CN109705679A - Preparation technology of water-based nano metal coating - Google Patents
Preparation technology of water-based nano metal coating Download PDFInfo
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- CN109705679A CN109705679A CN201910024002.7A CN201910024002A CN109705679A CN 109705679 A CN109705679 A CN 109705679A CN 201910024002 A CN201910024002 A CN 201910024002A CN 109705679 A CN109705679 A CN 109705679A
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- Prior art keywords
- water
- methane
- solution
- zinc
- metallic paint
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 117
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 238000000576 coating method Methods 0.000 title claims abstract description 29
- 239000011248 coating agent Substances 0.000 title claims abstract description 26
- 239000002184 metal Substances 0.000 title abstract 5
- 229910052751 metal Inorganic materials 0.000 title abstract 5
- 238000005516 engineering process Methods 0.000 title description 6
- 239000002253 acid Substances 0.000 claims abstract description 54
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000011701 zinc Substances 0.000 claims abstract description 45
- 239000003973 paint Substances 0.000 claims abstract description 44
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 44
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000005055 methyl trichlorosilane Substances 0.000 claims abstract description 20
- 239000000839 emulsion Substances 0.000 claims abstract description 13
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 25
- 239000012071 phase Substances 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 19
- 239000012530 fluid Substances 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000004094 surface-active agent Substances 0.000 claims description 15
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 14
- 229960001763 zinc sulfate Drugs 0.000 claims description 14
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 14
- 239000003960 organic solvent Substances 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 239000004064 cosurfactant Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000003921 oil Substances 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000003860 storage Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 7
- 239000010410 layer Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000012752 auxiliary agent Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 230000001376 precipitating effect Effects 0.000 claims description 6
- 239000003381 stabilizer Substances 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 230000004913 activation Effects 0.000 claims description 5
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims description 5
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 claims description 5
- 239000002270 dispersing agent Substances 0.000 claims description 5
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 5
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 5
- 239000000049 pigment Substances 0.000 claims description 5
- 239000012744 reinforcing agent Substances 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000002562 thickening agent Substances 0.000 claims description 5
- 238000004945 emulsification Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 239000000178 monomer Substances 0.000 claims description 4
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 4
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 4
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 238000004062 sedimentation Methods 0.000 claims description 4
- 229910000975 Carbon steel Inorganic materials 0.000 claims description 3
- KHSLHYAUZSPBIU-UHFFFAOYSA-M benzododecinium bromide Chemical group [Br-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 KHSLHYAUZSPBIU-UHFFFAOYSA-M 0.000 claims description 3
- 239000010962 carbon steel Substances 0.000 claims description 3
- 230000006837 decompression Effects 0.000 claims description 3
- 238000010828 elution Methods 0.000 claims description 3
- 125000000373 fatty alcohol group Chemical group 0.000 claims description 3
- 239000004615 ingredient Substances 0.000 claims description 3
- 239000011229 interlayer Substances 0.000 claims description 3
- 239000012074 organic phase Substances 0.000 claims description 3
- 239000012066 reaction slurry Substances 0.000 claims description 3
- 239000006254 rheological additive Substances 0.000 claims description 3
- 230000003068 static effect Effects 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 2
- 239000003599 detergent Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- 239000007864 aqueous solution Substances 0.000 claims 1
- WQSRXNAKUYIVET-UHFFFAOYSA-N sulfuric acid;zinc Chemical compound [Zn].OS(O)(=O)=O WQSRXNAKUYIVET-UHFFFAOYSA-N 0.000 claims 1
- 238000000593 microemulsion method Methods 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 3
- 238000002411 thermogravimetry Methods 0.000 abstract description 3
- 238000004566 IR spectroscopy Methods 0.000 abstract description 2
- 239000000945 filler Substances 0.000 abstract description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 abstract 1
- 238000002441 X-ray diffraction Methods 0.000 abstract 1
- 239000012456 homogeneous solution Substances 0.000 abstract 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 1
- 238000004627 transmission electron microscopy Methods 0.000 abstract 1
- JRPGMCRJPQJYPE-UHFFFAOYSA-N zinc;carbanide Chemical group [CH3-].[CH3-].[Zn+2] JRPGMCRJPQJYPE-UHFFFAOYSA-N 0.000 abstract 1
- 239000000463 material Substances 0.000 description 13
- 238000011161 development Methods 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000004530 micro-emulsion Substances 0.000 description 5
- 239000002086 nanomaterial Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000003301 hydrolyzing effect Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000006115 industrial coating Substances 0.000 description 2
- 239000006210 lotion Substances 0.000 description 2
- NCWQJOGVLLNWEO-UHFFFAOYSA-N methylsilicon Chemical compound [Si]C NCWQJOGVLLNWEO-UHFFFAOYSA-N 0.000 description 2
- 239000000693 micelle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- XYRAEZLPSATLHH-UHFFFAOYSA-N trisodium methoxy(trioxido)silane Chemical compound [Na+].[Na+].[Na+].CO[Si]([O-])([O-])[O-] XYRAEZLPSATLHH-UHFFFAOYSA-N 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910003910 SiCl4 Inorganic materials 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 1
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 description 1
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- DIOQZVSQGTUSAI-NJFSPNSNSA-N decane Chemical group CCCCCCCCC[14CH3] DIOQZVSQGTUSAI-NJFSPNSNSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000006471 dimerization reaction Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- SNRUBQQJIBEYMU-NJFSPNSNSA-N dodecane Chemical group CCCCCCCCCCC[14CH3] SNRUBQQJIBEYMU-NJFSPNSNSA-N 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- NULGSOGHGHDGBH-UHFFFAOYSA-N n,n-dimethyl-1-phenylmethanamine;hydrobromide Chemical compound [Br-].C[NH+](C)CC1=CC=CC=C1 NULGSOGHGHDGBH-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920000734 polysilsesquioxane polymer Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- HVTHJRMZXBWFNE-UHFFFAOYSA-J sodium zincate Chemical compound [OH-].[OH-].[OH-].[OH-].[Na+].[Na+].[Zn+2] HVTHJRMZXBWFNE-UHFFFAOYSA-J 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
- 235000013618 yogurt Nutrition 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
Abstract
本发明公开了一种水性纳米金属涂料的制备工艺，包括以下步骤：制备倍半硅氧烷，制备超细甲基硅酸锌，制备纳米甲基硅酸锌均质液，制备水性纳米金属漆涂料，以甲基三氯硅烷为原料，采用微乳液法合成纳米甲基硅酸锌,利用差热‑热重，X‑射线衍射，透射电镜，红外光谱等多种分析方法对纳米甲基硅酸锌进行表征，然后将纳米甲基硅酸锌作为填料添加到以丙烯酸乳液为主体原料的混合体系中，制备水性纳米金属涂料，并对涂料涂层的防锈性进行探究。本发明采用上述水性纳米金属涂料的制备工艺，解决了甲基三氯硅烷大量累积的问题，使甲基三氯硅烷得到了充分利用，环保且性能较高，且制备工艺简单，降低了成本。
The invention discloses a preparation process of water-based nanometer metal paint, which comprises the following steps: preparing silsesquioxane, preparing ultrafine zinc methyl silicate, preparing nano-zinc methyl silicate homogeneous solution, and preparing water-based nanometer metal paint Coating, using methyl trichlorosilane as raw material, using microemulsion method to synthesize nano-zinc methyl silicate, using differential thermal-thermogravimetry, X-ray diffraction, transmission electron microscopy, infrared spectroscopy and other analytical methods to analyze nano-methyl silicon silicate. Zinc acid was characterized, and then nano-zinc methyl silicate was added as a filler to the mixed system with acrylic emulsion as the main raw material to prepare water-based nano-metal coatings, and the rust resistance of the coatings was explored. The invention adopts the above-mentioned preparation process of the water-based nano metal coating, solves the problem of a large amount of methyltrichlorosilane accumulating, makes the methyltrichlorosilane fully utilized, is environmentally friendly and has high performance, and the preparation process is simple and the cost is reduced.
Description
Technical field
The present invention relates to metallic paint technical fields, more particularly, to a kind of preparation process of water nano metallic paint.
Background technique
With preserving the ecological environment and the increasing of energy-saving and emission-reduction dynamics and oil price rise steadily, so that solvent type applies
Material price is constantly promoted.The exploitation of aqueous industrial coating is current good opportunity to develop and following development trend.Influence water
Property industrial coating development key problem in technology be water-base resin and high pure and ultra-fine solid additive research and development.In recent years, water-base resin
The progress and development of production technology, so that water paint gradually replaces solvent based coating to become possible.Consolidate used in water paint
Body additives are mainly titanium dioxide and silica, also use zinc oxide, trbasic zinc phosphate, calcium carbonate etc., these pigment or filler
Sand is needed to grind or high speed dispersion since particle is big, density is big, difficulty of processing is larger, the paint stability difference of preparation and at high cost,
And acid and alkali-resistance and hydrophobicity are poor.The preparation of ultrafine solids additive or high degree of dispersion technology, which have become, influences water paint hair
One of bottleneck of exhibition.All the time, domestic and foreign scholars are devoted to the research and development of solvent type nano paint, in water nano
Research in terms of coating is at the early-stage, and key is how solid packing is steadily distributed to nanoscale.Because at aqueous point
In dispersion media, the high surface of nano material can be allowed to strong adsorption water with specific surface area and generate R-OH based structures, make between each other
Polymerization easily occurs or generates link object, nano material and slurry body is caused to be also easy to produce reunion, to influence its dispersibility.To understand
Certainly the problems such as nano-waterborne coating storage stability, many scholars pass through resistance to inorganic nano materials such as titanium dioxide and silica
The only generation of its surface hydroxyl layer prevents water etc. from Chemisorption occurs；Change interfacial structure feature；Using dispersing agent, have
Machine surfactant, coupling agent etc. generate the methods of absorption protection and surface coating modification on surface and have carried out experimental study, but
Put into the seldom of practical application.Application study of the ultra-fine methane-siliconic acid zinc in water-thinned nanometer paint has not been reported.It studies hydrophobic
Property nano inorganic/organic composite material be solve water-thinned nanometer paint stability problem effective way and development trend.
The body material of preparation nanometer methane-siliconic acid zinc is by-product-methyl trichlorine silicon in the production of silicone base raw material
Alkane.The method of the current direct synthesizing methyl-chloro-silane under copper catalyst effect using chloromethanes and silicon powder main both at home and abroad.It should
Method is except generation target product (CH3)2SiCl2Outside, along with generation part by-product: CH3SiCl3, content 3-5%；
(CH3)3SiCl, content 3%；CH3HSiCl2, content 1-3%；(CH3)2HSiCl, content 0.5%；(CH3)4Si, content
It is 0.1%；SiCl4High-boiling components, content 1-6%.Wherein CH3SiCl3Ratio is maximum.Currently, CH3SiCl3Do not filled
Development and utilization are divided to cause largely to accumulate.Due to CH3SiCl3Facile hydrolysis generates HCl in air, brings immense pressure to environment.Institute
With CH3SiCl3Processing not only become the bottleneck for restricting organosilicon industry development with application, be also bound to become and guide whole production
The key of industry chain sustainable development.By CH3SiCl3Catalytic disproportionation is converted into (CH3)2SiCl2Research have many reports, but it is related
Technology is still immature.By CH3SiCl3Though preparing nano-gas-phase white carbon black to have industrialized, technology is mainly big by external several families
Company monopolizing.Methyl silicon resin is prepared, silane coupling agent prepares sodium methyl silicate (potassium) and stablizes as waterproofing agent and oil drilling
There are also reports for agent and the research for preparing polymethyl siloxane hydrophober etc..So the exploitation benefit of methyl trichlorosilane
With with great strategic significance.
This century, nano-functional material are most promising new materials, because of its unique nano effect, will usually be received
Rice material, which is added to, to be dispersed in traditional coating and can assign coating excellent performance after being modified to former coating.Nanometer material
Material refers to a kind of material for reaching nano-grade size level in the microstructures such as crystal grain and crystal boundary.Preparation method is a variety of more
Sample, traditional method include solid phase method, and liquid phase method (chemical precipitation method, sol-gel method, hydrothermal synthesis method), vapor phase method is (by spraying
Thermal decomposition method, chemical vapor phase oxidation process, induced with laser vapour deposition process), new method includes air-liquid-solid and gas-solid evaporation mass transfer
Method and microemulsion method.Microemulsion is to be reported for the first time in nineteen forty-three by Hoar and schulman, is referred to as the micelle of swelling at that time
Or the micelle of solubilising.Until nineteen fifty-nine, above-mentioned system is named as micro emulsion or microemulsion for the first time by Schulman et al..Earliest
It is proposed that using Preparing Nano-Materials in Microemulsions be Boutonnet, he is molten using hydrazine hydrate or hydrogen reducing precious metal salt
Nanoscale Pt, Pd, Ph and Ir simple substance is made in liquid.Hereafter, the semiconductors such as CdS, the superconductors such as YBa2Cu4O8, ferrous acid
The magnetic pipe recording materials such as barium and various compounds or compound particle all prepare in microemulsion.The experiment of microemulsion method fills
It sets simply, it is easy to operate, and can control the granularity of synthesis particle, there is its unique excellent in terms of nanoparticle preparation
Point.Microemulsion method increasingly by the attention of researcher, and waste water control, extraction and separation, catalysis, food, biological medicine,
The fields such as cosmetics, material preparation, chemical reaction medium, coating all have potential application prospect.
Water-thinned nanometer paint refers to the coating using water as decentralized medium, less, pollution-free, the safe nothing of organic solvent volatilization
Poison is the main flow direction of modern coatings development.Therefore make nano material really with nano-dispersion in water paint, play it
Nano effect, obtaining the good water-thinned nanometer paint of high-performance, stability has highly important application value.
Summary of the invention
The object of the present invention is to provide a kind of preparation processes of water nano metallic paint, and it is big to solve methyl trichlorosilane
The problem of amount accumulation, methyl trichlorosilane is made to be fully used, environmentally friendly and performance is higher, and preparation process is simple, reduces
Cost.
To achieve the above object, the present invention provides a kind of preparation processes of water nano metallic paint, including following step
It is rapid:
(1) silsesquioxane is prepared
By deionized water: organic solvent: methyl trichlorosilane is the ingredient proportion of 2-2.5:1-1.2:1-1.2 in mass ratio
It is configured, deionized water is first added in a kettle, added organic solvent and be stirred, form organic-water two phase liquid,
It is passed through cold water in reaction kettle interlayer to control temperature at 25-40 DEG C, starts blender and by head tank into reaction kettle
Methyl trichlorosilane is added dropwise, time control is added dropwise at 30-50 minutes, the reaction was continued 45 minutes after being added dropwise, and stops stirring
It mixes, reaction slurry is released to and is transferred to filter decompression suction filtration, with water elution precipitating 2~3 times, until pH value is 5-6, precipitating is transferred to
It is dried in 100 DEG C of constant temperature drying rooms, finally obtains dry silsesquioxane；
(2) ultra-fine methane-siliconic acid zinc is prepared
Above-mentioned silsesquioxane is added in sodium hydroxide solution after activation 2-4 hours through 300 DEG C and carries out heating stirring
Until clear solution, methane-siliconic acid sodium solution, i.e. solution A is made；
Zinc sulfate is added in distilled water heating stirring to being completely dissolved to obtain zinc sulfate solution, as water phase,
The ratio of middle zinc sulfate and distilled water is 4.5:10, and then by surfactant, cosurfactant and oil are mutually in electric stirring
It is uniformly mixed on machine, wherein the mass ratio of surfactant, cosurfactant and oily phase is 4:1:12, is then added
Zinc sulfate solution is stirred to obtain B solution；
Solution A is added drop-wise in B solution in proportion, carries out it in 30-50 DEG C of water bath with thermostatic control, pH value is controlled, stirs
Dehydrated alcohol is added after mixing 0.5 hour to continue to stir 10 minutes, then sonicated, sedimentation filtration, after washing, drying to obtain the final product
Ultra-fine methane-siliconic acid zinc；
(3) nanometer methane-siliconic acid zinc homogenizing fluid is prepared
100 parts of ultra-fine methane-siliconic acid zinc and 400-800 parts of water and 20 parts of LS-1050 dispersing agents and 15 parts of FS-03 are steady
Determine agent mixing, 1000 liters of flow velocity carries out at the dispersion of high-voltage pulse air-flow with the pressure of 70 megapascal and per hour by homogenizer
Nanometer methane-siliconic acid zinc homogenizing fluid is made in reason；
(4) water nano metallic paint is prepared
By raw material based on above-mentioned nanometer methane-siliconic acid zinc homogenizing fluid and 250-450 parts of acrylic emulsions, it is added to 0-150
It is stirred in part water, until stirring evenly, addition auxiliary agent is by emulsification cutter with the revolving speed emulsion dispersion 30 of 600-800 turns/h
Water nano metallic paint is obtained after minute.
Preferably, the organic solvent in the step (1) is decane or dodecane；
Mixed filtrate in filter, which is pumped into reaction kettle, to be reused, when the water phase hydrogen cloride concentration in mixed filtrate reaches
When 30%, static lower layer's water phase of isolating is stand-by as industrial concentrated hydrochloric acid storage, and washing filtrate water is by initial proportion as water phase
It adds to mix to be pumped into reaction kettle in organic phase and be recycled, the hydrogen chloride gas for reacting generation is returned by reaction kettle collected overhead
Chloromethanes is prepared to organic silicon monomer beginning of production.
Preferably, the temperature heated in the solution A preparation process in the step (2) is controlled at 80 DEG C, and the surface is living
Property agent be fatty alcohol polyoxyethylene ether, cosurfactant is dodecyl dimethyl benzyl ammonium bromide, oil mutually be normal octane, institute
State the HLB value 3-6 of surfactant.
Preferably, the detergent that washing uses in the step (2) is dehydrated alcohol, and drying temperature is 80 DEG C.
Preferably, the auxiliary agent added in the step (4) is dipropylene, reinforcing agent, thickener, levelling are modified
Agent, pigment, storage stabilizer.
Preferably, coating template is made in above-mentioned water nano metallic paint to be used to detect, the coating preparation of specimen
Method is that carbon steel test piece is immersed in water nano metallic paint, takes out after 3 seconds, dries in an oven, coating template is made.
Therefore, the present invention uses the preparation process of above-mentioned water nano metallic paint, and it is a large amount of to solve methyl trichlorosilane
The problem of accumulation, makes methyl trichlorosilane be fully used, and environmentally friendly and performance is higher, and preparation process is simple, reduces
Cost.
Below by drawings and examples, technical scheme of the present invention will be described in further detail.
Detailed description of the invention
Fig. 1 is a kind of process flow chart of the preparation process embodiment of water nano metallic paint of the present invention；
Fig. 2 is the infrared spectrogram of nanometer methane-siliconic acid zinc；
Fig. 3 is the TEM shape appearance figure of nanometer methane-siliconic acid zinc；
Fig. 4 is the XRD diagram of nanometer methane-siliconic acid zinc；
Fig. 5 is differential thermal-thermal multigraph of nanometer methane-siliconic acid zinc.
Specific embodiment
As shown in Figure 1, the present invention provides a kind of preparation processes of water nano metallic paint, comprising the following steps:
(1) silsesquioxane is prepared
By deionized water: organic solvent: methyl trichlorosilane is the ingredient proportion of 2-2.5:1-1.2:1-1.2 in mass ratio
It is configured, deionized water is first added in a kettle, added organic solvent and be stirred, form organic-water two phase liquid,
Organic solvent is decane or dodecane, and cold water is passed through in reaction kettle interlayer and controls temperature at 25-40 DEG C, starts blender
And methyl trichlorosilane is added dropwise into reaction kettle by head tank, time control is added dropwise at 30-50 minutes, after being added dropwise
The reaction was continued 45 minutes, stops stirring, and reaction slurry is released to and is transferred to filter decompression suction filtration, with water elution precipitating 2~3
Secondary, until pH value is 5-6, precipitating, which is transferred in 100 DEG C of constant temperature drying rooms, is dried, and finally obtains dry silsesquioxane, filter
In mixed filtrate be pumped into reaction kettle and reuse, when the water phase hydrogen cloride concentration in mixed filtrate is up to 30%, static point
It is stand-by as industrial concentrated hydrochloric acid storage to separate out lower layer's water phase, washing filtrate water is added in organic phase by initial proportion as water phase
Mixing, which is pumped into reaction kettle, to be recycled, and the hydrogen chloride gas for reacting generation returns to organic silicon monomer life by reaction kettle collected overhead
It produces source and prepares chloromethanes；
(2) ultra-fine methane-siliconic acid zinc is prepared
Above-mentioned silsesquioxane is added in sodium hydroxide solution after activation 2-4 hours through 300 DEG C and carries out heating stirring
Until clear solution, the temperature of heating is controlled at 80 DEG C, and methane-siliconic acid sodium solution, i.e. solution A is made；
Zinc sulfate is added in distilled water heating stirring to being completely dissolved to obtain zinc sulfate solution, as water phase,
The ratio of middle zinc sulfate and distilled water is 4.5:10, and then by surfactant, cosurfactant and oil are mutually in electric stirring
It is uniformly mixed on machine, wherein the mass ratio of surfactant, cosurfactant and oily phase is 4:1:12, is then added
Zinc sulfate solution is stirred to obtain B solution, and the surfactant is fatty alcohol polyoxyethylene ether, and HLB value 3-6 helps table
Face activating agent is dodecyl dimethyl benzyl ammonium bromide, and oil is mutually normal octane；
Solution A is added drop-wise in B solution in proportion, carries out it in 30-50 DEG C of water bath with thermostatic control, pH value is controlled, stirs
After mixing 0.5 hour be added dehydrated alcohol continue stirring 10 minutes, then sonicated, sedimentation filtration, using dehydrated alcohol into
Up to ultra-fine methane-siliconic acid zinc after row washing, drying, drying temperature is 80 DEG C；
(3) nanometer methane-siliconic acid zinc homogenizing fluid is prepared
100 parts of ultra-fine methane-siliconic acid zinc and 400-800 parts of water and 20 parts of LS-1050 dispersing agents and 15 parts of FS-03 are steady
Determine agent mixing, 1000 liters of flow velocity carries out at the dispersion of high-voltage pulse air-flow with the pressure of 70 megapascal and per hour by homogenizer
Nanometer methane-siliconic acid zinc homogenizing fluid is made in reason；
(4) water nano metallic paint is prepared
By raw material based on above-mentioned nanometer methane-siliconic acid zinc homogenizing fluid and 250-450 parts of acrylic emulsions, it is added to 0-150
It is stirred in part water, until stirring evenly, addition auxiliary agent is by emulsification cutter with the revolving speed emulsion dispersion 30 of 600-800 turns/h
Obtain water nano metallic paint after minute, auxiliary agent be dipropylene, reinforcing agent, thickener, rheological modifier, pigment,
Storage stabilizer.
Further, coating template is made in above-mentioned water nano metallic paint to be used to detect, coating preparation of specimen side
Method is that carbon steel test piece is immersed in water nano metallic paint, takes out after 3 seconds, dries in an oven, coating template is made.
Reaction principle: methyl trichlorosilane is directly reacted with water, and the methane-siliconic acid for reacting generation is self condensed, formation
Silsesquioxane does not fix form, it may be possible to which dimerization, four poly-, six is poly-, and eight cage structures, the hydrolytic condensations shown such as poly- are anti-
Should very acutely, bad control can only obtain the biggish cotton-shaped polysilsesquioxane crude product of particle.Due to cotton-shaped crude product caged knot
Structure is not easy to be opened, and density very little, and liquid surface is swum in when preparing downstream product and is unfavorable for sufficiently reacting.To control water
Reaction speed, hydrolysate structure and granularity are solved, the organic solvent (last of the ten Heavenly stems that selection is nontoxic, tasteless, nonflammable, volatility is small is taken
Alkane) with water formed two-phase system in hydrolyze.In this way, organic solvent is soluble in using the methyl on methyl trichlorosilane, and silicon
Chlorine key is dissolved in the characteristic (i.e. similar compatibility principle) of water layer, so that methyl trichlorosilane just forms between water layer and organic layer
One conversion zone.Methyl trichlorosilane occur hydrolysis only phase interface carry out, so self-condensation reaction be also all by
Mutually carried out between the methane-siliconic acid of boundary layer, thus make the silsesquioxane generated form a kind of reticulated microstructure and
It is not cage structure.This not only controls hydrolytic condensation speed, keeps product grain smaller, and changes condensation product structure,
The reaction for preparing downstream product sodium methyl silicate etc. is set to be easier to carry out.The hydrogen chloride gas generated is reacted by reaction kettle collected overhead
It returns to organic silicon monomer production line source and prepares chloromethanes, the water phase of hydrolyzation system may separate out hydrochloric acid byproduct, organic addition
Water is reusable.The basic three-waste free discharge of hydrolytic process, and constitute Recycling Economy System.
Netted silsesquioxane is sufficiently dissolved in sodium hydroxide solution after 300 DEG C of activation, obtained methane-siliconic acid
The reaction in two kinds of mutual exclusive solvents of water and organic solvent of sodium and sodium zincate prepares methane-siliconic acid zinc, and when reaction is living on surface
Property agent and help under the action of surfactant the thermodynamic stable system (cream for being allowed to be formed a uniform isotropic
Liquid), the processes such as nucleation, growth, coalescence, reunion can be made to be confined in a small spherical droplets from solid phase is precipitated in lotion,
So as to form spheric granules, and avoid further reuniting between particle.So this heterogeneous lotion synthetic method can make grain
It spends narrow distribution and is easy to control, isolate methane-siliconic acid zinc powder body, mother liquor can be recycled.
Prepare water nano metallic paint by the following examples, then using scanning electron microscope, differential thermal-thermogravimetric analysis,
Infrared spectroscopy, XRD etc. are characterized.
Embodiment 1
Influence of the reaction temperature to ultra-fine methane-siliconic acid zinc:
Silsesquioxane in step (1) is added in sodium hydroxide solution after activation 2-4 hours through 300 DEG C and is added
Until thermal agitation to clear solution, the temperature of heating is controlled at 80 DEG C, and methane-siliconic acid sodium solution, i.e. solution A is made；By zinc sulfate
Heating stirring is added in distilled water to being completely dissolved to obtain zinc sulfate solution, as water phase, wherein zinc sulfate and distilled water
Ratio be 4.5:10, then by surfactant, cosurfactant and oil are mutually uniformly mixed in electric blender,
Wherein the mass ratio of surfactant, cosurfactant and oily phase is 4:1:12, then adds zinc sulfate solution progress
B solution is stirred to get, the surfactant is fatty alcohol polyoxyethylene ether, and HLB value 3-6, cosurfactant is dodecane
Base dimethylbenzyl ammonium bromide, oil are mutually normal octane；Solution A is added drop-wise in B solution in proportion, makes it respectively in 30 DEG C, 40
DEG C, carry out in 50 DEG C of water bath with thermostatic control, control pH value, dehydrated alcohol be added after stirring 0.5 hour and continues stirring 10 minutes, then
Sonicated, sedimentation filtration, up to ultra-fine methane-siliconic acid zinc after being washed, being dried using dehydrated alcohol, drying temperature is
80 DEG C, reaction bath temperature is different, and the influence to ultra-fine methane-siliconic acid zinc granule diameter, such as table 1, other steps are as above.
Table 1
| Reaction temperature (DEG C) | 30 | 40 | 50 |
| Particle diameter (nm) | 97.0 | 36.2 | 136.7 |
40 DEG C are optimal reactive temperature as can be seen from Table 1.
Embodiment 2
Different water consumptions prepare nanometer methane-siliconic acid zinc homogenizing fluid:
Take 100 parts of superfine nano methane-siliconic acid zinc, 20 parts of FS-1050 dispersing agent, amount of water is respectively 400 parts, 500 parts,
600 parts, 700 parts, 800 parts, then stir evenly, respectively by homogenizer with the pressure of 70 megapascal and 1000 liters of stream per hour
Speed carries out high-voltage pulse air-flow decentralized processing, nanometer methane-siliconic acid zinc homogenizing fluid is made, different water consumptions are to nanometer methane-siliconic acid
The influence of the zinc homogenizing fluid uniformity, such as table 2, other steps are as above.
Table 2
| Water consumption (part) | 400 | 500 | 600 | 700 | 800 |
| The uniformity of homogeneous material | It is sticky | It is slightly sticky thick | Uniformly | It is slightly dilute | It crosses dilute |
As shown in Table 2, when water consumption is 600 parts, the uniformity of homogeneous material is preferably less than more sticky at 600 parts, coating
Unevenly；Diluter when greater than 600 parts, coating coverage is poor.
Embodiment 3
Influence of the amount of different acrylic emulsions to water nano metallic paint film forming situation:
Take 100 parts of nanometer methane-siliconic acid homogenizing fluid, 30 parts of dipropylene, 4 parts of rheological modifier, 10 parts of thickener,
20 parts of storage stabilizer, 20 parts of reinforcing agent, 50 parts of water, 2 parts of pigment, acrylic emulsion is respectively 250 parts, 300 parts, 350 parts,
400 parts, 450 parts, are stirred evenly by blender respectively, by emulsification cutter with the revolving speed emulsion dispersion of 600-800 turns/h
Obtain water nano metallic paint after 30 minutes, the shadow of the amounts of different acrylic emulsions to water nano metallic paint film forming situation
It rings, such as table 3, other steps are as above.
Table 3
| The dosage (part) of acrylic emulsion | 250 | 300 | 350 | 400 | 150 |
| Form a film situation | It is excessively thin | It is relatively thin | Uniformly | It is slightly dilute | It crosses dilute |
By can be seen that in table 3, uniformly, film is too thin when dosage is less, and adhesive force is or not film forming when acrylic emulsion is 350 parts
Good, film is too thick when dosage is more, influences specification coating preparation of specimen.
Embodiment 4
Influence of the different water consumptions to water nano metallic paint:
100 parts of nanometer methane-siliconic acid homogenizing fluid, propylene yogurt are taken on the basis of embodiment 1, embodiment 2 and embodiment 3
Liquid be 350 parts, 30 parts of dipropylene, 4 parts of levelling agent, 10 parts of thickener, 20 parts of storage stabilizer, 20 parts of reinforcing agent, face
2 parts of material, water is respectively 0 part, and 50 parts, 100 parts, 150 parts, blender stirs evenly, and the water nano gold of different water consumptions is made
Belong to coating, the influence to the corrosion time of coating template, such as table 4, other steps are as above.
Table 4
| Water consumption (part) | 0 | 50 | 100 | 150 |
| Start the time (h) of corrosion | 23 | 48 | 39 | 26 |
As shown in Table 4, when water consumption is 50 parts, rustless property is best；When amount of water is 0, form a film thicker, attachment
Power is poor, and resistance to corrosion is poor；When water consumption is greater than 50 parts, form a film relatively thin, resistance to corrosion is poor.
The nanometer methane-siliconic acid zinc homogenizing fluid of preparation is characterized, nanometer methane-siliconic acid zinc homogenizing fluid is carried out first red
External spectrum analysis, as shown in Fig. 2, in 3419cm-1There is a strong peak in place, is O-H stretching vibration peak；In 1637cm-1Locate
An existing peak is Si-O flexural vibrations peak；In 1273cm-1There is a peak in place, is Si-CH3Stretching vibration peak；?
1122cm-1There is a strong peak in place, is Si-O-Si stretching vibration peak；In 779cm-1There is a peak in place, is bent for H-O
Vibration peak；In 613cm-1There is a peak in place, is Si-O-Zn nonsymmetrical vibration absorption peak.
The nanometer methane-siliconic acid zinc homogenizing fluid of preparation is dried, TEM morphology analysis is then carried out, as shown in figure 3, receiving
Rice methane-siliconic acid zinc is nanoscale white powder.
The nanometer methane-siliconic acid zinc homogenizing fluid of preparation is dried, XRD diagram analysis is then carried out, as shown in figure 4, nanometer
Methane-siliconic acid zinc is manocrystalline powders.
Differential thermal-thermogravimetric analysis is carried out to nanometer methane-siliconic acid zinc, as can be seen from Figure 5: occurring at 100 DEG C one small strong
Peak illustrates that 100 DEG C of nanometer methane-siliconic acid zinc has physical absorption water to fall off, and 210 DEG C of appearance, one small Qiang Feng illustrates a nanometer methyl silicon
Sour zinc has some associated waters or associate hydrogen bond to start to be dehydrated at 210 DEG C, then heats to 1000 DEG C, and differential thermal curve is gentle, says
Bright nanometer methane-siliconic acid zinc decomposition temperature has preferable thermal stability at 1000 DEG C or more.
Therefore, the present invention uses the preparation process of above-mentioned water nano metallic paint, and it is a large amount of to solve methyl trichlorosilane
The problem of accumulation, makes methyl trichlorosilane be fully used, and environmentally friendly and performance is higher, and preparation process is simple, reduces
Cost.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than is limited,
Although the present invention is described in detail with reference to preferred embodiments, those skilled in the art should understand that: its according to
So can be with modification or equivalent replacement of the technical solution of the present invention are made, and these modifications or equivalent replacement cannot also make to repair
Technical solution after changing is detached from the spirit and scope of technical solution of the present invention.
Claims (6)
1. a kind of preparation process of water nano metallic paint, which comprises the following steps:
(1) silsesquioxane is prepared
By deionized water: organic solvent: methyl trichlorosilane is that the ingredient proportion of 2-2.5:1-1.2:1-1.2 carries out in mass ratio
Configuration, deionized water is first added in a kettle, adds organic solvent and is stirred, and organic-water two phase liquid is formed, anti-
It answers and is passed through cold water in kettle interlayer for temperature control at 25-40 DEG C, start blender and be added dropwise by head tank into reaction kettle
Time control was added dropwise at 30-50 minutes in methyl trichlorosilane, and the reaction was continued 45 minutes after being added dropwise, and stops stirring, will
Reaction slurry releases and is transferred to filter decompression and filters, and with water elution precipitating 2~3 times, until pH value is 5-6, precipitating is transferred to 100 DEG C
Constant temperature drying is dried in room, finally obtains dry silsesquioxane；
(2) ultra-fine methane-siliconic acid zinc is prepared
Above-mentioned silsesquioxane is added to after activation 2-4 hours in sodium hydroxide solution through 300 DEG C and carries out heating stirring to clear
Until clear solution, methane-siliconic acid sodium solution, i.e. solution A is made；
Zinc sulfate is added in distilled water heating stirring to being completely dissolved to obtain zinc sulfate solution, as water phase, wherein sulphur
The ratio of sour zinc and distilled water is 4.5:10, and then by surfactant, cosurfactant and oil phase are in electric blender
It is uniformly mixed, wherein the mass ratio of surfactant, cosurfactant and oily phase is 4:1:12, then adds sulfuric acid
Zinc aqueous solution is stirred to obtain B solution；
Solution A is added drop-wise in B solution in proportion, carries out it in 30-50 DEG C of water bath with thermostatic control, controls pH value, stirring 0.5
Dehydrated alcohol is added after hour and continues stirring 10 minutes, then sonicated, sedimentation filtration, up to ultra-fine after washing, drying
Methane-siliconic acid zinc；
(3) nanometer methane-siliconic acid zinc homogenizing fluid is prepared
By 100 parts of ultra-fine methane-siliconic acid zinc and 400-800 parts of water and 20 parts of LS-1050 dispersing agents and 15 parts of FS-03 stabilizers
Mixing, by homogenizer, with the pressure of 70 megapascal and per hour, 1000 liters of flow velocity carries out high-voltage pulse air-flow decentralized processing, system
Obtain nanometer methane-siliconic acid zinc homogenizing fluid；
(4) water nano metallic paint is prepared
By raw material based on above-mentioned nanometer methane-siliconic acid zinc homogenizing fluid and 250-450 parts of acrylic emulsions, it is added to 0-150 parts of water
In be stirred, until stir evenly, addition auxiliary agent turns with 600-800 by emulsification cutter/revolving speed emulsion dispersion 30 minutes of h
After obtain water nano metallic paint.
2. the preparation process of water nano metallic paint according to claim 1, it is characterised in that:
Organic solvent in the step (1) is decane or dodecane；
Mixed filtrate in filter, which is pumped into reaction kettle, to be reused, when the water phase hydrogen cloride concentration in mixed filtrate is up to 30%
When, static lower layer's water phase of isolating is stand-by as industrial concentrated hydrochloric acid storage, and washing filtrate water is supplemented by initial proportion as water phase
Into organic phase, mixing, which is pumped into reaction kettle, is recycled, and the hydrogen chloride gas for reacting generation has been returned to by reaction kettle collected overhead
Machine silicon monomer beginning of production prepares chloromethanes.
3. the preparation process of water nano metallic paint according to claim 2, it is characterised in that: in the step (2)
Solution A preparation process in the temperature control heated at 80 DEG C, the surfactant is fatty alcohol polyoxyethylene ether, helps surface
Activating agent is dodecyl dimethyl benzyl ammonium bromide, and oil is mutually normal octane, the HLB value 3-6 of the surfactant.
4. the preparation process of water nano metallic paint according to claim 3, it is characterised in that: in the step (2)
Washing the detergent used is dehydrated alcohol, and drying temperature is 80 DEG C.
5. the preparation process of water nano metallic paint according to claim 4, it is characterised in that: in the step (4)
The auxiliary agent of addition is dipropylene, reinforcing agent, thickener, rheological modifier, pigment, storage stabilizer.
6. the preparation process of water nano metallic paint according to claim 5, it is characterised in that: by above-mentioned water nano
Metallic paint is made coating template and is used to detect, and the coating preparation of specimen method is that carbon steel test piece is immersed in water nano
It in metallic paint, takes out after 3 seconds, dries in an oven, coating template is made.
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| CN103013337A (en) * | 2011-09-28 | 2013-04-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Metal protective coating and hot galvanizing metal material as well as hot-dip aluminium-zinc metal material |
| CN104327650A (en) * | 2014-11-25 | 2015-02-04 | 廊坊师范学院 | Preparation method of methyl silicate aqueous nano antirust agent |
| CN104356159A (en) * | 2014-11-25 | 2015-02-18 | 廊坊师范学院 | Method for preparing silsesquioxane by virtue of hydrolysis of methyl trichlorosilane |
| CN104447834A (en) * | 2014-11-25 | 2015-03-25 | 廊坊师范学院 | Preparation method for nano methyl zinc silicate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110042396A (en) * | 2019-05-30 | 2019-07-23 | 廊坊师范学院 | The preparation method of water base long term antirust agent |
| CN110042396B (en) * | 2019-05-30 | 2021-07-02 | 廊坊师范学院 | Preparation method of water-based long-term rust inhibitor |
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