CN101950128A - Photosensitive resin for plasma display screen - Google Patents
Photosensitive resin for plasma display screen Download PDFInfo
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- CN101950128A CN101950128A CN2010105027873A CN201010502787A CN101950128A CN 101950128 A CN101950128 A CN 101950128A CN 2010105027873 A CN2010105027873 A CN 2010105027873A CN 201010502787 A CN201010502787 A CN 201010502787A CN 101950128 A CN101950128 A CN 101950128A
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- photosensitive resin
- display screen
- plasma display
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- 239000011347 resin Substances 0.000 title claims abstract description 186
- 229920005989 resin Polymers 0.000 title claims abstract description 186
- 239000002904 solvent Substances 0.000 claims abstract description 78
- 239000013530 defoamer Substances 0.000 claims abstract description 45
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 165
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 150
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 146
- -1 ether acetic acid esters Chemical class 0.000 claims description 104
- 229920001577 copolymer Polymers 0.000 claims description 84
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 75
- 238000002156 mixing Methods 0.000 claims description 69
- TUVYSBJZBYRDHP-UHFFFAOYSA-N acetic acid;methoxymethane Chemical compound COC.CC(O)=O TUVYSBJZBYRDHP-UHFFFAOYSA-N 0.000 claims description 47
- 229920001296 polysiloxane Polymers 0.000 claims description 41
- 238000000034 method Methods 0.000 claims description 38
- 238000002360 preparation method Methods 0.000 claims description 38
- 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 claims description 33
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 31
- 239000004305 biphenyl Substances 0.000 claims description 21
- 235000010290 biphenyl Nutrition 0.000 claims description 21
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 21
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 20
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 17
- QYGBYAQGBVHMDD-XQRVVYSFSA-N (z)-2-cyano-3-thiophen-2-ylprop-2-enoic acid Chemical compound OC(=O)C(\C#N)=C/C1=CC=CS1 QYGBYAQGBVHMDD-XQRVVYSFSA-N 0.000 claims description 15
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 claims description 10
- IKOAVSIGNGDTNP-UHFFFAOYSA-N 3-hydroxy-1-phenylbutan-1-one Chemical compound CC(O)CC(=O)C1=CC=CC=C1 IKOAVSIGNGDTNP-UHFFFAOYSA-N 0.000 claims description 9
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 9
- XXXPIFADCVUZSA-UHFFFAOYSA-N 2-(3-chlorophenyl)-1-phenylethanone Chemical compound ClC1=CC=CC(CC(=O)C=2C=CC=CC=2)=C1 XXXPIFADCVUZSA-UHFFFAOYSA-N 0.000 claims description 8
- 235000015511 Liquidambar orientalis Nutrition 0.000 claims description 8
- 239000004870 Styrax Substances 0.000 claims description 8
- 235000000126 Styrax benzoin Nutrition 0.000 claims description 8
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 8
- OTKCEEWUXHVZQI-UHFFFAOYSA-N 1,2-diphenylethanone Chemical compound C=1C=CC=CC=1C(=O)CC1=CC=CC=C1 OTKCEEWUXHVZQI-UHFFFAOYSA-N 0.000 claims description 7
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims description 7
- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- YLHXLHGIAMFFBU-UHFFFAOYSA-N methyl phenylglyoxalate Chemical compound COC(=O)C(=O)C1=CC=CC=C1 YLHXLHGIAMFFBU-UHFFFAOYSA-N 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 6
- NLGDWWCZQDIASO-UHFFFAOYSA-N 2-hydroxy-1-(7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-yl)-2-phenylethanone Chemical compound OC(C(=O)c1cccc2Oc12)c1ccccc1 NLGDWWCZQDIASO-UHFFFAOYSA-N 0.000 claims description 5
- 238000007046 ethoxylation reaction Methods 0.000 claims description 5
- LVHBHZANLOWSRM-UHFFFAOYSA-N itaconic acid Chemical compound OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 5
- GZBSIABKXVPBFY-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)propane-1,3-diol;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.OC(=O)C=C.OCC(CO)(CO)CO GZBSIABKXVPBFY-UHFFFAOYSA-N 0.000 claims description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 4
- 239000007983 Tris buffer Substances 0.000 claims description 4
- 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 claims description 4
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 4
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 claims description 4
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 4
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical group CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 3
- 238000007334 copolymerization reaction Methods 0.000 claims description 3
- 239000001530 fumaric acid Substances 0.000 claims description 3
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 3
- 239000011976 maleic acid Substances 0.000 claims description 3
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 3
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 claims description 3
- XLYMOEINVGRTEX-ONEGZZNKSA-N (e)-4-ethoxy-4-oxobut-2-enoic acid Chemical compound CCOC(=O)\C=C\C(O)=O XLYMOEINVGRTEX-ONEGZZNKSA-N 0.000 claims description 2
- AYAUWVRAUCDBFR-ONEGZZNKSA-N (e)-4-oxo-4-propoxybut-2-enoic acid Chemical compound CCCOC(=O)\C=C\C(O)=O AYAUWVRAUCDBFR-ONEGZZNKSA-N 0.000 claims description 2
- AYAUWVRAUCDBFR-ARJAWSKDSA-N (z)-4-oxo-4-propoxybut-2-enoic acid Chemical compound CCCOC(=O)\C=C/C(O)=O AYAUWVRAUCDBFR-ARJAWSKDSA-N 0.000 claims description 2
- IZUVGRMMRWJVKU-UHFFFAOYSA-N 3-ethoxycarbonylbut-3-enoic acid Chemical compound CCOC(=O)C(=C)CC(O)=O IZUVGRMMRWJVKU-UHFFFAOYSA-N 0.000 claims description 2
- NEAHVGRDHLQWPP-UHFFFAOYSA-N 3-propoxycarbonylbut-3-enoic acid Chemical compound CCCOC(=O)C(=C)CC(O)=O NEAHVGRDHLQWPP-UHFFFAOYSA-N 0.000 claims description 2
- IEPRKVQEAMIZSS-UHFFFAOYSA-N Di-Et ester-Fumaric acid Natural products CCOC(=O)C=CC(=O)OCC IEPRKVQEAMIZSS-UHFFFAOYSA-N 0.000 claims description 2
- IEPRKVQEAMIZSS-WAYWQWQTSA-N Diethyl maleate Chemical compound CCOC(=O)\C=C/C(=O)OCC IEPRKVQEAMIZSS-WAYWQWQTSA-N 0.000 claims description 2
- SSOONFBDIYMPEU-UHFFFAOYSA-N [3-hydroxy-2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propyl] prop-2-enoate Chemical compound OCC(CO)(CO)COCC(CO)(CO)COC(=O)C=C SSOONFBDIYMPEU-UHFFFAOYSA-N 0.000 claims description 2
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 claims description 2
- HSDFKDZBJMDHFF-UHFFFAOYSA-N methyl 3-ethoxypropanoate Chemical class CCOCCC(=O)OC HSDFKDZBJMDHFF-UHFFFAOYSA-N 0.000 claims description 2
- BOQSSGDQNWEFSX-UHFFFAOYSA-N propan-2-yl 2-methylprop-2-enoate Chemical compound CC(C)OC(=O)C(C)=C BOQSSGDQNWEFSX-UHFFFAOYSA-N 0.000 claims description 2
- 244000028419 Styrax benzoin Species 0.000 claims 2
- 239000000203 mixture Substances 0.000 claims 1
- 230000004888 barrier function Effects 0.000 abstract description 4
- 206010034972 Photosensitivity reaction Diseases 0.000 abstract 1
- 229920006026 co-polymeric resin Polymers 0.000 abstract 1
- 239000003999 initiator Substances 0.000 abstract 1
- 230000036211 photosensitivity Effects 0.000 abstract 1
- 230000006837 decompression Effects 0.000 description 34
- 238000004821 distillation Methods 0.000 description 34
- WROUWQQRXUBECT-UHFFFAOYSA-M 2-ethylacrylate Chemical compound CCC(=C)C([O-])=O WROUWQQRXUBECT-UHFFFAOYSA-M 0.000 description 29
- 206010034960 Photophobia Diseases 0.000 description 7
- 208000013469 light sensitivity Diseases 0.000 description 7
- 241000736148 Styrax Species 0.000 description 6
- 239000003292 glue Substances 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- RLAHWVDQYNDAGG-UHFFFAOYSA-N Methanetriol Chemical compound OC(O)O RLAHWVDQYNDAGG-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 229920002120 photoresistant polymer Polymers 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 2
- 208000034189 Sclerosis Diseases 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- MTPIZGPBYCHTGQ-UHFFFAOYSA-N 2-[2,2-bis(2-prop-2-enoyloxyethoxymethyl)butoxy]ethyl prop-2-enoate Chemical group C=CC(=O)OCCOCC(CC)(COCCOC(=O)C=C)COCCOC(=O)C=C MTPIZGPBYCHTGQ-UHFFFAOYSA-N 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002114 biscuit porcelain Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 238000005227 gel permeation chromatography Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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- Gas-Filled Discharge Tubes (AREA)
- Materials For Photolithography (AREA)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
The invention discloses a photosensitive resin for a plasma display screen. The photosensitive resin for the plasma display screen comprises acrylate copolymer resin and solvent as well as photoplymerization initiator and defoamer. Compared with the existing photosensitive resin, the photosensitive resin for the plasma display screen provided by the invention has the advantages of higher resolution, excellent photosensitivity and image developing performance, and is particularly suitable for preparing a barrier of a PDP screen.
Description
Technical field
The present invention relates to a kind of used for plasma display screen photosensitive resin.
Background technology
Plasma panel (Plasma display panel is called for short PDP) is the electronic installation that utilizes plasma (plasma) discharge formation image.Make it that plasma discharge effect takes place after applying voltage on the electrode that in the PDP discharge space, distributes, and visual by the vacuum ultraviolet (VUV) that in the plasma discharge process, sends thereby come the fluorescence excitation bisque to form.
Along with market is vigorous day by day to the demand of flat-panel monitors such as PDP, LCD and OLED, manufacturers have added big picture exploitation dynamics, thereby require the high-resolution of display device, and the cry of high image resolution is also very high.
Barrier is not only the works that discharge space is provided in PDP, its more important role is to prevent to occur between the adjacent display unit (cell) simultaneously, the works that crosstalk mutually (the cross talk) of optics aspect forms on the plate of back is so it is bringing into play important effect in PDP image display quality.
And existing P DP barrier form in required photoresist be on the attaching power of substrate certain limitation is arranged, and resolution is not high yet.
Summary of the invention
The purpose of this invention is to provide a kind of used for plasma display screen photosensitive resin.
Used for plasma display screen photosensitive resin provided by the invention comprises acrylic copolymeric resin, Photoepolymerizationinitiater initiater, defoamer and solvent.
Above-mentioned used for plasma display screen photosensitive resin also can only be made up of above-mentioned four components.In this photosensitive resin, the weight-average molecular weight of described acrylic copolymeric resin is 20000-80000, specifically can be 20000-60000,20000-50000,20000-40000,20000-25000,25000-60000,25000-50000,25000-40000,30000-60000,30000-50000,30000-40000,40000-60000,40000-50000 or 50000-60000, preferred 30000-50000.
Described solvent is selected from least a in ethylene glycol monoemethyl ether acetate, the only methyl ether acetate of propylene glycol, propylene glycol monomethyl ether, the only ether acetic acid esters of propylene glycol, diethylene glycol dimethyl ether, diethylene glycol ethylmethyl ether, cyclohexanone, 3-methoxy propyl acetoacetic ester, 3-ethoxy-propionic acid methyl esters, 3-ethoxyl ethyl propionate, butanone, isopropyl alcohol, ethanol and the methyl alcohol, at least a in preferred only methyl ether acetate of propylene glycol and the ethylene glycol monoemethyl ether acetate.
Described Photoepolymerizationinitiater initiater is the I type light trigger of free radical polymerization in the photochemical reaction, the initiating agent of various the type all is suitable for, as being selected from least a in styrax, benzoin ether, styrax diether, methyl benzoylformate, S-(4-benzoyl) thiobenzoate phenyl ester, 3-hydroxy-3-methyl propiophenone, benzyl phenyl ketone and the m-chloro benzyl phenyl ketone;
Described defoamer is a silicon oil foam killer, is selected from least a in methyl polysiloxane and the dimethyl diphenyl polysiloxane; This methyl polysiloxane and dimethyl diphenyl polysiloxane can be bought by open commercial sources and obtain, and its viscosity can be 80-120cp or 100cp;
The ratio of quality and the number of copies of described acrylic copolymeric resin, Photoepolymerizationinitiater initiater, defoamer and solvent is 10-40: 0.5-10: 0.1-2: 50-90, specifically can be 10-35: 0.5-5: 0.1-2: 60-89,10-30: 0.5-5: 0.1-2: 60-89,10-20: 0.5-4: 0.1-1: 60-88,20-35: 1-5: 0.5-2: 63-89,20-30: 1-4: 0.5-1: 63-88 or 20-30: 1-3: 0.5-1: 65-77, preferred 10-30: 0.5-5: 0.5-2: 60-90, more preferably 20-30: 2-4: 1-2: 60-80.
In the above-mentioned used for plasma display screen photosensitive resin, the mass fraction of acrylic copolymeric resin must be in above-mentioned 10-40 mass fraction scope, and its mass fraction surpasses 40 easy gels, and photoresist is when depositing, and its stability can decline; Its mass fraction is lower than and occurs the long phenomenon of development time in the development work in 10 o'clock easily.The mass fraction of Photoepolymerizationinitiater initiater must be controlled at the 0.5-10 scope, and its mass fraction is lower than at 0.5 o'clock, and the molecular weight of acrylic copolymeric resin polymkeric substance can roll up; Mass fraction surpasses at 10 o'clock, and the molecular weight of acrylic copolymeric resin polymkeric substance can reduce and then cause sensitivity to descend in a large number, and the figure pattern is not good.The effect of defoamer is that each component is easier in the photosensitive resin mixes in order to make, and prevents pin hole (pin hole) phenomenon, reduces because of film is inhomogeneous and causes problems such as being coated with bad generation, according to circumstances can suitably add.The effect of solvent is the dissolubility that improves each component in the photosensitive resin, reduces the preceding viscosity of acryl resin system coating, to improve coating, adds as required.
Wherein, described acrylic copolymeric resin is by behind unsaturated carboxylic acid, comonomer and the organic solvent mixing copolyreaction taking place, and steams with the method for decompression distillation to desolventize the back and get again;
Described unsaturated carboxylic acid is selected from least a in acrylic acid, methacrylate, methylene succinic acid, maleic acid and the fumaric acid;
Described comonomer is selected from ethyl acrylate, propyl acrylate, acrylic acid oxo two-2, the 1-ethyl, the trimethylolpropane double methacrylate, trimethylolpropane triacrylate, pentaerythritol triacrylate, tetramethylol methane tetraacrylate, ethoxylation trihydroxy methyl propyl group triacrylate, the propoxylation trimethylolpropane triacrylate, dipentaerythritol five acrylate contract, dipentaerythritol acrylate contracts, ethyl 2-methacrylate, the 2-propyl methacrylate, 2-methacrylic acid oxo two-2, the 1-ethyl, the two 2-methacrylates of trimethylolpropane, trimethylolpropane tris 2-methacrylate, pentaerythrite three 2-methacrylates, pentaerythrite four 2-methacrylates, ethoxylation trihydroxy methyl propyl group three 2-methacrylates, propoxylation trimethylolpropane tris 2-methacrylate, dipentaerythritol five 2-methacrylates contract, dipentaerythritol six 2-methacrylates contract, the methylene succinic acid ethyl ester, the methylene succinic acid propyl ester, ethyl maleate, in maleic acid propyl ester and fumaric acid ethyl ester and the fumaric acid propyl ester at least two kinds;
Described organic solvent is selected from least a in ethylene glycol monoemethyl ether acetate, the only methyl ether acetate of propylene glycol, propylene glycol monomethyl ether, the only ether acetic acid esters of propylene glycol, diethylene glycol dimethyl ether and the diethylene glycol ethylmethyl ether, at least a in preferred only methyl ether acetate of propylene glycol and the ethylene glycol monoemethyl ether acetate;
The mass ratio of described unsaturated carboxylic acid and comonomer is 1: 10-1: 1, preferred 3: 7-4: 6; The quality sum of unsaturated carboxylic acid and comonomer and the quality of organic solvent are in a ratio of 1: 0.25-1, preferred 1: 0.5-1.
In the described copolymerization step, temperature is 50-200 ℃, and preferred 100-150 ℃, the time is 2-10 hour, preferred 4-5 hour.
The method of the above-mentioned used for plasma display screen photosensitive resin of preparation provided by the invention comprises the steps: described acrylic copolymeric resin, Photoepolymerizationinitiater initiater, defoamer and solvent, obtains described used for plasma display screen photosensitive resin.
The application of the used for plasma display screen photosensitive resin that the invention described above provides in the preparation plasma panel also belongs to protection scope of the present invention.
Used for plasma display screen photosensitive resin provided by the invention is compared than existing photoresist, has high resolution, and outstanding photonasty and developing performance are highly suitable for preparing the barrier that PDP shields.
Embodiment
The invention will be further described below in conjunction with specific embodiment, but the present invention is not limited to following examples.Method is conventional method if no special instructions described in the following embodiment, and described compound all can obtain from open commercial sources purchase if no special instructions.Used ethoxylation trihydroxy methyl propyl group triacrylate is available from the grand brightness chemical industry of Yixing City company limited among the embodiment, production code member is CAS 28961-43-5, the propoxylation trimethylolpropane triacrylate is available from the grand brightness chemical industry of Yixing City company limited, production code member is CAS 53879-54-2, used methyl polysiloxane is available from the lucky roc fluosilicic in Shenzhen Materials Co., Ltd, production code member is 201 methyl-silicone oil 201-100 (viscosity 100cp), used dimethyl diphenyl polysiloxane is available from Chengdu Gracia chemical technology company limited, and production code member is 1026963 (viscosity 100cp).The weight-average molecular weight that following embodiment step 1) prepares the gained acrylic copolymeric resin all gets according to the gel chromatography of routine.
Embodiment 1
1) preparation acrylic copolymeric resin:
With acrylic acid 10 weight portions, trimethylolpropane triacrylate 40 weight portions, acrylic acid oxo two-2,1-ethyl 40 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only ether acetic acid esters 27.5 weight portions of solvent propylene glycol, under 50 ℃, carried out polyreaction 2 hours, steam with the method for decompression distillation then and desolventize the only ether acetic acid esters of propylene glycol, obtain weight-average molecular weight and be 20,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 25 that step 1) is prepared the gained weight-average molecular weight, only methyl ether acetate 89 weight portions of 000 acrylic copolymeric resin 10 weight portions, Photoepolymerizationinitiater initiater styrax 0.5 weight portion, defoamer methyl polysiloxane 0.5 weight portion and solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 2
1) preparation acrylic copolymeric resin:
With acrylic acid 10 weight portions, trimethylolpropane triacrylate 40 weight portions, acrylic acid oxo two-2,1-ethyl 40 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only ether acetic acid esters 55 weight portions of solvent propylene glycol, under 100 ℃, carried out polyreaction 2 hours, steam with the method for decompression distillation then and desolventize the only ether acetic acid esters of propylene glycol, obtain weight-average molecular weight and be 20,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 20 that step 1) is prepared the gained weight-average molecular weight, only methyl ether acetate 88 weight portions of 000 acrylic copolymeric resin 10 weight portions, Photoepolymerizationinitiater initiater styrax 1 weight portion, defoamer methyl polysiloxane 1 weight portion and solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 3
1) with acrylic acid 10 weight portion, trimethylolpropane triacrylate 40 weight portions, acrylic acid oxo two-2,1-ethyl 40 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only ether acetic acid esters 110 weight portions of solvent propylene glycol, under 200 ℃, carried out polyreaction 10 hours, steam with the method for decompression distillation then and desolventize the only ether acetic acid esters of propylene glycol, obtain weight-average molecular weight and be 20,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 20 that step 1) is prepared the gained weight-average molecular weight, only methyl ether acetate 83 weight portions of 000 acrylic copolymeric resin 10 weight portions, Photoepolymerizationinitiater initiater styrax 5 weight portions, defoamer methyl polysiloxane 2 weight portions and solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 4
1) with acrylic acid 30 weight portion, trimethylolpropane triacrylate 30 weight portions, acrylic acid oxo two-2,1-ethyl 30 weight portions and 2-ethyl acrylate 10 weight portions are mixing in only ether acetic acid esters 50 weight portions of solvent propylene glycol, under 100 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize the only ether acetic acid esters of propylene glycol, obtain weight-average molecular weight and be 30,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 30 that step 1) is prepared the gained weight-average molecular weight, only methyl ether acetate 89 weight portions of 000 acrylic copolymeric resin 10 weight portions, Photoepolymerizationinitiater initiater benzoin ether 0.5 weight portion, defoamer methyl polysiloxane 0.5 weight portion and solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 5
1) with acrylic acid 30 weight portion, trimethylolpropane triacrylate 30 weight portions, acrylic acid oxo two-2,1-ethyl 30 weight portions and 2-ethyl acrylate 10 weight portions are mixing in only ether acetic acid esters 50 weight portions of solvent propylene glycol, under 100 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize the only ether acetic acid esters of propylene glycol, obtain weight-average molecular weight and be 30,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 30 that step 1) is prepared the gained weight-average molecular weight, only methyl ether acetate 77 weight portions of 000 acrylic copolymeric resin 20 weight portions, Photoepolymerizationinitiater initiater benzoin ether 2 weight portions, defoamer methyl polysiloxane 1 weight portion and solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 6
1) with acrylic acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only ether acetic acid esters 50 weight portions of solvent propylene glycol, under 150 ℃, carried out polyreaction 4 hours, steam with the method for decompression distillation then and desolventize the only ether acetic acid esters of propylene glycol, obtain weight-average molecular weight and be 50,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 50 that step 1) is prepared the gained weight-average molecular weight, only methyl ether acetate 66 weight portions of 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater benzoin ether 2 weight portions, defoamer methyl polysiloxane 2 weight portions and solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 7
1) with acrylic acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only ether acetic acid esters 100 weight portions of solvent propylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize the only ether acetic acid esters of propylene glycol, obtain weight-average molecular weight and be 50,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 50 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater styrax diether 2 weight portions, defoamer methyl polysiloxane 2 weight portions and only methyl ether acetate 66 weight portions of solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 8
1) with acrylic acid 50 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 10 weight portions are mixing in only ether acetic acid esters 100 weight portions of solvent propylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize the only ether acetic acid esters of propylene glycol, obtain weight-average molecular weight and be 60,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 60 that step 1) is prepared the gained weight-average molecular weight, only methyl ether acetate 66 weight portions of 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater methyl benzoylformate 2 weight portions, defoamer methyl polysiloxane 2 weight portions and solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 9
1) with acrylic acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only ether acetic acid esters 100 weight portions of solvent propylene glycol, under 200 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize the only ether acetic acid esters of propylene glycol, obtain weight-average molecular weight and be 80,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 60 that step 1) is prepared the gained weight-average molecular weight, only methyl ether acetate 66 weight portions of 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater methyl benzoylformate 2 weight portions, defoamer methyl polysiloxane 2 weight portions and solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 10
1) with acrylic acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only ether acetic acid esters 100 weight portions of solvent propylene glycol, under 150 ℃, carried out polyreaction 10 hours, steam with the method for decompression distillation then and desolventize the only ether acetic acid esters of propylene glycol, obtain weight-average molecular weight and be 80,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 60 that step 1) is prepared the gained weight-average molecular weight, only methyl ether acetate 66 weight portions of 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater methyl benzoylformate 2 weight portions, defoamer methyl polysiloxane 2 weight portions and solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 11
1) with acrylic acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only ether acetic acid esters 100 weight portions of solvent propylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize the only ether acetic acid esters of propylene glycol, obtain weight-average molecular weight and be 50,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 50 that step 1) is prepared the gained weight-average molecular weight, only methyl ether acetate 63 weight portions of 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater methyl benzoylformate 5 weight portions, defoamer methyl polysiloxane 2 weight portions and solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 12
1) with acrylic acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only ether acetic acid esters 100 weight portions of solvent propylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize the only ether acetic acid esters of propylene glycol, obtain weight-average molecular weight and be 50,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 50 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater S-(4-benzoyl) thiobenzoate phenyl ester 2 weight portions, defoamer methyl polysiloxane 0.1 weight portion and only methyl ether acetate 67.9 weight portions of solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 13
1) with acrylic acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only ether acetic acid esters 100 weight portions of solvent propylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize the only ether acetic acid esters of propylene glycol, obtain weight-average molecular weight and be 50,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 50 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater S-(4-benzoyl) thiobenzoate phenyl ester 2 weight portions, defoamer methyl polysiloxane 0.5 weight portion and only methyl ether acetate 67.5 weight portions of solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 14
1) with acrylic acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only ether acetic acid esters 100 weight portions of solvent propylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize the only ether acetic acid esters of propylene glycol, obtain weight-average molecular weight and be 50,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 50 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater S-(4-benzoyl) thiobenzoate phenyl ester 2 weight portions, defoamer methyl polysiloxane 1 weight portion and only methyl ether acetate 67 weight portions of solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 15
1) with acrylic acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only ether acetic acid esters 100 weight portions of solvent propylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize the only ether acetic acid esters of propylene glycol, obtain weight-average molecular weight and be 50,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 50 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater S-(4-benzoyl) thiobenzoate phenyl ester 1 weight portion, defoamer methyl polysiloxane 1 weight portion and only methyl ether acetate 68 weight portions of solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 16
1) with acrylic acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only ether acetic acid esters 100 weight portions of solvent propylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize the only ether acetic acid esters of propylene glycol, obtain weight-average molecular weight and be 50,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 50 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater 3-hydroxy-3-methyl propiophenone 4 weight portions, defoamer methyl polysiloxane 1 weight portion and only methyl ether acetate 65 weight portions of solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 17
1) with acrylic acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only ether acetic acid esters 100 weight portions of solvent propylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize the only ether acetic acid esters of propylene glycol, obtain weight-average molecular weight and be 50,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 50 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater 3-hydroxy-3-methyl propiophenone 5 weight portions, defoamer dimethyl diphenyl polysiloxane 1 weight portion and only methyl ether acetate 64 weight portions of solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 18
1) with acrylic acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only ether acetic acid esters 100 weight portions of solvent propylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize the only ether acetic acid esters of propylene glycol, obtain weight-average molecular weight and be 50,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 50 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 35 weight portions, Photoepolymerizationinitiater initiater 3-hydroxy-3-methyl propiophenone 3 weight portions, defoamer dimethyl diphenyl polysiloxane 2 weight portions and only methyl ether acetate 60 weight portions of solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 19
1) with acrylic acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only methyl ether acetate 100 weight portions of solvent ethylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize ethylene glycol monoemethyl ether acetate, obtain weight-average molecular weight and be 50,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 50 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater 3-hydroxy-3-methyl propiophenone 2 weight portions, defoamer dimethyl diphenyl polysiloxane 1 weight portion and only methyl ether acetate 67 weight portions of solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 20
1) with acrylic acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions mixing in solvent propylene glycol monomethyl ether 100 weight portions, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize propylene glycol monomethyl ether, obtain weight-average molecular weight and be 50,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 50 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater 3-hydroxy-3-methyl propiophenone 2 weight portions, defoamer dimethyl diphenyl polysiloxane 1 weight portion and only methyl ether acetate 67 weight portions of solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 21
1) with acrylic acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in solvent diethylene glycol dimethyl ether 50 weight portions and diethylene glycol ethylmethyl ether 50 weight portions, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize diethylene glycol dimethyl ether and diethylene glycol ethylmethyl ether, obtain weight-average molecular weight and be 50,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 50 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater 3-hydroxy-3-methyl propiophenone 2 weight portions, defoamer dimethyl diphenyl polysiloxane 1 weight portion and only methyl ether acetate 67 weight portions of solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 22
1) with acrylic acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only methyl ether acetate 100 weight portions of solvent ethylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize ethylene glycol monoemethyl ether acetate, obtain weight-average molecular weight and be 50,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 50 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater 3-hydroxy-3-methyl propiophenone 2 weight portions, defoamer dimethyl diphenyl polysiloxane 1 weight portion and only methyl ether acetate 67 weight portions of solvent propylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 23
1) with acrylic acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only methyl ether acetate 100 weight portions of solvent ethylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize ethylene glycol monoemethyl ether acetate, obtain weight-average molecular weight and be 50,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 50 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater benzyl phenyl ketone 2 weight portions, defoamer dimethyl diphenyl polysiloxane 1 weight portion and solvent propylene glycol monomethyl ether 67 weight portions are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 24
1) with acrylic acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only methyl ether acetate 100 weight portions of solvent ethylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize ethylene glycol monoemethyl ether acetate, obtain weight-average molecular weight and be 50,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 50 that step 1) is prepared the gained weight-average molecular weight, only ether acetic acid esters 67 weight portions of 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater benzyl phenyl ketone 2 weight portions, defoamer dimethyl diphenyl polysiloxane 1 weight portion and solvent propylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 25
1) with acrylic acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only methyl ether acetate 100 weight portions of solvent ethylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize ethylene glycol monoemethyl ether acetate, obtain weight-average molecular weight and be 50,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 50 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater benzyl phenyl ketone 2 weight portions, defoamer dimethyl diphenyl polysiloxane 1 weight portion and solvent diethylene glycol ethylmethyl ether 67 weight portions are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 26
1) with methacrylate 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only methyl ether acetate 100 weight portions of solvent ethylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize diethylene glycol dimethyl ether and diethylene glycol ethylmethyl ether, obtain weight-average molecular weight and be 50,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 50 that step 1) is prepared the gained weight-average molecular weight, only methyl ether acetate 67 weight portions of 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater benzyl phenyl ketone 2 weight portions, defoamer dimethyl diphenyl polysiloxane 1 weight portion and solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 27
1) with methylene succinic acid olefin(e) acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only methyl ether acetate 100 weight portions of solvent ethylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize diethylene glycol dimethyl ether and diethylene glycol ethylmethyl ether, obtain weight-average molecular weight and be 50,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 50 that step 1) is prepared the gained weight-average molecular weight, only methyl ether acetate 67 weight portions of 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater benzyl phenyl ketone 2 weight portions, defoamer dimethyl diphenyl polysiloxane 1 weight portion and solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 28
1) with maleic acid acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only methyl ether acetate 100 weight portions of solvent ethylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize diethylene glycol dimethyl ether and diethylene glycol ethylmethyl ether, obtain weight-average molecular weight and be 40,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 40 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater m-chloro benzyl phenyl ketone 2 weight portions, defoamer dimethyl diphenyl polysiloxane 1 weight portion and only methyl ether acetate 67 weight portions of solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 29
1) with fumaric acid acid 40 weight portion, trimethylolpropane triacrylate 20 weight portions, acrylic acid oxo two-2,1-ethyl 20 weight portions and 2-ethyl acrylate 20 weight portions are mixing in only methyl ether acetate 100 weight portions of solvent ethylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize diethylene glycol dimethyl ether and diethylene glycol ethylmethyl ether, obtain weight-average molecular weight and be 40,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 40 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater m-chloro benzyl phenyl ketone 2 weight portions, defoamer dimethyl diphenyl polysiloxane 1 weight portion and only methyl ether acetate 67 weight portions of solvent ethylene glycol are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 30
1) with acrylic acid 40 weight portion, ethyl acrylate 20 weight portions, propyl acrylate 20 weight portions and trimethylolpropane double methacrylate 20 weight portions are mixing in only methyl ether acetate 100 weight portions of solvent ethylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize ethylene glycol monoemethyl ether acetate, obtain weight-average molecular weight and be 40,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 40 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater m-chloro benzyl phenyl ketone 2 weight portions, defoamer dimethyl diphenyl polysiloxane 1 weight portion and solvent diethylene glycol ethylmethyl ether 67 weight portions are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 31
1) with acrylic acid 40 weight portion, pentaerythritol triacrylate 20 weight portions, tetramethylol methane tetraacrylate 20 weight portions and trihydroxy methyl propyl group oxirane sex change orthoformic acid acrylate 20 weight portions mixing in only methyl ether acetate 100 weight portions of solvent ethylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize ethylene glycol monoemethyl ether acetate, obtain weight-average molecular weight and be 40,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 40 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater m-chloro benzyl phenyl ketone 2 weight portions, defoamer dimethyl diphenyl polysiloxane 1 weight portion and solvent diethylene glycol ethylmethyl ether 67 weight portions are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 32
1) with acrylic acid 40 weight portion, trihydroxy methyl propyl group epoxypropane sex change orthoformic acid acrylate 30 weight portions and trihydroxy methyl propyl group oxirane sex change orthoformic acid acrylate 30 weight portions mixing in only methyl ether acetate 100 weight portions of solvent ethylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize ethylene glycol monoemethyl ether acetate, obtain weight-average molecular weight and be 40,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 40 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater m-chloro benzyl phenyl ketone 2 weight portions, defoamer dimethyl diphenyl polysiloxane 1 weight portion and solvent diethylene glycol ethylmethyl ether 67 weight portions are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
Embodiment 33
1) with acrylic acid 40 weight portion, pentaerythritol triacrylate 30 weight portions and tetramethylol methane tetraacrylate 30 weight portions are mixing in only methyl ether acetate 100 weight portions of solvent ethylene glycol, under 150 ℃, carried out polyreaction 5 hours, steam with the method for decompression distillation then and desolventize ethylene glycol monoemethyl ether acetate, obtain weight-average molecular weight and be 40,000 acrylic copolymeric resin;
2) preparation used for plasma display screen photosensitive resin provided by the invention:
It is 40 that step 1) is prepared the gained weight-average molecular weight, 000 acrylic copolymeric resin 30 weight portions, Photoepolymerizationinitiater initiater m-chloro benzyl phenyl ketone 2 weight portions, defoamer dimethyl diphenyl polysiloxane 1 weight portion and solvent diethylene glycol ethylmethyl ether 67 weight portions are mixing at normal temperatures, obtains used for plasma display screen photosensitive resin provided by the invention.
After the various embodiments described above are prepared gained used for plasma display screen photosensitive resin coating film forming, graphics resolution behind its developing performance, photosensitive property and the post bake is estimated.
The development evaluation:
Apply the back at the photosensitive compoistion that the various embodiments described above was obtained in 1 minute with the even glue speed rotation of 3500r/min with rotary glue spreader on the substrate and forming the thick film of 2.5um～3um after with 90 ℃ of bakings on the hot plate, it is 15mw/cm with 365nm, intensity that the film that above-mentioned all thickness is identical covers the back with mask plate
2Ultraviolet ray irradiation exposed in 20 seconds, being 5% tetramethylammonium hydroxide aqueous solution with mass percentage concentration again cleaned 1 minute with ultrapure water after developing 5 minutes down at 25 ℃, and pattern edge on substrate flatness and the residue situation after through development observed with 50 power microscopes in the back that disposes.
One, flatness
Zero: it is clean to be expressed as pattern edge, smooth no burr
*: it is unclean to be expressed as pattern edge, out-of-flatness and burr are arranged
Two, residue:
Whether the figure position of observing after aforesaid substrate has developed with 250 power microscopes has residue.
Zero: be expressed as no residue,
△: level of residue is few
*: level of residue is many
The light sensitivity evaluation criterion is as follows:
Applying the back at the photosensitive resin that the various embodiments described above was obtained in 1 minute with the even glue speed rotation of 3500r/min with rotary glue spreader on the substrate and forming the thick film of 2.5um～3um after with 90 ℃ of bakings on the hot plate, is 15mw/cm with 365nm, intensity after the film that above-mentioned all thickness is identical covers with the mask plate of 20 μ m live widths
2Ultraviolet ray irradiation different time expose, again with mass percentage concentration be 5% tetramethylammonium hydroxide aqueous solution 25 ℃ developed 5 minutes down after with ultrapure water cleaning 1 minute, be 15mw/cm with figure with 365nm, intensity afterwards
235～40 seconds of ultraviolet ray irradiation after, the temperature baking is 3 minutes in 120 ℃, heating made its sclerosis post bake in 60 minutes in 220 ℃ of hot stoves again, obtained graphic films, with the resolution of scanning electron microscope test pattern film.To obtain the evaluation criterion of outstanding graphic films required exposure time of resolution as light sensitivity, time shutter is short more, light sensitivity is good more: when time shutter during less than 10 seconds, outstanding for light sensitivity, the time shutter is when being 10～20 seconds, for light sensitivity better, time shutter is when being 20～30 seconds, common for light sensitivity, the time shutter is during greater than 30 seconds, for light sensitivity poor.
The graphics resolution evaluation of graphic films:
Applying the back at the photosensitive resin that the various embodiments described above was obtained in 1 minute with the even glue speed rotation of 3500r/min with rotary glue spreader on the substrate and forming the thick film of 2.5um～3um after with 90 ℃ of bakings on the hot plate, is 15mw/cm with 365nm, intensity after the film that above-mentioned all thickness is identical covers with the mask plate of 20 μ m live widths
2Ultraviolet ray irradiation exposed in 20 seconds, again with mass percentage concentration be 1% tetramethylammonium hydroxide aqueous solution 25 ℃ developed 2 minutes down after with ultrapure water cleaning 1 minute, be 15mw/cm with figure with 365nm, intensity afterwards
235～40 seconds of ultraviolet ray irradiation after, the temperature baking is 3 minutes in 120 ℃, heating made its sclerosis post bake in 60 minutes in 220 ℃ of hot stoves again, obtained graphic films, with the resolution of scanning electron microscope test pattern film.Live width is even, and no burr or burr resolution are outstanding less than resolution 0.5 μ m, and the live width edge is burr slightly, and the burr size is common 0.5～1 μ m's, and live width edge burr are more, and size 1～3 μ m for poor.
Above-mentioned testing result is all listed in the table 1.
The measurement result of the graphics resolution of the developing performance of table 1, photosensitive resin, photosensitive property and graphic films
As shown in Table 1, adopt acrylic copolymeric resin, Photoepolymerizationinitiater initiater, defoamer and the solvent of system of the present invention, control suitable mass ratio, can the very outstanding used for plasma display screen photosensitive resin of obtained performance.
Claims (10)
1. a used for plasma display screen photosensitive resin comprises acrylic copolymeric resin, solvent, Photoepolymerizationinitiater initiater and defoamer.
2. photosensitive resin according to claim 1 is characterized in that: the weight-average molecular weight of described acrylic copolymeric resin is 20000-50000, preferred 30000-50000.
3. photosensitive resin according to claim 1 and 2, it is characterized in that: described solvent is selected from least a in ethylene glycol monoemethyl ether acetate, the only methyl ether acetate of propylene glycol, propylene glycol monomethyl ether, the only ether acetic acid esters of propylene glycol, diethylene glycol dimethyl ether, diethylene glycol ethylmethyl ether, cyclohexanone, 3-methoxy propyl acetoacetic ester, 3-ethoxy-propionic acid methyl esters, 3-ethoxyl ethyl propionate, butanone, isopropyl alcohol, ethanol and the methyl alcohol, at least a in preferred only methyl ether acetate of propylene glycol and the ethylene glycol monoemethyl ether acetate;
Described Photoepolymerizationinitiater initiater is selected from least a in styrax, benzoin ether, styrax diether, methyl benzoylformate, S-(4-benzoyl) thiobenzoate phenyl ester, 3-hydroxy-3-methyl propiophenone, benzyl phenyl ketone and the m-chloro benzyl phenyl ketone;
Described defoamer is selected from least a in methyl polysiloxane and the dimethyl diphenyl polysiloxane.
4. according to the arbitrary described photosensitive resin of claim 1-3, it is characterized in that: described used for plasma display screen photosensitive resin is by acrylic copolymeric resin, Photoepolymerizationinitiater initiater, defoamer and solvent composition.
5. according to the arbitrary described photosensitive resin of claim 1-4, it is characterized in that: the ratio of quality and the number of copies of described acrylic copolymeric resin, Photoepolymerizationinitiater initiater, defoamer and solvent is 10-40: 0.2-10: 0.1-2: 50-90, preferred 10-30: 0.5-5: 0.5-2: 60-90, more preferably 20-30: 2-4: 1-2: 60-80.
6. according to the arbitrary described photosensitive resin of claim 1-5, it is characterized in that: described acrylic copolymeric resin is to be got by copolymerization behind unsaturated carboxylic acid, comonomer and the organic solvent mixing;
Described unsaturated carboxylic acid is selected from least a in acrylic acid, methacrylate, methylene succinic acid, maleic acid and the fumaric acid;
Described comonomer is selected from ethyl acrylate, propyl acrylate, acrylic acid oxo two-2, the 1-ethyl, the trimethylolpropane double methacrylate, pentaerythritol triacrylate, tetramethylol methane tetraacrylate, ethoxylation trihydroxy methyl propyl group triacrylate, the propoxylation trimethylolpropane triacrylate, dipentaerythritol five acrylate contract, dipentaerythritol acrylate contracts, ethyl 2-methacrylate, the 2-propyl methacrylate, 2-methacrylic acid oxo two-2, the 1-ethyl, the two 2-methacrylates of trimethylolpropane, trimethylolpropane tris 2-methacrylate, pentaerythrite three 2-methacrylates, pentaerythrite four 2-methacrylates, ethoxylation trihydroxy methyl propyl group three 2-methacrylates, propoxylation trimethylolpropane tris 2-methacrylate, dipentaerythritol five 2-methacrylates contract, dipentaerythritol six 2-methacrylates contract, the methylene succinic acid ethyl ester, the methylene succinic acid propyl ester, ethyl maleate, in maleic acid propyl ester and fumaric acid ethyl ester and the fumaric acid propyl ester at least two kinds;
Described organic solvent is selected from least a in ethylene glycol monoemethyl ether acetate, propylene glycol monomethyl ether, the only methyl ether acetate of propylene glycol, the only ether acetic acid esters of propylene glycol, diethylene glycol dimethyl ether and the diethylene glycol ethylmethyl ether, at least a in preferred only methyl ether acetate of propylene glycol and the ethylene glycol monoemethyl ether acetate.
7. according to the arbitrary described photosensitive resin of claim 6, it is characterized in that: the mass ratio of described unsaturated carboxylic acid and comonomer is 1: 10-1: 1, preferred 3: 7-4: 6; The quality sum of described unsaturated carboxylic acid and comonomer and the mass ratio of organic solvent are 1: 0.25-1, preferred 1: 0.5-1.
8. according to claim 6 or 7 arbitrary described photosensitive resins, it is characterized in that: in the described copolymerization step, temperature is 50-200 ℃, and preferred 100-150 ℃, the time is 2-10 hour, preferred 4-5 hour.
9. method for preparing the arbitrary described used for plasma display screen photosensitive resin of claim 1-8, comprise the steps: described acrylic copolymeric resin, described Photoepolymerizationinitiater initiater, described defoamer and described solvent mixing are obtained described used for plasma display screen photosensitive resin.
10. the application of the arbitrary described used for plasma display screen photosensitive resin of claim 1-9 in the preparation plasma panel.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107329369A (en) * | 2017-05-19 | 2017-11-07 | 合肥市惠科精密模具有限公司 | A kind of plasma display screen electrode is with high-strength photosensitive developable resin |
| CN107359099A (en) * | 2017-07-12 | 2017-11-17 | 合肥轻风飏电气科技有限责任公司 | A kind of electronic display |
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| CN101196686A (en) * | 2006-12-04 | 2008-06-11 | 旭化成电子材料元件株式会社 | Photosensitive resin composition and use of the same |
| CN101201543A (en) * | 2006-12-15 | 2008-06-18 | 北京化工大学 | A kind of light curing inkjet resist for printed circuit board and preparation method thereof |
| CN101206399A (en) * | 2006-12-14 | 2008-06-25 | 第一毛织株式会社 | Photosensitive resin composition for column spacers for liquid crystal display device, column spacers formed using the composition and display device comprising the column spacers |
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| JPS646014A (en) * | 1987-06-30 | 1989-01-10 | Somar Corp | Curable composition |
| CN101125475A (en) * | 2006-08-15 | 2008-02-20 | 大连路明发光科技股份有限公司 | UV curing luminescent film and manufacturing method thereof |
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| CN101206399A (en) * | 2006-12-14 | 2008-06-25 | 第一毛织株式会社 | Photosensitive resin composition for column spacers for liquid crystal display device, column spacers formed using the composition and display device comprising the column spacers |
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| CN107329369A (en) * | 2017-05-19 | 2017-11-07 | 合肥市惠科精密模具有限公司 | A kind of plasma display screen electrode is with high-strength photosensitive developable resin |
| CN107359099A (en) * | 2017-07-12 | 2017-11-17 | 合肥轻风飏电气科技有限责任公司 | A kind of electronic display |
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