CN106146894A - A kind of preparation method of the high transparent hot phase-change material of high thermal insulation - Google Patents
A kind of preparation method of the high transparent hot phase-change material of high thermal insulation Download PDFInfo
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- CN106146894A CN106146894A CN201510201646.0A CN201510201646A CN106146894A CN 106146894 A CN106146894 A CN 106146894A CN 201510201646 A CN201510201646 A CN 201510201646A CN 106146894 A CN106146894 A CN 106146894A
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- 238000009413 insulation Methods 0.000 title claims abstract description 90
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 239000012782 phase change material Substances 0.000 title claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 215
- 239000011858 nanopowder Substances 0.000 claims abstract description 100
- 239000011164 primary particle Substances 0.000 claims abstract description 62
- 239000002243 precursor Substances 0.000 claims abstract description 42
- 238000004108 freeze drying Methods 0.000 claims abstract description 40
- 239000000463 material Substances 0.000 claims abstract description 40
- 239000006185 dispersion Substances 0.000 claims abstract description 29
- 238000000227 grinding Methods 0.000 claims abstract description 27
- -1 tungsten cesium compound Chemical class 0.000 claims abstract description 27
- 238000009826 distribution Methods 0.000 claims abstract description 20
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 19
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000012298 atmosphere Substances 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 13
- KVXKIRARVMGHKF-UHFFFAOYSA-G indium(3+);tin(4+);heptahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[In+3].[Sn+4] KVXKIRARVMGHKF-UHFFFAOYSA-G 0.000 claims abstract description 10
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 239000011521 glass Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 5
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 50
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 48
- 239000008367 deionised water Substances 0.000 claims description 46
- 229910021641 deionized water Inorganic materials 0.000 claims description 46
- 230000007704 transition Effects 0.000 claims description 41
- 238000000034 method Methods 0.000 claims description 36
- 239000004576 sand Substances 0.000 claims description 34
- 230000009466 transformation Effects 0.000 claims description 30
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 238000001354 calcination Methods 0.000 claims description 20
- 150000001875 compounds Chemical class 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 19
- 239000002244 precipitate Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 16
- 239000002270 dispersing agent Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 12
- 229910052792 caesium Inorganic materials 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- 229910052720 vanadium Inorganic materials 0.000 claims description 10
- 229910021529 ammonia Inorganic materials 0.000 claims description 8
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 8
- 230000003068 static effect Effects 0.000 claims description 8
- 239000003638 chemical reducing agent Substances 0.000 claims description 7
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- GVFOJDIFWSDNOY-UHFFFAOYSA-N antimony tin Chemical compound [Sn].[Sb] GVFOJDIFWSDNOY-UHFFFAOYSA-N 0.000 claims description 6
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000012046 mixed solvent Substances 0.000 claims description 6
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 229910052738 indium Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 claims description 5
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 5
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- KOPBYBDAPCDYFK-UHFFFAOYSA-N Cs2O Inorganic materials [O-2].[Cs+].[Cs+] KOPBYBDAPCDYFK-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- FAPDDOBMIUGHIN-UHFFFAOYSA-K antimony trichloride Chemical compound Cl[Sb](Cl)Cl FAPDDOBMIUGHIN-UHFFFAOYSA-K 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 4
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 claims description 4
- UUUGYDOQQLOJQA-UHFFFAOYSA-L vanadyl sulfate Chemical compound [V+2]=O.[O-]S([O-])(=O)=O UUUGYDOQQLOJQA-UHFFFAOYSA-L 0.000 claims description 4
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- 229920003023 plastic Polymers 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
- UEEJHVSXFDXPFK-UHFFFAOYSA-O N-dimethylethanolamine Chemical compound C[NH+](C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-O 0.000 claims description 2
- 229910019501 NaVO3 Inorganic materials 0.000 claims description 2
- 239000011324 bead Substances 0.000 claims description 2
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- OGUCKKLSDGRKSH-UHFFFAOYSA-N oxalic acid oxovanadium Chemical compound [V].[O].C(C(=O)O)(=O)O OGUCKKLSDGRKSH-UHFFFAOYSA-N 0.000 claims description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 2
- OMDPSZJSEZKXSY-UHFFFAOYSA-N oxygen(2-) propan-2-ol vanadium(2+) Chemical compound [O-2].[V+2].CC(C)O.CC(C)O.CC(C)O OMDPSZJSEZKXSY-UHFFFAOYSA-N 0.000 claims description 2
- 238000006385 ozonation reaction Methods 0.000 claims description 2
- JBIQAPKSNFTACH-UHFFFAOYSA-K vanadium oxytrichloride Chemical compound Cl[V](Cl)(Cl)=O JBIQAPKSNFTACH-UHFFFAOYSA-K 0.000 claims description 2
- 229910000352 vanadyl sulfate Inorganic materials 0.000 claims description 2
- AKUNKIJLSDQFLS-UHFFFAOYSA-M dicesium;hydroxide Chemical group [OH-].[Cs+].[Cs+] AKUNKIJLSDQFLS-UHFFFAOYSA-M 0.000 claims 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims 1
- 239000011248 coating agent Substances 0.000 abstract description 5
- 238000000576 coating method Methods 0.000 abstract description 5
- 238000004134 energy conservation Methods 0.000 abstract 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 25
- 238000005245 sintering Methods 0.000 description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 22
- KFZMGEQAYNKOFK-UHFFFAOYSA-N isopropyl alcohol Natural products CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 22
- 210000002469 basement membrane Anatomy 0.000 description 20
- 238000012360 testing method Methods 0.000 description 20
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 description 13
- 238000001035 drying Methods 0.000 description 12
- 238000002834 transmittance Methods 0.000 description 11
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 11
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 10
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 10
- 239000007888 film coating Substances 0.000 description 10
- 238000009501 film coating Methods 0.000 description 10
- 230000003287 optical effect Effects 0.000 description 9
- 235000013339 cereals Nutrition 0.000 description 8
- 239000002086 nanomaterial Substances 0.000 description 8
- 241000209094 Oryza Species 0.000 description 7
- 235000007164 Oryza sativa Nutrition 0.000 description 7
- 230000008859 change Effects 0.000 description 7
- 238000012545 processing Methods 0.000 description 7
- 235000009566 rice Nutrition 0.000 description 7
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 7
- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 235000020265 peanut milk Nutrition 0.000 description 6
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 229910052721 tungsten Inorganic materials 0.000 description 5
- 239000010937 tungsten Substances 0.000 description 5
- 239000004698 Polyethylene Substances 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 4
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 4
- 238000006748 scratching Methods 0.000 description 4
- 230000002393 scratching effect Effects 0.000 description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 229910001930 tungsten oxide Inorganic materials 0.000 description 3
- 102000004160 Phosphoric Monoester Hydrolases Human genes 0.000 description 2
- 108090000608 Phosphoric Monoester Hydrolases Proteins 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910001942 caesium oxide Inorganic materials 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 229920002799 BoPET Polymers 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
- BWCRCMAQBZVTOM-UHFFFAOYSA-N [W]=O.[V] Chemical compound [W]=O.[V] BWCRCMAQBZVTOM-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- GLQMDRJYEQDASO-UHFFFAOYSA-N antimony;trihydrate Chemical compound O.O.O.[Sb] GLQMDRJYEQDASO-UHFFFAOYSA-N 0.000 description 1
- 210000005252 bulbus oculi Anatomy 0.000 description 1
- 150000001664 caesium compounds Chemical class 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 125000003916 ethylene diamine group Chemical group 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
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- 150000004676 glycans Chemical class 0.000 description 1
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- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- VVRQVWSVLMGPRN-UHFFFAOYSA-N oxotungsten Chemical compound [W]=O VVRQVWSVLMGPRN-UHFFFAOYSA-N 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
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- 230000002441 reversible effect Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000012815 thermoplastic material Substances 0.000 description 1
- 229910021509 tin(II) hydroxide Inorganic materials 0.000 description 1
- 150000003658 tungsten compounds Chemical class 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
The invention discloses the preparation method of a kind of high transparent hot phase-change material of high thermal insulation, comprise the steps: that (one) prepares the VO that primary particle size is not more than 20nm2Nano-powder, i.e. V powder；(2) the antimony stannum hydroxide precursor that primary particle size is not more than 20nm, i.e. A powder are prepared；(3) for preparing primary particle size no more than 20nm prepares indium tin hydroxide precursor, i.e. I powder；(4) the tungsten cesium compound precursor that primary particle size is not more than 20nm, i.e. W powder are prepared；(5) by V powder according to percentage by weight 1%-99% join in A powder, I powder and W powder any one, any two or three combination formed compositions in; put into dispersion tank; grinding distribution; pour into again in crucible after lyophilization; under the atmosphere of inert gas shielding; calcine 3-48 hour at 460-680 DEG C, after cooling, it is thus achieved that the hot phase-change material of high transparent high thermal insulation.The nano-powder that the present invention is obtained, can be widely applied to the sight glass coating material such as automobile, building, has important economy, energy-conservation value.
Description
Technical field
The present invention relates to the preparation method of a kind of high transparent hot phase-change material of high thermal insulation, prepared out
Nano-powder and nano pulp there is the function of the high transparent hot phase transformation of high thermal insulation.
Background technology
At present both at home and abroad it has been found that the nano material of associated hot phase transition function of report or the transparency heat insulation
The preparation method of material is a lot, but, disclosed technical data when provided in technical method all
It is limited.
Involved by a kind of nano ATO raw powder's production technology disclosed in Chinese patent CN103318951A
Nanometer-sized Antimony Doped Tin ATO raw powder's production technology in, one is to make simply to have employed traditional reaction,
Washing, filters, the method for sintering, is not involved with reactant limit dispersion at one's side limit reaction controlling once
The method of particle diameter, does not take the size of multiple controlling measurement primary particle size, and two is that ATO itself also only has
Single transparent heat-insulated function, is not involved with phase-change characteristic.
A kind of heat-insulating and energy-saving new material WO disclosed in Chinese patent CN102583552A3Nano-powder and system thereof
Provided in Preparation Method, although the raw material of employing has WO3、Cs2O、Sb(OH)3、Sn(OH)2Class
As raw material, but, prepare and the method for powder body simply have employed traditional reaction stirring, dry, burn
The methods such as knot, prepared nano-powder primary particle size out is also more than 40 nanometers, although have certain
Transparent and high heat-proof quality, but be not involved with reactant and use multiple controlling measurement when starting to react
The method of primary particle size and technique, be also not involved with hot phase transition function.
A kind of thermochromic particulate disclosed in Chinese patent CN102066261A and dispersion liquid thereof and manufacture method
And light modulation property coating, light modulation property film, light modulation property ink, this patent contains VO2The particle of (R phase) and
TiO2Particle, elaborates that emphatically the hot phase transition function light modulation of the hot Phase-change particles of below mean diameter 200nm is made
With, and do not illustrate high transparent high thermal insulation, and have heat-insulating and energy-saving function and effect.
Carbon cladding vanadium dioxide nano granule and preparation method thereof disclosed in Chinese patent CN103554997A
In, the nanoparticle related to be the three-dimensional dimension of inner core material of the vanadium dioxide used also be 100nm
Particles below pattern, and use traditional hydro-thermal reaction situ carbon coating technology, producing preparation
Nanometer VO2Powder process adds WO3And polysaccharide material, obtain under pyroreaction and can reduce phase transformation
Temperature, has the carbon cladding VO of certain heat absorption, heat insulating function2The related content of nano-powder, this side
Vanadium oxide primary particle size prepared by method is relatively big, and prepares VO2The technical process link of powder body is too many, industry
Metaplasia product control is relatively difficult.
In a kind of Vanadium dioxide composite powder and preparation method thereof disclosed in Chinese patent CN103073942B,
Elaborate emphatically the vanadium dioxide primary particle size state at below 200nm, be simply mentioned to use pass
The mix and blend mode of system is adulterated and is added various metallic elements, it is achieved have the compound of certain hot phase transition function
Raw powder's production technology, and it is little to be not involved with primary particle size, high transparent, high thermal insulation, and have
The preparation method of hot phase-change material,
These method major defects are VO2The primary particle size of nanoparticle is excessive, is confined to micron order, sub-micro
The VO of meter level2Relevant phase-change material, is confined to by traditional hydro-thermal reaction mode or the mode of mix and blend
Prepare the VO in 100nm-200nm particle size range2Phase-change material, these materials are relatively big because of primary particle size,
And function is more single, preparation process is the most loaded down with trivial details and complicated, uses coating out prepared by these materials
The spectrophotometric data of material is the most all at visible light transmissivity less than 40%, IR rejection rate less than 40%.Cause
This, in use maximum defect is that light transmission is bad, and heat-proof quality is poor, if it is desired to be applied to vapour
Car windshield or other high transparent applications etc. have significant limitation, and marketing is relatively difficult.
The many defects existed based on these product technologies, research and probe to solve nano-functional material
Multiplicity demand, should solve primary particle size big, the problem that light transmission is the highest, heat-proof quality to be solved
The problem that difference is more single with function, has the most urgent market demand.
Vanadium dioxide VO2There are some isomerisms to crystallize, are respectively defined as A, B, C, D, M, R phase,
It is wherein R phase in the most stable of crystalline phase of near room temperature, crystalline texture as having with rutile, so also known as
For Rutile Type.R phase hypovanadic oxide VO2There is hot phase-change characteristic.
Hot phase-change characteristic, refers to that the optical property of material such as passes through, reflects or absorption etc. is with the temperature of material
There is reversible change performance in change.Such as infrared ray wave band, the i.e. change of the wave band transmitance more than 780nm
Change, although but the invisible change transmitance with material temperature of naked eyes eyeball there occurs change, thus environment
Temperature changes the most therewith, is defined as hot phase transformation.
Rutile phase hypovanadic oxide purely is monoclinic crystal (M phase) when less than 68 degree, special in quasiconductor
Property, i.e. infrared ray is had higher transmitance；When higher than 68 degree, become regular crystal (R phase), in
Metallic character, becomes high reflection to infrared ray.
Vanadium dioxide VO2Phase transition temperature can by mix wolfram element amount or change structure regulating.Also have specially
Profit report mixes other element or compound changes and thinks temperature.So the VO in the present invention2(phase) is received
Rice flour body and slurry include the rutile phase hypovanadic oxide VO mixed of wolfram element2。
Summary of the invention
For the above-mentioned deficiency of prior art, according to embodiments of the invention, it is desirable to provide a kind of high transparency
Property the hot phase-change material of high thermal insulation preparation method, it is intended to one be intended to improve nano-functional material transparent
Property, two are intended to improve the heat-insulating and energy-saving efficiency of nano-functional material, and three are intended to reduce hot phase transition temperature, and
Will the high transparent of nano material to be met, high thermal insulation and hot phase transition performance.Therefore, want simultaneously
Meet high transparent, high thermal insulation and the characteristic of low transformation temperature.
According to embodiment, the preparation side of a kind of high transparent hot phase-change material of high thermal insulation that the present invention provides
Method, comprises the steps:
(1) VO that primary particle size is not more than 20nm is prepared2Nano-powder
By the vanadium-containing compound of following weight percent, Tungstenic compound, mixed solvent, dispersant and
Reducing agent is put in the reactor containing mill ball, the stirring rotator of high speed rotating reactor, rotor speed
For 1000-8000 rev/min, the temperature in hydrothermal reaction kettle is 160-300 DEG C, and pressure is 1-20kg,
Reaction jitter time is 16-100 hour, obtains primary particle size and be not more than after grinding, reacting and disperse
The VO of 10nm2Precursor, i.e. V powder；
1. vanadium-containing compound: 5%-20%；
2. Tungstenic compound: 0.1%-1%；
3. dispersant: 0.1-1%；
4. mixed solvent: 80%-94.7%；
5. reducing agent: 0.1%-1%；
(2) the antimony stannum hydroxide precursor that primary particle size is not more than 20nm is prepared
Butter of antimony. SbCl3Powder body and stannum grain are put according to the different weight ratio in the range of weight ratio 1%-99%
Enter in the hydrochloric acid solution that concentration is 36%, after adding appropriate deionized water heating for dissolving, pour into equipped with grinding
In the sand mill of ball, while speed lapping disperses 6 hours, add appropriate ammonia adjusting pH value is 7,
After the most static placement 72 hours, transparency liquid above is taken out, big following precipitate adds
Amount deionized water, repeats procedures described above 3 times, the precipitate lyophilization finally precipitated
Method obtains the antimony tin compound precursor that primary particle size is not more than 20nm, i.e. A powder；
(3) for preparing primary particle size no more than 20nm prepares indium tin hydroxide precursor
It is 36% that indium nail and stannum grain are put into concentration according to the different ratio in the range of weight ratio 1%-99%
In the mixed solution of nitric acid and hydrochloric acid, after adding appropriate deionized water heating for dissolving, pour into equipped with grinding
In the sand mill of ball, while starting speed lapping dispersion 6 hours, add appropriate ammonia and adjust pH value
Be 7, then after static placement 72 hours, transparency liquid above taken out, in following precipitate again
Adding a large amount of deionized water, repeat procedures described above 3 times, the precipitate finally precipitated is with cold
Lyophilizing drying method obtains the indium tin hydroxide precursor that primary particle size is not more than 20nm, i.e. I powder；
(4) the tungsten cesium compound precursor that primary particle size is not more than 20nm is prepared
Tungstenic compound and containing cesium compound according to the different weight ratio mixing in the range of 1%-99% after,
Pour into equipped with in the sand mill of mill ball, then add appropriate deionized water and a small amount of dispersant phosphoric acid,
After speed lapping disperses 6 hours, obtain, with freeze-drying method, the tungsten caesium that primary particle size is not more than 20nm
Compound precursor, i.e. W powder；
(5) by V powder according to percentage by weight 1%-99% join in A powder, I powder and W powder any
In the compositions that two or three combination a kind of, any is formed, put into dispersion tank, grinding distribution, freezing
Pour into again in crucible after drying, under the atmosphere of inert gas shielding, at 460-680 DEG C, calcine 3-48
Hour, after cooling, it is thus achieved that the hot phase-change material of high transparent high thermal insulation.
According to an embodiment, the preparation method of the present invention aforementioned high transparent hot phase-change material of high thermal insulation
Step () in, mill ball be the glass bead of a diameter of 0.05mm-3mm, metal ball, zirconia ball,
One or more in cerium oxide ball and alumina balls；Mill ball is (1-3) with the volume ratio of reactant:
(1-30)；Vanadium-containing compound is vanadium pentoxide V2O5, sodium metavanadate NaVO3, vanadium oxysulfate VOSO4·nH2O、
Vanadyl oxalate VOC2O4·nH2O, vanadium oxytrichloride VOCl3With Triisopropoxyvanadium(V) oxide C9H21O4One in V；Contain
Tungsten compound is phosphotungstic acid, Sodium phosphotungstate and WO3In at least one；Reducing agent is ethylenediamine, three ethanol
At least one in amine and N.N-dimethylethanolamine；Dispersant is in phosphoric acid, nitric acid, hydrochloric acid and oxalic acid
At least one；Reaction dissolvent is methanol and deionized water volume ratio 1:1 mixed liquor；
According to an embodiment, the preparation method of the present invention aforementioned high transparent hot phase-change material of high thermal insulation
Step (four) in, Tungstenic compound is phosphotungstic acid, Sodium phosphotungstate and WO3In at least one；Containing caesium
Compound is Cs2O Cs2O, cesium peroxide Cs2O2, super Cs2O CsO2With ozonisation caesium CsO3In one
Plant and multiple.
According to an embodiment, the preparation method of the present invention aforementioned high transparent hot phase-change material of high thermal insulation
Step (five) in, V powder and A powder combination after, grinding distribution, obtained powder body after lyophilization, i.e.
VA powder；VA powder obtains high transparent high thermal insulation hot phase transformation nano-powder, i.e. VAO after calcining, cooling
Nano-powder.
According to an embodiment, the preparation method of the present invention aforementioned high transparent hot phase-change material of high thermal insulation
Step (five) in, V powder and I powder combination after, grinding distribution, obtained powder body after lyophilization, i.e.
VI powder；VI powder obtains high transparent high thermal insulation hot phase transformation nano-powder, i.e. VIO after calcining, cooling
Nano-powder.
According to an embodiment, the preparation method of the present invention aforementioned high transparent hot phase-change material of high thermal insulation
Step (five) in, V powder and W powder combination after, grinding distribution, obtained powder body after lyophilization, i.e.
VW powder；VW powder obtains high transparent high thermal insulation hot phase transformation nano-powder, i.e. VWO after calcining, cooling
Nano-powder.
According to an embodiment, the preparation method of the present invention aforementioned high transparent hot phase-change material of high thermal insulation
Step (five) in, V powder, A powder and I powder combination after, grinding distribution, obtained powder after lyophilization
Body, i.e. VAI powder；VA powder obtains high transparent high thermal insulation hot phase transformation nano powder after calcining, cooling
Body, i.e. VAIO nano-powder.
According to an embodiment, the preparation method of the present invention aforementioned high transparent hot phase-change material of high thermal insulation
Step (five) in, after V powder and A powder, I powder, the combination of W powder, grinding distribution, institute after lyophilization
Obtain powder body, i.e. VAIW powder；VAIW powder obtains the high transparent hot phase of high thermal insulation after calcining, cooling
Become nano-powder, i.e. VAIWO nano-powder.
According to embodiment, the preparation method of this kind of high transparent hot phase-change material of high thermal insulation provided,
Appoint and take aforementioned VAO nano-powder, VIO nano-powder, VWO nano-powder, VAIO nano-powder or VAIWO
One in nano-powder, puts in sand mill, adds deionized water or organic solvent, and dispersant,
Add the mill ball of a diameter of 0.05-3mm of nano-powder weight 1-20 times, with 3000-12000 turn/
Minute rotating speed, speed lapping 1-30 hour, prepare high transparent high thermal insulation hot phase transformation nano pulp,
Wherein: the consumption of nano-powder be the consumption of 1wt%-50wt%, deionized water or organic solvent be 1wt%-99
Wt%, the consumption of dispersant is 0.1wt%-30wt%.
According to embodiment, the high transparent high thermal insulation hot phase transformation nanometer that aforementioned preparation process of the present invention obtains
Powder body and nano pulp add PVB, EVA, PET, PC, PP, PE, PMMA or TPO raw materials for production to
In, stir, extrude obtain have the high transparent hot phase transition function of high thermal insulation functional plastic master batch and
Sheet material or coiled material product.
Relative to prior art, in the present invention, one relates to Nanometer-sized Antimony Doped Tin and nano V tungsten oxygen
The nano-functional material of special lattice structure between compound, i.e. ATO precursor nano-powder and VO2 (B phase)
Nano-powder, after mixing according to certain weight ratio before heat treatment sinters, then through grinding distribution,
Lyophilization, the nanorize processing technique such as high temperature sintering, and the high transparent hot phase transformation of high thermal insulation obtained
The nano material of function, is called for short: VAO powder body.Two relate to nano indium tin hydroxide and nano V tungsten
The nano-functional material of special lattice structure between oxide, i.e. ITO precursor nano-powder and VO2 (B
Phase) nano-powder, after mixing according to certain weight ratio before heat treatment sinters, then through grinding
Dispersion, lyophilization, the nanorize processing technique such as high temperature sintering, and the high transparent high thermal insulation obtained
The nano material of hot phase transition function, is called for short: VIO powder body.Three relate to nanometer tungsten caesium oxide and nanometer
The nano-functional material of special lattice structure between vanadium tungsten oxide, i.e. mixes the WO3 precursor of cesium element
Nano-powder and VO2 (B phase) nano-powder, any according between 1%-99% before heat treatment sinters
After weight ratio mixing, then through nanorize processing technique such as grinding distribution, lyophilization, high temperature sinterings,
And the nano material of the high transparent hot phase transition function of high thermal insulation obtained, it is called for short VWO powder body.Four is to relate to
And to Nanometer-sized Antimony Doped Tin, nano indium tin hydroxide, between this three classes material of nano V tungsten oxide
The nano-functional material of special lattice structure, i.e. ATO precursor nano-powder, ITO precursor nano-powder,
VO2 (B phase) nano-powder, this three classes material is before heat treatment sinters, according to appointing between 1%-99%
After meaning weight ratio mixing, then through nanorize processing works such as grinding distribution, lyophilization, high temperature sinterings
Skill, and the nano material of the high transparent hot phase transition function of high thermal insulation obtained, be called for short VAIO powder body.Five
Relate to Nanometer-sized Antimony Doped Tin, nano indium tin hydroxide, nanometer tungsten caesium oxide and nano V tungsten
The nano-functional material of special lattice structure, i.e. ATO precursor nano powder between this four classes material of oxide
Body, ITO precursor nano-powder, mix the WO3 precursor nano-powder of cesium element, VO2 (B phase)
Nano-powder, this four classes material, before heat treatment sinters, mixes according to any weight ratio between 1%-99%
After conjunction, then through nanorize processing technique such as grinding distribution, lyophilization, high temperature sinterings, and obtain
The nano material of the high transparent hot phase transition function of high thermal insulation, be called for short VAIWO powder body.Six be take many
Weight control measure, control the primary particle size of nano material at no more than 20nm yardstick.I.e. in reactor
Adding appropriate, the Wear-resistant, high-temperature resistant mill ball of certain size size, by reaction temperature, rotating speed, ball
Diameter and with the weight ratio of reactant, pressure, the grinding distribution time, reflecting time etc. multiple because of
Have effect and control primary particle size size.
Present invention embodiment subsequently will demonstrate that, the high transparent high thermal insulation hot phase transformation material that the present invention prepares
The coated optical index light transmittance of material (nano-powder and nano pulp) can be more than 75%, IR rejection rate
More than 90%；Nano-powder has the good transparency, thermal insulation, and hot phase transformation critical temperature is less than 68
Degree；Nano-powder 2% mixes with common PET section, after reconstruction function master batch, then cuts with common PET
The thermal insulation film that the sheet 1:1 23um that draws of mixing is thick, in optical wavelength at the near infrared range of 950nm point
IR rejection rate can be reached more than 75%, it is seen that light transmission rate is more than 90%.
Nano-powder out prepared by the present invention is added to the polyvinyl butyral in PVB raw materials for production
In powder, stir, extrude to obtain there is the heat insulation glued membrane of PVB of the high transparent hot phase transition function of high thermal insulation.
Nano-powder out prepared by the present invention is added to the polyester slice in PET raw materials for production or poly-
In ester powder material, stir, extrude obtain have the PET of the light high transparent hot phase transition function of high thermal insulation every
Thermoplastic materials master batch and various functional PET film and sheet metal coil.
Nano-powder out prepared by the present invention is added to the polyethylene section or poly-in PE raw materials for production
In ethylene powder material, stir, extrude and obtain that to have the PE of the high transparent hot phase transition function of high thermal insulation heat insulation
Plastic master batch and sheet metal coil.
Nano-powder out prepared by the present invention is added to the polyester slice in PC raw materials for production or polyester
In powder material, stir, extrude to obtain there is the PC heatpiston of the high transparent hot phase transition function of high thermal insulation
Master batch and sheet metal coil.
Nano-powder out prepared by the present invention add to the PMMA section in PMMA raw materials for production or
In powder material, stir, extrude to obtain there is the heat insulation mother of PMMA of the high transparent hot phase transition function of high thermal insulation
Grain and sheet material.
Nano-powder out prepared by the present invention is added to the EVA granule in EVA raw materials for production or EVA
In powder material, stir, extrude to obtain there is the EVA adiabatic gum of the high transparent hot phase transition function of high thermal insulation
Film.
Nano pulp out prepared by the present invention is added to the resin slurry in oil paint raw materials for production
In, stir, disperse to obtain the oil paint with the high transparent hot phase transition function of high thermal insulation.
Nano-powder out prepared by the present invention is added to the water-base resin in water paint raw materials for production
In slurry, stir, disperse to obtain the Water-based thermal insulation coating with the high transparent hot phase transition function of high thermal insulation.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture (TEM) of precursor solution according to embodiments of the present invention.
Detailed description of the invention
Below in conjunction with the accompanying drawings and specific embodiment, the present invention is expanded on further.These embodiments are interpreted as
It is merely to illustrate the present invention rather than limits the scope of the invention.Reading what the present invention recorded
After content, the present invention can be made various changes or modifications by those skilled in the art, these equivalence changes
The scope of the claims in the present invention is fallen into equally with amendment.
Embodiment 1
First prepare the VO that primary particle size is not more than 20nm2(B phase) solution: at 10L high-temperature high-pressure reaction kettle
In be respectively charged into according to this, the zirconia ball 6kg of the most a diameter of 0.1mm, 2. isopropanol vanadyl 200g, 3.
Phosphotungstic acid 4g, 4. methanol and pure water mixed solvent: 3788g, 5. dispersant: phosphatase 24 g, 6. reducing agent:
Triethanolamine 4g, builds lid, begins to warm up pressurization, and high speed rotating reactor stirring rotator, temperature sets
Being set to 260 degree, pressure is set as 15kg, and speed setting is 6000 revs/min, and reaction jitter time sets
It is set to 24 hours.Reacted through 24 hours, grind, disperse after obtain primary particle size be not more than 20nm's
VO2(B phase) precursor solution, as shown in Figure 1.
Again the VO of above-mentioned acquisition2(B phase) solution obtains VO through lyophilization2(B phase) nano-powder,
It is called for short: V powder.
Prepare the precursor that primary particle size is not more than the high heat insulation nano powder body of 20 nanometers, i.e. ATO, ITO,
WO3Precursor nano-powder before sintering.
Prepare antimony stannum hydroxide, it may be assumed that precursor before preparation ATO sintering.Prepare 1000ml glass beaker,
Pour 200g hydrochloric acid (36%), 50g deionized water, 80g Butter of antimony. (SbCl successively into3), 20g
Stannum grain, heating for dissolving, after waiting until to be completely dissolved, then pour what the zirconium oxide equipped with a diameter of 0.1mm was asked into
In sand mill, the PH adjusting solution with ammonia is 7, and motor speed is transferred to 12000 revs/min, starts
Speed lapping disperseed after 6 hours, then after static placement 72 hours, transparency liquid above was taken out,
Following precipitate adds a large amount of deionized water, repeats procedures described above 3 times, finally precipitate
The precipitate freeze-drying method that gets off obtains primary particle size and is not more than body before the antimony tin compound of 20nm
Body, is called for short: A powder.
Prepare indium tin hydroxide, it may be assumed that prepare the precursor before the sintering of ITO powder body.Prepare 1000ml
Glass beaker, pours 200g hydrochloric acid (36%), 50g deionized water successively into, and 100g indium is followed closely, 10g stannum
Grain, heating for dissolving, after waiting until to be completely dissolved, then pour the sand that the zirconium oxide equipped with a diameter of 0.1mm is asked into
In grinding machine, the PH adjusting solution with ammonia is 7, and motor speed is transferred to 12000 revs/min, starts height
After speed grinding distribution after 6 hours, more static placement 72 hours, transparency liquid above is taken out, under
The precipitate in face adds a large amount of deionized water, repeats procedures described above 3 times, finally under precipitation
The precipitate freeze-drying method come obtains the antimony tin compound precursor that primary particle size is not more than 20nm.
It is called for short: I powder.
Prepare tungsten cesium compound, it may be assumed that WO3Precursor before sintering.In sand mill tank, it is sequentially added into straight
Footpath is zirconia ball 500g, the 70g tungsten oxide (WO of 0.1mm3), 30g cesium peroxide (Cs2O), 200g
Deionized water, 1g dispersant (phosphoric acid), rotating speed is transferred to 12000 revs/min.Speed lapping dispersion 6
After hour, obtain the tungsten cesium compound precursor that primary particle size is not more than 20nm, letter with freeze-drying method
Claim: W powder.
Prepared by VA powder body: V powder and A powder are according to the mixed nano-powder of 1:1 ratio.Take i.e.: respectively
10gV powder, 10gA powder, 80g deionized water, 1g phosphoric acid, pour into successively and aoxidize equipped with a diameter of 0.1mm
In the sand mill of zirconium ball, adjustment of rotational speed is 12000 revs/min, start dispersion 12 hours, takes out dispersion
Liquid, the VA nano-powder before lyophilization acquisition primary particle size is not more than the sintering of 20nm.
Prepared by VAO powder body: again VA powder is installed to alumina crucible, puts at atmosphere furnace 580 degree calcining heat
Obtain antimony stannum vanadium class high transparent high thermal insulation hot phase transformation nano-powder after managing 12 hours, be called for short: VAO powder
Body.
Prepared by VAO nano pulp: again VAO powder body is taken 10g, deionized water (or ethanol) 89.9g,
The zirconia ball 300g of phosphoric acid 0.1g, a diameter of 0.1mm, is sequentially loaded in sand mill, and speed setting is
12000 revs/min, jitter time is set as 6 hours.Take out after shutdown, it is thus achieved that primary particle size is little
In aqueous (oiliness) nano pulp of the high transparency height insulation thermal phase transition function of 20 nanometers, it is called for short VAO and receives
Rice & peanut milk material.
Spectrophotometric data test result: take 10gVAO nano pulp, takes 40g acrylate pressure sensitive adhesive, takes
50g isopropanol, after mixing and stirring, scratches, with wet film applicator, the 23um that visible light transmissivity is 90%
On thick PET basement membrane, fit the PET that light transmittance is 90% thick for 23um again in 130 degree of 30 seconds drying rear surfaces
Basement membrane, is coated with dry film coating thickness 8um, records with the optical testing instrument of 950nm point and 1400nm point
Result is respectively 7085 and 7088；Hot phase transition temperature 44 degree.
Prepared by VI powder body: V powder and the I powder mixed nano-powder of 1:1 ratio.Take 10gV i.e.: respectively
Powder, 10gI powder, 80g deionized water, 1g phosphoric acid, pour into successively equipped with a diameter of 0.1mm zirconia ball
Sand mill in, adjustment of rotational speed is 12000 revs/min, start dispersion 12 hours, take out dispersion liquid,
VI nano-powder before lyophilization acquisition primary particle size is not more than the sintering of 20nm.
Prepared by VIO powder body: again VI powder is installed to alumina crucible, puts at atmosphere furnace 580 degree calcining heat
Obtain antimony stannum vanadium class high transparent high thermal insulation hot phase transformation nano-powder after managing 12 hours, be called for short VIO powder body.
Prepared by VIO nano pulp: again VIO powder body is taken 10g, deionized water (or ethanol) 89.9g,
The zirconia ball 300g of phosphoric acid 0.1g, a diameter of 0.1mm, is sequentially loaded in sand mill, and speed setting is
12000 revs/min, jitter time is set as 6 hours.Take out after shutdown, it is thus achieved that primary particle size is little
In aqueous (oiliness) nano pulp of the high transparency height insulation thermal phase transition function of 20 nanometers, it is called for short VIO and receives
Rice & peanut milk material.
Spectrophotometric data test result: take 10gVIO nano pulp, takes 40g acrylate pressure sensitive adhesive, takes
50g isopropanol, after mixing and stirring, scratches, with wet film applicator, the 23um that visible light transmissivity is 90%
On thick PET basement membrane, fit the PET that light transmittance is 90% thick for 23um again in 130 degree of 30 seconds drying rear surfaces
Basement membrane, is coated with dry film coating thickness 8um, records with the optical testing instrument of 950nm point and 1400nm point
Result is respectively 7870 and 7895；Hot phase transition temperature 44 degree.
Prepared by VW powder body: V powder and the W powder mixed nano-powder of 1:1 ratio.Take 10gV i.e.: respectively
Powder, 10gW powder, 80g deionized water, 1g phosphoric acid, pour into successively equipped with a diameter of 0.1mm zirconia ball
Sand mill in, adjustment of rotational speed is 12000 revs/min, start dispersion 12 hours, take out dispersion liquid,
VW nano-powder before lyophilization acquisition primary particle size is not more than the sintering of 20nm.
Prepared by VWO powder body: again VW powder is installed to alumina crucible, puts at atmosphere furnace 580 degree calcining heat
Obtain antimony stannum vanadium class high transparent high thermal insulation hot phase transformation nano-powder after managing 12 hours, be called for short VWO powder body.
Prepared by VWO nano pulp: again VWO powder body is taken 10g, deionized water (or ethanol) 89.9g,
The zirconia ball 300g of phosphoric acid 0.1g, a diameter of 0.1mm, is sequentially loaded in sand mill, and speed setting is
12000 revs/min, jitter time is set as 6 hours.Take out after shutdown, it is thus achieved that primary particle size is little
In aqueous (oiliness) nano pulp of the high transparency height insulation thermal phase transition function of 20 nanometers, it is called for short VWO and receives
Rice & peanut milk material.
Spectrophotometric data test result: take 10gVWO nano pulp, takes 40g acrylate pressure sensitive adhesive, takes
50g isopropanol, after mixing and stirring, scratches, with wet film applicator, the 23um that visible light transmissivity is 90%
On thick PET basement membrane, fit the PET that light transmittance is 90% thick for 23um again in 130 degree of 30 seconds drying rear surfaces
Basement membrane, is coated with dry film coating thickness 8um, records with the optical testing instrument of 950nm point and 1400nm point
Result is respectively 7590 and 7594；Hot phase transition temperature 44 degree.
Prepared by VIA powder body: V powder, A powder, and I powder is according to the mixed nano-powder of 1:1:1 ratio.
Take 10gV powder, 5gA powder, 5gI powder, 80g deionized water, 1g phosphoric acid i.e.: respectively, pour dress successively into
Having in the sand mill of a diameter of 0.1mm zirconia ball, adjustment of rotational speed is 12000 revs/min, start point
Dissipate 12 hours, take out dispersion liquid, before lyophilization obtains the sintering that primary particle size is not more than 20nm
VAI nano-powder.
Prepared by VAIO powder body: again VAI powder is installed to alumina crucible, puts into atmosphere furnace 580 degree calcining heat
Obtain antimony stannum vanadium class high transparent high thermal insulation hot phase transformation nano-powder after processing 12 hours, be called for short VAIO
Powder body.
Prepared by VAIO nano pulp: again VAIO powder body is taken 10g, deionized water (or ethanol) 89.9g,
The zirconia ball 300g of phosphoric acid 0.1g, a diameter of 0.1mm, is sequentially loaded in sand mill, and speed setting is
12000 revs/min, jitter time is set as 6 hours.Take out after shutdown, it is thus achieved that primary particle size is little
In aqueous (oiliness) nano pulp of the high transparency height insulation thermal phase transition function of 20 nanometers, it is called for short VAIO
Nano pulp.
Spectrophotometric data test result: take 10gVAIO nano pulp, takes 40g acrylate pressure sensitive adhesive,
Taking 50g isopropanol, after mixing and stirring, scratching visible light transmissivity with wet film applicator is 90%
PET basement membrane thick for 23um on, within 30 seconds, drying fit the again light transmittance of 23um thickness of rear surface for 130 degree is
The PET basement membrane of 90%, is coated with dry film coating thickness 8um, with 950nm point and the optic test of 1400nm point
Instrument records result and is respectively 7282 and 7290；Hot phase transition temperature is 44 degree.
Prepared by VAIW powder body: V powder, A powder, I powder, and W powder is according to the mixed nanometer of 1:1:1:1 ratio
Powder body.Take 15gV1 powder i.e.: respectively, 5gA1 powder, 5gI1 powder, 5gW1 powder, 120g deionized water,
1.5g phosphoric acid, pours in the sand mill equipped with a diameter of 0.1mm zirconia ball successively, and adjustment of rotational speed is
12000 revs/min, start dispersion 12 hours, take out dispersion liquid, obtain once grain through lyophilization
Footpath is not more than the VAIW nano-powder before the sintering of 20nm.
Prepared by VAIWO powder body: again VAIW powder is installed to alumina crucible, puts into atmosphere furnace 580 degree calcining
Heat treatment obtains antimony stannum vanadium class high transparent high thermal insulation hot phase transformation nano-powder after 12 hours, be called for short VAIWO
Powder body.
Prepared by VAIWO nano pulp: again VAIWO powder body is taken 10g, deionized water (or ethanol) 89.9g,
The zirconia ball 300g of phosphoric acid 0.1g, a diameter of 0.1mm, is sequentially loaded in sand mill, and speed setting is
12000 revs/min, jitter time is set as 6 hours.Take out after shutdown, it is thus achieved that primary particle size is little
In aqueous (oiliness) nano pulp of the high transparency height insulation thermal phase transition function of 20 nanometers, it is called for short VAIWO
Nano pulp.
Spectrophotometric data test result: take 10gVAIWO nano pulp, takes 40g acrylate pressure sensitive adhesive,
Taking 50g isopropanol, after mixing and stirring, scratching visible light transmissivity with wet film applicator is 90%
PET basement membrane thick for 23um on, within 30 seconds, drying fit the again light transmittance of 23um thickness of rear surface for 130 degree is
The PET basement membrane of 90%, is coated with dry film coating thickness 8um, with 950nm point and the optic test of 1400nm point
Instrument records result and is respectively 7388 and 7393；Hot phase transition temperature 44 degree.
Embodiment 2
First prepare the VO that primary particle size is not more than 20nm2(B phase) solution: at 10L high-temperature high-pressure reaction kettle
In be respectively charged into according to this, the zirconia ball 5kg of the most a diameter of 0.1mm, 2. isopropanol vanadyl 400g, 3.
Sodium phosphotungstate 12g；4. methanol and pure water mixed solvent 3564g, 5. dispersant: phosphatase 11 2g, 6. also
Former dose: triethanolamine 12g, build lid, begin to warm up pressurization, high speed rotating reactor stirring rotator,
Temperature is set as 260 degree, and pressure is set as 15kg, and speed setting is 6000 revs/min, reaction dispersion
Time is set as 24 hours.Reacted through 24 hours, grind, disperse after obtain primary particle size be not more than
The VO of 20nm2(B phase) precursor solution.
Again VO2 (B phase) solution of above-mentioned acquisition is obtained VO through lyophilization2(B phase) nano-powder,
It is called for short: V powder.
Prepare the precursor that primary particle size is not more than the high heat insulation nano powder body of 20 nanometers, i.e. ATO, ITO,
WO3Precursor nano-powder before sintering.
Prepare antimony stannum hydroxide, it may be assumed that precursor before preparation ATO sintering.Prepare 1000ml glass beaker,
Pour 200g hydrochloric acid (36%), 50g deionized water, 80g Butter of antimony. (SbCl successively into3), 20g
Stannum grain, heating for dissolving, after waiting until to be completely dissolved, then pour what the zirconium oxide equipped with a diameter of 0.1mm was asked into
In sand mill, the PH adjusting solution with ammonia is 7, and motor speed is transferred to 12000 revs/min, starts
Speed lapping disperseed after 6 hours, then after static placement 72 hours, transparency liquid above was taken out,
Following precipitate adds a large amount of deionized water, repeats procedures described above 3 times, finally precipitate
The precipitate freeze-drying method that gets off obtains primary particle size and is not more than body before the antimony tin compound of 20nm
Body, is called for short: A powder.
Prepare indium tin hydroxide, it may be assumed that prepare the precursor before the sintering of ITO powder body.Prepare 1000ml
Glass beaker, pours 200g hydrochloric acid (36%), 50g deionized water successively into, and 100g indium is followed closely, 10g stannum
Grain, heating for dissolving, after waiting until to be completely dissolved, then pour the sand that the zirconium oxide equipped with a diameter of 0.1mm is asked into
In grinding machine, the PH adjusting solution with ammonia is 7, and motor speed is transferred to 12000 revs/min, starts height
After speed grinding distribution after 6 hours, more static placement 72 hours, transparency liquid above is taken out, under
The precipitate in face adds a large amount of deionized water, repeats procedures described above 3 times, finally under precipitation
The precipitate freeze-drying method come obtains the antimony tin compound precursor that primary particle size is not more than 20nm,
It is called for short: I powder.
Prepare tungsten cesium compound, it may be assumed that the precursor before WO3 sintering.In sand mill tank, it is sequentially added into straight
Footpath is zirconia ball 500g, the 70g tungsten oxide (WO of 0.1mm3), 30g cesium peroxide (Cs2O), 200g
Deionized water, 1g dispersant (phosphoric acid), rotating speed is transferred to 12000 revs/min.Speed lapping dispersion 6
After hour, obtain the tungsten cesium compound precursor that primary particle size is not more than 20nm, letter with freeze-drying method
Claim: W powder.
Prepared by VA powder body: V powder and A powder are according to the mixed nano-powder of 1:1 ratio.Take i.e.: respectively
10gV powder, 10gA powder, 80g deionized water, 1g phosphoric acid, pour into successively and aoxidize equipped with a diameter of 0.1mm
In the sand mill of zirconium ball, adjustment of rotational speed is 12000 revs/min, start dispersion 12 hours, takes out dispersion
Liquid, the VA nano-powder before lyophilization acquisition primary particle size is not more than the sintering of 20nm.
Prepared by VAO powder body: again VA powder is installed to alumina crucible, puts at atmosphere furnace 580 degree calcining heat
Obtain antimony stannum vanadium class high transparent high thermal insulation hot phase transformation nano-powder after managing 12 hours, be called for short VAO powder body.
Prepared by VAO nano pulp: again VAO powder body is taken 10g, deionized water (or ethanol) 89.9g,
The zirconia ball 300g of phosphoric acid 0.1g, a diameter of 0.1mm, is sequentially loaded in sand mill, and speed setting is
12000 revs/min, jitter time is set as 6 hours.Take out after shutdown, it is thus achieved that primary particle size is little
In aqueous (oiliness) nano pulp of the high transparency height insulation thermal phase transition function of 20 nanometers, it is called for short VAO and receives
Rice & peanut milk material.
Spectrophotometric data test result: take 10gVAO nano pulp, takes 40g acrylate pressure sensitive adhesive, takes
50g isopropanol, after mixing and stirring, scratches, with wet film applicator, the 23um that visible light transmissivity is 90%
On thick PET basement membrane, fit the PET that light transmittance is 90% thick for 23um again in 130 degree of 30 seconds drying rear surfaces
Basement membrane, is coated with dry film coating thickness 8um, records with the optical testing instrument of 950nm point and 1400nm point
Result is respectively 7085 and 7088；Hot phase transition temperature is 38 degree.
Prepared by VI powder body: V powder and the I powder mixed nano-powder of 1:1 ratio.Take 10gV i.e.: respectively
Powder, 10gI powder, 80g deionized water, 1g phosphoric acid, pour into successively equipped with a diameter of 0.1mm zirconia ball
Sand mill in, adjustment of rotational speed is 12000 revs/min, start dispersion 12 hours, take out dispersion liquid,
VI nano-powder before lyophilization acquisition primary particle size is not more than the sintering of 20nm.
Prepared by VIO powder body: again VI powder is installed to alumina crucible, puts at atmosphere furnace 580 degree calcining heat
Obtain antimony stannum vanadium class high transparent high thermal insulation hot phase transformation nano-powder after managing 12 hours, be called for short VIO powder body.
Prepared by VIO nano pulp: again VIO powder body is taken 10g, deionized water (or ethanol) 89.9g,
The zirconia ball 300g of phosphoric acid 0.1g, a diameter of 0.1mm, is sequentially loaded in sand mill, and speed setting is
12000 revs/min, jitter time is set as 6 hours.Take out after shutdown, it is thus achieved that primary particle size is little
In aqueous (oiliness) nano pulp of the high transparency height insulation thermal phase transition function of 20 nanometers, it is called for short VIO and receives
Rice & peanut milk material.
Spectrophotometric data test result: take 10gVIO nano pulp, takes 40g acrylate pressure sensitive adhesive, takes
50g isopropanol, after mixing and stirring, scratches, with wet film applicator, the 23um that visible light transmissivity is 90%
On thick PET basement membrane, fit the PET that light transmittance is 90% thick for 23um again in 130 degree of 30 seconds drying rear surfaces
Basement membrane, is coated with dry film coating thickness 8um, records with the optical testing instrument of 950nm point and 1400nm point
Result is respectively 7870 and 7895；Hot phase transition temperature is 38 degree.
Prepared by VW powder body: V powder and the W powder mixed nano-powder of 1:1 ratio.Take 10gV i.e.: respectively
Powder, 10gW powder, 80g deionized water, 1g phosphoric acid, pour into successively equipped with a diameter of 0.1mm zirconia ball
Sand mill in, adjustment of rotational speed is 12000 revs/min, start dispersion 12 hours, take out dispersion liquid,
VW nano-powder before lyophilization acquisition primary particle size is not more than the sintering of 20nm.
Prepared by VWO powder body: again VW powder is installed to alumina crucible, puts at atmosphere furnace 580 degree calcining heat
Antimony stannum vanadium class high transparent high thermal insulation hot phase transformation nano-powder is obtained after managing 12 hours.It is called for short VWO powder body.
Prepared by VWO nano pulp: again VWO powder body is taken 10g, deionized water (or ethanol) 89.9g,
The zirconia ball 300g of phosphoric acid 0.1g, a diameter of 0.1mm, is sequentially loaded in sand mill, and speed setting is
12000 revs/min, jitter time is set as 6 hours.Take out after shutdown, it is thus achieved that primary particle size is little
In aqueous (oiliness) nano pulp of the high transparency height insulation thermal phase transition function of 20 nanometers, it is called for short VWO and receives
Rice & peanut milk material.
Spectrophotometric data test result: take 10gVWO nano pulp, takes 40g acrylate pressure sensitive adhesive, takes
50g isopropanol, after mixing and stirring, scratches, with wet film applicator, the 23um that visible light transmissivity is 90%
On thick PET basement membrane, fit the PET that light transmittance is 90% thick for 23um again in 130 degree of 30 seconds drying rear surfaces
Basement membrane, is coated with dry film coating thickness 8um, records with the optical testing instrument of 950nm point and 1400nm point
Result is respectively 7590 and 7594；Hot phase transition temperature is 38 degree.
Prepared by VIA powder body: V powder, A powder, and I powder is according to the mixed nano-powder of 1:1:1 ratio.
Take 10gV powder, 5gA powder, 5gI powder, 80g deionized water, 1g phosphoric acid i.e.: respectively, pour dress successively into
Having in the sand mill of a diameter of 0.1mm zirconia ball, adjustment of rotational speed is 12000 revs/min, start point
Dissipate 12 hours, take out dispersion liquid, before lyophilization obtains the sintering that primary particle size is not more than 20nm
VAI nano-powder.
Prepared by VAIO powder body: again VAI powder is installed to alumina crucible, puts into atmosphere furnace 580 degree calcining heat
Antimony stannum vanadium class high transparent high thermal insulation hot phase transformation nano-powder is obtained after processing 12 hours.It is called for short VAIO
Powder body.
Prepared by VAIO nano pulp: again VAIO powder body is taken 10g, deionized water (or ethanol) 89.9g,
The zirconia ball 300g of phosphoric acid 0.1g, a diameter of 0.1mm, is sequentially loaded in sand mill, and speed setting is
12000 revs/min, jitter time is set as 6 hours.Take out after shutdown, it is thus achieved that primary particle size is little
In aqueous (oiliness) nano pulp of the high transparency height insulation thermal phase transition function of 20 nanometers, it is called for short VAIO
Nano pulp.
Spectrophotometric data test result: take 10gVAIO nano pulp, takes 40g acrylate pressure sensitive adhesive,
Taking 50g isopropanol, after mixing and stirring, scratching visible light transmissivity with wet film applicator is 90%
PET basement membrane thick for 23um on, within 30 seconds, drying fit the again light transmittance of 23um thickness of rear surface for 130 degree is
The PET basement membrane of 90%, is coated with dry film coating thickness 8um, with 950nm point and the optic test of 1400nm point
Instrument records result and is respectively 7282 and 7290；Hot phase transition temperature is 38 degree.
Prepared by VAIW powder body: V powder, A powder, I powder and W powder are according to the mixed nanometer of 1:1:1:1 ratio
Powder body.Take 15gV powder, 5gA powder, 5gI powder, 5gW powder, 120g deionized water, 1.5g i.e.: respectively
Phosphoric acid, pours in the sand mill equipped with a diameter of 0.1mm zirconia ball successively, and adjustment of rotational speed is 12000
Rev/min, start dispersion 12 hours, take out dispersion liquid, obtain primary particle size through lyophilization little
VAIW nano-powder before the sintering of 20nm.
Prepared by VAIWO powder body: again VAIW powder is installed to alumina crucible, puts into atmosphere furnace 580 degree calcining
Heat treatment obtains antimony stannum vanadium class high transparent high thermal insulation hot phase transformation nano-powder after 12 hours, be called for short VAIWO
Powder body.
Prepared by VAIWO nano pulp: again VAIWO powder body is taken 10g, deionized water (or ethanol) 89.9g,
The zirconia ball 300g of phosphoric acid 0.1g, a diameter of 0.1mm, is sequentially loaded in sand mill, and speed setting is
12000 revs/min, jitter time is set as 6 hours.Take out after shutdown, it is thus achieved that primary particle size is little
In aqueous (oiliness) nano pulp of the high transparency height insulation thermal phase transition function of 20 nanometers, it is called for short VAIWO
Nano pulp.
Spectrophotometric data test result: take 10gVAIWO nano pulp, takes 40g acrylate pressure sensitive adhesive,
Taking 50g isopropanol, after mixing and stirring, scratching visible light transmissivity with wet film applicator is 90%
PET basement membrane thick for 23um on, within 30 seconds, drying fit the again light transmittance of 23um thickness of rear surface for 130 degree is
The PET basement membrane of 90%, is coated with dry film coating thickness 8um, with 950nm point and the optic test of 1400nm point
Instrument records result and is respectively 7388 and 7393；Hot phase transition temperature is 38 degree.
Claims (10)
1. the preparation method of the high transparent hot phase-change material of high thermal insulation, it is characterised in that comprise the steps:
(1) VO that primary particle size is not more than 20nm is prepared2Nano-powder
The vanadium-containing compound of following weight percent, Tungstenic compound, mixed solvent, dispersant and reducing agent are put in the reactor containing mill ball, the stirring rotator of high speed rotating reactor, rotor speed is 1000-8000 rev/min, temperature in hydrothermal reaction kettle is 160-300 DEG C, pressure is 1-20kg, reaction jitter time is 16-100 hour, obtains the VO that primary particle size is not more than 10nm after grinding, reacting and disperse2Precursor, i.e. V powder；
1. vanadium-containing compound: 5%-20%；
2. Tungstenic compound: 0.1%-1%；
3. dispersant: 0.1-1%；
4. mixed solvent: 80%-94.7%；
5. reducing agent: 0.1%-1%；
(2) the antimony stannum hydroxide precursor that primary particle size is not more than 20nm is prepared
Butter of antimony. SbCl3Powder body and stannum grain are put in the hydrochloric acid solution that concentration is 36% according to the different weight ratio in the range of weight ratio 1%-99%, after adding appropriate deionized water heating for dissolving, pour into equipped with in the sand mill of mill ball, while speed lapping disperses 6 hours, add appropriate ammonia adjusting pH value is 7, after the most static placement 72 hours, transparency liquid above is taken out, following precipitate adds a large amount of deionized water, repeat procedures described above 3 times, the precipitate freeze-drying method finally precipitated obtains the antimony tin compound precursor that primary particle size is not more than 20nm, i.e. A powder；
(3) for preparing primary particle size no more than 20nm prepares indium tin hydroxide precursor
Indium nail and stannum grain are put in the mixed solution of nitric acid that concentration is 36% and hydrochloric acid according to the different ratio in the range of weight ratio 1%-99%, after adding appropriate deionized water heating for dissolving, pour into equipped with in the sand mill of mill ball, while starting speed lapping dispersion 6 hours, add appropriate ammonia adjusting pH value is 7, after the most static placement 72 hours, transparency liquid above is taken out, following precipitate adds a large amount of deionized water, repeat procedures described above 3 times, the precipitate freeze-drying method finally precipitated obtains the indium tin hydroxide precursor that primary particle size is not more than 20nm, i.e. I powder；
(4) the tungsten cesium compound precursor that primary particle size is not more than 20nm is prepared
Tungstenic compound and containing cesium compound according to the different weight ratio mixing in the range of 1%-99% after, pour into equipped with in the sand mill of mill ball, add appropriate deionized water and a small amount of dispersant phosphoric acid again, after speed lapping disperses 6 hours, the tungsten cesium compound precursor that primary particle size is not more than 20nm, i.e. W powder is obtained with freeze-drying method；
(5) by V powder according to percentage by weight 1%-99% join in A powder, I powder and W powder any one, any two or three combination formed compositions in; put into dispersion tank; grinding distribution; pour into again in crucible after lyophilization; under the atmosphere of inert gas shielding; calcine 3-48 hour at 460-680 DEG C, after cooling, it is thus achieved that the hot phase-change material of high transparent high thermal insulation.
The preparation method of the high transparent hot phase-change material of high thermal insulation the most according to claim 1, it is characterized in that, in step (), mill ball is one or more in the glass bead of a diameter of 0.05mm-3mm, metal ball, zirconia ball, cerium oxide ball and alumina balls；Mill ball is (1-3) with the volume ratio of reactant: (1-30)；Vanadium-containing compound is vanadium pentoxide V2O5, sodium metavanadate NaVO3, vanadium oxysulfate VOSO4·nH2O, vanadyl oxalate VOC2O4·nH2O, vanadium oxytrichloride VOCl3With Triisopropoxyvanadium(V) oxide C9H21O4One in V；Tungstenic compound is phosphotungstic acid, Sodium phosphotungstate and WO3In at least one；Reducing agent is at least one in ethylenediamine, triethanolamine and N.N-dimethylethanolamine；Dispersant is at least one in phosphoric acid, nitric acid, hydrochloric acid and oxalic acid；Reaction dissolvent is methanol and deionized water volume ratio 1:1 mixed liquor.
The preparation method of the high transparent hot phase-change material of high thermal insulation the most according to claim 1, it is characterised in that in step (four), Tungstenic compound is phosphotungstic acid, Sodium phosphotungstate and WO3In at least one；It is Cs2O Cs containing cesium compound2O, cesium peroxide Cs2O2, super Cs2O CsO2With ozonisation caesium CsO3In one and multiple.
4. according to the preparation method of the high transparent hot phase-change material of high thermal insulation described in claim 1 or 2 or 3, it is characterised in that in step (five), after V powder and the combination of A powder, grinding distribution, obtained powder body after lyophilization, i.e. VA powder；VA powder obtains high transparent high thermal insulation hot phase transformation nano-powder, i.e. VAO nano-powder after calcining, cooling.
5. according to the preparation method of the high transparent hot phase-change material of high thermal insulation described in claim 1 or 2 or 3, it is characterised in that in step (five), after V powder and the combination of I powder, grinding distribution, obtained powder body after lyophilization, i.e. VI powder；VI powder obtains high transparent high thermal insulation hot phase transformation nano-powder, i.e. VIO nano-powder after calcining, cooling.
6. according to the preparation method of the high transparent hot phase-change material of high thermal insulation described in claim 1 or 2 or 3, it is characterised in that in step (five), after V powder and the combination of W powder, grinding distribution, obtained powder body after lyophilization, i.e. VW powder；VW powder obtains high transparent high thermal insulation hot phase transformation nano-powder, i.e. VWO nano-powder after calcining, cooling.
7. according to the preparation method of the high transparent hot phase-change material of high thermal insulation described in claim 1 or 2 or 3, it is characterised in that in step (five), after V powder, A powder and the combination of I powder, grinding distribution, obtained powder body after lyophilization, i.e. VAI powder；VA powder obtains high transparent high thermal insulation hot phase transformation nano-powder, i.e. VAIO nano-powder after calcining, cooling.
8. according to the preparation method of the high transparent hot phase-change material of high thermal insulation described in claim 1 or 2 or 3, it is characterised in that in step (five), after V powder and A powder, I powder, W powder combine, grinding distribution, obtained powder body after lyophilization, i.e. VAIW powder；VAIW powder obtains high transparent high thermal insulation hot phase transformation nano-powder, i.e. VAIWO nano-powder after calcining, cooling.
null9. the preparation method of the high transparent hot phase-change material of high thermal insulation，It is characterized in that，Appoint and take the VAO nano-powder that claim 4-8 prepares、VIO nano-powder、VWO nano-powder、One in VAIO nano-powder or VAIWO nano-powder，Put in sand mill，Add deionized water or organic solvent，And dispersant，Add the mill ball of a diameter of 0.05-3mm of nano-powder weight 1-20 times，With the rotating speed of 3000-12000 rev/min，Speed lapping 1-30 hour，Prepare high transparent high thermal insulation hot phase transformation nano pulp，Wherein: the consumption of nano-powder is 1wt%-50wt%，The consumption of deionized water or organic solvent is 1wt%-99wt%，The consumption of dispersant is 0.1wt%-30wt%.
10. in claim 1-9, arbitrary preparation method obtains high transparent high thermal insulation hot phase transformation nano-powder and nano pulp add in PVB, EVA, PET, PC, PP, PE, PMMA or TPO raw materials for production, stir, extrude to obtain and have the functional plastic master batch of the high transparent hot phase transition function of high thermal insulation and sheet material or coiled material product.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107603102A (en) * | 2017-09-15 | 2018-01-19 | 四川大学 | Lucite and preparation method thereof |
| CN107652604A (en) * | 2017-10-27 | 2018-02-02 | 四川大学 | Lucite production system |
| CN107936617A (en) * | 2017-11-22 | 2018-04-20 | 上海沪正实业有限公司 | A kind of weather-proof low-transmittance inorganic thermal insulation pigment of superelevation and preparation method thereof |
| CN111499957A (en) * | 2020-06-12 | 2020-08-07 | 济南大学 | Composite film with heat insulation effect and preparation method |
| CN115197545A (en) * | 2021-04-14 | 2022-10-18 | 上海沪正实业有限公司 | Medical sanitary hydrophilic anti-static functional filling master batch and application thereof |
| CN115403064A (en) * | 2022-09-20 | 2022-11-29 | 中国科学院长春应用化学研究所 | Cerium oxide and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1673096A (en) * | 2005-02-25 | 2005-09-28 | 昆明理工大学 | Prepn process of nano In-Sn oxide powder |
| US20070276072A1 (en) * | 2004-02-06 | 2007-11-29 | Thomas Schmidt | Method for the Production of Polyester Resins Containing Nanoscale Additives for Coating Powders |
| CN101993657A (en) * | 2009-08-14 | 2011-03-30 | 北京建筑技术发展有限责任公司 | Intelligent nano transparent insulating glass coating |
| CN102559025A (en) * | 2011-11-18 | 2012-07-11 | 上海沪正纳米科技有限公司 | Preparation method for high-performance transparent glass heat-insulating coating |
| CN104073027A (en) * | 2014-06-20 | 2014-10-01 | 尹作栋 | Preparation method of tin antimony oxide (ATO) water-based nano-dispersion slurry |
-
2015
- 2015-04-24 CN CN201510201646.0A patent/CN106146894B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070276072A1 (en) * | 2004-02-06 | 2007-11-29 | Thomas Schmidt | Method for the Production of Polyester Resins Containing Nanoscale Additives for Coating Powders |
| CN1673096A (en) * | 2005-02-25 | 2005-09-28 | 昆明理工大学 | Prepn process of nano In-Sn oxide powder |
| CN101993657A (en) * | 2009-08-14 | 2011-03-30 | 北京建筑技术发展有限责任公司 | Intelligent nano transparent insulating glass coating |
| CN102559025A (en) * | 2011-11-18 | 2012-07-11 | 上海沪正纳米科技有限公司 | Preparation method for high-performance transparent glass heat-insulating coating |
| CN104073027A (en) * | 2014-06-20 | 2014-10-01 | 尹作栋 | Preparation method of tin antimony oxide (ATO) water-based nano-dispersion slurry |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107603102A (en) * | 2017-09-15 | 2018-01-19 | 四川大学 | Lucite and preparation method thereof |
| CN107603102B (en) * | 2017-09-15 | 2019-11-08 | 四川大学 | Organic glass and preparation method thereof |
| CN107652604A (en) * | 2017-10-27 | 2018-02-02 | 四川大学 | Lucite production system |
| CN107936617A (en) * | 2017-11-22 | 2018-04-20 | 上海沪正实业有限公司 | A kind of weather-proof low-transmittance inorganic thermal insulation pigment of superelevation and preparation method thereof |
| CN111499957A (en) * | 2020-06-12 | 2020-08-07 | 济南大学 | Composite film with heat insulation effect and preparation method |
| CN115197545A (en) * | 2021-04-14 | 2022-10-18 | 上海沪正实业有限公司 | Medical sanitary hydrophilic anti-static functional filling master batch and application thereof |
| CN115403064A (en) * | 2022-09-20 | 2022-11-29 | 中国科学院长春应用化学研究所 | Cerium oxide and preparation method thereof |
| CN115403064B (en) * | 2022-09-20 | 2023-10-13 | 中国科学院长春应用化学研究所 | Cerium oxide and preparation method thereof |
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