CN115521081B - Fireproof layer material and preparation method thereof and non-heat-insulation composite fireproof glass - Google Patents
Fireproof layer material and preparation method thereof and non-heat-insulation composite fireproof glass Download PDFInfo
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- CN115521081B CN115521081B CN202211223526.7A CN202211223526A CN115521081B CN 115521081 B CN115521081 B CN 115521081B CN 202211223526 A CN202211223526 A CN 202211223526A CN 115521081 B CN115521081 B CN 115521081B
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- fireproof
- layer material
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- 239000011521 glass Substances 0.000 title claims abstract description 196
- 239000000463 material Substances 0.000 title claims abstract description 156
- 239000002131 composite material Substances 0.000 title claims abstract description 102
- 238000009413 insulation Methods 0.000 title claims description 37
- 238000002360 preparation method Methods 0.000 title abstract description 32
- 239000002245 particle Substances 0.000 claims abstract description 140
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 129
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 110
- 239000011258 core-shell material Substances 0.000 claims abstract description 69
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 62
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 46
- 239000002994 raw material Substances 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000004014 plasticizer Substances 0.000 claims abstract description 29
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000003381 stabilizer Substances 0.000 claims abstract description 26
- VLSRKCIBHNJFHA-UHFFFAOYSA-N 2-(trifluoromethyl)prop-2-enoic acid Chemical compound OC(=O)C(=C)C(F)(F)F VLSRKCIBHNJFHA-UHFFFAOYSA-N 0.000 claims abstract description 23
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000008367 deionised water Substances 0.000 claims abstract description 23
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 23
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 22
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 20
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 19
- 238000003860 storage Methods 0.000 claims abstract description 17
- 238000005516 engineering process Methods 0.000 claims abstract description 8
- 239000010410 layer Substances 0.000 claims description 240
- 239000000243 solution Substances 0.000 claims description 49
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 44
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 44
- 230000009970 fire resistant effect Effects 0.000 claims description 42
- 239000000377 silicon dioxide Substances 0.000 claims description 42
- 238000003756 stirring Methods 0.000 claims description 27
- 239000011259 mixed solution Substances 0.000 claims description 23
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 20
- 238000009826 distribution Methods 0.000 claims description 20
- 239000003063 flame retardant Substances 0.000 claims description 20
- 239000012792 core layer Substances 0.000 claims description 18
- 229930091371 Fructose Natural products 0.000 claims description 16
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 16
- 239000005715 Fructose Substances 0.000 claims description 16
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 16
- 229930006000 Sucrose Natural products 0.000 claims description 16
- 229910021538 borax Inorganic materials 0.000 claims description 16
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 16
- 239000004327 boric acid Substances 0.000 claims description 16
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 16
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 16
- 239000004328 sodium tetraborate Substances 0.000 claims description 16
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 16
- 239000005720 sucrose Substances 0.000 claims description 16
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 15
- 239000011229 interlayer Substances 0.000 claims description 14
- 150000002500 ions Chemical class 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 14
- 238000006116 polymerization reaction Methods 0.000 claims description 14
- 239000000839 emulsion Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 229910052710 silicon Inorganic materials 0.000 claims description 11
- 239000010703 silicon Substances 0.000 claims description 11
- 229920001577 copolymer Polymers 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- -1 poly (2- (trifluoromethyl) acrylic acid-butyl acrylate-methacrylic acid-methyl methacrylate Chemical compound 0.000 claims description 8
- CUVLMZNMSPJDON-UHFFFAOYSA-N 1-(1-butoxypropan-2-yloxy)propan-2-ol Chemical compound CCCCOCC(C)OCC(C)O CUVLMZNMSPJDON-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 235000003642 hunger Nutrition 0.000 claims description 6
- OQZCJRJRGMMSGK-UHFFFAOYSA-M potassium metaphosphate Chemical compound [K+].[O-]P(=O)=O OQZCJRJRGMMSGK-UHFFFAOYSA-M 0.000 claims description 6
- 239000012966 redox initiator Substances 0.000 claims description 6
- 230000037351 starvation Effects 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 239000012760 heat stabilizer Substances 0.000 claims description 5
- 229910003471 inorganic composite material Inorganic materials 0.000 claims description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 5
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 claims description 4
- CUDYYMUUJHLCGZ-UHFFFAOYSA-N 2-(2-methoxypropoxy)propan-1-ol Chemical compound COC(C)COC(C)CO CUDYYMUUJHLCGZ-UHFFFAOYSA-N 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 4
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 claims description 4
- 229920002472 Starch Polymers 0.000 claims description 4
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 4
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 4
- 235000019797 dipotassium phosphate Nutrition 0.000 claims description 4
- 229910000396 dipotassium phosphate Inorganic materials 0.000 claims description 4
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 4
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 4
- 235000019800 disodium phosphate Nutrition 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 4
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 4
- 235000019828 potassium polyphosphate Nutrition 0.000 claims description 4
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 4
- 235000019830 sodium polyphosphate Nutrition 0.000 claims description 4
- 239000008107 starch Substances 0.000 claims description 4
- 235000019698 starch Nutrition 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 239000011737 fluorine Substances 0.000 claims description 3
- 235000021552 granulated sugar Nutrition 0.000 claims description 3
- 238000010030 laminating Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 2
- 239000003112 inhibitor Substances 0.000 claims 2
- 238000006243 chemical reaction Methods 0.000 abstract description 15
- 239000002105 nanoparticle Substances 0.000 abstract description 10
- 238000000265 homogenisation Methods 0.000 abstract description 7
- 238000011049 filling Methods 0.000 abstract description 2
- 239000011257 shell material Substances 0.000 description 18
- 239000005341 toughened glass Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- 235000011187 glycerol Nutrition 0.000 description 14
- 229920000388 Polyphosphate Polymers 0.000 description 13
- 239000001205 polyphosphate Substances 0.000 description 13
- 235000011176 polyphosphates Nutrition 0.000 description 13
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 11
- 239000006185 dispersion Substances 0.000 description 11
- 238000005303 weighing Methods 0.000 description 11
- 239000012790 adhesive layer Substances 0.000 description 10
- 235000019353 potassium silicate Nutrition 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 238000002834 transmittance Methods 0.000 description 9
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 239000000853 adhesive Substances 0.000 description 7
- 230000001070 adhesive effect Effects 0.000 description 7
- 239000002390 adhesive tape Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 229940072033 potash Drugs 0.000 description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 6
- 235000015320 potassium carbonate Nutrition 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000007789 sealing Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 230000006870 function Effects 0.000 description 5
- 125000001165 hydrophobic group Chemical group 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 3
- 239000004111 Potassium silicate Substances 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- 239000011368 organic material Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 3
- 229910052913 potassium silicate Inorganic materials 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000005336 safety glass Substances 0.000 description 3
- MOMKYJPSVWEWPM-UHFFFAOYSA-N 4-(chloromethyl)-2-(4-methylphenyl)-1,3-thiazole Chemical compound C1=CC(C)=CC=C1C1=NC(CCl)=CS1 MOMKYJPSVWEWPM-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 239000011162 core material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- OBNCKNCVKJNDBV-UHFFFAOYSA-N ethyl butyrate Chemical compound CCCC(=O)OCC OBNCKNCVKJNDBV-UHFFFAOYSA-N 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000009477 glass transition Effects 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 230000033444 hydroxylation Effects 0.000 description 2
- 238000005805 hydroxylation reaction Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229940099402 potassium metaphosphate Drugs 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 235000019983 sodium metaphosphate Nutrition 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000000834 fixative Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- RLQWHDODQVOVKU-UHFFFAOYSA-N tetrapotassium;silicate Chemical compound [K+].[K+].[K+].[K+].[O-][Si]([O-])([O-])[O-] RLQWHDODQVOVKU-UHFFFAOYSA-N 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
- C03C27/06—Joining glass to glass by processes other than fusing
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K21/00—Fireproofing materials
- C09K21/14—Macromolecular materials
-
- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
- Y02A30/24—Structural elements or technologies for improving thermal insulation
- Y02A30/249—Glazing, e.g. vacuum glazing
-
- 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
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B80/00—Architectural or constructional elements improving the thermal performance of buildings
- Y02B80/22—Glazing, e.g. vaccum glazing
Abstract
The invention relates to non-heat-insulating composite fireproof glass and a preparation method of a fireproof layer material thereof. The fireproof layer material comprises the following raw materials in parts by weight: 50-500 parts of hydroxylated gas phase nano silicon dioxide particles, 0.5-5 parts of tetraethoxysilane, 50-200 parts of deionized water, 5-20 parts of anti-condensing agent, 0.2-10 parts of char-forming auxiliary agent, 0.2-10 parts of heat-resistant stabilizer, 0.01-1.5 parts of 2- (trifluoromethyl) acrylic acid, 0.01-1.5 parts of butyl acrylate, 0.01-1.5 parts of methacrylic acid, 0.01-1.5 parts of methyl methacrylate, 0.1-2 parts of ion fixing agent, 0.01-1.5 parts of storage stabilizer, 0.04-0.5 parts of plasticizer and 17-280 parts of potassium hydroxide with purity of 85%. The organic/inorganic hybrid particles with the nano core-shell structure are multimodal and widely distributed nano particles prepared by using a gradient high-pressure homogenization technology. The pre-reaction solution of the fireproof material has the characteristics of small viscosity and low reaction rate at room temperature (20 ℃), and can be used for filling thinner and larger-sized glass cavities.
Description
Technical Field
The invention relates to the field of safety glass, in particular to a hydrophobic-hydrophilic amphoteric fireproof layer material, a preparation method thereof and non-heat-insulation composite fireproof glass.
Background
As the urban development proceeds faster and faster, the building window of the house becomes larger and larger. The glass member with elegant and beautiful appearance and safe function is gradually favored by designers at home and abroad, which directly leads to the rapid development of various safety glass and special glass in the building glass industry. The building glass has been developed from the single lighting material to the composite material with the functions of controlling light, regulating room temperature, reducing noise, improving living environment, etc.
Besides certain properties of common glass, the fireproof glass has the properties of controlling fire spreading, smoke isolation, heat insulation and the like, provides valuable rescue time for effective rescue in case of fire, and reduces losses of personnel, property and buildings to the greatest extent. The fire-proof glass can prevent the escape and rescue personnel from being damaged by heat radiation and reduce the destructive power of fire disaster to the minimum. Because of the recent frequent fires of certain well-known large buildings at home and abroad, people begin to pay attention to the research, development, production and use effects of the composite fireproof glass. The poor cold resistance is one of the main factors restricting the application of the composite fireproof glass, so that the high-performance composite fireproof glass with excellent low temperature resistance and ultraviolet irradiation resistance is developed, the leap of the product performance is realized, the application area of the product is enlarged, and the method is an important direction for the industrialized development of the safety glass.
At present, the work done for the special fireproof layer material of the composite fireproof glass at home is in the basic research stage. The existing composite fireproof glass has poor low-temperature service performance, a large amount of condensing agents are needed to be used, most products can freeze and whiten under the low-temperature condition, and the long-term service requirements of outdoor windows and curtain walls cannot be met in northern cold areas; the main component water glass of the fireproof layer material of the existing composite fireproof glass is limited by the factors of self viscosity, leveling property and the like, so that the fireproof layer material is easy to form thickness difference in the preparation process, and the surface of the fireproof layer is uneven; meanwhile, the fireproof layer of the existing composite fireproof glass is easy to generate bubbles, a large number of microbubbles are easy to exist in an interlayer, the actual fireproof effect of the fireproof layer is reduced due to the existence of the microbubbles, and the apparent quality of the composite fireproof glass is poor; the existing composite fireproof glass also has the problems of insufficient hardness of the fireproof layer and the like, and seriously influences the use effect and the service life of the composite fireproof glass.
Disclosure of Invention
The invention mainly aims to provide non-heat-insulating composite fireproof glass without an anti-reflection layer, a fireproof layer material and a preparation method thereof, which overcome the defect that the fireproof layer material in the prior art uses a large amount of condensing agents to improve low temperature resistance, and avoid the defects of poor adhesive force of the fireproof layer, easy generation of a large amount of microbubbles in a glass interlayer, poor apparent quality and the like.
The aim and the technical problems of the invention are realized by adopting the following technical proposal.
According to the non-heat-insulating composite fireproof glass provided by the invention, the composite fireproof glass is formed by laminating at least two pieces of glass; an interlayer is arranged between two adjacent glass sheets, at least one interlayer is a fireproof layer, the fireproof layer is made of the following materials in parts by weight: 50-500 parts of hydroxylated gas phase nano silicon dioxide particles, 0.5-5 parts of tetraethoxysilane, 50-200 parts of deionized water, 5-20 parts of anti-condensing agent, 0.2-10 parts of char-forming auxiliary agent, 0.2-10 parts of heat-resistant stabilizer, 0.01-1.5 parts of 2- (trifluoromethyl) acrylic acid, 0.01-1.5 parts of butyl acrylate, 0.01-1.5 parts of methacrylic acid, 0.1-2 parts of methyl methacrylate, 0.01-1.5 parts of ion fixing agent, 0.01-1.5 parts of storage stabilizer, 0.04-0.5 parts of plasticizer and 17-280 parts of potassium hydroxide with purity of 95%, wherein the fluorine modified nano core-shell structure organic/inorganic hybrid particles are multimodal and widely distributed nano particles; wherein the hydrophobic-hydrophilic amphoteric nano core-shell structure organic/inorganic hybrid particles are widely distributed nano particles prepared by means of gradient high-pressure homogenization technology, core layer substances are hydroxylated nano silicon dioxide particles and agglomerates thereof, shell substances are poly (2- (trifluoromethyl) acrylic acid, butyl acrylate, methacrylic acid and methyl methacrylate) hydrophobic-hydrophilic amphoteric copolymers, and the modulus of the fireproof material is between 4.2 and 5.5.
The aim and the technical problems of the invention can be further realized by adopting the following technical measures.
Preferably, the fireproof layer material comprises the following raw materials in parts by weight: 100-250 parts of hydroxylated nano core-shell structure organic/inorganic hybrid particles, 0.5-2 parts of tetraethoxysilane, 70-100 parts of deionized water, 10-15 parts of anti-condensing agent, 1-3 parts of carbonizing auxiliary agent, 1-3 parts of heat stabilizer, 0.01-1.5 parts of 2- (trifluoromethyl) acrylic acid, 0.01-1.5 parts of butyl acrylate, 0.01-1.5 parts of methacrylic acid, 0.01-1.5 parts of methyl methacrylate, 0.1-0.5 parts of ion fixing agent, 0.4-0.6 parts of storage stabilizer, 0.1-0.3 parts of plasticizer and 34-140 parts of potassium hydroxide with the purity of 85%.
Preferably, the flame-retardant layer material, wherein the particle size of the organic/inorganic hybrid particles with the hydroxylated nano core-shell structure is 200nm-550nm, the particle size of the core layer is 150nm-500nm, and the specific surface area is 25-35 m 2 Per gram, the density of silicon hydroxyl groups is 2-4 per nm 2 The particle size distribution is a multimodal broad distribution; the thickness of the shell layer is 20nm-30nm.
Preferably, the foregoing fire-resistant layer material, wherein the anti-condensing agent is at least one of ethylene glycol, propylene glycol, glycerol, and pentaerythritol; the char forming agent is at least one of sucrose, fructose, glucose, granulated sugar and maltose; the carbon forming auxiliary agent is at least one of potassium dihydrogen phosphate, potassium hydrogen phosphate, sodium dihydrogen phosphate and sodium hydrogen phosphate; the heat-resistant stabilizer is at least one of borax and boric acid; the ion fixing agent is at least one of zinc oxide, aluminum oxide and starch; the storage stabilizer is at least one of sodium polyphosphate and potassium polyphosphate; the plasticizer is at least one of dipropylene glycol butyl ether and dipropylene glycol methyl ether.
The aim of the invention and the technical problems are also achieved by adopting the following technical proposal.
The preparation method of the hydrophobic-hydrophilic amphoteric fireproof layer material provided by the invention comprises the following steps:
condensing-resistant agent, ethyl n-butyrate, char forming agent, char forming auxiliary agent, heat-resistant stabilizer, potassium hydroxide and deionized water according to the ratio of 5-20:0.5-5:0.2-10:0.2-10:0.01-0.2: 50-200 weight portions of the raw materials are mixed, and the mixture is kept still and aged for 24 hours, and after the ethyl orthosilicate is alcoholized, a silicon dioxide seed solution is generated, and the particle size of silicon dioxide particles is 20-40 nm, so that a first mixed solution is prepared;
gradually dispersing by means of gradient high-pressure homogenization, sequentially adding 50-500 parts by weight of hydroxylated gas-phase nano silicon dioxide particles into a first mixed solution according to 30%, 25%, 20%, 15% and 10% by weight respectively, and homogenizing under 20-180 MPa, wherein each high-pressure homogenization time is 12min, 10min, 8min, 6min and 4min in sequence to obtain a nuclear layer solution;
mixing 2- (trifluoromethyl) acrylic acid, butyl acrylate, methacrylic acid and methyl methacrylate according to the weight parts of 0.01-1.5:0.01-1.5 to prepare a second mixed solution;
Dropwise adding 0.04-5 parts by weight of a second mixed solution and 0.001-0.05 parts by weight of redox initiator into 100-900 parts by weight of core layer solution at a constant speed under the temperature condition of 60-65 ℃ by means of starvation polymerization, and coating a layer of organic/inorganic composite material on the surfaces of nano silicon dioxide particles after polymerization to obtain onion-type hydrophobic-hydrophilic amphoteric nano core-shell structure organic/inorganic hybrid silicon dioxide particle emulsion;
under the condition of high stirring, 0.1-2 parts by weight of ion fixing agent, 0.01-1.5 parts by weight of storage stabilizer and 0.04-0.5 part by weight of plasticizer are sequentially added into 100-900 parts by weight of hydrophobic-hydrophilic amphoteric nano core-shell structure organic/inorganic hybrid silicon dioxide particle emulsion, and stirring is carried out for 30min, and uniform mixing is carried out, thus obtaining a base solution of the fireproof layer material;
and adding 17-280 parts by weight of potassium hydroxide with the purity of 85% into 100-900 parts by weight of the base solution of the fireproof layer material, vacuumizing, and uniformly stirring to obtain the fireproof layer material.
The aim and the technical problems of the invention can be further realized by adopting the following technical measures.
Preferably, the non-heat-insulating composite fireproof glass, wherein the thickness of the fireproof layer is 0.4-1mm.
By means of the technical scheme, the preparation method of the non-heat-insulation composite fireproof glass and the fireproof layer material thereof provided by the invention has at least the following advantages:
1. by means of the gradient high-pressure homogenization method, the grading effect of the nano silicon dioxide particles is further optimized, and the viscosity of the system is greatly reduced: compared with the silicon dioxide solution prepared by other technologies, the high-pressure homogenized organic/inorganic hybrid silicon dioxide solution with the hydrophobic-hydrophilic amphoteric nano core-shell structure has lower viscosity on the premise of the same solid content, and meanwhile, the wide-distribution organic/inorganic hybrid silicon dioxide particles with the hydrophobic-hydrophilic amphoteric nano core-shell structure ensures that the pre-reaction solution of the fireproof layer material has the shear thinning characteristic and can be poured into a thinner glass cavity.
2. According to the invention, nano silicon dioxide particles are adopted as a main raw material, the hydrophobic-hydrophilic nano core-shell structure organic/inorganic hybrid silicon dioxide particles are widely distributed nano particles, the core layer material is gas phase nano silicon dioxide particles and aggregates thereof, the shell layer material is a copolymer of poly (2- (trifluoromethyl) acrylic acid-butyl acrylate-methacrylic acid-methyl methacrylate), and after the raw material-containing fireproof layer material contacts with glass, a diffusion layer with a certain thickness is formed on the surface of the glass by corroding, so that the adhesive force between a fireproof adhesive layer and the glass is improved; when the glass is heated to generate cracks, the cracks can not be expanded, so that the whole glass can not be cracked, and the strength of the fireproof glass is greatly improved.
3. By adding other auxiliary agents into the organic/inorganic hybrid particles with the nano core-shell structure, the synergistic effect is generated among the components of the fireproof layer material, and the bubbles of the composite fireproof glass interlayer are eliminated, so that the high-performance microbubble-free, low-temperature and non-heat-insulation composite fireproof glass which has good adhesive force, high hardness of 6H, 75-88% transmittance and fire resistance time of about 310min and can be used in a low-temperature environment (-40 ℃) is prepared.
4. The reason that the fireproof layer material has low temperature resistance is as follows: the particle size distribution of the hydrophobic-hydrophilic amphoteric nano-core-shell structure organic-inorganic hybrid silicon dioxide particles is wider, so that the solid content of the silicon dioxide is improved (can exceed 55 percent), and correspondingly, the free water in the fireproof layer material is reduced; the organic material of the outer layer of the hydrophobic-hydrophilic amphoteric nano core-shell structure organic-inorganic hybrid particle contains hydrophobic groups, so that the adsorption of free water is reduced, the viscosity of a reaction system is further reduced, and the composite fireproof glass with thinner thickness can be poured; the hydrophilic groups such as silicon hydroxyl are utilized to continuously lock free water in the fireproof layer material, so that the low temperature resistance of the fireproof layer material is improved.
The foregoing description is only an overview of the present invention, and is intended to provide a better understanding of the present invention, as it is embodied in the following description, with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is a schematic structural view of a non-insulating composite fire-resistant glass according to an embodiment of the present invention;
FIG. 2 is a schematic structural view of a non-insulating composite fire-resistant glass according to another embodiment of the present invention;
FIG. 3 is a graph of viscosity versus shear rate for a dispersion of hydrophobic-hydrophilic amphiphilic nano-core shell structured organic/inorganic hybrid silica particles of the present invention;
FIG. 4 is a graph showing the particle size distribution of a dispersion of hydrophobic-hydrophilic amphiphilic nano-core-shell structured organic/inorganic hybrid silica particles of the present invention.
Detailed Description
The non-heat-insulating composite fireproof glass is formed by laminating at least two pieces of glass, an interlayer is arranged between two adjacent pieces of glass, and at least one interlayer is a fireproof layer made of fireproof layer materials. Wherein, the fireproof layer material comprises the following raw materials in parts by weight:
50-500 parts of hydroxylated gas phase nano silicon dioxide particles, 50-200 parts of deionized water, 5-20 parts of anti-condensing agent, 0.5-5 parts of tetraethoxysilane, 0.2-10 parts of char forming agent, 0.2-10 parts of char forming auxiliary agent, 0.2-10 parts of heat resistant stabilizer, 0.01-1.5 parts of 2- (trifluoromethyl) acrylic acid, 0.01-1.5 parts of butyl acrylate, 0.01-1.5 parts of methacrylic acid, 0.1-2 parts of methyl methacrylate, 0.01-1.5 parts of ion fixing agent, 0.01-1.5 parts of storage stabilizer, 0.04-0.5 parts of plasticizer and 17-280 parts of potassium hydroxide with 85% purity, wherein the fluorine modified nano core-shell structure organic/inorganic hybrid particles are multimodal and widely distributed nano particles; the organic/inorganic hybrid particles with the hydrophobic-hydrophilic amphoteric nano core-shell structure are wide-distribution nano particles prepared by means of gradient high-pressure homogenization technology, the core layer material is nano silicon dioxide particles and aggregates thereof, the shell layer material is poly (trifluoroethyl methacrylate-butyl acrylate-methyl methacrylate) hydrophobic-hydrophilic amphoteric copolymer, and the modulus of the fireproof material is between 4.2 and 5.5.
As a preferred embodiment, the fireproof layer material comprises the following raw materials in parts by weight: 100-250 parts of nano core-shell structure organic/inorganic hybrid particles, 0.5-2 parts of tetraethoxysilane, 70-100 parts of deionized water, 10-15 parts of anti-condensing agent, 1-3 parts of char-forming auxiliary agent, 1-3 parts of heat-resistant stabilizer, 0.1-0.5 part of ion fixing agent, 0.4-0.6 part of storage stabilizer, 0.1-0.3 part of plasticizer and 34-140 parts of potassium hydroxide with the purity of 85%.
As a preferred embodiment, the particle size of the organic/inorganic hybrid particles with the nano core-shell structure is 200nm-550nm, the particle size of the core layer is 150nm-500nm, and the specific surface area is 25-35 m 2 Per gram, the density of silicon hydroxyl groups is 2-4 per nm 2 The particle size distribution is a multimodal broad distribution; the thickness of the shell layer is 20nm-30nm.
The invention uses hydrophobic-hydrophilic amphoteric nano-core-shell structure organic/inorganic hybrid particles as the main raw material of the fireproof layer material, wherein the hydrophobic-hydrophilic amphoteric nano-core-shell structure organic/inorganic hybrid silicon dioxide particles are widely distributed nano-particles, the particle size is 150nm-800nm, and the particle size distribution is wider; the core layer material is hydroxylation gas phase nanometer silicon dioxide particles and agglomeration body thereof, the particle diameter is 110nm-720nm, the specific surface area is 20-40 m 2 Per gram, the density of silicon hydroxyl groups is 2-4 per nm 2 The particle size distribution is a multimodal broad distribution; the shell material is poly (2- (trifluoromethyl) acrylic acid-butyl acrylate-methacrylic acid-methyl methacrylate) copolymer, and the thickness of the shell is 20nm-40nm. The hydrophobic-hydrophilic amphoteric nano-core-shell structure organic/inorganic hybrid silica particles are widely distributed nano-particles. The invention has the characteristics of small viscosity, low reaction rate at room temperature (20 ℃), thinner filling and larger sizeIs provided. Meanwhile, the organic-inorganic hybrid particles with wide-distribution hydrophobic-hydrophilic amphoteric nano core-shell structures have low temperature resistance.
The reason for the low temperature resistance of the wide-distribution hydrophobic-hydrophilic amphoteric nano-core-shell structure organic-inorganic hybrid silica particles is as follows:
1. the organic-inorganic hybrid silicon dioxide particles with the hydrophobic-hydrophilic amphoteric nano-core-shell structure have higher system solid content (which can exceed 55 percent), and correspondingly, the free water in the fireproof layer material is reduced;
2. the organic material of the outer layer of the hydrophobic-hydrophilic amphoteric nano core-shell structure organic-inorganic hybrid particle contains hydrophobic groups, so that the adsorption of free water is reduced;
3. utilizing hydrophilic groups such as silicon hydroxyl groups and carboxyl groups to continuously lock free water in the fireproof layer material;
The hydrophobic-hydrophilic amphoteric nano-core-shell structured organic/inorganic hybrid particles exist in the form of dispersion liquid, and the mass concentration of the dispersion liquid is 50% -60%.
As a preferred embodiment, the anti-condensing agent is at least one of ethylene glycol, propylene glycol, glycerol and pentaerythritol.
As a preferred embodiment, the char-forming agent is at least one of sucrose, fructose, glucose, granulated sugar and maltose; the carbon forming auxiliary agent is at least one of potassium dihydrogen phosphate, potassium hydrogen phosphate, sodium dihydrogen phosphate and sodium hydrogen phosphate.
As a preferred embodiment, the heat stabilizer is at least one of borax and boric acid; the ion fixing agent is at least one of zinc oxide, aluminum oxide and starch; the storage stabilizer is at least one of sodium polyphosphate and potassium polyphosphate; the plasticizer is at least one of dipropylene glycol butyl ether and dipropylene glycol methyl ether.
The fireproof layer material of the invention adopts the following raw materials:
hydrophobic-hydrophilic amphiphilic nano core-shell structured organic-inorganic hybrid particles: the hydrophobic-hydrophilic amphoteric nano-core-shell structure organic/inorganic hybrid particles are mixed with deionized water to form a hydrophobic-hydrophilic amphoteric nano-core-shell structure organic/inorganic hybrid silicon dioxide particle solution, and after a fireproof layer material containing the solution contacts with glass, the surface of the glass can be corroded to form a diffusion layer with a certain thickness, so that the adhesive force between a fireproof adhesive layer and the glass is improved; when the glass is heated to generate cracks, the cracks can not be expanded, so that the whole glass can not be cracked, and the strength of the non-heat-insulation composite fireproof glass is greatly improved; meanwhile, the pre-reaction solution of the fireproof layer material has the characteristic of shear thinning.
The hydrophobic-hydrophilic amphoteric nano core-shell structure organic-inorganic hybrid particles adopted by the embodiment of the invention are of a core-shell structure, namely two or more monomers are polymerized in stages or sections under certain conditions, so that the inner side or the outer side of the particles are respectively enriched with different components, namely core-shell particles, thereby endowing the cores with different functions with the shells, and obtaining the particles with excellent performance; wherein the core layer material is hydroxylated gas phase nano silicon dioxide particles, and the shell layer material is poly (2- (trifluoromethyl) acrylic acid-butyl acrylate-methacrylic acid-methyl methacrylate) copolymer. At normal temperature or low temperature, the shell material of the hydrophobic-hydrophilic amphoteric nano core-shell structure organic-inorganic hybrid particles in the fireproof liquid wraps the core material silicon dioxide particles, and separates the silicon dioxide particles from the potassium hydroxide solution in the fireproof material, so that no reaction occurs; when the temperature is higher, namely, the glass transition temperature of the shell polymer is higher, the hydrophobic-hydrophilic amphoteric shell polymer is changed from a glassy state to a rubbery state, the potassium hydroxide solution permeates into the shell layer and reacts with the silicon dioxide particles to obtain potassium silicate solution, namely, potash water glass (the structural formula is K 2 O·nSiO 2 N is modulus), the hardness of the silicon dioxide net skeleton formed after the potassium water glass is hardened has little reduction at high temperature, has good flame retardance, can resist high temperature and fire, has higher hardness, and enhances the hardness and heat resistance of the non-heat-insulation composite fireproof glass.
The hydrophobic-hydrophilic amphoteric nano-core-shell structure organic-inorganic hybrid particles are widely distributed nano-particles, and the particle size of the particles is 150nm-800nm. The research finds that: by means of the particle design principle, the prepared Si-based composite material has a near-spherical core-shell structure, high solid content and low viscosityO 2 The dispersion likewise has shear thinning properties, and the addition of further auxiliaries, by preference, does not affect the shear-thinning properties of the system, so that the resulting pre-reaction solution for the flame-retardant coating material also has shear-thinning properties.
Because the hydrophobic-hydrophilic amphoteric nano core-shell structure organic-inorganic hybrid particles are widely distributed nano particles, the composite fireproof glass has the characteristics of small viscosity and low room temperature (20 ℃) reaction rate, and can be filled with thinner and larger-sized glass cavities, so that the prepared non-heat-insulation composite fireproof glass is thinner and larger. The result and the action mechanism are different from those of SiO with a non-core-shell structure 2 As shown in FIG. 3, the dispersion is nano SiO of the organic/inorganic hybrid particles with nano core-shell structure 2 The viscosity of the microparticle dispersion is plotted against the shear rate. SiO of non-core-shell structure 2 In the dispersion, siO is contained in the core-shell dispersion 2 The solids content of (2) far exceeds the former, but two key factors affecting the initial viscosity of the system: the silicon hydroxyl group content of the particle surface and the cavity area inside the particle have far different influence degrees. For SiO with near spherical core-shell structure 2 For the dispersion liquid, the silicon hydroxyl groups on the surface and the hollow holes in the surface are completely or partially wrapped by the shell polymer, so that the influence of the two factors on the viscosity of the system is greatly reduced, and the initial viscosity of the system is reduced. With increasing shear rate, those of about 500nm to 800nm are composed of several hundred SiO 2 The particles are clustered together, have small-size particles of core-shell structure, are equivalent to sliding beads in gears, are filled with about 5-6 microns and are composed of thousands of SiO 2 The particles are clustered together and also have large-size particles with a core-shell structure, so that the lubricating effect is achieved, and the higher the shearing rate is, the lower the viscosity is. The following equation can be satisfied by fitting the relationship between the system viscosity μ and the rotational speed V to fig. 3:
μ＝238.21+229.05e (-V/14.43)
the hydrophobic-hydrophilic amphoteric nano-core-shell structured organic-inorganic hybrid particles are hydrophobic-hydrophilic amphoteric, which means that shell materials are positioned on the surfaces of core-shell particles due to the hydrophobic-hydrophilic amphoteric properties, which are obtained by the preparation methodThe hydrophobic groups can exist in an ionic form at a certain pH value or can depend on the steric hindrance effect between the hydrophobic groups to ensure that the core-shell particles reach a stable state, and the embodiment of the invention adopts the poly (2- (trifluoromethyl) acrylic acid-butyl acrylate-methacrylic acid-methyl methacrylate) copolymer as a shell material, so that the effect can be achieved, because the methacrylic acid is a water-soluble monomer and contains hydrophilic groups-COOH and hydrophobic groups-CH at the same time 3 Therefore, part of the monomers can approximately play a role in isolating an emulsifier and can play a role in polymerizing the monomers, and the glass transition temperatures of polymethyl methacrylate, polymethyl acrylic acid and poly (2- (trifluoromethyl) acrylic acid) are high (more than 100 ℃), and the copolymer is in a glass state at normal temperature according to a Fox formula, has certain rigidity, avoids sticky adsorption among particles, is favorable for protecting silicon dioxide particles, prevents the silicon dioxide particles from agglomerating, can be uniformly dispersed in the fireproof glue, and can fully react with potassium hydroxide solution.
It is important to say that in the fireproof layer material, the nano core-shell structure organic-inorganic hybrid particles have low temperature resistance, and the condensing agent resistance only enhances the performance.
The reason why the fireproof layer material has low temperature resistance is that:
1. the organic-inorganic hybrid silicon dioxide particles with the hydrophobic-hydrophilic amphoteric nano-core-shell structure have higher system solid content (which can exceed 55 percent), and correspondingly, the free water in the fireproof layer material is reduced;
2. the organic material of the outer layer of the hydrophobic-hydrophilic amphoteric nano core-shell structure organic-inorganic hybrid particle contains hydrophobic groups, so that the adsorption of free water is reduced;
3. And the hydrophilic groups such as silicon hydroxyl are utilized to continuously lock the free water in the fireproof layer material.
Anti-condensing agent: the low-molecular polyol is selected as an anti-condensing agent, has the function of a surfactant to a certain extent, and has a certain defoaming and antifreezing effect.
Char-forming agent and char-forming auxiliary agent: at high temperature, the fireproof glue layer foams to generate pores, the char forming agent and the char forming auxiliary agent carbonize to form long-chain carbide, and the long-chain carbide is deposited in the pores and can absorb a large amount of heat, so that the fireproof performance of the glass is enhanced. The char-forming agent adopted in the embodiment of the invention is at least one selected from sucrose, fructose, glucose and maltose, and all the char-forming agents can form long-chain carbide at high temperature; the charring auxiliary agent can help the charring agent to charre rapidly at high temperature; the char-forming auxiliary agent of the embodiment of the invention is at least one selected from potassium dihydrogen phosphate, potassium hydrogen phosphate, sodium dihydrogen phosphate and sodium hydrogen phosphate; when a fire disaster occurs, the temperature of the environment rises to 400-700 ℃, at this time, the carbon forming auxiliary agent can generate intramolecular dehydration condensation reaction to generate sodium metaphosphate or potassium metaphosphate, the polymerization degree is closely related to the temperature and time of the fire disaster environment, the higher the temperature and the longer the time are, the higher the polymerization degree is, the carbonized product generated by the carbonization reaction of the carbon forming agent under the high temperature condition can be attached to long-chain sodium metaphosphate or potassium metaphosphate, and the long-chain carbonized product can absorb a large amount of heat, so that the fire resistance of glass is enhanced. In addition, the shell material poly (2- (trifluoromethyl) acrylic acid-butyl acrylate-methacrylic acid-methyl methacrylate) copolymer of the organic-inorganic hybrid particles with the nano core-shell structure adopted in the embodiment of the invention also has the function of a char former, can be carbonized at high temperature to form long-chain carbonized substances, absorbs a large amount of heat, and enhances the fireproof performance of glass.
Heat resistant stabilizer: the heat-resistant stabilizer adopted by the embodiment of the invention is at least one selected from borax and boric acid, can improve the heat resistance and the transparency of the fireproof adhesive layer, and controls the thermal expansion rate of the fireproof layer material, thereby improving the chemical stability of the low-temperature non-heat-insulation composite fireproof glass and the mechanical shock resistance and the thermal shock resistance.
Ion fixative: the ion fixing agent adopted in the embodiment of the invention is at least one selected from zinc oxide, aluminum oxide and starch; the silicon dioxide reacts with potassium hydroxide solution to form potash water glass (the structural formula is K 2 O·nSiO 2 N is modulus), i.e., aqueous solutions of potassium silicate, sodium oxide or sodium silicate in the flame retardant layer material can be modified by the addition of the ionic fixing agents described aboveThe activity of potassium oxide can improve the water resistance of the fireproof layer material by adding a proper amount of amphoteric metal compound.
Storage stabilizer: because silicon dioxide reacts with potassium hydroxide solution, aqueous solution of potassium silicate is formed, silicate has strong polymerization capability in alkaline aqueous solution with pH value of 7-9, silicate gel is easy to generate, the stability of the system is destroyed, and the storage stability is reduced. By adding a storage stabilizer, silicate can be dispersed or form stable suspension to prevent adhesion and agglomeration of the suspension; the storage stabilizer adopted in the embodiment of the invention is at least one selected from sodium polyphosphate and potassium polyphosphate, and the polyphosphate is a polymeric dielectric medium and has the characteristic of inorganic surfactant, so that insoluble substances in the solution can be dispersed or form stable suspension, and the adhesion and aggregation of the suspension are prevented.
And (3) a plasticizer: the plasticizer adopted in the embodiment of the invention is at least one selected from dipropylene glycol butyl ether and dipropylene glycol methyl ether, and the plasticizer can soften the formed fireproof layer material, reduce the internal stress of the fireproof layer material, enable the fireproof layer material to be uniformly attached to glass, improve the apparent mass and the fireproof strength of low-temperature non-heat-insulation composite fireproof glass, and meanwhile, trace up the ether material to have the defoaming capability, so as to avoid the influence of micro-bubbles on the apparent mass of the non-heat-insulation composite fireproof glass.
Crosslinking agent: the 4 silicon hydroxyl groups formed after hydrolysis of the tetraethoxysilane adopted by the embodiment of the invention can form a reticular cross-linked structure of Si-O-Si with the fireproof layer material, promote the reaction and hardening of the organic/inorganic hybrid particles with the nano core-shell structure, and improve the mechanical strength and weather resistance of the fireproof adhesive layer of the non-heat-insulation composite fireproof glass.
The invention also provides a preparation method of the fireproof layer material, which comprises the following steps:
(1) Condensing-resistant agent, tetraethoxysilane, char forming agent, char forming auxiliary agent, heat-resistant stabilizer, potassium hydroxide and deionized water according to the ratio of 5-20:0.5-5:0.2-10:0.2-10:0.01-0.2: 50-200 weight portions of the raw materials are mixed, and the mixture is kept still and aged for 24 hours, and after the ethyl orthosilicate is alcoholized, a silicon dioxide seed solution is generated, and the particle size of silicon dioxide particles is 20-40 nm, so that a first mixed solution is prepared;
(2) Gradually dispersing by means of a gradient high-pressure homogenizing technology, sequentially adding 50-500 parts by weight of hydroxylated gas-phase nano silicon dioxide particles into a first mixed solution according to 30%, 25%, 20%, 15% and 10% by weight respectively, and homogenizing under 20-180 MPa for 12min, 10min, 8min, 6min and 4min each time to obtain a nuclear layer solution;
(3) Mixing 2- (trifluoromethyl) acrylic acid, butyl acrylate, methacrylic acid and methyl methacrylate according to the weight parts of 0.01-1.5:0.01-1.5 to prepare a second mixed solution;
(4) Dropwise adding 0.04-5 parts by weight of a second mixed solution and 0.001-0.05 parts by weight of redox initiator into 100-900 parts by weight of core layer solution at a constant speed under the temperature condition of 60-65 ℃ by means of starvation polymerization, and coating a layer of organic/inorganic composite material on the surfaces of nano silicon dioxide particles after polymerization to obtain onion-type hydrophobic-hydrophilic amphoteric nano core-shell structure organic/inorganic hybrid silicon dioxide particle emulsion;
(5) Under the condition of high stirring, 0.1-2 parts by weight of ion fixing agent, 0.01-1.5 parts by weight of storage stabilizer and 0.04-0.5 part by weight of plasticizer are sequentially added into 100-900 parts by weight of hydrophobic-hydrophilic amphoteric nano core-shell structure organic/inorganic hybrid silicon dioxide particle emulsion, and stirring is carried out for 30min, and uniform mixing is carried out, thus obtaining a base solution of the fireproof layer material;
(6) And adding 17-280 parts by weight of potassium hydroxide with the purity of 85% into 100-900 parts by weight of the base solution of the fireproof layer material, vacuumizing, and uniformly stirring to obtain the fireproof layer material.
Further, in the step (1), the particle size of the hydrophobic-hydrophilic amphoteric nano-core-shell structure organic/inorganic hybrid particles is 150nm-800nm, and the particle size distribution is wider; the core layer material is hydroxylation gas phase nanometer silicon dioxide particles and agglomerates thereof, the particle size is 110nm-720nm, and the particle size distribution is multimodal wide distribution; the shell material is poly (2- (trifluoromethyl) acrylic acid-butyl acrylate-methacrylic acid-methyl methacrylate) copolymer, and the thickness of the shell is 20nm-40nm. Further, in the step (5), the stirring time is 30 to 60 minutes, preferably 30 minutes.
When the non-heat-insulating composite fireproof glass fireproof adhesive is prepared, firstly, an anti-condensing agent, tetraethoxysilane, a char forming agent, a char forming auxiliary agent, a heat stabilizer and potassium hydroxide are added into deionized water, and uniformly stirred to obtain a first solution; gradually dispersing by means of gradient high-pressure homogenization technology, and adding hydroxylated gas-phase nano silicon dioxide particles into the first mixed solution to obtain a nuclear layer solution; mixing 2- (trifluoromethyl) acrylic acid, butyl acrylate, methacrylic acid and methyl methacrylate to prepare a second mixed solution; dropwise adding a second mixed solution and a redox initiator into the core layer solution by means of a starvation polymerization method to obtain onion-type, hydrophobic-hydrophilic amphoteric nano-core-shell structure organic/inorganic hybrid silicon dioxide particle emulsion; under the condition of high stirring, sequentially adding an ion fixing agent, a storage stabilizer and a plasticizer, stirring uniformly while adding, and finally stirring until the solution is completely reacted, wherein the sequentially adding and stirring uniformly is used for ensuring better dissolution of each component, avoiding the generation of bubbles in the system again due to the difference of stirring speeds, and stirring until the solution is completely reacted is used for ensuring that the crosslinking degree reaches the design requirement; finally, adding potassium hydroxide with the purity of 85% into the second solution, and slowly stirring under the condition of vacuumizing, wherein the aim is to remove microbubbles in the system by utilizing negative pressure, thereby obtaining the non-microbubble fireproof adhesive.
Because the base solution of the fireproof layer material and the potassium hydroxide are mixed to react, before the fireproof layer material is used, the base solution of the fireproof layer material and the potassium hydroxide are required to be stored respectively, and the base solution of the fireproof layer material can be stored for a long time for standby, and the quality guarantee period of the base solution of the fireproof layer material, which is stored in a sealed and light-proof way, is not less than 180 days; and (5) conventionally preserving potassium hydroxide. When in use, the base solution of the fireproof layer material is mixed with potassium hydroxide on site, so that the performance of the fireproof layer material can be better ensured.
When the non-heat-insulating composite fireproof glass provided by the embodiment of the invention encounters a fire, the fireproof layer in the non-heat-insulating composite fireproof glass rapidly foams and expands to form a heat-insulating fireproof heat-insulating foam layer, so that a large amount of heat generated by the fire is absorbed, and the non-heat-insulating composite fireproof glass has good fireproof performance; the fireproof layer in the non-heat-insulation type composite fireproof glass is formed by adopting the prepared fireproof layer material, so that the non-heat-insulation type composite fireproof glass has the advantages of no microbubbles, high transmittance and long fireproof time. Preferably, at least two interlayers are provided, one interlayer is a vacuum layer, and the rest interlayers are fireproof layers.
More preferably, the interlayer between two adjacent sheets of glass is a fire resistant layer.
As a preferred embodiment, as shown in fig. 1, a non-thermal insulation type composite fire-proof glass sequentially includes a first glass layer 11, a first fire-proof layer 21, a second glass layer 12, a second fire-proof layer 22 and a third glass layer 13, wherein the first fire-proof layer 21 and the second fire-proof layer 22 are made of the fire-proof layer materials described above.
The glass of the invention is glass without an anti-reflection layer, because the fireproof layer material contains the plasticizer, the possibility of chemical reaction between the plasticizer and the anti-reflection layer material cannot be avoided, and because the glass is mainly an ether substance, titanium dioxide in the anti-reflection layer has a photocatalysis effect, and the ether substance and the silicon dioxide in the anti-reflection layer can undergo a polycondensation reaction to form corrosion spots, so that the glass cannot be wiped.
As a preferred embodiment, as shown in fig. 2, a non-heat-insulating composite fire-proof glass includes, in order, a first glass layer 11, a first fire-proof layer 21, a second glass layer 12, a second fire-proof layer 22, and a third glass layer 13, wherein the first fire-proof layer 21 and the second fire-proof layer 22 are made of the fire-proof layer materials described above.
As another preferred embodiment, as shown in fig. 3, a non-heat-insulating composite fire-proof glass includes a first glass layer 11, a first fire-proof layer 21, a second glass layer 12, a second fire-proof layer 22, a third glass layer 13, a vacuum layer 31, a fourth glass layer 14, a third fire-proof layer 23 and a fifth glass layer 15 in this order, wherein the first fire-proof layer 21, the second fire-proof layer 22 and the third fire-proof layer 23 are made of the fire-proof layer materials described above, and the vacuum layer is formed by sealing two glass sheets around, evacuating the gap therebetween and sealing the exhaust holes.
As a preferred embodiment, the thickness of the fire-resistant layer is 0.4-1mm.
The thickness of the fireproof layer can be controlled to be 0.4-1mm, and on the premise of ensuring the fireproof performance of the non-heat-insulation composite fireproof glass, the thickness of the manufactured non-heat-insulation composite fireproof glass is thinner, the production cost of the glass is reduced, and the application range of the glass is enlarged. The fireproof layer in the non-heat-insulating composite fireproof glass expands to form a porous heat-insulating layer after encountering fire, the thickness of the expansion layer is about 10-15 times that of the original fireproof layer, the glass facing the fire can be first burst after encountering fire, and then the fireproof adhesive layer attached to the glass can gradually form the heat-insulating layer with the thickness of about 10-30 mm; if the thickness of the fireproof adhesive layer is less than 0.4mm, the fireproof adhesive layer is too thin, and the formed heat insulation layer cannot isolate heat transfer within a certain time, so that the integrity of the glass is lower than a design value; if the thickness of the fireproof adhesive layer is greater than 1mm, the fireproof adhesive layer is too thick, the overall weight of the non-heat-insulation composite fireproof glass is increased, the cost is overlarge, meanwhile, the fireproof adhesive layer is expanded layer by layer, and the excessively thick expansion layer can lead to the overall falling of the glass, so that the fireproof performance is reduced.
The invention will be further illustrated, but is not limited, by the following examples.
The reagents used in the various examples of the present invention are all commercially available products.
Example 1
The fireproof layer material in this embodiment is prepared by the following steps:
(1) Weighing the raw materials of the fireproof layer material according to the following weight:
400kg of nano-silica particles with a particle size of 180nm, 200kg of deionized water, 12.5kg of ethylene glycol/glycerol (1:1), 1kg of ethyl orthosilicate, 0.5kg of sucrose/fructose (4:1), 0.5kg of potassium dihydrogen phosphate, 0.2kg of borax, 0.2kg of boric acid, 0.5kg of 2- (trifluoromethyl) acrylic acid, 1kg of butyl acrylate, 0.15kg of methacrylic acid, 0.3kg of methyl methacrylate, 0.2kg of alumina, 0.3kg of polyphosphate 4, 0.2kg of plasticizer and 168.8kg of potassium hydroxide with a purity of 85%; since the particle size of the hydrophobic-hydrophilic amphoteric nano-core-shell structure organic/inorganic hybrid particles isThe core-layer particles with wide distribution and various particle size can exist in the invention, as shown in figure 4, which is SiO of the hydrophobic-hydrophilic amphoteric nano-core-shell structure organic/inorganic hybrid particle 2 The particle size distribution of the dispersion liquid was multimodal, and similarly, the particle size of the core layer fine particles in the following examples was also widely distributed;
(2) The fireproof layer material is prepared from the raw materials according to the following steps:
Mixing 12.5kg of glycol/glycerin (1:1), 1kg of ethyl orthosilicate, 0.5kg of sucrose/fructose (4:1), 0.5kg of monopotassium phosphate, 0.2kg of borax, 0.2kg of boric acid, 1kg of potassium hydroxide with the purity of 85% and 200kg of deionized water, standing and aging for 24 hours, and obtaining a silicon dioxide seed solution after the ethyl orthosilicate is alcoholized, wherein the particle size of silicon dioxide particles is 20-40 nm, so as to obtain a first mixed solution;
gradually dispersing by gradient high pressure homogenizing technique, and dispersing 400kg with particle diameter of 180nm and specific surface area of 30m 2 Per gram, the density of silicon hydroxyl groups is 2/nm 2 Respectively adding 30%, 25%, 20%, 15% and 10% of the total weight of the components into the first mixed solution in sequence, wherein the homogenizing pressure is 50MPa, 80MPa, 110MPa, 140MPa and 170MPa each time, and the homogenizing time is 12min, 10min, 8min, 6min and 4min each time to obtain a nuclear layer solution;
mixing 0.5kg of 2- (trifluoromethyl) acrylic acid, 1kg of butyl acrylate, 0.15kg of methacrylic acid and 0.3kg of methyl methacrylate to prepare a second mixed solution;
dropwise adding a second mixed solution and 0.05kg of redox initiator into the core layer solution at a constant speed under the temperature condition of 60-65 ℃ by means of a starvation polymerization method, and coating an organic/inorganic composite material on the surfaces of the nano silicon dioxide particles after polymerization to obtain onion-type hydrophobic-hydrophilic amphoteric nano core-shell structure organic/inorganic hybrid silicon dioxide particle emulsion;
Adding 0.2kg of aluminum oxide into the onion-shaped, hydrophobic-hydrophilic amphoteric nano-core-shell structure organic/inorganic hybrid silicon dioxide particle emulsion, and continuously stirring;
after stirring evenly, adding 0.3kg of polyphosphate, and continuing stirring;
after stirring evenly, 0.2kg dipropylene glycol butyl ether (DPNB) is added, and stirring is continued;
after stirring uniformly, adding 168.8kg of potassium hydroxide with the purity of 85%, vacuumizing, slowly stirring for 30 minutes to obtain a solution which is the fireproof layer material, and sealing and preserving the solution for later use.
The non-heat-insulating composite fireproof glass in the embodiment is prepared from the fireproof layer material through the following steps:
(1) Preparing 4 pieces of glass with the thickness of 3mm, wherein two pieces of glass are physically toughened glass; in order to ensure that the prepared non-heat-insulating composite fireproof glass has higher strength, the glass positioned in the middle is preferably slightly thicker than other layers of glass;
(2) The 1 piece of physical toughened glass is used as the outermost layer glass to be synthesized with 1 piece of non-physical toughened glass into a cavity with the thickness of 0.5mm by utilizing a thickness-fixing adhesive tape, the rest 2 pieces of non-physical toughened glass are sequentially overlapped by utilizing the thickness-fixing adhesive tape, the cavity with the thickness of 0.5mm is reserved among each piece of glass, and finally the other piece of physical toughened glass is laminated with the multi-layer cavity glass by utilizing the thickness-fixing adhesive tape, and a layer of cavity with the thickness of 0.5mm is additionally arranged to ensure that the outer surfaces of the multi-layer cavity glass are all the physical toughened glass;
(4) Quantitatively pouring the prepared fireproof layer material into the cavities of the multi-layer cavity glass (4 glass 3 cavities) in sequence, standing for defoaming, and sealing;
(5) And (3) putting the sealed multi-layer glass into an oven, heating to about 75 ℃, heating for 8-10 hours, and taking out to obtain the low-temperature non-heat-insulation composite fireproof glass.
Example 2
The fireproof layer material in this embodiment is prepared by the following steps:
(1) Weighing the raw materials of the fireproof layer material according to the following weight:
375kg of nano-silica particles having a particle size of 180nm, 200kg of deionized water, 12.5kg of ethylene glycol/glycerol (1:1), 1kg of ethyl orthosilicate, 0.5kg of sucrose/fructose (4:1), 0.5kg of potassium dihydrogen phosphate, 0.2kg of borax, 0.2kg of boric acid, 0.5kg of 2- (trifluoromethyl) acrylic acid, 1kg of butyl acrylate, 0.15kg of methacrylic acid, 0.3kg of methyl methacrylate, 0.2kg of alumina, 0.3kg of polyphosphate, 0.2kg of plasticizer and 168.8kg of potassium hydroxide having a purity of 85%.
(2) The above raw materials were prepared into a flame retardant layer material in the same preparation method as in example 1.
The preparation method of the non-heat-insulating composite fire-resistant glass in this example is the same as that of the non-heat-insulating composite fire-resistant glass in example 1, except that the composition of the fire-resistant layer material is different.
Example 3
The fireproof layer material in this embodiment is prepared by the following steps:
(1) Weighing the raw materials of the fireproof layer material according to the following weight:
350kg of nano-silica particles having a particle size of 180nm, 200kg of deionized water, 12.5kg of ethylene glycol/glycerol (1:1), 1kg of ethyl orthosilicate, 0.5kg of sucrose/fructose (4:1), 0.5kg of potassium dihydrogen phosphate, 0.2kg of borax, 0.2kg of boric acid, 0.5kg of 2- (trifluoromethyl) acrylic acid, 1kg of butyl acrylate, 0.15kg of methacrylic acid, 0.3kg of methyl methacrylate, 0.2kg of alumina, 0.3kg of polyphosphate, 0.2kg of plasticizer and 168.8kg of potassium hydroxide having a purity of 85%.
(2) The above raw materials were prepared into a flame retardant layer material in the same preparation method as in example 1.
The preparation method of the non-heat-insulating composite fire-resistant glass in this example is the same as that of the non-heat-insulating composite fire-resistant glass in example 1, except that the composition of the fire-resistant layer material is different.
Example 4
The fireproof layer material in this embodiment is prepared by the following steps:
(1) Weighing the raw materials of the fireproof layer material according to the following weight:
325kg of nano-silica particles having a particle size of 180nm, 200kg of deionized water, 12.5kg of ethylene glycol/glycerol (1:1), 1kg of ethyl orthosilicate, 0.5kg of sucrose/fructose (4:1), 0.5kg of potassium dihydrogen phosphate, 0.2kg of borax, 0.2kg of boric acid, 0.5kg of 2- (trifluoromethyl) acrylic acid, 1kg of butyl acrylate, 0.15kg of methacrylic acid, 0.3kg of methyl methacrylate, 0.2kg of alumina, 0.3kg of polyphosphate, 0.2kg of plasticizer and 168.8kg of potassium hydroxide having a purity of 85%.
(2) The above raw materials were prepared into a flame retardant layer material in the same preparation method as in example 1.
The preparation method of the non-heat-insulating composite fire-resistant glass in this example is the same as that of the non-heat-insulating composite fire-resistant glass in example 1, except that the composition of the fire-resistant layer material is different.
Example 5
The fireproof layer material in this embodiment is prepared by the following steps:
(1) Weighing the raw materials of the fireproof layer material according to the following weight:
425kg of nano-silica particles having a particle size of 180nm, 200kg of deionized water, 12.5kg of ethylene glycol/glycerol (1:1), 1kg of ethyl orthosilicate, 0.5kg of sucrose/fructose (4:1), 0.5kg of potassium dihydrogen phosphate, 0.2kg of borax, 0.2kg of boric acid, 0.5kg of 2- (trifluoromethyl) acrylic acid, 1kg of butyl acrylate, 0.15kg of methacrylic acid, 0.3kg of methyl methacrylate, 0.2kg of alumina, 0.3kg of polyphosphate, 0.2kg of plasticizer and 168.8kg of potassium hydroxide having a purity of 85%.
(2) The above raw materials were prepared into a flame retardant layer material in the same preparation method as in example 1.
The preparation method of the non-heat-insulating composite fire-resistant glass in this example is the same as that of the non-heat-insulating composite fire-resistant glass in example 1, except that the composition of the fire-resistant layer material is different.
Example 6
The fireproof layer material in this embodiment is prepared by the following steps:
(1) Weighing the raw materials of the fireproof layer material according to the following weight:
400kg of nano-silica particles having a particle size of 180nm, 200kg of deionized water, 13.5kg of ethylene glycol/glycerol (1:1), 1kg of ethyl orthosilicate, 0.5kg of sucrose/fructose (4:1), 0.5kg of potassium dihydrogen phosphate, 0.2kg of borax, 0.2kg of boric acid, 0.5kg of 2- (trifluoromethyl) acrylic acid, 1kg of butyl acrylate, 0.15kg of methacrylic acid, 0.3kg of methyl methacrylate, 0.2kg of alumina, 0.3kg of polyphosphate, 0.2kg of plasticizer and 168.8kg of potassium hydroxide having a purity of 85%;
(2) The above raw materials were prepared into a flame retardant layer material in the same preparation method as in example 1.
The preparation method of the non-heat-insulating composite fire-resistant glass in this example is the same as that of the non-heat-insulating composite fire-resistant glass in example 1, except that the composition of the fire-resistant layer material is different.
Example 7
The fireproof layer material in this embodiment is prepared by the following steps:
(1) Weighing the raw materials of the fireproof layer material according to the following weight:
400kg of nano-silica particles having a particle size of 180nm, 200kg of deionized water, 14.5kg of ethylene glycol/glycerol (1:1), 1kg of ethyl orthosilicate, 0.5kg of sucrose/fructose (4:1), 0.5kg of potassium dihydrogen phosphate, 0.2kg of borax, 0.2kg of boric acid, 0.5kg of 2- (trifluoromethyl) acrylic acid, 1kg of butyl acrylate, 0.15kg of methacrylic acid, 0.3kg of methyl methacrylate, 0.2kg of alumina, 0.3kg of polyphosphate, 0.2kg of plasticizer and 168.8kg of potassium hydroxide having a purity of 85%;
(2) The above raw materials were prepared into a flame retardant layer material in the same preparation method as in example 1.
The embodiment of the invention also provides a method for preparing non-heat-insulating composite fireproof glass by using the fireproof layer material, which is the same as the preparation method of the embodiment 1.
Example 8
The fireproof layer material in this embodiment is prepared by the following steps:
(1) Weighing the raw materials of the fireproof layer material according to the following weight:
400kg of nano-silica particles having a particle size of 180nm, 200kg of deionized water, 11.5kg of ethylene glycol/glycerol (1:1), 1kg of ethyl orthosilicate, 0.5kg of sucrose/fructose (4:1), 0.5kg of potassium dihydrogen phosphate, 0.2kg of borax, 0.2kg of boric acid, 0.5kg of 2- (trifluoromethyl) acrylic acid, 1kg of butyl acrylate, 0.15kg of methacrylic acid, 0.3kg of methyl methacrylate, 0.2kg of alumina, 0.3kg of polyphosphate, 0.2kg of plasticizer and 168.8kg of potassium hydroxide having a purity of 85%;
(2) The above raw materials were prepared into a flame retardant layer material in the same preparation method as in example 1.
The preparation method of the non-heat-insulating composite fire-resistant glass in this example is the same as that of the non-heat-insulating composite fire-resistant glass in example 1, except that the composition of the fire-resistant layer material is different.
Example 9
The fireproof layer material in this embodiment is prepared by the following steps:
(1) Weighing the raw materials of the fireproof layer material according to the following weight:
400kg of nano-silica particles having a particle size of 180nm, 225kg of deionized water, 12.5kg of ethylene glycol/glycerol (1:1), 1kg of ethyl orthosilicate, 0.5kg of sucrose/fructose (4:1), 0.5kg of potassium dihydrogen phosphate, 0.2kg of borax, 0.2kg of boric acid, 0.5kg of 2- (trifluoromethyl) acrylic acid, 1kg of butyl acrylate, 0.15kg of methacrylic acid, 0.3kg of methyl methacrylate, 0.2kg of alumina, 0.3kg of polyphosphate, 0.2kg of plasticizer and 168.8kg of potassium hydroxide having a purity of 85%;
(2) The above raw materials were prepared into a flame retardant layer material in the same preparation method as in example 1.
The preparation method of the non-heat-insulating composite fire-resistant glass in this example is the same as that of the non-heat-insulating composite fire-resistant glass in example 1, except that the composition of the fire-resistant layer material is different.
Example 10
The flame retardant layer material in the examples was prepared by the following steps:
(1) Weighing the raw materials of the fireproof layer material according to the following weight:
400kg of nano-silica particles having a particle size of 180nm, 250kg of deionized water, 12.5kg of ethylene glycol/glycerol (1:1), 1kg of ethyl orthosilicate, 0.5kg of sucrose/fructose (4:1), 0.5kg of potassium dihydrogen phosphate, 0.2kg of borax, 0.2kg of boric acid, 0.5kg of 2- (trifluoromethyl) acrylic acid, 1kg of butyl acrylate, 0.15kg of methacrylic acid, 0.3kg of methyl methacrylate, 0.2kg of alumina, 0.3kg of polyphosphate, 0.2kg of plasticizer and 168.8kg of potassium hydroxide having a purity of 85%;
(2) The above raw materials were prepared into a flame retardant layer material in the same preparation method as in example 1.
The preparation method of the non-heat-insulating composite fire-resistant glass in this example is the same as that of the non-heat-insulating composite fire-resistant glass in example 1, except that the composition of the fire-resistant layer material is different.
Example 11
The fireproof layer material in this embodiment is prepared by the following steps:
(1) Weighing the raw materials of the fireproof layer material according to the following weight:
400kg of nano-silica particles with a particle size of 180nm, 175kg of deionized water, 12.5kg of ethylene glycol/glycerol (1:1), 1kg of ethyl orthosilicate, 0.5kg of sucrose/fructose (4:1), 0.5kg of potassium dihydrogen phosphate, 0.2kg of borax, 0.2kg of boric acid, 0.5kg of 2- (trifluoromethyl) acrylic acid, 1kg of butyl acrylate, 0.15kg of methacrylic acid, 0.3kg of methyl methacrylate, 0.2kg of alumina, 0.3kg of polyphosphate, 0.2kg of plasticizer 168.8kg of potassium hydroxide with a purity of 85%;
(2) The above raw materials were prepared into a flame retardant layer material in the same preparation method as in example 1.
The preparation method of the non-heat-insulating composite fire-resistant glass in this example is the same as that of the non-heat-insulating composite fire-resistant glass in example 1, except that the composition of the fire-resistant layer material is different.
Example 12
The fireproof layer material in this embodiment is prepared by the following steps:
(1) The same raw materials of the flame retardant layer material as in example 1 were weighed:
(2) The above raw materials were prepared into a flame retardant layer material in the same preparation method as in example 1.
The non-heat-insulating composite fireproof glass in the embodiment is prepared from the fireproof layer material through the following steps:
(1) Preparing 3 pieces of glass with the thickness of 3mm, wherein two pieces of glass are physically toughened glass; in order to ensure that the prepared non-heat-insulating composite fireproof glass has higher strength, the glass positioned in the middle is preferably slightly thicker than other layers of glass;
(2) The 1 piece of physical toughened glass is used as the outermost layer glass to be synthesized with 1 piece of non-physical toughened glass into a cavity with the thickness of 0.5mm by utilizing a thickness-fixing adhesive tape, the rest 1 piece of non-physical toughened glass is sequentially overlapped by utilizing the thickness-fixing adhesive tape, the cavity with the thickness of 0.5mm is reserved among each piece of glass, and finally the other piece of physical toughened glass is laminated with the multi-layer cavity glass by utilizing the thickness-fixing adhesive tape, and a layer of cavity with the thickness of 0.5mm is additionally arranged to ensure that the outer surfaces of the multi-layer cavity glass are all the physical toughened glass;
(4) Quantitatively pouring the prepared fireproof layer material into the cavities of the multi-layer cavity glass (3 glass 2 cavities) in sequence, standing for defoaming, and sealing;
(5) And (3) putting the sealed multi-layer glass into an oven, heating to about 75 ℃, heating for 6-8 hours, and taking out to obtain the low-temperature non-heat-insulation composite fireproof glass.
Example 13
The fireproof layer material in this embodiment is prepared by the following steps:
(1) The same raw materials of the flame retardant layer material as in example 1 were weighed:
(2) The above raw materials were prepared into a flame retardant layer material in the same preparation method as in example 1.
The non-heat-insulating composite fireproof glass in the embodiment is prepared from the fireproof layer material through the following steps:
(1) Preparing 2 pieces of glass with the thickness of 3mm, which are all physically toughened glass; in order to ensure that the prepared non-heat-insulating composite fireproof glass has higher strength, the glass positioned in the middle is preferably slightly thicker than other layers of glass;
(2) The 1 piece of physical toughened glass is used as the outermost layer glass and is synthesized with the other 1 piece of physical toughened glass by using a fixed-thickness adhesive tape to form a cavity with the thickness of 0.5 mm;
(4) Quantitatively pouring the prepared fireproof layer material into the cavity of the multi-layer cavity glass (2 glass 1 cavity) in sequence, standing for defoaming, and sealing;
(5) And (3) putting the sealed multi-layer glass into an oven, heating to about 75 ℃, heating for 4-6 hours, and taking out to obtain the low-temperature non-heat-insulation composite fireproof glass.
Comparative example 1
The comparative example provides a fire-resistant layer material which is made of pure potash water glass with a modulus of 3.4.
The method of producing the fire-resistant glass in this comparative example was the same as that of the non-heat-insulating composite fire-resistant glass in example 1, except that the composition of the fire-resistant layer material was different.
Comparative example 2
The fireproof material layer in this comparative example was prepared by the following steps:
1kg of water and 1kg of potash water glass with the modulus of 3.4 are taken and uniformly mixed to form the fireproof layer material.
The method of producing the fire-resistant glass in this comparative example was the same as that of the non-heat-insulating composite fire-resistant glass in example 1, except that the composition of the fire-resistant layer material was different.
According to a GB/T12513-2006 glazed member fire resistance test method, fire resistance tests are carried out on low-temperature non-heat-insulation type composite fire-proof glass prepared from the fire-proof layer materials provided in examples 1-13 and comparative examples 1-2 to obtain the fire resistance time of the non-heat-insulation type composite fire-proof glass, 4 parallel samples are taken in the tests, and the average value of the data is taken as an experimental result; the transmittance of each non-heat-insulation composite fireproof glass is obtained through glass transmittance detection; and the apparent mass of each non-heat-insulation composite fireproof glass is obtained through naked eye observation. The viscosity of the pre-reaction solution of the fireproof layer material prepared in the examples and comparative examples of the present invention and the performance parameters of the fireproof glass are shown in tables 1 and 2.
TABLE 1 viscosity of the pre-reaction solution for flame retardant coating materials
TABLE 2 Performance parameter Table for non-insulating composite fire glass
| Examples | Transmittance% | Low temperature/°c resistance | Glass integrity/min | Apparent mass | Strength of |
| Example 1 | 84±1 | -45±2 | 245±5 | No microbubble | 6H |
| Example 2 | 84±1 | -45±2 | 235±5 | No microbubble | 5H |
| Example 3 | 84±1 | -45±2 | 215±5 | No microbubble | 4H |
| Example 4 | 84±1 | -45±2 | 205±5 | No microbubble | 3H |
| Example 5 | 84±1 | -25±2 | 245±5 | No microbubble | 6H |
| Example 6 | 84±1 | -40±2 | 245±5 | No microbubble | 4H |
| Example 7 | 84±1 | -40±2 | 245±5 | No microbubble | 4H |
| Example 8 | 84±1 | -20±2 | 235±5 | No microbubble | 5H |
| Example 9 | 84±1 | -20±2 | 225±5 | No microbubble | 4H |
| Example 10 | 84±1 | -10±2 | 225±5 | No microbubble | 3H |
| Example 11 | 84±1 | -20±2 | 205±5 | With microbubbles | 6H |
| Example 12 | 88±1 | -45±2 | 195±5 | No microbubble | 6H |
| Example 13 | 92±1 | -45±2 | 155±5 | No microbubble | 6H |
| Comparative example 1 | 78±1 | -5±2 | 65±5 | With microbubbles | 5B |
| Comparative example 2 | 79±1 | -3±2 | 35±5 | With microbubbles | 4B |
As can be seen from Table 2, the low-temperature, non-heat-insulating composite fire-proof glass of the present invention has no microbubbles, while the fire-proof glass prepared in the comparative example has a large number of microbubbles inside; the fire-proof time of the low-temperature non-heat-insulation composite fire-proof glass is 1.5-2.5 times that of the non-heat-insulation composite fire-proof glass of the comparative example, and the transmittance is obviously higher than that of the fire-proof glass of the comparative example. The above description adopts potash water glass or pure potash water glass as the fireproof layer of the fireproof glass, so that a large number of microbubbles are easily generated in the glass, the existence of the microbubbles reduces the hardness and the fireproof heat resistance of the non-heat-insulation type composite fireproof glass, and the light transmittance and the apparent quality of the non-heat-insulation type composite fireproof glass are seriously affected. According to the embodiment of the invention, the formula of the fireproof layer is improved, the organic-inorganic hybrid particles with the nano core-shell structure and the potassium hydroxide aqueous solution are mixed, a synergistic effect is generated among the components of the fireproof layer, bubbles in the non-heat-insulation composite fireproof glass interlayer are eliminated, the non-heat-insulation composite fireproof glass has better fireproof heat resistance, meanwhile, the low temperature resistance of the non-heat-insulation composite fireproof glass is improved, and the fireproof glass can be used in a low-temperature environment (-40 ℃). The non-heat-insulating composite fireproof glass prepared by the embodiment of the invention has the advantages of no microbubbles, good adhesive force, high transmittance, long fireproof time and low temperature resistance.
As is clear from the data shown in table 1, the non-heat-insulating composite fire-proof glass of the present invention has no microbubbles, because the pre-reaction solution of the fire-proof layer material of the present invention has low viscosity, which is favorable for the escape of bubbles, thereby facilitating the discharge of the medium gas of the fire-proof layer when preparing the fire-proof layer and saving the man-hour for preparing the non-heat-insulating composite fire-proof glass.
As is evident from the comparison of examples 1 to 11 with comparative examples 1 to 2, when the number of layers of glass is gradually decreased by using the same fireproof layer material, the transmittance is better and the low temperature resistance is not changed and the fireproof time is gradually decreased as the glass sheet is decreased.
The hardness of the low-temperature type non-thermal insulation composite fireproof glass provided by the embodiment of the invention can reach more than 2H, and some of the low-temperature type non-thermal insulation composite fireproof glass can reach 6H.
In the foregoing embodiments, the descriptions of the embodiments are emphasized, and for parts of one embodiment that are not described in detail, reference may be made to related descriptions of other embodiments.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention in any way, but any simple modification, equivalent variation and modification made to the above embodiments according to the technical substance of the present invention still fall within the scope of the technical solution of the present invention.
Claims (6)
1. The non-heat-insulating composite fireproof glass is formed by laminating at least two pieces of glass, an interlayer is arranged between two adjacent pieces of glass, and at least one interlayer is a fireproof layer made of fireproof layer materials, and the non-heat-insulating composite fireproof glass is characterized in that the fireproof layer materials comprise fluorine-modified nano core-shell structure organic/inorganic hybrid particles, a core layer of the fluorine-modified nano core-shell structure organic/inorganic hybrid particles is nano silicon dioxide particles and aggregates thereof, and the fluorine-modified nano core-shell structure organic/inorganic hybrid particles are poly (2- (trifluoromethyl) acrylic acid-butyl acrylate-methacrylic acid-methyl methacrylate) hydrophobic-hydrophilic amphoteric copolymers; the fireproof layer material is prepared by the following steps:
step 1), condensing inhibitor, ethyl orthosilicate, char forming agent, char forming auxiliary agent, heat stabilizer, potassium hydroxide with purity of 85%, deionized water according to 5-20:0.5-5:0.2-10:0.2-10:0.01-0.2: 50-200 weight portions; standing and aging for 24 hours, and generating a silicon dioxide seed solution after the ethyl orthosilicate is alcoholized, wherein the particle size of silicon dioxide particles is 20-40 nm, so as to prepare a first mixed solution;
Step 2), gradually dispersing by means of a gradient high-pressure homogenizing technology, sequentially adding 50-500 parts by weight of hydroxylated gas-phase nano silicon dioxide particles into a first mixed solution according to 30%, 25%, 20%, 15% and 10% by weight respectively, and homogenizing under 20-180 MPa for 12min, 10min, 8min, 6min and 4min each time to obtain a nuclear layer solution;
step 3), mixing 0.01-1.5 parts by weight of 2- (trifluoromethyl) acrylic acid, 0.01-1.5 parts by weight of butyl acrylate, 0.01-1.5 parts by weight of methacrylic acid and methyl methacrylate to prepare a second mixed solution;
step 4), dropwise adding 0.04-5 parts by weight of a second mixed solution and 0.001-0.05 parts by weight of redox initiator into 100-900 parts by weight of core layer solution at a constant speed under the temperature condition of 60-65 ℃ by means of a starvation polymerization method, and coating the surfaces of the nano silicon dioxide particles with a layer of organic/inorganic composite material after polymerization to obtain onion-type hydrophobic-hydrophilic amphoteric nano core-shell structure organic/inorganic hybrid silicon dioxide particle emulsion;
step 5), under the condition of high stirring, sequentially adding 0.1-2 parts by weight of ion fixing agent, 0.01-1.5 parts by weight of storage stabilizer and 0.04-0.5 part by weight of plasticizer into 100-900 parts by weight of the hydrophobic-hydrophilic nano core-shell structure organic/inorganic hybrid silicon dioxide particle emulsion, stirring for 30min, and uniformly mixing to obtain a fireproof layer material base solution;
And 6) adding 17-280 parts by weight of potassium hydroxide with the purity of 85% into 100-900 parts by weight of the base solution of the fireproof layer material, vacuumizing, and uniformly stirring to obtain the fireproof layer material.
2. The non-insulating composite fire resistant glazing of claim 1, wherein the fire resistant layer material has a modulus of 4.2 to 5.5.
3. The non-thermal insulation composite fireproof glass according to claim 1 or 2, wherein the particle size of the hydrophobic-hydrophilic amphoteric nano-core-shell structure organic/inorganic hybrid silica particles is 150nm-800nm, the particle size of the core layer is 110nm-720nm, and the specific surface area is 20-40 m 2 Per gram, the density of silicon hydroxyl groups is 2-4 per nm 2 The particle size distribution is a multimodal broad distribution; the thickness of the shell layer is 20nm-40nm.
4. The non-insulating composite fire-resistant glass according to claim 1 or 2, wherein the anti-condensing agent is at least one of ethylene glycol, propylene glycol, glycerol and pentaerythritol;
the char forming agent is at least one of sucrose, fructose, glucose, granulated sugar and maltose;
the carbon forming auxiliary agent is at least one of potassium dihydrogen phosphate, potassium hydrogen phosphate, sodium dihydrogen phosphate and sodium hydrogen phosphate;
the heat-resistant stabilizer is at least one of borax and boric acid;
The ion fixing agent is at least one of zinc oxide, aluminum oxide and starch;
the storage stabilizer is at least one of sodium polyphosphate and potassium polyphosphate;
the plasticizer is at least one of dipropylene glycol butyl ether and dipropylene glycol methyl ether.
5. The non-insulating composite fire protection glass according to claim 1 or 2, wherein the layer of fire protection material has a thickness of 0.4-1.0mm.
6. A method for producing a flame retardant coating material according to any one of claims 1 to 4, comprising the steps of:
step 1), condensing inhibitor, ethyl orthosilicate, char forming agent, char forming auxiliary agent, heat stabilizer, potassium hydroxide with purity of 85%, deionized water according to 5-20:0.5-5:0.2-10:0.2-10:0.01-0.2: 50-200 weight portions of the raw materials are mixed, and the mixture is kept still and aged for 24 hours, and after the ethyl orthosilicate is alcoholized, a silicon dioxide seed solution is generated, and the particle size of silicon dioxide particles is 20-40 nm, so that a first mixed solution is prepared;
step 2), gradually dispersing by means of a gradient high-pressure homogenizing technology, sequentially adding 50-500 parts by weight of hydroxylated gas-phase nano silicon dioxide particles into a first mixed solution according to 30%, 25%, 20%, 15% and 10% by weight respectively, and homogenizing under 20-180 MPa for 12min, 10min, 8min, 6min and 4min each time to obtain a nuclear layer solution;
Step 3), mixing 0.01-1.5 parts by weight of 2- (trifluoromethyl) acrylic acid, 0.01-1.5 parts by weight of butyl acrylate, 0.01-1.5 parts by weight of methacrylic acid and methyl methacrylate to prepare a second mixed solution;
step 4), dropwise adding 0.04-5 parts by weight of a second mixed solution and 0.001-0.05 parts by weight of redox initiator into 100-900 parts by weight of core layer solution at a constant speed under the temperature condition of 60-65 ℃ by means of a starvation polymerization method, and coating the surfaces of the nano silicon dioxide particles with a layer of organic/inorganic composite material after polymerization to obtain onion-type hydrophobic-hydrophilic amphoteric nano core-shell structure organic/inorganic hybrid silicon dioxide particle emulsion;
step 5), under the condition of high stirring, sequentially adding 0.1-2 parts by weight of ion fixing agent, 0.01-1.5 parts by weight of storage stabilizer and 0.04-0.5 part by weight of plasticizer into 100-900 parts by weight of fluorine modified nano core-shell structure organic/inorganic hybrid silicon dioxide particle emulsion, stirring for 30min, and uniformly mixing to obtain a fireproof layer material base solution;
and 6) adding 17-280 parts by weight of potassium hydroxide with the purity of 85% into 100-900 parts by weight of the base solution of the fireproof layer material, vacuumizing, and uniformly stirring to obtain the fireproof layer material.
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| CN102659990A (en) * | 2012-05-02 | 2012-09-12 | 西北工业大学 | Method for preparing stable-dispersibility pigment/polymer core-shell structure composite granules by using by polymer-wrapped pigment particles |
| CN112204097A (en) * | 2018-03-29 | 2021-01-08 | 新加坡科技研究局 | Reinforced polyolefin composite material |
| KR102328902B1 (en) * | 2021-06-03 | 2021-11-19 | 주식회사 서일 | Gas barrier coating composition, and Gas barrier layer using this |
| CN114409279A (en) * | 2022-01-24 | 2022-04-29 | 广东卫屋防火科技有限公司 | Fireproof interlayer adhesive, preparation method thereof and fireproof glass comprising fireproof interlayer adhesive |
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| CN102659990A (en) * | 2012-05-02 | 2012-09-12 | 西北工业大学 | Method for preparing stable-dispersibility pigment/polymer core-shell structure composite granules by using by polymer-wrapped pigment particles |
| CN112204097A (en) * | 2018-03-29 | 2021-01-08 | 新加坡科技研究局 | Reinforced polyolefin composite material |
| KR102328902B1 (en) * | 2021-06-03 | 2021-11-19 | 주식회사 서일 | Gas barrier coating composition, and Gas barrier layer using this |
| CN114409279A (en) * | 2022-01-24 | 2022-04-29 | 广东卫屋防火科技有限公司 | Fireproof interlayer adhesive, preparation method thereof and fireproof glass comprising fireproof interlayer adhesive |
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