CN105936771A - Graphene printing ink and preparation method thereof - Google Patents
Graphene printing ink and preparation method thereof Download PDFInfo
- Publication number
- CN105936771A CN105936771A CN201610546376.1A CN201610546376A CN105936771A CN 105936771 A CN105936771 A CN 105936771A CN 201610546376 A CN201610546376 A CN 201610546376A CN 105936771 A CN105936771 A CN 105936771A
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- CN
- China
- Prior art keywords
- graphene
- acrylate
- ink
- ester
- methyl
- 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
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 154
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 150
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000007639 printing Methods 0.000 title abstract description 8
- 229920000728 polyester Polymers 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 21
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000000178 monomer Substances 0.000 claims abstract description 16
- 239000006185 dispersion Substances 0.000 claims description 70
- -1 polyparaphenylene Polymers 0.000 claims description 41
- 238000006243 chemical reaction Methods 0.000 claims description 20
- 125000000524 functional group Chemical group 0.000 claims description 20
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 19
- 150000002148 esters Chemical class 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 12
- RUMACXVDVNRZJZ-UHFFFAOYSA-N 2-methylpropyl 2-methylprop-2-enoate Chemical compound CC(C)COC(=O)C(C)=C RUMACXVDVNRZJZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000007385 chemical modification Methods 0.000 claims description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 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 6
- CERQOIWHTDAKMF-UHFFFAOYSA-N alpha-methacrylic acid Natural products CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 6
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 6
- 229940119545 isobornyl methacrylate Drugs 0.000 claims description 6
- NDWUBGAGUCISDV-UHFFFAOYSA-N 4-hydroxybutyl prop-2-enoate Chemical compound OCCCCOC(=O)C=C NDWUBGAGUCISDV-UHFFFAOYSA-N 0.000 claims description 5
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 claims description 5
- RYZOOQNIKUEQFJ-UHFFFAOYSA-N C(C)C=CC.[O].C1=CC=CC=C1 Chemical group C(C)C=CC.[O].C1=CC=CC=C1 RYZOOQNIKUEQFJ-UHFFFAOYSA-N 0.000 claims description 4
- OBOXTJCIIVUZEN-UHFFFAOYSA-N [C].[O] Chemical group [C].[O] OBOXTJCIIVUZEN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- FWLDHHJLVGRRHD-UHFFFAOYSA-N decyl prop-2-enoate Chemical compound CCCCCCCCCCOC(=O)C=C FWLDHHJLVGRRHD-UHFFFAOYSA-N 0.000 claims description 4
- 150000007519 polyprotic acids Chemical class 0.000 claims description 4
- LYBIZMNPXTXVMV-UHFFFAOYSA-N propan-2-yl prop-2-enoate Chemical compound CC(C)OC(=O)C=C LYBIZMNPXTXVMV-UHFFFAOYSA-N 0.000 claims description 4
- 150000005846 sugar alcohols Polymers 0.000 claims description 4
- KAESVJOAVNADME-UHFFFAOYSA-N 1H-pyrrole Natural products C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 3
- WKACYGQNLXLXEB-UHFFFAOYSA-N 2-ethyl-2-(hydroxymethyl)propane-1,3-diol 3-methylbut-2-enoic acid Chemical compound CC(=CC(=O)O)C.C(O)C(CC)(CO)CO WKACYGQNLXLXEB-UHFFFAOYSA-N 0.000 claims description 3
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical group CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims description 3
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 3
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 claims description 3
- 229940092714 benzenesulfonic acid Drugs 0.000 claims description 3
- KBLWLMPSVYBVDK-UHFFFAOYSA-N cyclohexyl prop-2-enoate Chemical compound C=CC(=O)OC1CCCCC1 KBLWLMPSVYBVDK-UHFFFAOYSA-N 0.000 claims description 3
- 125000004185 ester group Chemical group 0.000 claims description 3
- 125000002541 furyl group Chemical group 0.000 claims description 3
- 125000000623 heterocyclic group Chemical group 0.000 claims description 3
- ULDDEWDFUNBUCM-UHFFFAOYSA-N pentyl prop-2-enoate Chemical compound CCCCCOC(=O)C=C ULDDEWDFUNBUCM-UHFFFAOYSA-N 0.000 claims description 3
- 229920001197 polyacetylene Polymers 0.000 claims description 3
- 229920000767 polyaniline Polymers 0.000 claims description 3
- 229920000128 polypyrrole Polymers 0.000 claims description 3
- 229920000123 polythiophene Polymers 0.000 claims description 3
- 125000001544 thienyl group Chemical group 0.000 claims description 3
- RWXMAAYKJDQVTF-UHFFFAOYSA-N 2-(2-hydroxyethoxy)ethyl prop-2-enoate Chemical compound OCCOCCOC(=O)C=C RWXMAAYKJDQVTF-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 2
- RDBNAQJXOYZUFL-UHFFFAOYSA-N 2-methylidenetetradecanoic acid Chemical compound CCCCCCCCCCCCC(=C)C(O)=O RDBNAQJXOYZUFL-UHFFFAOYSA-N 0.000 claims description 2
- NQSLZEHVGKWKAY-UHFFFAOYSA-N 6-methylheptyl 2-methylprop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C(C)=C NQSLZEHVGKWKAY-UHFFFAOYSA-N 0.000 claims description 2
- 229920000265 Polyparaphenylene Polymers 0.000 claims description 2
- 125000005396 acrylic acid ester group Chemical group 0.000 claims description 2
- 238000007334 copolymerization reaction Methods 0.000 claims description 2
- WQPDQJCBHQPNCZ-UHFFFAOYSA-N cyclohexa-2,4-dien-1-one Chemical compound O=C1CC=CC=C1 WQPDQJCBHQPNCZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- VLCAYQIMSMPEBW-UHFFFAOYSA-N methyl 3-hydroxy-2-methylidenebutanoate Chemical compound COC(=O)C(=C)C(C)O VLCAYQIMSMPEBW-UHFFFAOYSA-N 0.000 claims description 2
- KRLHYNPADOCLAJ-UHFFFAOYSA-N undecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCOC(=O)C(C)=C KRLHYNPADOCLAJ-UHFFFAOYSA-N 0.000 claims description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- VKEQBMCRQDSRET-UHFFFAOYSA-N Methylone Chemical compound CNC(C)C(=O)C1=CC=C2OCOC2=C1 VKEQBMCRQDSRET-UHFFFAOYSA-N 0.000 claims 1
- OLLMEZGFCPWTGD-UHFFFAOYSA-N hexane;methanol Chemical compound OC.OC.CCCCCC OLLMEZGFCPWTGD-UHFFFAOYSA-N 0.000 claims 1
- 229940059574 pentaerithrityl Drugs 0.000 claims 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims 1
- 239000011248 coating agent Substances 0.000 abstract description 10
- 238000000576 coating method Methods 0.000 abstract description 10
- 239000012752 auxiliary agent Substances 0.000 abstract description 6
- 238000004383 yellowing Methods 0.000 abstract 1
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 14
- 239000000463 material Substances 0.000 description 12
- 239000007822 coupling agent Substances 0.000 description 10
- 238000002604 ultrasonography Methods 0.000 description 9
- 238000001291 vacuum drying Methods 0.000 description 9
- 238000004140 cleaning Methods 0.000 description 8
- 238000001914 filtration Methods 0.000 description 8
- 229910002804 graphite Inorganic materials 0.000 description 8
- 239000010439 graphite Substances 0.000 description 8
- 239000012535 impurity Substances 0.000 description 8
- 238000007711 solidification Methods 0.000 description 7
- 230000008023 solidification Effects 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000004014 plasticizer Substances 0.000 description 6
- 238000004513 sizing Methods 0.000 description 6
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 description 5
- 150000001336 alkenes Chemical class 0.000 description 5
- 239000004593 Epoxy Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical class C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 description 4
- 239000013530 defoamer Substances 0.000 description 4
- VFHVQBAGLAREND-UHFFFAOYSA-N diphenylphosphoryl-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 VFHVQBAGLAREND-UHFFFAOYSA-N 0.000 description 4
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 239000012956 1-hydroxycyclohexylphenyl-ketone Substances 0.000 description 3
- CFVWNXQPGQOHRJ-UHFFFAOYSA-N 2-methylpropyl prop-2-enoate Chemical compound CC(C)COC(=O)C=C CFVWNXQPGQOHRJ-UHFFFAOYSA-N 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- MQDJYUACMFCOFT-UHFFFAOYSA-N bis[2-(1-hydroxycyclohexyl)phenyl]methanone Chemical compound C=1C=CC=C(C(=O)C=2C(=CC=CC=2)C2(O)CCCCC2)C=1C1(O)CCCCC1 MQDJYUACMFCOFT-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- OIWOHHBRDFKZNC-UHFFFAOYSA-N cyclohexyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1CCCCC1 OIWOHHBRDFKZNC-UHFFFAOYSA-N 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- XNGIFLGASWRNHJ-UHFFFAOYSA-N o-dicarboxybenzene Natural products OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- PSGCQDPCAWOCSH-UHFFFAOYSA-N (4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl) prop-2-enoate Chemical group C1CC2(C)C(OC(=O)C=C)CC1C2(C)C PSGCQDPCAWOCSH-UHFFFAOYSA-N 0.000 description 2
- LMVLVUPTDRWATB-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propan-1-ol Chemical compound CO[Si](C)(OC)CCCO LMVLVUPTDRWATB-UHFFFAOYSA-N 0.000 description 2
- VVBLNCFGVYUYGU-UHFFFAOYSA-N 4,4'-Bis(dimethylamino)benzophenone Chemical compound C1=CC(N(C)C)=CC=C1C(=O)C1=CC=C(N(C)C)C=C1 VVBLNCFGVYUYGU-UHFFFAOYSA-N 0.000 description 2
- 229920002799 BoPET Polymers 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- LYJZNXAVZMEXDH-UHFFFAOYSA-N octadecan-8-yl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCC(OC(=O)C(C)=C)CCCCCCC LYJZNXAVZMEXDH-UHFFFAOYSA-N 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- RSJKGSCJYJTIGS-UHFFFAOYSA-N undecane Chemical compound CCCCCCCCCCC RSJKGSCJYJTIGS-UHFFFAOYSA-N 0.000 description 2
- PIZHFBODNLEQBL-UHFFFAOYSA-N 2,2-diethoxy-1-phenylethanone Chemical compound CCOC(OCC)C(=O)C1=CC=CC=C1 PIZHFBODNLEQBL-UHFFFAOYSA-N 0.000 description 1
- KMNCBSZOIQAUFX-UHFFFAOYSA-N 2-ethoxy-1,2-diphenylethanone Chemical compound C=1C=CC=CC=1C(OCC)C(=O)C1=CC=CC=C1 KMNCBSZOIQAUFX-UHFFFAOYSA-N 0.000 description 1
- MRDMGGOYEBRLPD-UHFFFAOYSA-N 2-ethoxy-1-(2-ethoxyphenyl)ethanone Chemical compound CCOCC(=O)C1=CC=CC=C1OCC MRDMGGOYEBRLPD-UHFFFAOYSA-N 0.000 description 1
- GWZMWHWAWHPNHN-UHFFFAOYSA-N 2-hydroxypropyl prop-2-enoate Chemical compound CC(O)COC(=O)C=C GWZMWHWAWHPNHN-UHFFFAOYSA-N 0.000 description 1
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 1
- SXNICUVVDOTUPD-UHFFFAOYSA-N CC1=CC(C)=CC(C)=C1C(=O)P(=O)C1=CC=CC=C1 Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)C1=CC=CC=C1 SXNICUVVDOTUPD-UHFFFAOYSA-N 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 150000008062 acetophenones Chemical class 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000006735 epoxidation reaction Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229940063557 methacrylate Drugs 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000007645 offset printing Methods 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- YVYAGJBDMPIZSI-UHFFFAOYSA-N phenyl 2,4,6-trimethylbenzoate Chemical compound CC1=CC(C)=CC(C)=C1C(=O)OC1=CC=CC=C1 YVYAGJBDMPIZSI-UHFFFAOYSA-N 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical group CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000009450 smart packaging Methods 0.000 description 1
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- 239000002904 solvent Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/101—Inks specially adapted for printing processes involving curing by wave energy or particle radiation, e.g. with UV-curing following the printing
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a graphene printing ink and a preparation method thereof. The graphene printing ink comprises the following raw materials in percentage by weight: 0.01 to 40% of graphene, 5 to 50% of oligomer, 20 to 80% of monomer, 0.1 to 25% of photoinitiator, and 0 to 20% of auxiliary agent; wherein the oligomer is polyester acrylate, and the monomer is (meth)acrylate. Due to the graphene component, the cured coating has an excellent electro-conductive performance; based on the properties of polyester acrylate, the coating has excellent characteristics such as excellent flexibility, good caking property, weatherability, performance on resisting yellowing, high refractive index, and the like, and thus the graphene printing ink has a good using property. Furthermore, by controlling the ratio of monomers to oligomer, the rubber system has a proper viscosity so as to ensure that graphene is well dispersed in the system.
Description
Technical field
Embodiment of the present invention relates to electrically conductive ink technical field, particularly relates to a kind of Graphene ink and preparation side thereof
Method.
Background technology
Electrically conductive ink is a kind of functional ink, has certain electric conductivity and antistatic effect, is widely used in printing
The materials such as wiring board, integrated circuit, radio-frequency (RF) tag.Traditional electrically conductive ink is all by gold, silver, copper powder or other metal powders or carbon
The ink that powder forms with binder etc., there is the shortcomings such as cost height, complex process, resistivity is high, forming and hardening temperature is high in it.
Along with electronic product develops to directions such as light, thin, little, low cost, multi-functional, high reliability with equipment, flexible electrical
The consumption on road is increasing, utilize electrically conductive ink or conductive ink by printing or printing by the way of, on flexible insulating substrate
The technical scheme forming conducting wire attracts wide attention.
Graphene, as the emerging family of material with carbon element, is by the new material of carbon atom monolayer laminated structure, has preferable machine
Tool performance and special electric property, in Graphene, the conduction velocity of electronics is 8 × 105m/s；Conductivity 1250～7000s/
m.Graphene can make composite material conductive by providing the passage of electron transfer.With existing nano metal (such as nanometer silver
Powder, copper nanoparticle etc.) electrically conductive ink compares, and Graphene ink has huge cost advantage.
Graphene ink be the composition such as a class Graphene, binder, auxiliary agent and solvent there is the specific functions such as conduction
Ink product, has electric conductivity excellence, printed patterns light weight, printability are good, condition of cure is gentle and with low cost
Etc. advantage, printing can be realized on the multiple base materials such as plastic sheeting, paper and tinsel.
Graphene ink is applicable to the modes such as wire mark, gravure, flexo, offset printing and ink jet printing, can apply to track
In terms of road plate (PCB), RF identification (RFI D), display device (such as OLED), electrode sensor etc., can potential be applied to organic
Above solaode, printed battery and ultracapacitor.Therefore Graphene ink is expected in radio-frequency (RF) tag, intelligent packaging, thin
Being used widely in frivolous, the flexible electronic product of future generation such as membrane switch, conducting wire and sensor, market prospect is wide
Wealthy.
But in existing Graphene ink is studied, for industrialization large-scale production and every ink of Graphene ink
Water serviceability, such as pliability, the remaining a need for of caking property etc. is further probed into and is promoted.
Summary of the invention
For solving above-mentioned technical problem, embodiment of the present invention provides a kind of Graphene ink and preparation method thereof, it is possible to
The serviceability of Graphene ink that promotes and meet large-scale industrial production requirement.
For solving above-mentioned technical problem, the technical scheme that embodiment of the present invention uses is: provide a kind of Graphene
Ink.This Graphene ink, by weight percentage, its raw material consists of:
Described oligomer is polyester (methyl) acrylate；Described monomer is (methyl) acrylate.
Alternatively, by weight percentage, the raw material of described Graphene ink consists of:
Alternatively, by weight percentage, the raw material of described Graphene ink consists of:
Alternatively, described Graphene also includes: chemical modification Graphene and chemical doping Graphene；
The doping molecule of described chemical doping Graphene includes: polyaniline, polythiophene, polypyrrole, polyacetylene and poly-to benzene
One or more in support；
The functional group of described chemical modification Graphene includes: hydroxyl, ester group, pyrrole radicals, imidazole radicals, thienyl, furyl,
One or more in the deriveding group of phenyl, benzenesulfonic acid base, anilino-and above-mentioned functional group.
Alternatively, the mean molecule quantity of described oligomer is 10000-60000, and average viscosity is 200-50000cps, official
Can degree of group be 1-6.
Alternatively, described polyester (methyl) acrylate by (methyl) acrylic acid, include that polyprotic acid and long-chain polyhydric alcohol are altogether
Gather and form.
Alternatively, the lamellar spacing of described Graphene be 0.34nm-10nm, planar dimension be 2nm-1000nm.
Alternatively, described (methyl) acrylate is (methyl) acrylate containing hydrocarbon or carbon oxygen backbone, carries miscellaneous
One or more of (methyl) acrylate of ring structure and (methyl) acrylate of hydroxyl structure.
Alternatively, described monomer is isobornyl acrylate, isobornyl methacrylate, 2-(Acryloyloxy)ethanol, methyl
2-(Acryloyloxy)ethanol, 4-hydroxybutyl acrylate, 1,4 cyclohexane dimethanol mono acrylic ester, diethylene glycol list acrylic acid
Ester, 1,6-HD mono acrylic ester, pentaerythritol triacrylate, trimethylolpropane dimethylacrylate, cyclopenta
Acrylate, 2-cyclohexyl acrylate, 2-cyclohexyl methacrylate, isopropyl acrylate, dicyclo benzene oxygen ethylacrylic acid
Ester, isobutyl methacrylate, acrylic acid n-pentyl ester, Isobutyl 2-propenoate, Isooctyl acrylate monomer, 2-Propenoic acid, 2-methyl-, isooctyl ester,
Lauryl acrylate, n-octyl, decyl acrylate, decyl-octyl methacrylate, methacrylic acid undecyl ester, 2-third
One or more in olefin(e) acid dodecyl ester.
For solving above-mentioned technical problem, another technical scheme that embodiment of the present invention uses is: provide a kind of graphite
The preparation method of alkene ink.Wherein, the method includes:
Take raw material as above, in reaction vessel, be stirred mixing with predetermined mixing speed and filter, being formed
Graphene just dispersion；
At normal temperatures, graphene dispersion body is carried out vacuum deaerator；
To the graphene dispersion body ultrasonic disperse after vacuum deaerator, form Graphene size dispersions；
Nano-milled Graphene size dispersions, forms Graphene ink.
Embodiment of the present invention provides the benefit that: Graphene is filled into polyester acrylate body by embodiment of the present invention
In system, give the solidification good electric conductivity of coating and the pliability that has based on polyester acrylate sizing material is good, caking property
The excellent specific properties such as good, weather-proof color inhibition, refractive index are high, so that Graphene ink has good serviceability.It addition, it is logical
Cross the proportioning controlling monomer with oligomer so that paste system has suitable viscosity, it is ensured that Graphene maintains good dispersion
State.
Accompanying drawing explanation
Fig. 1 is the flow chart of the preparation method of the Graphene ink of the embodiment of the present invention.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, right
The present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, not
For limiting the present invention.
The embodiment of the present invention provides a kind of Graphene ink, and its raw material consists of: count by weight percentage, Graphene
0.01%-40%；Oligomer 5%-50%；Monomer 20%-80%；Light trigger 0.1%-25%；Auxiliary agent 0-20%.Wherein,
Described oligomer is polyester (methyl) acrylate；Described monomer is (methyl) acrylate, forms polyester acrylate sizing material
System.
Polyester acrylate has characteristic transparent, that pliability is good, caking property good, weather-proof color inhibition, refractive index are high, can
Well to meet the properties requirement of Graphene ink application.It addition, the proportioning of this monomer and oligomer can provide proper
When system viscosity, to guarantee that Graphene can keep good dispersion in sizing material.
Described Graphene can also include the Graphene of chemical doping and the Graphene of chemical modification.Wherein, describedization
The doping molecule learning doped graphene includes: one in polyaniline, polythiophene, polypyrrole, polyacetylene and polyparaphenylene or
Multiple.
The functional group of described chemical modification Graphene includes: hydroxyl, ester group, pyrrole radicals, imidazole radicals, thienyl, furyl,
One or more in the deriveding group of phenyl, benzenesulfonic acid base, anilino-and above-mentioned functional group.
By above-mentioned chemical doping and chemical modification group, Graphene component can be improved at polyester acrylate sizing material
In dispersion stabilization, it is to avoid Graphene component is in use assembled.The lamellar spacing of this Graphene is the most permissible
It is 2nm-1000nm for 0.34nm-10nm, planar dimension.
The mean molecule quantity of described oligomer (i.e. polyester (methyl) acrylate) is 10000-60000, and average viscosity is
200-50000cps, functional group's degree is 1-6.
In the present embodiment, this oligomer can be by (methyl) acrylic monomers, polyprotic acid and long-chain polyhydric alcohol copolymerization
Become.Specifically, the long-chain polyhydric alcohol structure in oligomer can improve the pliability of ink coating, makes the most resistance to curling of coating
And folding.And polyprotic acid can make oligomer possess stronger cohesiveness and relatively low viscosity, the bonding improving paste system is strong
Degree.
In the present embodiment, described monomer can carry miscellaneous by (methyl) acrylate containing hydrocarbon or carbon oxygen backbone
One or more of (methyl) acrylate of ring structure and (methyl) acrylate of hydroxyl structure.Specifically, single
Hydrocarbon or the carbon oxygen backbone of body can give the pliability that coating is good, and heterocycle structure is favorably improved the viscous of paste system
Knot power and intensity.Especially, the phenyl ring in heterocycle structure can also improve the refractive index of coating.Further, since energy between hydroxyl
Enough generate hydrogen bond such that it is able to improve the ink adhesive force for PET film.By the cooperation of above-mentioned group, tool can be formed
There is the paste system of good serviceability.
Preferably, this monomer specifically can select to use: isobornyl acrylate, isobornyl methacrylate, propylene
Acid hydroxyl ethyl ester, hydroxyethyl methylacrylate, 4-hydroxybutyl acrylate, 1,4 cyclohexane dimethanol mono acrylic ester, diethyl
Diol mono-acrylate, 1,6-HD mono acrylic ester, pentaerythritol triacrylate, trimethylolpropane dimethyl allene
Acid esters, cyclopentylpropenoic acid ester, 2-cyclohexyl acrylate, 2-cyclohexyl methacrylate, isopropyl acrylate, dicyclo benzene oxygen
Ethyl propylene acid esters, isobutyl methacrylate, acrylic acid n-pentyl ester, Isobutyl 2-propenoate, Isooctyl acrylate monomer, metering system
Acid different monooctyl ester, lauryl acrylate, n-octyl, decyl acrylate, decyl-octyl methacrylate, methacrylic acid hendecane
One or more in base ester, 2-dodecylacrylate.
Described light trigger constitutes the initiator system of this Graphene ink.Wherein, effective functional group of light trigger can
To include: benzoin class, a-hydroxyl ketone, acetophenones, a-amino ketones, acylphosphine oxide or other suitable senses
Group.
It is also preferred that the left this light trigger is specifically as follows: 1-hydroxycyclohexyl phenyl ketone, dihydroxy benaophenonel, 2-hydroxyl-
2-phenyl acetophenone, 2,2 '-diethoxy acetophenone, 4,4'-bis-(N, N-dimethylamino) benzophenone, 2-hydroxy-2-methyl-
1-phenyl-1-acetone, 2,4,6-trimethylbenzoyl-diphenyl phosphine oxide, double (2,4,6-trimethylbenzoyl) phenyl oxygen
Change in phosphine, Benzoinum methyl ether, benzoin ethyl ether and Cyanuric Chloride one or more.
The initiator system of Graphene ink should have relatively low solidification energy and higher solidification rate.Ink is coated in
After on base material, it is possible to complete solidification rapidly thus avoid the gathering of Graphene component.
It should be noted that, in the Graphene ink of the embodiment of the present invention, auxiliary agent, specifically can basis for selecting component
Actual performance requirement or service condition are selected to use by those skilled in the art, give Graphene ink more excellent or not
Same serviceability.Concrete, this auxiliary agent may include that one or more in coupling agent, defoamer, plasticizer.
Wherein, coupling agent is used for increasing adhesion strength between coating and PET film, and defoamer is used for suppressing, reduce or disappearing
Except the bubble in dispersion, plasticizer is for further increasing coating flexibility.Preferably, coupling agent can be 3-methyl-prop
Alkene monomethacryloxypropyl trimethoxy silane, 3-[(2,3)-epoxy the third oxygen] hydroxypropyl methyl dimethoxysilane, 3-aminopropyl front three
In TMOS, chlorinated polypropylene, VTES, 3-(2,3-epoxy the third oxygen) propyl trimethoxy silicane one
Plant or multiple.Defoamer can be the one in polydimethylsiloxane, polyacrylate, tributyl phosphate, polyethers or many
Kind.Plasticizer can be phthalic acid ester, fatty group dibasic acid, alkyl sulfonic ester, phosphate ester, the many acid esters of benzene, epoxidation
One or more in compound.
Refer to Fig. 1, for the Graphene ink preparation method of the embodiment of the present invention.This preparation method includes:
S101: by weight percentage, takes off and states raw material: Graphene 0.01%-40%；Oligomer 5%-50%；Monomer
20%-80%；Light trigger 0.1%-25%；Auxiliary agent 0-20%；To reaction vessel.
S103: by the raw material stirring mix homogeneously in reaction vessel and filter, it is thus achieved that Graphene just dispersion.
In the present embodiment, can mixing speed be controlled at 1000-1500r/mi n, mixing time controls at 60-
240mi n, it is thus achieved that preferably stirring and mixing effect.
S105: at normal temperatures, carries out vacuum deaerator to Graphene just dispersion.This room temperature specifically refers to 25 DEG C.In reality
In operating process, it is possible to use vacuum drying oven carries out vacuum deaerator operation.
In this embodiment, the operation of vacuum deaerator, specifically can be in the environment of vacuum be 0-0.1MPa, inclined heated plate
Control at 10-60mi n, Graphene just dispersion is carried out thorough deaeration.
S107: to the just dispersion ultrasonic disperse of the Graphene after vacuum deaerator, form Graphene size dispersions.
After Graphene just dispersion deaeration thoroughly, ultrasound wave nano-dispersed instrument it is carried out ultrasonic disperse.Ultrasonic
Extremely after dispersion time enough, just can obtain Graphene size dispersions, specifically can be at a temperature of 0-60 DEG C, to subtracting
Graphene dispersion body after pressure-off bubble carries out ultrasonic disperse.
In the present embodiment, ultrasonic power can control at 600-900W, and ultrasonic frequency controls at 28-132KHz,
The ultrasonic disperse time is that 0.5-12h is to obtain the transparent graphene size dispersions that degree of scatter is enough.
S109: nano-milled Graphene size dispersions, forms the Graphene ink of embodiment of the present invention.
After obtaining transparent Graphene size dispersions, by nano-milled prepare embodiment of the present invention stone
Ink alkene ink.
In the present embodiment, it is also possible to use above-mentioned raw material to form, other routine operation techniques in application prior art,
Such as stirring, deaeration and dispersion etc., preparation forms this Graphene ink, and concrete ink preparation technology and technological parameter are this
Known to skilled person.In actual applications, it is also possible to according to actual preparation requirement, prepare environment practical situation, add
Adding or economization certain operations step, preparation forms this Graphene ink.To the routine variations of the step of the embodiment of the present invention, replace
The technical scheme changed, merge or adjust all can by those skilled in the art in the case of being not required to pay creative work complete
Become.
For technical scheme is expanded on further, the Graphene ink preparation method of the present invention presented below some
Embodiment.
Embodiment 1:
First, following raw material is taken:
5g Graphene；
15g oligomer；
35g 4-hydroxybutyl acrylate；
35g 1,6-HD mono acrylic ester；
2g 1-hydroxycyclohexyl phenyl ketone (light trigger)；
2g VTES (coupling agent)
6g phthalic acid ester (plasticizer)；
In the reaction vessel join cleaning, being dried.
Wherein, described oligomer is: average viscosity is 4000cps, mean molecule quantity is 40000, the polyester of functional group's degree 3
Acrylate.
Secondly, to being stirred in reaction vessel, filtering and impurity removing, obtain Graphene just dispersion.
Again, Graphene just dispersion vacuum drying oven is carried out vacuum deaerator under room temperature (25 DEG C).
After deaeration thoroughly, carry out dispersion ultrasound wave nano-dispersed instrument extremely disperseing 4h, obtain transparent graphite
Alkene size dispersions.
Finally, Graphene ink is prepared by nano-milled for Graphene size dispersions.
Embodiment 2:
First, following raw material is taken:
0.1g Graphene；
20g oligomer；
15g 4-hydroxybutyl acrylate；
25g isobornyl methacrylate；
10g isobutyl methacrylate；
25g lauryl acrylate；
2g 2,2-diethoxy acetophenone (light trigger)；
8g 3-methyl allyl acyloxypropyl trimethoxysilane (coupling agent)；
In the reaction vessel join cleaning, being dried.
Wherein, described oligomer is: average viscosity is 6000cps, mean molecule quantity is 30000, the polyester of functional group's degree 2
Acrylate.
Secondly, to being stirred in reaction vessel, filtering and impurity removing, obtain Graphene just dispersion.
Again, Graphene just dispersion vacuum drying oven is carried out vacuum deaerator under room temperature (25 DEG C).
After deaeration thoroughly, carry out dispersion ultrasound wave nano-dispersed instrument extremely disperseing 6h, obtain transparent graphite
Alkene size dispersions.
Finally, Graphene ink is prepared by nano-milled for Graphene size dispersions.
Embodiment 3:
First, following raw material is taken:
10g Graphene；
30g oligomer；
30g isobutyl methacrylate；
25g trimethylolpropane dimethylacrylate；
1g 2-hydroxyl-2-phenyl acetophenone (light trigger)；
1g 2,4,6-trimethylbenzoyl-diphenyl phosphine oxide (light trigger)；
1g 3-(2,3-epoxy the third oxygen) propyl trimethoxy silicane (coupling agent)；
2g polydimethylsiloxane (defoamer)；
In the reaction vessel join cleaning, being dried.
Wherein, described oligomer is: average viscosity is 7000cps, mean molecule quantity is 40000, functional group's degree 1.5 poly-
METH acrylate.
Secondly, to being stirred in reaction vessel, filtering and impurity removing, obtain Graphene just dispersion.
Again, Graphene just dispersion vacuum drying oven is carried out vacuum deaerator under room temperature (25 DEG C).
After deaeration thoroughly, carry out dispersion ultrasound wave nano-dispersed instrument extremely disperseing 2h, obtain transparent graphite
Alkene size dispersions.
Finally, Graphene ink is prepared by nano-milled for Graphene size dispersions.
Embodiment 4:
First, following raw material is taken:
20g Graphene；
10g the first oligomer；
15g the second oligomer；
15g isobornyl methacrylate；
15g dicyclo benzene oxygen ethyl propylene acid esters；
20g pentaerythritol triacrylate；
Double (2,4,6-trimethylbenzoyl) phenyl phosphine oxide (light trigger) of 3g；
2g 3-[(2,3)-epoxy the third oxygen] hydroxypropyl methyl dimethoxysilane (coupling agent)；
In the reaction vessel join cleaning, being dried.
Wherein, described first oligomer is: average viscosity is 8000cps, mean molecule quantity is 20000, functional group's degree 2
Polyester acrylate；
Described second oligomer is: average viscosity is 10000cps, mean molecule quantity is 45000, functional group's degree 1.5 poly-
Ester acrylate.
Secondly, to being stirred in reaction vessel, filtering and impurity removing, obtain Graphene just dispersion.
Again, Graphene just dispersion vacuum drying oven is carried out vacuum deaerator under room temperature (25 DEG C).
After deaeration thoroughly, carry out dispersion ultrasound wave nano-dispersed instrument extremely disperseing 12h, obtain transparent graphite
Alkene size dispersions.
Finally, Graphene ink is prepared by nano-milled for Graphene size dispersions.
Embodiment 5:
First, following raw material is taken:
15g Graphene；
45g oligomer；
15g isobornyl methacrylate；
5g isobutyl methacrylate；
15g Isobutyl 2-propenoate；
2g 2-hydroxy-2-methyl-1-phenyl-1-acetone (light trigger)；
3g VTES (coupling agent)；
In the reaction vessel join cleaning, being dried.
Wherein, described oligomer is: average viscosity is 7500cps, mean molecule quantity is 30000, functional group's degree 1.5 poly-
Ester acrylate.
Secondly, to being stirred in reaction vessel, filtering and impurity removing, obtain Graphene just dispersion.
Again, Graphene just dispersion vacuum drying oven is carried out vacuum deaerator under room temperature (25 DEG C).
After deaeration thoroughly, carry out dispersion ultrasound wave nano-dispersed instrument extremely disperseing 8h, obtain transparent graphite
Alkene size dispersions.
Finally, Graphene ink is prepared by nano-milled for Graphene size dispersions.
Embodiment 6:
First, following raw material is taken:
0.5g Graphene；
35g oligomer；
13g isobutyl methacrylate；
17g lauryl acrylate；
15g diethylene glycol monoacrylate；
10g pentaerythritol triacrylate；
1g 1-hydroxycyclohexyl phenyl ketone (light trigger)；
1.5g 2,4,6-trimethylbenzoyl-diphenyl phosphine oxide (light trigger)；
3g alkyl sulfonic ester (dispersant)；
4g trimethoxy [2-(7-oxabicyclo [4.1.0] hept-3-yl) ethyl] silane) propyl trimethoxy silicane
(coupling agent).
In the reaction vessel join cleaning, being dried.
Wherein, described oligomer is: average viscosity is 7200cps, mean molecule quantity is 20000, the polyester of functional group's degree 3
Methacrylate.
Secondly, to being stirred in reaction vessel, filtering and impurity removing, obtain Graphene just dispersion.
Again, Graphene just dispersion vacuum drying oven is carried out vacuum deaerator under room temperature (25 DEG C).
After deaeration thoroughly, carry out dispersion ultrasound wave nano-dispersed instrument extremely disperseing 1h, obtain transparent graphite
Alkene size dispersions.
Finally, Graphene ink is prepared by nano-milled for Graphene size dispersions.
Embodiment 7:
First, following raw material is taken:
0.01g Graphene；
35g the first oligomer；
15g the second oligomer；
25g 2-cyclohexyl methacrylate；
7g isopropyl acrylate；
8g dicyclo benzene oxygen ethyl propylene acid esters；
0.75g 2-hydroxyl-2-phenyl acetophenone (light trigger)；
0.75g 2,4,6-trimethylbenzoyl-diphenyl phosphine oxide (light trigger)；
The many acid esters of 3.5g benzene (plasticizer)；
In the reaction vessel join cleaning, being dried.
Wherein, described first oligomer is: average viscosity is 6000cps, mean molecule quantity is 30000, functional group's degree 2
Polyester acrylate；
Described second oligomer is: average viscosity is 10000cps, mean molecule quantity is 35000, the polyester of functional group's degree 1
Acrylate.
Secondly, to being stirred in reaction vessel, filtering and impurity removing, obtain just graphene dispersion body.
Again, first graphene dispersion body vacuum drying oven is carried out vacuum deaerator under room temperature (25 DEG C).
After deaeration thoroughly, carry out dispersion ultrasound wave nano-dispersed instrument extremely disperseing 12h, obtain transparent graphite
Alkene size dispersions.
Finally, Graphene ink is prepared by nano-milled for Graphene size dispersions.
Embodiment 8:
First, following raw material is taken:
8g Graphene；
10g the first oligomer；
30g the second oligomer；
25g isobutyl methacrylate；
8g cyclopentylpropenoic acid ester；
12g pentaerythritol triacrylate；
2g 2-hydroxy-2-methyl-1-phenyl-1-acetone (light trigger)；
2g VTES (coupling agent)；
3g phthalic acid ester (plasticizer)；
In the reaction vessel join cleaning, being dried.
Wherein, described first oligomer is: average viscosity is 7000cps, mean molecule quantity is 35000, functional group's degree 1
Polyester acrylate；
Described second oligomer is: average viscosity is 7000cps, mean molecule quantity is 40000, the polyester of functional group's degree 3
Acrylate.
Secondly, to being stirred in reaction vessel, filtering and impurity removing, obtain just graphene dispersion body.
Again, first graphene dispersion body vacuum drying oven is carried out vacuum deaerator under room temperature (25 DEG C).
After deaeration thoroughly, carry out dispersion ultrasound wave nano-dispersed instrument extremely disperseing 2.5h, obtain transparent stone
Ink alkene size dispersions.
Finally, Graphene ink is prepared by nano-milled for Graphene size dispersions.
For the serviceability of the Graphene ink of the checking embodiment of the present invention, below embodiment it is further elaborated.
Embodiment 9: the present embodiment uses the Graphene ink that embodiment 1-8 is prepared by high-speed inkjet printer, prints
The smooth performance test of brush.
Wherein, test temperature is 25 DEG C, and testing humidity is 70%, and concrete test result is as shown in the table:
In sum, the Graphene ink of the embodiment of the present invention, it is possible to will have Graphene and the change of excellent conductive performance
Learn doping, chemical modification Graphene is filled in polyester acrylate paste system, and good dispersion.Graphene layer imparts
The electric conductivity that solidification coating is good, chemical doping, modified group can improve graphene dispersion stability effectively.Polyester
Acid esters sizing material has the excellent specific properties such as appearance transparent, pliability is good, caking property good, weather-proof color inhibition, refractive index are high, can be comprehensive
Meet application properties requirement.On the other hand, by controlling monomer ratio, it is provided that appropriate system viscosity, can either be easy to
Graphene dispersion is possible to prevent again Graphene to reunite.Further, it is also possible to by the selection of initiator system is reduced solidification
Energy, raising solidification rate, can solidify rapidly when scattered Graphene sizing material is coated on base material, prevents Graphene solid
Assemble during change.Whole preparation process is controlled, simple to operate, with low cost, solvent-free volatilization, environmental friendliness, is suitable for
Large-scale industrial production.
The foregoing is only embodiments of the present invention, not thereby limit the scope of the claims of the present invention, every utilization is originally
Equivalent structure or equivalence flow process that description of the invention and accompanying drawing content are made convert, or are directly or indirectly used in what other were correlated with
Technical field, is the most in like manner included in the scope of patent protection of the present invention.
Claims (10)
1. a Graphene ink, it is characterised in that by weight percentage, its raw material consists of:
Described oligomer is polyester (methyl) acrylate；Described monomer is (methyl) acrylate.
Graphene ink the most according to claim 1, it is characterised in that by weight percentage, described Graphene ink
Raw material consist of:
Graphene ink the most according to claim 1, it is characterised in that by weight percentage, described Graphene ink
Raw material consist of:
4. according to the arbitrary described Graphene ink of claim 1-3, it is characterised in that described Graphene also includes: chemistry changes
Property Graphene and chemical doping Graphene；
The doping molecule of described chemical doping Graphene includes: in polyaniline, polythiophene, polypyrrole, polyacetylene and polyparaphenylene
One or more；
The functional group of described chemical modification Graphene includes: hydroxyl, ester group, pyrrole radicals, imidazole radicals, thienyl, furyl, benzene
One or more in the deriveding group of base, benzenesulfonic acid base, anilino-and above-mentioned functional group.
5. according to the arbitrary described Graphene ink of claim 1-3, it is characterised in that the mean molecule quantity of described oligomer is
10000-60000, average viscosity is 200-50000cps, and functional group's degree is 1-6.
6. according to the arbitrary described Graphene ink of claim 1-3, it is characterised in that described polyester (methyl) acrylate by
(methyl) acrylic acid, polyprotic acid and long-chain polyhydric alcohol copolymerization form.
7. according to the arbitrary described Graphene ink of claim 1-3, it is characterised in that the lamellar spacing of described Graphene is
0.34nm-10nm, planar dimension are 2nm-1000nm.
8. according to the arbitrary described Graphene ink of claim 1-3, it is characterised in that described (methyl) acrylate is carbon containing
(methyl) acrylate of hydrogen or carbon oxygen backbone, (methyl) acrylate of band heterocycle structure and the (first of hydroxyl structure
Base) one or more of acrylate.
9. according to the arbitrary described Graphene ink of claim 1-3, it is characterised in that described monomer is isobomyl acrylate
Ester, isobornyl methacrylate, 2-(Acryloyloxy)ethanol, hydroxyethyl methylacrylate, 4-hydroxybutyl acrylate, 1,4-ring
Hexane dimethanol mono acrylic ester, diethylene glycol monoacrylate, 1,6-HD mono acrylic ester, tetramethylolmethane three acrylic acid
Ester, trimethylolpropane dimethylacrylate, cyclopentylpropenoic acid ester, 2-cyclohexyl acrylate, 2-methacrylic acid ring
Own ester, isopropyl acrylate, dicyclo benzene oxygen ethyl propylene acid esters, isobutyl methacrylate, acrylic acid n-pentyl ester, acrylic acid are different
Butyl ester, Isooctyl acrylate monomer, 2-Propenoic acid, 2-methyl-, isooctyl ester, lauryl acrylate, n-octyl, decyl acrylate, methyl
One or more in decyl acrylate, methacrylic acid undecyl ester, 2-dodecylacrylate.
10. the preparation method of a Graphene ink, it is characterised in that including:
Take the arbitrary described raw material of claim 1-9, in reaction vessel, be stirred mixing mistake with predetermined mixing speed
Filter, forms Graphene just dispersion；
At normal temperatures, Graphene just dispersion is carried out vacuum deaerator；
To the just dispersion ultrasonic disperse of the Graphene after vacuum deaerator, form Graphene size dispersions；
Nano-milled Graphene size dispersions, forms Graphene ink.
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| CN106800817A (en) * | 2017-02-28 | 2017-06-06 | 北京银百汇网络科技有限公司 | A kind of digital UV ink-jets for commodity concealed anti-false and preparation method thereof |
| CN107384224A (en) * | 2017-08-24 | 2017-11-24 | 深圳市国创珈伟石墨烯科技有限公司 | A kind of graphene thermal conductivity UV glue and preparation method thereof |
| CN108276825A (en) * | 2018-02-11 | 2018-07-13 | 安徽省中彩印务有限公司 | A kind of environmental protection stable type cured printing ink and preparation method thereof |
| CN108323023A (en) * | 2018-01-16 | 2018-07-24 | 湖南国盛石墨科技有限公司 | One kind being based on heat cure Graphene conductive ink printing process |
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| CN110408267A (en) * | 2019-08-19 | 2019-11-05 | 泰能环保科技（浙江）有限公司 | A kind of Graphene conductive ink and preparation method thereof |
| CN115491077A (en) * | 2022-09-21 | 2022-12-20 | 刘智惠 | Quick-drying high-stability printing ink and preparation method thereof |
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| CN108323023B (en) * | 2018-01-16 | 2020-07-17 | 湖南国盛石墨科技有限公司 | Printing method based on thermosetting graphene conductive ink |
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| CN110408267A (en) * | 2019-08-19 | 2019-11-05 | 泰能环保科技（浙江）有限公司 | A kind of Graphene conductive ink and preparation method thereof |
| CN115491077A (en) * | 2022-09-21 | 2022-12-20 | 刘智惠 | Quick-drying high-stability printing ink and preparation method thereof |
| CN115491077B (en) * | 2022-09-21 | 2023-09-15 | 武汉易锦包装印务有限公司 | A kind of fast-drying and highly stable printing ink and preparation method thereof |
| CN118652475A (en) * | 2024-07-31 | 2024-09-17 | 四川亿欣新材料有限公司 | A calcium-based powder material for PVC hard products and a preparation method thereof |
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