing quality of silicon carbide fine micro powder |
| CN104211064B (en) * | 2014-08-29 | 2016-08-03 | 平顶山易成新材料有限公司 | A kind of impurity removal process promoting fine powder of silicon carbide quality |
| CN104650633A (en) * | 2015-02-10 | 2015-05-27 | 吕铁铮 | Preparation method of porous silicone coating |
| CN105032897A (en) * | 2015-07-30 | 2015-11-11 | 辰硕电子(九江)有限公司 | Method for regenerating power radiator through monocrystalline silicon waste |
| CN106082233A (en) * | 2016-06-15 | 2016-11-09 | 大工（青岛）新能源材料技术研究院有限公司 | The method reclaiming silica flour from diamond wire cutting slurry |
| CN109809414A (en) * | 2019-03-25 | 2019-05-28 | 江苏中江材料技术研究院有限公司 | A kind of solar panel cutting waste material recycling processing method |
| CN110282634A (en) * | 2019-08-12 | 2019-09-27 | 东北大学 | A method of micron silica is prepared with crystalline silicon diamond wire cutting waste material |
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