CN117304767B - Fireproof coating and preparation method thereof - Google Patents
Fireproof coating and preparation method thereof Download PDFInfo
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- CN117304767B CN117304767B CN202310834673.6A CN202310834673A CN117304767B CN 117304767 B CN117304767 B CN 117304767B CN 202310834673 A CN202310834673 A CN 202310834673A CN 117304767 B CN117304767 B CN 117304767B
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- 238000000576 coating method Methods 0.000 title claims abstract description 102
- 239000011248 coating agent Substances 0.000 title claims abstract description 99
- 238000002360 preparation method Methods 0.000 title claims abstract description 62
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 152
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 81
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 78
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 76
- 239000011787 zinc oxide Substances 0.000 claims abstract description 76
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 74
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 73
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 72
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 72
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 44
- 239000003822 epoxy resin Substances 0.000 claims abstract description 42
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 42
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 41
- BQPNUOYXSVUVMY-UHFFFAOYSA-N [4-[2-(4-diphenoxyphosphoryloxyphenyl)propan-2-yl]phenyl] diphenyl phosphate Chemical compound C=1C=C(OP(=O)(OC=2C=CC=CC=2)OC=2C=CC=CC=2)C=CC=1C(C)(C)C(C=C1)=CC=C1OP(=O)(OC=1C=CC=CC=1)OC1=CC=CC=C1 BQPNUOYXSVUVMY-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000002994 raw material Substances 0.000 claims abstract description 22
- KMRIWYPVRWEWRG-UHFFFAOYSA-N 2-(6-oxobenzo[c][2,1]benzoxaphosphinin-6-yl)benzene-1,4-diol Chemical compound OC1=CC=C(O)C(P2(=O)C3=CC=CC=C3C3=CC=CC=C3O2)=C1 KMRIWYPVRWEWRG-UHFFFAOYSA-N 0.000 claims abstract 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 105
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 80
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 79
- 239000011777 magnesium Substances 0.000 claims description 75
- 229910052742 iron Inorganic materials 0.000 claims description 73
- 229910052802 copper Inorganic materials 0.000 claims description 69
- 239000010949 copper Substances 0.000 claims description 69
- 239000003063 flame retardant Substances 0.000 claims description 64
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 60
- 239000006185 dispersion Substances 0.000 claims description 55
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 38
- 238000003756 stirring Methods 0.000 claims description 38
- 239000008367 deionised water Substances 0.000 claims description 35
- 229910021641 deionized water Inorganic materials 0.000 claims description 35
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 30
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 20
- 239000007822 coupling agent Substances 0.000 claims description 20
- 229910052725 zinc Inorganic materials 0.000 claims description 20
- 239000011701 zinc Substances 0.000 claims description 20
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 19
- 239000011975 tartaric acid Substances 0.000 claims description 19
- 235000002906 tartaric acid Nutrition 0.000 claims description 19
- MBNRBJNIYVXSQV-UHFFFAOYSA-N 3-[diethoxy(methyl)silyl]propane-1-thiol Chemical compound CCO[Si](C)(OCC)CCCS MBNRBJNIYVXSQV-UHFFFAOYSA-N 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 17
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 claims description 15
- 229940009827 aluminum acetate Drugs 0.000 claims description 15
- YQMWDQQWGKVOSQ-UHFFFAOYSA-N trinitrooxystannyl nitrate Chemical compound [Sn+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YQMWDQQWGKVOSQ-UHFFFAOYSA-N 0.000 claims description 15
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 14
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 claims description 14
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 14
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 14
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 6
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 6
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 6
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 239000002270 dispersing agent Substances 0.000 claims description 5
- 239000003381 stabilizer Substances 0.000 claims description 5
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 4
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 3
- NGCDGPPKVSZGRR-UHFFFAOYSA-J 1,4,6,9-tetraoxa-5-stannaspiro[4.4]nonane-2,3,7,8-tetrone Chemical compound [Sn+4].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O NGCDGPPKVSZGRR-UHFFFAOYSA-J 0.000 claims description 3
- IKYAJDOSWUATPI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propane-1-thiol Chemical compound CO[Si](C)(OC)CCCS IKYAJDOSWUATPI-UHFFFAOYSA-N 0.000 claims description 3
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 3
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 3
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 3
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 3
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 3
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 3
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 claims description 3
- 239000011654 magnesium acetate Substances 0.000 claims description 3
- 235000011285 magnesium acetate Nutrition 0.000 claims description 3
- 229940069446 magnesium acetate Drugs 0.000 claims description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 3
- 229940078494 nickel acetate Drugs 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- YJGJRYWNNHUESM-UHFFFAOYSA-J triacetyloxystannyl acetate Chemical compound [Sn+4].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O YJGJRYWNNHUESM-UHFFFAOYSA-J 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000004246 zinc acetate Substances 0.000 claims description 3
- 239000011592 zinc chloride Substances 0.000 claims description 3
- 235000005074 zinc chloride Nutrition 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims 2
- 238000001291 vacuum drying Methods 0.000 claims 2
- -1 2, 5-dihydroxyphenyl Chemical group 0.000 abstract description 3
- 229920006334 epoxy coating Polymers 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 16
- 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 description 12
- 229910000861 Mg alloy Inorganic materials 0.000 description 7
- 239000000654 additive Substances 0.000 description 6
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000004593 Epoxy Substances 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 230000003993 interaction Effects 0.000 description 4
- 125000002524 organometallic group Chemical group 0.000 description 4
- 239000002861 polymer material Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000013530 defoamer Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000012796 inorganic flame retardant Substances 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 229920002379 silicone rubber Polymers 0.000 description 2
- 239000004945 silicone rubber Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical group CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 1
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 1
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical group CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229960003237 betaine Drugs 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000006255 coating slurry Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000013329 compounding 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
- 230000007547 defect Effects 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical class 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
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229920003063 hydroxymethyl cellulose Polymers 0.000 description 1
- 229940031574 hydroxymethyl cellulose Drugs 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003348 petrochemical agent Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 229910001954 samarium oxide Inorganic materials 0.000 description 1
- 229940075630 samarium oxide Drugs 0.000 description 1
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002023 wood 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
Description
技术领域Technical Field
本发明属于涂料技术领域。更具体地，涉及一种防火涂料及其制备方法。The present invention belongs to the technical field of coatings, and more specifically, relates to a fire retardant coating and a preparation method thereof.
背景技术Background Art
当今人类社会快速发展的基础离不开各种材料，但随着越来越快的工业进步，天然资源已经跟不上发展的脚步，而高分子材料应运而生，填补了这个空缺。高分子材料凭借高强度，耐腐蚀，轻便，易加工等诸多优点。高分子材料可以分为热塑性塑料和热固性塑料。环氧树脂作为热固性塑料的一种，具备多种优点，如机械强度优异，介电性能良好，粘结性能好和成型条件宽泛且简单等，普遍应用于粘结剂，电子器件，石油化工，军工航天等各种领域。The rapid development of human society today is inseparable from various materials. However, with the increasingly rapid industrial progress, natural resources have been unable to keep up with the pace of development, and polymer materials have emerged to fill this gap. Polymer materials have many advantages such as high strength, corrosion resistance, lightness, and easy processing. Polymer materials can be divided into thermoplastics and thermosetting plastics. Epoxy resin, as a kind of thermosetting plastic, has many advantages, such as excellent mechanical strength, good dielectric properties, good bonding properties, and wide and simple molding conditions. It is widely used in various fields such as adhesives, electronic devices, petrochemicals, military and aerospace.
CN116285665A公开了一种镁合金用膨胀型陶瓷化防火涂层材料及其制备方法和应用。该涂层包括有机成膜剂、无机粉料、有机阻燃剂粉料、碳化硅纤维和其他助剂，无机粉料包括无机阻燃剂、陶瓷微球和膨胀石墨；其中，有机硅橡胶、碳化硅纤维、陶瓷微球和膨胀石墨的质量比为(30-50):(1-5):(0.5-2):(10-30)。该涂层材料应用于在镁合金表面得到膨胀型阻燃涂层，具体包括以下步骤：将镁合金基体表面喷砂处理得到具有粗糙度的表面；洗净、干燥后，将涂层浆料均匀喷涂在镁合金表面，并进行固化；硅橡胶固化交联反应完全后，待有机溶剂完全挥发，在镁合金表面得到膨胀型阻燃涂层。与现有技术相比，本发明具有提升镁合金耐高温能力、热稳定性、抗随机振动性能，带本发明涂层镁合金可在1200℃长期使用。CN116285665A discloses an intumescent ceramic fire-retardant coating material for magnesium alloys, and its preparation method and application. The coating comprises an organic film-forming agent, an inorganic powder, an organic flame retardant powder, silicon carbide fiber and other additives, wherein the inorganic powder comprises an inorganic flame retardant, ceramic microspheres and expanded graphite; wherein the mass ratio of organic silicone rubber, silicon carbide fiber, ceramic microspheres and expanded graphite is (30-50):(1-5):(0.5-2):(10-30). The coating material is used to obtain an intumescent flame-retardant coating on the surface of a magnesium alloy, and specifically comprises the following steps: sandblasting the surface of a magnesium alloy substrate to obtain a surface with a roughness; after washing and drying, spraying the coating slurry uniformly on the surface of the magnesium alloy and curing it; after the curing and cross-linking reaction of the silicone rubber is complete, the organic solvent is completely volatilized to obtain an intumescent flame-retardant coating on the surface of the magnesium alloy. Compared with the prior art, the present invention has the advantages of improving the high temperature resistance, thermal stability and random vibration resistance of the magnesium alloy, and the magnesium alloy with the coating of the present invention can be used for a long time at 1200°C.
CN116285581A公开了一种新型树枝状有机金属基环氧膨胀防火涂层的制备，其制备方法包括以下步骤：(1)DPANI/PA@Cu有机金属阻燃剂的制备；(2)新型树枝状有机金属基环氧膨胀防火涂层的制备；本发明中结合DPANI优异的自成炭能力、PA阻燃剂的气相阻燃作用以及Cu2+离子催化成炭的综合作用，制备出一种具有高性能、生态化的有机金属基环氧膨胀防火涂层(DPANI/PA@Cu基环氧膨胀防火涂层)；在涂层样品燃烧期间，5％DPANI/PA@Cu的样品表现出最低的背面温度(174.9℃)，最大的膨胀高度(18.5mm)和膨胀率(14.57％)，表明其最优异的隔热性能。CN116285581A discloses the preparation of a novel dendritic organometallic epoxy intumescent fireproof coating, and the preparation method thereof comprises the following steps: (1) preparation of DPANI/PA@Cu organometallic flame retardant; (2) preparation of a novel dendritic organometallic epoxy intumescent fireproof coating; in the present invention, the excellent self-carbonizing ability of DPANI, the gas phase flame retardant effect of PA flame retardant and the comprehensive effect of Cu2 + ion catalysis carbonization are combined to prepare a high-performance and ecological organometallic epoxy intumescent fireproof coating (DPANI/PA@Cu-based epoxy intumescent fireproof coating); during the combustion of the coating sample, the 5% DPANI/PA@Cu sample exhibited the lowest back surface temperature (174.9°C), the largest expansion height (18.5mm) and the expansion rate (14.57%), indicating its best thermal insulation performance.
CN116004095A公开了一种防火涂层及其制备方法和应用。按重量份计，所述防火涂层的原料包括：环氧树脂55-75份；硅烷改性的负载有铜和镍的蒙脱土4～10份；氧化钐1～3份；镧和钴共掺杂的硫化钼2～6份；六苯氧基环三磷腈3～7份；偶联剂3～6份；填料6～14份；助剂1～5份与水24～32份。本发明的防火涂层，利于组分之间的相互作用可以显著改善防火涂层的附着力，阻燃性能，具有优异的应用前景。CN116004095A discloses a fireproof coating and its preparation method and application. The raw materials of the fireproof coating include, by weight: 55-75 parts of epoxy resin; 4-10 parts of silane-modified montmorillonite loaded with copper and nickel; 1-3 parts of samarium oxide; 2-6 parts of molybdenum sulfide co-doped with lanthanum and cobalt; 3-7 parts of hexaphenoxy cyclotriphosphazene; 3-6 parts of coupling agent; 6-14 parts of filler; 1-5 parts of auxiliary agent and 24-32 parts of water. The fireproof coating of the present invention is conducive to the interaction between the components, can significantly improve the adhesion and flame retardant properties of the fireproof coating, and has excellent application prospects.
CN116285438A公开了一种硅铝型水性防火涂层及其制备方法，属于防火涂料技术领域。本发明的硅铝型水性防火涂层由50～60份硅铝溶胶、30～60份玻璃粉、5～50份耐火材料混合而成，其中还添加了少量成膜剂，制得的硅铝型水性防火涂料涂覆于基体表面，经干燥后即可得到硅铝型水性防火涂层。本发明所制备的硅铝型水性防火涂层，当暴露在火焰中时，可以形成完整的具有内部多孔结构的耐热、不燃陶瓷保护层，具有隔热屏蔽作用，能够阻止质量和热量的传递，使易燃的木材、聚氨酯泡沫等能够快速自熄，并维持基体材料的力学和物理性能，最终起到保护基体材料的作用。CN116285438A discloses a silicon-aluminum water-based fireproof coating and a preparation method thereof, belonging to the technical field of fireproof coatings. The silicon-aluminum water-based fireproof coating of the present invention is mixed with 50-60 parts of silicon-aluminum sol, 30-60 parts of glass powder, and 5-50 parts of refractory materials, wherein a small amount of film-forming agent is also added, and the prepared silicon-aluminum water-based fireproof coating is applied to the surface of the substrate, and the silicon-aluminum water-based fireproof coating can be obtained after drying. The silicon-aluminum water-based fireproof coating prepared by the present invention, when exposed to flames, can form a complete heat-resistant, non-combustible ceramic protective layer with an internal porous structure, has a heat-insulating shielding effect, can prevent the transfer of mass and heat, and enable flammable wood, polyurethane foam, etc. to quickly self-extinguish, and maintain the mechanical and physical properties of the substrate material, and finally play a role in protecting the substrate material.
通过现有技术的了解，通过将高分子有机材料与有机阻燃剂以及无机阻燃剂进行复合来改善高分子材料的阻燃性能，但是现有技术中的产品，因阻燃性能差或者力学性能差而不能满足实际生产的需求。According to the prior art, the flame retardant properties of polymer materials can be improved by compounding polymer organic materials with organic flame retardants and inorganic flame retardants. However, the products in the prior art cannot meet the needs of actual production due to poor flame retardant properties or poor mechanical properties.
发明内容Summary of the invention
本发明要解决的技术问题是克服现有技术中存在的缺陷和不足，提供一种防火涂料及其制备方法。所述防火涂层的原料包括：环氧树脂E4460-80份、Mg、Fe和Al共掺杂的氧化锌2～4份；Ni、Cu和Ce共掺杂氧化锡4～8份；双酚A-双(二苯基磷酸酯)(BDP)2～6份、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)3～7份，硅烷偶联剂4～10份、助剂3～7份与水35～45份。本发明制备的防火涂料具有优异的力学性能和防火性能，具有优异的应用前景。The technical problem to be solved by the present invention is to overcome the defects and shortcomings in the prior art, and provide a fire retardant coating and a preparation method thereof. The raw materials of the fire retardant coating include: 60-80 parts of epoxy resin E44, 2 to 4 parts of zinc oxide co-doped with Mg, Fe and Al; 4 to 8 parts of tin oxide co-doped with Ni, Cu and Ce; 2 to 6 parts of bisphenol A-bis(diphenyl phosphate) (BDP), 3 to 7 parts of 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), 4 to 10 parts of silane coupling agent, 3 to 7 parts of auxiliary agent and 35 to 45 parts of water. The fire retardant coating prepared by the present invention has excellent mechanical properties and fire retardant properties, and has excellent application prospects.
本发明的目的是提供一种防火涂料。The purpose of the present invention is to provide a fire retardant coating.
本发明另一目的是提供一种防火涂料的制备方法。Another object of the present invention is to provide a method for preparing a fire retardant coating.
本发明上述目的通过以下技术方案实现：The above-mentioned purpose of the present invention is achieved through the following technical solutions:
1.一种防火涂料，按重量份计，所述防火涂层的原料包括：环氧树脂60-80份、Mg、Fe和Al共掺杂的氧化锌2～4份；Ni、Cu和Ce共掺杂氧化锡4～8份；双酚A-双(二苯基磷酸酯)(BDP)2～6份、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)3～7份，硅烷偶联剂4～10份、助剂3～7份与水35～45份。1. A fire retardant coating, wherein the raw materials of the fire retardant coating include, by weight: 60-80 parts of epoxy resin, 2-4 parts of zinc oxide co-doped with Mg, Fe and Al; 4-8 parts of tin oxide co-doped with Ni, Cu and Ce; 2-6 parts of bisphenol A-bis(diphenyl phosphate) (BDP), 3-7 parts of 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), 4-10 parts of silane coupling agent, 3-7 parts of auxiliary agent and 35-45 parts of water.
优选的，所述Mg、Fe和Al共掺杂的氧化锌的制备方法包括以下步骤：Preferably, the method for preparing the Mg, Fe and Al co-doped zinc oxide comprises the following steps:
将镁源、铁源、铝源、柠檬酸和锌源超声分散到去离子水中得到分散液，然后采用浓度为4～6mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为10～12，然后转移到反应釜中进行水热反应，水热反应条件为140～180℃反应10～14h，过滤、洗涤、于60～80℃真空干燥8～12h，然后进行焙烧，所述焙烧条件为400～600℃焙烧2～4h，得到Mg、Fe和Al共掺杂的氧化锌。A magnesium source, an iron source, an aluminum source, citric acid and a zinc source are ultrasonically dispersed in deionized water to obtain a dispersion, and then a sodium hydroxide solution with a concentration of 4 to 6 mol/L is slowly added dropwise to the dispersion to adjust the pH value of the solution to 10 to 12, and then the dispersion is transferred to a reactor for a hydrothermal reaction at 140 to 180° C. for 10 to 14 hours, filtered, washed, and vacuum dried at 60 to 80° C. for 8 to 12 hours, and then calcined at 400 to 600° C. for 2 to 4 hours to obtain zinc oxide co-doped with Mg, Fe and Al.
优选的，所述镁源为硝酸镁、氯化镁和醋酸镁中的至少一种；所述铁源为硝酸铁、氯化铁和醋酸铁中的至少一种；所述铝源为硝酸铝、氯化铝和醋酸铝中的至少一种；所述锌源为硝酸锌、氯化锌和醋酸锌中的至少一种。Preferably, the magnesium source is at least one of magnesium nitrate, magnesium chloride and magnesium acetate; the iron source is at least one of ferric nitrate, ferric chloride and ferric acetate; the aluminum source is at least one of aluminum nitrate, aluminum chloride and aluminum acetate; the zinc source is at least one of zinc nitrate, zinc chloride and zinc acetate.
优选的，所述镁源、铁源、铝源、柠檬酸和锌源的摩尔比为：0.01～0.03:0.02～0.04:0.015～0.025：0.4～0.6：1。Preferably, the molar ratio of the magnesium source, iron source, aluminum source, citric acid and zinc source is: 0.01-0.03:0.02-0.04:0.015-0.025:0.4-0.6:1.
优选的，所述Ni、Cu和Ce共掺杂氧化锡的制备方法包括以下步骤：Preferably, the method for preparing Ni, Cu and Ce co-doped tin oxide comprises the following steps:
将镍源、铜源、铈源、酒石酸和锡源超声分散到去离子水中，然后采用浓度为2～4mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为9～11，然后转移到反应釜中进行水热反应，水热反应条件为120～140℃反应10～20h，过滤、洗涤、于60～80℃真空干燥8～12h，然后进行焙烧，所述焙烧条件为400～600℃焙烧1～3h，得到Ni、Cu和Ce共掺杂的氧化锡。A nickel source, a copper source, a cerium source, tartaric acid and a tin source are ultrasonically dispersed in deionized water, and then a sodium hydroxide solution with a concentration of 2 to 4 mol/L is slowly added dropwise to the dispersion, and the pH value of the solution is adjusted to 9 to 11, and then the solution is transferred to a reactor for a hydrothermal reaction under the conditions of 120 to 140° C. for 10 to 20 hours, filtered, washed, and vacuum dried at 60 to 80° C. for 8 to 12 hours, and then calcined under the conditions of 400 to 600° C. for 1 to 3 hours to obtain Ni, Cu and Ce co-doped tin oxide.
优选的，所述镍源为硝酸镍、氯化镍和醋酸镍中的至少一种；所述铜源为硝酸铜、氯化铜和醋酸铜中的至少一种；所述铈源为硝酸铈、氯化铈和醋酸铈中的至少一种；所述锡源为硝酸锡、草酸锡、醋酸锡中的至少一种。Preferably, the nickel source is at least one of nickel nitrate, nickel chloride and nickel acetate; the copper source is at least one of copper nitrate, copper chloride and copper acetate; the cerium source is at least one of cerium nitrate, cerium chloride and cerium acetate; the tin source is at least one of tin nitrate, tin oxalate and tin acetate.
优选的，所述镍源、铜源、铈源、酒石酸和锡源的摩尔比为：0.005～0.015:0.015～0.025:0.02～0.04:0.2～0.6:1。Preferably, the molar ratio of the nickel source, copper source, cerium source, tartaric acid and tin source is: 0.005-0.015:0.015-0.025:0.02-0.04:0.2-0.6:1.
优选的，所述偶联剂为γ-巯丙基三甲氧基硅烷、γ-巯丙基甲基二乙氧基硅烷、γ-巯丙基甲基二甲氧基硅烷中的至少一种。Preferably, the coupling agent is at least one of γ-mercaptopropyltrimethoxysilane, γ-mercaptopropylmethyldiethoxysilane and γ-mercaptopropylmethyldimethoxysilane.
优选的，所述的助剂为分散剂、膜助剂、消泡剂、pH稳定剂、流平剂与防沉剂。Preferably, the auxiliary agent is a dispersant, a membrane auxiliary agent, a defoaming agent, a pH stabilizer, a leveling agent and an anti-settling agent.
基于上述所述的一种防火涂料的制备方法，所述防火涂料的制备方法包括以下步骤，先将环氧树脂、Mg、Fe和Al共掺杂的氧化锌；Ni、Cu和Ce共掺杂氧化锡；双酚A-双(二苯基磷酸酯)(BDP)、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)，硅烷偶联剂与水放入高速搅拌机中混合，搅拌速率为2000～4000r/min，搅拌40～60min，然后将助剂添加到上述混合物中继续搅拌30～50min，得到环氧涂料。Based on the above-mentioned method for preparing a fire-retardant coating, the method for preparing the fire-retardant coating comprises the following steps: firstly, epoxy resin, zinc oxide co-doped with Mg, Fe and Al; tin oxide co-doped with Ni, Cu and Ce; bisphenol A-bis(diphenyl phosphate) (BDP), 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), silane coupling agent and water are put into a high-speed stirrer and mixed at a stirring rate of 2000 to 4000 r/min for 40 to 60 minutes, and then an additive is added to the above mixture and stirring is continued for 30 to 50 minutes to obtain an epoxy coating.
本发明具有以下有益效果：The present invention has the following beneficial effects:
(1)通过Mn、Fe和Al共掺杂氧化锌，利用掺杂组分的相互作用，来改善涂料的防火等性能；(1) By co-doping zinc oxide with Mn, Fe and Al, the interaction between the doped components is used to improve the fire retardant properties of the coating;
(2)通过Ni、Cu和Ce共掺杂氧化锡，利用掺杂组分的相互作用，来改善涂料的防火等性能；(2) Co-doping tin oxide with Ni, Cu and Ce and utilizing the interaction of the doped components to improve the fire retardant properties of the coating;
(3)通过掺杂的氧化锌、掺杂的氧化锡以及BDP和ODOPB的相互作用来改善涂料的防火性能，同时通过添加硅烷偶联剂来改善无机组分的分散性。(3) The fire retardant properties of the coating are improved by the interaction of doped zinc oxide, doped tin oxide, and BDP and ODOPB, while the dispersibility of the inorganic components is improved by adding a silane coupling agent.
(4)本发明的制备的涂层具有优异的力学和防火等性能。(4) The coating prepared by the present invention has excellent mechanical and fire retardant properties.
具体实施方式DETAILED DESCRIPTION
以下结合具体实施例来进一步说明本发明，但实施例并不对本发明做任何形式的限定。除非特别说明，本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。The present invention is further described below with reference to specific examples, but the examples do not limit the present invention in any form. Unless otherwise specified, the reagents, methods and equipment used in the present invention are conventional reagents, methods and equipment in the art.
除非特别说明，以下实施例所用试剂和材料均为市购。Unless otherwise specified, the reagents and materials used in the following examples are commercially available.
本发明中实施例与对比例中所采用的助剂均为分散剂、膜助剂、消泡剂、pH稳定剂、流平剂与防沉剂；所述分散剂为十八烷基二甲基甜菜碱；膜助剂为三甲基戊乙醇单异丁酸酯；消泡剂为FoamStar A34；pH稳定剂为AMP-95、流平剂为乙二醇单丁醚；防沉剂为羟甲基纤维素，可从市场购得；在本发明中，分散剂、膜助剂、消泡剂、pH稳定剂、流平剂与防沉剂的质量相同。The additives used in the embodiments and comparative examples of the present invention are all dispersants, film additives, defoamers, pH stabilizers, leveling agents and anti-settling agents; the dispersant is octadecyl dimethyl betaine; the film additive is trimethylpentyl ethanol monoisobutyrate; the defoamer is FoamStar A34; the pH stabilizer is AMP-95, and the leveling agent is ethylene glycol monobutyl ether; the anti-settling agent is hydroxymethyl cellulose, which can be purchased from the market; in the present invention, the dispersant, film additive, defoamer, pH stabilizer, leveling agent and anti-settling agent have the same quality.
实施例1Example 1
一种防火涂料，按重量份计，所述防火涂层的原料包括：环氧树脂E4470份、Mg、Fe和Al共掺杂的氧化锌3份；Ni、Cu和Ce共掺杂氧化锡6份；双酚A-双(二苯基磷酸酯)(BDP)4份、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)5份，硅烷偶联剂7份、助剂5份与水40份。A fireproof coating, wherein the raw materials of the fireproof coating include, by weight: 70 parts of epoxy resin E44, 3 parts of zinc oxide co-doped with Mg, Fe and Al; 6 parts of tin oxide co-doped with Ni, Cu and Ce; 4 parts of bisphenol A-bis(diphenyl phosphate) (BDP), 5 parts of 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), 7 parts of silane coupling agent, 5 parts of auxiliary agent and 40 parts of water.
所述Mg、Fe和Al共掺杂的氧化锌的制备方法包括以下步骤：The preparation method of the Mg, Fe and Al co-doped zinc oxide comprises the following steps:
将0.02mol硝酸镁、0.03mol氯化铁、0.02mol醋酸铝、0.5mol柠檬酸和1mol锌源超声分散到200mL去离子水中得到分散液，然后采用浓度为5mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为11，然后转移到反应釜中进行水热反应，水热反应条件为160℃反应12h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧3h，得到Mg、Fe和Al共掺杂的氧化锌。0.02 mol of magnesium nitrate, 0.03 mol of ferric chloride, 0.02 mol of aluminum acetate, 0.5 mol of citric acid and 1 mol of zinc source are ultrasonically dispersed in 200 mL of deionized water to obtain a dispersion, and then a sodium hydroxide solution with a concentration of 5 mol/L is slowly added dropwise to the dispersion, the pH value of the solution is adjusted to 11, and then the solution is transferred to a reactor for a hydrothermal reaction at 160° C. for 12 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 3 h to obtain Mg, Fe and Al co-doped zinc oxide.
所述Ni、Cu和Ce共掺杂氧化锡的制备方法包括以下步骤：The preparation method of Ni, Cu and Ce co-doped tin oxide comprises the following steps:
将0.01mol硝酸镍、0.02mol氯化铜、0.03mol醋酸铈、0.4mol酒石酸和1mol硝酸锡超声分散到200mL去离子水中，然后采用浓度为3mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为10，然后转移到反应釜中进行水热反应，水热反应条件为130℃反应15h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧2h，得到Ni、Cu和Ce共掺杂的氧化锡。0.01 mol nickel nitrate, 0.02 mol copper chloride, 0.03 mol cerium acetate, 0.4 mol tartaric acid and 1 mol tin nitrate were ultrasonically dispersed in 200 mL deionized water, and then a 3 mol/L sodium hydroxide solution was slowly added dropwise to the dispersion, the pH value of the solution was adjusted to 10, and then the solution was transferred to a reactor for hydrothermal reaction at 130° C. for 15 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 2 h to obtain Ni, Cu and Ce co-doped tin oxide.
所述偶联剂为γ-巯丙基甲基二乙氧基硅烷；The coupling agent is γ-mercaptopropylmethyldiethoxysilane;
所述防火涂料的制备方法包括以下步骤，先将环氧树脂E44、Mg、Fe和Al共掺杂的氧化锌；Ni、Cu和Ce共掺杂氧化锡；双酚A-双(二苯基磷酸酯)(BDP)、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)，硅烷偶联剂与水放入高速搅拌机中混合，搅拌速率为3000r/min，搅拌50min，然后将助剂添加到上述混合物中继续搅拌40min，得到环氧涂料。The preparation method of the fire retardant coating comprises the following steps: firstly, epoxy resin E44, zinc oxide co-doped with Mg, Fe and Al; tin oxide co-doped with Ni, Cu and Ce; bisphenol A-bis(diphenyl phosphate) (BDP), 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), silane coupling agent and water are put into a high-speed stirrer for mixing at a stirring rate of 3000 r/min for 50 minutes, and then an auxiliary agent is added to the mixture and the stirring is continued for 40 minutes to obtain the epoxy coating.
实施例2Example 2
一种防火涂料，按重量份计，所述防火涂层的原料包括：环氧树脂E4480份、Mg、Fe和Al共掺杂的氧化锌2份；Ni、Cu和Ce共掺杂氧化锡8份；双酚A-双(二苯基磷酸酯)(BDP)2份、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)7份，硅烷偶联剂4份、助剂7份与水45份。A fireproof coating, wherein the raw materials of the fireproof coating include, by weight: 80 parts of epoxy resin E44, 2 parts of zinc oxide co-doped with Mg, Fe and Al; 8 parts of tin oxide co-doped with Ni, Cu and Ce; 2 parts of bisphenol A-bis(diphenyl phosphate) (BDP), 7 parts of 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), 4 parts of silane coupling agent, 7 parts of auxiliary agent and 45 parts of water.
所述Mg、Fe和Al共掺杂的氧化锌的制备方法包括以下步骤：The preparation method of the Mg, Fe and Al co-doped zinc oxide comprises the following steps:
将0.03mol氯化镁、0.02mol醋酸铁、0.025mol硝酸铝、0.4mol柠檬酸和1mol氯化锌超声分散到200mL去离子水中得到分散液，然后采用浓度为6mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为12，然后转移到反应釜中进行水热反应，水热反应条件为180℃反应10h，过滤、洗涤、于80℃真空干燥8h，然后进行焙烧，所述焙烧条件为600℃焙烧2h，得到Mg、Fe和Al共掺杂的氧化锌；0.03 mol of magnesium chloride, 0.02 mol of ferric acetate, 0.025 mol of aluminum nitrate, 0.4 mol of citric acid and 1 mol of zinc chloride are ultrasonically dispersed in 200 mL of deionized water to obtain a dispersion, and then a sodium hydroxide solution with a concentration of 6 mol/L is slowly added dropwise to the dispersion to adjust the pH value of the solution to 12, and then transferred to a reactor for hydrothermal reaction, the hydrothermal reaction conditions are 180° C. for 10 h, filtered, washed, vacuum dried at 80° C. for 8 h, and then calcined, the calcination conditions are 600° C. for 2 h, to obtain Mg, Fe and Al co-doped zinc oxide;
所述Ni、Cu和Ce共掺杂氧化锡的制备方法包括以下步骤：The preparation method of Ni, Cu and Ce co-doped tin oxide comprises the following steps:
将0.015mol氯化镍、0.015mol醋酸铜、0.04mol硝酸铈、0.2mol酒石酸和1mol草酸锡超声分散到200mL去离子水中，然后采用浓度为4mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为11，然后转移到反应釜中进行水热反应，水热反应条件为140℃反应10h，过滤、洗涤、于80℃真空干燥8h，然后进行焙烧，所述焙烧条件为600℃焙烧1h，得到Ni、Cu和Ce共掺杂的氧化锡。0.015 mol of nickel chloride, 0.015 mol of copper acetate, 0.04 mol of cerium nitrate, 0.2 mol of tartaric acid and 1 mol of tin oxalate were ultrasonically dispersed in 200 mL of deionized water, and then a sodium hydroxide solution with a concentration of 4 mol/L was slowly added dropwise to the dispersion, and the pH value of the solution was adjusted to 11. The solution was then transferred to a reactor for a hydrothermal reaction at 140° C. for 10 h, filtered, washed, and vacuum dried at 80° C. for 8 h, and then calcined at 600° C. for 1 h to obtain Ni, Cu and Ce co-doped tin oxide.
所述偶联剂为γ-巯丙基三甲氧基硅烷；The coupling agent is γ-mercaptopropyltrimethoxysilane;
所述防火涂料的制备方法包括以下步骤，先将环氧树脂E44、Mg、Fe和Al共掺杂的氧化锌；Ni、Cu和Ce共掺杂氧化锡；双酚A-双(二苯基磷酸酯)(BDP)、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)，硅烷偶联剂与水放入高速搅拌机中混合，搅拌速率为4000r/min，搅拌40min，然后将助剂添加到上述混合物中继续搅拌30min，得到环氧涂料。The preparation method of the fire retardant coating comprises the following steps: firstly, epoxy resin E44, zinc oxide co-doped with Mg, Fe and Al; tin oxide co-doped with Ni, Cu and Ce; bisphenol A-bis(diphenyl phosphate) (BDP), 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), silane coupling agent and water are put into a high-speed stirrer for mixing at a stirring rate of 4000 r/min for 40 minutes, and then an auxiliary agent is added to the above mixture and the stirring is continued for 30 minutes to obtain the epoxy coating.
实施例3Example 3
一种防火涂料，按重量份计，所述防火涂层的原料包括：环氧树脂E4460份、Mg、Fe和Al共掺杂的氧化锌4份；Ni、Cu和Ce共掺杂氧化锡4份；双酚A-双(二苯基磷酸酯)(BDP)6份、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)3份，硅烷偶联剂10份、助剂3份与水35份。A fireproof coating, wherein the raw materials of the fireproof coating include, by weight: 60 parts of epoxy resin E44, 4 parts of zinc oxide co-doped with Mg, Fe and Al; 4 parts of tin oxide co-doped with Ni, Cu and Ce; 6 parts of bisphenol A-bis(diphenyl phosphate) (BDP), 3 parts of 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), 10 parts of silane coupling agent, 3 parts of auxiliary agent and 35 parts of water.
所述Mg、Fe和Al共掺杂的氧化锌的制备方法包括以下步骤：The preparation method of the Mg, Fe and Al co-doped zinc oxide comprises the following steps:
将0.01mol醋酸镁、0.04mol硝酸铁、0.015mol氯化铝、0.6mol柠檬酸和1mol醋酸锌超声分散到200mL去离子水中得到分散液，然后采用浓度为4mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为10，然后转移到反应釜中进行水热反应，水热反应条件为140℃反应14h，过滤、洗涤、于60℃真空干燥12h，然后进行焙烧，所述焙烧条件为400℃焙烧4h，得到Mg、Fe和Al共掺杂的氧化锌。0.01 mol of magnesium acetate, 0.04 mol of ferric nitrate, 0.015 mol of aluminum chloride, 0.6 mol of citric acid and 1 mol of zinc acetate are ultrasonically dispersed in 200 mL of deionized water to obtain a dispersion, and then a sodium hydroxide solution with a concentration of 4 mol/L is slowly added dropwise to the dispersion, the pH value of the solution is adjusted to 10, and then the solution is transferred to a reactor for a hydrothermal reaction at 140° C. for 14 hours, filtered, washed, and vacuum dried at 60° C. for 12 hours, and then calcined at 400° C. for 4 hours to obtain Mg, Fe and Al co-doped zinc oxide.
所述Ni、Cu和Ce共掺杂氧化锡的制备方法包括以下步骤：The preparation method of Ni, Cu and Ce co-doped tin oxide comprises the following steps:
将0.005mol醋酸镍、0.025mol硝酸铜、0.02mol氯化铈、0.6mol酒石酸和1mol醋酸锡超声分散到200mL去离子水中，然后采用浓度为2mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为9，然后转移到反应釜中进行水热反应，水热反应条件为120℃反应20h，过滤、洗涤、于60℃真空干燥12h，然后进行焙烧，所述焙烧条件为400℃焙烧3h，得到Ni、Cu和Ce共掺杂的氧化锡。0.005 mol of nickel acetate, 0.025 mol of copper nitrate, 0.02 mol of cerium chloride, 0.6 mol of tartaric acid and 1 mol of tin acetate were ultrasonically dispersed in 200 mL of deionized water, and then a 2 mol/L sodium hydroxide solution was slowly added dropwise to the dispersion, the pH value of the solution was adjusted to 9, and then the solution was transferred to a reactor for a hydrothermal reaction at 120° C. for 20 h, filtered, washed, and vacuum dried at 60° C. for 12 h, and then calcined at 400° C. for 3 h to obtain Ni, Cu and Ce co-doped tin oxide.
所述偶联剂为γ-巯丙基甲基二甲氧基硅烷；The coupling agent is γ-mercaptopropylmethyldimethoxysilane;
所述防火涂料的制备方法包括以下步骤，先将环氧树脂E44、Mg、Fe和Al共掺杂的氧化锌；Ni、Cu和Ce共掺杂氧化锡；双酚A-双(二苯基磷酸酯)(BDP)、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)，硅烷偶联剂与水放入高速搅拌机中混合，搅拌速率为2000r/min，搅拌60min，然后将助剂添加到上述混合物中继续搅拌50min，得到环氧涂料。The preparation method of the fire retardant coating comprises the following steps: firstly, epoxy resin E44, zinc oxide co-doped with Mg, Fe and Al; tin oxide co-doped with Ni, Cu and Ce; bisphenol A-bis(diphenyl phosphate) (BDP), 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), silane coupling agent and water are put into a high-speed stirrer for mixing at a stirring rate of 2000 r/min for 60 minutes, and then an auxiliary agent is added to the above mixture and the stirring is continued for 50 minutes to obtain the epoxy coating.
对比例1Comparative Example 1
一种防火涂料，按重量份计，所述防火涂层的原料包括：环氧树脂E4470份、Mg和Al共掺杂的氧化锌3份；Ni、Cu和Ce共掺杂氧化锡6份；双酚A-双(二苯基磷酸酯)(BDP)4份、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)5份，硅烷偶联剂7份、助剂5份与水40份。A fireproof coating, wherein the raw materials of the fireproof coating include, by weight: 70 parts of epoxy resin E44, 3 parts of zinc oxide co-doped with Mg and Al, 6 parts of tin oxide co-doped with Ni, Cu and Ce, 4 parts of bisphenol A-bis(diphenyl phosphate) (BDP), 5 parts of 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), 7 parts of silane coupling agent, 5 parts of auxiliary agent and 40 parts of water.
所述Mg和Al共掺杂的氧化锌的制备方法包括以下步骤：The preparation method of the Mg and Al co-doped zinc oxide comprises the following steps:
将0.05mol硝酸镁、0.02mol醋酸铝、0.5mol柠檬酸和1mol锌源超声分散到200mL去离子水中得到分散液，然后采用浓度为5mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为11，然后转移到反应釜中进行水热反应，水热反应条件为160℃反应12h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧3h，得到Mg和Al共掺杂的氧化锌。0.05 mol of magnesium nitrate, 0.02 mol of aluminum acetate, 0.5 mol of citric acid and 1 mol of zinc source are ultrasonically dispersed in 200 mL of deionized water to obtain a dispersion, and then a sodium hydroxide solution with a concentration of 5 mol/L is slowly added dropwise to the dispersion, the pH value of the solution is adjusted to 11, and then the solution is transferred to a reactor for a hydrothermal reaction at 160° C. for 12 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 3 h to obtain Mg and Al co-doped zinc oxide.
所述Ni、Cu和Ce共掺杂氧化锡的制备方法包括以下步骤：The preparation method of Ni, Cu and Ce co-doped tin oxide comprises the following steps:
将0.01mol硝酸镍、0.02mol氯化铜、0.03mol醋酸铈、0.4mol酒石酸和1mol硝酸锡超声分散到200mL去离子水中，然后采用浓度为3mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为10，然后转移到反应釜中进行水热反应，水热反应条件为130℃反应15h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧2h，得到Ni、Cu和Ce共掺杂的氧化锡。0.01 mol nickel nitrate, 0.02 mol copper chloride, 0.03 mol cerium acetate, 0.4 mol tartaric acid and 1 mol tin nitrate were ultrasonically dispersed in 200 mL deionized water, and then a 3 mol/L sodium hydroxide solution was slowly added dropwise to the dispersion, the pH value of the solution was adjusted to 10, and then the solution was transferred to a reactor for hydrothermal reaction at 130° C. for 15 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 2 h to obtain Ni, Cu and Ce co-doped tin oxide.
所述偶联剂为γ-巯丙基甲基二乙氧基硅烷；The coupling agent is γ-mercaptopropylmethyldiethoxysilane;
所述防火涂料的制备方法包括以下步骤，先将环氧树脂E44、Mg和Al共掺杂的氧化锌；Ni、Cu和Ce共掺杂氧化锡；双酚A-双(二苯基磷酸酯)(BDP)、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)，硅烷偶联剂与水放入高速搅拌机中混合，搅拌速率为3000r/min，搅拌50min，然后将助剂添加到上述混合物中继续搅拌40min，得到环氧涂料。The preparation method of the fire retardant coating comprises the following steps: firstly, epoxy resin E44, zinc oxide co-doped with Mg and Al; tin oxide co-doped with Ni, Cu and Ce; bisphenol A-bis(diphenyl phosphate) (BDP), 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), a silane coupling agent and water are put into a high-speed stirrer for mixing at a stirring rate of 3000 r/min for 50 minutes, and then an auxiliary agent is added to the mixture and the stirring is continued for 40 minutes to obtain the epoxy coating.
对比例2Comparative Example 2
一种防火涂料，按重量份计，所述防火涂层的原料包括：环氧树脂E4470份、Fe和Al共掺杂的氧化锌3份；Ni、Cu和Ce共掺杂氧化锡6份；双酚A-双(二苯基磷酸酯)(BDP)4份、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)5份，硅烷偶联剂7份、助剂5份与水40份。A fireproof coating, wherein the raw materials of the fireproof coating include, by weight: 70 parts of epoxy resin E44, 3 parts of zinc oxide co-doped with Fe and Al, 6 parts of tin oxide co-doped with Ni, Cu and Ce, 4 parts of bisphenol A-bis(diphenyl phosphate) (BDP), 5 parts of 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), 7 parts of silane coupling agent, 5 parts of auxiliary agent and 40 parts of water.
所述Fe和Al共掺杂的氧化锌的制备方法包括以下步骤：The preparation method of the Fe and Al co-doped zinc oxide comprises the following steps:
将0.05mol氯化铁、0.02mol醋酸铝、0.5mol柠檬酸和1mol锌源超声分散到200mL去离子水中得到分散液，然后采用浓度为5mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为11，然后转移到反应釜中进行水热反应，水热反应条件为160℃反应12h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧3h，得到Fe和Al共掺杂的氧化锌。0.05 mol of ferric chloride, 0.02 mol of aluminum acetate, 0.5 mol of citric acid and 1 mol of zinc source are ultrasonically dispersed in 200 mL of deionized water to obtain a dispersion, and then a sodium hydroxide solution with a concentration of 5 mol/L is slowly added dropwise to the dispersion, the pH value of the solution is adjusted to 11, and then the solution is transferred to a reactor for a hydrothermal reaction at 160° C. for 12 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 3 h to obtain Fe and Al co-doped zinc oxide.
所述Ni、Cu和Ce共掺杂氧化锡的制备方法包括以下步骤：The preparation method of Ni, Cu and Ce co-doped tin oxide comprises the following steps:
将0.01mol硝酸镍、0.02mol氯化铜、0.03mol醋酸铈、0.4mol酒石酸和1mol硝酸锡超声分散到200mL去离子水中，然后采用浓度为3mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为10，然后转移到反应釜中进行水热反应，水热反应条件为130℃反应15h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧2h，得到Ni、Cu和Ce共掺杂的氧化锡。0.01 mol nickel nitrate, 0.02 mol copper chloride, 0.03 mol cerium acetate, 0.4 mol tartaric acid and 1 mol tin nitrate were ultrasonically dispersed in 200 mL deionized water, and then a 3 mol/L sodium hydroxide solution was slowly added dropwise to the dispersion, the pH value of the solution was adjusted to 10, and then the solution was transferred to a reactor for hydrothermal reaction at 130° C. for 15 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 2 h to obtain Ni, Cu and Ce co-doped tin oxide.
所述偶联剂为γ-巯丙基甲基二乙氧基硅烷；The coupling agent is γ-mercaptopropylmethyldiethoxysilane;
所述防火涂料的制备方法包括以下步骤，先将环氧树脂E44、Fe和Al共掺杂的氧化锌；Ni、Cu和Ce共掺杂氧化锡；双酚A-双(二苯基磷酸酯)(BDP)、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)，硅烷偶联剂与水放入高速搅拌机中混合，搅拌速率为3000r/min，搅拌50min，然后将助剂添加到上述混合物中继续搅拌40min，得到环氧涂料。The preparation method of the fire retardant coating comprises the following steps: firstly, epoxy resin E44, zinc oxide co-doped with Fe and Al; tin oxide co-doped with Ni, Cu and Ce; bisphenol A-bis(diphenyl phosphate) (BDP), 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), a silane coupling agent and water are put into a high-speed stirrer for mixing at a stirring rate of 3000 r/min for 50 minutes, and then an auxiliary agent is added to the mixture and the stirring is continued for 40 minutes to obtain the epoxy coating.
对比例3Comparative Example 3
一种防火涂料，按重量份计，所述防火涂层的原料包括：环氧树脂E4470份、Mg和Fe共掺杂的氧化锌3份；Ni、Cu和Ce共掺杂氧化锡6份；双酚A-双(二苯基磷酸酯)(BDP)4份、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)5份，硅烷偶联剂7份、助剂5份与水40份。A fireproof coating, wherein the raw materials of the fireproof coating include, by weight: 70 parts of epoxy resin E44, 3 parts of zinc oxide co-doped with Mg and Fe, 6 parts of tin oxide co-doped with Ni, Cu and Ce, 4 parts of bisphenol A-bis(diphenyl phosphate) (BDP), 5 parts of 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), 7 parts of silane coupling agent, 5 parts of auxiliary agent and 40 parts of water.
所述Mg、Fe和Al共掺杂的氧化锌的制备方法包括以下步骤：The preparation method of the Mg, Fe and Al co-doped zinc oxide comprises the following steps:
将0.02mol硝酸镁、0.05mol氯化铁、0.5mol柠檬酸和1mol锌源超声分散到200mL去离子水中得到分散液，然后采用浓度为5mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为11，然后转移到反应釜中进行水热反应，水热反应条件为160℃反应12h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧3h，得到Mg和Fe共掺杂的氧化锌。0.02 mol of magnesium nitrate, 0.05 mol of ferric chloride, 0.5 mol of citric acid and 1 mol of zinc source are ultrasonically dispersed in 200 mL of deionized water to obtain a dispersion, and then a sodium hydroxide solution with a concentration of 5 mol/L is slowly added dropwise to the dispersion, the pH value of the solution is adjusted to 11, and then the solution is transferred to a reactor for a hydrothermal reaction at 160° C. for 12 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 3 h to obtain Mg and Fe co-doped zinc oxide.
所述Ni、Cu和Ce共掺杂氧化锡的制备方法包括以下步骤：The preparation method of Ni, Cu and Ce co-doped tin oxide comprises the following steps:
将0.01mol硝酸镍、0.02mol氯化铜、0.03mol醋酸铈、0.4mol酒石酸和1mol硝酸锡超声分散到200mL去离子水中，然后采用浓度为3mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为10，然后转移到反应釜中进行水热反应，水热反应条件为130℃反应15h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧2h，得到Ni、Cu和Ce共掺杂的氧化锡。0.01 mol nickel nitrate, 0.02 mol copper chloride, 0.03 mol cerium acetate, 0.4 mol tartaric acid and 1 mol tin nitrate were ultrasonically dispersed in 200 mL deionized water, and then a 3 mol/L sodium hydroxide solution was slowly added dropwise to the dispersion, the pH value of the solution was adjusted to 10, and then the solution was transferred to a reactor for hydrothermal reaction at 130° C. for 15 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 2 h to obtain Ni, Cu and Ce co-doped tin oxide.
所述偶联剂为γ-巯丙基甲基二乙氧基硅烷；The coupling agent is γ-mercaptopropylmethyldiethoxysilane;
所述防火涂料的制备方法包括以下步骤，先将环氧树脂E44、Mg和Fe共掺杂的氧化锌；Ni、Cu和Ce共掺杂氧化锡；双酚A-双(二苯基磷酸酯)(BDP)、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)，硅烷偶联剂与水放入高速搅拌机中混合，搅拌速率为3000r/min，搅拌50min，然后将助剂添加到上述混合物中继续搅拌40min，得到环氧涂料。The preparation method of the fire retardant coating comprises the following steps: firstly, epoxy resin E44, zinc oxide co-doped with Mg and Fe; tin oxide co-doped with Ni, Cu and Ce; bisphenol A-bis(diphenyl phosphate) (BDP), 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), a silane coupling agent and water are put into a high-speed stirrer for mixing at a stirring rate of 3000 r/min for 50 minutes, and then an auxiliary agent is added to the mixture and the stirring is continued for 40 minutes to obtain the epoxy coating.
对比例4Comparative Example 4
一种防火涂料，按重量份计，所述防火涂层的原料包括：环氧树脂E4470份、Mg和Al共掺杂的氧化锌3份；Ni、Cu和Ce共掺杂氧化锡6份；双酚A-双(二苯基磷酸酯)(BDP)4份、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)5份，硅烷偶联剂7份、助剂5份与水40份。A fireproof coating, wherein the raw materials of the fireproof coating include, by weight: 70 parts of epoxy resin E44, 3 parts of zinc oxide co-doped with Mg and Al, 6 parts of tin oxide co-doped with Ni, Cu and Ce, 4 parts of bisphenol A-bis(diphenyl phosphate) (BDP), 5 parts of 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), 7 parts of silane coupling agent, 5 parts of auxiliary agent and 40 parts of water.
所述Mg、Fe和Al共掺杂的氧化锌的制备方法包括以下步骤：The preparation method of the Mg, Fe and Al co-doped zinc oxide comprises the following steps:
将0.02mol硝酸镁、0.05mol醋酸铝、0.5mol柠檬酸和1mol锌源超声分散到200mL去离子水中得到分散液，然后采用浓度为5mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为11，然后转移到反应釜中进行水热反应，水热反应条件为160℃反应12h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧3h，得到Mg和Al共掺杂的氧化锌。0.02 mol of magnesium nitrate, 0.05 mol of aluminum acetate, 0.5 mol of citric acid and 1 mol of zinc source are ultrasonically dispersed in 200 mL of deionized water to obtain a dispersion, and then a sodium hydroxide solution with a concentration of 5 mol/L is slowly added dropwise to the dispersion, the pH value of the solution is adjusted to 11, and then the solution is transferred to a reactor for a hydrothermal reaction at 160° C. for 12 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 3 h to obtain Mg and Al co-doped zinc oxide.
所述Ni、Cu和Ce共掺杂氧化锡的制备方法包括以下步骤：The preparation method of Ni, Cu and Ce co-doped tin oxide comprises the following steps:
将0.01mol硝酸镍、0.02mol氯化铜、0.03mol醋酸铈、0.4mol酒石酸和1mol硝酸锡超声分散到200mL去离子水中，然后采用浓度为3mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为10，然后转移到反应釜中进行水热反应，水热反应条件为130℃反应15h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧2h，得到Ni、Cu和Ce共掺杂的氧化锡。0.01 mol nickel nitrate, 0.02 mol copper chloride, 0.03 mol cerium acetate, 0.4 mol tartaric acid and 1 mol tin nitrate were ultrasonically dispersed in 200 mL deionized water, and then a 3 mol/L sodium hydroxide solution was slowly added dropwise to the dispersion, the pH value of the solution was adjusted to 10, and then the solution was transferred to a reactor for hydrothermal reaction at 130° C. for 15 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 2 h to obtain Ni, Cu and Ce co-doped tin oxide.
所述偶联剂为γ-巯丙基甲基二乙氧基硅烷；The coupling agent is γ-mercaptopropylmethyldiethoxysilane;
所述防火涂料的制备方法包括以下步骤，先将环氧树脂E44、Mg和Al共掺杂的氧化锌；Ni、Cu和Ce共掺杂氧化锡；双酚A-双(二苯基磷酸酯)(BDP)、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)，硅烷偶联剂与水放入高速搅拌机中混合，搅拌速率为3000r/min，搅拌50min，然后将助剂添加到上述混合物中继续搅拌40min，得到环氧涂料。The preparation method of the fire retardant coating comprises the following steps: firstly, epoxy resin E44, zinc oxide co-doped with Mg and Al; tin oxide co-doped with Ni, Cu and Ce; bisphenol A-bis(diphenyl phosphate) (BDP), 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), a silane coupling agent and water are put into a high-speed stirrer for mixing at a stirring rate of 3000 r/min for 50 minutes, and then an auxiliary agent is added to the mixture and the stirring is continued for 40 minutes to obtain the epoxy coating.
对比例5Comparative Example 5
一种防火涂料，按重量份计，所述防火涂层的原料包括：环氧树脂E4470份、Mg、Fe和Al共掺杂的氧化锌3份；Ni和Ce共掺杂氧化锡6份；双酚A-双(二苯基磷酸酯)(BDP)4份、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)5份，硅烷偶联剂7份、助剂5份与水40份。A fireproof coating, wherein the raw materials of the fireproof coating include, by weight: 70 parts of epoxy resin E44, 3 parts of zinc oxide co-doped with Mg, Fe and Al; 6 parts of tin oxide co-doped with Ni and Ce; 4 parts of bisphenol A-bis(diphenyl phosphate) (BDP), 5 parts of 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), 7 parts of silane coupling agent, 5 parts of auxiliary agent and 40 parts of water.
所述Mg、Fe和Al共掺杂的氧化锌的制备方法包括以下步骤：The preparation method of the Mg, Fe and Al co-doped zinc oxide comprises the following steps:
将0.02mol硝酸镁、0.03mol氯化铁、0.02mol醋酸铝、0.5mol柠檬酸和1mol锌源超声分散到200mL去离子水中得到分散液，然后采用浓度为5mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为11，然后转移到反应釜中进行水热反应，水热反应条件为160℃反应12h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧3h，得到Mg、Fe和Al共掺杂的氧化锌。0.02 mol of magnesium nitrate, 0.03 mol of ferric chloride, 0.02 mol of aluminum acetate, 0.5 mol of citric acid and 1 mol of zinc source are ultrasonically dispersed in 200 mL of deionized water to obtain a dispersion, and then a sodium hydroxide solution with a concentration of 5 mol/L is slowly added dropwise to the dispersion, the pH value of the solution is adjusted to 11, and then the solution is transferred to a reactor for a hydrothermal reaction at 160° C. for 12 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 3 h to obtain Mg, Fe and Al co-doped zinc oxide.
所述Ni和Ce共掺杂氧化锡的制备方法包括以下步骤：The preparation method of Ni and Ce co-doped tin oxide comprises the following steps:
将0.03mol硝酸镍、0.03mol醋酸铈、0.4mol酒石酸和1mol硝酸锡超声分散到200mL去离子水中，然后采用浓度为3mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为10，然后转移到反应釜中进行水热反应，水热反应条件为130℃反应15h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧2h，得到Ni和Ce共掺杂的氧化锡。0.03 mol of nickel nitrate, 0.03 mol of cerium acetate, 0.4 mol of tartaric acid and 1 mol of tin nitrate were ultrasonically dispersed in 200 mL of deionized water, and then a 3 mol/L sodium hydroxide solution was slowly added dropwise to the dispersion, the pH value of the solution was adjusted to 10, and then the solution was transferred to a reactor for a hydrothermal reaction at 130° C. for 15 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 2 h to obtain Ni and Ce co-doped tin oxide.
所述偶联剂为γ-巯丙基甲基二乙氧基硅烷；The coupling agent is γ-mercaptopropylmethyldiethoxysilane;
所述防火涂料的制备方法包括以下步骤，先将环氧树脂E44、Mg、Fe和Al共掺杂的氧化锌；Ni和Ce共掺杂氧化锡；双酚A-双(二苯基磷酸酯)(BDP)、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)，硅烷偶联剂与水放入高速搅拌机中混合，搅拌速率为3000r/min，搅拌50min，然后将助剂添加到上述混合物中继续搅拌40min，得到环氧涂料。The preparation method of the fire retardant coating comprises the following steps: firstly, epoxy resin E44, zinc oxide co-doped with Mg, Fe and Al; tin oxide co-doped with Ni and Ce; bisphenol A-bis(diphenyl phosphate) (BDP), 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), a silane coupling agent and water are put into a high-speed stirrer for mixing at a stirring rate of 3000 r/min for 50 minutes, and then an auxiliary agent is added to the above mixture and the stirring is continued for 40 minutes to obtain the epoxy coating.
对比例6Comparative Example 6
一种防火涂料，按重量份计，所述防火涂层的原料包括：环氧树脂E4470份、Mg、Fe和Al共掺杂的氧化锌3份；Cu和Ce共掺杂氧化锡6份；双酚A-双(二苯基磷酸酯)(BDP)4份、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)5份，硅烷偶联剂7份、助剂5份与水40份。A fireproof coating, wherein the raw materials of the fireproof coating include, by weight: 70 parts of epoxy resin E44, 3 parts of zinc oxide co-doped with Mg, Fe and Al; 6 parts of tin oxide co-doped with Cu and Ce; 4 parts of bisphenol A-bis(diphenyl phosphate) (BDP), 5 parts of 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), 7 parts of silane coupling agent, 5 parts of auxiliary agent and 40 parts of water.
所述Mg、Fe和Al共掺杂的氧化锌的制备方法包括以下步骤：The preparation method of the Mg, Fe and Al co-doped zinc oxide comprises the following steps:
将0.02mol硝酸镁、0.03mol氯化铁、0.02mol醋酸铝、0.5mol柠檬酸和1mol锌源超声分散到200mL去离子水中得到分散液，然后采用浓度为5mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为11，然后转移到反应釜中进行水热反应，水热反应条件为160℃反应12h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧3h，得到Mg、Fe和Al共掺杂的氧化锌。0.02 mol of magnesium nitrate, 0.03 mol of ferric chloride, 0.02 mol of aluminum acetate, 0.5 mol of citric acid and 1 mol of zinc source are ultrasonically dispersed in 200 mL of deionized water to obtain a dispersion, and then a sodium hydroxide solution with a concentration of 5 mol/L is slowly added dropwise to the dispersion, the pH value of the solution is adjusted to 11, and then the solution is transferred to a reactor for a hydrothermal reaction at 160° C. for 12 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 3 h to obtain Mg, Fe and Al co-doped zinc oxide.
所述Cu和Ce共掺杂氧化锡的制备方法包括以下步骤：The preparation method of Cu and Ce co-doped tin oxide comprises the following steps:
将0.03mol氯化铜、0.03mol醋酸铈、0.4mol酒石酸和1mol硝酸锡超声分散到200mL去离子水中，然后采用浓度为3mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为10，然后转移到反应釜中进行水热反应，水热反应条件为130℃反应15h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧2h，得到Cu和Ce共掺杂的氧化锡。0.03 mol of copper chloride, 0.03 mol of cerium acetate, 0.4 mol of tartaric acid and 1 mol of tin nitrate were ultrasonically dispersed in 200 mL of deionized water, and then a 3 mol/L sodium hydroxide solution was slowly added dropwise to the dispersion, the pH value of the solution was adjusted to 10, and then the solution was transferred to a reactor for a hydrothermal reaction at 130° C. for 15 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 2 h to obtain Cu and Ce co-doped tin oxide.
所述偶联剂为γ-巯丙基甲基二乙氧基硅烷；The coupling agent is γ-mercaptopropylmethyldiethoxysilane;
所述防火涂料的制备方法包括以下步骤，先将环氧树脂E44、Mg、Fe和Al共掺杂的氧化锌；Cu和Ce共掺杂氧化锡；双酚A-双(二苯基磷酸酯)(BDP)、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)，硅烷偶联剂与水放入高速搅拌机中混合，搅拌速率为3000r/min，搅拌50min，然后将助剂添加到上述混合物中继续搅拌40min，得到环氧涂料。The preparation method of the fire retardant coating comprises the following steps: firstly, epoxy resin E44, zinc oxide co-doped with Mg, Fe and Al; tin oxide co-doped with Cu and Ce; bisphenol A-bis(diphenyl phosphate) (BDP), 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), a silane coupling agent and water are put into a high-speed stirrer for mixing at a stirring rate of 3000 r/min for 50 minutes, and then an auxiliary agent is added to the above mixture and the stirring is continued for 40 minutes to obtain the epoxy coating.
对比例7Comparative Example 7
一种防火涂料，按重量份计，所述防火涂层的原料包括：环氧树脂E4470份、Mg、Fe和Al共掺杂的氧化锌3份；Ni和Cu共掺杂氧化锡6份；双酚A-双(二苯基磷酸酯)(BDP)4份、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)5份，硅烷偶联剂7份、助剂5份与水40份。A fireproof coating, wherein the raw materials of the fireproof coating include, by weight: 70 parts of epoxy resin E44, 3 parts of zinc oxide co-doped with Mg, Fe and Al; 6 parts of tin oxide co-doped with Ni and Cu; 4 parts of bisphenol A-bis(diphenyl phosphate) (BDP), 5 parts of 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), 7 parts of silane coupling agent, 5 parts of auxiliary agent and 40 parts of water.
所述Mg、Fe和Al共掺杂的氧化锌的制备方法包括以下步骤：The preparation method of the Mg, Fe and Al co-doped zinc oxide comprises the following steps:
将0.02mol硝酸镁、0.03mol氯化铁、0.02mol醋酸铝、0.5mol柠檬酸和1mol锌源超声分散到200mL去离子水中得到分散液，然后采用浓度为5mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为11，然后转移到反应釜中进行水热反应，水热反应条件为160℃反应12h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧3h，得到Mg、Fe和Al共掺杂的氧化锌。0.02 mol of magnesium nitrate, 0.03 mol of ferric chloride, 0.02 mol of aluminum acetate, 0.5 mol of citric acid and 1 mol of zinc source are ultrasonically dispersed in 200 mL of deionized water to obtain a dispersion, and then a sodium hydroxide solution with a concentration of 5 mol/L is slowly added dropwise to the dispersion, the pH value of the solution is adjusted to 11, and then the solution is transferred to a reactor for a hydrothermal reaction at 160° C. for 12 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 3 h to obtain Mg, Fe and Al co-doped zinc oxide.
所述Ni和Cu共掺杂氧化锡的制备方法包括以下步骤：The preparation method of Ni and Cu co-doped tin oxide comprises the following steps:
将0.01mol硝酸镍、0.05mol氯化铜、0.4mol酒石酸和1mol硝酸锡超声分散到200mL去离子水中，然后采用浓度为3mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为10，然后转移到反应釜中进行水热反应，水热反应条件为130℃反应15h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧2h，得到Ni和Cu共掺杂的氧化锡。0.01 mol nickel nitrate, 0.05 mol copper chloride, 0.4 mol tartaric acid and 1 mol tin nitrate were ultrasonically dispersed in 200 mL deionized water, and then a 3 mol/L sodium hydroxide solution was slowly added dropwise to the dispersion, the pH value of the solution was adjusted to 10, and then the solution was transferred to a reactor for hydrothermal reaction at 130° C. for 15 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 2 h to obtain Ni and Cu co-doped tin oxide.
所述偶联剂为γ-巯丙基甲基二乙氧基硅烷；The coupling agent is γ-mercaptopropylmethyldiethoxysilane;
所述防火涂料的制备方法包括以下步骤，先将环氧树脂E44、Mg、Fe和Al共掺杂的氧化锌；Ni和Cu共掺杂氧化锡；双酚A-双(二苯基磷酸酯)(BDP)、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)，硅烷偶联剂与水放入高速搅拌机中混合，搅拌速率为3000r/min，搅拌50min，然后将助剂添加到上述混合物中继续搅拌40min，得到环氧涂料。The preparation method of the fire retardant coating comprises the following steps: firstly, epoxy resin E44, zinc oxide co-doped with Mg, Fe and Al; tin oxide co-doped with Ni and Cu; bisphenol A-bis(diphenyl phosphate) (BDP), 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), a silane coupling agent and water are put into a high-speed stirrer for mixing at a stirring rate of 3000 r/min for 50 minutes, and then an auxiliary agent is added to the mixture and the stirring is continued for 40 minutes to obtain the epoxy coating.
对比例8Comparative Example 8
一种防火涂料，按重量份计，所述防火涂层的原料包括：环氧树脂E4470份、Mg、Fe和Al共掺杂的氧化锌3份；Ni和Ce共掺杂氧化锡6份；双酚A-双(二苯基磷酸酯)(BDP)4份、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)5份，硅烷偶联剂7份、助剂5份与水40份。A fireproof coating, wherein the raw materials of the fireproof coating include, by weight: 70 parts of epoxy resin E44, 3 parts of zinc oxide co-doped with Mg, Fe and Al; 6 parts of tin oxide co-doped with Ni and Ce; 4 parts of bisphenol A-bis(diphenyl phosphate) (BDP), 5 parts of 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), 7 parts of silane coupling agent, 5 parts of auxiliary agent and 40 parts of water.
所述Mg、Fe和Al共掺杂的氧化锌的制备方法包括以下步骤：The preparation method of the Mg, Fe and Al co-doped zinc oxide comprises the following steps:
将0.02mol硝酸镁、0.03mol氯化铁、0.02mol醋酸铝、0.5mol柠檬酸和1mol锌源超声分散到200mL去离子水中得到分散液，然后采用浓度为5mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为11，然后转移到反应釜中进行水热反应，水热反应条件为160℃反应12h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧3h，得到Mg、Fe和Al共掺杂的氧化锌。0.02 mol of magnesium nitrate, 0.03 mol of ferric chloride, 0.02 mol of aluminum acetate, 0.5 mol of citric acid and 1 mol of zinc source are ultrasonically dispersed in 200 mL of deionized water to obtain a dispersion, and then a sodium hydroxide solution with a concentration of 5 mol/L is slowly added dropwise to the dispersion, the pH value of the solution is adjusted to 11, and then the solution is transferred to a reactor for a hydrothermal reaction at 160° C. for 12 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 3 h to obtain Mg, Fe and Al co-doped zinc oxide.
所述Ni和Ce共掺杂氧化锡的制备方法包括以下步骤：The preparation method of Ni and Ce co-doped tin oxide comprises the following steps:
将0.01mol硝酸镍、0.05mol醋酸铈、0.4mol酒石酸和1mol硝酸锡超声分散到200mL去离子水中，然后采用浓度为3mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为10，然后转移到反应釜中进行水热反应，水热反应条件为130℃反应15h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧2h，得到Ni和Ce共掺杂的氧化锡。0.01 mol nickel nitrate, 0.05 mol cerium acetate, 0.4 mol tartaric acid and 1 mol tin nitrate were ultrasonically dispersed in 200 mL deionized water, and then a 3 mol/L sodium hydroxide solution was slowly added dropwise to the dispersion, the pH value of the solution was adjusted to 10, and then the solution was transferred to a reactor for hydrothermal reaction at 130° C. for 15 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 2 h to obtain Ni and Ce co-doped tin oxide.
所述偶联剂为γ-巯丙基甲基二乙氧基硅烷；The coupling agent is γ-mercaptopropylmethyldiethoxysilane;
所述防火涂料的制备方法包括以下步骤，先将环氧树脂E44、Mg、Fe和Al共掺杂的氧化锌；Ni和Ce共掺杂氧化锡；双酚A-双(二苯基磷酸酯)(BDP)、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)，硅烷偶联剂与水放入高速搅拌机中混合，搅拌速率为3000r/min，搅拌50min，然后将助剂添加到上述混合物中继续搅拌40min，得到环氧涂料。The preparation method of the fire retardant coating comprises the following steps: firstly, epoxy resin E44, zinc oxide co-doped with Mg, Fe and Al; tin oxide co-doped with Ni and Ce; bisphenol A-bis(diphenyl phosphate) (BDP), 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), a silane coupling agent and water are put into a high-speed stirrer for mixing at a stirring rate of 3000 r/min for 50 minutes, and then an auxiliary agent is added to the above mixture and the stirring is continued for 40 minutes to obtain the epoxy coating.
对比例9Comparative Example 9
一种防火涂料，按重量份计，所述防火涂层的原料包括：环氧树脂E4470份、Mg、Fe和Al共掺杂的氧化锌9份；双酚A-双(二苯基磷酸酯)(BDP)4份、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)5份，硅烷偶联剂7份、助剂5份与水40份。A fire retardant coating, wherein the raw materials of the fire retardant coating include, by weight: 70 parts of epoxy resin E44, 9 parts of zinc oxide co-doped with Mg, Fe and Al, 4 parts of bisphenol A-bis(diphenyl phosphate) (BDP), 5 parts of 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), 7 parts of silane coupling agent, 5 parts of auxiliary agent and 40 parts of water.
所述Mg、Fe和Al共掺杂的氧化锌的制备方法包括以下步骤：The preparation method of the Mg, Fe and Al co-doped zinc oxide comprises the following steps:
将0.02mol硝酸镁、0.03mol氯化铁、0.02mol醋酸铝、0.5mol柠檬酸和1mol锌源超声分散到200mL去离子水中得到分散液，然后采用浓度为5mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为11，然后转移到反应釜中进行水热反应，水热反应条件为160℃反应12h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧3h，得到Mg、Fe和Al共掺杂的氧化锌。0.02 mol of magnesium nitrate, 0.03 mol of ferric chloride, 0.02 mol of aluminum acetate, 0.5 mol of citric acid and 1 mol of zinc source are ultrasonically dispersed in 200 mL of deionized water to obtain a dispersion, and then a sodium hydroxide solution with a concentration of 5 mol/L is slowly added dropwise to the dispersion, the pH value of the solution is adjusted to 11, and then the solution is transferred to a reactor for a hydrothermal reaction at 160° C. for 12 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 3 h to obtain Mg, Fe and Al co-doped zinc oxide.
所述偶联剂为γ-巯丙基甲基二乙氧基硅烷；The coupling agent is γ-mercaptopropylmethyldiethoxysilane;
所述防火涂料的制备方法包括以下步骤，先将环氧树脂E44、Mg、Fe和Al共掺杂的氧化锌；双酚A-双(二苯基磷酸酯)(BDP)、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)，硅烷偶联剂与水放入高速搅拌机中混合，搅拌速率为3000r/min，搅拌50min，然后将助剂添加到上述混合物中继续搅拌40min，得到环氧涂料。The preparation method of the fire retardant coating comprises the following steps: firstly, epoxy resin E44, zinc oxide co-doped with Mg, Fe and Al, bisphenol A-bis(diphenyl phosphate) (BDP), 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), a silane coupling agent and water are put into a high-speed stirrer for mixing at a stirring rate of 3000 r/min for 50 minutes, and then an auxiliary agent is added to the mixture and the stirring is continued for 40 minutes to obtain the epoxy coating.
对比例10Comparative Example 10
一种防火涂料，按重量份计，所述防火涂层的原料包括：环氧树脂E4470份、Ni、Cu和Ce共掺杂氧化锡9份；双酚A-双(二苯基磷酸酯)(BDP)4份、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)5份，硅烷偶联剂7份、助剂5份与水40份。A fire retardant coating, wherein the raw materials of the fire retardant coating include, by weight: 70 parts of epoxy resin E44, 9 parts of tin oxide co-doped with Ni, Cu and Ce, 4 parts of bisphenol A-bis(diphenyl phosphate) (BDP), 5 parts of 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), 7 parts of silane coupling agent, 5 parts of auxiliary agent and 40 parts of water.
所述Ni、Cu和Ce共掺杂氧化锡的制备方法包括以下步骤：The preparation method of Ni, Cu and Ce co-doped tin oxide comprises the following steps:
将0.01mol硝酸镍、0.02mol氯化铜、0.03mol醋酸铈、0.4mol酒石酸和1mol硝酸锡超声分散到200mL去离子水中，然后采用浓度为3mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为10，然后转移到反应釜中进行水热反应，水热反应条件为130℃反应15h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧2h，得到Ni、Cu和Ce共掺杂的氧化锡。0.01 mol nickel nitrate, 0.02 mol copper chloride, 0.03 mol cerium acetate, 0.4 mol tartaric acid and 1 mol tin nitrate were ultrasonically dispersed in 200 mL deionized water, and then a 3 mol/L sodium hydroxide solution was slowly added dropwise to the dispersion, the pH value of the solution was adjusted to 10, and then the solution was transferred to a reactor for hydrothermal reaction at 130° C. for 15 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 2 h to obtain Ni, Cu and Ce co-doped tin oxide.
所述偶联剂为γ-巯丙基甲基二乙氧基硅烷；The coupling agent is γ-mercaptopropylmethyldiethoxysilane;
所述防火涂料的制备方法包括以下步骤，先将环氧树脂E44、Ni、Cu和Ce共掺杂氧化锡；双酚A-双(二苯基磷酸酯)(BDP)、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)，硅烷偶联剂与水放入高速搅拌机中混合，搅拌速率为3000r/min，搅拌50min，然后将助剂添加到上述混合物中继续搅拌40min，得到环氧涂料。The preparation method of the fire retardant coating comprises the following steps: firstly, epoxy resin E44, Ni, Cu and Ce are co-doped with tin oxide; bisphenol A-bis(diphenyl phosphate) (BDP), 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), a silane coupling agent and water are put into a high-speed stirrer for mixing at a stirring rate of 3000 r/min for 50 minutes; then, an auxiliary agent is added to the mixture and the stirring is continued for 40 minutes to obtain the epoxy coating.
对比例11Comparative Example 11
一种防火涂料，按重量份计，所述防火涂层的原料包括：环氧树脂E4470份、Mg、Fe和Al共掺杂的氧化锌3份；Ni、Cu和Ce共掺杂氧化锡10份；10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)5份，硅烷偶联剂7份、助剂5份与水40份。A fire retardant coating, wherein the raw materials of the fire retardant coating include, by weight: 70 parts of epoxy resin E44, 3 parts of zinc oxide co-doped with Mg, Fe and Al; 10 parts of tin oxide co-doped with Ni, Cu and Ce; 5 parts of 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), 7 parts of silane coupling agent, 5 parts of auxiliary agent and 40 parts of water.
所述Mg、Fe和Al共掺杂的氧化锌的制备方法包括以下步骤：The preparation method of the Mg, Fe and Al co-doped zinc oxide comprises the following steps:
将0.02mol硝酸镁、0.03mol氯化铁、0.02mol醋酸铝、0.5mol柠檬酸和1mol锌源超声分散到200mL去离子水中得到分散液，然后采用浓度为5mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为11，然后转移到反应釜中进行水热反应，水热反应条件为160℃反应12h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧3h，得到Mg、Fe和Al共掺杂的氧化锌。0.02 mol of magnesium nitrate, 0.03 mol of ferric chloride, 0.02 mol of aluminum acetate, 0.5 mol of citric acid and 1 mol of zinc source are ultrasonically dispersed in 200 mL of deionized water to obtain a dispersion, and then a sodium hydroxide solution with a concentration of 5 mol/L is slowly added dropwise to the dispersion, the pH value of the solution is adjusted to 11, and then the solution is transferred to a reactor for a hydrothermal reaction at 160° C. for 12 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 3 h to obtain Mg, Fe and Al co-doped zinc oxide.
所述Ni、Cu和Ce共掺杂氧化锡的制备方法包括以下步骤：The preparation method of Ni, Cu and Ce co-doped tin oxide comprises the following steps:
将0.01mol硝酸镍、0.02mol氯化铜、0.03mol醋酸铈、0.4mol酒石酸和1mol硝酸锡超声分散到200mL去离子水中，然后采用浓度为3mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为10，然后转移到反应釜中进行水热反应，水热反应条件为130℃反应15h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧2h，得到Ni、Cu和Ce共掺杂的氧化锡。0.01 mol nickel nitrate, 0.02 mol copper chloride, 0.03 mol cerium acetate, 0.4 mol tartaric acid and 1 mol tin nitrate were ultrasonically dispersed in 200 mL deionized water, and then a 3 mol/L sodium hydroxide solution was slowly added dropwise to the dispersion, the pH value of the solution was adjusted to 10, and then the solution was transferred to a reactor for hydrothermal reaction at 130° C. for 15 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 2 h to obtain Ni, Cu and Ce co-doped tin oxide.
所述偶联剂为γ-巯丙基甲基二乙氧基硅烷；The coupling agent is γ-mercaptopropylmethyldiethoxysilane;
所述防火涂料的制备方法包括以下步骤，先将环氧树脂E44、Mg、Fe和Al共掺杂的氧化锌；Ni、Cu和Ce共掺杂氧化锡；10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)，硅烷偶联剂与水放入高速搅拌机中混合，搅拌速率为3000r/min，搅拌50min，然后将助剂添加到上述混合物中继续搅拌40min，得到环氧涂料。The preparation method of the fire retardant coating comprises the following steps: firstly, epoxy resin E44, zinc oxide co-doped with Mg, Fe and Al; tin oxide co-doped with Ni, Cu and Ce; 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), a silane coupling agent and water are put into a high-speed stirrer for mixing at a stirring rate of 3000 r/min for 50 minutes, and then an auxiliary agent is added to the above mixture and the stirring is continued for 40 minutes to obtain the epoxy coating.
对比例12Comparative Example 12
一种防火涂料，按重量份计，所述防火涂层的原料包括：环氧树脂E4470份、Mg、Fe和Al共掺杂的氧化锌3份；双酚A-双(二苯基磷酸酯)(BDP)10份、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)5份，硅烷偶联剂7份、助剂5份与水40份。A fire retardant coating, wherein the raw materials of the fire retardant coating include, by weight: 70 parts of epoxy resin E44, 3 parts of zinc oxide co-doped with Mg, Fe and Al, 10 parts of bisphenol A-bis(diphenyl phosphate) (BDP), 5 parts of 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), 7 parts of silane coupling agent, 5 parts of auxiliary agent and 40 parts of water.
所述Mg、Fe和Al共掺杂的氧化锌的制备方法包括以下步骤：The preparation method of the Mg, Fe and Al co-doped zinc oxide comprises the following steps:
将0.02mol硝酸镁、0.03mol氯化铁、0.02mol醋酸铝、0.5mol柠檬酸和1mol锌源超声分散到200mL去离子水中得到分散液，然后采用浓度为5mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为11，然后转移到反应釜中进行水热反应，水热反应条件为160℃反应12h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧3h，得到Mg、Fe和Al共掺杂的氧化锌。0.02 mol of magnesium nitrate, 0.03 mol of ferric chloride, 0.02 mol of aluminum acetate, 0.5 mol of citric acid and 1 mol of zinc source are ultrasonically dispersed in 200 mL of deionized water to obtain a dispersion, and then a sodium hydroxide solution with a concentration of 5 mol/L is slowly added dropwise to the dispersion, the pH value of the solution is adjusted to 11, and then the solution is transferred to a reactor for a hydrothermal reaction at 160° C. for 12 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 3 h to obtain Mg, Fe and Al co-doped zinc oxide.
所述偶联剂为γ-巯丙基甲基二乙氧基硅烷；The coupling agent is γ-mercaptopropylmethyldiethoxysilane;
所述防火涂料的制备方法包括以下步骤，先将环氧树脂E44、Mg、Fe和Al共掺杂的氧化锌；双酚A-双(二苯基磷酸酯)(BDP)、10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)，硅烷偶联剂与水放入高速搅拌机中混合，搅拌速率为3000r/min，搅拌50min，然后将助剂添加到上述混合物中继续搅拌40min，得到环氧涂料。The preparation method of the fire retardant coating comprises the following steps: firstly, epoxy resin E44, zinc oxide co-doped with Mg, Fe and Al, bisphenol A-bis(diphenyl phosphate) (BDP), 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), a silane coupling agent and water are put into a high-speed stirrer for mixing at a stirring rate of 3000 r/min for 50 minutes, and then an auxiliary agent is added to the mixture and the stirring is continued for 40 minutes to obtain the epoxy coating.
对比例13Comparative Example 13
一种防火涂料，按重量份计，所述防火涂层的原料包括：环氧树脂E4470份、Mg、Fe和Al共掺杂的氧化锌3份；Ni、Cu和Ce共掺杂氧化锡6份；双酚A-双(二苯基磷酸酯)(BDP)9份，硅烷偶联剂7份、助剂5份与水40份。A fireproof coating, wherein the raw materials of the fireproof coating include, by weight: 70 parts of epoxy resin E44, 3 parts of zinc oxide co-doped with Mg, Fe and Al; 6 parts of tin oxide co-doped with Ni, Cu and Ce; 9 parts of bisphenol A-bis(diphenyl phosphate) (BDP), 7 parts of silane coupling agent, 5 parts of auxiliary agent and 40 parts of water.
所述Mg、Fe和Al共掺杂的氧化锌的制备方法包括以下步骤：The preparation method of the Mg, Fe and Al co-doped zinc oxide comprises the following steps:
将0.02mol硝酸镁、0.03mol氯化铁、0.02mol醋酸铝、0.5mol柠檬酸和1mol锌源超声分散到200mL去离子水中得到分散液，然后采用浓度为5mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为11，然后转移到反应釜中进行水热反应，水热反应条件为160℃反应12h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧3h，得到Mg、Fe和Al共掺杂的氧化锌。0.02 mol of magnesium nitrate, 0.03 mol of ferric chloride, 0.02 mol of aluminum acetate, 0.5 mol of citric acid and 1 mol of zinc source are ultrasonically dispersed in 200 mL of deionized water to obtain a dispersion, and then a sodium hydroxide solution with a concentration of 5 mol/L is slowly added dropwise to the dispersion, the pH value of the solution is adjusted to 11, and then the solution is transferred to a reactor for a hydrothermal reaction at 160° C. for 12 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 3 h to obtain Mg, Fe and Al co-doped zinc oxide.
所述Ni、Cu和Ce共掺杂氧化锡的制备方法包括以下步骤：The preparation method of Ni, Cu and Ce co-doped tin oxide comprises the following steps:
将0.01mol硝酸镍、0.02mol氯化铜、0.03mol醋酸铈、0.4mol酒石酸和1mol硝酸锡超声分散到200mL去离子水中，然后采用浓度为3mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为10，然后转移到反应釜中进行水热反应，水热反应条件为130℃反应15h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧2h，得到Ni、Cu和Ce共掺杂的氧化锡。0.01 mol nickel nitrate, 0.02 mol copper chloride, 0.03 mol cerium acetate, 0.4 mol tartaric acid and 1 mol tin nitrate were ultrasonically dispersed in 200 mL deionized water, and then a 3 mol/L sodium hydroxide solution was slowly added dropwise to the dispersion, the pH value of the solution was adjusted to 10, and then the solution was transferred to a reactor for hydrothermal reaction at 130° C. for 15 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 2 h to obtain Ni, Cu and Ce co-doped tin oxide.
所述偶联剂为γ-巯丙基甲基二乙氧基硅烷；The coupling agent is γ-mercaptopropylmethyldiethoxysilane;
所述防火涂料的制备方法包括以下步骤，先将环氧树脂E44、Mg、Fe和Al共掺杂的氧化锌；Ni、Cu和Ce共掺杂氧化锡；双酚A-双(二苯基磷酸酯)(BDP)，硅烷偶联剂与水放入高速搅拌机中混合，搅拌速率为3000r/min，搅拌50min，然后将助剂添加到上述混合物中继续搅拌40min，得到环氧涂料。The preparation method of the fire retardant coating comprises the following steps: firstly, epoxy resin E44, zinc oxide co-doped with Mg, Fe and Al; tin oxide co-doped with Ni, Cu and Ce; bisphenol A-bis(diphenyl phosphate) (BDP), a silane coupling agent and water are put into a high-speed stirrer and mixed at a stirring rate of 3000 r/min for 50 minutes, and then an auxiliary agent is added to the above mixture and the stirring is continued for 40 minutes to obtain the epoxy coating.
对比例14Comparative Example 14
一种防火涂料，按重量份计，所述防火涂层的原料包括：环氧树脂E4470份、Mg、Fe和Al共掺杂的氧化锌3份；Ni、Cu和Ce共掺杂氧化锡6份；10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)9份，硅烷偶联剂7份、助剂5份与水40份。A fire retardant coating, wherein the raw materials of the fire retardant coating include, by weight: 70 parts of epoxy resin E44, 3 parts of zinc oxide co-doped with Mg, Fe and Al; 6 parts of tin oxide co-doped with Ni, Cu and Ce; 9 parts of 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), 7 parts of silane coupling agent, 5 parts of auxiliary agent and 40 parts of water.
所述Mg、Fe和Al共掺杂的氧化锌的制备方法包括以下步骤：The preparation method of the Mg, Fe and Al co-doped zinc oxide comprises the following steps:
将0.02mol硝酸镁、0.03mol氯化铁、0.02mol醋酸铝、0.5mol柠檬酸和1mol锌源超声分散到200mL去离子水中得到分散液，然后采用浓度为5mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为11，然后转移到反应釜中进行水热反应，水热反应条件为160℃反应12h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧3h，得到Mg、Fe和Al共掺杂的氧化锌。0.02 mol of magnesium nitrate, 0.03 mol of ferric chloride, 0.02 mol of aluminum acetate, 0.5 mol of citric acid and 1 mol of zinc source are ultrasonically dispersed in 200 mL of deionized water to obtain a dispersion, and then a sodium hydroxide solution with a concentration of 5 mol/L is slowly added dropwise to the dispersion, the pH value of the solution is adjusted to 11, and then the solution is transferred to a reactor for a hydrothermal reaction at 160° C. for 12 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 3 h to obtain Mg, Fe and Al co-doped zinc oxide.
所述Ni、Cu和Ce共掺杂氧化锡的制备方法包括以下步骤：The preparation method of Ni, Cu and Ce co-doped tin oxide comprises the following steps:
将0.01mol硝酸镍、0.02mol氯化铜、0.03mol醋酸铈、0.4mol酒石酸和1mol硝酸锡超声分散到200mL去离子水中，然后采用浓度为3mol/L的氢氧化钠溶液缓慢滴加到分散液中，调节溶液的pH值为10，然后转移到反应釜中进行水热反应，水热反应条件为130℃反应15h，过滤、洗涤、于70℃真空干燥10h，然后进行焙烧，所述焙烧条件为500℃焙烧2h，得到Ni、Cu和Ce共掺杂的氧化锡。0.01 mol nickel nitrate, 0.02 mol copper chloride, 0.03 mol cerium acetate, 0.4 mol tartaric acid and 1 mol tin nitrate were ultrasonically dispersed in 200 mL deionized water, and then a 3 mol/L sodium hydroxide solution was slowly added dropwise to the dispersion, the pH value of the solution was adjusted to 10, and then the solution was transferred to a reactor for hydrothermal reaction at 130° C. for 15 h, filtered, washed, and vacuum dried at 70° C. for 10 h, and then calcined at 500° C. for 2 h to obtain Ni, Cu and Ce co-doped tin oxide.
所述偶联剂为γ-巯丙基甲基二乙氧基硅烷；The coupling agent is γ-mercaptopropylmethyldiethoxysilane;
所述防火涂料的制备方法包括以下步骤，先将环氧树脂E44、Mg、Fe和Al共掺杂的氧化锌；Ni、Cu和Ce共掺杂氧化锡；10-(2,5-二羟基苯基)-10-氢-9-氧杂-10-磷杂菲-10-氧化物(ODOPB)，硅烷偶联剂与水放入高速搅拌机中混合，搅拌速率为3000r/min，搅拌50min，然后将助剂添加到上述混合物中继续搅拌40min，得到环氧涂料。The preparation method of the fire retardant coating comprises the following steps: firstly, epoxy resin E44, zinc oxide co-doped with Mg, Fe and Al; tin oxide co-doped with Ni, Cu and Ce; 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (ODOPB), a silane coupling agent and water are put into a high-speed stirrer for mixing at a stirring rate of 3000 r/min for 50 minutes, and then an auxiliary agent is added to the above mixture and the stirring is continued for 40 minutes to obtain the epoxy coating.
实施例1-3与对比例1-14性能测试的具体结果见表1：The specific results of the performance tests of Examples 1-3 and Comparative Examples 1-14 are shown in Table 1:
其中，附着力(拉开发附着力)：GB/T5210；耐冲击力：GB1732；极限氧指数(LOI值)参照GB/T 2406-2009进行测试。Among them, adhesion (pulling adhesion): GB/T5210; impact resistance: GB1732; limiting oxygen index (LOI value) is tested with reference to GB/T 2406-2009.
由表1可以看出，本发明制备的防火涂料，利用组分之间的相互协同作用，掺杂组分之间的协同作用，具有优异的力学性能和防火性能，具有优异的应用前景。It can be seen from Table 1 that the fire retardant coating prepared by the present invention utilizes the mutual synergistic effect between components and the synergistic effect between doped components, has excellent mechanical properties and fire retardant properties, and has excellent application prospects.
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。The above embodiments are preferred implementation modes of the present invention, but the implementation modes of the present invention are not limited to the above embodiments. Any other changes, modifications, substitutions, combinations, and simplifications that do not deviate from the spirit and principles of the present invention should be equivalent replacement methods and are included in the protection scope of the present invention.
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