CN111748231A - Synthesis method of antimony oxide sol and flame-retardant auxiliary - Google Patents
Synthesis method of antimony oxide sol and flame-retardant auxiliary Download PDFInfo
- Publication number
- CN111748231A CN111748231A CN202010595627.1A CN202010595627A CN111748231A CN 111748231 A CN111748231 A CN 111748231A CN 202010595627 A CN202010595627 A CN 202010595627A CN 111748231 A CN111748231 A CN 111748231A
- Authority
- CN
- China
- Prior art keywords
- sol
- water
- halogen
- gamma
- antimony
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 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 title claims abstract description 31
- 239000003063 flame retardant Substances 0.000 title claims abstract description 31
- 229910000410 antimony oxide Inorganic materials 0.000 title claims abstract description 20
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000001308 synthesis method Methods 0.000 title claims abstract description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 52
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims abstract description 48
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 239000003381 stabilizer Substances 0.000 claims abstract description 11
- 239000003607 modifier Substances 0.000 claims abstract description 7
- 229910052736 halogen Inorganic materials 0.000 claims description 24
- 150000002367 halogens Chemical class 0.000 claims description 24
- 239000007787 solid Substances 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000011347 resin Substances 0.000 claims description 21
- 229920005989 resin Polymers 0.000 claims description 20
- 238000002360 preparation method Methods 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 8
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 claims description 8
- 229910000342 sodium bisulfate Inorganic materials 0.000 claims description 8
- 239000000839 emulsion Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 229920002635 polyurethane Polymers 0.000 claims description 7
- 239000004814 polyurethane Substances 0.000 claims description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 230000002194 synthesizing effect Effects 0.000 claims description 6
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 6
- 239000004925 Acrylic resin Substances 0.000 claims description 5
- 229920000178 Acrylic resin Polymers 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 5
- 239000003822 epoxy resin Substances 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-M hydrogensulfate Chemical compound OS([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-M 0.000 claims description 5
- 229920000647 polyepoxide Polymers 0.000 claims description 5
- 229920000728 polyester Polymers 0.000 claims description 5
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 5
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 4
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 4
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 claims description 4
- 229920005672 polyolefin resin Polymers 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims description 3
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 239000004626 polylactic acid Substances 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 claims description 3
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 claims description 3
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 claims description 3
- 229920006305 unsaturated polyester Polymers 0.000 claims description 3
- HXLAEGYMDGUSBD-UHFFFAOYSA-N 3-[diethoxy(methyl)silyl]propan-1-amine Chemical compound CCO[Si](C)(OCC)CCCN HXLAEGYMDGUSBD-UHFFFAOYSA-N 0.000 claims description 2
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 2
- WOXXJEVNDJOOLV-UHFFFAOYSA-N ethenyl-tris(2-methoxyethoxy)silane Chemical compound COCCO[Si](OCCOC)(OCCOC)C=C WOXXJEVNDJOOLV-UHFFFAOYSA-N 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims description 2
- INJVFBCDVXYHGQ-UHFFFAOYSA-N n'-(3-triethoxysilylpropyl)ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CCCNCCN INJVFBCDVXYHGQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 239000004094 surface-active agent Substances 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims 1
- 229910001854 alkali hydroxide Inorganic materials 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 239000003002 pH adjusting agent Substances 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- 239000003973 paint Substances 0.000 abstract description 7
- 239000012752 auxiliary agent Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 239000004530 micro-emulsion Substances 0.000 abstract 1
- LJCFOYOSGPHIOO-UHFFFAOYSA-N antimony pentoxide Chemical compound O=[Sb](=O)O[Sb](=O)=O LJCFOYOSGPHIOO-UHFFFAOYSA-N 0.000 description 22
- 239000000243 solution Substances 0.000 description 21
- 238000000576 coating method Methods 0.000 description 16
- 239000011248 coating agent Substances 0.000 description 14
- 229910052787 antimony Inorganic materials 0.000 description 9
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- 239000002245 particle Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- 229910019142 PO4 Inorganic materials 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 5
- 239000010452 phosphate Substances 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 3
- -1 alkyl phosphate Chemical compound 0.000 description 3
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 3
- 229910052794 bromium Inorganic materials 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- LXWPJAGZRHTAOO-UHFFFAOYSA-N [Sb].[Br] Chemical compound [Sb].[Br] LXWPJAGZRHTAOO-UHFFFAOYSA-N 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 2
- 229920000915 polyvinyl chloride Polymers 0.000 description 2
- 229910000343 potassium bisulfate Inorganic materials 0.000 description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 2
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 2
- BZQKBFHEWDPQHD-UHFFFAOYSA-N 1,2,3,4,5-pentabromo-6-[2-(2,3,4,5,6-pentabromophenyl)ethyl]benzene Chemical compound BrC1=C(Br)C(Br)=C(Br)C(Br)=C1CCC1=C(Br)C(Br)=C(Br)C(Br)=C1Br BZQKBFHEWDPQHD-UHFFFAOYSA-N 0.000 description 1
- HJTAZXHBEBIQQX-UHFFFAOYSA-N 1,5-bis(chloromethyl)naphthalene Chemical compound C1=CC=C2C(CCl)=CC=CC2=C1CCl HJTAZXHBEBIQQX-UHFFFAOYSA-N 0.000 description 1
- JTNCEQNHURODLX-UHFFFAOYSA-N 2-phenylethanimidamide Chemical compound NC(=N)CC1=CC=CC=C1 JTNCEQNHURODLX-UHFFFAOYSA-N 0.000 description 1
- ZYAASQNKCWTPKI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propan-1-amine Chemical compound CO[Si](C)(OC)CCCN ZYAASQNKCWTPKI-UHFFFAOYSA-N 0.000 description 1
- LWFBRHSTNWMMGN-UHFFFAOYSA-N 4-phenylpyrrolidin-1-ium-2-carboxylic acid;chloride Chemical compound Cl.C1NC(C(=O)O)CC1C1=CC=CC=C1 LWFBRHSTNWMMGN-UHFFFAOYSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- 239000004114 Ammonium polyphosphate Substances 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 229920002433 Vinyl chloride-vinyl acetate copolymer Polymers 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 235000019826 ammonium polyphosphate Nutrition 0.000 description 1
- 229920001276 ammonium polyphosphate Polymers 0.000 description 1
- GOLCXWYRSKYTSP-UHFFFAOYSA-N arsenic trioxide Inorganic materials O1[As]2O[As]1O2 GOLCXWYRSKYTSP-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- CEDDGDWODCGBFQ-UHFFFAOYSA-N carbamimidoylazanium;hydron;phosphate Chemical compound NC(N)=N.OP(O)(O)=O CEDDGDWODCGBFQ-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- WHHGLZMJPXIBIX-UHFFFAOYSA-N decabromodiphenyl ether Chemical compound BrC1=C(Br)C(Br)=C(Br)C(Br)=C1OC1=C(Br)C(Br)=C(Br)C(Br)=C1Br WHHGLZMJPXIBIX-UHFFFAOYSA-N 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- QGEOKXWFGANCJL-UHFFFAOYSA-N ethenyl acetate;hydrochloride Chemical compound Cl.CC(=O)OC=C QGEOKXWFGANCJL-UHFFFAOYSA-N 0.000 description 1
- 239000005038 ethylene vinyl acetate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012796 inorganic flame retardant Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229940050176 methyl chloride Drugs 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- CMPQUABWPXYYSH-UHFFFAOYSA-N phenyl phosphate Chemical compound OP(O)(=O)OC1=CC=CC=C1 CMPQUABWPXYYSH-UHFFFAOYSA-N 0.000 description 1
- XZTOTRSSGPPNTB-UHFFFAOYSA-N phosphono dihydrogen phosphate;1,3,5-triazine-2,4,6-triamine Chemical compound NC1=NC(N)=NC(N)=N1.OP(O)(=O)OP(O)(O)=O XZTOTRSSGPPNTB-UHFFFAOYSA-N 0.000 description 1
- XFZRQAZGUOTJCS-UHFFFAOYSA-N phosphoric acid;1,3,5-triazine-2,4,6-triamine Chemical compound OP(O)(O)=O.NC1=NC(N)=NC(N)=N1 XFZRQAZGUOTJCS-UHFFFAOYSA-N 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- CHKVPAROMQMJNQ-UHFFFAOYSA-M potassium bisulfate Chemical compound [K+].OS([O-])(=O)=O CHKVPAROMQMJNQ-UHFFFAOYSA-M 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 1
- 239000010455 vermiculite Substances 0.000 description 1
- 229910052902 vermiculite Inorganic materials 0.000 description 1
- 235000019354 vermiculite Nutrition 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
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- Paints Or Removers (AREA)
Abstract
The invention discloses a synthesis method of antimony oxide sol and a flame-retardant auxiliary agent. The method comprises the following steps: (1) uniformly dispersing water, a sol stabilizer, antimony trioxide, a modifier and the like, dropwise adding hydrogen peroxide, and heating the mixture to 70-95 ℃ to obtain a mixture of antimony oxides in a sol state; (2) adding a pH regulator, and adding one or two of molybdenum trioxide sol or molybdenum disulfide sol; (3) concentrating to the required concentration. The sol prepared by the invention is stable, transparent and micro-emulsion white. The material prepared by the method is a flame retardant auxiliary agent with excellent performance in the field of water-based paint.
Description
Technical Field
The invention relates to a method for synthesizing antimony oxide sol and a flame-retardant auxiliary agent, and the product is particularly suitable for application of a water-based paint system.
Background
China is the most abundant country in the world with antimony ore. The nationwide reserve of antimony accounts for 51.8% of the world's total reserves. Although the supply amount of antimony products accounts for nearly half of the world, the deep processing rate of antimony products in China is low, antimony trioxide is the most important product consuming antimony resources in China, the using amount of the antimony trioxide reaches more than 80%, and 60% of antimony is used for producing the flame retardant antimony trioxide, so that the saving and application of the non-renewable antimony resources are of great significance. At present, the high-efficiency flame retardance of a bromine-antimony flame retardant system still has wide application in the flame retardant industry, so that the consumption of low-efficiency antimony materials in China is reduced, and the effective application of the antimony materials is urgent.
Antimony trioxide and hydrogen peroxide (H)2O2) Under the condition of heating, the nano antimony pentoxide sol can be easily prepared, and because the antimony pentoxide is dispersed in water solution in nano level and the grain size is less than 20 nm, the antimony pentoxide sol has a large chemical reaction interface and can be more quickly preparedChemical response improves the synergistic flame retardance to the organic bromine. The molar ratio of the antimony trioxide to the hydrogen peroxide is more than or equal to 1: 2, hydrogen peroxide is liable to remain in the reaction system, and this causes unnecessary damage to the aqueous coating system.
CN 101941737A discloses mixing antimony trioxide, hydrogen peroxide, deionized water and an inert porous material, filtering and drying a product after the reaction is finished, and obtaining a white antimony pentoxide solid with a core-shell structure. For a water-based paint system, the powder with the core-shell structure is easy to agglomerate and difficult to disperse, and the interface of antimony oxide is easy to reduce, namely the synergistic flame retardance of antimony pentoxide is reduced.
CN 108793250A discloses a synthesis method for preparing antimony pentoxide by adding hydrogen peroxide dropwise after heating, wherein the molar ratio of antimony trioxide to hydrogen peroxide is 2.0-2.5, and stabilizer triethanolamine is added more than or equal to 4 times. The aqueous solution prepared by the method has low concentration, and the existence of excessive hydrogen peroxide has great destructiveness to the stability of the coating for a water-based coating system, so that the aqueous solution can not be applied to a steel structure flame-retardant coating.
CN 104828866A discloses a preparation method of colloidal antimony oxide dry powder with low volatility at high temperature. And adding metal hydroxide (sodium hydroxide and/or potassium hydroxide) into the prepared antimony pentoxide solution to adjust the pH value, and adding a reducing agent for partial reduction to obtain antimony oxide sol. Removing alkali metal ions in the antimony oxide sol by ion exchange. The method has the advantages of complex process flow, high energy consumption and solid waste generation.
CN 106366723A discloses a burn-through resistant water-based flame retardant adhesive for textile, which comprises a water-based adhesive, a water-based flame retardant adhesive, a halogen flame retardant, a synergistic flame retardant, an auxiliary agent and water. Wherein the water-based adhesive comprises ethylene-vinyl acetate copolymer emulsion and auxiliary adhesive; the water-based flame-retardant gum phosphate flame retardant comprises one or more of ammonium polyphosphate, ammonium phosphate, guanidine phosphate, guanylurea phosphate, melamine phosphate and melamine pyrophosphate, or one or more of alkyl phosphate, condensed phosphate, phenyl phosphate, cage-shaped and spiro-shaped phosphate and cyclic phosphate. The halogen flame retardant comprises one or more of decabromodiphenyl ether, decabromodiphenyl ethane, brominated epoxy resin, polyvinyl chloride, chlorinated paraffin, methyl chloride and the like; the inorganic flame retardant comprises one or more of antimony trioxide, zinc borate, zinc oxide, aluminum hydroxide, arsenic trioxide, antimony pentoxide, magnesium hydroxide, vermiculite powder, talcum powder, calcium carbonate, titanium dioxide, montmorillonite, kaolin, barium sulfate, mica powder, fluorite powder, glass micropowder, expanded graphite, a molecular sieve and zeolite. In order to improve the good dispersibility of the particles, the method needs to break the particles in the liquid by grinding equipment, and the obtained liquid contains micron-sized solid particles, so that the application of the method has certain limitation for thin coatings.
CN 1550453a discloses a method for synthesizing antimony pentoxide by doping molybdate or tungstate, which must use soluble molybdate or tungstate to effectively dope antimony pentoxide.
Disclosure of Invention
The water-based thin coating system has strict requirements on the filler type flame retardant, such as the particle size and the addition amount of the filler. Improper addition can result in poor adhesion of the coating to the substrate and the coating is prone to cracking. The bromine antimony flame retardant has the advantages of small addition amount in the coating, high flame retardant efficiency and small influence on the coating, and is a very effective flame retardant auxiliary agent. However, antimony trioxide used in the industry is white powder with the particle size of about 1-5 microns, and is white suspension in an aqueous system, so that the coating is easy to delaminate, a film-forming substance is easy to crack, and the antimony trioxide cannot be applied to a transparent coating, so that the development and enrichment of antimony pentoxide flame retardant additives are necessary. Aiming at the problems, the invention provides a stable and transparent water-based flame retardant additive, which takes water-based resin and inorganic salt as stabilizers and has good intermiscibility and good film forming property in water-based paint. The paint prepared by the material realizes good flame retardance, strong coating adhesion and difficult cracking, and can also be applied to the field of transparent flame retardant coatings.
The technical scheme adopted by the invention for solving the technical problems is as follows: the synthesis of antimony oxide sol and the preparation of flame retardant additive comprise the following steps:
(1) uniformly dispersing water, a sol stabilizer, antimony trioxide, a modifier and the like, dropwise adding hydrogen peroxide, and heating the mixture to 70-95 ℃ to obtain a mixture of antimony oxides in a sol state;
(2) adding a pH regulator, and adding one or two of molybdenum trioxide sol and molybdenum disulfide sol;
(3) concentrating to the required concentration.
According to the claims: uniformly dispersing water, a sol stabilizer, antimony trioxide, a modifier and the like, dropwise adding hydrogen peroxide, and heating the mixture to 70-95 ℃ to obtain a mixture of antimony oxides in a sol state.
The sol stabilizer is one or more of bisulfate and organic resin, and the bisulfate is preferably sodium bisulfate. The organic resin can be dispersed in water, and comprises one or more of water-based halogen-free or halogen-containing saturated polyester, water-based halogen-free or halogen-containing unsaturated polyester, water-based halogen-free or halogen-containing polyurethane, water-based halogen-free or halogen-containing epoxy resin, water-based halogen-free or halogen-containing acrylic resin, water-based halogen-free or halogen-containing polyolefin resin, polyethylene glycol, polyvinylpyrrolidone, polyethylene oxide, polylactic acid and polyvinyl alcohol.
The resin is capable of aqueous dispersion and has the following characteristics: the resin is soluble in water or a mixed solvent of water and alcohol; or the resin can be dissolved in an organic solvent, and the resulting solution can be dispersed in water with added surfactant to form a water-soluble emulsion. The resin comprises and not only comprises one or more of aqueous halogen-free or halogen-containing saturated polyester, aqueous halogen-free or halogen-containing unsaturated polyester, aqueous halogen-free or halogen-containing polyurethane, aqueous halogen-free or halogen-containing epoxy resin, aqueous halogen-free or halogen-containing acrylic resin, aqueous halogen-free or halogen-containing olefin resin, polyethylene glycol, polyvinylpyrrolidone, polylactic acid and polyvinyl alcohol. Preferably waterborne polyurethane or waterborne epoxy resin, and the weight ratio of the mass of the bromine element to the total mass of the resin is not less than 5 percent.
The molecular weight and alcoholysis degree of the polyvinyl alcohol and resin have great influence on the hydrolyzability and the film forming property, and the grade 1799 is preferred. The aqueous halogen-free or halogen-containing polyester is preferably a low molecular weight water-soluble polyester. The aqueous halogen-free or halogen-containing polyurethane is preferably aqueous polyurethane resin containing bromine. The water-based halogen-free or halogen-containing acrylic resin is preferably an organosilicon modified acrylic resin. The aqueous halogen-free or halogen-containing olefin resin is preferably polyethylene-vinyl acetate copolymer.
The hydrogen peroxide is liquid containing hydrogen peroxide with the concentration of 25-50%, and the concentration of 30% is preferred.
The modifier is a silane coupling agent and comprises one or more of tetramethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, tetraethoxysilane, methyltrimethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, propyltrimethoxysilane, dimethyldimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, N-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane, N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane, N-beta- (aminoethyl) -gamma-aminopropyl-trimethoxysilane, and/or a mixture thereof, One or more of gamma-aminopropylmethyldimethoxysilane, gamma-aminopropylmethyldiethoxysilane, vinyltriethoxysilane, vinyltrimethoxysilane, vinyltris (beta-methoxyethoxy) silane, silica powder or silica sol; gamma-aminopropyltriethoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma- (2, 3-glycidoxy) propyltrimethoxysilane are preferred. Preferably, the mixture of tetramethoxysilane, methyltrimethoxysilane and gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane, silicon dioxide powder or silicon dioxide sol is prepared from the following components in a mass ratio of 2: 2: 1.
the molybdenum trioxide sol and the molybdenum disulfide sol refer to a nano aqueous dispersion of molybdenum trioxide or molybdenum disulfide, and the molybdenum trioxide sol is characterized in that the particle size of molybdenum trioxide is less than 200 nanometers, the solid content of the molybdenum trioxide sol is less than or equal to 45 percent, the molybdenum trioxide sol is a colorless transparent liquid, and the shape of the nano particles is spherical. The molybdenum disulfide is a flake nano dispersion liquid, the flake diameter is less than 200 nanometers, and the flake thickness is less than 50 nanometers. Molybdenum trioxide sols are preferred.
The mass ratio of the water to the stabilizer to the antimony trioxide to the silane coupling agent is 3-8: 0.05-0.2: 1: 0.02 to 0.15. Wherein the mass ratio of the sodium bisulfate to the solid content of the water-based resin is 1: 0.1 to 10. In the preparation process, sodium bisulfate needs to be dissolved to 10-18 percent, a high-concentration solution is not suitable, otherwise, the solution obtained in the step (1) is milky turbid. The aqueous resin addition time was complete before the addition of the sodium bisulfate solution. Before adding, the pH value of the aqueous resin needs to be tested and adjusted to be 5-8, the pH value of an acidic aqueous resin solution does not need to be regulated, and an organic or inorganic acid aqueous solution needs to be used for adjusting an alkaline aqueous resin solution to be 5-8.
The molar ratio of the hydrogen peroxide to the antimony trioxide in the hydrogen peroxide is less than 2, preferably 1.60-1.99. Excessive hydrogen peroxide can cause hydrogen peroxide residue in reaction products, and the residual hydrogen peroxide can affect the preparation of the water-based paint and cause the occurrence of poor coating.
The pH regulator comprises an alkali metal or alkaline earth metal hydroxide, preferably sodium hydroxide or potassium hydroxide, or a mixture thereof.
One or two of the molybdenum trioxide sol and the molybdenum disulfide sol. The mass ratio of the total mass of the solids contained in the molybdenum trioxide or molybdenum disulfide sol to the total mass of the solids of the antimony oxide sol prepared in the step (1) is 0.05-0.2, and the preferred mass ratio is 0.1.
And (3) concentrating the liquid in the step (3), wherein the concentration temperature is 75-105 ℃. Distillation under atmospheric or reduced pressure, preferably reduced pressure.
The flame-retardant auxiliary agent prepared by the invention has the following characteristics:
the product is a transparent white aqueous solution, is easy to add into a water-based paint, can be added in a large amount, has excellent flame retardant property, and reduces the harm to the environment due to the smoke suppressant. The product has excellent stability, can be stored and transported for a long time, and the obtained coating does not crack, has flat and smooth surface and crystal-clear and transparent appearance. The solution contains particles with the particle size less than 200 nanometers, so the solution has strong permeability to base materials and good permeability to wood or artificial boards, and the product is particularly suitable for floor flame retardance.
The invention is described in detail below by way of examples, which are intended to be within the scope of the claims. It should be noted that the following examples are only intended to illustrate the present invention and should not be construed as limiting the scope of the present invention, and that some insubstantial modifications and adaptations made in accordance with the present invention are still within the scope of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples.
The raw materials or chemical reagents used in the examples of the present invention are commercially available unless otherwise specified.
Example 1
The main raw materials are as follows: hydrogen peroxide (hydrogen peroxide content 30.0%), polyvinyl alcohol 1799 type diluent (solid content 15.0%), antimony trioxide (content 99.5%), methyltrimethoxysilane (purity 99.0%), sodium bisulfate (15.0%), molybdenum trioxide sol (solid content 18.5%), sodium hydroxide (solid content 15.0%).
The preparation method comprises the following steps: adding 800L of water into a reaction kettle, adding 8.7 g of sodium bisulfate, dropwise adding 12.5 g of methyltrimethoxysilane under stirring at room temperature, stirring for 30 minutes, adding 35.1 g of polyvinyl alcohol solution, adding 180.2 g of antimony trioxide, heating to 75 ℃, dropwise adding 126.6 g of hydrogen peroxide, and continuing stirring for 1 hour after the solution is transparent; 32.5 g of sodium hydroxide solution is dropwise added, 120.9 g of self-made molybdenum trioxide solution is added, the measured solid content is 18.7%, the temperature is continuously raised to 95 ℃, the solution is distilled and concentrated to the required concentration, and the heating is stopped.
Example 2
The main raw materials are as follows: hydrogen peroxide (hydrogen peroxide content 30.0%), vinyl chloride-vinyl acetate copolymer emulsion (solid content 35.0%), antimony trioxide (content 99.5%), methyltrimethoxysilane and tetramethoxysilane (mass ratio 1: 1), molybdenum disulfide sol (solid content 26.0%) and sodium hydroxide solution (solid content 15.0%).
The preparation method comprises the following steps: adding 1500L of water into a reaction kettle, dropwise adding 32.5 g of a mixture of methyltrimethoxysilane and tetramethoxysilane under stirring at room temperature, stirring for 30 minutes, adding 25.3 g of polyvinyl chloride-vinyl acetate emulsion, adding 350.1 g of antimony trioxide, heating to 85 ℃, dropwise adding 245.8 g of hydrogen peroxide, and continuously stirring for 1.5 hours after the solution is transparent; and (3) dropwise adding 41.8 g of sodium hydroxide solution, adding 199.5 g of self-made molybdenum disulfide solution, actually measuring the solid content to be 20.4%, continuously heating to 95 ℃, concentrating the distilled excessive water to the required concentration, and stopping heating to finish the preparation.
Example 3
The main raw materials are as follows: hydrogen peroxide (hydrogen peroxide content 50.0%), potassium bisulfate (solid content 10.0%), aqueous brominated polyurethane and aqueous organic silicon modified acrylic acid mixed emulsion (self-made, solid content 35.0%), antimony trioxide (solid content 99.5%) and molybdenum disulfide sol (solid content 26.0%).
The preparation method comprises the following steps: adding 450.0 g of water into a reaction kettle, dropwise adding 14.5 g of potassium hydrogen sulfate while stirring at room temperature, stirring for 30 minutes, adding 45.3 g of aqueous brominated polyurethane and aqueous organic silicon modified acrylic acid mixed emulsion, adding 120.0 g of antimony trioxide, heating to 85 ℃, dropwise adding 72.0 g of hydrogen peroxide, and continuously stirring for 1 hour after the solution is transparent; adding 34.5 g of self-made molybdenum disulfide solution, actually measuring the solid content to be 21.5%, continuously heating to 100 ℃, concentrating the distilled excessive water to the required concentration, stopping heating, and finishing the preparation.
Claims (8)
1. The synthesis method of the antimony oxide sol and the flame retardant additive are characterized by comprising the following three steps of: uniformly dispersing water, a sol stabilizer, antimony trioxide, a modifier and the like, dropwise adding hydrogen peroxide, and heating the mixture to 70-95 ℃ to obtain an antimony oxide-containing mixture; adding a pH regulator, and adding one or two of molybdenum trioxide sol and molybdenum disulfide sol; and (3) concentrating to the required concentration.
2. The method for synthesizing antimony oxide sol and the flame retardant additive according to claim 1, wherein the method comprises the following steps: in the step (1), the sol stabilizer is one or a mixture of bisulfate and organic resin, and the modifier is a silane coupling agent; the molar ratio of the hydrogen peroxide to the antimony trioxide in the hydrogen peroxide is less than 2, and the preferred molar ratio is 1.60-1.99; the heating temperature is 70-95 ℃, and the reaction time is 2-6 hours.
3. The preparation method according to claim 2, wherein the modifier comprises one or more organic or inorganic agents containing silicon; which comprises tetramethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, tetraethoxysilane, methyltrimethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, propyltrimethoxysilane, dimethyldimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, gamma- (2, 3-glycidoxy) propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, N-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane, N-beta- (aminoethyl) -gamma-aminopropylmethyldimethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, tetraethoxysilane, methyltrimethoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, ethyltrimethoxysilane, propyltrimethoxysilane, dimethyldimethoxysilane, dimethyldimethoxy, One or more of gamma-aminopropylmethyldiethoxysilane, vinyltriethoxysilane, vinyltrimethoxysilane, vinyltris (beta-methoxyethoxy) silane, silica powder or silica sol; one or more of gamma-aminopropyltriethoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma- (2, 3-glycidoxy) propyltrimethoxysilane, silica powder or silica sol is preferably used.
4. The preparation method according to claim 2, wherein the sol stabilizer is one or more of hydrogen sulfate and organic resin, and the hydrogen sulfate is preferably sodium hydrogen sulfate; the organic resin can be dispersed in water, and comprises one or more of water-based halogen-free or halogen-containing saturated polyester, water-based halogen-free or halogen-containing unsaturated polyester, water-based halogen-free or halogen-containing polyurethane, water-based halogen-free or halogen-containing epoxy resin, water-based halogen-free or halogen-containing acrylic resin, water-based halogen-free or halogen-containing polyolefin resin, polyethylene glycol, polyvinylpyrrolidone, polyethylene oxide, polylactic acid and polyvinyl alcohol; the organic resin is capable of aqueous dispersion and has the following characteristics: the resin is soluble in water or a mixed solvent of water and alcohol; or the resin can be dissolved in an organic solvent, and the resulting solution can be dispersed in water with added surfactant to form a water-soluble emulsion.
5. The preparation method of claim 2, wherein the mass ratio of the water, the stabilizer, the antimony trioxide and the silane coupling agent is 3-8: 0.05-0.2: 1: 0.02 to 0.15; wherein the mass ratio of the sodium bisulfate to the solid content of the water-based resin is 1: 0.1 to 10.
6. The method for synthesizing a sol of antimony oxide and preparing a flame retardant aid according to claim 1, wherein the method comprises the following steps: adding one or two of molybdenum trioxide sol and molybdenum disulfide sol in the step (2), wherein the diameter of the nano particles in the sol is less than 200 nanometers, and the molybdenum trioxide sol is preferably selected; a PH adjusting agent comprising an alkali or alkaline earth metal hydroxide, preferably sodium hydroxide or potassium hydroxide.
7. The method for synthesizing a sol of antimony oxide and preparing a flame retardant aid according to claim 1, wherein the method comprises the following steps: firstly, dripping a PH regulator, and then adding one or two of molybdenum trioxide sol and molybdenum disulfide sol; the mass ratio of the total mass of the solids contained in the molybdenum trioxide or molybdenum disulfide sol to the total mass of the solids of the antimony oxide sol prepared in the step (1) is 0.05-0.2, and the preferred mass ratio is 0.1.
8. The method for synthesizing a sol of antimony oxide and preparing a flame retardant aid according to claim 1, wherein the method comprises the following steps: the concentration temperature of the liquid in the step (3) is 75-105 ℃; distillation under atmospheric or reduced pressure, preferably reduced pressure.
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Application publication date: 20201009 |