CN102515180A - Method for preparing large particle size silica sol and superfine silicon carbide using tailings in waste mortar - Google Patents
Method for preparing large particle size silica sol and superfine silicon carbide using tailings in waste mortar Download PDFInfo
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- CN102515180A CN102515180A CN2011104162069A CN201110416206A CN102515180A CN 102515180 A CN102515180 A CN 102515180A CN 2011104162069 A CN2011104162069 A CN 2011104162069A CN 201110416206 A CN201110416206 A CN 201110416206A CN 102515180 A CN102515180 A CN 102515180A
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Abstract
The invention discloses a method for preparing large particle size silica sol and superfine silicon carbide using tailings in resource recycling process of silicon wafer cutting waste mortar, which comprises the following six steps: de-ironing, primary conversion, secondary conversion, trinary conversion, superfine silicon carbide collection, and silica sol parent nucleus growth. The method disclosed by the invention realizes comprehensive utilization of silicon component in tailings and resource recycling of superfine silicon carbide micro powder, and can be used for industrial production with good economic and environmental benefits.
Description
Technical field
The present invention relates to a kind of method of utilizing tailings material in the crystal silicon cutting waste mortar resource utilization removal process to prepare big particle diameter silicon sol and superfine silicon carbide.Its Application Areas mainly is the environment protection that crystal silicon cutting waste mortar resource utilization reclaims industry, realizes that the comprehensive utilization of silicon component resource and the resource utilization of superfine silicon carbide reclaim.
Background technology
Silicon chip is the important foundation of development solar energy industry.Along with developing rapidly of solar energy industry in the global range, silicon chip demand and amount of finish gather growth.According to the industry statistic data, Chinese silicon chip production capacity has been sure to occupy the whole world from 2008 the first, and the nearly 14GW of domestic silicon chip aggregated capacity in 2010 has accounted for global aggregated capacity more than 50%.
The line cutting is the current mode that present silicon chip is in the world produced.The process of line cutting processing depends on being used of crystal silicon cutting liquid (claim not only cutting fluid, suspension-s), silicon carbide micro-powder (but also claiming abrasive material, cutting sand), simultaneously can a large amount of crystal silicon cutting waste mortar of association.According to the average state of the art of domestic silicon chip enterprise, the 1MW silicon chip need consume 12 tons of crystalline silicons approximately, in cutting process, produces about 7.6～7.9 tons of cutting waste mortars.In the line cutting process that silicon chip is produced, damaged as silit component part in cutting process of abrasive material, the size distribution situation changes; Silicon carbide micro-powder total amount in cutting waste mortar system more than the GC2000# can reach 3-5% and (be referred to as: superfine silicon carbide micro powder).On the other hand, also produce a large amount of silica flours (cutting slit) in the time of silicon rod cutting processing silicon chip, enter into the cutting mortar in the lump; The content of silicon component can reach 8%-10% in the cutting waste mortar.Statistic data according to domestic silicon chip industry in 2010; Expected 2012; Domestic silicon chip enterprise contracts cutting waste mortar total amount can reach 2,000,000 tons, and wherein the stock number of silicon component will reach 16～200,000 tons, the stock number of superfine silicon carbide micro powder and will reach ten thousand tons of 6-10.
As everyone knows, the silicon chip production link has and surpasses 50% crystal silicon and be cut into silica flour and get into slurry, effectively reclaims and comprehensive utilization technique owing to lack, and so a large amount of crystal silicon materials is arranged by losing in vain every year.In the recycling recovery process of cutting waste mortar; A large amount of superfine silicon carbide micro powders can be deposited in the tailings material and (often mix with the silicon component); Most cases is that the mode through chemical washing changes into water-soluble substances with the silicon component, and superfine silicon carbide micro powder is then directly as solid waste.
Silicon single crystal, polysilicon, silit etc. all are through high energy consumption, expensive obtaining.If can be to the tailings material in the cutting waste mortar resource utilization removal process; Silicon component that is wherein comprised and superfine silicon carbide component are reclaimed or fully utilize; Make it embody due recycling economy and be worth, have extremely huge economy, society and environmental benefit undoubtedly.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing tailings material in the crystal silicon cutting waste mortar resource utilization removal process to prepare big particle diameter silicon sol and superfine silicon carbide.General, the tailings material in the crystal silicon cutting waste mortar resource utilization removal process is mainly the mixture of silit, silicon component, metal component.Each component content (w/w) in the tailings material that is produced in state's incised waste mortar resource utilization removal process at present: (wherein 60-95% is D to silit 5-15%
50Superfine silicon carbide below 5 μ m), the silicon component (comprises Si and SiO
2) 70-85%, cutting liquid component 1-10%, metal component 0.5-7.5%.The present invention relates to the comprehensive utilization of silicon component in the tailings material and the resource utilization of superfine silicon carbide micro powder are reclaimed.
Tailings material involved in the present invention is to refer in particular to silicon carbide micro-powder content at the sand material mixture (w/w) below 15%.Surpass 15% sand material system to SiC content, still have important silit resource utilization and be worth, can continue to reclaim silicon carbide micro-powder, and finally obtain the tailings material of 15% following carborundum content through separation method commonly used.
The objective of the invention is to realize like this: a kind of method of utilizing waste mortar tailings material to prepare big particle diameter silicon sol and superfine silicon carbide is characterized in that this method may further comprise the steps:
(1) deironing: the tailings material is removed the metal component in the tailings material through Magnet Separater, reduce to (sand material solids relatively) below 0.5% up to the total content of metal component; Through the further deironing of pickling, reduce to (sand material solids relatively) below 0.1% up to the total content of metal component; Through membrane-concentrated, in liquid concentrator, add clear water again, be mixed with the mixed slurry that solid content is 5-50%;
(2) once transform: in above-mentioned mixed slurry, add a certain amount of sodium silicate solution or sodium hydroxide solution as catalyzer, under 60-140 ℃, pressure 0.7-8atm, the sol solutions after obtaining behind the reaction 0.5-8h once to transform;
(3) twice transformation: the sol solutions after the above-mentioned once conversion is concentrated through accurate filter, and filtrate is for once transforming resulting silicon sol; Add clear water at filtering and concentrating liquid, be mixed with the mixed slurry of 5-50% again; Add a certain amount of sodium silicate solution or sodium hydroxide solution again as catalyzer, under 100-140 ℃, pressure 1-10atm, obtain the sol solutions behind the twice transformation behind the reaction 0.5-8h;
Transform for (4) three times: the sol solutions behind the above-mentioned twice transformation is concentrated through accurate filter, and filtrate is the resulting silicon sol of twice transformation; Directly add remaining silicon component (silica flour and silicon-dioxide) in the sheet alkali transformation system of excessive 20-50% at filtering and concentrating liquid, the mixed solution after obtaining transforming for three times; Concentrate through accurate filter again, add the acid neutralization in the gained filtrate or sodium silicate solution is wherein changed into active silicic acid solution through highly acidic resin;
(5) superfine silicon carbide is collected: will transform back mixed solution gained liquid concentrator after concentrating for (4) three times and carry out drying, and collect and obtain superfine silicon carbide;
(6) the silicon sol parent nucleus increases: merge once conversion, the resulting silicon sol of twice transformation as parent nucleus; Gradual slow adds resulting active silicic acid solution and 1-10% concentration hydrogen sodium hydroxide solution in the step (4), increases through parent nucleus to obtain the bigger silicon sol of particle diameter.
A kind of method of utilizing waste mortar tailings material to prepare big particle diameter silicon sol and superfine silicon carbide according to the invention is characterized in that: waste mortar comprises the crystal silicon cutting waste mortar of photovoltaic industry and the crystal silicon cutting waste mortar of electron trade.
A kind of method of utilizing waste mortar tailings material to prepare big particle diameter silicon sol and superfine silicon carbide according to the invention is characterized in that: the addition of said sodium silicate solution of step (2) (3) or sodium hydroxide solution (conversion is water glass or sodium hydroxide) is the 2-15% (w/w) of amount of solid in the mixed slurry.
A kind of method of utilizing waste mortar tailings material to prepare big particle diameter silicon sol and superfine silicon carbide according to the invention is characterized in that: the D of said big particle diameter silicon sol
50>=70nm.
A kind of method of utilizing waste mortar tailings material to prepare big particle diameter silicon sol and superfine silicon carbide according to the invention is characterized in that: the D of said superfine silicon carbide
50≤5 microns.
Embodiment
Below in conjunction with embodiment the present invention is further specified.
Embodiment 1:
Get the tailings material in the 27.5Kg crystal silicon cutting waste mortar resource utilization removal process, through detection, wherein silicon component (Si+SiO
2) content 84.6%, carborundum content 10.4%, cutting liquid component content 2.5%, metal component content 2.5% (wherein being iron powder more than 97%).
Utilize 12000 Gausses' bar magnet that above-mentioned tailings material is carried out magnetic separation, the metal component content of sand material is 0.42% after the detection magnetic separation; Add the 50g vitriol oil again and further remove the metal component in the sand material system, after pickling, the washing, metal component content is 0.07% in the detection sand material; Concentrate and in above-mentioned mixed slurry, to add the 200kg pure water for solid content 70% mixed slurry is total to 24kg through ceramic membrane again, be heated to 90 ℃; Under the normal pressure; Silica flour is carried out activation, add sodium silicate solution 75kg (water glass content 3.6%, modulus 3.4; PH 11.7), the sol solutions after obtaining once to transform behind the continuation reaction 7.5h.
Sol solutions after the above-mentioned once conversion is concentrated through accurate filter, collect filtrate and liquid concentrator.Filtrate is for once transforming resulting silicon sol, and the transformation efficiency that calculates the silicon component is 38%.Carry out agitation and dilution with adding the 100kg pure water in the gained 14.5kg liquid concentrator, be heated to 110 ℃, under the pressure 2.5atm; Drip sodium silicate solution 35kg (water glass content 3.6% with fed-batch mode; Modulus 3.4, pH 11.7), continue the sol solutions reaction obtains twice transformation after 7 hours after.
Sol solutions behind the above-mentioned twice transformation is concentrated through accurate filter, collect filtrate and liquid concentrator.Filtrate is the resulting silicon sol of twice transformation, and the total conversion rate that calculates silicon component after first and second conversion reaches 74.5%.In collected 8.5kg liquid concentrator, add 1.25kg sodium hydroxide with transformation system in remaining silicon component (Si and SiO
2) be water glass; After secondary filter, filtrate obtains the rare silicate solution 104.5kg of activatory after through strongly acidic styrene's Zeo-karb, obtains silicon carbide micro-powder 2.05kg after liquid concentrator is spray-dried.
Through detecting, the carborundum content of gained silicon carbide micro-powder is 96.5%, D
50Value is 3.4 microns.
Merge the resulting silicon sol liquid of first and second conversion and obtain the 415.5kg silicon sol, through detecting its particle diameter D
90Value is 82.7 microns, D
50Value is 73.5 microns, D
3Value is 65.7 microns.With above-mentioned silicon sol system is parent nucleus, adds the rare silicate solution of activation of aforementioned gained and 4% sodium hydroxide solution, and the control parent nucleus increases and avoids new nuclear to produce, and obtains the silicon sol 522.5kg of bigger particle diameter behind the Dropwise 5 h.
Through detecting, gained silicon strength of solution is 7.8%, particle diameter D
90Value is 128.6 microns, D
50Value is 112 microns, D
3Value is 95.4 microns.
Embodiment 2:
Get the tailings material in the 250Kg crystal silicon cutting waste mortar resource utilization removal process, through detection, wherein silicon component (Si+SiO
2) content 84.3%, carborundum content 10.7%, cutting liquid component content 2.4%, metal component content 2.6% (wherein being iron powder more than 98%).
Utilize 15000 Gausses' Magnet Separater that above-mentioned tailings material is carried out magnetic separation, the metal component content of sand material is 0.32% after the detection magnetic separation; Add the 500g vitriol oil again and further remove the metal component in the sand material system, after pickling, the washing, metal component content is 0.05% in the detection sand material; Concentrate and in above-mentioned mixed slurry, to add the 2000kg pure water for solid content 87% mixed slurry is total to 245kg through ceramic membrane again, be heated to 85 ℃; Under the pressure 2atm; Silica flour is carried out activation, add sodium silicate solution 750kg (water glass content 3.7%, modulus 3.4; PH 11.5), the sol solutions after obtaining once to transform behind the continuation reaction 8h.
Sol solutions after the above-mentioned once conversion is concentrated through accurate filter, collect filtrate and liquid concentrator.Filtrate 3015.5Kg is for once transforming resulting silicon sol, and the transformation efficiency that calculates the silicon component is 36.2%.Carry out agitation and dilution with adding the 1200kg pure water in the gained 168.5kg liquid concentrator, be heated to 115 ℃, under the pressure 4atm; Drip sodium silicate solution 420kg (water glass content 3.7% with fed-batch mode; Modulus 3.4, pH 11.5), continue the sol solutions reaction obtains twice transformation after 10 hours after.
Sol solutions behind the above-mentioned twice transformation is concentrated through accurate filter, collect filtrate and liquid concentrator.Filtrate 1724.6Kg is the resulting silicon sol of twice transformation, and the total conversion rate that calculates silicon component after first and second conversion reaches 85.7%.In collected 60.2kg liquid concentrator, add 10.5kg sodium hydroxide with transformation system in remaining silicon component (Si and SiO
2) be water glass; After secondary filter, filtrate adds the 12.8Kg vitriol oil and forms the rare silicate solution of activatory, obtains silicon carbide micro-powder 20.15kg after liquid concentrator is spray-dried.
Through detecting, the carborundum content of gained silicon carbide micro-powder is 97.2%, D
50Value is 3.3 microns.
Merge the resulting silicon sol liquid of first and second conversion and obtain the 4740.1kg silicon sol, through detecting its particle diameter D
90Value is 81.3 microns, D
50Value is 62.8 microns, D
3Value is 55.4 microns.With above-mentioned silicon sol system is parent nucleus, adds the rare silicate solution of activation of aforementioned gained and 4% sodium hydroxide solution, controls the parent nucleus growth and also avoids new nuclear to produce, and obtains the silicon sol 5112.4kg of bigger particle diameter behind the dropping 7h.
Through detecting, the gained thickness of silica gel is 8.2%, particle diameter D
90Value is 112.3 microns, D
50Value is 105.2 microns, D
3Value is 97.3 microns.
Claims (5)
1. method of utilizing waste mortar tailings material to prepare big particle diameter silicon sol and superfine silicon carbide is characterized in that this method may further comprise the steps:
(1) deironing: the tailings material is removed the metal component in the tailings material through Magnet Separater, reduce to (sand material solids relatively) below 0.5% up to the total content of metal component; Through the further deironing of pickling, reduce to (sand material solids relatively) below 0.1% up to the total content of metal component; Through membrane-concentrated, in liquid concentrator, add clear water again, be mixed with the mixed slurry that solid content is 5-50%;
(2) once transform: in above-mentioned mixed slurry, add a certain amount of sodium silicate solution or sodium hydroxide solution as catalyzer, under 60-140 ℃, pressure 0.7-8atm, the sol solutions after obtaining behind the reaction 0.5-8h once to transform;
(3) twice transformation: the sol solutions after the above-mentioned once conversion is concentrated through accurate filter, and filtrate is for once transforming resulting silicon sol; Add clear water at filtering and concentrating liquid, be mixed with the mixed slurry of 5-50% again; Add a certain amount of sodium silicate solution or sodium hydroxide solution again as catalyzer, under 100-140 ℃, pressure 1-10atm, obtain the sol solutions behind the twice transformation behind the reaction 0.5-8h;
Transform for (4) three times: the sol solutions behind the above-mentioned twice transformation is concentrated through accurate filter, and filtrate is the resulting silicon sol of twice transformation; Directly add remaining silicon component (silica flour and silicon-dioxide) in the sheet alkali transformation system of excessive 20-50% at filtering and concentrating liquid, the mixed solution after obtaining transforming for three times; Concentrate through accurate filter again, add the acid neutralization in the gained filtrate or sodium silicate solution is wherein changed into active silicic acid solution through highly acidic resin;
(5) superfine silicon carbide is collected: will transform back mixed solution gained liquid concentrator after concentrating for (4) three times and carry out drying, and collect and obtain superfine silicon carbide;
(6) the silicon sol parent nucleus increases: merge once conversion, the resulting silicon sol of twice transformation as parent nucleus; Gradual slow adds resulting active silicic acid solution and 1-10% concentration hydrogen sodium hydroxide solution in the step (4), increases through parent nucleus to obtain the bigger silicon sol of particle diameter.
2. according to the said a kind of method of utilizing waste mortar tailings material to prepare big particle diameter silicon sol and superfine silicon carbide of claim 1, it is characterized in that: waste mortar comprises the crystal silicon cutting waste mortar of photovoltaic industry and the crystal silicon cutting waste mortar of electron trade.
3. according to the said a kind of method of utilizing waste mortar tailings material to prepare big particle diameter silicon sol and superfine silicon carbide of claim 1, it is characterized in that: the addition of said sodium silicate solution of step (2) (3) or sodium hydroxide solution (conversion is water glass or sodium hydroxide) is the 2-15% (w/w) of amount of solid in the mixed slurry.
4. according to the said a kind of method of utilizing waste mortar tailings material to prepare big particle diameter silicon sol and superfine silicon carbide of claim 1, it is characterized in that: the D of said big particle diameter silicon sol
50>=70nm.
5. according to the said a kind of method of utilizing waste mortar tailings material to prepare big particle diameter silicon sol and superfine silicon carbide of claim 1, it is characterized in that: the D of said superfine silicon carbide
50≤5 microns.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746935A (en) * | 2012-08-02 | 2012-10-24 | 无锡和荣科技有限公司 | Method for recycling silicon cutting waste mortar |
| CN103601199A (en) * | 2013-10-14 | 2014-02-26 | 浙江晶盛硅晶材料有限公司 | Method for preparing silica sol by using waste mortar produced by cutting wafers |
| CN104671248A (en) * | 2013-11-30 | 2015-06-03 | 天津晶美微纳科技有限公司 | Method for directly preparing high-purity silica sol with large particle size by using silicon powder method |
| CN108251893A (en) * | 2018-02-11 | 2018-07-06 | 中铭瓷(苏州)纳米粉体技术有限公司 | The method that silicon carbide and zirconium oxide composite crystal palpus are recycled from crystal silicon cutting waste material |
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| EP1840083A1 (en) * | 2006-03-28 | 2007-10-03 | Council Of Scientific & Industrial Research | A process for the production of silicon carbide |
| CN101691216A (en) * | 2009-10-05 | 2010-04-07 | 山东科技大学 | Method for recycling silicon carbide and co-producing white carbon black from waste mortar for wire cutting |
| CN102120576A (en) * | 2011-01-25 | 2011-07-13 | 西安通鑫半导体辅料有限公司 | Method for recycling silicon carbide micropowder from waste mortar produced by cutting silicon wafer |
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2011
- 2011-12-14 CN CN2011104162069A patent/CN102515180A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1840083A1 (en) * | 2006-03-28 | 2007-10-03 | Council Of Scientific & Industrial Research | A process for the production of silicon carbide |
| CN101691216A (en) * | 2009-10-05 | 2010-04-07 | 山东科技大学 | Method for recycling silicon carbide and co-producing white carbon black from waste mortar for wire cutting |
| CN102120576A (en) * | 2011-01-25 | 2011-07-13 | 西安通鑫半导体辅料有限公司 | Method for recycling silicon carbide micropowder from waste mortar produced by cutting silicon wafer |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746935A (en) * | 2012-08-02 | 2012-10-24 | 无锡和荣科技有限公司 | Method for recycling silicon cutting waste mortar |
| CN103601199A (en) * | 2013-10-14 | 2014-02-26 | 浙江晶盛硅晶材料有限公司 | Method for preparing silica sol by using waste mortar produced by cutting wafers |
| CN104671248A (en) * | 2013-11-30 | 2015-06-03 | 天津晶美微纳科技有限公司 | Method for directly preparing high-purity silica sol with large particle size by using silicon powder method |
| CN108251893A (en) * | 2018-02-11 | 2018-07-06 | 中铭瓷(苏州)纳米粉体技术有限公司 | The method that silicon carbide and zirconium oxide composite crystal palpus are recycled from crystal silicon cutting waste material |
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Application publication date: 20120627 |