CN116948579A - Water-based single-component epoxy fastening adhesive - Google Patents
Water-based single-component epoxy fastening adhesive Download PDFInfo
- Publication number
- CN116948579A CN116948579A CN202210382323.6A CN202210382323A CN116948579A CN 116948579 A CN116948579 A CN 116948579A CN 202210382323 A CN202210382323 A CN 202210382323A CN 116948579 A CN116948579 A CN 116948579A
- Authority
- CN
- China
- Prior art keywords
- epoxy
- epoxy resin
- water
- parts
- microcapsule
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000004593 Epoxy Substances 0.000 title claims abstract description 112
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000000853 adhesive Substances 0.000 title claims abstract description 52
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 52
- 239000003094 microcapsule Substances 0.000 claims abstract description 75
- 239000003822 epoxy resin Substances 0.000 claims abstract description 55
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 55
- 239000000203 mixture Substances 0.000 claims abstract description 43
- 229920002396 Polyurea Polymers 0.000 claims abstract description 35
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 35
- 239000002775 capsule Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000004850 liquid epoxy resins (LERs) Substances 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000013008 thixotropic agent Substances 0.000 claims abstract description 5
- 239000000049 pigment Substances 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 40
- 239000012948 isocyanate Substances 0.000 claims description 33
- 150000002513 isocyanates Chemical class 0.000 claims description 33
- 239000003292 glue Substances 0.000 claims description 29
- 229920000768 polyamine Polymers 0.000 claims description 17
- 239000000839 emulsion Substances 0.000 claims description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 13
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 13
- 125000001931 aliphatic group Chemical group 0.000 claims description 12
- -1 glycidyl ester Chemical class 0.000 claims description 11
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 10
- 239000003085 diluting agent Substances 0.000 claims description 10
- 238000012695 Interfacial polymerization Methods 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 125000003118 aryl group Chemical group 0.000 claims description 8
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 8
- 239000003995 emulsifying agent Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 6
- 229910021485 fumed silica Inorganic materials 0.000 claims description 6
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 6
- 230000007062 hydrolysis Effects 0.000 claims description 5
- 238000006460 hydrolysis reaction Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 5
- NNOZGCICXAYKLW-UHFFFAOYSA-N 1,2-bis(2-isocyanatopropan-2-yl)benzene Chemical compound O=C=NC(C)(C)C1=CC=CC=C1C(C)(C)N=C=O NNOZGCICXAYKLW-UHFFFAOYSA-N 0.000 claims description 4
- FKTHNVSLHLHISI-UHFFFAOYSA-N 1,2-bis(isocyanatomethyl)benzene Chemical compound O=C=NCC1=CC=CC=C1CN=C=O FKTHNVSLHLHISI-UHFFFAOYSA-N 0.000 claims description 4
- AOBIOSPNXBMOAT-UHFFFAOYSA-N 2-[2-(oxiran-2-ylmethoxy)ethoxymethyl]oxirane Chemical compound C1OC1COCCOCC1CO1 AOBIOSPNXBMOAT-UHFFFAOYSA-N 0.000 claims description 4
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 4
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims description 4
- 229920001577 copolymer Polymers 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 229920000058 polyacrylate Polymers 0.000 claims description 4
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 229920001451 polypropylene glycol Polymers 0.000 claims description 3
- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical compound CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 claims description 2
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 claims description 2
- YSUQLAYJZDEMOT-UHFFFAOYSA-N 2-(butoxymethyl)oxirane Chemical compound CCCCOCC1CO1 YSUQLAYJZDEMOT-UHFFFAOYSA-N 0.000 claims description 2
- QNYBOILAKBSWFG-UHFFFAOYSA-N 2-(phenylmethoxymethyl)oxirane Chemical compound C1OC1COCC1=CC=CC=C1 QNYBOILAKBSWFG-UHFFFAOYSA-N 0.000 claims description 2
- KFUSXMDYOPXKKT-UHFFFAOYSA-N 2-[(2-methylphenoxy)methyl]oxirane Chemical compound CC1=CC=CC=C1OCC1OC1 KFUSXMDYOPXKKT-UHFFFAOYSA-N 0.000 claims description 2
- WTYYGFLRBWMFRY-UHFFFAOYSA-N 2-[6-(oxiran-2-ylmethoxy)hexoxymethyl]oxirane Chemical compound C1OC1COCCCCCCOCC1CO1 WTYYGFLRBWMFRY-UHFFFAOYSA-N 0.000 claims description 2
- 229920000663 Hydroxyethyl cellulose Chemical class 0.000 claims description 2
- 239000004354 Hydroxyethyl cellulose Chemical class 0.000 claims description 2
- FQYUMYWMJTYZTK-UHFFFAOYSA-N Phenyl glycidyl ether Chemical compound C1OC1COC1=CC=CC=C1 FQYUMYWMJTYZTK-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- HIFVAOIJYDXIJG-UHFFFAOYSA-N benzylbenzene;isocyanic acid Chemical class N=C=O.N=C=O.C=1C=CC=CC=1CC1=CC=CC=C1 HIFVAOIJYDXIJG-UHFFFAOYSA-N 0.000 claims description 2
- 239000005038 ethylene vinyl acetate Substances 0.000 claims description 2
- 125000000623 heterocyclic group Chemical group 0.000 claims description 2
- 238000009775 high-speed stirring Methods 0.000 claims description 2
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 2
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims description 2
- AFEQENGXSMURHA-UHFFFAOYSA-N oxiran-2-ylmethanamine Chemical compound NCC1CO1 AFEQENGXSMURHA-UHFFFAOYSA-N 0.000 claims description 2
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 2
- 229920002401 polyacrylamide Polymers 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 239000005056 polyisocyanate Substances 0.000 claims description 2
- 229920001228 polyisocyanate Polymers 0.000 claims description 2
- 150000008442 polyphenolic compounds Chemical class 0.000 claims description 2
- 235000013824 polyphenols Nutrition 0.000 claims description 2
- 229920006295 polythiol Polymers 0.000 claims description 2
- 239000011118 polyvinyl acetate Substances 0.000 claims description 2
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 150000003512 tertiary amines Chemical class 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims 1
- 150000004985 diamines Chemical class 0.000 claims 1
- 229920000573 polyethylene Polymers 0.000 claims 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract description 22
- 238000003860 storage Methods 0.000 abstract description 16
- 238000000034 method Methods 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000002904 solvent Substances 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 4
- 231100000331 toxic Toxicity 0.000 abstract description 3
- 230000002588 toxic effect Effects 0.000 abstract description 3
- 238000013459 approach Methods 0.000 abstract description 2
- 229920001807 Urea-formaldehyde Polymers 0.000 description 13
- ODGAOXROABLFNM-UHFFFAOYSA-N polynoxylin Chemical compound O=C.NC(N)=O ODGAOXROABLFNM-UHFFFAOYSA-N 0.000 description 13
- 230000032683 aging Effects 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- 238000012360 testing method Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 238000006116 polymerization reaction Methods 0.000 description 7
- 239000003960 organic solvent Substances 0.000 description 6
- 125000002723 alicyclic group Chemical group 0.000 description 5
- 238000011065 in-situ storage Methods 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- OXEZLYIDQPBCBB-UHFFFAOYSA-N 4-(3-piperidin-4-ylpropyl)piperidine Chemical compound C1CNCCC1CCCC1CCNCC1 OXEZLYIDQPBCBB-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000004132 cross linking Methods 0.000 description 4
- 230000036541 health Effects 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 3
- 229920005739 STYRONAL® ND 811 Polymers 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 230000002411 adverse Effects 0.000 description 3
- 239000008346 aqueous phase Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 2
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- JCIIKRHCWVHVFF-UHFFFAOYSA-N 1,2,4-thiadiazol-5-amine;hydrochloride Chemical compound Cl.NC1=NC=NS1 JCIIKRHCWVHVFF-UHFFFAOYSA-N 0.000 description 1
- RNLHGQLZWXBQNY-UHFFFAOYSA-N 3-(aminomethyl)-3,5,5-trimethylcyclohexan-1-amine Chemical compound CC1(C)CC(N)CC(C)(CN)C1 RNLHGQLZWXBQNY-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 238000012645 aldehyde polymerization Methods 0.000 description 1
- 229910000288 alkali metal carbonate Inorganic materials 0.000 description 1
- 150000008041 alkali metal carbonates Chemical class 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 description 1
- 150000008051 alkyl sulfates Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000012975 dibutyltin dilaurate Substances 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000008098 formaldehyde solution Substances 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- LZKLAOYSENRNKR-LNTINUHCSA-N iron;(z)-4-oxoniumylidenepent-2-en-2-olate Chemical compound [Fe].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O LZKLAOYSENRNKR-LNTINUHCSA-N 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- DMTRWFMFBIMXBX-UHFFFAOYSA-L lead(2+);6-methylheptanoate Chemical compound [Pb+2].CC(C)CCCCC([O-])=O.CC(C)CCCCC([O-])=O DMTRWFMFBIMXBX-UHFFFAOYSA-L 0.000 description 1
- DSSXKBBEJCDMBT-UHFFFAOYSA-M lead(2+);octanoate Chemical compound [Pb+2].CCCCCCCC([O-])=O DSSXKBBEJCDMBT-UHFFFAOYSA-M 0.000 description 1
- YJOMWQQKPKLUBO-UHFFFAOYSA-L lead(2+);phthalate Chemical compound [Pb+2].[O-]C(=O)C1=CC=CC=C1C([O-])=O YJOMWQQKPKLUBO-UHFFFAOYSA-L 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- HSKWPCYTBKWRNQ-UHFFFAOYSA-M mercury(1+);naphthalene-1-carboxylate Chemical compound [Hg+].C1=CC=C2C(C(=O)[O-])=CC=CC2=C1 HSKWPCYTBKWRNQ-UHFFFAOYSA-M 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- GEMHFKXPOCTAIP-UHFFFAOYSA-N n,n-dimethyl-n'-phenylcarbamimidoyl chloride Chemical compound CN(C)C(Cl)=NC1=CC=CC=C1 GEMHFKXPOCTAIP-UHFFFAOYSA-N 0.000 description 1
- YWFWDNVOPHGWMX-UHFFFAOYSA-N n,n-dimethyldodecan-1-amine Chemical class CCCCCCCCCCCCN(C)C YWFWDNVOPHGWMX-UHFFFAOYSA-N 0.000 description 1
- 229940049964 oleate Drugs 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- OOCYPIXCHKROMD-UHFFFAOYSA-M phenyl(propanoyloxy)mercury Chemical compound CCC(=O)O[Hg]C1=CC=CC=C1 OOCYPIXCHKROMD-UHFFFAOYSA-M 0.000 description 1
- 229940096826 phenylmercuric acetate Drugs 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 229940096992 potassium oleate Drugs 0.000 description 1
- MLICVSDCCDDWMD-KVVVOXFISA-M potassium;(z)-octadec-9-enoate Chemical compound [K+].CCCCCCCC\C=C/CCCCCCCC([O-])=O MLICVSDCCDDWMD-KVVVOXFISA-M 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- WSFQLUVWDKCYSW-UHFFFAOYSA-M sodium;2-hydroxy-3-morpholin-4-ylpropane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CC(O)CN1CCOCC1 WSFQLUVWDKCYSW-UHFFFAOYSA-M 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- ADJMNWKZSCQHPS-UHFFFAOYSA-L zinc;6-methylheptanoate Chemical compound [Zn+2].CC(C)CCCCC([O-])=O.CC(C)CCCCC([O-])=O ADJMNWKZSCQHPS-UHFFFAOYSA-L 0.000 description 1
- CHJMFFKHPHCQIJ-UHFFFAOYSA-L zinc;octanoate Chemical compound [Zn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O CHJMFFKHPHCQIJ-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a water-based single-component epoxy fastening adhesive, which is prepared by mixing the following components in parts by weight: 15-65 parts of epoxy resin polyurea microcapsules, 3-40 parts of epoxy curing agent, 2-40 parts of film forming agent, 0-5 parts of thixotropic agent, 0-3 parts of pigment and 5-50 parts of water; the epoxy resin polyurea microcapsule consists of a capsule core and a wall material, wherein the capsule core of the epoxy resin polyurea microcapsule is liquid epoxy resin or liquid epoxy mixture, and the wall material of the epoxy resin polyurea microcapsule is polyurea. The invention solves the problem that the epoxy microcapsule fastening adhesive has poor storage stability when toxic formaldehyde and water-based epoxy microcapsule fastening adhesive are used in the production process, so that the process of microencapsulating the epoxy resin is safer and more environment-friendly, and the storage stability of the fastening adhesive reaches or approaches to the level of solvent-based epoxy microcapsule fastening adhesive.
Description
Technical Field
The invention relates to a water-based single-component epoxy fastening adhesive, and belongs to the technical field of precoated fastening adhesives.
Background
The single-component reactive precoating fastener glue of the epoxy resin microcapsule (hereinafter referred to as epoxy microcapsule fastening glue for short) is widely applied to locking and sealing of a threaded fastener, and the epoxy microcapsule fastening glue is generally microcapsule dispersion liquid, and the main components of the epoxy resin microcapsule comprise microcapsule-coated epoxy resin, an epoxy curing agent, a film forming agent, a touch adhesive and a solvent. Under normal temperature, the microcapsule wall can effectively separate the epoxy resin in the microcapsule core and the epoxy curing agent in the solution, so that the epoxy resin and the epoxy curing agent do not undergo a crosslinking reaction, and therefore, the microcapsule has good storage stability. When the fastener is used, the shearing force generated by the relative movement between the threads causes the microcapsule wall to be broken along with the screwing of the threads between the connecting pieces, and the epoxy resin flows out from the capsule core and then carries out cross-linking curing reaction with the epoxy curing agent, so that the locking and sealing of the threads are realized.
At present, some patents related to epoxy microcapsule fastening glue are disclosed at home and abroad, for example, patent application document with publication number CN104893635A filed by the technology of Nicotiana, inc. discloses a single-component screw locking epoxy pre-glue and a preparation method thereof, and for example, patent application document with publication number US5283266A filed by Three Bond Co Ltd. Compared with the traditional anaerobic precoating fastener adhesive, the epoxy microcapsule fastener adhesive has high strength and good moisture and temperature resistance, can be used repeatedly, and is simultaneously suitable for metal and plastic threaded fasteners. However, the existing epoxy microcapsule fastening adhesives are usually solvent type, and the products contain organic solvents such as toluene. In the process of gluing, the organic solvent may have an adverse effect on the health of the production personnel, and the organic solvent discharged from the production process may also cause environmental pollution. Therefore, the fastener adhesive industry needs an epoxy microcapsule fastener adhesive which is free of organic solvents and is safer and more environment-friendly.
The water-based epoxy microcapsule fastening adhesive replaces organic solvent with water, so that the adhesive is safer and more environment-friendly. There are also some patents of aqueous epoxy microcapsule fastening adhesives at home and abroad, such as aqueous adhesive compositions and polyurethane curing agents and adhesives disclosed in patent application document No. WO2005000990A2 filed by 3M company, and adhesive compositions and articles comprising the adhesives disclosed in patent application document No. WO2016040231A1 filed by ND Industrial inc. These patents all microcapsule epoxy resins by in situ polymerization (in-situ polymerization) and the microcapsule wall formed consists of urea-formaldehyde (urea-formaldehyde) polymers. In situ polymerization microencapsulation uses water-soluble polymeric monomers, the polymerization taking place in the aqueous phase, the resulting polymer migrating to the oil/water interface to form the microcapsule wall, and in situ polymerization generally using formaldehyde as the polymeric monomer. Formaldehyde is easy to volatilize, is a relatively high toxic substance capable of causing cancer and teratogenesis, and can threaten the health of production personnel after long-term contact with formaldehyde; and the formaldehyde-containing wastewater can cause environmental pollution if the wastewater can not be properly treated; in addition, the urea-formaldehyde polymer has certain hydrophilicity, and under the aqueous environment, microcapsule walls formed by the urea-formaldehyde polymer can swell to a certain extent, and when the epoxy curing agent exists in the aqueous phase, the microcapsule walls swell to accelerate the penetration of the epoxy curing agent into the capsule core and the reaction with the epoxy resin in the capsule core.
Therefore, the single-component aqueous epoxy microcapsule fastening adhesive has lower storage stability, and although the permeation of the epoxy curing agent to the capsule core can be slowed down by selecting different epoxy resins, epoxy curing agents and film forming agents, the storage stability of the single-component aqueous epoxy microcapsule fastening adhesive is still greatly different from that of solvent-type epoxy microcapsule fastening adhesive, and the storage and use of the fastening adhesive are inconvenient for users.
Disclosure of Invention
The invention solves the technical problems that: aiming at the problems of the epoxy microcapsule fastening adhesive, a novel water-based single-component epoxy fastening adhesive is provided.
The invention is realized by adopting the following technical scheme:
the water-based single-component epoxy fastening adhesive is prepared by mixing the following components in parts by weight: 15-65 parts of epoxy resin polyurea microcapsules, 3-40 parts of epoxy curing agent, 2-40 parts of film forming agent, 0-5 parts of thixotropic agent, 0-3 parts of pigment and 5-50 parts of water; the epoxy resin polyurea microcapsule consists of a capsule core and a wall material, wherein the capsule core is liquid epoxy resin or liquid epoxy mixture, and the wall material is polyurea.
In the water-based single-component epoxy fastening adhesive, specifically, the particle size of the epoxy resin polyurea microcapsule is 0.5-1000 microns, and the capsule core accounts for 30-95% of the total mass of the microcapsule.
Further preferably, the particle size of the epoxy resin polyurea microcapsule is 5 micrometers to 300 micrometers, and the capsule core accounts for 50 to 90 percent of the total mass of the microcapsule.
In the water-based single-component epoxy fastening adhesive, the wall material of the epoxy resin polyurea microcapsule is specifically formed by interfacial polymerization reaction participated by the multifunctional group isocyanate, and the specific steps are as follows:
(1) Adding 40-95 parts of liquid epoxy resin and 4-49 parts of multifunctional isocyanate into a beaker, and fully mixing to prepare uniform mixed solution;
(2) Adding 1-5 parts of an emulsifying agent or a dispersing agent into the reaction flask, and stirring to enable the emulsifying agent or the dispersing agent to be fully dissolved or dispersed in 100-500 parts of water;
(3) Adding the mixed solution into the reaction flask for dispersion under high-speed stirring;
(4) Then adding 1-15 parts of water-soluble polyamine or isocyanate hydrolysis promoter into the reaction flask, and starting interfacial polymerization reaction;
(5) After reacting for 0-2 hours at normal temperature, the reaction temperature is increased to 40-95 ℃, and then the reaction is continued for 0.5-3 hours;
(6) After the reaction is finished, the epoxy resin polyurea microcapsule powder is prepared through neutralization, filtration, washing and drying.
In the water-based one-component epoxy fastening adhesive of the present invention, specifically, the liquid epoxy resin has a viscosity of less than 50000mpa.s at 25 ℃, and the liquid epoxy resin includes, but is not limited to, bisphenol a type epoxy resin, bisphenol F type epoxy resin, polyphenol type glycidyl ether epoxy resin, aliphatic glycidyl ether epoxy resin, glycidyl ester type epoxy resin, glycidyl amine type epoxy resin, epoxidized olefin compound, heterocyclic type and hybrid type epoxy resin.
In the water-based single-component epoxy fastening adhesive, specifically, the viscosity of the epoxy mixture is less than 50000mPa.s at 25 ℃, the liquid epoxy mixture is mixed with the epoxy diluent according to the mass ratio of 1-20:1, and the epoxy diluent comprises but is not limited to butyl glycidyl ether, alkylene glycidyl ether, 1, 4-dibutanol diglycidyl ether, ethylene glycol diglycidyl ether, phenyl glycidyl ether, polypropylene glycol diglycidyl ether, C12-C14 aliphatic glycidyl ether, benzyl glycidyl ether, 1, 6-hexanediol diglycidyl ether, o-tolylglycidyl ether and Xin Wu glycol diglycidyl ether. . The epoxy diluent comprises an inactive diluent and an active diluent, wherein the epoxy inactive diluent plays roles of diluting and reducing the viscosity of the epoxy resin and does not react with the epoxy resin and the epoxy curing agent; epoxy reactive diluents refer to low molecular weight compounds with one or more epoxy groups that can directly participate in the curing reaction of the epoxy resin as part of the crosslinked network structure of the epoxy resin cure.
In the water-based single-component epoxy fastening adhesive, specifically, the multifunctional isocyanate comprises aromatic multifunctional isocyanate, aliphatic multifunctional isocyanate and a mixture of the aromatic multifunctional isocyanate and the aliphatic multifunctional isocyanate, wherein the molecular structure of the mixture contains two or more isocyanate groups,
the aromatic polyfunctional isocyanates include, but are not limited to, toluene Diisocyanate (TDI), diphenylmethane diisocyanate (MDI), polymeric diphenylmethane diisocyanate (polymeric MDI), diphenylmethane diisocyanate derivatives (MDI derivatives) and blends (blends) and prepolymers thereof,
the aliphatic polyisocyanates include, but are not limited to, hexamethylene Diisocyanate (HDI), isophorone diisocyanate (IPDI), dicyclohexylmethane-4, 4-diisocyanate (HMDI), xylylene Diisocyanate (XDI), tetramethylxylylene diisocyanate (TMXDI), and blends (blends) and prepolymers (prepolymers) thereof.
In the water-based one-component epoxy fastening glue of the present invention, the emulsifier or dispersant includes, but is not limited to, polyoxyethylene ether, polyoxypropylene ether, ethylene oxide and propylene oxide block copolymer, polyvinyl alcohol, polyol fatty acid ester, sodium alkylbenzenesulfonate, alkyl sulfate, N-dodecyl dimethylamine and other amine derivatives, pickering (Pickering) emulsifier. The emulsifier and the dispersant can reduce the interfacial tension of the epoxy resin or the epoxy mixture and water, so that the epoxy resin or the epoxy mixture forms a uniform and stable dispersion system material in the water.
In the water-based one-component epoxy fastening adhesive of the present invention, specifically, the water-soluble polyamine refers to a compound which is soluble in water and has two or more active amino groups, including but not limited to ethylenediamine, diethylenetriamine, triethyltetramine, tetraethylpentamine, 1, 3-dipropylamine, 1, 4-dibutylamine, 1, 6-hexamethylenediamine, isophoronediamine.
In the water-based one-component epoxy fastening glue, the isocyanate hydrolysis accelerator is a compound capable of accelerating the reaction of isocyanate and water and accelerating the polymerization reaction of multifunctional isocyanate at an oil/water interface, and comprises, but is not limited to, alkali metal hydroxide, alkaline earth metal hydroxide, alkali metal carbonate (including hydride), ammonia water, stannous octoate, dibutyl tin dilaurate, lead isooctanoate, lead octoate, zinc isooctanoate, zinc octoate, mercury octoate, phenylmercuric acetate, mercury naphthalate, phenylmercuric propionate, phenylmercuric oleate, lead phthalate, iron acetylacetonate, zinc naphthenate, cobalt naphthenate and potassium oleate.
In the water-based one-component epoxy fastening glue, the epoxy curing agent comprises aliphatic polyamine, alicyclic polyamine, aromatic polyamine, polythiol, tertiary amine (2, 4, 6-tris (dimethylaminomethyl) phenol) and polyethylenediamine. The epoxy curing agent is solid at normal temperature and normal pressure, can be dissolved in water at normal temperature and normal pressure or can be uniformly dispersed in water phase, and can be subjected to crosslinking curing reaction with liquid epoxy resin or liquid epoxy mixture.
In the water-based one-component epoxy fastening glue, the thixotropic agent comprises fumed silica, hydroxyethyl cellulose derivatives, polyvinyl alcohol and polyacrylate water-soluble resins for an aqueous system.
In the water-based single-component epoxy fastening adhesive, the film forming agent is an organic polymer material which can be dissolved in water or uniformly dispersed in water phase and can form a continuous film, and the film forming agent comprises polyvinyl alcohol, polyacrylamide, polyethylene glycol, polyvinyl butyral dispersion liquid, polyvinyl acetate emulsion, ethylene-vinyl acetate copolymer emulsion, ethylene-vinyl acetate-ethylene chloride copolymer emulsion, polyacrylate emulsion, styrene-acrylate copolymer emulsion and styrene-butadiene copolymer emulsion.
In the epoxy resin polyurea microcapsule of the invention, the polyurea wall material is generated by interfacial polymerization reaction of multifunctional isocyanate and polyamine or isocyanate hydrolysis accelerator.
The epoxy resin polyurea microcapsule is produced through interfacial polymerization reaction participated by the multifunctional isocyanate. The interfacial polymerization means that a polycondensation polymerization reaction occurs at the interface of the oil/water two phases. The epoxy resin polyurea microcapsule polyurea wall material prepared by the method has compact structure and hydrophobic performance, and can effectively isolate the liquid epoxy resin or epoxy mixture of the capsule core and the epoxy curing agent in the fastening glue phase in the aqueous environment, prevent the epoxy curing agent from penetrating and reacting the capsule core through the wall material, so that the aqueous single-component fastening glue has good storage stability.
The water-based one-component epoxy fastening glue is coated on the threaded surface of the fastener to form a solid coating, and the solid coating has good adhesive force on the threaded surface of the fastener. When the fastener is used, the shearing force generated by the relative movement between the threads enables the epoxy resin polyurea microcapsules to be mechanically broken, liquid epoxy resin or liquid epoxy mixture flows out of the microcapsule cores and is subjected to cross-linking curing reaction with the epoxy curing agent dispersed in the solid coating, so that the locking and sealing of the bolt are realized.
The invention has the following beneficial effects:
(1) The invention can replace solvent type single-component fastening glue used in the current market, does not use organic solvent, avoids adverse effect of using solvent on health of glue spreading personnel, and is beneficial to reducing environmental pollution.
(2) The invention adopts a multifunctional isocyanate/polyamine or multifunctional isocyanate/isocyanate hydrolysis accelerator interfacial polymerization method to synthesize the polyurea microcapsule taking epoxy resin or epoxy mixture as a capsule core. Compared with the traditional in-situ polymerization method for preparing the epoxy microcapsule, the interfacial polymerization method avoids using toxic formaldehyde as a reactant, reduces adverse effects of the microencapsulation process on the health of production personnel, avoids generating wastewater containing formaldehyde, and is beneficial to reducing the damage to the environment.
(3) Compared with the water-based reactive single-component fastening adhesive based on the urea-formaldehyde epoxy microcapsule, the polyurea epoxy microcapsule adopted by the invention has better room-temperature storage stability, and the good storage stability is derived from the good hydrophobic property of the capsule wall of the polyurea epoxy microcapsule. Under the aqueous environment, the hydrophobic capsule wall can effectively separate the epoxy resin or the epoxy mixture of the capsule core from the epoxy curing agent in water, and the curing reaction of the epoxy resin or the epoxy mixture in water during storage is avoided or reduced, so that the storage period of the single-component fastening adhesive is prolonged.
In summary, the water-based single-component epoxy fastening glue provided by the invention solves the problem that the storage stability of the epoxy microcapsule fastening glue is poor due to toxic formaldehyde and the water-based epoxy microcapsule fastening glue in the production process, so that the process of microencapsulating the epoxy resin is safer and more environment-friendly, and the storage stability of the fastening glue reaches or approaches to the level of solvent-based epoxy microcapsule fastening glue.
The invention is further described below in conjunction with the detailed description.
Detailed Description
Comparative example (Urea-aldehyde polymerization)
The comparative example is a specific example of an epoxy resin microcapsule for preparing an epoxy fastening glue by adopting urea-formaldehyde (urea-formaldehyde) polymer in the prior art, and the specific preparation steps are as follows:
the first step: 68g of bisphenol A epoxy resin (CYD-128 of Baling petrochemical Co., ltd.) and 17g of epoxy diluent (LS-501 of Hubei green home materials science and technology Co., ltd.) were sequentially added into a 100mL beaker, and the mixture was sufficiently stirred to obtain an epoxy mixture A.
And a second step of: 20g of urea, 4g of melamine, 0.5g of triethylamine and 60g of 37% formaldehyde solution are sequentially added into a 500mL three-necked flask at room temperature, the mixture is heated to 75 ℃ after being uniformly mixed, the reaction temperature is reduced to room temperature after 2 hours of reaction, and 120g of deionized water is added to obtain a urea-formaldehyde prepolymer solution B.
And a third step of: to the urea-formaldehyde prepolymer solution B, 2g of sodium chloride and 85g of epoxy mixture A were added in this order with high stirring at 1000 rpm. After 10 minutes of full dispersion, concentrated sulfuric acid (98%) was added dropwise to the suspension until ph=2.5, then the reaction temperature was raised to 65 ℃ and kept for 4 hours of reaction, after the reaction was completed, the product was suction-filtered, washed to neutrality with deionized water, and dried with an oven to obtain urea-formaldehyde microcapsule powder.
Fourth step: a comparative one-component reactive pre-coat fastening adhesive was obtained by uniformly mixing 20g of urea-formaldehyde microcapsule powder, 15g of deionized water, 4.6g of styrene-butadiene copolymer emulsion (film former, styronal ND811 of Basoff company), 7.0g of alicyclic polyamine epoxy curing agent (1, 3-bis (4-piperidinyl) propane), and 0.2g of fumed silica.
Example 1
The first step: 68g of bisphenol A epoxy resin CYD-128 and 17g of epoxy diluent (Hubei green home materials science and technology Co., ltd., LS-501) are sequentially added into a 100mL beaker, and the mixture is stirred uniformly to obtain an epoxy mixture A. To the epoxy mixture A, 15g of polyfunctional isocyanate (Wannate PM-200) was added and mixed uniformly to obtain an epoxy/isocyanate mixture C.
And a second step of: 200g of deionized water and 2g of polyvinyl alcohol were added in sequence to a 500mL three-necked flask at room temperature, and the mixture was rapidly stirred (1000 rpm) until the polyvinyl alcohol was completely dissolved. To the polyvinyl alcohol solution was added 100g of epoxy/isocyanate mixture C with rapid stirring (1000 rpm). After 15 minutes of sufficient dispersion, 7.4g of diethylenetriamine (water-soluble polyamine) was added to the suspension, and the reaction was continued at room temperature for 1 hour. The reaction temperature was raised to 65℃and after a further 1 hour the reaction was cooled to room temperature. A 10% hydrochloric acid solution was added dropwise until ph=7.0. And after the reaction is finished, filtering the product, fully washing the product with deionized water, and drying the product by using an oven to obtain polyurea microcapsule powder D.
And a third step of: a single-component reactive pre-coat fastening adhesive of this example was obtained by uniformly mixing 20g of polyurea microcapsule powder D, 15g of deionized water, 4.6g of styrene-butadiene copolymer emulsion (film former, styronal ND811, basf Co.), 7.0g of alicyclic polyamine epoxy curing agent (1, 3-bis (4-piperidinyl) propane), and 0.2g of fumed silica.
Example 2
The single-component reactive pre-coat fastening adhesive of this example was obtained by uniformly mixing 20g of polyurea microcapsule powder D prepared in example 1, 17.5g of deionized water, 2.5g of polyvinyl alcohol (film forming agent), 7.0g of alicyclic polyamine epoxy curing agent (1, 3-bis (4-piperidinyl) propane), and 0.2g of fumed silica.
Example 3
The first step: 85g of bisphenol A epoxy resin CYD-128 and 15g of polyfunctional isocyanate (Wannate PM-200) were sequentially added to a 100mL beaker and mixed uniformly to obtain an epoxy/isocyanate mixture E.
And a second step of: 200g of deionized water and 2g of polyvinyl alcohol were added in sequence to a 500mL three-necked flask at room temperature, and the mixture was rapidly stirred (1000 rpm) until the polyvinyl alcohol was completely dissolved. After the temperature of the polyvinyl alcohol solution had risen to 65℃100g of the epoxy/isocyanate mixture E were added to the polyvinyl alcohol solution with rapid stirring (1000 rpm). After 15 minutes of adequate dispersion, 7.4g of diethylenetriamine (water-soluble polyamine) was added to the suspension. After continuing the reaction at 65℃for 1 hour, the reaction was cooled to room temperature. A 10% hydrochloric acid solution was added dropwise until ph=7.0. And after the reaction is finished, filtering the product, fully washing the product with deionized water, and drying the product by using an oven to obtain polyurea microcapsule powder F.
And a third step of: a single-component reactive pre-coat fastening adhesive of this example was obtained by uniformly mixing 20g of polyurea microcapsule powder F, 15g of deionized water, 4.6g of styrene-butadiene copolymer emulsion (film former, styronal ND811, basf Co.), 7.0g of alicyclic polyamine epoxy curing agent (1, 3-bis (4-piperidinyl) propane), and 0.2g of fumed silica.
Performance test:
the single-component reactive precoated fastening glue prepared in the comparative example and the examples 1-3 is uniformly coated on 8.8-grade M10 galvanized bolts for performance comparison test, the bolts coated with the fastening glue are respectively placed into a 90 ℃ oven for 30 minutes, and nuts are assembled after cooling to room temperature. The screwing-in torque, the loosening torque and the screwing-out torque of the bolt after the bolt is screwed into the nut for 24 hours under the conditions of no pretightening force and room temperature are tested according to GB/T35480-2017. To test the storage stability of the one-component reactive pre-coat fastening adhesive, the freshly prepared one-component reactive pre-coat fastening adhesive was put into a 50 ℃ oven for 10 days of aging. And uniformly coating the aged single-component reactive precoated fastening adhesive on an 8.8-grade M10 galvanized color bolt, putting the bolt into a 90 ℃ oven for 30 minutes, and assembling the nut after cooling to room temperature. The screwing-in torque, the loosening torque and the screwing-out torque of the bolt after the bolt is screwed into the nut for 24 hours under the conditions of no pretightening force and room temperature are tested according to GB/T35480-2017.
The test results are shown in Table I:
table one: single-component reactive precoated epoxy fastening adhesive test result
The comparison of the properties of the adhesive before and after aging can be used to demonstrate the storage stability of the adhesive. From the results shown in Table I, the viscosity of the comparative example before aging was similar to that of the examples, and the screwing-in torque, the loosening torque and the unscrewing torque all satisfied the GB/T35480-2017 requirements. After aging, the comparative examples showed severe gels, lost fluidity, and could not be applied to test bolts for testing. The comparative example shows gel during the aging test, which indicates that the urea-formaldehyde microcapsule wall material cannot effectively isolate the epoxy mixture of the microcapsule core and the epoxy curing agent in the aqueous solution, and the curing reaction of the two materials occurs under the aging test condition. The viscosity of examples 1-3 increased slightly after aging, but still had good flowability, compared to before aging, and the gumming test was possible. This demonstrates that the polyurea microcapsule wall material can effectively isolate the epoxy mixture of the microcapsule core from the epoxy curing agent in the aqueous phase under the aging experimental conditions. The screwing-in torque, loosening torque and unscrewing torque before and after ageing of examples 1-3 all meet the requirements of GB/T35480-2017. The results in Table I demonstrate that examples 1-3 using polyurea microcapsules have better storage stability than the comparative examples using urea-formaldehyde microcapsules.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the above-described embodiments, and that the above-described embodiments and descriptions are only preferred embodiments of the present invention, and are not intended to limit the invention, and that various changes and modifications may be made therein without departing from the spirit and scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The water-based single-component epoxy fastening adhesive is characterized by being prepared by mixing the following components in parts by weight: 15-65 parts of epoxy resin polyurea microcapsules, 3-40 parts of epoxy curing agent, 2-40 parts of film forming agent, 0-5 parts of thixotropic agent, 0-3 parts of pigment and 5-50 parts of water; the epoxy resin polyurea microcapsule consists of a capsule core and a wall material, wherein the capsule core is liquid epoxy resin or liquid epoxy mixture, and the wall material is polyurea.
2. The water-based single-component epoxy fastening glue according to claim 1, wherein the particle size of the epoxy resin polyurea microcapsule is 0.5-1000 microns, and the capsule core accounts for 30-95% of the total mass of the microcapsule.
3. The water-based single-component epoxy fastening adhesive according to claim 2, wherein the particle size of the epoxy resin polyurea microcapsule is 5-300 microns, and the capsule core accounts for 50-90% of the total mass of the microcapsule.
4. The water-based single-component epoxy fastening adhesive according to claim 1, wherein the wall material of the epoxy resin polyurea microcapsule is generated by interfacial polymerization reaction participated by multifunctional isocyanate, and the specific steps are as follows:
(1) Adding 40-95 parts of liquid epoxy resin and 4-49 parts of multifunctional isocyanate into a beaker, and fully mixing to prepare uniform mixed solution;
(2) Adding 1-5 parts of an emulsifying agent or a dispersing agent into the reaction flask, and stirring to enable the emulsifying agent or the dispersing agent to be fully dissolved or dispersed in 100-500 parts of water;
(3) Adding the mixed solution into the reaction flask for dispersion under high-speed stirring;
(4) Then adding 1-15 parts of water-soluble polyamine or isocyanate hydrolysis promoter into the reaction flask, and starting interfacial polymerization reaction;
(5) After reacting for 0-2 hours at normal temperature, the reaction temperature is increased to 40-95 ℃, and then the reaction is continued for 0.5-3 hours;
(6) After the reaction is finished, the epoxy resin polyurea microcapsule powder is prepared through neutralization, filtration, washing and drying.
5. The water-based one-component epoxy fastening glue of claim 1, the liquid epoxy resin having a viscosity of less than 50000mpa.s at 25 ℃, the liquid epoxy resin including, but not limited to, bisphenol a type epoxy resin, bisphenol F type epoxy resin, polyphenol type glycidyl ether epoxy resin, aliphatic glycidyl ether epoxy resin, glycidyl ester type epoxy resin, glycidyl amine type epoxy resin, epoxidized olefin compound, heterocyclic type and hybrid type epoxy resin.
6. The water-based one-component epoxy fastening glue of claim 1, the epoxy mixture having a viscosity of less than 50000mpa.s at 25 ℃, the liquid epoxy mixture being mixed by the liquid epoxy resin and an epoxy diluent including, but not limited to, butyl glycidyl ether, alkylene glycidyl ether, 1, 4-dibutanol diglycidyl ether, ethylene glycol diglycidyl ether, phenyl glycidyl ether, polypropylene glycol diglycidyl ether, C12-C14 aliphatic glycidyl ether, benzyl glycidyl ether, 1, 6-hexanediol diglycidyl ether, o-tolyl glycidyl ether, xin Wu glycol diglycidyl ether in a mass ratio of 1-20:1.
7. The water-based one-component epoxy fastening glue of claim 1, the multi-functional isocyanate comprising an aromatic multi-functional isocyanate, an aliphatic multi-functional isocyanate, and a mixture of an aromatic multi-functional isocyanate and an aliphatic multi-functional isocyanate, wherein
The aromatic polyfunctional isocyanates include, but are not limited to, toluene Diisocyanate (TDI), diphenylmethane diisocyanate (MDI), polymeric diphenylmethane diisocyanate (polymeric MDI), diphenylmethane diisocyanate derivatives (MDI derivatives) and blends (blends) and prepolymers thereof,
the aliphatic polyisocyanates include, but are not limited to, hexamethylene Diisocyanate (HDI), isophorone diisocyanate (IPDI), dicyclohexylmethane-4, 4-diisocyanate (HMDI), xylylene Diisocyanate (XDI), tetramethylxylylene diisocyanate (TMXDI), and blends (blends) and prepolymers (prepolymers) thereof.
8. The water-based one-component epoxy fastening glue of claim 1, the epoxy curing agent including, but not limited to, aliphatic polyamines, cycloaliphatic polyamines, aromatic polyamines, polythiols, tertiary amines (2, 4, 6-tris (dimethylaminomethyl) phenol), polyethylene diamine.
9. The water-based one-component epoxy fastening glue of claim 1, the thixotropic agent comprising fumed silica, hydroxyethylcellulose derivative, polyvinyl alcohol, polyacrylate water-soluble resin for aqueous systems.
10. The water-based one-component epoxy fastening glue of claim 1, the film forming agent including, but not limited to, polyvinyl alcohol, polyacrylamide, polyethylene glycol, polyvinyl butyral dispersion, polyvinyl acetate emulsion, ethylene-vinyl acetate copolymer emulsion, ethylene-vinyl acetate-ethylene chloride copolymer emulsion, polyacrylate emulsion, styrene-acrylate copolymer emulsion, styrene-butadiene copolymer emulsion.
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