CN109592886A - The method for preparing foam glass based on crystalline silicon cutting waste material - Google Patents

The method for preparing foam glass based on crystalline silicon cutting waste material Download PDF

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Publication number
CN109592886A
CN109592886A CN201710934289.8A CN201710934289A CN109592886A CN 109592886 A CN109592886 A CN 109592886A CN 201710934289 A CN201710934289 A CN 201710934289A CN 109592886 A CN109592886 A CN 109592886A
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Prior art keywords
waste material
crystalline silicon
cutting waste
silicon cutting
warming
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CN201710934289.8A
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朱玉梅
周玲杰
李志宏
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Tianjin University
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Tianjin University
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00Other methods of shaping glass
    • C03B19/08Other methods of shaping glass by foaming
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • C03C1/002Use of waste materials, e.g. slags
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C11/00Multi-cellular glass ; Porous or hollow glass or glass particles
    • C03C11/007Foam glass, e.g. obtained by incorporating a blowing agent and heating

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacturing & Machinery (AREA)
  • Glass Compositions (AREA)

Abstract

The invention discloses a kind of methods for preparing foam glass based on crystalline silicon cutting waste material, the following steps are included: crystalline silicon cutting waste material, silica and carbon black are uniformly mixed, obtain crystalline silicon cutting waste material mixture, using wet ball grinding to crystalline silicon cutting waste material mixture ball milling 6~8 hours, 200~250 meshes are crossed in drying, 2h~3h is sintered after sieving at 450~500 DEG C, with 5wt% salt acid soak 6~8 hours, filtering obtained waste material;By waste material, Na2CO3、CaCO3、Al2O3、H3BO3And Li2CO3Uniformly mixing, obtains mixture, mixture is warming up to T by 20~25 DEG C of room temperature1DEG C and keep the temperature 30~60min, then by T1DEG C it is warming up to T2DEG C and keep the temperature 1~2h.By T2It is warming up to 900~950 DEG C and keeps the temperature 1~2h, furnace cooling after heat preservation.Crystalline silicon cutting waste material is used to prepare foam glass by the present invention, utilizes each ingredient of cutting waste material to greatest extent, without complicated separating-purifying process, has widened the application range of crystalline silicon cutting waste material.

Description

The method for preparing foam glass based on crystalline silicon cutting waste material
Technical field
The invention belongs to secondary resource technical field of comprehensive utilization, relate in particular to a kind of based on crystalline silicon cutting waste material The method for preparing foam glass.
Background technique
As fossil energy is critical, environmental pollution is on the rise, solar-energy photo-voltaic cell because its is safe and clean, efficient, just The features such as sharp, the strategic emerging industries for already becoming countries in the world extensive concern and developing emphatically, high-purity crystal silicon material also obtain Extensive use has been arrived, has had more than 90% solar battery at present using high purity polycrystalline silicon or monocrystalline silicon as raw material.High-purity crystal silicon Cutting generallys use the viscous mediums such as high by hardness, granularity is small silicon carbide abrasive micro mist and polyethylene glycol (PEG) and mixes Mortar mix multi-wire saw complete.The silicon carbide micro-powder of the heat and breakage that generate when cutting, being mixed into for sawdust make to cut mortar Property changes, and becomes waste mortar because can not meet cutting requirement.With regard to existing crystalline silicon cutting waste mortar recovery and utilization technology, It is easier to isolate viscous medium and bulky grain silicon carbide and removes metal impurities, and being difficult to be completely separated size distribution has overlapping And little particle silicon carbide and silicon similar in physicochemical properties.
Solar energy is nexhaustible due to possessing, clean and environmental protection and safe and reliable unique advantage, it has also become the mankind solve energy The preferred new energy of source crisis, environmental pollution and global warming issue.Currently, solar photovoltaic industry is sent out rapidly in the whole world Exhibition, as important photoelectric material, semiconductor material, the whole world is more and more to crystalline silicon cutting demand.In opto-electronics, Need to be cut to satisfactory silicon wafer, but in cutting process, about 50% or so crystalline silicon is in the form of silicon powder It loses to form waste slurry.These waste slurry bulk depositions easily cause certain safety and environmental problem, to soil, air It is polluted with water resource, it is therefore, imperative with the means processing cutting waste material of science.
Foam glass is a kind of made special glass material, by glass phase and a large amount of diameters in 0.5mm to 5mm Uniform stomata composition inorganic non-metallic foamed material.By raw materials such as cullet, foaming agent and additives, by it is finely divided simultaneously Mixing forms batch, is put into particular mold, is made using technical process such as high temperature melting, foaming, annealing.
Most important industrial process is powder sintering in current foam glass manufacture.Powder sintering mainly has three Step process process: the sintering of the raw material powder of the foam glass 2. molding 3. green body of raw material powder green body is 1. prepared.
Summary of the invention
Insufficient problem is recycled for crystalline silicon cutting waste material in the prior art, the purpose of the present invention is to provide one The method that kind prepares foam glass based on crystalline silicon cutting waste material.
The purpose of the present invention is what is be achieved by following technical proposals.
A method of foam glass is prepared based on crystalline silicon cutting waste material, comprising the following steps:
Step 1, crystalline silicon cutting waste material, silica and carbon black are uniformly mixed, obtains crystalline silicon cutting waste material mixing Object, using wet ball grinding to crystalline silicon cutting waste material mixture ball milling 6~8 hours, drying crosses 200~250 meshes, after sieving It is sintered 2h~3h at 450~500 DEG C, for removing the PEG (polyethylene glycol) in crystalline silicon cutting waste material mixture, uses 5wt% salt acid soak 6~8 hours, filtering, for removing the oxide of iron and iron in crystalline silicon cutting waste material mixture, obtains To waste material;Wherein, the quality of silica is 0.12~0.16 times of crystalline silicon cutting waste material quality, and the quality of carbon black is crystal 0.05~0.1 times of silicon cutting waste material quality;
Step 2, by step 1 gained waste material, Na2CO3、CaCO3、Al2O3、H3BO3And Li2CO3Uniformly mixing, is mixed Object, wherein the waste material, Na2CO3、CaCO3、Al2O3、H3BO3And Li2CO3Mass fraction ratio be (60~75): (10~ 15): (5~10): (3~7): (5~10): (1~4);
Step 3, it preheats: step 2 gained mixture is warming up to T by 20~25 DEG C of room temperature1DEG C and keep the temperature 30~60min, Wherein, T1=350~450;
In the step 3, by room temperature to T1DEG C heating rate be 3~8 DEG C/min.
Step 4, then by T1DEG C it is warming up to T2DEG C and keep the temperature 1~2h, wherein T2=800~850;
In the step 4, by T1DEG C it is warming up to T2DEG C heating rate be 2~5 DEG C/min;
Step 5, it foams: by T2It is warming up to 900~950 DEG C and keeps the temperature 1~2h, furnace cooling after heat preservation.
In the step 5, by T2The heating rate for being warming up to 900~950 DEG C is 1~10 DEG C/min.
The foam glass being prepared such as the above method.
The above method is improving the application in foam glass bending strength.
The present invention compared with prior art, has the beneficial effect that:
(1) crystalline silicon cutting waste material is used to prepare foam glass by the present invention, utilizes each of cutting waste material to greatest extent A ingredient widened the application range of crystalline silicon cutting waste material without complicated separating-purifying process, effective solution crystal The stacking problem of silicon cutting waste material, turns waste into wealth, and not only brings economic benefit, but also solve environmental problem.
(2) present invention utilizes waste material, introduces Na with above-mentioned raw materials2O-CaO-Al2O3-Li2O-B2O3As additive, use Powder sintering prepares foam glass, by 800 DEG C~1000 DEG C low-firings, obtains bulk density lower than 1.8g/cm3, machine Tool compression strength is up to the foam glass product of 8MPa, does not need harsh preparation condition, the cost greatlyd save, and economic effect Benefit is good.
(3) present invention process system simple possible, raw material is inexpensively inexpensive, is conducive to the foam glass product industrially Produce in enormous quantities.
Specific embodiment
A kind of new approaches are provided for the recycling of crystalline silicon cutting waste material.The present invention provides crystalline silicon cutting waste materials Applied in preparing foam glass, by cutting waste material prepare glass can to greatest extent using the silicon carbide in cutting waste material, Silicon powder and other compositions, not only have an economic benefit, and there are also certain environmental benefits, prepare and steep currently with crystalline silicon cutting waste material Foam glass is rarely reported.
In a specific embodiment of the invention, required drug mainly has: Na2CO3(Ke Miou), CaCO3(triumphant horse It is special), Al2O3(the vertical chemical industry of member), H3BO3(Kmart) and Li2CO3(the vertical chemical industry of member) SiO2(Kmart), carbon black (nine ancient cooking vessels chemistry), Technical solution of the present invention is further illustrated combined with specific embodiments below.
Embodiment 1
A method of foam glass is prepared based on crystalline silicon cutting waste material, comprising the following steps:
Step 1, crystalline silicon cutting waste material and silica are uniformly mixed, obtain crystalline silicon cutting waste material mixture, In, the quality of silica is 0.15 times of of crystalline silicon cutting waste material quality
Using wet ball grinding to crystalline silicon cutting waste material mixture ball milling 8 hours, drying, cross 200 meshes, after sieving in It is sintered 180min at 450 DEG C, for removing the PEG in crystalline silicon cutting waste material mixture, with 5wt% salt acid soak 6 hours, mistake Filter, for removing the oxide of iron and iron in crystalline silicon cutting waste material mixture, obtains waste material;
Step 2, by step 1 gained waste material, Na2CO3、CaCO3、Al2O3、H3BO3And Li2CO3Uniformly mixing, it is mixed Object, wherein waste material, Na2CO3、CaCO3、Al2O3、H3BO3And Li2CO3Mass fraction ratio be 65:15:5:3:10:2;
Step 3, it preheats: step 2 gained mixture is warming up to T by 20~25 DEG C of room temperature1DEG C and keep the temperature 60min, wherein T1=450, heating rate is 5 DEG C/min.
Step 4, then by T1DEG C it is warming up to T2DEG C and keep the temperature 2h, wherein T2=800 DEG C, heating rate is 5 DEG C/min;
Step 5, it foams: by T2It is warming up to 920 DEG C and keeps the temperature 1h, furnace cooling after heat preservation, heating rate is 10℃/min。
Embodiment 2
A method of foam glass is prepared based on crystalline silicon cutting waste material, comprising the following steps:
Step 1, crystalline silicon cutting waste material, silica and carbon black are uniformly mixed, obtains crystalline silicon cutting waste material mixing Object, wherein the quality of silica is 0.15 times of crystalline silicon cutting waste material quality, and the quality of carbon black is crystalline silicon cutting waste material 0.05 times of quality;
Using wet ball grinding to crystalline silicon cutting waste material mixture ball milling 8 hours, drying, cross 200 meshes, after sieving in It is sintered 180min at 450 DEG C, for removing the PEG in crystalline silicon cutting waste material mixture, with 5wt% salt acid soak 6 hours, mistake Filter, for removing the oxide of iron and iron in crystalline silicon cutting waste material mixture, obtains waste material;
Step 2, by step 1 gained waste material, Na2CO3、CaCO3、Al2O3、H3BO3And Li2CO3Uniformly mixing, it is mixed Object, wherein waste material, Na2CO3、CaCO3、Al2O3、H3BO3And Li2CO3Mass fraction ratio be 65:15:5:3:10: 2;
Step 3, it preheats: step 2 gained mixture is warming up to T by 20~25 DEG C of room temperature1DEG C and keep the temperature 60min, wherein T1=450 DEG C, heating rate is 5 DEG C/min.
Step 4, then by T1DEG C it is warming up to T2DEG C and keep the temperature 2h, wherein T2=850 DEG C, heating rate is 5 DEG C/min;
Step 5, it foams: by T2It is warming up to 920 DEG C and keeps the temperature 2h, furnace cooling after heat preservation, heating rate is 10℃/min。
Embodiment 3
A method of foam glass is prepared based on crystalline silicon cutting waste material, comprising the following steps:
Step 1, crystalline silicon cutting waste material, silica and carbon black are uniformly mixed, obtains crystalline silicon cutting waste material mixing Object, wherein the quality of silica is 0.15 times of crystalline silicon cutting waste material quality, and the quality of carbon black is crystalline silicon cutting waste material 0.07 times of quality;
Using wet ball grinding to crystalline silicon cutting waste material mixture ball milling 8 hours, drying, cross 200 meshes, after sieving in It is sintered 180min at 450 DEG C, for removing the PEG in crystalline silicon cutting waste material mixture, with 5wt% salt acid soak 6 hours, mistake Filter, for removing the oxide of iron and iron in crystalline silicon cutting waste material mixture, obtains waste material;
Step 2, by step 1 gained waste material, Na2CO3、CaCO3、Al2O3、H3BO3And Li2CO3Uniformly mixing, it is mixed Object, wherein waste material, Na2CO3、CaCO3、Al2O3、H3BO3And Li2CO3Mass fraction ratio be 65:15:5:3:10: 2;
Step 3, it preheats: step 2 gained mixture is warming up to T by 20~25 DEG C of room temperature1DEG C and keep the temperature 60min, wherein T1=450 DEG C, heating rate is 5 DEG C/min.
Step 4, then by T1DEG C it is warming up to T2DEG C and keep the temperature 2h, wherein T2=850 DEG C, heating rate is 5 DEG C/min;
Step 5, it foams: by T2It is warming up to 920 DEG C and keeps the temperature 2h, furnace cooling after heat preservation, heating rate is 10℃/min。
Embodiment 4
A method of foam glass is prepared based on crystalline silicon cutting waste material, comprising the following steps:
Step 1, crystalline silicon cutting waste material, silica and carbon black are uniformly mixed, obtains crystalline silicon cutting waste material mixing Object, wherein the quality of silica is 0.15 times of crystalline silicon cutting waste material quality, and the quality of carbon black is crystalline silicon cutting waste material 0.10 times of quality;
Using wet ball grinding to crystalline silicon cutting waste material mixture ball milling 8 hours, drying, cross 200 meshes, after sieving in It is sintered 180min at 450 DEG C, for removing the PEG in crystalline silicon cutting waste material mixture, with 5wt% salt acid soak 6 hours, mistake Filter, for removing the oxide of iron and iron in crystalline silicon cutting waste material mixture, obtains waste material;
Step 2, by step 1 gained waste material, Na2CO3、CaCO3、Al2O3、H3BO3And Li2CO3Uniformly mixing, it is mixed Object, wherein waste material, Na2CO3、CaCO3、Al2O3、H3BO3And Li2CO3Mass fraction ratio be 65:15:5:3:10: 2;
Step 3, it preheats: step 2 gained mixture is warming up to T by 20~25 DEG C of room temperature1DEG C and keep the temperature 60min, wherein T1=450 DEG C, heating rate is 5 DEG C/min.
Step 4, then by T1DEG C it is warming up to T2DEG C and keep the temperature 2h, wherein T2=850 DEG C, heating rate is 5 DEG C/min;
Step 5, it foams: by T2It is warming up to 920 DEG C and keeps the temperature 2h, furnace cooling after heat preservation, heating rate is 10℃/min。
By embodiment 2, embodiment 3, the bending strength of foam glass prepared by embodiment 4 is respectively 5MPa, 3.5MPa, 2MPa shows the increase with content of carbon black, and the compression strength of foam glass reduces, and not plus the bending resistance of the embodiment 1 of carbon black is strong Degree only has 1.5MPa, illustrates that the addition of carbon black facilitates the raising of foam glass bending strength.
Illustrative description has been done to the present invention above, it should explanation, the case where not departing from core of the invention Under, any simple deformation, modification or other skilled in the art can not spend the equivalent replacement of creative work equal Fall into protection scope of the present invention.

Claims (6)

1. a kind of method for preparing foam glass based on crystalline silicon cutting waste material, which comprises the following steps:
Step 1, crystalline silicon cutting waste material, silica and carbon black are uniformly mixed, obtains crystalline silicon cutting waste material mixture, adopts With wet ball grinding to crystalline silicon cutting waste material mixture ball milling 6~8 hours, drying crosses 200~250 meshes, in 450 after sieving 2h~3h is sintered at~500 DEG C, for removing the PEG in crystalline silicon cutting waste material mixture, with salt acid soak 6~8 hours, mistake Filter, for removing the oxide of iron and iron in crystalline silicon cutting waste material mixture, obtains waste material;Wherein, the matter of silica Amount is 0.12~0.16 times of crystalline silicon cutting waste material quality, the quality of carbon black be crystalline silicon cutting waste material quality 0.05~ 0.1 times;
Step 2, by step 1 gained waste material, Na2CO3、CaCO3、Al2O3、H3BO3And Li2CO3Uniformly mixing, obtains mixture, In, the waste material, Na2CO3、CaCO3、Al2O3、H3BO3And Li2CO3Mass fraction ratio be (60~75): (10~15): (5 ~10): (3~7): (5~10): (1~4);
Step 3, it preheats: step 2 gained mixture is warming up to T by 20~25 DEG C of room temperature1DEG C and keep the temperature 30~60min, wherein T1=350~450;
Step 4, then by T1DEG C it is warming up to T2DEG C and keep the temperature 1~2h, wherein T2=800~850;
Step 5, it foams: by T2It is warming up to 900~950 DEG C and keeps the temperature 1~2h, furnace cooling after heat preservation.
2. the method according to claim 1, wherein in the step 3, by room temperature to T1DEG C heating Rate is 3~8 DEG C/min.
3. the method according to claim 1, wherein in the step 4, by T1DEG C it is warming up to T2DEG C heating Rate is 2~5 DEG C/min.
4. the method according to claim 1, wherein in the step 5, by T2It is warming up to 900~950 DEG C Heating rate is 1~10 DEG C/min.
5. the foam glass being prepared such as Claims 1 to 4 any one the method.
6. as Claims 1 to 4 any one the method is improving the application in foam glass bending strength.
CN201710934289.8A 2017-09-30 2017-09-30 The method for preparing foam glass based on crystalline silicon cutting waste material Pending CN109592886A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0579990A1 (en) * 1992-07-04 1994-01-26 Heraklith Baustoffe Ag Foamed glass and method of preparation
CN101531462A (en) * 2009-04-10 2009-09-16 北京工业大学 Method for preparing borosilicate foam glass
CN101941699A (en) * 2010-09-14 2011-01-12 东北大学 Method for reclaiming silicon and silicon carbide from cutting waste materials of monocrystalline silicon and polycrystalline silicon
CN103370366A (en) * 2011-01-25 2013-10-23 萨巴瑞提股份有限公司 Separating fluid, method and installation for separating multilayer systems
CN106517777A (en) * 2016-11-15 2017-03-22 济南大学 Application of crystalline silicon cutting waste material in preparation of color glass and the obtained product thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0579990A1 (en) * 1992-07-04 1994-01-26 Heraklith Baustoffe Ag Foamed glass and method of preparation
CN101531462A (en) * 2009-04-10 2009-09-16 北京工业大学 Method for preparing borosilicate foam glass
CN101941699A (en) * 2010-09-14 2011-01-12 东北大学 Method for reclaiming silicon and silicon carbide from cutting waste materials of monocrystalline silicon and polycrystalline silicon
CN103370366A (en) * 2011-01-25 2013-10-23 萨巴瑞提股份有限公司 Separating fluid, method and installation for separating multilayer systems
CN106517777A (en) * 2016-11-15 2017-03-22 济南大学 Application of crystalline silicon cutting waste material in preparation of color glass and the obtained product thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
钟颖: "硼硅酸盐泡沫玻璃无机浮质载体的研究", 《中国硕士学位论文全文数据库 工程科技I辑》 *

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Application publication date: 20190409