CN105655570A - Refining preparation method of nanoscale silicon powder material - Google Patents
Refining preparation method of nanoscale silicon powder material Download PDFInfo
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- CN105655570A CN105655570A CN201610206766.4A CN201610206766A CN105655570A CN 105655570 A CN105655570 A CN 105655570A CN 201610206766 A CN201610206766 A CN 201610206766A CN 105655570 A CN105655570 A CN 105655570A
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- 239000000463 material Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title abstract description 9
- 239000011863 silicon-based powder Substances 0.000 title abstract 5
- 238000007670 refining Methods 0.000 title abstract 3
- 238000000227 grinding Methods 0.000 claims abstract description 93
- 239000002904 solvent Substances 0.000 claims abstract description 65
- 239000002245 particle Substances 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000005516 engineering process Methods 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 422
- 239000000377 silicon dioxide Substances 0.000 claims description 211
- 235000013312 flour Nutrition 0.000 claims description 159
- 239000002002 slurry Substances 0.000 claims description 106
- 239000000843 powder Substances 0.000 claims description 97
- 239000006185 dispersion Substances 0.000 claims description 93
- 239000003795 chemical substances by application Substances 0.000 claims description 67
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 56
- 238000002203 pretreatment Methods 0.000 claims description 39
- 239000002253 acid Substances 0.000 claims description 29
- 229920001296 polysiloxane Polymers 0.000 claims description 29
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 26
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 26
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 22
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- -1 polyoxyethylene Polymers 0.000 claims description 19
- 239000001267 polyvinylpyrrolidone Chemical class 0.000 claims description 16
- 229920000036 polyvinylpyrrolidone Chemical class 0.000 claims description 16
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 16
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 14
- 239000004202 carbamide Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 235000019830 sodium polyphosphate Nutrition 0.000 claims description 12
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 11
- 235000011187 glycerol Nutrition 0.000 claims description 11
- 150000004760 silicates Chemical class 0.000 claims description 11
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 10
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 10
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- FOGYNLXERPKEGN-UHFFFAOYSA-N 3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfopropyl)phenoxy]propane-1-sulfonic acid Chemical class COC1=CC=CC(CC(CS(O)(=O)=O)OC=2C(=CC(CCCS(O)(=O)=O)=CC=2)OC)=C1O FOGYNLXERPKEGN-UHFFFAOYSA-N 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 4
- 150000001555 benzenes Chemical class 0.000 claims description 4
- 239000004021 humic acid Substances 0.000 claims description 4
- 150000002576 ketones Chemical class 0.000 claims description 4
- 238000003801 milling Methods 0.000 claims description 4
- 229920000620 organic polymer Polymers 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- 159000000000 sodium salts Chemical class 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 235000019351 sodium silicates Nutrition 0.000 claims description 2
- 239000002270 dispersing agent Substances 0.000 abstract 3
- 238000010923 batch production Methods 0.000 abstract 1
- 239000002210 silicon-based material Substances 0.000 abstract 1
- 125000003158 alcohol group Chemical group 0.000 description 9
- 229910001416 lithium ion Inorganic materials 0.000 description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 8
- 229910052710 silicon Inorganic materials 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 4
- 229910052744 lithium Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000005518 electrochemistry Effects 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000005543 nano-size silicon particle Substances 0.000 description 2
- 229910000733 Li alloy Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006253 efflorescence Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002153 silicon-carbon composite material Substances 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a refining preparation method of a nanoscale silicon powder material. The preparation method comprises steps as follows: a powdery coarse silicon material and a dispersing agent are added to a solvent and dispersed evenly at a high speed for grinding, then the solvent and the dispersing agent are added again, and the nanoscale silicon powder material is prepared after secondary grinding. The method has the benefits as follows: types and dosage of solvents and dispersing agents are adjusted with technologies for secondary ball-milling and gradient replacement of grinding balls with specific diameters, and the nanoscale silicon powder material can be subjected to classified batch production with the particle size capable of being controlled in the range of 50-500 nm. The refining preparation method of the nanoscale silicon powder material has the characteristics of high efficiency, stability and accurately controllable particle size.
Description
Technical field
The present invention relates to battery material field, a kind of method that particularly nano silicone powder material becomes more meticulous and prepares.
Background technology
At present, the negative material that lithium ion battery is conventional has carbon negative pole material (comprising graphite, soft carbon and hard carbon) and metatitanic acid lithium, but their gram volume room for promotion is all very limited, is unfavorable for the design and development of lithium ion battery with high energy density. Along with industry is to the active demand of lithium ion battery with high energy density, the lithium ion battery negative material of development and production heavy body and high stability, extremely urgent.
In the lithium ion battery negative material system of research at present, metal alloy compositions such as Si, Sn, Al etc. owing to it can form many lithium alloys with Li and have the theoretical specific capacity more much higher than conventional graphite negative material, simultaneously, the removal lithium embedded current potential of this metalloid alloy class material relatively conventional graphite negative material height, not easily produces Li dendrite in fast charging and discharging process. Therefore, this kind of alloy material has excellent safety performance, is the ideal chose of lithium ion battery negative material of future generation. Wherein, the silica-base material in this kind of alloy material, because it has the highest theoretical specific capacity 4200mAh/g, intercalation potential is 0.2V (vs.Li/Li+), safety performance is good, and reserves enrich, and cost performance is higher, obtains extensive concern and the research of academia and industry member in recent years. But the significant challenge that silica-base material faces is it shows huge volume change (300%) in the process of removal lithium embedded, this can cause the fragmentation of silicon grain, efflorescence and electrode materials to lose the problems such as electrical contact, therefore, the electrochemistry stable circulation performance of silica-base material is poor. Meanwhile, owing to silicon is a kind of semiconductor material, its electronic conductivity and ionic conductivity are all relatively low, can not effectively meet the requirement of lithium ion battery high power charging-discharging.
The difficult problem solving silicon base class material electrochemical cycle performance difference at present mainly by reducing particle size, doping and coated realize. Wherein, the volume effect of silicon itself can be reduced by preparing the silica-base material of nanoscale, shorten the delivering path of lithium ion, thus improve its electrochemical reaction speed, improve the electrochemistry cycle performance of silica-base material. At present, particle size equally distributed superfine nano silica flour material is the core persursor material of emerging generation lithium cell cathode material-silicon-carbon cathode material equally.
Therefore, preparing nano silicone powder material at present is the crucial method improved silica-base material electrochemistry cycle performance and promote silicon-carbon composite cathode material performance, and its common preparation technology mainly contains vapour deposition process, liquid phase method, hot reducing method etc. But these preparation method's costs are higher, output is lower, and is difficult to obtain that size-grade distribution is concentrated, stable, the regulatable nano silicon material of particle diameter.
Summary of the invention
It is an object of the invention to overcome the shortcoming of prior art, it is provided that a kind of method that nano silicone powder material becomes more meticulous and prepares.
The object of the present invention is achieved through the following technical solutions: a kind of method that nano silicone powder material becomes more meticulous and prepares, and concrete preparation process is as follows:
(1) pre-treatment fine silica powder slurry is prepared: get the thick silica flour that particle diameter is 5 ��m��50 ��m, add solvent and dispersion agent respectively, after high speed dispersion is even, obtain thick silica flour slurry, adding diameter in thick silica flour slurry is the grinding of 0.5mm��5mm zirconium oxide abrasive ball, after grinding, obtain pre-treatment fine silica powder slurry, wherein solvent is water, alcohol, dehydrated alcohol, ethylene glycol, glycerine, polyvinylpyrrolidone, acetone, hexanaphthene, butanone, in butanols, one or more in benzene class, dispersion agent is Witco 1298 Soft Acid class, urea, sodium polyphosphate, silicates, polyoxyethylene glycol, Xylo-Mucine, Lalgine class, polyacrylic, polyvinylpyrrolidone, lignosulfonic acid class, one or more in Sodium salts humic acids,
(2) prepare nano level silica flour slurry: obtain in step (1) pre-treatment fine silica powder slurry in, add solvent and dispersion agent, high speed dispersion is even, the zirconium oxide abrasive ball grinding that diameter is 0.01mm��0.5mm is added in fine silica powder slurry, after grinding, obtain nano level silica flour slurry;
(3) preparing nano level silica flour: step (2) is obtained nano level silica flour slurry, is dried, after dry, powder body is pulverized and is broken up, and obtains nano level silica flour.
Preferably, a kind of nano silicone powder material as above becomes more meticulous the method for preparation, and the solvent used in step (1) and step (2) is water, one or more combination in alcohol class, polyvinylpyrrolidone, ketone class, hexanaphthene, benzene class.
Preferably, the method that a kind of nano silicone powder material as above becomes more meticulous and prepares, described alcohol class is one or more the combination in alcohol, dehydrated alcohol, ethylene glycol, glycerine, butanols; Described ketone class is one or both the combination in acetone or butanone.
Preferably, the method that a kind of nano silicone powder material as above becomes more meticulous and prepares, the dispersion agent used in step (1) and step (2) is one or more the combination in polymer organic polymer class, organic molecule class and mineral-type dispersion agent.
Preferably, the method that a kind of nano silicone powder material as above becomes more meticulous and prepares, described polymer organic polymer class is one or more the combination in polyoxyethylene glycol, Xylo-Mucine, Lalgine class, polyacrylic, polyvinylpyrrolidone, lignosulfonic acid class, Sodium salts humic acids; Described organic molecule class is one or both in Witco 1298 Soft Acid class or urea; Described mineral-type dispersion agent is one or both in sodium polyphosphate or silicates.
Preferably, the method that a kind of nano silicone powder material as above becomes more meticulous and prepares, in step (1), the weight ratio of thick silica flour, solvent and dispersion agent is 1:0.5��20:0.001��0.2.
Preferably, the weight ratio of described thick silica flour and grinding ball is 10:1��3.
Preferably, a kind of nano silicone powder material as above become more meticulous preparation method, described step (1) be ground to ball-milling technology, milling time 2h��10h; Step (2) be ground to ball-milling technology, milling time 2h��8h.
Preferably, the method that a kind of nano silicone powder material as above becomes more meticulous and prepares, the drying process described in step (3), dry atmosphere is inert atmosphere or vacuum-drying, drying temperature is room temperature��50 DEG C, dry until material moisture content is less than 1000ppm.
Preferably, the method that a kind of nano silicone powder material as above becomes more meticulous and prepares, the dry rear nano level silica flour obtained in step (3), the total scope of its particle diameter is 50nm��500nm, and nano silicone powder footpath can control to 50��100nm, 100��200nm, 200��300nm, 300��400nm, 400��500nm, five intervals respectively.
The present invention has the following advantages: the present invention provides a kind of method that nano silicone powder material for cell negative electrode material becomes more meticulous and prepares. The present invention is with the method for secondary ball milling, and thick silica flour is that nano level silica flour prepared by material. By adjusting kind and the consumption of solvent and dispersion agent, control process of lapping grinds diameter and the add-on of ball, realize the nano silicone total scope of powder material particle diameter between 50nm��500nm, and it can be controlled in 0��100nm, 100��200nm, 200��300nm, 300��400nm, 400��500nm, five intervals respectively. The present invention solves the difficult problem that existing nano-silicon preparation technology's cost is higher, output is lower, size-grade distribution is not concentrated, thus obtains size-grade distribution high concentration, batch stable, the regulatable nano silicone powder material of primary particle size.
Accompanying drawing explanation
Fig. 1: the SEM photograph of the obtained nano level silica flour powder body 50-100nm of the embodiment of the present invention 1;
Fig. 2: the SEM photograph of the obtained nano level silica flour powder body 100-200nm of the embodiment of the present invention 2;
Fig. 3: the SEM photograph of the obtained nano level silica flour powder body 400-500nm of the embodiment of the present invention 5.
Embodiment
Below in conjunction with drawings and Examples, the present invention will be further described, and protection scope of the present invention is not limited to the following stated:
Embodiment 1:
Particle diameter of the present invention is the preparation of 50nm��100nm silica flour:
(1) pre-treatment fine silica powder slurry is prepared: get the thick silica flour that particle diameter is 5 ��m, solvent alcohol is added by solvent 5kg in the thick silica flour of every 1kg, dispersion agent Witco 1298 Soft Acid class is added again by dispersion agent 200g in the thick silica flour of every 1kg, after high speed dispersion is even, adding diameter by the mass ratio 3:10 of grinding ball and thick silica flour in thick silica flour slurry is the grinding of 0.5mm zirconium oxide abrasive ball, grinding 10h, obtains pre-treatment fine silica powder slurry.
(2) nano level silica flour slurry is prepared: in the pre-treatment fine silica powder slurry obtained in step (1), add solvent dehydrated alcohol and dispersion agent Witco 1298 Soft Acid class, high speed dispersion is even, add, by the mass ratio 3:10 of grinding ball and thick silica flour, the zirconium oxide abrasive ball grinding that diameter is 0.01mm in fine silica powder slurry, grinding 4h, again adding solvent dehydrated alcohol and the grinding of dispersion agent Witco 1298 Soft Acid class, grinding 4h, obtains nano level silica flour slurry;
(3) nano level silica flour is prepared: step (2) is obtained nano level silica flour slurry, it is dried under an inert atmosphere, drying temperature is 50 DEG C, it is dry until material moisture content is less than 1000ppm, after dry, powder body is pulverized and is broken up, obtaining nano level silica flour, its particle size range is 50��100nm, as shown in Figure 1.
Embodiment 2:
Particle diameter of the present invention is the preparation of 100nm��200nm silica flour:
(1) pre-treatment fine silica powder slurry is prepared: get the thick silica flour that particle diameter is 10 ��m, solvent dehydrated alcohol is added by solvent 10kg in the thick silica flour of every 1kg, dispersion agent Witco 1298 Soft Acid class is added again by dispersion agent 100g in the thick silica flour of every 1kg, after high speed dispersion is even, adding diameter by the mass ratio 2:10 of grinding ball and thick silica flour in thick silica flour slurry is the grinding of 1mm zirconium oxide abrasive ball, grinding 8h, obtains pre-treatment fine silica powder slurry.
(2) nano level silica flour slurry is prepared: in the pre-treatment fine silica powder slurry obtained in step (1), add solvent alcohol and dispersion agent Witco 1298 Soft Acid class, high speed dispersion is even, add, by the mass ratio 2:10 of grinding ball and thick silica flour, the zirconium oxide abrasive ball grinding that diameter is 0.1mm in fine silica powder slurry, grinding 4h, again adding solvent dehydrated alcohol and the grinding of dispersion agent Witco 1298 Soft Acid class, grinding 2h, obtains nano level silica flour slurry;
(3) nano level silica flour is prepared: step (2) is obtained nano level silica flour slurry, it is dried under an inert atmosphere, drying temperature is 50 DEG C, it is dry until material moisture content is less than 1000ppm, after dry, powder body is pulverized and is broken up, obtaining nano level silica flour, its particle size range is 100��200nm, as shown in Figure 2.
Embodiment 3:
Particle diameter of the present invention is the preparation of 200nm��300nm silica flour:
(1) pre-treatment fine silica powder slurry is prepared: get the thick silica flour that particle diameter is 15 ��m, solvent alcohol is added by solvent 20kg in the thick silica flour of every 1kg, dispersion agent Witco 1298 Soft Acid class is added again by dispersion agent 100g in the thick silica flour of every 1kg, after high speed dispersion is even, adding diameter by the mass ratio 2:10 of grinding ball and thick silica flour in thick silica flour slurry is the grinding of 1.5mm zirconium oxide abrasive ball, grinding 6h, obtains pre-treatment fine silica powder slurry.
(2) nano level silica flour slurry is prepared: in the pre-treatment fine silica powder slurry obtained in step (1), add solvent alcohol and dispersion agent Witco 1298 Soft Acid class, high speed dispersion is even, add, by the mass ratio 1.5:10 of grinding ball and thick silica flour, the zirconium oxide abrasive ball grinding that diameter is 0.2mm in fine silica powder slurry, grinding 3h, again adding solvent dehydrated alcohol and the grinding of dispersion agent Witco 1298 Soft Acid class, grinding 2h, obtains nano level silica flour slurry;
(3) nano level silica flour is prepared: step (2) is obtained nano level silica flour slurry, it is dried under an inert atmosphere, drying temperature is 50 DEG C, it is dry until material moisture content is less than 1000ppm, after dry, powder body is pulverized and is broken up, obtaining nano level silica flour, its particle size range is 200��300nm.
Embodiment 4:
Particle diameter of the present invention is the preparation of 300nm��400nm silica flour:
(1) pre-treatment fine silica powder slurry is prepared: get the thick silica flour that particle diameter is 20 ��m, solvent alcohol is added by solvent 2kg in the thick silica flour of every 1kg, dispersion agent Witco 1298 Soft Acid class is added again by dispersion agent 50g in the thick silica flour of every 1kg, after high speed dispersion is even, adding diameter by the mass ratio 1.5:10 of grinding ball and thick silica flour in thick silica flour slurry is the grinding of 3mm zirconium oxide abrasive ball, grinding 4h, obtains pre-treatment fine silica powder slurry.
(2) nano level silica flour slurry is prepared: in the pre-treatment fine silica powder slurry obtained in step (1), add solvent dehydrated alcohol and dispersion agent Witco 1298 Soft Acid class, high speed dispersion is even, add, by the mass ratio 1.5:10 of grinding ball and thick silica flour, the zirconium oxide abrasive ball grinding that diameter is 0.3mm in fine silica powder slurry, grinding 2h, again adding solvent alcohol and the grinding of dispersion agent Witco 1298 Soft Acid class, grinding 2h, obtains nano level silica flour slurry;
(3) nano level silica flour is prepared: step (2) is obtained nano level silica flour slurry, it is dried under an inert atmosphere, drying temperature is 50 DEG C, it is dry until material moisture content is less than 1000ppm, after dry, powder body is pulverized and is broken up, obtaining nano level silica flour, its particle size range is 300��400nm.
Embodiment 5:
Particle diameter of the present invention is the preparation of 400nm��500nm silica flour:
(1) pre-treatment fine silica powder slurry is prepared: get the thick silica flour that particle diameter is 50 ��m, solvent alcohol is added by solvent 0.5kg in the thick silica flour of every 1kg, dispersion agent Witco 1298 Soft Acid class is added again by dispersion agent 1g in the thick silica flour of every 1kg, after high speed dispersion is even, adding diameter by the mass ratio 1:10 of grinding ball and thick silica flour in thick silica flour slurry is the grinding of 5mm zirconium oxide abrasive ball, grinding 2h, obtains pre-treatment fine silica powder slurry.
(2) nano level silica flour slurry is prepared: in the pre-treatment fine silica powder slurry obtained in step (1), add solvent dehydrated alcohol and dispersion agent Witco 1298 Soft Acid class, high speed dispersion is even, add, by the mass ratio 1:10 of grinding ball and thick silica flour, the zirconium oxide abrasive ball grinding that diameter is 0.5mm in fine silica powder slurry, grinding 2h, obtains nano level silica flour slurry;
(3) nano level silica flour is prepared: step (2) is obtained nano level silica flour slurry, it is dried under an inert atmosphere, drying temperature is 50 DEG C, it is dry until material moisture content is less than 1000ppm, after dry, powder body is pulverized and is broken up, obtaining nano level silica flour, its particle size range is 400��500nm, as shown in Figure 3.
Embodiment 6:
Particle diameter of the present invention is the preparation of 100nm��200nm silica flour:
(1) pre-treatment fine silica powder slurry is prepared: get the thick silica flour that particle diameter is 10 ��m, solvent dehydrated alcohol is added by solvent 10kg in the thick silica flour of every 1kg, Witco 1298 Soft Acid class dispersion agent is added again by dispersion agent 100g in the thick silica flour of every 1kg, after high speed dispersion is even, adding diameter by the mass ratio 2:10 of grinding ball and thick silica flour in thick silica flour slurry is the grinding of 1mm zirconium oxide abrasive ball, grinding 8h, obtains pre-treatment fine silica powder slurry.
(2) prepare nano level silica flour slurry: obtain in step (1) pre-treatment fine silica powder slurry in, add solvent and dispersion agent, high speed dispersion is even, add, by the mass ratio 2:10 of grinding ball and thick silica flour, the zirconium oxide abrasive ball grinding that diameter is 0.1mm in fine silica powder slurry, grinding 4h, again add solvent and dispersion agent grinding 2h, obtain nano level silica flour slurry; Wherein, the solvent in step (2) is alcohol, and dispersion agent is Witco 1298 Soft Acid class, urea.
(3) nano level silica flour is prepared: step (2) is obtained nano level silica flour slurry, it is dried under an inert atmosphere, drying temperature is 50 DEG C, it is dry until material moisture content is less than 1000ppm, it is dried, after dry, powder body is pulverized and is broken up, and obtains nano level silica flour, and its particle size range is 100��200nm.
Embodiment 7:
Particle diameter of the present invention is the preparation of 100nm��200nm silica flour:
(1) pre-treatment fine silica powder slurry is prepared: get the thick silica flour that particle diameter is 10 ��m, solvent is added by solvent 10kg in the thick silica flour of every 1kg, dispersion agent is added again by dispersion agent 100g in the thick silica flour of every 1kg, after high speed dispersion is even, adding diameter by the mass ratio 2:10 of grinding ball and thick silica flour in thick silica flour slurry is the grinding of 1mm zirconium oxide abrasive ball, grinding 8h, obtain pre-treatment fine silica powder slurry, wherein in step (1), solvent is alcohol, ethylene glycol, and dispersion agent is Witco 1298 Soft Acid class, urea, sodium polyphosphate.
(2) prepare nano level silica flour slurry: obtain in step (1) pre-treatment fine silica powder slurry in, add solvent and dispersion agent, high speed dispersion is even, add, by the mass ratio 2:10 of grinding ball and thick silica flour, the zirconium oxide abrasive ball grinding that diameter is 0.1mm in fine silica powder slurry, grinding 4h, again add solvent and dispersion agent grinding 2h, obtain nano level silica flour slurry, wherein in step (2), solvent is alcohol, ethylene glycol, glycerine, and dispersion agent is Witco 1298 Soft Acid class, urea, sodium polyphosphate, silicates.
(3) nano level silica flour is prepared: step (2) is obtained nano level silica flour slurry, it is dried under an inert atmosphere, drying temperature is 50 DEG C, it is dry until material moisture content is less than 1000ppm, it is dried, after dry, powder body is pulverized and is broken up, and obtains nano level silica flour, and its particle size range is 100��200nm.
Embodiment 8:
Particle diameter of the present invention is the preparation of 100nm��200nm silica flour:
(1) pre-treatment fine silica powder slurry is prepared: get the thick silica flour that particle diameter is 10 ��m, solvent is added by solvent 10kg in the thick silica flour of every 1kg, dispersion agent is added again by dispersion agent 100g in the thick silica flour of every 1kg, after high speed dispersion is even, adding diameter by the mass ratio 2:10 of grinding ball and thick silica flour in thick silica flour slurry is the grinding of 1mm zirconium oxide abrasive ball, grinding 8h, obtain pre-treatment fine silica powder slurry, wherein in step (1), solvent is alcohol, ethylene glycol, glycerine, polyvinylpyrrolidone, dispersion agent is Witco 1298 Soft Acid class, urea, sodium polyphosphate, silicates, polyoxyethylene glycol.
(2) prepare nano level silica flour slurry: obtain in step (1) pre-treatment fine silica powder slurry in, add solvent and dispersion agent, high speed dispersion is even, add, by the mass ratio 2:10 of grinding ball and thick silica flour, the zirconium oxide abrasive ball grinding that diameter is 0.1mm in fine silica powder slurry, grinding 4h, again add solvent and dispersion agent grinding 2h, obtain nano level silica flour slurry, wherein in step (2), solvent is alcohol, ethylene glycol, glycerine, polyvinylpyrrolidone, acetone, dispersion agent is Witco 1298 Soft Acid class, urea, sodium polyphosphate, silicates, polyoxyethylene glycol, Xylo-Mucine.
(3) nano level silica flour is prepared: step (2) is obtained nano level silica flour slurry, carry out vacuum-drying, drying temperature is 30 DEG C, it is dry until material moisture content is less than 1000ppm, it is dried, after dry, powder body is pulverized and is broken up, and obtains nano level silica flour, and its particle size range is 100��200nm.
Embodiment 9:
Particle diameter of the present invention is the preparation of 200nm��300nm silica flour:
(1) pre-treatment fine silica powder slurry is prepared: get the thick silica flour that particle diameter is 15 ��m, solvent acetone is added by solvent 20kg in the thick silica flour of every 1kg, Lalgine class dispersion agent is added again by dispersion agent 100g in the thick silica flour of every 1kg, after high speed dispersion is even, adding diameter by the mass ratio 2:10 of grinding ball and thick silica flour in thick silica flour slurry is the grinding of 1.5mm zirconium oxide abrasive ball, grinding 6h, obtain pre-treatment fine silica powder slurry, wherein in step (1), solvent is alcohol, ethylene glycol, glycerine, polyvinylpyrrolidone, acetone, hexanaphthene, dispersion agent is Witco 1298 Soft Acid class, urea, sodium polyphosphate, silicates, polyoxyethylene glycol, Xylo-Mucine, Lalgine class.
(2) prepare nano level silica flour slurry: obtain in step (1) pre-treatment fine silica powder slurry in, add solvent and dispersion agent, high speed dispersion is even, add, by the mass ratio 1.5:10 of grinding ball and thick silica flour, the zirconium oxide abrasive ball grinding that diameter is 0.2mm in fine silica powder slurry, grinding 3h, again add solvent and dispersion agent grinding 2h, obtain nano level silica flour slurry, wherein in step (2), solvent is alcohol, ethylene glycol, glycerine, polyvinylpyrrolidone, acetone, hexanaphthene, butanone, dispersion agent is Witco 1298 Soft Acid class, urea, sodium polyphosphate, silicates, polyoxyethylene glycol, Xylo-Mucine, Lalgine class, polyacrylic.
(3) nano level silica flour is prepared: step (2) is obtained nano level silica flour slurry, carry out vacuum-drying, drying temperature is 40 DEG C, it is dry until material moisture content is less than 1000ppm, it is dried, after dry, powder body is pulverized and is broken up, and obtains nano level silica flour, and its particle size range is 200��300nm.
Embodiment 10:
Particle diameter of the present invention is the preparation of 200��300nm silica flour:
(1) pre-treatment fine silica powder slurry is prepared: get the thick silica flour that particle diameter is 15 ��m, solvent is added by solvent 20kg in the thick silica flour of every 1kg, dispersion agent is added again by dispersion agent 100g in the thick silica flour of every 1kg, after high speed dispersion is even, adding diameter by the mass ratio 2:10 of grinding ball and thick silica flour in thick silica flour slurry is the grinding of 1.5mm zirconium oxide abrasive ball, grinding 6h, obtain pre-treatment fine silica powder slurry, wherein in step (1), solvent is alcohol, ethylene glycol, glycerine, polyvinylpyrrolidone, acetone, hexanaphthene, butanone, butanols, dispersion agent is Witco 1298 Soft Acid class, urea, sodium polyphosphate, silicates, polyoxyethylene glycol, Xylo-Mucine, Lalgine class, polyacrylic, polyvinylpyrrolidone.
(2) prepare nano level silica flour slurry: obtain in step (1) pre-treatment fine silica powder slurry in, add solvent and dispersion agent, high speed dispersion is even, add, by the mass ratio 1.5:10 of grinding ball and thick silica flour, the zirconium oxide abrasive ball grinding that diameter is 0.2mm in fine silica powder slurry, grinding 3h, again add solvent and dispersion agent grinding 2h, obtain nano level silica flour slurry, wherein in step (2), solvent is alcohol, ethylene glycol, glycerine, polyvinylpyrrolidone, acetone, hexanaphthene, butanone, butanols, benzene class, dispersion agent is Witco 1298 Soft Acid class, urea, sodium polyphosphate, silicates, polyoxyethylene glycol, Xylo-Mucine, Lalgine class, polyacrylic, polyvinylpyrrolidone, lignosulfonic acid class.
(3) nano level silica flour is prepared: step (2) is obtained nano level silica flour slurry, it is dried under an inert atmosphere, drying temperature is 50 DEG C, it is dry until material moisture content is less than 1000ppm, it is dried, after dry, powder body is pulverized and is broken up, and obtains nano level silica flour, and its particle size range is 200��300nm.
Embodiment 11:
Particle diameter of the present invention is the preparation of 200��300nm silica flour:
(1) pre-treatment fine silica powder slurry is prepared: get the thick silica flour that particle diameter is 15 ��m, solvent is added by solvent 20kg in the thick silica flour of every 1kg, dispersion agent is added again by dispersion agent 100g in the thick silica flour of every 1kg, after high speed dispersion is even, adding diameter by the mass ratio 2:10 of grinding ball and thick silica flour in thick silica flour slurry is the grinding of 1.5mm zirconium oxide abrasive ball, grinding 2h, obtain pre-treatment fine silica powder slurry, wherein in step (1), solvent is alcohol, ethylene glycol, glycerine, polyvinylpyrrolidone, acetone, hexanaphthene, butanone, butanols, benzene, dispersion agent is Witco 1298 Soft Acid class, urea, sodium polyphosphate, silicates, polyoxyethylene glycol, Xylo-Mucine, Lalgine class, polyacrylic, polyvinylpyrrolidone, lignosulfonic acid class, Sodium salts humic acids.
(2) prepare nano level silica flour slurry: obtain in step (1) pre-treatment fine silica powder slurry in, add aqueous solvent and dispersion agent urea, high speed dispersion is even, add, by the mass ratio 1.5:10 of grinding ball and thick silica flour, the zirconium oxide abrasive ball grinding that diameter is 0.2mm in fine silica powder slurry, grinding 3h, again add solvent and dispersion agent grinding 2h, obtain nano level silica flour slurry;
Prepare nano level silica flour: step (2) is obtained nano level silica flour slurry, it is dried under an inert atmosphere, drying temperature is 50 DEG C, it is dry until material moisture content is less than 1000ppm, it is dried, after dry, powder body is pulverized and is broken up, and obtains nano level silica flour, and its particle size range is 200��300nm.
Claims (10)
1. the method that a nano silicone powder material becomes more meticulous and prepares, it is characterised in that, concrete preparation process is as follows:
(1) pre-treatment fine silica powder slurry is prepared: get the thick silica flour that particle diameter is 5 ��m��50 ��m, add solvent and dispersion agent, after high speed dispersion is even, obtained thick silica flour slurry, adding diameter in thick silica flour slurry again is the grinding of 0.5mm��5mm zirconium oxide abrasive ball, after grinding, obtain pre-treatment fine silica powder slurry;
(2) nano level silica flour slurry is prepared: in the pre-treatment fine silica powder slurry obtained in step (1), add solvent and dispersion agent, high speed dispersion is even, the zirconium oxide abrasive ball grinding that diameter is 0.01mm��0.5mm is added in fine silica powder slurry, after grinding, obtain nano level silica flour slurry;
Preparing nano level silica flour: step (2) is obtained nano level silica flour slurry and is dried, after dry, powder body is pulverized and is broken up, and obtains nano level silica flour.
2. a kind of nano silicone powder material according to claim 1 becomes more meticulous the method for preparation, it is characterised in that: the solvent used in described step (1) and step (2) is water, one or more combination in alcohol class, polyvinylpyrrolidone, ketone class, hexanaphthene, benzene class.
3. the method that a kind of nano silicone powder material according to claim 2 becomes more meticulous and prepares, it is characterised in that: described alcohol class is one or more the combination in alcohol, dehydrated alcohol, ethylene glycol, glycerine, butanols; Described ketone class is one or both the combination in acetone or butanone.
4. the method that a kind of nano silicone powder material according to claim 1 becomes more meticulous and prepares, it is characterized in that: the dispersion agent used in described step (1) and step (2) is one or more the combination in polymer organic polymer class, organic molecule class and mineral-type dispersion agent.
5. the method that a kind of nano silicone powder material according to claim 4 becomes more meticulous and prepares, it is characterised in that: described polymer organic polymer class is one or more the combination in polyoxyethylene glycol, Xylo-Mucine, Lalgine class, polyacrylic, polyvinylpyrrolidone, lignosulfonic acid class, Sodium salts humic acids; Described organic molecule class is one or both in Witco 1298 Soft Acid class or urea; Described mineral-type dispersion agent is one or both in sodium polyphosphate or silicates.
6. the method that a kind of nano silicone powder material according to claim 1 becomes more meticulous and prepares, it is characterised in that: in described step (1), the weight ratio of thick silica flour, solvent and dispersion agent is 1:0.5��20:0.001��0.2.
7. the method that a kind of nano silicone powder material according to claim 1 becomes more meticulous and prepares, it is characterised in that: the weight ratio of described thick silica flour and grinding ball is 10:1��3.
8. a kind of nano silicone powder material according to claim 1 become more meticulous preparation method, it is characterised in that: described step (1) be ground to ball-milling technology, milling time 2h��10h; Step (2) be ground to ball-milling technology, milling time 2h��8h.
9. the method that a kind of nano silicone powder material according to claim 1 becomes more meticulous and prepares, it is characterized in that: the described dry atmosphere in step (3) is inert atmosphere or vacuum-drying, drying temperature is room temperature ~ 50 DEG C, dry until material moisture content is less than 1000ppm.
10. the method that a kind of nano silicone powder material according to claim 1 becomes more meticulous and prepares, it is characterized in that: obtaining the total scope in nano silicone powder footpath after dry in described step (3) is 50nm��500nm, and nano silicone powder footpath can control to 50��100nm, 100��200nm, 200��300nm, 300��400nm, 400��500nm, five intervals respectively.
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