CN110512257B - High-thermal-corrosion-resistance coating hole sealing agent - Google Patents
High-thermal-corrosion-resistance coating hole sealing agent Download PDFInfo
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- CN110512257B CN110512257B CN201910710623.0A CN201910710623A CN110512257B CN 110512257 B CN110512257 B CN 110512257B CN 201910710623 A CN201910710623 A CN 201910710623A CN 110512257 B CN110512257 B CN 110512257B
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- 238000007789 sealing Methods 0.000 title claims abstract description 78
- 239000011248 coating agent Substances 0.000 title claims abstract description 27
- 238000000576 coating method Methods 0.000 title claims abstract description 27
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 24
- 239000010455 vermiculite Substances 0.000 claims abstract description 32
- 229910052902 vermiculite Inorganic materials 0.000 claims abstract description 32
- 235000019354 vermiculite Nutrition 0.000 claims abstract description 32
- 239000002245 particle Substances 0.000 claims abstract description 27
- 238000005260 corrosion Methods 0.000 claims abstract description 21
- 230000007797 corrosion Effects 0.000 claims abstract description 21
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000009471 action Effects 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims description 99
- 239000000463 material Substances 0.000 claims description 71
- 239000000203 mixture Substances 0.000 claims description 47
- 238000006243 chemical reaction Methods 0.000 claims description 39
- 239000003153 chemical reaction reagent Substances 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- 239000000126 substance Substances 0.000 claims description 27
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 24
- 238000001914 filtration Methods 0.000 claims description 24
- 239000012065 filter cake Substances 0.000 claims description 21
- 239000000654 additive Substances 0.000 claims description 20
- 230000000996 additive effect Effects 0.000 claims description 20
- 239000002131 composite material Substances 0.000 claims description 19
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 18
- 239000012752 auxiliary agent Substances 0.000 claims description 18
- 239000002270 dispersing agent Substances 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 18
- 239000002518 antifoaming agent Substances 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000004202 carbamide Substances 0.000 claims description 12
- 235000013877 carbamide Nutrition 0.000 claims description 12
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 12
- 239000000376 reactant Substances 0.000 claims description 12
- 239000012266 salt solution Substances 0.000 claims description 12
- 238000007873 sieving Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000000565 sealant Substances 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 7
- 239000003822 epoxy resin Substances 0.000 claims description 7
- -1 polydimethylsiloxane Polymers 0.000 claims description 7
- 229920000647 polyepoxide Polymers 0.000 claims description 7
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 7
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- 239000001509 sodium citrate Substances 0.000 claims description 7
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 7
- 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 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 6
- 229920000663 Hydroxyethyl cellulose Polymers 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 6
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 6
- GPLRAVKSCUXZTP-UHFFFAOYSA-N diglycerol Chemical compound OCC(O)COCC(O)CO GPLRAVKSCUXZTP-UHFFFAOYSA-N 0.000 claims description 6
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 6
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 6
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- KHIWWQKSHDUIBK-UHFFFAOYSA-N periodic acid Chemical compound OI(=O)(=O)=O KHIWWQKSHDUIBK-UHFFFAOYSA-N 0.000 claims description 6
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 6
- 229920002401 polyacrylamide Polymers 0.000 claims description 6
- 235000019353 potassium silicate Nutrition 0.000 claims description 6
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 claims description 6
- 229940116357 potassium thiocyanate Drugs 0.000 claims description 6
- 238000002390 rotary evaporation Methods 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 claims description 6
- 229910000342 sodium bisulfate Inorganic materials 0.000 claims description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 6
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 6
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 6
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 6
- 229920002554 vinyl polymer Polymers 0.000 claims description 6
- OIFLLGNCLZLPAF-UHFFFAOYSA-M trimethyl-(5-methyl-4-oxohex-5-enyl)azanium;chloride Chemical compound [Cl-].CC(=C)C(=O)CCC[N+](C)(C)C OIFLLGNCLZLPAF-UHFFFAOYSA-M 0.000 claims description 3
- 239000013530 defoamer Substances 0.000 claims 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical class [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 17
- 230000000694 effects Effects 0.000 abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 5
- 238000011049 filling Methods 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 3
- 229910001593 boehmite Inorganic materials 0.000 abstract description 3
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000002841 Lewis acid Substances 0.000 abstract description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 2
- 238000010668 complexation reaction Methods 0.000 abstract description 2
- 150000007517 lewis acids Chemical group 0.000 abstract description 2
- 229920002521 macromolecule Polymers 0.000 abstract description 2
- 239000011777 magnesium Substances 0.000 abstract description 2
- 229910052749 magnesium Inorganic materials 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 2
- 239000010703 silicon Substances 0.000 abstract description 2
- 230000009920 chelation Effects 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 16
- 229910052782 aluminium Inorganic materials 0.000 description 15
- 239000010410 layer Substances 0.000 description 9
- 229910000838 Al alloy Inorganic materials 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 239000010407 anodic oxide Substances 0.000 description 5
- 229940113088 dimethylacetamide Drugs 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 239000013543 active substance Substances 0.000 description 3
- KVFFVDVAFFSIIL-UHFFFAOYSA-M dimethyl-(3-methyl-2-oxobut-3-enyl)-propylazanium;chloride Chemical compound [Cl-].CCC[N+](C)(C)CC(=O)C(C)=C KVFFVDVAFFSIIL-UHFFFAOYSA-M 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000004227 thermal cracking Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 229920006317 cationic polymer Polymers 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000002500 ions Chemical group 0.000 description 2
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- QBUKAFSEUHGMMX-MTJSOVHGSA-N (5z)-5-[[3-(1-hydroxyethyl)thiophen-2-yl]methylidene]-10-methoxy-2,2,4-trimethyl-1h-chromeno[3,4-f]quinolin-9-ol Chemical group C1=CC=2NC(C)(C)C=C(C)C=2C2=C1C=1C(OC)=C(O)C=CC=1O\C2=C/C=1SC=CC=1C(C)O QBUKAFSEUHGMMX-MTJSOVHGSA-N 0.000 description 1
- 206010012442 Dermatitis contact Diseases 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 208000003251 Pruritus Diseases 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical group [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 208000002029 allergic contact dermatitis Diseases 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000007743 anodising Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 229940117975 chromium trioxide Drugs 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N chromium trioxide Inorganic materials O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- GAMDZJFZMJECOS-UHFFFAOYSA-N chromium(6+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Cr+6] GAMDZJFZMJECOS-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 229910001701 hydrotalcite Inorganic materials 0.000 description 1
- 229960001545 hydrotalcite Drugs 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000007803 itching Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- DBJLJFTWODWSOF-UHFFFAOYSA-L nickel(ii) fluoride Chemical compound F[Ni]F DBJLJFTWODWSOF-UHFFFAOYSA-L 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical group [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/24—Chemical after-treatment
- C25D11/246—Chemical after-treatment for sealing layers
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention discloses a high-thermal-corrosion-resistance coating hole sealing agent, and belongs to the technical field of hole sealing agents. The basalt is treated by acid, then oxidized, the activity of the basalt is improved by using a surface active substance, the combination degree between the basalt and other macromolecular substances is enhanced by using organic silicon, gas is generated to emit heat when the basalt is heated, a boehmite component is formed in the longitudinal direction of a gap of the basalt by a hydrothermal method for nano-scale filling, so that the high temperature resistance is improved, the hot corrosion performance is improved, and the sealing and filling of the gap of a coating are completed; the thioglycollic acid is utilized to react with active centers or active groups such as Lewis acid on the surface of the vermiculite, so that the surface tension between particles is remarkably reduced under the action of high temperature, and a good hole sealing effect can be formed; magnesium and aluminum metal salt are used as raw materials, hydrotalcite-like compound components with good adsorbability are prepared by a hydrothermal method, chelation is generated by complexation, and the thermal corrosion resistance is improved. The invention solves the problem of poor high-temperature heat corrosion resistance of the conventional coating hole sealing agent.
Description
Technical Field
The invention relates to the technical field of hole sealing agents, in particular to a high-heat-corrosion-resistance coating hole sealing agent.
Background
Aluminum is one of the most widely distributed elements in nature. Pure aluminum is soft, small in density, good in ductility and high in plasticity, can be subjected to various machining processes, and has good electrical conductivity and thermal conductivity, and the electrical conductivity of the pure aluminum is second to that of the pure aluminum, so that the pure aluminum has wide application. Because pure aluminum has low strength, only by alloying it, can an aluminum alloy with low density and high strength be used as a structural material. The aluminum alloy material has a series of excellent physical, chemical, mechanical and processing properties, can meet various use requirements of various industries from kitchen utensils to advanced technologies, from building assembly industry to transportation industry and aerospace industry, and is widely applied to various fields of national economy.
Aluminum is a chemically active substance and forms a thin oxide film on the surface in air, which has good corrosion resistance in dry atmosphere, but does not have sufficient protective properties in polluted atmosphere and in water, seawater, soil and various corrosive media. Therefore, surface treatment is required for both aluminum and aluminum alloy surfaces in many cases, and anodizing is the most common surface treatment means for aluminum alloys. The method is that the aluminum alloy is soaked in acid electrolyte such as sulfuric acid, oxalic acid, phosphoric acid and other oxidizing liquid and certain external positive current is applied, so that a hard protective film with the thickness of dozens of microns and mainly composed of amorphous aluminum oxide can be formed on the surface of the aluminum alloy. The anodic oxide film has a double-layer structure, the inner layer is thin and compact, called a barrier layer, the outer layer is a thicker porous layer, the porous layer has excellent adsorption capacity and is often used as a bottom layer for coloring aluminum materials or a transition layer of an outer cover coating, but the corrosion resistance, the weather resistance, the pollution resistance and the like can not meet the use requirements, so from the practical application, the micropores of the aluminum anodic oxide film need to be sealed. The anode oxide film without holes is characterized in that the effective surface area of a workpiece or a sample exposed in the environment is increased by dozens of times to hundreds of times due to the area in a large number of micropores, so that the corresponding corrosion rate is greatly increased. Therefore, the anodic oxide film of aluminum must be subjected to a sealing treatment from the viewpoint of improving corrosion resistance and contamination resistance in addition to the respective hard oxide films such as abrasion resistant hard oxide films.
The common sealing operation methods in industry include 4 methods: high-temperature hole sealing, cold hole sealing, medium-temperature hole sealing and organic hole sealing.
High-temperature hole sealing, also called boiling water hole sealing, is realized by an oxide film (Al) on the surface of an aluminum product2O3) The boehmite body is good in corrosion resistance, and the micropores of the oxide film are closed by the expansion of the molecular volume of the oxide film during the hydration reaction. The cold sealing hole can be operated at room temperature without heating, so the hole sealing is called room temperature hole sealing. The cold sealing hole is generally made of nickel fluoride, and mainly depends on positive divalent nickel ions and negative monovalent fluorine ions.
The medium-temperature hole sealing refers to a hole sealing technology with the hole sealing temperature between high-temperature hole sealing and cold hole sealing, and the main hole sealing agent is nickel acetate, so that the stability is good and the control is easy.
And (4) sealing holes by using organic matters, namely coating an organic polymer coating on an aluminum oxide film.
In the prior aluminum alloy anodic oxidation post-treatment process, in order to reduce the void ratio and the adsorption capacity of an anodic oxide film, a large amount of sealant containing medium and low temperature is adopted, the sealant is fast in sealing, simple to operate, capable of effectively preventing the leaching of dye during sealing, high in impurity tolerance, extremely small in sealing weightlessness, and capable of meeting the requirements on product performance and appearance. However, since the nickel-containing metal ornament is in contact with human skin for a long time, Ni is dissociated under the action of human sweat stain2+The use of the sealing agent for itching skin and allergic contact dermatitis is prohibited in many countries, and relevant limiting standards are met, so that the development of a nickel-free sealing process capable of realizing mass production is urgent. There are many reports on the nickel-free sealing technology, but it is mature that: a nickel-free medium-temperature hole sealing agent of fluotitanate. The hole sealing agent is 5-10g/l potassium fluotitanate, 0.05-0.15g/l cyclohexanone and 0.05-0.15g/l isoamyl alcohol. The temperature of the hole sealing agent is 55-65 ℃ when hole sealing is carried out, and the treatment time is 1.0-1.5 um/min. Although the hole sealing agent solvesThe nickel is harmful to human bodies and pollutes the environment, but the coating hole sealing agent has the problem of poor high-temperature heat corrosion resistance.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problem that the conventional coating hole sealing agent has poor high-temperature heat corrosion resistance, the high-heat corrosion resistance coating hole sealing agent is provided.
In order to solve the technical problems, the invention adopts the following technical scheme:
the high-thermal-corrosion-resistance coating hole sealing agent comprises the following components in parts by weight: 3~7 parts of sodium tungstate, 0.2~0.5 parts of defoaming agent, 1~4 parts of dispersant, 25~50 parts of water, still include: 30-50 parts of composite hole sealing base material and 15-25 parts of auxiliary material.
The preparation method of the composite hole sealing base material comprises the following steps:
(1) at the temperature of 70-85 ℃, according to the mass ratio of 1: 12-20, mixing the basalt with a hydrochloric acid solution, preserving heat, filtering while hot, collecting filter residues according to a mass ratio of 1: adding 10-15 parts of periodic acid solution, mixing, keeping the temperature at 80-90 ℃, cooling, filtering, collecting filter cakes, washing, drying, collecting dried substances, grinding 15-30 parts of the dried substances, 2-5 parts of vinyltriethoxysilane, 3-7 parts of hexadecyltrimethylammonium bromide and 6-10 parts of absolute ethyl alcohol according to parts by weight, and collecting grinding materials;
(2) according to the weight portion, 30-40 portions of grinding materials, 17-23 portions of polyvinyl alcohol, 15-20 portions of dimethylacetamide, 4-7 portions of methacryloylpropyl trimethyl ammonium chloride and 50-70 portions of water are mixed, nitrogen is introduced for protection, stirring is carried out at 100-120 ℃, cooling and centrifugation are carried out, and the mass ratio of a centrifugate is 1: 6-10, adding the reagent A, mixing, stirring at the temperature of 50-65 ℃, filtering, collecting a filter cake, calcining to obtain a calcined substance, pulverizing and sieving the calcined substance, collecting and sieving particles, and obtaining the composite hole sealing base material.
The reagent A in the step (2): according to the mass ratio of 1: 2-4: and (3) mixing 30-50 parts of sodium metaaluminate, urea and water to obtain a reagent A.
The preparation of the auxiliary material comprises the following steps: at the temperature of 30-45 ℃, according to the mass ratio of 12-16: and 1, mixing the reagent B and water glass to obtain a mixture, adding an auxiliary agent accounting for 10-15% of the mass of the mixture into the mixture, raising the temperature to 120-145 ℃ in a closed manner, carrying out heat preservation reaction to obtain a reaction material, removing the closed condition, adding an additive accounting for 3-7% of the mass of the reaction material and pretreated vermiculite accounting for 7-13% of the mass of the reaction material, mixing and stirring, and carrying out rotary evaporation to obtain the auxiliary action material.
The reagent B: according to the weight parts, 5-8 parts of magnesium nitrate, 2-5 parts of aluminum nitrate, 6-10 parts of zinc nitrate and 150-200 parts of water are mixed to obtain a mixed salt solution, and the mixed salt solution is prepared from the following components in parts by mass: 1, adding carbamide and mixing to obtain a reagent B.
The auxiliary agent is as follows: according to the mass ratio of 3-6: 1, mixing potassium thiocyanate and sodium citrate to obtain the auxiliary agent.
The additive is as follows: taking fatty alcohol-polyoxyethylene ether at the temperature of 30-40 ℃ according to the mass ratio of 3-7: 1, adding triethanolamine and mixing to obtain a mixture, and mixing the mixture according to a mass ratio of 10: 1: and 2-5, adding hydroxyethyl cellulose and epoxy resin, and mixing to obtain the additive.
The pretreated vermiculite comprises the following components: taking vermiculite to be crushed and sieved at the temperature of 20-25 ℃, and taking sieved particles according to the mass ratio of 1: 3-7, adding dimethylformamide, uniformly mixing, heating to 30-45 ℃, adding mercaptoacetic acid accounting for 30-55% of the mass of the sieved particles and sodium bisulfate accounting for 12-20% of the mass of the sieved particles, mixing, sealing, and carrying out heat preservation reaction at 110-125 ℃ to obtain a reactant, wherein the mass ratio of the reactant is 20-35: 1, adding sodium sulfide, mixing, preserving heat, cooling, filtering, taking filter residue, washing with water, and drying to obtain the pretreated vermiculite.
The defoaming agent comprises the following components: according to the mass ratio of 1: and 3-7, mixing the polyoxypropyl polyoxyethyl glyceryl ether and the polydimethylsiloxane to obtain the defoaming agent.
The dispersing agent is as follows: according to the mass ratio of 2-5: 1, mixing vinyl distearamide and polyacrylamide to obtain the dispersing agent.
Compared with other methods, the method has the beneficial technical effects that:
(1) the invention firstly treats the basalt with acid, then oxidizes the basalt, improves the activity of the basalt with surface active substances, enhances the binding degree with other macromolecular substances by using organic silicon, and the basalt fine particle part is wrapped by utilizing the polyvinyl alcohol component, then the polymer is modified by using the long-chain cationic active substance, the cationic density is increased, the cationic polymer is formed and uniformly distributed in the polymer, under the action of high temperature, the cationic polymer can be decomposed, the generated gas can eliminate partial polar groups on the surface, simultaneously the released gas emits heat, and tiny pores are generated on the surface, the reagent A can be added to form boehmite components in the longitudinal direction of gaps of the reagent A by a hydrothermal method for nano filling, the high temperature resistance of the coating is improved, the hot corrosion performance can be improved, and the coating pores are sealed and filled;
(2) the invention utilizes thioglycollic acid to react with active centers or active groups such as Lewis acid and the like on the surface of the vermiculite, through covalent bonding and electrostatic interaction, the sulfur-containing group and internal free metal ions form stable complexes and can keep good compatibility with other internal components, and the expansion of vermiculite when heated can also strengthen the plugging effect, other substances in the vermiculite can play a filling role, and the additive is prepared by combining fatty alcohol-polyoxyethylene ether, triethanolamine and the like with epoxy resin, can remarkably reduce the surface tension among particles when being acted by high temperature, plays the role of emulsification foaming to a certain extent, forms tiny and non-through air bubbles, the continuity of capillaries in the hole sealing agent is damaged, open holes are changed into closed holes, especially under the action of continuous heat, defoaming can be accelerated, and a good hole sealing effect can be formed;
(3) the invention takes magnesium and aluminum metal salt as raw materials, has good adsorbability hydrotalcite-like component by a hydrothermal method, wherein sodium citrate contained in an auxiliary agent contains three carboxyl groups in the molecular structure, and can generate complexation with the formed hydrotalcite-like component in the hydrothermal process to form metal chelate particles, improve the dispersion stability of the hydrotalcite-like component, and induce the nucleation and crystallization process of crystals, and the ions can be vertically arranged between hydrotalcite layers in a single layer manner to obtain the hydrotalcite-like component with larger specific surface area, so that the contact effect between the hydrotalcite-like component and other components is enhanced, and the promotion of the thermal corrosion resistance is facilitated.
Detailed Description
Additive: taking fatty alcohol-polyoxyethylene ether at the temperature of 30-40 ℃ according to the mass ratio of 3-7: 1, adding triethanolamine and mixing for 30-60 min to obtain a mixture, wherein the mixture is prepared from the following raw materials in a mass ratio of 10: 1: and 2-5, adding hydroxyethyl cellulose and epoxy resin, and mixing to obtain the additive.
Reagent A: according to the mass ratio of 1: 2-4: and (3) mixing 30-50 parts of sodium metaaluminate, urea and water to obtain a reagent A.
And (3) reagent B: according to the weight parts, 5-8 parts of magnesium nitrate, 2-5 parts of aluminum nitrate, 6-10 parts of zinc nitrate and 150-200 parts of water are mixed to obtain a mixed salt solution, and the mixed salt solution is prepared from the following components in parts by mass: 1, adding carbamide and mixing to obtain a reagent B.
Auxiliary agent: according to the mass ratio of 3-6: 1, mixing potassium thiocyanate and sodium citrate to obtain the auxiliary agent.
Dispersing agent: according to the mass ratio of 2-5: 1, mixing vinyl distearamide and polyacrylamide to obtain the dispersing agent.
Defoaming agent: according to the mass ratio of 1: and 3-7, mixing the polyoxypropyl polyoxyethyl glyceryl ether and the polydimethylsiloxane to obtain the defoaming agent.
Pretreating vermiculite: at the temperature of 20-25 ℃, taking vermiculite to be crushed in a crusher and sieving the crushed vermiculite with a 100-mesh sieve, and taking sieved particles according to the mass ratio of 1: 3-7, adding dimethylformamide, uniformly mixing, heating to 30-45 ℃, adding mercaptoacetic acid accounting for 30-55% of the mass of the sieved particles and sodium bisulfate accounting for 12-20% of the mass of the sieved particles, mixing, sealing, and carrying out heat preservation reaction at 110-125 ℃ for 1-3 hours to obtain a reactant, wherein the mass ratio of the reactant is 20-35: 1, adding sodium sulfide, mixing, keeping the temperature for 40-60 min, naturally cooling to room temperature, filtering, taking filter residues, washing the filter residues with water for 2-4 times, and drying at 50-65 ℃ for 4-8 hours to obtain the pretreated vermiculite.
The preparation method of the composite hole sealing base material comprises the following steps:
(1) at the temperature of 70-85 ℃, according to the mass ratio of 1: 12-20, mixing basalt and a hydrochloric acid solution with the mass fraction of 12%, preserving heat for 1-3 hours at a speed of 400-700 r/min, filtering while hot, collecting filter residues according to a mass ratio of 1: adding 1mol/L periodic acid solution into 10-15 parts of the mixture, mixing the mixture, preserving heat for 45-60 min at 80-90 ℃, naturally cooling the mixture to room temperature, filtering the mixture, collecting filter cakes, washing the filter cakes with water for 2-4 times, transferring the filter cakes to an oven, drying the filter cakes for 3-5 h at 65-80 ℃, collecting dried substances, grinding 15-30 parts of the dried substances, 2-5 parts of vinyltriethoxysilane, 3-7 parts of hexadecyltrimethylammonium bromide and 6-10 parts of absolute ethyl alcohol in a mortar for 3-5 h according to parts by weight, and collecting grinding materials;
(2) according to the weight parts, 30-40 parts of grinding materials, 17-23 parts of polyvinyl alcohol, 15-20 parts of dimethylacetamide, 4-7 parts of methacryloylpropyl trimethyl ammonium chloride and 50-70 parts of water are mixed in a reaction kettle, nitrogen is introduced for protection, the mixture is stirred for 3-5 hours at 100-120 ℃ at 350-550 r/min, the mixture is naturally cooled to room temperature, the mixture is moved to a centrifuge and centrifuged for 12-25 minutes at 3000-4000 r/min, and the centrifugate is collected according to the mass ratio of 1: 6-10, adding the reagent A into a container, mixing, stirring for 25-55 min at a temperature of 50-65 ℃, filtering, collecting a filter cake, calcining for 2-4 h at a temperature of 500-700 ℃ to obtain a calcined substance, crushing the calcined substance in a crusher, sieving with a 150-mesh sieve, collecting sieved particles, and obtaining the composite hole sealing base material.
Preparation of auxiliary materials: at the temperature of 30-45 ℃, according to the mass ratio of 12-16: and 1, mixing a reagent B and water glass in a reaction kettle to obtain a mixture, adding an auxiliary agent accounting for 10-15% of the mass of the mixture into the mixture, heating the closed reaction kettle to 120-145 ℃, carrying out heat preservation reaction for 20-35 h to obtain a reaction material, removing the closure, adding an additive accounting for 3-7% of the mass of the reaction material and pretreated vermiculite accounting for 7-13% of the mass of the reaction material, mixing, stirring for 40-60 min at 2000-4000 r/min, and carrying out rotary evaporation at 60-75 ℃ to 30-45% of the original volume to obtain the auxiliary action material.
The high-thermal-corrosion-resistance coating hole sealing agent comprises the following components in parts by weight: 3-7 parts of sodium tungstate, 0.2-0.5 part of defoaming agent, 1-4 parts of dispersing agent, 25-50 parts of water, 30-50 parts of composite hole sealing base material and 15-25 parts of auxiliary material.
Example 1
Additive: taking fatty alcohol-polyoxyethylene ether at 30 ℃ according to a mass ratio of 3: 1, adding triethanolamine and mixing for 30min to obtain a mixture, and mixing the mixture according to a mass ratio of 10: 1: 2, adding hydroxyethyl cellulose and epoxy resin, and mixing to obtain the additive.
Reagent A: according to the mass ratio of 1: 2: 30 mixing sodium metaaluminate, urea and water to obtain the reagent A.
And (3) reagent B: mixing 5 parts of magnesium nitrate, 2 parts of aluminum nitrate, 6 parts of zinc nitrate and 150 parts of water according to parts by weight to obtain a mixed salt solution, wherein the mixed salt solution is prepared from the following components in parts by weight: 1, adding carbamide and mixing to obtain a reagent B.
Auxiliary agent: according to the mass ratio of 3: 1, mixing potassium thiocyanate and sodium citrate to obtain the auxiliary agent.
Dispersing agent: according to the mass ratio of 2: 1, mixing vinyl distearamide and polyacrylamide to obtain the dispersing agent.
Defoaming agent: according to the mass ratio of 1: and 3, mixing the polyoxypropyl polyoxyethyl glyceryl ether and the polydimethylsiloxane to obtain the defoaming agent.
Pretreating vermiculite: crushing vermiculite in a crusher at 20 ℃, sieving the crushed vermiculite with a 100-mesh sieve, and taking sieved particles according to a mass ratio of 1: 3, adding dimethylformamide, uniformly mixing, heating to 30 ℃, adding thioglycolic acid accounting for 30% of the mass of the sieved particles and sodium bisulfate accounting for 12% of the mass of the sieved particles, mixing, sealing, carrying out heat preservation reaction at 110 ℃ for 1 hour to obtain a reactant, and taking the reactant according to the mass ratio of 20: 1, adding sodium sulfide, mixing, keeping the temperature for 40min, naturally cooling to room temperature, filtering, taking filter residue, washing with water for 2 times, and drying at 50 ℃ for 4h to obtain the pretreated vermiculite.
The preparation method of the composite hole sealing base material comprises the following steps:
(1) at 70 ℃, according to the mass ratio of 1: 12, mixing basalt and a hydrochloric acid solution with the mass fraction of 12%, preserving heat for 1h at 400r/min, filtering while hot, collecting filter residues according to the mass ratio of 1: adding 1mol/L periodic acid solution into 10, mixing, keeping the temperature at 80 ℃ for 45min, naturally cooling to room temperature, filtering, collecting filter cakes, washing for 2 times by using water, transferring to an oven, drying at 65 ℃ for 3h, collecting dried substances, grinding 15 parts of the dried substances, 2 parts of vinyltriethoxysilane, 3 parts of hexadecyltrimethylammonium bromide and 6 parts of absolute ethyl alcohol in a mortar for 3h according to parts by weight, and collecting grinding media;
(2) according to the weight portion, 30 portions of grinding material, 17 portions of polyvinyl alcohol, 15 portions of dimethyl acetamide, 4 portions of methacryl propyl trimethyl ammonium chloride and 50 portions of water are mixed in a reaction kettle, nitrogen is introduced for protection, the mixture is stirred for 3 hours at 100 ℃ at 350r/min, the mixture is naturally cooled to room temperature, the mixture is moved to a centrifuge for centrifugation for 12 minutes at 3000r/min, and the centrifugation material is collected according to the mass ratio of 1: 6 adding the reagent A into a container, mixing, keeping the temperature at 50 ℃, stirring for 25min, filtering, collecting a filter cake, calcining for 2h at 500 ℃ to obtain a calcined substance, crushing the calcined substance in a crusher, sieving with a 150-mesh sieve, collecting sieved particles, and obtaining the composite hole sealing base material.
Preparation of auxiliary materials: at 30 ℃, according to the mass ratio of 12: 1, mixing a reagent B and water glass in a reaction kettle to obtain a mixture, adding an auxiliary agent accounting for 10% of the mass of the mixture into the mixture, heating the closed reaction kettle to 120 ℃, preserving heat, reacting for 20 hours to obtain a reaction material, removing the closure, adding an additive accounting for 3% of the mass of the reaction material and pretreated vermiculite accounting for 7% of the mass of the reaction material, mixing for 40 minutes at 2000r/min, and performing rotary evaporation at 60 ℃ to 30% of the original volume to obtain an auxiliary action material.
The high-thermal-corrosion-resistance coating hole sealing agent comprises the following components in parts by weight: 3 parts of sodium tungstate, 0.2 part of defoaming agent, 1 part of dispersing agent, 25 parts of water, 30 parts of composite hole sealing base material and 15 parts of auxiliary material.
Example 2
Additive: taking fatty alcohol-polyoxyethylene ether at 40 ℃ according to a mass ratio of 7: 1, adding triethanolamine and mixing for 60min to obtain a mixture, and mixing the mixture according to a mass ratio of 10: 1: and 5, adding hydroxyethyl cellulose and epoxy resin, and mixing to obtain the additive.
Reagent A: according to the mass ratio of 1: 4: 50, mixing sodium metaaluminate, urea and water to obtain a reagent A.
And (3) reagent B: mixing 8 parts of magnesium nitrate, 5 parts of aluminum nitrate, 10 parts of zinc nitrate and 200 parts of water according to parts by weight to obtain a mixed salt solution, wherein the mixed salt solution is prepared from the following components in parts by weight: 1, adding carbamide and mixing to obtain a reagent B.
Auxiliary agent: according to the mass ratio of 6: 1, mixing potassium thiocyanate and sodium citrate to obtain the auxiliary agent.
Dispersing agent: according to the mass ratio of 5: 1, mixing vinyl distearamide and polyacrylamide to obtain the dispersing agent.
Defoaming agent: according to the mass ratio of 1: and 7, mixing the polyoxypropyl polyoxyethyl glyceryl ether and the polydimethylsiloxane to obtain the defoaming agent.
Pretreating vermiculite: crushing vermiculite in a crusher at 25 ℃, sieving the crushed vermiculite with a 100-mesh sieve, and taking sieved particles according to a mass ratio of 1: and 7, adding dimethylformamide, uniformly mixing, heating to 45 ℃, adding thioglycolic acid accounting for 55% of the mass of the sieved particles and sodium bisulfate accounting for 20% of the mass of the sieved particles, mixing, sealing, carrying out heat preservation reaction at 125 ℃ for 3 hours to obtain a reactant, and taking the reactant according to the mass ratio of 35: 1, adding sodium sulfide, mixing, keeping the temperature for 60min, naturally cooling to room temperature, filtering, taking filter residue, washing with water for 4 times, and drying at 65 ℃ for 8h to obtain the pretreated vermiculite.
The preparation method of the composite hole sealing base material comprises the following steps:
(1) at 85 ℃, according to the mass ratio of 1: 20, mixing basalt with a hydrochloric acid solution with the mass fraction of 12%, preserving heat for 3 hours at 700r/min, filtering while hot, collecting filter residues according to a mass ratio of 1: adding 1mol/L periodic acid solution into the mixture 15, mixing the mixture, preserving heat at 90 ℃ for 60min, naturally cooling the mixture to room temperature, filtering the mixture, collecting filter cakes, washing the filter cakes with water for 4 times, transferring the filter cakes to an oven, drying the filter cakes at 80 ℃ for 5h, collecting dried substances, grinding 30 parts of the dried substances, 5 parts of vinyltriethoxysilane, 7 parts of hexadecyltrimethylammonium bromide and 10 parts of absolute ethyl alcohol in a mortar for 5h according to parts by weight, and collecting grinding media;
(2) taking 40 parts of grinding material, 23 parts of polyvinyl alcohol, 20 parts of dimethylacetamide, 7 parts of methacryl propyl trimethyl ammonium chloride and 70 parts of water, mixing in a reaction kettle, introducing nitrogen for protection, stirring at 120 ℃ at 550r/min for 5 hours, naturally cooling to room temperature, transferring to a centrifuge, centrifuging for 25min at 4000r/min, and collecting a centrifugal substance according to a mass ratio of 1: 10 adding the reagent A into a container, mixing, keeping the temperature at 65 ℃ and stirring for 55min, filtering, collecting a filter cake, calcining for 4h at 700 ℃ to obtain a calcined substance, crushing the calcined substance in a crusher, sieving with a 150-mesh sieve, collecting sieved particles, and obtaining the composite hole sealing base material.
Preparation of auxiliary materials: at 45 ℃, according to the mass ratio of 16: 1, mixing a reagent B and water glass in a reaction kettle to obtain a mixture, adding an auxiliary agent accounting for 15% of the mass of the mixture into the mixture, heating the closed reaction kettle to 145 ℃, preserving heat for reacting for 35 hours to obtain a reaction material, removing the closure, adding an additive accounting for 7% of the mass of the reaction material and pretreated vermiculite accounting for 13% of the mass of the reaction material, mixing for 60 minutes at 4000r/min, and performing rotary evaporation at 75 ℃ to reach 45% of the original volume to obtain an auxiliary action material.
The high-thermal-corrosion-resistance coating hole sealing agent comprises the following components in parts by weight: 7 parts of sodium tungstate, 0.5 part of defoaming agent, 4 parts of dispersing agent, 50 parts of water, 50 parts of composite hole sealing base material and 25 parts of auxiliary material.
Example 3
Additive: taking fatty alcohol-polyoxyethylene ether at 35 ℃ according to a mass ratio of 4: 1, adding triethanolamine and mixing for 50min to obtain a mixture, and mixing the mixture according to a mass ratio of 10: 1: and 3, adding hydroxyethyl cellulose and epoxy resin, and mixing to obtain the additive.
Reagent A: according to the mass ratio of 1: 3: 40 mixing sodium metaaluminate, urea and water to obtain the reagent A.
And (3) reagent B: mixing 7 parts of magnesium nitrate, 3 parts of aluminum nitrate, 8 parts of zinc nitrate and 180 parts of water according to parts by weight to obtain a mixed salt solution, wherein the mixed salt solution is prepared from the following components in parts by weight: 1, adding carbamide and mixing to obtain a reagent B.
Auxiliary agent: according to the mass ratio of 5: 1, mixing potassium thiocyanate and sodium citrate to obtain the auxiliary agent.
Dispersing agent: according to the mass ratio of 3: 1, mixing vinyl distearamide and polyacrylamide to obtain the dispersing agent.
Defoaming agent: according to the mass ratio of 1: and 4, mixing the polyoxypropyl polyoxyethyl glyceryl ether and the polydimethylsiloxane to obtain the defoaming agent.
Pretreating vermiculite: crushing vermiculite in a crusher at 22 ℃, sieving the crushed vermiculite with a 100-mesh sieve, and taking sieved particles according to a mass ratio of 1: and 5, adding dimethylformamide, uniformly mixing, heating to 35 ℃, adding thioglycolic acid accounting for 45% of the mass of the sieved particles and sodium bisulfate accounting for 16% of the mass of the sieved particles, mixing, sealing, carrying out heat preservation reaction at 115 ℃ for 2 hours to obtain a reactant, and taking the reactant according to the mass ratio of 25: 1, adding sodium sulfide, mixing, keeping the temperature for 50min, naturally cooling to room temperature, filtering, taking filter residue, washing with water for 3 times, and drying at 55 ℃ for 6h to obtain the pretreated vermiculite.
The preparation method of the composite hole sealing base material comprises the following steps:
(1) at 75 ℃, according to the mass ratio of 1: 15, mixing basalt with a hydrochloric acid solution with the mass fraction of 12%, preserving heat for 2 hours at a speed of 500r/min, filtering while hot, collecting filter residues according to a mass ratio of 1: 13 adding 1mol/L periodic acid solution, mixing, keeping the temperature at 85 ℃ for 50min, naturally cooling to room temperature, filtering, collecting filter cakes, washing the filter cakes with water for 3 times, transferring the filter cakes to an oven, drying the filter cakes at 70 ℃ for 4h, collecting dried substances, grinding 20 parts of the dried substances, 3 parts of vinyltriethoxysilane, 4 parts of hexadecyltrimethylammonium bromide and 8 parts of absolute ethyl alcohol in a mortar for 4h according to parts by mass, and collecting a grinding material;
(2) according to the weight portion, 35 portions of grinding material, 20 portions of polyvinyl alcohol, 19 portions of dimethyl acetamide, 5 portions of methacryl propyl trimethyl ammonium chloride and 60 portions of water are mixed in a reaction kettle, nitrogen is introduced for protection, the mixture is stirred for 4 hours at 110 ℃ at 450r/min, the mixture is naturally cooled to the room temperature, the mixture is moved to a centrifuge for centrifugation for 15 minutes at 3500r/min, and the centrifugation material is collected according to the mass ratio of 1: 8 adding the reagent A into a container, mixing, keeping the temperature at 55 ℃, stirring for 35min, filtering, collecting a filter cake, calcining for 3h at 600 ℃ to obtain a calcined substance, crushing the calcined substance in a crusher, sieving with a 150-mesh sieve, collecting sieved particles, and obtaining the composite hole sealing base material.
Preparation of auxiliary materials: at 35 ℃, according to the mass ratio of 15: 1, mixing a reagent B and water glass in a reaction kettle to obtain a mixture, adding an auxiliary agent accounting for 13% of the mass of the mixture into the mixture, heating the closed reaction kettle to 135 ℃, preserving heat and reacting for 25 hours to obtain a reaction material, removing the closure, adding an additive accounting for 5% of the mass of the reaction material and pretreated vermiculite accounting for 11% of the mass of the reaction material, mixing for 50 minutes at 3000r/min, and performing rotary evaporation at 65 ℃ to 35% of the original volume to obtain an auxiliary action material.
The high-thermal-corrosion-resistance coating hole sealing agent comprises the following components in parts by weight: 5 parts of sodium tungstate, 0.3 part of defoaming agent, 3 parts of dispersing agent, 30 parts of water, 40 parts of composite hole sealing base material and 20 parts of auxiliary material.
Comparative example 1: the preparation method is basically the same as that of example 1, except that the composite sealing binder is absent.
Comparative example 2: essentially the same procedure as in example 1, except for the absence of auxiliary materials.
Comparative example 3: sealing agent produced by a company of Changchun City.
The sealant obtained in the above examples and comparative examples is tested, and the method implements national standard GB/T8753.1-2005: the evaluation method of the sealing quality of the anodic oxide film of aluminum and aluminum alloy comprises the phosphoric chromic acid method without nitric acid presoaking in part 1. Specifically, the method comprises the following steps: after hole sealing, the aluminum material is firstly put into an acetone solvent for 30s, oil stain is removed, the aluminum material is vertically put into a drying oven preheated to 60 ℃ after air drying, drying is carried out for 15min, and then a sample is placed above silica gel in a sealed dryer and cooled for 30 min. Immediately weigh the sample mass (m)1) To the nearest 0.1 mg. Secondly, completely immersing the sample vertically in a corrosive liquid preheated to 38 +/-1 ℃ for 15min, taking out the test piece, cleaning and drying, and then putting the test piece into a drying oven preheated to 60 ℃ for drying for 15 min. The sample was then placed over silica gel in a sealed desiccator and cooled for 30 min. Immediately weigh the sample mass (m)2) To the nearest 0.1 mg. m is1And m2The difference value is the weight loss value, and the corrosion solution comprises the following components: 35mL of 85% wt phosphoric acid and 20g of chromium trioxide were dissolved in 500mL of water, and transferred to a 1000mL volumetric flask to a constant volume. The test of thermal cracking resistance is that the workpiece is firstly put into acetone solvent for 30s, oil stain is washed off, the workpiece is air-dried, then the workpiece is vertically put into a preheated oven with certain temperature, the workpiece is baked for one hour and taken out, whether cracks exist on the surface is observed by a visual method, if no cracks are observed by the visual method, an inspection method of oxide film continuity (copper sulfate method) is adopted, if no obvious change is observed on the surface, the workpiece can pass the test of thermal cracking resistance at the temperature, and the results are shown in table 1.
Table 1:
| detecting items | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Weight loss performance/mg/dm2 | 10.9 | 11.2 | 11.6 | 18.9 | 19.4 | 25.3 |
| Thermal cracking resistance/. degree.C | 100 | 98 | 99 | 85 | 87 | 80 |
In summary, it can be seen from table 1 that the sealant of the present invention is more effective and is worth popularizing, the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. The high-thermal-corrosion-resistance coating hole sealing agent comprises the following components in parts by weight: 3~7 parts of sodium tungstate, 0.2~0.5 parts of defoaming agent, 1~4 parts of dispersant, 25~50 parts of water, its characterized in that still includes: 30-50 parts of a composite hole sealing base material and 15-25 parts of an auxiliary material;
the preparation method of the composite hole sealing base material comprises the following steps:
(1) at the temperature of 70-85 ℃, according to the mass ratio of 1: 12-20, mixing the basalt with a hydrochloric acid solution, preserving heat, filtering while hot, collecting filter residues according to a mass ratio of 1: adding 10-15 parts of periodic acid solution, mixing, keeping the temperature at 80-90 ℃, cooling, filtering, collecting filter cakes, washing, drying, collecting dried substances, and grinding 15-30 parts of the dried substances, 2-5 parts of vinyltriethoxysilane, 3-7 parts of hexadecyltrimethylammonium bromide and 6-10 parts of absolute ethyl alcohol according to parts by weight to obtain a grinding material;
(2) according to the weight portion, 30-40 portions of grinding materials, 17-23 portions of polyvinyl alcohol, 15-20 portions of dimethylacetamide, 4-7 portions of methacryloylpropyl trimethyl ammonium chloride and 50-70 portions of water are mixed, nitrogen is introduced for protection, stirring is carried out at 100-120 ℃, cooling and centrifugation are carried out, and the mass ratio of a centrifugate is 1: 6-10, adding the reagent A, mixing, stirring at the temperature of 50-65 ℃, filtering, collecting a filter cake, calcining to obtain a calcined substance, crushing and sieving the calcined substance, collecting and sieving particles to obtain the composite hole sealing base material;
the preparation of the auxiliary material comprises the following steps: at the temperature of 30-45 ℃, according to the mass ratio of 12-16: and 1, mixing the reagent B and water glass to obtain a mixture, adding an auxiliary agent accounting for 10-15% of the mass of the mixture into the mixture, raising the temperature to 120-145 ℃ in a closed manner, carrying out heat preservation reaction to obtain a reaction material, removing the closed condition, adding an additive accounting for 3-7% of the mass of the reaction material and pretreated vermiculite accounting for 7-13% of the mass of the reaction material, mixing and stirring, and carrying out rotary evaporation to obtain the auxiliary action material.
2. The high thermal corrosion resistance coating sealant according to claim 1, wherein the ratio of reagent A: according to the mass ratio of 1: 2-4: and (3) mixing 30-50 parts of sodium metaaluminate, urea and water to obtain a reagent A.
3. The high thermal corrosion resistance coating sealant according to claim 1, wherein the ratio of the reagent B: according to the weight parts, 5-8 parts of magnesium nitrate, 2-5 parts of aluminum nitrate, 6-10 parts of zinc nitrate and 150-200 parts of water are mixed to obtain a mixed salt solution, and the mixed salt solution is prepared from the following components in parts by mass: 1, adding carbamide and mixing to obtain a reagent B.
4. The high thermal corrosion resistance coating sealant according to claim 1, wherein the additive: according to the mass ratio of 3-6: 1, mixing potassium thiocyanate and sodium citrate to obtain the auxiliary agent.
5. The high thermal corrosion resistance coating sealant according to claim 1, wherein the additive: taking fatty alcohol-polyoxyethylene ether at the temperature of 30-40 ℃ according to the mass ratio of 3-7: 1, adding triethanolamine and mixing to obtain a mixture, and mixing the mixture according to a mass ratio of 10: 1: and 2-5, adding hydroxyethyl cellulose and epoxy resin, and mixing to obtain the additive.
6. The high thermal corrosion resistance coating sealant according to claim 1, wherein the pre-treated vermiculite: taking vermiculite to be crushed and sieved at the temperature of 20-25 ℃, and taking sieved particles according to the mass ratio of 1: 3-7, adding dimethylformamide, uniformly mixing, heating to 30-45 ℃, adding mercaptoacetic acid accounting for 30-55% of the mass of the sieved particles and sodium bisulfate accounting for 12-20% of the mass of the sieved particles, mixing, sealing, and carrying out heat preservation reaction at 110-125 ℃ to obtain a reactant, wherein the mass ratio of the reactant is 20-35: 1, adding sodium sulfide, mixing, preserving heat, cooling, filtering, taking filter residue, washing with water, and drying to obtain the pretreated vermiculite.
7. The high thermal corrosion resistance coating sealant according to claim 1, wherein the defoamer: according to the mass ratio of 1: and 3-7, mixing the polyoxypropyl polyoxyethyl glyceryl ether and the polydimethylsiloxane to obtain the defoaming agent.
8. The high thermal corrosion resistance coating sealant according to claim 1, wherein the dispersant: according to the mass ratio of 2-5: 1, mixing vinyl distearamide and polyacrylamide to obtain the dispersing agent.
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| US4528073A (en) * | 1982-12-22 | 1985-07-09 | Seiko Instruments & Electronics Ltd. | Method for manufacturing multicolored plate, multicolored filter and multicolored display device |
| CN107740167A (en) * | 2017-09-05 | 2018-02-27 | 江苏飞拓界面工程科技有限公司 | A kind of ambient stable high-efficiency aluminum and aluminium alloy environmental protection sealer |
| CN109971219A (en) * | 2019-02-20 | 2019-07-05 | 常州鼎众冷暖设备工程有限公司 | A kind of preparation method of inorganic sealing hole agent |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4528073A (en) * | 1982-12-22 | 1985-07-09 | Seiko Instruments & Electronics Ltd. | Method for manufacturing multicolored plate, multicolored filter and multicolored display device |
| CN107740167A (en) * | 2017-09-05 | 2018-02-27 | 江苏飞拓界面工程科技有限公司 | A kind of ambient stable high-efficiency aluminum and aluminium alloy environmental protection sealer |
| CN109971219A (en) * | 2019-02-20 | 2019-07-05 | 常州鼎众冷暖设备工程有限公司 | A kind of preparation method of inorganic sealing hole agent |
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