CN117736608A - Isoprene acrylic resin anti-welding ink and preparation method thereof - Google Patents
Isoprene acrylic resin anti-welding ink and preparation method thereof Download PDFInfo
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- CN117736608A CN117736608A CN202311759367.7A CN202311759367A CN117736608A CN 117736608 A CN117736608 A CN 117736608A CN 202311759367 A CN202311759367 A CN 202311759367A CN 117736608 A CN117736608 A CN 117736608A
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- acrylic resin
- isoprene
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- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 239000004925 Acrylic resin Substances 0.000 title claims abstract description 37
- 229920000178 Acrylic resin Polymers 0.000 title claims abstract description 37
- 238000003466 welding Methods 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 229920002873 Polyethylenimine Polymers 0.000 claims abstract description 34
- 239000000945 filler Substances 0.000 claims abstract description 24
- 239000002904 solvent Substances 0.000 claims abstract description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 14
- 239000003822 epoxy resin Substances 0.000 claims abstract description 13
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 13
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 12
- 239000000178 monomer Substances 0.000 claims abstract description 11
- WZRKSPFYXUXINF-UHFFFAOYSA-N 1-(bromomethyl)-4-methylbenzene Chemical group CC1=CC=C(CBr)C=C1 WZRKSPFYXUXINF-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 229910000679 solder Inorganic materials 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- RMCCONIRBZIDTH-UHFFFAOYSA-N 2-(2-methylprop-2-enoyloxy)ethyl 1,3-dioxo-2-benzofuran-5-carboxylate Chemical compound CC(=C)C(=O)OCCOC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 RMCCONIRBZIDTH-UHFFFAOYSA-N 0.000 claims description 4
- 239000007822 coupling agent Substances 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 239000012745 toughening agent Substances 0.000 claims description 4
- 239000003963 antioxidant agent Substances 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical group [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 3
- 239000006097 ultraviolet radiation absorber Substances 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M acrylate group Chemical group C(C=C)(=O)[O-] NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 2
- 230000003078 antioxidant effect Effects 0.000 claims description 2
- 239000013530 defoamer Substances 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- 230000002265 prevention Effects 0.000 claims 3
- 239000000976 ink Substances 0.000 description 29
- 239000000047 product Substances 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 10
- 239000000203 mixture Substances 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 5
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 5
- 238000009499 grossing Methods 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005336 cracking Methods 0.000 description 3
- QYMFNZIUDRQRSA-UHFFFAOYSA-N dimethyl butanedioate;dimethyl hexanedioate;dimethyl pentanedioate Chemical compound COC(=O)CCC(=O)OC.COC(=O)CCCC(=O)OC.COC(=O)CCCCC(=O)OC QYMFNZIUDRQRSA-UHFFFAOYSA-N 0.000 description 3
- 239000011256 inorganic filler Substances 0.000 description 3
- 229910003475 inorganic filler Inorganic materials 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- -1 polysiloxane Polymers 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000000016 photochemical curing Methods 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 238000005476 soldering Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
- GOSUEHGEXLVDBV-UHFFFAOYSA-N 2-methylbuta-1,3-diene;prop-2-enoic acid Chemical group CC(=C)C=C.OC(=O)C=C GOSUEHGEXLVDBV-UHFFFAOYSA-N 0.000 description 1
- 125000006181 4-methyl benzyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1C([H])([H])[H])C([H])([H])* 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 229920000298 Cellophane Polymers 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- GSNUFIFRDBKVIE-UHFFFAOYSA-N DMF Natural products CC1=CC=C(C)O1 GSNUFIFRDBKVIE-UHFFFAOYSA-N 0.000 description 1
- 229920000181 Ethylene propylene rubber Polymers 0.000 description 1
- 229920009204 Methacrylate-butadiene-styrene Polymers 0.000 description 1
- 229920000459 Nitrile rubber Polymers 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- MPIAGWXWVAHQBB-UHFFFAOYSA-N [3-prop-2-enoyloxy-2-[[3-prop-2-enoyloxy-2,2-bis(prop-2-enoyloxymethyl)propoxy]methyl]-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(COC(=O)C=C)(COC(=O)C=C)COCC(COC(=O)C=C)(COC(=O)C=C)COC(=O)C=C MPIAGWXWVAHQBB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 1
- 239000012965 benzophenone Substances 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 1
- 229920005549 butyl rubber Polymers 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 229920006235 chlorinated polyethylene elastomer Polymers 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 125000000664 diazo group Chemical group [N-]=[N+]=[*] 0.000 description 1
- 229940008099 dimethicone Drugs 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- YRIUSKIDOIARQF-UHFFFAOYSA-N dodecyl benzenesulfonate Chemical compound CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 YRIUSKIDOIARQF-UHFFFAOYSA-N 0.000 description 1
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 description 1
- 229940043264 dodecyl sulfate Drugs 0.000 description 1
- 229940071161 dodecylbenzenesulfonate Drugs 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- FRCAGVUKJQCWBD-UHFFFAOYSA-L iodine green Chemical compound [Cl-].[Cl-].C1=CC(N(C)C)=CC=C1C(\C=1C=CC(=CC=1)[N+](C)(C)C)=C/1C=C(C)C(=[N+](C)C)C=C\1 FRCAGVUKJQCWBD-UHFFFAOYSA-L 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000136 polysorbate Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 229920000468 styrene butadiene styrene block copolymer Polymers 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- AYEKOFBPNLCAJY-UHFFFAOYSA-O thiamine pyrophosphate Chemical compound CC1=C(CCOP(O)(=O)OP(O)(O)=O)SC=[N+]1CC1=CN=C(C)N=C1N AYEKOFBPNLCAJY-UHFFFAOYSA-O 0.000 description 1
- 150000003573 thiols Chemical class 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000010626 work up procedure Methods 0.000 description 1
Landscapes
- Inks, Pencil-Leads, Or Crayons (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to an isoprene acrylic resin anti-welding ink and a preparation method thereof, wherein the isoprene acrylic resin anti-welding ink comprises a component A and a component B; the component A comprises the following components in parts by weight: 10-50 parts of isoprene acrylic resin, 1-10 parts of active monomer, 1-10 parts of photoinitiator, 1-5 parts of modified polyethyleneimine, 1-10 parts of solvent and 10-40 parts of hydrophobically modified filler; the component B comprises the following components in parts by weight: 1-10 parts of epoxy resin, 1-10 parts of auxiliary agent and 1-10 parts of solvent; wherein the hydrophobic modified filler is silane coupling agent modified silicon dioxide; the modified polyethyleneimine is 4-methylbenzyl bromide modified polyethyleneimine. The invention enhances the compatibility among components, improves the stability of the anti-welding ink, gives the product higher surface precision and better mechanical property, and overcomes the problems in the prior art.
Description
Technical Field
The invention relates to the technical field of anti-welding ink, in particular to isoprene acrylic resin anti-welding ink and a preparation method thereof.
Background
In the electronics industry, printed circuit boards (Printed circuit board, abbreviated as PCBs) are indispensable and important constituent elements.
In the production of the PCB, the photo-curing ink needs to be coated, and then the finished product is prepared through the procedures of drying, covering a mask plate, exposing, developing, etching and the like. The photo-curing ink is dried to form an ink layer, and is subjected to exposure and heating treatment to be crosslinked and cured to form a protective layer. The protective layer can prevent circuit corrosion wire breakage and short circuit between wires caused by excessive welding points, and has multiple functions of adjusting the attachment amount of soldering tin, reducing the dissolved pollution of copper in the welding points, saving soldering tin, reducing the weight of the instrument, increasing the high density of wiring, avoiding cold joint, improving the inspection speed and the like.
However, in the existing solder resist ink, inorganic fillers such as silica and the like have poor compatibility with organic resin due to strong hydrophilicity, and when the content of the inorganic fillers is high, the inorganic fillers are often unevenly distributed and easily agglomerated, so that the solder resist ink has rough appearance, insufficient glossiness, stability and strength, and cannot meet the performance requirement of the high-frequency communication era on a high-precision circuit board.
In view of the foregoing, it is necessary to develop a new technical solution to solve the drawbacks of the prior art.
Disclosure of Invention
Based on the above, the invention provides an isoprene acrylic resin anti-welding ink and a preparation method thereof. The invention adopts the isoprene acrylic resin as the main resin and is compounded with components such as the hydrophobic modified filler, the modified polyethyleneimine and the like, thereby enhancing the compatibility among the components, improving the stability of the anti-welding ink, endowing the product with higher surface precision and better mechanical property and overcoming the problems in the prior art.
An object of the present invention is to provide an isoprene acrylic resin solder resist ink, which comprises a component a and a component B;
wherein,
the component A comprises the following components in parts by weight:
the component B comprises the following components in parts by weight:
1-10 parts of epoxy resin
1-10 parts of auxiliary agent
1-10 parts of a solvent;
wherein,
the hydrophobic modified filler is silane coupling agent modified silicon dioxide;
the modified polyethyleneimine is 4-methylbenzyl bromide modified polyethyleneimine.
Further, the preparation method of the hydrophobically modified filler comprises the following steps:
adding silicon dioxide into a silane coupling agent solution, carrying out ultrasonic heating reaction, and purifying to obtain the hydrophobic modified filler.
Further, the silane coupling agent is an aminosilane coupling agent.
Further, the temperature of the ultrasonic heating reaction is 60-90 ℃ and the time is 6-14h.
Further, the preparation method of the modified polyethyleneimine comprises the following steps:
adding polyethylenimine and a catalyst into a solvent, heating and stirring, adding 4-methylbenzyl bromide, heating for reaction, cooling, and purifying to obtain the modified polyethylenimine.
Further, the temperature of the heating and stirring is 50-60 ℃; the temperature of the heating reaction is 90-100 ℃ and the time is 5-8h.
Further, the reactive monomer is a monomer having a monofunctional or polyfunctional acrylate unit.
Further, the auxiliary agent is one or more selected from toner, flatting agent, defoamer, ultraviolet absorber, dispersant, antioxidant and flexibilizer.
The toner may be, but is not limited to: phthalocyanine blue, phthalocyanine green, iodine green, diazo yellow, crystal violet, titanium dioxide, carbon black, naphthalene black, and the like.
Leveling agents may be, but are not limited to: silicone, polyurethane, alcohol, polyalcohol, acrylic, inorganic, etc., such as isopropyl alcohol, polysiloxane, dimethicone, glycerin, polyether, alumina, calcium oxide, etc., and mixtures of any of the above alternatives blended in any mass ratio.
The dispersant may be, but is not limited to: a series of anionic surfactants such as AES, AOS, LAS, MES and the like; a non-ionic surfactant series, such as the AEO series, the span series, the tween series, etc., and mixtures of any of the above alternatives blended in any mass ratio.
Defoamers may be, but are not limited to: mineral oil, polydimethyl silicone oil, tributyl phosphate, silicone resin, and the like, and mixtures of any of the above alternatives, blended in any mass ratio.
The ultraviolet absorber may be, but is not limited to: benzophenone, benzotriazole, acrylonitrile, triazine, and the like, and mixtures of any of the foregoing alternatives, blended in any mass ratio.
Antioxidants may be, but are not limited to: phenols, thiols, etc., and mixtures of any of the above alternatives, blended in any mass ratio.
Toughening agents may be, but are not limited to: rubber-based toughening agents, resin-based toughening agents, and the like, such as ethylene propylene rubber, polybutadiene rubber, butyl rubber, nitrile rubber, styrene-butadiene rubber, SBS, ABS, MBS, CPE, DOP, DBP, TCP, TPP, and the like, and mixtures of any of the above alternatives blended in any mass ratio.
Further, the dispersant is selected from anionic surfactants, preferably one or more of dodecylbenzene sulfonate, dodecylsulfate, lunar silicate, stearate.
Further, the solvent is selected from organic solvents such as methanol, ethanol, propanol, butanol, chlorobenzene, toluene, tetrahydrofuran, dichloromethane, chloroform, petroleum ether, benzene, DMF, DMSO, DBE, or derivatives of the above alternatives, and mixtures of any of the above alternatives blended in any mass ratio.
Further, the isoprene acrylic resin contains an alkali-soluble carboxylic acid group and a polymerizable acrylic double bond.
Further, the isoprene acrylic resin is preferably colali UV-203M.
The invention also provides a preparation method of the isoprene acrylic resin anti-welding ink, which comprises the following steps:
blending isoprene acrylic resin, an active monomer, a photoinitiator, modified polyethyleneimine, a solvent and a hydrophobic modified filler to obtain a component A; and (3) blending epoxy resin, an auxiliary agent and a solvent to obtain a component B, blending the component A and the component B, uniformly stirring and dispersing, grinding and filtering to obtain a product.
Another object of the present invention is to provide an application of the above-mentioned isoprene acrylic solder resist ink in a PCB substrate.
The invention has the following beneficial effects:
the isoprene acrylic resin anti-welding ink provided by the invention is compounded by adopting components such as hydrophobic modified filler, modified polyethyleneimine, isoprene acrylic resin and the like. The hydrophobic modified filler is silica modified by KH550 aminosilane coupling agent, the surface of the modified silica is bonded with the coupling agent, the number of hydroxyl groups is greatly reduced, the aggregation of particles is avoided, and the dispersibility of the filler is obviously improved; the modified polyethylenimine is obtained by heating and reacting 4-methylbenzyl bromide and polyethylenimine in an alcohol solvent with potassium carbonate as a catalyst, and the component is obtained by introducing 4-methylbenzyl into the polyethylenimine, so that the lipophilicity of the polyethylenimine is improved, the polyethylenimine has stronger interfacial activity and emulsification effect, and the stability of the ink is enhanced. On the other hand, the modified polyethyleneimine has good compatibility with the hydrophobic modified filler, a synergistic effect is generated, the modified polyethyleneimine can promote the more uniform distribution of the modified filler, and meanwhile, the modified filler is crosslinked with components such as isoprene acrylic resin, epoxy resin and the like through introduced amino groups, and intermolecular acting force is generated between active groups, so that a uniform and stable reticular structure is formed, the stability and strength of the ink are improved, and the appearance precision, adhesive force, strength and other performances of the ink coating are further enhanced.
Detailed Description
In order to more clearly illustrate the technical solution of the present invention, the following examples are set forth. The starting materials, reactions and workup procedures used in the examples are those commonly practiced in the market and known to those skilled in the art unless otherwise indicated.
The words "preferred," "more preferred," and the like in the present disclosure refer to embodiments of the present disclosure that may provide certain benefits in some instances. However, other embodiments may be preferred under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
It should be understood that, except in any operating examples, or where otherwise indicated, quantities or all numbers expressing, for example, quantities of ingredients used in the specification and claims are to be understood as being modified in all instances by the term "about". Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and attached claims are approximations that may vary depending upon the desired properties to be obtained by the present invention.
The active monomers in the embodiment of the invention are trimethylolpropane triacrylate (TMPTA) and polydipentaerythritol hexaacrylate (DPHA) with the mass ratio of 1:1.
The photoinitiator in the embodiment of the invention is ITX and 819.
The solvent in the examples of the present invention is dibasic ester (DBE).
The epoxy resin in the embodiment of the invention is bisphenol A epoxy resin E-12.
The auxiliary agent in the embodiment of the invention is a leveling agent and a dispersing agent in a mass ratio of 1:1, wherein the leveling agent is isopropanol, and the dispersing agent is sodium dodecyl sulfate.
In the embodiment of the invention, the isoprene acrylic resin is colali UV-203M.
The polyethyleneimine of the examples of the present invention was purchased from Shanghai Ala Biotechnology Co., ltd., M W ＝10000。
The preparation method of the modified polyethyleneimine in the embodiment of the invention comprises the following steps:
1.2g of 4-methylbenzyl bromide was dissolved in 75mL of n-propanol to obtain a 4-methylbenzyl bromide solution;
6.3g of polyethyleneimine was added to 75mL of n-propanol, and after dissolution by stirring, 4. 4g K was added 2 CO 3 Then heating to 60 ℃, dropwise adding the 4-methylbenzyl bromide solution at a speed of 5mL/min, then carrying out reflux reaction at 90 ℃ for 6 hours, cooling, centrifuging, and distilling under reduced pressure to remove the solvent in the supernatant to obtain the modified polyethyleneimine.
The silica in the examples of the present invention was obtained from nano fumed silica of the company of Wake chemistry (China).
The preparation method of the hydrophobically modified filler in the embodiment of the invention comprises the following steps:
mixing KH550, water and ethanol according to a mass ratio of 2:10:88 to obtain KH550 solution;
adding silicon dioxide into the KH550 solution (silicon dioxide: KH 550=100:4, m/m), performing ultrasonic reaction at 80 ℃ for 10 hours, filtering, washing and drying to obtain the hydrophobically modified filler.
In the embodiment of the invention, "parts" refer to parts by weight.
Example 1
An isoprene acrylic resin anti-welding ink, which consists of a component A and a component B;
wherein,
the component A comprises the following components in parts by weight:
the component B comprises the following components in parts by weight:
epoxy resin 5 parts
Auxiliary 1 part
3 parts of solvent;
the preparation method of the isoprene acrylic resin anti-welding ink comprises the following steps:
blending isoprene acrylic resin, an active monomer, a photoinitiator, modified polyethylenimine, a solvent and a hydrophobic modified filler according to the parts by weight to obtain a component A; and (3) blending epoxy resin, an auxiliary agent and a solvent to obtain a component B, blending the component A and the component B, uniformly stirring and dispersing, grinding until the fineness is less than or equal to 20 mu m, and sieving with a 120-mesh sieve to obtain a product.
Example 2
An isoprene acrylic resin anti-welding ink, which consists of a component A and a component B;
wherein,
the component A comprises the following components in parts by weight:
the component B comprises the following components in parts by weight:
8 parts of epoxy resin
Auxiliary 2 parts
5 parts of solvent;
the preparation method of the isoprene acrylic acid ring resin anti-welding ink comprises the following steps:
blending isoprene acrylic resin, an active monomer, a photoinitiator, modified polyethylenimine, a solvent and a hydrophobic modified filler according to the parts by weight to obtain a component A; and (3) blending epoxy resin, an auxiliary agent and a solvent to obtain a component B, blending the component A and the component B, uniformly stirring and dispersing, grinding until the fineness is less than or equal to 20 mu m, and sieving with a 120-mesh sieve to obtain a product.
Example 3
An isoprene acrylic resin anti-welding ink, which consists of a component A and a component B;
wherein,
the component A comprises the following components in parts by weight:
the component B comprises the following components in parts by weight:
10 parts of epoxy resin
Auxiliary agent 5 parts
5 parts of solvent;
the preparation method of the isoprene acrylic resin anti-welding ink comprises the following steps:
blending isoprene acrylic resin, an active monomer, a photoinitiator, modified polyethylenimine, a solvent and a hydrophobic modified filler according to the parts by weight to obtain a component A; and (3) blending epoxy resin, an auxiliary agent and a solvent to obtain a component B, blending the component A and the component B, uniformly stirring and dispersing, grinding until the fineness is less than or equal to 20 mu m, and sieving with a 120-mesh sieve to obtain a product.
Comparative example 1
The difference between the present comparative example and example 1 is that: the same mass of hydrophobically modified filler was replaced with unmodified silica, and the other ingredients and preparation method were the same as in example 1.
Comparative example 2
The difference between the present comparative example and example 1 is that: the mass of modified polyethyleneimine was replaced with unmodified polyethyleneimine, and the other components and the preparation method were the same as in example 1.
Test case
Performance tests were conducted on the isoprene acrylic resin solder resist inks prepared in examples 1 to 3 and comparative examples 1 to 2.
The test method is as follows:
the solder resist inks prepared in examples and comparative examples were applied to a PCB, respectively, and photo-cured for 1h (wavelength 395nm, intensity 25.0mW/cm 2 Is then thermally cured at 150℃for 1 hour to form a film of 0.5mm thickness.
Pencil hardness: measured based on JIS K5400.
Adhesion: the films were each scored x-shaped with a needle tip, then attached to the score with cellophane adhesive tape and pulled, as assessed according to the following criteria:
excellent: not torn off;
poor: a large amount of the paper is torn off.
Bending resistance: 180 ° bending was performed with the solder resist ink film as the outer side, and evaluation was performed with the following criteria:
excellent: the film has no cracks;
poor: the film had cracks.
Cold and hot cycle impact:
firstly, pretreatment is carried out: after 24 hours at 125 ℃, the mixture was left at 60 ℃ and 60% RH for 52 hours; then, cold and hot condition circulation is carried out: after 15min at-65 ℃, 15min at 150 ℃ again, the cycle is performed, the conversion time is less than 10s, and the cycle times are 1000 times. The decision criteria are as follows:
qualified: the cracking, falling and other conditions are avoided;
disqualification: cracking and falling off occur.
Acid/alkali resistance: at 20 ℃, the PCB circuit board coated with the solder resist ink is immersed in 10% sulfuric acid solution or 10% sodium hydroxide solution, taken out after 30min, and the state and the adhesiveness of the coating film are evaluated, and the judgment standard is as follows:
qualified: no or slight changes were found;
disqualification: the coating film is swelled or swelled and falls off.
Heat resistance: the thermal shock performance test was performed according to the method in IPC-SM-840E, and the criterion was as follows:
qualified: no bubbles or cracks;
disqualification: air bubbles and cracking occur.
The test results are shown in Table 1.
TABLE 1 Performance test results
| Project | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 |
| Hardness of pencil | 4H | 4H | 4H | 3H | 3H |
| Appearance of | Smoothing | Smoothing | Smoothing | Coarser | Smoothing |
| Adhesion property | Excellent and excellent properties | Excellent and excellent properties | Excellent and excellent properties | Poor quality | Poor quality |
| Bending resistance | Excellent and excellent properties | Excellent and excellent properties | Excellent and excellent properties | Poor quality | Excellent and excellent properties |
| Thermal cycle shock | Qualified product | Qualified product | Qualified product | Failure to pass | Failure to pass |
| Acid resistance | Qualified product | Qualified product | Qualified product | Failure to pass | Failure to pass |
| Alkali resistance | Qualified product | Qualified product | Qualified product | Failure to pass | Failure to pass |
| Heat resistance | Qualified product | Qualified product | Qualified product | Failure to pass | Failure to pass |
As can be seen from Table 1, the isoprene acrylic resin solder resist ink prepared in the examples 1-3 of the present invention has good comprehensive properties, which is significantly better than that of the comparative examples 1-2; comparative examples 1-2 replaced hydrophobically modified fillers or modified polyethylenimines, resulting in less than ideal improvement in dispersibility, compatibility of the components and reduced mechanical properties and stability. In conclusion, the isoprene acrylic resin anti-welding ink has excellent performance, overcomes the defects in the prior art, and has good application prospect.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (10)
1. An isoprene acrylic resin welding-preventing ink, which is characterized by comprising a component A and a component B;
wherein,
the component A comprises the following components in parts by weight:
the component B comprises the following components in parts by weight:
1-10 parts of epoxy resin
1-10 parts of auxiliary agent
1-10 parts of a solvent;
wherein,
the hydrophobic modified filler is silane coupling agent modified silicon dioxide;
the modified polyethyleneimine is 4-methylbenzyl bromide modified polyethyleneimine.
2. The isoprene acrylic resin solder resist ink according to claim 1, wherein said hydrophobically modified filler is prepared by a process comprising the steps of:
adding silicon dioxide into a silane coupling agent solution, carrying out ultrasonic heating reaction, and purifying to obtain the hydrophobic modified filler.
3. The isoprene acrylic resin solder resist ink according to claim 2, wherein said silane coupling agent is an aminosilane coupling agent.
4. The isoprene acrylic resin welding prevention ink according to claim 2, wherein the temperature of the ultrasonic heating reaction is 60-90 ℃ for 6-14h.
5. The isoprene acrylic resin solder resist ink according to claim 1, wherein said modified polyethyleneimine is prepared by a method comprising the steps of:
adding polyethylenimine and a catalyst into a solvent, heating and stirring, adding 4-methylbenzyl bromide, heating for reaction, cooling, and purifying to obtain the modified polyethylenimine.
6. The isoprene acrylic resin welding ink according to claim 5, wherein the temperature of the heating and stirring is 50-60 ℃; the temperature of the heating reaction is 90-100 ℃ and the time is 5-8h.
7. The isoprene acrylic solder resist ink according to claim 1, wherein said reactive monomer is a monomer having a monofunctional or polyfunctional acrylate unit.
8. The isoprene acrylic solder resist ink according to claim 1, wherein said auxiliary agent is one or more selected from the group consisting of toner, leveling agent, defoamer, ultraviolet absorber, dispersant, antioxidant and toughening agent.
9. The method for preparing the isoprene acrylic resin welding prevention ink according to any one of claims 1-8, characterized in that the method for preparing the isoprene acrylic resin welding prevention ink comprises the following steps:
blending isoprene acrylic resin, an active monomer, a photoinitiator, modified polyethyleneimine, a solvent and a hydrophobic modified filler to obtain a component A; and (3) blending epoxy resin, an auxiliary agent and a solvent to obtain a component B, blending the component A and the component B, uniformly stirring and dispersing, grinding and filtering to obtain a product.
10. Use of the isoprene acrylic solder resist ink according to any one of claims 1-8 in PCB substrates.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09270576A (en) * | 1996-03-29 | 1997-10-14 | Taisei Shokai:Kk | Solder ball generation preventive agent and solder ball generation prevention |
| JPH09304926A (en) * | 1996-04-24 | 1997-11-28 | E I Du Pont De Nemours & Co | Durable multilayer coating material capable of processing in aqueous condition and forming image photochemically for printed circuit |
| TW202000839A (en) * | 2018-06-21 | 2020-01-01 | 日商東洋紡股份有限公司 | Adhesive composition comprising polyamideimide resin copolymerized with acrylonitrile butadiene rubber |
| CN114940884A (en) * | 2022-07-26 | 2022-08-26 | 深圳市板明科技股份有限公司 | Adhesive for increasing binding force between copper surface and dielectric material of printed circuit board |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09270576A (en) * | 1996-03-29 | 1997-10-14 | Taisei Shokai:Kk | Solder ball generation preventive agent and solder ball generation prevention |
| JPH09304926A (en) * | 1996-04-24 | 1997-11-28 | E I Du Pont De Nemours & Co | Durable multilayer coating material capable of processing in aqueous condition and forming image photochemically for printed circuit |
| TW202000839A (en) * | 2018-06-21 | 2020-01-01 | 日商東洋紡股份有限公司 | Adhesive composition comprising polyamideimide resin copolymerized with acrylonitrile butadiene rubber |
| CN114940884A (en) * | 2022-07-26 | 2022-08-26 | 深圳市板明科技股份有限公司 | Adhesive for increasing binding force between copper surface and dielectric material of printed circuit board |
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