CN114479743A - Reactive polyurethane hot melt adhesive for TWS earphone bonding and preparation method thereof - Google Patents
Reactive polyurethane hot melt adhesive for TWS earphone bonding and preparation method thereof Download PDFInfo
- Publication number
- CN114479743A CN114479743A CN202210216893.8A CN202210216893A CN114479743A CN 114479743 A CN114479743 A CN 114479743A CN 202210216893 A CN202210216893 A CN 202210216893A CN 114479743 A CN114479743 A CN 114479743A
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- CN
- China
- Prior art keywords
- parts
- bonding
- hot melt
- melt adhesive
- polyurethane hot
- Prior art date
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- 239000004814 polyurethane Substances 0.000 title claims abstract description 27
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 25
- 239000004831 Hot glue Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229920005906 polyester polyol Polymers 0.000 claims abstract description 27
- 239000004925 Acrylic resin Substances 0.000 claims abstract description 19
- 229920000178 Acrylic resin Polymers 0.000 claims abstract description 19
- 230000009477 glass transition Effects 0.000 claims abstract description 14
- 229920005862 polyol Polymers 0.000 claims abstract description 13
- 150000003077 polyols Chemical class 0.000 claims abstract description 13
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 12
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000000853 adhesive Substances 0.000 claims abstract description 10
- 230000001070 adhesive effect Effects 0.000 claims abstract description 10
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 7
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 229920000570 polyether Polymers 0.000 claims abstract description 7
- 239000005056 polyisocyanate Substances 0.000 claims abstract description 7
- 229920001228 polyisocyanate Polymers 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 12
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 12
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 11
- 239000004917 carbon fiber Substances 0.000 claims description 11
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 8
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 8
- 239000004417 polycarbonate Substances 0.000 claims description 8
- 238000005086 pumping Methods 0.000 claims description 8
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims description 8
- 229910052582 BN Inorganic materials 0.000 claims description 7
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- -1 polyoxypropylene Polymers 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- 235000019270 ammonium chloride Nutrition 0.000 claims description 6
- 229910021538 borax Inorganic materials 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229920001610 polycaprolactone Polymers 0.000 claims description 6
- 239000004632 polycaprolactone Substances 0.000 claims description 6
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 6
- 239000004328 sodium tetraborate Substances 0.000 claims description 6
- 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 6
- 150000002009 diols Chemical class 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- QSRJVOOOWGXUDY-UHFFFAOYSA-N 2-[2-[2-[3-(3-tert-butyl-4-hydroxy-5-methylphenyl)propanoyloxy]ethoxy]ethoxy]ethyl 3-(3-tert-butyl-4-hydroxy-5-methylphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C)=CC(CCC(=O)OCCOCCOCCOC(=O)CCC=2C=C(C(O)=C(C)C=2)C(C)(C)C)=C1 QSRJVOOOWGXUDY-UHFFFAOYSA-N 0.000 claims description 4
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 4
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 4
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 4
- 239000001361 adipic acid Substances 0.000 claims description 4
- 235000011037 adipic acid Nutrition 0.000 claims description 4
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 claims description 4
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 4
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 4
- 238000006068 polycondensation reaction Methods 0.000 claims description 4
- DCQBZYNUSLHVJC-UHFFFAOYSA-N 3-triethoxysilylpropane-1-thiol Chemical compound CCO[Si](OCC)(OCC)CCCS DCQBZYNUSLHVJC-UHFFFAOYSA-N 0.000 claims description 3
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 3
- 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 3
- 229920000515 polycarbonate Polymers 0.000 claims description 3
- 229920001451 polypropylene glycol Polymers 0.000 claims description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 2
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 2
- FMGBDYLOANULLW-UHFFFAOYSA-N 3-isocyanatopropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCN=C=O FMGBDYLOANULLW-UHFFFAOYSA-N 0.000 claims description 2
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 2
- ZMSQJSMSLXVTKN-UHFFFAOYSA-N 4-[2-(2-morpholin-4-ylethoxy)ethyl]morpholine Chemical compound C1COCCN1CCOCCN1CCOCC1 ZMSQJSMSLXVTKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 2
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 2
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 2
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 2
- IAXXETNIOYFMLW-COPLHBTASA-N [(1s,3s,4s)-4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl] 2-methylprop-2-enoate Chemical compound C1C[C@]2(C)[C@@H](OC(=O)C(=C)C)C[C@H]1C2(C)C IAXXETNIOYFMLW-COPLHBTASA-N 0.000 claims description 2
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 2
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 2
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims description 2
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 2
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 2
- 229940119545 isobornyl methacrylate Drugs 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
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 229920000909 polytetrahydrofuran Polymers 0.000 claims description 2
- 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 claims description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 2
- 210000004243 sweat Anatomy 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 4
- 239000003292 glue Substances 0.000 description 16
- 238000012360 testing method Methods 0.000 description 14
- 230000032683 aging Effects 0.000 description 9
- 239000011521 glass Substances 0.000 description 9
- 239000002585 base Substances 0.000 description 8
- 239000000945 filler Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 238000004026 adhesive bonding Methods 0.000 description 5
- 239000004744 fabric Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 229920001730 Moisture cure polyurethane Polymers 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 239000012948 isocyanate Substances 0.000 description 3
- 210000001503 joint Anatomy 0.000 description 3
- 238000007639 printing Methods 0.000 description 3
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000011167 hydrochloric acid Nutrition 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 238000004804 winding Methods 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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4266—Polycondensates having carboxylic or carbonic ester groups in the main chain prepared from hydroxycarboxylic acids and/or lactones
- C08G18/4269—Lactones
- C08G18/4277—Caprolactone and/or substituted caprolactone
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/44—Polycarbonates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to a reactive polyurethane hot melt adhesive for bonding TWS earphones and a preparation method thereof, wherein the reactive polyurethane hot melt adhesive comprises the following components in parts by weight: 10-30 parts of polyether polyol; 10-30 parts of crystalline polyester polyol; 10-30 parts of liquid polyester polyol; 20-30 parts of high glass transition temperature acrylic resin; 15-25 parts of polyisocyanate; 15-30 parts of modified perovskite wire; 0.01-1 part of catalyst; 0.1-3 parts of a silane coupling agent; 0.01-1 part of antioxidant. The adhesive prepared by the invention is suitable for bonding the shell and the shell of TWS earphone equipment, has the characteristics of high curing speed, high initial adhesion strength, sweat resistance and the like, has the waterproof grade of 5ATM, can shorten the pressure maintaining time to 30 minutes in the assembling process of the TWS earphone, and greatly improves the assembling efficiency of a TWS earphone production line.
Description
Technical Field
The invention relates to an adhesive, in particular to a reactive polyurethane hot melt adhesive for bonding a TWS (two-way clutch) earphone and a preparation method thereof.
Background
TWS is an abbreviation of True Wireless Stereo, True Wireless Stereo. With the rapid development of the bluetooth technology and the pursuit of people for the characteristics of light weight, high efficiency and the like of wearing products, the TWS headset goes into the visual field of users and is accepted and favored by more and more people. Compared with the traditional wired earphone, the TWS earphone gets rid of the constraint of an earphone wire, avoids the troubles of winding, wire breaking, stethoscope effect and the like, and has the advantages of portability, attractive appearance and the like. At present, the pressure maintaining time for gluing for structural part bonding in the industries of mobile phones, flat plates, intelligent wearing and earphones in the market is usually 2 hours, but due to the fact that the TWS earphones are complex in structure, large in part quantity and various in production and assembly processes, the quick positioning is realized for structural part bonding glue in urgent need of short pressure maintaining products, and the production efficiency of a production line is improved. TWS earphones are widely applied and are often used in the process of sports, and the TWS earphones put higher requirements on the waterproof and sweat aging resistance of the adhesive for structural bonding.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a reactive polyurethane hot melt adhesive (hereinafter referred to as PUR hot melt adhesive) for bonding a TWS earphone and a preparation method thereof, wherein the prepared PUR hot melt adhesive has the advantages of high curing speed, high initial adhesion strength and sweat resistance, meets the 5ATM waterproof requirement, can shorten the pressure holding time to 30 minutes in the TWS assembling process, and greatly improves the assembling efficiency of a TWS earphone production line.
The technical scheme of the invention is as follows:
a reactive polyurethane hot melt adhesive for bonding a TWS earphone is characterized by comprising the following components in parts by weight:
10-30 parts of polyether polyol;
10-30 parts of crystalline polyester polyol;
10-30 parts of liquid polyester polyol;
20-30 parts of high glass transition temperature acrylic resin;
15-25 parts of polyisocyanate;
15-30 parts of perovskite powder;
0.01-1 part of catalyst;
0.1-3 parts of a silane coupling agent;
0.01-1 part of antioxidant.
Further, the polyether polyol is one or more of polyoxypropylene glycol, polyoxypropylene-oxyethylene glycol and polytetrahydrofuran glycol with the molecular weight of 1000-4000.
Further, the crystalline polyester polyol is one or more of adipic acid and sebacic acid, and one or more of polyester polyol, polycaprolactone polyol and polycarbonate diol with the molecular weight of 1000-6000 are obtained through polycondensation reaction with one or more of ethylene glycol, propylene glycol, 1, 4-butanediol, diethylene glycol, 1, 6-hexanediol and neopentyl glycol.
Further, the liquid polyester polyol is one or more of adipic acid, sebacic acid, phthalic anhydride, isophthalic acid and terephthalic acid, and is an oligomer with the molecular weight of 1000-6000, which is obtained by polycondensation with one or more of ethylene glycol, propylene glycol, 1, 4-butanediol, diethylene glycol, 1, 6-hexanediol and neopentyl glycol.
Further, the high glass transition temperature acrylic resin is a high molecular compound which is obtained by one or more of methyl methacrylate, butyl methacrylate, hydroxyethyl methacrylate, isobornyl methacrylate, methyl acrylate and butyl acrylate through high molecular polymerization reaction and has a glass transition temperature (Tg) of 65-85 ℃ and a molecular weight of 8000-80000.
Further, the polyisocyanate is one or more of toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate and hexamethylene diisocyanate.
Further, the catalyst is one or more of triethyldiamine, dimorpholinodiethyl ether, triethylamine, dibutyltin dilaurate and stannous octoate.
Further, the silane coupling agent is one or more of gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-mercaptopropyltrimethoxysilane, gamma-mercaptopropyltriethoxysilane, gamma-isocyanatopropyltrimethoxysilane and gamma-isocyanatopropyltriethoxysilane.
Further, the antioxidant is one or more of an antioxidant 245, an antioxidant 1010, an antioxidant 1035 and an antioxidant 1076.
A preparation method of a reactive polyurethane hot melt adhesive for bonding a TWS earphone is characterized by comprising the following steps:
adding polyether polyol, crystalline polyester polyol, liquid polyester polyol and high glass transition temperature acrylic resin into a reaction kettle, vacuumizing and dehydrating at 140-150 ℃ for 2-3h until the water content is less than 200ppm, and cooling to 80-90 ℃; adding polyisocyanate and perovskite into the system while stirring under the protection of nitrogen, after the addition is finished, carrying out vacuum pumping reaction, slowly heating to 105-115 ℃, keeping the temperature for 2-3h, adding a catalyst, a silane coupling agent and an antioxidant under the protection of nitrogen, and carrying out vacuum pumping reaction for 0.5-1h to obtain a polyurethane adhesive;
the preparation method of the modified perovskite filament comprises the steps of mixing borax, perovskite, filamentous carbon fibers, 12% of mass fraction ammonium chloride solution and 15% of solubility hydrochloric acid according to the weight portion ratio of 1:1:1:10:10, putting the mixture into a stirrer, reacting for 1-2 hours at the temperature of 35-50 ℃, filtering, cleaning and drying to obtain the modified perovskite filament wrapped in the carbon fiber filament and filled with boron nitride.
By the scheme, the invention at least has the following advantages:
the invention mainly uses acrylic resin with high glass transition temperature when preparing polyurethane prepolymer. The thermoplastic acrylic resin is used as one of tackifying resins, has good compatibility with polyurethane prepolymer, and can adjust the melting viscosity of a system. The acrylic resin has various types, different glass transition temperatures, and the acrylic resin with high glass transition temperature at room temperature has higher conversion speed, can shorten the positioning time and obtain higher initial bonding strength. Meanwhile, the acrylic resin has high polarity and forms stronger interaction with a solid substrate to obtain better wetting effect, thereby greatly improving the bonding property to the substrate. The acrylic resin has good weather resistance, chemical resistance and water resistance, and can improve the weather resistance and acid and alkali resistance of the whole system when added into the polyurethane prepolymer.
The invention has another innovation point that the modified perovskite wire is used as the filler, when the glue is cured after the modified perovskite wire is used as the filler, the filler can also extend to the bonding surface of the whole TWS earphone due to the fact that the filler is distributed in the modified perovskite wire, and the hardness of the perovskite wire of the filler is far greater than that of the plastic of the TWS earphone, so that the filler can penetrate into the plastic through external force extrusion after bonding, and a firmer connecting structure is formed.
As for the filler, boron nitride is generated through the reaction of borax, hydrochloric acid and ammonium chloride, the perovskite has the characteristic of porosity, the generated boron nitride can enter the air, and meanwhile, due to the existence of the carbon fiber yarns, the three components are mutually wrapped and wound to form a stable connection structure.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
Adding 10 parts of polyoxypropylene glycol with the molecular weight of 1000, 10 parts of crystalline polyester polyol (polycaprolactone polyol with the molecular weight of 1000), 10 parts of liquid polyester polyol (with the molecular weight of 1000) and 20 parts of high-glass transition temperature acrylic resin (with the molecular weight of 8000 and the Tg of 65 ℃) into a reaction kettle, vacuumizing and dehydrating at 140 ℃ for 2-h until the water content is less than 200ppm, and cooling to 80 ℃; adding 15 parts of toluene diisocyanate and 15 parts of modified perovskite filament into the system while stirring under the protection of nitrogen, vacuumizing for reaction after the addition is finished, slowly heating to 105 ℃, keeping for 2 hours, adding 0.01 part of dimorpholinyl diethyl ether agent, 0.1 part of gamma-aminopropyl trimethoxy silane and 0.01 part of antioxidant under the protection of nitrogen, and vacuumizing for reaction for 0.5-hours to obtain a polyurethane adhesive;
the preparation method of the modified perovskite filament comprises the steps of mixing borax, perovskite, filamentous carbon fibers, 12% of mass fraction ammonium chloride solution and 15% of solubility hydrochloric acid according to the weight portion ratio of 1:1:1:10:10, putting the mixture into a stirrer, and reacting for 1 hour at the temperature of 35 ℃ to obtain the modified perovskite filament wrapped in the carbon fiber filament and filled with boron nitride.
Example 2
Adding 20 parts of polyoxypropylene-ethylene oxide glycol with the molecular weight of 2000, 20 parts of crystalline polyester polyol (polycarbonate glycol with the molecular weight of 3000), 20 parts of liquid polyester polyol (molecular weight of 3000) and 25 parts of high-glass transition temperature acrylic resin (the molecular weight of 20000 and the Tg of 75 ℃) into a reaction kettle, vacuumizing and dehydrating at 145 ℃ for 2.5h until the water content is less than 200ppm, and cooling to 85 ℃; adding 20 parts of diphenylmethane diisocyanate and 20 parts of modified perovskite filaments into the system while stirring under the protection of nitrogen, performing vacuum pumping reaction after the addition is finished, slowly heating to 110 ℃, keeping the temperature for 2.5 hours, adding 0.5 part of triethyldiamine, 1 part of gamma-mercaptopropyltriethoxysilane and 0.5 part of antioxidant 1035 under the protection of nitrogen, and performing vacuum pumping reaction for 0.7 hour to obtain a polyurethane adhesive;
the preparation method of the modified perovskite filament comprises the steps of mixing borax, perovskite, filamentous carbon fibers, 12% of mass fraction ammonium chloride solution and 15% of solubility hydrochloric acid according to the weight portion ratio of 1:1:1:10:10, putting the mixture into a stirrer, and reacting for 1-2 hours at the temperature of 35-50 ℃ to obtain the modified perovskite filament wrapped in the carbon fiber filament and filled with boron nitride.
Example 3
Adding 30 parts of polyoxypropylene-ethylene oxide glycol with the molecular weight of 4000, 30 parts of crystalline polyester polyol (polycaprolactone polyol with the molecular weight of 6000), 30 parts of liquid polyester polyol (molecular weight of 6000) and 30 parts of acrylic resin with high glass transition temperature (the molecular weight of 80000 and Tg of 85 ℃) into a reaction kettle, vacuumizing and dehydrating at 150 ℃ for 3 hours until the water content is less than 200ppm, and cooling to 90 ℃; adding 25 parts of toluene diisocyanate and 30 parts of modified perovskite filament into the system while stirring under the protection of nitrogen, after the addition is finished, performing vacuum pumping reaction, slowly heating to 115 ℃, keeping the temperature for 3 hours, adding 1 part of triethyldiamine, 3 parts of gamma-isocyanate propyl triethoxysilane and 1 part of antioxidant 245 under the protection of nitrogen, and performing vacuum pumping reaction for 1 hour to obtain a polyurethane adhesive;
the preparation method of the modified perovskite filament comprises the steps of mixing borax, perovskite, filamentous carbon fibers, 12% of mass fraction ammonium chloride solution and 15% of solubility hydrochloric acid according to the weight portion ratio of 1:1:1:10:10, putting the mixture into a stirrer, and reacting for 2 hours at the temperature of 50 ℃ to obtain the modified perovskite filament wrapped in the carbon fiber filament and filled with boron nitride.
Comparative example 1
Adding 30 parts of polyoxypropylene-ethylene oxide glycol with the molecular weight of 4000, 30 parts of crystalline polyester polyol (polycaprolactone polyol with the molecular weight of 6000), 30 parts of liquid polyester polyol (molecular weight of 6000) and 30 parts of acrylic resin into a reaction kettle, vacuumizing and dehydrating at 150 ℃ for 3 hours until the water content is less than 200ppm, and cooling to 90 ℃; adding 25 parts of toluene diisocyanate and 30 parts of modified perovskite filaments into the system while stirring under the protection of nitrogen, vacuumizing for reaction after the addition is finished, slowly heating to 115 ℃, keeping the temperature for 3 hours, adding 1 part of triethyldiamine, 3 parts of gamma-isocyanate propyl triethoxysilane and 1 part of antioxidant 245 under the protection of nitrogen, and vacuumizing for reaction for 1 hour to obtain the polyurethane adhesive.
Comparative example 1 is different from the above examples in that the acrylic resin is a conventional resin.
Comparative example 2
Adding 30 parts of polyoxypropylene-ethylene oxide glycol with the molecular weight of 4000, 30 parts of crystalline polyester polyol (polycaprolactone polyol with the molecular weight of 6000), 30 parts of liquid polyester polyol (molecular weight of 6000) and 30 parts of acrylic resin with high glass transition temperature (the molecular weight of 80000 and Tg of 85 ℃) into a reaction kettle, vacuumizing and dehydrating at 150 ℃ for 3 hours until the water content is less than 200ppm, and cooling to 90 ℃; adding 25 parts of toluene diisocyanate into the system while stirring under the protection of nitrogen, vacuumizing for reaction after the addition is finished, slowly heating to 115 ℃, keeping for 3 hours, adding 1 part of triethyldiamine, 3 parts of gamma-isocyanate propyl triethoxysilane and 245, 1 part of antioxidant under the protection of nitrogen, and vacuumizing for reaction for 1 hour to obtain the polyurethane adhesive.
Comparative example 2 differs from the above examples in that no modified perovskite filaments were used as filler.
The following table shows the results of the performance tests of examples 1-3 and comparative examples 1-2:
the acid-base aging strength test is a shear bonding strength test, the bonding strength test base material is PC + GF// ink glass, and the waterproof and acid-base aging waterproof sample test base materials are PC + GF// transparent glass and PA + GF// transparent glass.
The test methods of examples 1-5 and comparative examples of the present invention are as follows:
and (3) viscosity testing:
the temperature was 110. + -. 1 ℃ using a Brookfield DV2T viscometer, using a 27 spindle.
Testing the butt joint bonding strength:
gluing a PC + GF (90mm x 50mm x 5mm) substrate by using a glue sprayer, wherein the glue line is in a circular shape with the diameter of 25.4mm, the width of the glue line is 1mm after the glue line is pressed, the thickness of the glue line is 0.15mm, the printing ink glass (50mm x 6mm) substrate is pressed on the circular glue line, the pressure is maintained for 0.5h by using a 1kg weight, the weight is taken down to test the butt joint bonding strength for 0.5h, and the butt joint bonding strength is tested after the printing ink glass is cured for 72 h. Curing conditions are as follows: the temperature is 23 +/-2 ℃, and the humidity is 60 +/-10% RH; testing speed: 10 mm/min.
Acid-base aging strength test:
and (3) gluing the PC + GF (101.6mm by 25.4mm by 2mm) base material by using a glue sprayer, wherein the size of a glue line is 25.4mm linear, the width is 1mm after the gluing is carried out, the thickness of the glue layer is 0.15mm, the printing ink glass (101.6mm by 25.4mm by 2mm) base material is pressed on the glue line, the pressure is maintained for 0.5h by using a 1kg weight, and the weight is taken down and cured for 72 h. Preparing acidic artificial sweat with pH value of 4.7 and alkaline artificial sweat with pH value of 9.5, soaking the acidic artificial sweat and the alkaline artificial sweat respectively in dust-free cloth, wrapping the sample with the dust-free cloth soaked with the artificial sweat, sealing the sample with a valve bag, aging the sample in an aging box with temperature and humidity of 55 ℃/95% RH for 72h, taking out the sample, standing the sample at room temperature for 1 day, and testing the shearing and bonding strength. Curing conditions are as follows: the temperature is 23 +/-2 ℃, and the humidity is 60 +/-10% RH; testing speed: 10 mm/min.
50m waterproof test:
the method comprises the steps of gluing a transparent glass (101.6mm × 25.4mm × 2mm) substrate by a glue sprayer, placing yellow water-sensitive paper with the size of 5mm × 0.1mm in a rectangular glue line with the size of 20.4mm × 96.6mm rectangle, the width of 0.4-0.6mm after lamination and the thickness of a glue layer of 0.1mm, laminating PC + GF (101.6mm × 25.4mm × 2mm) or PA + GF (101.6mm × 25.4mm × 2mm) substrate on the glue line, maintaining the pressure for 0.5h by using 2 weights of 1kg, taking down the weights and curing for 72 h. Putting the sample into water, pressurizing at 0.5MPa, keeping for 30min, and observing whether the yellow water-sensitive paper in the sample turns blue or not after pressure relief, wherein the yellow water-sensitive paper is unqualified if the yellow water-sensitive paper turns blue, and the yellow water-sensitive paper is marked as 'N', and the yellow water-sensitive paper is qualified if the yellow water-sensitive paper turns yellow, and is marked as 'Y'. Curing conditions are as follows: the temperature is 23 +/-2 ℃, and the humidity is 60 +/-10% RH.
50m water resistance + acid-base aging test:
preparing acidic artificial sweat with pH value of 4.7 and alkaline artificial sweat with pH value of 9.5, soaking with dust-free cloth, wrapping the dust-free cloth soaked with artificial sweat with a waterproof sample, sealing with a valve bag, aging in an aging oven with temperature and humidity of 55 ℃/95% RH for 72h, taking out, standing at room temperature for 1 day, and performing 50m waterproof test.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A reactive polyurethane hot melt adhesive for bonding a TWS earphone is characterized by comprising the following components in parts by weight:
10-30 parts of polyether polyol;
10-30 parts of crystalline polyester polyol;
10-30 parts of liquid polyester polyol;
20-30 parts of high glass transition temperature acrylic resin;
15-25 parts of polyisocyanate;
15-30 parts of modified perovskite wire;
0.01-1 part of catalyst;
0.1-3 parts of a silane coupling agent;
0.01-1 part of antioxidant.
2. The reactive polyurethane hot melt adhesive for bonding the TWS earphones according to claim 1, wherein: the polyether polyol is one or the mixture of more than two of polyoxypropylene diol, polyoxypropylene-oxyethylene diol and polytetrahydrofuran diol with the molecular weight of 1000-4000.
3. The reactive polyurethane hot melt adhesive for bonding the TWS earphones according to claim 1, wherein: the crystalline polyester polyol is one or more of adipic acid and sebacic acid, and one or more of polyester polyol, polycaprolactone polyol and polycarbonate diol with the molecular weight of 1000-6000 are obtained by the polycondensation reaction of the crystalline polyester polyol and one or more of ethylene glycol, propylene glycol, 1, 4-butanediol, diethylene glycol, 1, 6-hexanediol and neopentyl glycol.
4. The reactive polyurethane hot melt adhesive for bonding the TWS earphones according to claim 1, wherein: the liquid polyester polyol is one or more of adipic acid, sebacic acid, phthalic anhydride, isophthalic acid and terephthalic acid, and is an oligomer with the molecular weight of 1000-6000, which is obtained by the polycondensation reaction of one or more of ethylene glycol, propylene glycol, 1, 4-butanediol, diethylene glycol, 1, 6-hexanediol and neopentyl glycol.
5. The reactive polyurethane hot melt adhesive for bonding the TWS earphones according to claim 1, wherein: the high glass transition temperature acrylic resin is a high molecular compound which is obtained by one or more of methyl methacrylate, butyl methacrylate, hydroxyethyl methacrylate, isobornyl methacrylate, methyl acrylate and butyl acrylate through high molecular polymerization reaction and has the glass transition temperature (Tg) of 8000-80000 and 65-85 ℃.
6. The reactive polyurethane hot melt adhesive for bonding the TWS earphones according to claim 1, wherein: the polyisocyanate is one or more of toluene diisocyanate, diphenylmethane diisocyanate, isophorone diisocyanate and hexamethylene diisocyanate.
7. The reactive polyurethane hot melt adhesive for bonding the TWS earphones according to claim 1, wherein: the catalyst is one or more of triethyldiamine, dimorpholinodiethyl ether, triethylamine, dibutyltin dilaurate and stannous octoate.
8. The reactive polyurethane hot melt adhesive for bonding the TWS earphones according to claim 1, wherein: the silane coupling agent is one or more of gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-mercaptopropyltrimethoxysilane, gamma-mercaptopropyltriethoxysilane, gamma-isocyanatopropyltrimethoxysilane and gamma-isocyanatopropyltriethoxysilane.
9. The reactive polyurethane hot melt adhesive for bonding the TWS earphones according to claim 1, wherein: the antioxidant is one or more of antioxidant 245, antioxidant 1010, antioxidant 1035 and antioxidant 1076.
10. A preparation method of a reactive polyurethane hot melt adhesive for bonding a TWS earphone is characterized by comprising the following steps:
adding polyether polyol, crystalline polyester polyol, liquid polyester polyol and high glass transition temperature acrylic resin into a reaction kettle, vacuumizing and dehydrating at 140-150 ℃ for 2-3h until the water content is less than 200ppm, and cooling to 80-90 ℃; adding polyisocyanate and modified perovskite filament into the system while stirring under the protection of nitrogen, performing vacuum pumping reaction after the addition is finished, slowly heating to 105-115 ℃, keeping for 2-3h, adding a catalyst, a silane coupling agent and an antioxidant under the protection of nitrogen, and performing vacuum pumping reaction for 0.5-1h to obtain a polyurethane adhesive;
the preparation method of the modified perovskite filament comprises the steps of mixing borax, perovskite, filamentous carbon fibers, 12% of mass fraction ammonium chloride solution and 15% of solubility hydrochloric acid according to the weight portion ratio of 1:1:1:10:10, putting the mixture into a stirrer, and reacting for 1-2 hours at the temperature of 35-50 ℃ to obtain the modified perovskite filament wrapped in the carbon fiber filament and filled with boron nitride.
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