KR102506282B1 - Dipole particle suspension containing liquid dispersion stabilizer, light transmission controllable film using the same and preparation method thereof - Google Patents
Dipole particle suspension containing liquid dispersion stabilizer, light transmission controllable film using the same and preparation method thereof Download PDFInfo
- Publication number
- KR102506282B1 KR102506282B1 KR1020220025200A KR20220025200A KR102506282B1 KR 102506282 B1 KR102506282 B1 KR 102506282B1 KR 1020220025200 A KR1020220025200 A KR 1020220025200A KR 20220025200 A KR20220025200 A KR 20220025200A KR 102506282 B1 KR102506282 B1 KR 102506282B1
- Authority
- KR
- South Korea
- Prior art keywords
- poly
- phthalate
- oligomer
- particle suspension
- formula
- Prior art date
Links
- 239000002245 particle Substances 0.000 title claims abstract description 84
- 239000000725 suspension Substances 0.000 title claims abstract description 68
- 239000006185 dispersion Substances 0.000 title claims abstract description 45
- 239000003381 stabilizer Substances 0.000 title claims abstract description 45
- 239000007788 liquid Substances 0.000 title claims abstract description 31
- 230000005540 biological transmission Effects 0.000 title description 2
- 238000002360 preparation method Methods 0.000 title 1
- 239000002952 polymeric resin Substances 0.000 claims abstract description 37
- 229920003002 synthetic resin Polymers 0.000 claims abstract description 33
- 238000002834 transmittance Methods 0.000 claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- -1 2-ethylhexyl Chemical group 0.000 claims description 85
- MLFHJEHSLIIPHL-UHFFFAOYSA-N isoamyl acetate Chemical compound CC(C)CCOC(C)=O MLFHJEHSLIIPHL-UHFFFAOYSA-N 0.000 claims description 32
- 238000002156 mixing Methods 0.000 claims description 15
- 229920001223 polyethylene glycol Polymers 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 12
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000005191 phase separation Methods 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 8
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 claims description 8
- 229920000728 polyester Polymers 0.000 claims description 8
- 239000004593 Epoxy Substances 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 125000005395 methacrylic acid group Chemical group 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 229920001451 polypropylene glycol Polymers 0.000 claims description 7
- IRIAEXORFWYRCZ-UHFFFAOYSA-N Butylbenzyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCC1=CC=CC=C1 IRIAEXORFWYRCZ-UHFFFAOYSA-N 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 125000004386 diacrylate group Chemical group 0.000 claims description 6
- 230000035699 permeability Effects 0.000 claims description 6
- 239000004014 plasticizer Substances 0.000 claims description 6
- 229920006324 polyoxymethylene Polymers 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- ZVFDTKUVRCTHQE-UHFFFAOYSA-N Diisodecyl phthalate Chemical compound CC(C)CCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC(C)C ZVFDTKUVRCTHQE-UHFFFAOYSA-N 0.000 claims description 5
- 239000004734 Polyphenylene sulfide Substances 0.000 claims description 5
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical class OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 5
- 229920001281 polyalkylene Polymers 0.000 claims description 5
- 230000000379 polymerizing effect Effects 0.000 claims description 5
- 229920000069 polyphenylene sulfide Polymers 0.000 claims description 5
- 230000003381 solubilizing effect Effects 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 229920000298 Cellophane Polymers 0.000 claims description 4
- 239000004803 Di-2ethylhexylphthalate Substances 0.000 claims description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 claims description 4
- 238000004873 anchoring Methods 0.000 claims description 4
- ZDWGXBPVPXVXMQ-UHFFFAOYSA-N bis(2-ethylhexyl) nonanedioate Chemical compound CCCCC(CC)COC(=O)CCCCCCCC(=O)OCC(CC)CCCC ZDWGXBPVPXVXMQ-UHFFFAOYSA-N 0.000 claims description 4
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical group CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 4
- VJHINFRRDQUWOJ-UHFFFAOYSA-N dioctyl sebacate Chemical compound CCCCC(CC)COC(=O)CCCCCCCCC(=O)OCC(CC)CCCC VJHINFRRDQUWOJ-UHFFFAOYSA-N 0.000 claims description 4
- JZMPIUODFXBXSC-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)C=C.CCOC(N)=O JZMPIUODFXBXSC-UHFFFAOYSA-N 0.000 claims description 4
- 229920001483 poly(ethyl methacrylate) polymer Polymers 0.000 claims description 4
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 4
- 229920002492 poly(sulfone) Polymers 0.000 claims description 4
- 229920000120 polyethyl acrylate Polymers 0.000 claims description 4
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 4
- 239000011118 polyvinyl acetate Substances 0.000 claims description 4
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 4
- 235000012424 soybean oil Nutrition 0.000 claims description 4
- 239000003549 soybean oil Substances 0.000 claims description 4
- POYODSZSSBWJPD-UHFFFAOYSA-N 2-methylprop-2-enoyloxy 2-methylprop-2-eneperoxoate Chemical compound CC(=C)C(=O)OOOC(=O)C(C)=C POYODSZSSBWJPD-UHFFFAOYSA-N 0.000 claims description 3
- 229920002284 Cellulose triacetate Polymers 0.000 claims description 3
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 3
- 239000004677 Nylon Substances 0.000 claims description 3
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- 229920002319 Poly(methyl acrylate) Polymers 0.000 claims description 3
- 229930182556 Polyacetal Natural products 0.000 claims description 3
- 239000004642 Polyimide Substances 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical class OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 3
- KRADHMIOFJQKEZ-UHFFFAOYSA-N Tri-2-ethylhexyl trimellitate Chemical compound CCCCC(CC)COC(=O)C1=CC=C(C(=O)OCC(CC)CCCC)C(C(=O)OCC(CC)CCCC)=C1 KRADHMIOFJQKEZ-UHFFFAOYSA-N 0.000 claims description 3
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 claims description 3
- 125000002947 alkylene group Chemical group 0.000 claims description 3
- SAOKZLXYCUGLFA-UHFFFAOYSA-N bis(2-ethylhexyl) adipate Chemical compound CCCCC(CC)COC(=O)CCCCC(=O)OCC(CC)CCCC SAOKZLXYCUGLFA-UHFFFAOYSA-N 0.000 claims description 3
- RKELNIPLHQEBJO-UHFFFAOYSA-N bis(5-methylhexyl) benzene-1,2-dicarboxylate Chemical compound CC(C)CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCC(C)C RKELNIPLHQEBJO-UHFFFAOYSA-N 0.000 claims description 3
- 229920002301 cellulose acetate Polymers 0.000 claims description 3
- PUFGCEQWYLJYNJ-UHFFFAOYSA-N didodecyl benzene-1,2-dicarboxylate Chemical compound CCCCCCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCCCCCC PUFGCEQWYLJYNJ-UHFFFAOYSA-N 0.000 claims description 3
- HBGGXOJOCNVPFY-UHFFFAOYSA-N diisononyl phthalate Chemical compound CC(C)CCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCC(C)C HBGGXOJOCNVPFY-UHFFFAOYSA-N 0.000 claims description 3
- QQVHEQUEHCEAKS-UHFFFAOYSA-N diundecyl benzene-1,2-dicarboxylate Chemical compound CCCCCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCCCCC QQVHEQUEHCEAKS-UHFFFAOYSA-N 0.000 claims description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 3
- MHCLJIVVJQQNKQ-UHFFFAOYSA-N ethyl carbamate;2-methylprop-2-enoic acid Chemical compound CCOC(N)=O.CC(=C)C(O)=O MHCLJIVVJQQNKQ-UHFFFAOYSA-N 0.000 claims description 3
- MKVYSRNJLWTVIK-UHFFFAOYSA-N ethyl carbamate;2-methylprop-2-enoic acid Chemical compound CCOC(N)=O.CC(=C)C(O)=O.CC(=C)C(O)=O MKVYSRNJLWTVIK-UHFFFAOYSA-N 0.000 claims description 3
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 claims description 3
- 239000005038 ethylene vinyl acetate Substances 0.000 claims description 3
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical class OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 3
- 229920001778 nylon Polymers 0.000 claims description 3
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 3
- 229920001707 polybutylene terephthalate Polymers 0.000 claims description 3
- 239000004417 polycarbonate Substances 0.000 claims description 3
- 229920000515 polycarbonate Polymers 0.000 claims description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 3
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 3
- 229920001721 polyimide Polymers 0.000 claims description 3
- 229920000098 polyolefin Polymers 0.000 claims description 3
- 229920001955 polyphenylene ether Polymers 0.000 claims description 3
- 229920005650 polypropylene glycol diacrylate Polymers 0.000 claims description 3
- 229920005651 polypropylene glycol dimethacrylate Polymers 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 3
- 239000004800 polyvinyl chloride Substances 0.000 claims description 3
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- HHYYEQUQGLGKGP-UHFFFAOYSA-N CC(=C)C(O)=O.CC(=C)C(O)=O.CC(=C)C(O)=O.CC(=C)C(O)=O Chemical compound CC(=C)C(O)=O.CC(=C)C(O)=O.CC(=C)C(O)=O.CC(=C)C(O)=O HHYYEQUQGLGKGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- YKGYQYOQRGPFTO-UHFFFAOYSA-N bis(8-methylnonyl) hexanedioate Chemical compound CC(C)CCCCCCCOC(=O)CCCCC(=O)OCCCCCCCC(C)C YKGYQYOQRGPFTO-UHFFFAOYSA-N 0.000 claims description 2
- YCZJVRCZIPDYHH-UHFFFAOYSA-N ditridecyl benzene-1,2-dicarboxylate Chemical compound CCCCCCCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCCCCCCC YCZJVRCZIPDYHH-UHFFFAOYSA-N 0.000 claims description 2
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Chemical compound CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims 2
- GPZYYYGYCRFPBU-UHFFFAOYSA-N 6-Hydroxyflavone Chemical compound C=1C(=O)C2=CC(O)=CC=C2OC=1C1=CC=CC=C1 GPZYYYGYCRFPBU-UHFFFAOYSA-N 0.000 claims 1
- 229940067597 azelate Drugs 0.000 claims 1
- OPONDODNFLYDGJ-UHFFFAOYSA-N bis(6-methylheptyl) benzene-1,2-dicarboxylate 3,4-bis(6-methylheptyl)phthalic acid Chemical compound CC(C)CCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCC(C)C.CC(C)CCCCCC1=CC=C(C(O)=O)C(C(O)=O)=C1CCCCCC(C)C OPONDODNFLYDGJ-UHFFFAOYSA-N 0.000 claims 1
- FAXYTNFFGSIFBD-UHFFFAOYSA-N bis(8-methylnonyl) 7-oxabicyclo[4.1.0]hept-5-ene-3,4-dicarboxylate Chemical compound CC(C)CCCCCCCOC(=O)C1C(C(=O)OCCCCCCCC(C)C)CC2OC2=C1 FAXYTNFFGSIFBD-UHFFFAOYSA-N 0.000 claims 1
- VCJSWCRTDMLPLP-UHFFFAOYSA-N bis(8-methylnonyl) benzene-1,2-dicarboxylate 3,4-bis(8-methylnonyl)phthalic acid Chemical compound C(CCCCCCC(C)C)C=1C(=C(C(C(=O)O)=CC1)C(=O)O)CCCCCCCC(C)C.C(C=1C(C(=O)OCCCCCCCC(C)C)=CC=CC1)(=O)OCCCCCCCC(C)C VCJSWCRTDMLPLP-UHFFFAOYSA-N 0.000 claims 1
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Chemical compound CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims 1
- 125000005641 methacryl group Chemical group 0.000 claims 1
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 claims 1
- JQCXWCOOWVGKMT-UHFFFAOYSA-N phthalic acid diheptyl ester Natural products CCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCC JQCXWCOOWVGKMT-UHFFFAOYSA-N 0.000 claims 1
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical class OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims 1
- 230000005684 electric field Effects 0.000 abstract description 8
- 239000004815 dispersion polymer Substances 0.000 abstract description 3
- 238000004090 dissolution Methods 0.000 abstract description 2
- 230000010287 polarization Effects 0.000 abstract 3
- 230000036632 reaction speed Effects 0.000 abstract 1
- 229920000642 polymer Polymers 0.000 description 11
- 239000011159 matrix material Substances 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 4
- 229920006112 polar polymer Polymers 0.000 description 4
- 230000005653 Brownian motion process Effects 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 238000005537 brownian motion Methods 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- GCSJLQSCSDMKTP-UHFFFAOYSA-N ethenyl(trimethyl)silane Chemical compound C[Si](C)(C)C=C GCSJLQSCSDMKTP-UHFFFAOYSA-N 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 description 2
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 description 2
- IJFPVINAQGWBRJ-UHFFFAOYSA-N Diisooctyl phthalate Chemical compound CC(C)CCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCC(C)C IJFPVINAQGWBRJ-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- AYWLCKHHUFBVGJ-UHFFFAOYSA-N bis(7-methyloctyl) hexanedioate Chemical compound CC(C)CCCCCCOC(=O)CCCCC(=O)OCCCCCCC(C)C AYWLCKHHUFBVGJ-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 description 2
- HFTNNOZFRQLFQB-UHFFFAOYSA-N ethenoxy(trimethyl)silane Chemical compound C[Si](C)(C)OC=C HFTNNOZFRQLFQB-UHFFFAOYSA-N 0.000 description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000006194 liquid suspension Substances 0.000 description 2
- BSCJIBOZTKGXQP-UHFFFAOYSA-N n-(2-hydroxyethyl)-2-methylprop-2-enamide Chemical compound CC(=C)C(=O)NCCO BSCJIBOZTKGXQP-UHFFFAOYSA-N 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 238000000844 transformation Methods 0.000 description 2
- HYWCXWRMUZYRPH-UHFFFAOYSA-N trimethyl(prop-2-enyl)silane Chemical compound C[Si](C)(C)CC=C HYWCXWRMUZYRPH-UHFFFAOYSA-N 0.000 description 2
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2,2'-azo-bis-isobutyronitrile Substances N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 1
- BKMAEERFCKIKJR-UHFFFAOYSA-N 2-tridecoxycarbonylbenzoic acid Chemical compound CCCCCCCCCCCCCOC(=O)C1=CC=CC=C1C(O)=O BKMAEERFCKIKJR-UHFFFAOYSA-N 0.000 description 1
- ALKCLFLTXBBMMP-UHFFFAOYSA-N 3,7-dimethylocta-1,6-dien-3-yl hexanoate Chemical compound CCCCCC(=O)OC(C)(C=C)CCC=C(C)C ALKCLFLTXBBMMP-UHFFFAOYSA-N 0.000 description 1
- LLQHSBBZNDXTIV-UHFFFAOYSA-N 6-[5-[[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]methyl]-4,5-dihydro-1,2-oxazol-3-yl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC1CC(=NO1)C1=CC2=C(NC(O2)=O)C=C1 LLQHSBBZNDXTIV-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 230000004931 aggregating effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- PGJCWZHUWGVRSQ-UHFFFAOYSA-N dioctyl benzene-1,2-dicarboxylate 3,4-dioctylphthalic acid Chemical compound C(CCCCCCC)C=1C(=C(C(C(=O)O)=CC1)C(=O)O)CCCCCCCC.C(C=1C(C(=O)OCCCCCCCC)=CC=CC1)(=O)OCCCCCCCC PGJCWZHUWGVRSQ-UHFFFAOYSA-N 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- IGBZOHMCHDADGY-UHFFFAOYSA-N ethenyl 2-ethylhexanoate Chemical compound CCCCC(CC)C(=O)OC=C IGBZOHMCHDADGY-UHFFFAOYSA-N 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000005251 gamma ray Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920006389 polyphenyl polymer Polymers 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/17—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on variable-absorption elements not provided for in groups G02F1/015 - G02F1/169
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Abstract
Description
본 발명은 액상의 분산안정제를 포함하는 분극입자 현탁액, 이를 이용한 투과도 가변 필름 및 그 제조방법에 관한 것으로, 분극입자를 안정하게 분산시켜주는 액상의 분산안정제가 현탁액의 매체 역할을 동시에 수행할 수 있고, 이 액상의 분산안정제가 고분자 수지와 혼합되지 않으면서 현탁액의 액적 형태로 고분자 수지 내에 분산되어 있는 투과도 가변 필름 및 그 제조 방법에 관한 것이다.The present invention relates to a polarized particle suspension containing a liquid dispersion stabilizer, a variable permeability film using the same, and a method for manufacturing the same. , This liquid dispersion stabilizer is dispersed in the polymer resin in the form of droplets of suspension without being mixed with the polymer resin, and relates to a variable transmittance film and a manufacturing method thereof.
분극입자 현탁액을 이용한 투과도 가변 기술은 입자가 전기장 방향에 따라 배열함으로써 가시광선 영역의 투과율을 변화시켜 줌으로써 투과하는 빛의 차단 정도를 조절할 수 있는 특징이 있다. 그런데 액체의 경우에는 건축물 창호, 차량용 창호 등에 적용을 위해 대형화 할 경우, 중력이나 외부의 압력에 의해 부풀거나 눌리게 되어 빛 투과량이 국소적으로 일정하지 않고 불균질한 상태가 될 수 있다. 이를 개선하기 위하여 분극입자 현탁액을 액적 형태로 포함하는 필름을 개발하기 위한 노력이 경주되어 왔으며, 대한민국 특허출원 제 10-1992-0011659호(광변광 현탁액이 고분자 수지 내에 분산된 투과도 가변창용 필름 및 그 제조방법) 및 대한민국 특허출원 제10-1993-0702534호(캡슐화된 액체 현탁액을 함유한 필름, 이 필름을 포함환 광밸브 및 상기 필름의 제조 방법)를 통하여 대형화를 위한 분극입자 현탁액을 포함하는 필름화 기술이 개발되기 시작하였다. 전술한 특허에서는 현탁액과 고분자 수지 용액을 혼합하고 코팅한 후 용매 증발에 의한 상분리 방법에 의해 현탁액이 고분자 수지 내에 액적 형태로 분리되어 고형화된 필름 형태로 만들어지게 된다. 반면, 후술한 특허에서는 현탁액과 가교반응 가능한 중합체 기질을 에멀젼 형태로 혼합한 후, 필름 형태로 코팅한 다음 가교 반응을 시켜줌으로써 필름을 고형화하여 최종적으로 투과도 가변 필름을 형성하는 방법이다.Transmittance variable technology using a polarized particle suspension is characterized in that the degree of blocking of transmitted light can be adjusted by changing the transmittance in the visible ray region by arranging the particles according to the direction of the electric field. However, in the case of liquid, when large-sized for application to building windows, vehicle windows, etc., it is inflated or pressed by gravity or external pressure, so that the amount of light transmission is not uniform locally and may become inhomogeneous. In order to improve this, efforts have been made to develop a film containing a suspension of polarized particles in the form of droplets, and Korean Patent Application No. 10-1992-0011659 (a film for variable transmittance window in which a light-changing suspension is dispersed in a polymer resin and its Manufacturing method) and Korean Patent Application No. 10-1993-0702534 (Film Containing Encapsulated Liquid Suspension, Ring Light Valve Including the Film and Manufacturing Method of the Film) Fire technology began to develop. In the aforementioned patent, the suspension and the polymer resin solution are mixed and coated, and then the suspension is separated in the form of droplets in the polymer resin by a phase separation method by solvent evaporation to form a solidified film. On the other hand, in the patents described later, a suspension and a crosslinkable polymer matrix are mixed in an emulsion form, coated in a film form, and then solidified by a crosslinking reaction to finally form a variable permeability film.
한편, 분극입자는 음으로 하전된 I3 - 혹은 I5 -를 포함하는, 1 마이크로 이하 크기이며, 막대 형태인 형상 이방성 입자로써 입자들끼리 서로 응집하는 특성이 있기 때문에 이를 현탁매 내에 안정적으로 분산시키기 위해서는 분산안정제가 반드시 요구된다. 이러한 분산안정제는 분극입자에 결합하는 결합부(anchoring group)와 현탁매에 용해되는 용해부(solubilizing 혹은 stabilizing group)를 포함하고 있어서 분극입자에 견고하게 결합하고 현탁매 내에 용해되어 분극입자가 서로 응집되지 않고 안정적으로 부유되도록 도와주는 역할을 한다. 또한, 필름화하는 경우에는 현탁매와 마찬가지로 분산안정제의 용해부는 필름의 기질인 고분자 수지와는 상용성(compatibility) 혹은 혼합성(miscibility)이 낮아서 서로 쉽게 혼합되지 않아야 한다. 이러한 특성을 위하여 기존의 방법에서는 분자량이 100,000 이상으로 큰 고분자 분산안정제를 사용하였으나, 이 경우 현탁매에 용해하기 쉽지 않으며, 용해된 경우에도 점도가 높아지므로 전기에 의해 입자가 회전하거나 복귀하는 반응속도가 느려지는 단점이 있었다.On the other hand, polarized particles are rod-shaped shape anisotropic particles containing negatively charged I 3 - or I 5 - , with a size of less than 1 micron, and are stably dispersed in a suspension medium because the particles have a property of aggregating with each other. To achieve this, a dispersion stabilizer is required. The dispersion stabilizer includes an anchoring group that binds to the polarized particles and a solubilizing or stabilizing group that dissolves in the suspension medium, so that it firmly binds to the polarized particles and dissolves in the suspension medium so that the polarized particles aggregate with each other. It plays a role in helping to float stably without falling. In addition, in the case of film formation, like the suspension medium, the dissolving part of the dispersion stabilizer should not be easily mixed with the polymer resin, which is the substrate of the film, due to low compatibility or miscibility. For this characteristic, in the existing method, a high molecular weight dispersion stabilizer of 100,000 or more was used, but in this case, it is not easy to dissolve in the suspension medium, and even when dissolved, the viscosity is high, so the reaction rate of rotation or return of the particles by electricity had the downside of being slow.
본 발명에서는 이를 해결하기 위하여, 상온에서 액체이며, 분극입자에 대한 결합부와 함께 용해부를 갖는 액상의 분산 안정제를 사용함으로써, 별도의 현탁매를 사용하지 않거나 쉽게 용해되고, 반응속도도 개선된 분산안정제를 사용한 투과도 가변 필름 및 그 제조방법을 제공하고자 한다.In the present invention, in order to solve this problem, by using a liquid dispersion stabilizer that is liquid at room temperature and has a dissolving portion as well as a bonding portion for polarized particles, a dispersion that does not use a separate suspension medium or is easily dissolved and has improved reaction rate. It is intended to provide a variable transmittance film using a stabilizer and a manufacturing method thereof.
따라서 본 발명은 상기와 같은 문제점을 감안하여 안출된 것으로, 본 발명의 목적은 종래 고분자 분산안정제를 사용할 경우 발생할 수 있는 용해의 어려움 및 고점도의 문제를 해결하기 위하여 결합부(anchoring group)와 용해부(solubilizing group)로 이루어진 액상의 분산안정제를 포함하는 분극입자 현탁액을 제공하는 것이다.Therefore, the present invention has been made in view of the above problems, and an object of the present invention is to solve the problem of difficulty in dissolving and high viscosity that may occur when using a conventional polymer dispersion stabilizer. It is to provide a polarized particle suspension containing a liquid dispersion stabilizer composed of a solubilizing group.
또한, 본 발명의 또 다른 목적은 상기 분극입자 현탁액을 이용함으로써 분극입자 현탁액의 액적을 형성하게 되며, 전계 인가에 따라 투과도를 조절할 수 있는 투과도 가변 필름 및 그 제조 방법을 제공하는 것이다.In addition, another object of the present invention is to provide a variable transmittance film and a method for manufacturing the same, wherein droplets of the polarized particle suspension are formed by using the polarized particle suspension and the transmittance can be adjusted according to the application of an electric field.
상기와 같은 목적을 달성하기 위한 본 발명은, 결합부(anchoring group) 및 용해부(solubilizing group)로 이루어진 액상의 분산안정제를 포함하는 분극입자 현탁액을 제공한다.To achieve the above object, the present invention provides a polarized particle suspension containing a liquid dispersion stabilizer composed of an anchoring group and a solubilizing group.
상기 결합부는 하기 [화학식 1] 내지 [화학식 4]에서 선택된 어느 하나의 것으로 표시되는 화합물인 것을 특징으로 한다.The coupling part is characterized in that a compound represented by any one selected from the following [Formula 1] to [Formula 4].
[화학식 1] [화학식 2][Formula 1] [Formula 2]
[화학식 3] [화학식 4][Formula 3] [Formula 4]
(상기 화학식 1 내지 4에서, X는 N, O, F 또는 S이고, m은 2 내지 20 사이의 정수이며, n은 1 내지 5 사이의 정수이다)(In Formulas 1 to 4, X is N, O, F or S, m is an integer between 2 and 20, and n is an integer between 1 and 5)
상기 용해부는 하기 [화학식 5] 내지 [화학식 9]에서 선택된 어느 하나의 것으로 표시되는 화합물인 것을 특징으로 한다.The dissolving part is characterized in that the compound represented by any one selected from the following [Formula 5] to [Formula 9].
[화학식 5] [화학식 6][Formula 5] [Formula 6]
[화학식 7] [화학식 8][Formula 7] [Formula 8]
[화학식 9][Formula 9]
(상기 화학식 5 내지 9에서, o는 30 내지 200 사이의 정수이며, p는 4 내지 15 사이의 정수이다)(In Chemical Formulas 5 to 9, o is an integer between 30 and 200, and p is an integer between 4 and 15)
상기 용해부는 비닐트리메틸실란(vinyltrimethylsilane), 알릴트리메틸실란(allyltrimethylsilane), 비닐옥시트리메틸실란(vinyloxytrimethylsilane), 트리메톡시비닐실란(trimethoxyvinylsilane) 및 트리에톡시비닐실란(triethoxyvinylsilane)으로 이루어진 군으로부터 선택된 1종 이상의 것을 특징으로 한다.The dissolving part is one or more selected from the group consisting of vinyltrimethylsilane, allyltrimethylsilane, vinyloxytrimethylsilane, trimethoxyvinylsilane and triethoxyvinylsilane. characterized by
상기 분극입자는 그 크기가 300 nm 내지 1 ㎛인 것을 특징으로 한다.The polarized particles are characterized in that the size is 300 nm to 1 ㎛.
상기 분극입자 현탁액은 고비점 가소제를 더욱 포함하는 것을 특징으로 한다.The polarized particle suspension is characterized in that it further contains a high boiling point plasticizer.
상기 고비점 가소제는 디-2-에틸헥실프탈레이트(di-2-ethylhexyl phthalate), 디이소옥틸프탈레이트(di-isooctyl phthalate), 디카프릴프탈레이트(di-capryl phthalate), 디-n-옥틸프탈레이트(di-n-octyl phthalate), 부틸-벤질프탈레이트(butyl-benzyl phthalate), 디이소헵틸프탈레이트(di-isoheptyl phthalate), 디이소노닐프탈레이트(di-isononyl phthalate), 디이소데실프탈레이트(di-isodecyl phthalate), 디트리데실프탈레이트(di-tridecyl phthalate), 디운데실프탈레이트(di-undecyl phthalate), 디도데실프탈레이트(di-dodecyl phthalate), 디이소데실프탈레이트(di-isododecyl phthalate) 또는 이들의 이소프탈레이트 또는 테레프탈레이트, 또는 트리-2-에틸헥실트리멜리테이트(tri-2-ethylhexyl trimellitate), 디-2-에틸헥실아디페이트(di-2-ethylhexyl adipate), 디이소노닐아디페이트(di-isononyl adipate), 디이소데실아디페이트(di-isodecyl adipate), 디-2-에틸헥실세바케이트(di-2-ethylhexyl sebacate), 디-2-에틸헥실아젤레이트(di-2-ethylhexyl azelate), 에폭시화소이빈오일(epoxidized soy bean oil), 2-에틸헥실에폭시탈레이트(2-ethylhexyl epoxy tallate), 디이소데실테트라히드로-4,5-에폭시프탈레이트(di-isodecyl tetrahydro-4,5-epoxy phthalate), 폴리알킬렌아디페이트(poly(akylene adipates)), 폴리알킬렌세바케이트(poly(alkylene sebacates)) 및 폴리알킬렌아젤레이트(poly(alkylene azelates))로 이루어진 군으로부터 선택된 1종 이상의 것을 특징으로 한다.The high boiling point plasticizer is di-2-ethylhexyl phthalate, di-isooctyl phthalate, di-capryl phthalate, di-n-octyl phthalate (di -n-octyl phthalate), butyl-benzyl phthalate, di-isoheptyl phthalate, di-isononyl phthalate, di-isodecyl phthalate , di-tridecyl phthalate, di-undecyl phthalate, di-dodecyl phthalate, di-isodecyl phthalate, or isophthalates or terephthalates thereof phthalate, or tri-2-ethylhexyl trimellitate, di-2-ethylhexyl adipate, di-isononyl adipate, Di-isodecyl adipate, di-2-ethylhexyl sebacate, di-2-ethylhexyl azelate, epoxidized soybean Oil (epoxidized soy bean oil), 2-ethylhexyl epoxy tallate, di-isodecyl tetrahydro-4,5-epoxy phthalate, poly It is characterized by at least one selected from the group consisting of poly(akylene adipates), poly(alkylene sebacates), and poly(alkylene azelates).
또한, 본 발명은 상기 분극입자 현탁액이 액적 형태로 고분자 수지 내에 분산되어 있는 투과도 가변 필름을 제공한다.In addition, the present invention provides a variable transmittance film in which the polarized particle suspension is dispersed in a polymer resin in the form of droplets.
상기 고분자 수지는 폴리메틸메타크릴레이트(poly(methyl methacrylate)), 폴리에틸메타크릴레이트(poly(ethyl methacrylate)), 폴리메틸아크릴레이트(poly(methyl acrylate)), 폴리에틸아크릴레이트(poly(ethyl acrylate)), 폴리비닐아세테이트(poly(vinyl acetate)), 폴리우레탄(polyurethane), 폴리에틸렌-비닐아세테이트(poly(ethylene-vinyl acetate)), 나일론(Nylon), 폴리이미드(polyimides), 폴리술폰(polysulfones), 폴리에테르술폰(poly(ether sulfones)), 폴리에틸렌테레프탈레이트(polyethylene terephthalate), 폴리부틸렌테레프탈레이트(polybutylene terephthalate), 폴리비닐클로라이드(polyvinyl chloride), 셀룰로오스아세테이트(cellulose acetate), 셀로판(cellophane), 트리아세틸셀룰로오스(triacetyl cellulose), 폴리카보네이트(polycarbonate), 폴리아세탈 수지(polyacetal resin), 폴리페닐렌에테르(polyphenylene ether), 폴리옥시메틸렌(polyoxymethylene), 폴리옥시에틸렌(polyoxyethylene) 및 폴리페닐렌술피드(polyphenylene sulfide)로 이루어진 군으로부터 선택된 1종 이상의 것을 특징으로 한다.The polymer resin is poly(methyl methacrylate), poly(ethyl methacrylate), poly(methyl acrylate), poly(ethyl acrylate), poly(vinyl acetate), polyurethane, poly(ethylene-vinyl acetate), nylon, polyimides, polysulfones ), poly(ether sulfones), polyethylene terephthalate, polybutylene terephthalate, polyvinyl chloride, cellulose acetate, cellophane , triacetyl cellulose, polycarbonate, polyacetal resin, polyphenylene ether, polyoxymethylene, polyoxyethylene and polyphenylene sulfide It is characterized by at least one selected from the group consisting of (polyphenylene sulfide).
또한, 본 발명은 (I) 이소펜틸아세테이트에 분산된 분극입자를 액상의 분산안정제와 고르게 혼합한 후, 이소펜틸아세테이트를 건조하여 분극입자 현탁액을 형성하는 단계; (II) 고분자 수지를 용매에 용해하여 고분자 수지 용액을 얻는 단계; (III) 상기 분극입자 현탁액과 고분자 수지 용액을 혼합하는 단계; 및 (IV) 상기 혼합용액을 투명전도막이 코팅된 기판 위에 코팅하고 용매를 건조함으로써 상분리에 의해 분극입자 현탁액이 액적으로 분산된 고형의 필름을 형성하는 단계;를 포함하는 투과도 가변 필름의 제조방법을 제공한다.In addition, the present invention comprises the steps of (I) uniformly mixing the polarized particles dispersed in isopentyl acetate with a liquid dispersion stabilizer, and then drying the isopentyl acetate to form a polarized particle suspension; (II) dissolving the polymer resin in a solvent to obtain a polymer resin solution; (III) mixing the polarized particle suspension with a polymer resin solution; And (IV) coating the mixed solution on a transparent conductive film-coated substrate and drying the solvent to form a solid film in which the polarized particle suspension is dispersed in droplets by phase separation; to provide.
또한, 본 발명은 (i) 이소펜틸아세테이트에 분산된 분극입자를 액상의 분산안정제와 고르게 혼합한후, 이소펜틸아세테이트를 건조하여 분극입자 현탁액을 형성하는 단계; (ii) 상기 분극입자 현탁액과 반응성 올리고머를 혼합하는 단계; 및 (iii) 상기 혼합용액을 투명전도막이 코팅된 기판 위에 코팅하고 반응성 올리고머를중합함으로써 상분리에 의해 분극입자 현탁액이 액적으로 분산된 고형의 필름을 형성하는 단계;를 포함하는 투과도 가변 필름의 제조방법을 제공한다.In addition, the present invention includes the steps of (i) uniformly mixing the polarized particles dispersed in isopentyl acetate with a liquid dispersion stabilizer, and then drying the isopentyl acetate to form a polarized particle suspension; (ii) mixing the polarized particle suspension with a reactive oligomer; and (iii) forming a solid film in which the polarized particle suspension is dispersed in liquid droplets by phase separation by coating the mixed solution on a substrate coated with a transparent conductive film and polymerizing a reactive oligomer. provides
상기 반응성 올리고머는 실란 가교성 폴리에틸렌(silane crosslinkable polyolefins), 가교성 우레탄 아크릴레이트 올리고머(crosslinkable urethane acrylate oligomers), 우레탄 메타크릴레이트 올리고머(urethane methacrylate oligomer), 우레탄 디아크릴레이트 올리고머(urethane diacrylate oligomer), 우레탄 디메타크릴레이트 올리고머(urethane dimethacrylate oligomer), 에폭시 메타크릴레이트 올리고머(epoxy methacrylate oligomer), 에폭시 아크릴레이트 올리고머(epoxy acrylate oligomer), 아크릴화 아크릴 올리고머(acrylated acrylic oligomer), 아크릴화 메타크릴 올리고머(acrylated methacrylic oligomer), 메타크릴화 아크릴 올리고머(methacrylated acrylic oligomer), 메타크릴화 메타크릴 올리고머(methacrylated methacrylic oligomer), 폴리에스터 아크릴레이트 올리고머(polyester acrylate oligomer), 폴리에스터 메타크릴레이트 올리고머(polyester methacrylated oligomer), 폴리에틸렌글리콜 아크릴레이트(poly(ethylene glycol) acrylate), 폴리에틸렌글리콜 디아크릴레이트(poly(ethylene glycol) diacrylate), 폴리에틸렌글리콜 메타크릴레이트(poly(ethylene glycol) methacrylate), 폴리에틸렌글리콜 디메타크릴레이트(poly(ethylene glycol) dimethacrylate), 폴리프로필렌글리콜 아크릴레이트(poly(propylene glycol)acrylate), 폴리프로필렌글리콜 디아크릴레이트(poly(propylene glycol) diacrylate), 폴리프로필렌글리콜 메타크릴레이트(poly(propylene glycol) methacrylate), 폴리프로필렌글리콜 디메타크릴레이트(poly(propylene glycol) dimethacrylate), 폴리카보네이티드디올 디아크릴레이트(polycarbonatediol diacrylate) 및 폴리카보네이티드디올 디메타크릴레이트(polycarbonatediol dimethacrylate)로 이루어진 군으로부터 선택된 1종 이상의 것을 특징으로 한다.The reactive oligomer is silane crosslinkable polyolefins, crosslinkable urethane acrylate oligomers, urethane methacrylate oligomer, urethane diacrylate oligomer, urethane Dimethacrylate oligomer, epoxy methacrylate oligomer, epoxy acrylate oligomer, acrylated acrylic oligomer, acrylated methacrylic oligomer , methacrylated acrylic oligomer, methacrylated methacrylic oligomer, polyester acrylate oligomer, polyester methacrylated oligomer, polyethylene glycol acrylic Poly(ethylene glycol) acrylate, Poly(ethylene glycol) diacrylate, Poly(ethylene glycol) methacrylate, Poly(ethylene glycol) dimethacrylate dimethacrylate), poly(propylene glycol)acrylate, poly(propylene glycol) diacrylate), polypropylene glycol methacrylate (poly(pr) composed of opylene glycol) methacrylate), poly(propylene glycol) dimethacrylate, polycarbonatediol diacrylate and polycarbonatediol dimethacrylate. It is characterized by at least one selected from the group.
본 발명에 의하면, 종래 고분자 분산안정제를 사용할 경우 발생할 수 있는 용해의 어려움 및 고점도의 문제를 해결한 분극입자 현탁액을 이용함으로써 분극입자 현탁액의 액적을 형성하게 되며, 전계 인가에 따라 투과도를 조절할 수 있는 투과도 가변 필름을 제공할 수 있으며, 제조공정을 좀 더 단순화할 수 있을 뿐만 아니라 현탁액의 점도를 낮춰 줌으로써 반응속도를 개선할 수 있다.According to the present invention, by using a polarized particle suspension that solves the problems of dissolution difficulty and high viscosity that may occur when using a conventional polymer dispersion stabilizer, droplets of the polarized particle suspension are formed, and the transmittance can be adjusted according to the application of an electric field It is possible to provide a variable permeability film, and to further simplify the manufacturing process, as well as improve the reaction rate by lowering the viscosity of the suspension.
본 발명은 다양한 변환을 가할 수 있고 여러 가지 실시 예를 가질 수 있는 바, 특정 실시예들을 도면에 예시하고 상세하게 설명하고자 한다. 그러나, 이는 본 발명을 특정한 실시 형태에 한정하려는 것이 아니며, 분 발명의 사상 및 기술 범위에 포함되는 모든 변환, 균등물 내지 대체물을 포함하는 것으로 이해되어야 한다. 본 발명을 설명함에 있어서 관련된 공지 기술에 대한 구체적인 설명이 본 발명의 요지를 흐릴 수 있다고 판단되는 경우 그 상세한 설명을 생략한다.Since the present invention can apply various transformations and have various embodiments, specific embodiments will be illustrated in the drawings and described in detail. However, it should be understood that this is not intended to limit the present invention to specific embodiments, and includes all transformations, equivalents, and substitutes included in the spirit and technical scope of the present invention. In describing the present invention, if it is determined that a detailed description of related known technologies may obscure the gist of the present invention, the detailed description will be omitted.
본 출원에서 사용한 용어는 단지 특정한 실시예를 설명하기 위하여 사용된 것으로, 본 발명을 한정하려는 의도가 아니다. 분 출원에서, “포함하다” 또는 “가지다” 등의 용어는 명세서상에 기재된 특징, 숫자, 단계, 동작, 구성요소, 부품 또는 이들을 조합한 것이 존재함을 지정하려는 것이지, 하나 또는 그 이상의 다른 특징들이나 숫자, 단계, 동작, 구성요소, 부품 또는 이들을 조합한 것들의 존재 또는 부가 가능성을 미리 배제하지 않는 것으로 이해되어야 한다.Terms used in this application are only used to describe specific embodiments, and are not intended to limit the present invention. In a separate application, terms such as “comprise” or “have” are intended to indicate that there is a feature, number, step, operation, component, part, or combination thereof described in the specification, but one or more other features It should be understood that the presence or addition of numbers, steps, operations, components, parts, or combinations thereof is not precluded.
본 발명에서 극성은 상대적인 극성을 의미하며 마찬가지로 비극성은 상대적인 비극성을 의미한다. 또한 상용성이 낮다는 것은 고분자 물질 및 전분자 물질의 혼합에 있어서 유사한 것이 유사한 것을 녹인다(Like dissolve like)는 기본 개념에 덧붙여, 용해도 파라미터가 크게 차이 나는 경우를 의미한다. Hansen에 의하면 전체적인 용해도 파라미터는 아래와 같은 식에 의해 결정되어지며, 여기서 δ d , δ p , δ h 는 각각 분산력(dispersion force), 극성력(polar force), 수소결합력(hydrogen bonding force)을 의미한다. 따라서 전체적인 용해도 파라미터가 유사하더라도 극성력이나 수소결합력에 의한 용해도 파라미터 수치가 달라지면 용해도가 변하게 된다.In the present invention, polarity means relative polarity, and similarly, non-polarity means relative non-polarity. In addition, low compatibility means a case in which solubility parameters differ greatly in addition to the basic concept of like dissolve like in mixing polymeric substances and whole molecular substances. According to Hansen, the overall solubility parameter is determined by the following equation, where δ d , δ p , and δ h represent the dispersion force, polar force, and hydrogen bonding force, respectively. . Therefore, even if the overall solubility parameters are similar, the solubility changes when the solubility parameter values due to polar forces or hydrogen bonding forces are different.
δ 2 = δ D 2 + δ P 2 + δ H 2 δ 2 = δ D 2 + δ P 2 + δ H 2
위의 용해도 파라미터에서 고분자와 용매, 혹은 고분자와 고분자 사이의 친화성 정도는 각 결합력의 차이로 표시할 수 있으며, Skaarup에 의하면 실험적으로 아래와 같은 식으로 발전시켰다. 여기서 Ra는 용해도파라미터 차이, 하첨자 1은 용매 혹은 고분자, 하첨자 2는 고분자이다. 용해도 파라미터 차이가 감소하면 고분자와 용매 혹은 고분자와 고분자 사이의 친화성이 높다는 것을 의미한다.In the above solubility parameter, the degree of affinity between the polymer and the solvent or between the polymer and the polymer can be expressed as the difference in each binding force, and according to Skaarup, it was experimentally developed as follows. Here, R a is the solubility parameter difference, subscript 1 is the solvent or polymer, and subscript 2 is the polymer. A decrease in the solubility parameter difference means that the affinity between the polymer and the solvent or between the polymer and the polymer is high.
(R a ) 2 = 4(δ D2 δ D1 )2 + (δ P2 δ P1 )2 + (δ H2 δ H1 )2 (R a ) 2 = 4( δ D2 δ D1 ) 2 + ( δ P2 δ P1 ) 2 + ( δ H2 δ H1 ) 2
여기서 Ra는 고분자의 용해도 반경 R0와 비교할 수 있으며, 상대적인 에너지 차이(Relative Energy Difference, RED)로 아래와 같이 표시할 수 있다. RED 값이 0이면 에너지 차이가 없는 것이며, 1보다 작으면 친화성이 좋은 것이며, 그 값이 1이면 경계상태임을 나타내고, 그 값이 1이상이면 친화성이 낮은 상태를 의미한다.Here, R a can be compared with the solubility radius R 0 of the polymer, and can be expressed as the Relative Energy Difference (RED) as follows. If the RED value is 0, there is no energy difference, if it is less than 1, the affinity is good, if the value is 1, it indicates a boundary state, and if the value is 1 or more, it means a state with low affinity.
RED = R a / R 0 RED = R a / R 0
이하 본 발명에 따른 액상의 분산안정제를 포함하는 분극입자 현탁액, 이를 이용한 투과도 가변 필름 및 그 제조방법에 대하여 상세히 설명한다.Hereinafter, a polarized particle suspension containing a liquid dispersion stabilizer according to the present invention, a variable transmittance film using the same, and a manufacturing method thereof will be described in detail.
먼저, 본 발명에서는 결합부(anchoring group) 및 용해부(solubilizing group)로 이루어진 액상의 분산안정제를 포함하는 분극입자 현탁액을 제공한다.First, the present invention provides a polarized particle suspension containing a liquid dispersion stabilizer composed of an anchoring group and a solubilizing group.
상기 결합부는 분극입자와 수소결합에 의해 결합되어 잡아주며, 용해부는 액상의 형태로 분극입자의 브라운 운동을 가능하게 하고, 매트릭스를 구성하는 고분자 수지에 비해 상대적으로 비극성이어서 극성인 고분자 수지에 대하여 분리된 상을 유지하며, 따라서 분극입자가 분산된 액상의 현탁액이 고분자 수지 내에 액적 형태로 분포된다.The coupling part binds and holds the polarized particles by hydrogen bonding, and the dissolving part enables Brownian motion of the polarized particles in the form of a liquid, and is relatively non-polar compared to the polymer resin constituting the matrix, so it is separated from the polar polymer resin. Therefore, the liquid suspension in which the polarized particles are dispersed is distributed in the form of droplets in the polymer resin.
이때, 상기 결합부는 하기 [화학식 1] 내지 [화학식 4]에서 선택된 어느 하나의 것으로 표시되는 화합물일 수 있다.In this case, the bonding unit may be a compound represented by any one selected from [Formula 1] to [Formula 4].
[화학식 1] [화학식 2][Formula 1] [Formula 2]
[화학식 3] [화학식 4][Formula 3] [Formula 4]
(상기 화학식 1 내지 4에서, X는 N, O, F 또는 S이고, m은 2 내지 20 사이의 정수이며, n은 1 내지 5 사이의 정수이다)(In Formulas 1 to 4, X is N, O, F or S, m is an integer between 2 and 20, and n is an integer between 1 and 5)
상기 용해부는 하기 [화학식 5] 내지 [화학식 9]에서 선택된 어느 하나의 것으로 표시되는 화합물일 수 있다.The dissolving unit may be a compound represented by any one selected from the following [Formula 5] to [Formula 9].
[화학식 5] [화학식 6][Formula 5] [Formula 6]
[화학식 7] [화학식 8][Formula 7] [Formula 8]
[화학식 9][Formula 9]
(상기 화학식 5 내지 9에서, o는 30 내지 200 사이의 정수이며, p는 4 내지 15 사이의 정수이다)(In Chemical Formulas 5 to 9, o is an integer between 30 and 200, and p is an integer between 4 and 15)
상기 용해부는 비닐트리메틸실란(vinyltrimethylsilane), 알릴트리메틸실란(allyltrimethylsilane), 비닐옥시트리메틸실란(vinyloxytrimethylsilane), 트리메톡시비닐실란(trimethoxyvinylsilane) 및 트리에톡시비닐실란(triethoxyvinylsilane)으로 이루어진 군으로부터 선택된 1종 이상의 것일 수도 있다.The dissolving part is one or more selected from the group consisting of vinyltrimethylsilane, allyltrimethylsilane, vinyloxytrimethylsilane, trimethoxyvinylsilane and triethoxyvinylsilane. It may be.
상기 분산안정제는 상온에서 액체 상태로서, 결합부는 -OH, -NH, -SH를 포함하여 분극입자 표면에서 수소 결합이 가능하고, 용해부는 상대적으로 긴 알킬 사슬 또는 알킬 곁사슬을 가지고 있어서 비극성 특성을 나타내어 극성인 필름의 고분자 수지와 상용성이 낮은 것을 특징으로 한다.The dispersion stabilizer is in a liquid state at room temperature, and the bonding portion includes -OH, -NH, and -SH, and hydrogen bonding is possible on the surface of the polarized particle, and the dissolving portion has a relatively long alkyl chain or alkyl side chain, so it exhibits non-polar characteristics. It is characterized by low compatibility with the polymer resin of the polar film.
상기 액상의 분산안정제는 수평균 분자량이 3,000 내지 60,000 사이인 것을 특징으로 하며, 점도는 1,000 cp 내지 50,000 cp 사이인 것을 특징으로 한다, 분자량이 너무 낮고 점도가 낮은 경우 분극입자의 분산을 안정화시키는 역할을 수행하기 어려우며, 분자량이 높고 점도가 너무 높으면 분극입자가 자유로운 브라운 운동을 하기 어려울 수 있다.The liquid dispersion stabilizer is characterized in that the number average molecular weight is between 3,000 and 60,000, and the viscosity is between 1,000 cp and 50,000 cp. When the molecular weight is too low and the viscosity is too low, the role of stabilizing the dispersion of polarized particles is difficult to perform, and if the molecular weight is high and the viscosity is too high, it may be difficult for polarized particles to perform free Brownian motion.
상기 분극입자는 형상 이방성을 지니며, 300nm 이상, 1 마이크로 이하의 크기를 갖고, 전기장 혹은 자기장에 따라 배열할 수 있도록 이온을 포함하거나 극성이 매우 높거나 자성을 띨 수 있으며, 표면에 수소결합이 가능한 N, O, F, S의 원소를 포함하는 것을 특징으로 한다. 분극입자는 전기장이 형성되지 않은 상태에서는 브라운 운동을 하며 가시광선 영역의 빛을 차단하며, 전기장이 형성된 경우 전기장에 평행하게 배열함으로써 가시광선 영역의 빛을 통과시켜 투과율을 조절하게 되므로 형상 이방성을 지녀야 효과적으로 투과율을 조절할 수 있다. 또한 가시광선 영역은 대략 380~750nm의 파장을 가지므로 이의 차단 혹은 투과와 더불어 전기장에 따른 빠른 회전을 위해서 분극입자의 크기는 1 마이크로 이하인 것이 적절하며, 300 nm를 초과하는 경우 가시광선 영역의 빛을 차단하기에 부족하다. 또한 입자의 표면에는 전기음성도가 큰 N, O, F를 지니고 있어서 분산 안정제의 결합부와 수소결합에 의해 단단하게 결합하기 쉽다.The polarized particles have shape anisotropy, have a size of 300 nm or more and 1 micron or less, contain ions to be arranged according to an electric or magnetic field, have a very high polarity or be magnetic, and have hydrogen bonds on their surfaces. Characterized in that it contains the elements of N, O, F, and S possible. Polarized particles perform Brownian motion and block light in the visible ray region when an electric field is not formed, and when an electric field is formed, they are arranged in parallel to the electric field to pass light in the visible ray region and adjust the transmittance. Therefore, they must have shape anisotropy. The transmittance can be effectively controlled. In addition, since the visible light region has a wavelength of approximately 380 to 750 nm, it is appropriate for the size of the polarized particles to be less than 1 micron in order to block or transmit them and to rotate rapidly according to the electric field. is not enough to block In addition, since the surface of the particle has N, O, and F having high electronegativity, it is easy to firmly bond with the bonding portion of the dispersion stabilizer by hydrogen bonding.
상기 액상의 분산안정제의 용해부와 극성 고분자 수지는 분산력에 대한 용해도 파라미터 및 극성력에 대한 용해도 파라미터에서 2를 초과하여 차이나는 것을 특징으로 한다. 액상의 분산안정제의 용해부와 극성 고분자 수지는 분산력에 대한 용해도 파라미터 및 극성력에 대한 용해도 파라미터 2 이하인 경우 분리된 상을 만들기 어려워 분극입자 현탁액의 분리된 액적을 형성하기 곤란하다.It is characterized in that the dissolving part of the liquid dispersion stabilizer and the polar polymer resin differ by more than 2 in the solubility parameter for the dispersing force and the solubility parameter for the polar force. When the solubility parameter for the dispersion force and the solubility parameter for the polar force are 2 or less between the dissolving part of the dispersion stabilizer in the liquid phase and the polar polymer resin, it is difficult to form a separated phase and form separated droplets of the polarized particle suspension.
아울러 상기 분극입자 현탁액을 형성하는 경우, 액상의 분산안정제 외에 분산안정제의 용해부와 상용성이 높거나 용해도 파라미터가 유사한 고비점 가소제 등을 첨가하여 현탁매의 점도를 추가적으로 낮출 수 있는 바, 상기 고비점 가소제로서는 디-2-에틸헥실프탈레이트(di-2-ethylhexyl phthalate), 디이소옥틸프탈레이트(di-isooctyl phthalate), 디카프릴프탈레이트(di-capryl phthalate), 디-n-옥틸프탈레이트(di-n-octyl phthalate), 부틸-벤질프탈레이트(butyl-benzyl phthalate), 디이소헵틸프탈레이트(di-isoheptyl phthalate), 디이소노닐프탈레이트(di-isononyl phthalate), 디이소데실프탈레이트(di-isodecyl phthalate), 디트리데실프탈레이트(di-tridecyl phthalate), 디운데실프탈레이트(di-undecyl phthalate), 디도데실프탈레이트(di-dodecyl phthalate), 디이소데실프탈레이트(di-isododecyl phthalate) 또는 이들의 이소프탈레이트 또는 테레프탈레이트, 또는 트리-2-에틸헥실트리멜리테이트(tri-2-ethylhexyl trimellitate), 디-2-에틸헥실아디페이트(di-2-ethylhexyl adipate), 디이소노닐아디페이트(di-isononyl adipate), 디이소데실아디페이트(di-isodecyl adipate), 디-2-에틸헥실세바케이트(di-2-ethylhexyl sebacate), 디-2-에틸헥실아젤레이트(di-2-ethylhexyl azelate), 에폭시화소이빈오일(epoxidized soy bean oil), 2-에틸헥실에폭시탈레이트(2-ethylhexyl epoxy tallate), 디이소데실테트라히드로-4,5-에폭시프탈레이트(di-isodecyl tetrahydro-4,5-epoxy phthalate), 폴리알킬렌아디페이트(poly(akylene adipates)), 폴리알킬렌세바케이트(poly(alkylene sebacates)) 및 폴리알킬렌아젤레이트(poly(alkylene azelates))로 이루어진 군으로부터 선택된 1종 이상의 것일 수 있다.In addition, in the case of forming the polarized particle suspension, the viscosity of the suspension medium can be further lowered by adding a high boiling point plasticizer that is highly compatible with the dissolving part of the dispersion stabilizer or has a similar solubility parameter, in addition to the liquid dispersion stabilizer. As the point plasticizer, di-2-ethylhexyl phthalate, di-isooctyl phthalate, di-capryl phthalate, di-n-octyl phthalate -octyl phthalate), butyl-benzyl phthalate, di-isoheptyl phthalate, di-isononyl phthalate, di-isodecyl phthalate, di tridecyl phthalate, di-undecyl phthalate, di-dodecyl phthalate, di-isodecyl phthalate, or isophthalates or terephthalates thereof; Or tri-2-ethylhexyl trimellitate, di-2-ethylhexyl adipate, di-isononyl adipate, diiso Decyl adipate (di-isodecyl adipate), di-2-ethylhexyl sebacate (di-2-ethylhexyl sebacate), di-2-ethylhexyl azelate (di-2-ethylhexyl azelate), epoxied ybin oil ( epoxidized soy bean oil), 2-ethylhexyl epoxy tallate, di-isodecyl tetrahydro-4,5-epoxy phthalate, polyalkylene Adipates (poly(akylene adipates) )), poly(alkylene sebacates), and polyalkylene azelates (poly(alkylene azelates)).
또한, 본 발명에서는 상기 분극입자 현탁액이 액적 형태로 고분자 수지 내에 분산되어 있는 투과도 가변 필름을 제공한다.In addition, the present invention provides a variable transmittance film in which the polarized particle suspension is dispersed in a polymer resin in the form of droplets.
상기 투과도 가변 필름의 매트릭스(기재)가 되는 고분자 수지는 분산안정제의 용해부에 비하여 상대적으로 높은 극성을 지니고 있어서 분산안정제와의 상용성이 낮은 것을 특징으로 한다.The polymer resin, which is the matrix (substrate) of the variable permeability film, has a relatively high polarity compared to the dissolving portion of the dispersion stabilizer, and thus has low compatibility with the dispersion stabilizer.
이때, 상기 고분자 수지는 폴리메틸메타크릴레이트(poly(methyl methacrylate)), 폴리에틸메타크릴레이트(poly(ethyl methacrylate)), 폴리메틸아크릴레이트(poly(methyl acrylate)), 폴리에틸아크릴레이트(poly(ethyl acrylate)), 폴리비닐아세테이트(poly(vinyl acetate)), 폴리우레탄(polyurethane), 폴리에틸렌-비닐아세테이트(poly(ethylene-vinyl acetate)), 나일론(Nylon), 폴리이미드(polyimides), 폴리술폰(polysulfones), 폴리에테르술폰(poly(ether sulfones)), 폴리에틸렌테레프탈레이트(polyethylene terephthalate), 폴리부틸렌테레프탈레이트(polybutylene terephthalate), 폴리비닐클로라이드(polyvinyl chloride), 셀룰로오스아세테이트(cellulose acetate), 셀로판(cellophane), 트리아세틸셀룰로오스(triacetyl cellulose), 폴리카보네이트(polycarbonate), 폴리아세탈 수지(polyacetal resin), 폴리페닐렌에테르(polyphenylene ether), 폴리옥시메틸렌(polyoxymethylene), 폴리옥시에틸렌(polyoxyethylene) 및 폴리페닐렌술피드(polyphenylene sulfide)로 이루어진 군으로부터 선택된 1종 이상의 것일 수 있다.At this time, the polymer resin is poly (methyl methacrylate), poly (ethyl methacrylate), poly (methyl acrylate), polyethyl acrylate (poly (ethyl acrylate)), poly(vinyl acetate), polyurethane, poly(ethylene-vinyl acetate), nylon, polyimides, polysulfone (polysulfones), poly(ether sulfones), polyethylene terephthalate, polybutylene terephthalate, polyvinyl chloride, cellulose acetate, cellophane ( cellophane, triacetyl cellulose, polycarbonate, polyacetal resin, polyphenylene ether, polyoxymethylene, polyoxyethylene and polyphenyl It may be at least one selected from the group consisting of rensulfide (polyphenylene sulfide).
또한, 본 발명에서는 (I) 이소펜틸아세테이트에 분산된 분극입자를 액상의 분산안정제와 고르게 혼합한 후, 이소펜틸아세테이트를 건조하여 분극입자 현탁액을 형성하는 단계; (II) 고분자 수지를 용매에 용해하여 고분자 수지 용액을 얻는 단계; (III) 상기 분극입자 현탁액과 고분자 수지 용액을 혼합하는 단계; 및 (IV) 상기 혼합용액을 투명전도막이 코팅된 기판 위에 코팅하고 용매를 건조함으로써 상분리에 의해 분극입자 현탁액이 액적으로 분산된 고형의 필름을 형성하는 단계;를 포함하는 투과도 가변 필름의 제조방법을 제공한다.Further, in the present invention, (I) uniformly mixing the polarized particles dispersed in isopentyl acetate with a liquid dispersion stabilizer, and then drying the isopentyl acetate to form a polarized particle suspension; (II) dissolving the polymer resin in a solvent to obtain a polymer resin solution; (III) mixing the polarized particle suspension with a polymer resin solution; and (IV) coating the mixed solution on a substrate coated with a transparent conductive film and drying the solvent to form a solid film in which the polarized particle suspension is dispersed in droplets by phase separation. to provide.
이때, 상기 고분자 수지는 상술한 것과 같은바, 고분자 수지를 용해하기 위한 용매는 분산안정제와 고분자 수지를 동시에 용해시킬 수 있어서 용액 상태에서 분극입자 현탁액과 고분자 수지를 고르게 섞어 줄 수 있는 것을 특징으로 한다.At this time, the polymer resin is as described above, and the solvent for dissolving the polymer resin can dissolve the dispersion stabilizer and the polymer resin at the same time, so that the polarized particle suspension and the polymer resin can be evenly mixed in a solution state. .
또한, 본 발명에서는 (i) 이소펜틸아세테이트에 분산된 분극입자를 액상의 분산안정제와 고르게 혼합한후, 이소펜틸아세테이트를 건조하여 분극입자 현탁액을 형성하는 단계; (ii) 상기 분극입자 현탁액과 반응성 올리고머를 혼합하는 단계; 및 (iii) 상기 혼합용액을 투명전도막이 코팅된 기판 위에 코팅하고 반응성 올리고머를중합함으로써 상분리에 의해 분극입자 현탁액이 액적으로 분산된 고형의 필름을 형성하는 단계;를 포함하는 투과도 가변 필름의 제조방법을 제공한다.Further, in the present invention, the steps of (i) uniformly mixing the polarized particles dispersed in isopentyl acetate with a liquid dispersion stabilizer and then drying the isopentyl acetate to form a polarized particle suspension; (ii) mixing the polarized particle suspension with a reactive oligomer; and (iii) forming a solid film in which the polarized particle suspension is dispersed in liquid droplets by phase separation by coating the mixed solution on a substrate coated with a transparent conductive film and polymerizing a reactive oligomer. provides
상기 반응성 올리고머는 극성인 모노머가 다수 결합된 것으로서 고분자로 중합할 수 있는 반응기를 하나 이상 지니며, 상온에서 액체 상태이어서 분극입자 현탁액과 혼합 가능한 것을 특징으로 한다.The reactive oligomer is a combination of a plurality of polar monomers, has one or more reactors capable of polymerizing into a polymer, and is in a liquid state at room temperature, so that it can be mixed with the polarized particle suspension.
이때, 상기 반응성 올리고머로서는 실란 가교성 폴리에틸렌(silane crosslinkable polyolefins), 가교성 우레탄 아크릴레이트 올리고머(crosslinkable urethane acrylate oligomers), 우레탄 메타크릴레이트 올리고머(urethane methacrylate oligomer), 우레탄 디아크릴레이트 올리고머(urethane diacrylate oligomer), 우레탄 디메타크릴레이트 올리고머(urethane dimethacrylate oligomer), 에폭시 메타크릴레이트 올리고머(epoxy methacrylate oligomer), 에폭시 아크릴레이트 올리고머(epoxy acrylate oligomer), 아크릴화 아크릴 올리고머(acrylated acrylic oligomer), 아크릴화 메타크릴 올리고머(acrylated methacrylic oligomer), 메타크릴화 아크릴 올리고머(methacrylated acrylic oligomer), 메타크릴화 메타크릴 올리고머(methacrylated methacrylic oligomer), 폴리에스터 아크릴레이트 올리고머(polyester acrylate oligomer), 폴리에스터 메타크릴레이트 올리고머(polyester methacrylated oligomer), 폴리에틸렌글리콜 아크릴레이트(poly(ethylene glycol) acrylate), 폴리에틸렌글리콜 디아크릴레이트(poly(ethylene glycol) diacrylate), 폴리에틸렌글리콜 메타크릴레이트(poly(ethylene glycol) methacrylate), 폴리에틸렌글리콜 디메타크릴레이트(poly(ethylene glycol) dimethacrylate), 폴리프로필렌글리콜 아크릴레이트(poly(propylene glycol)acrylate), 폴리프로필렌글리콜 디아크릴레이트(poly(propylene glycol) diacrylate), 폴리프로필렌글리콜 메타크릴레이트(poly(propylene glycol) methacrylate), 폴리프로필렌글리콜 디메타크릴레이트(poly(propylene glycol) dimethacrylate), 폴리카보네이티드디올 디아크릴레이트(polycarbonatediol diacrylate) 및 폴리카보네이티드디올 디메타크릴레이트(polycarbonatediol dimethacrylate)로 이루어진 군으로부터 선택된 1종 이상의 것일 수 있다.At this time, as the reactive oligomer, silane crosslinkable polyolefins, crosslinkable urethane acrylate oligomers, urethane methacrylate oligomer, urethane diacrylate oligomer , urethane dimethacrylate oligomer, epoxy methacrylate oligomer, epoxy acrylate oligomer, acrylated acrylic oligomer, acrylated methacrylic oligomer oligomer), methacrylated acrylic oligomer, methacrylated methacrylic oligomer, polyester acrylate oligomer, polyester methacrylated oligomer, polyethylene Poly(ethylene glycol) acrylate, poly(ethylene glycol) diacrylate, poly(ethylene glycol) methacrylate, poly(ethylene glycol) dimethacrylate glycol) dimethacrylate), poly(propylene glycol)acrylate), poly(propylene glycol) diacrylate), polypropylene glycol methacrylate (p oly(propylene glycol) methacrylate), poly(propylene glycol) dimethacrylate, polycarbonatediol diacrylate and polycarbonatediol dimethacrylate It may be one or more selected from the group consisting of.
또한, 상기 반응성 올리고머는 분자량이 200내지 50,000인 사이인 것을 특징으로 하며, 상기 반응성 올리고머의 점도는 200 내지 100,000 cps 사이인 것을 특징으로 한다. 분자량이 너무 낮은 경우 상분리 시 분극입자 현탁액의 액적이 작게 형성될 우려가 있으며, 이 경우 입자가 회전하기 어려워 전압인계 전후의 투과율차이가 작아질 수 있다. 한편 분자량이 너무 큰 경우 반응성 작용기가 충분히 결합을 형성하기 어려워 미반응물이 많이 남게 될 우려가 있다.In addition, the reactive oligomer is characterized in that the molecular weight is between 200 and 50,000, and the viscosity of the reactive oligomer is characterized in that between 200 and 100,000 cps. If the molecular weight is too low, small droplets of the polarized particle suspension may be formed during phase separation. In this case, it is difficult for the particles to rotate, and the difference in transmittance before and after voltage transfer may be reduced. On the other hand, if the molecular weight is too large, it is difficult for the reactive functional group to form a sufficient bond, and there is a concern that a large amount of unreacted material may remain.
상기 반응성 올리고머의 반응을 개시하기 위한 개시제를 포함할 수 있으며, 이러한 개시제는 열, UV, 전자선, 감마선, 초음파 등에 의해 라디칼을 형성하여 반응을 개시할 수 있는 것을 특징으로 한다.It may include an initiator for initiating the reaction of the reactive oligomer, and this initiator is characterized in that it can initiate the reaction by forming radicals by heat, UV, electron beam, gamma ray, ultrasound, and the like.
이하 본 발명의 실시예를 구체적으로 서술한다.Hereinafter, embodiments of the present invention will be described in detail.
[실시 예 1 내지 3][Examples 1 to 3]
이소펜틸아세테이트에 분산된 폴리요오드 분극입자(10 wt%)를 액상의 비극성 분산안정제와 고르게 혼합한 후, 이소펜틸아세테이트를 건조하여 분극입자의 현탁액(분극입자:액상분산안정제=6:94)을 형성하였다. 한편, 매트릭스 재료로 극성의 고분자 수지를 용매에 25 wt%로 용해한 후, 분극입자 현탁액과 고분자 수지 용액을 혼합하고, 혼합 용액을 투명전도막이 코팅된 기판 위에 코팅하고 용매를 건조하여 투과도 가변 필름을 제조하였다. 이 건조된 투과도 가변 필름 위에 다른 투명전도막을 부착하고, 양 쪽의 투명 전도막 기판에 전기를 인가할 수 있는 버스바를 설치한 다음, 두 버스바에 전원 및 스위치를 연결하여 투과도 가변 필름을 제조하였다.After uniformly mixing polyiodine polarized particles (10 wt%) dispersed in isopentyl acetate with a liquid non-polar dispersion stabilizer, isopentyl acetate is dried to obtain a suspension of polarized particles (polarized particles:liquid dispersion stabilizer = 6:94). formed. On the other hand, after dissolving 25 wt% of a polar polymer resin in a solvent as a matrix material, the polarized particle suspension and the polymer resin solution are mixed, the mixed solution is coated on a substrate coated with a transparent conductive film, and the solvent is dried to obtain a variable permeability film. manufactured. Another transparent conductive film was attached on the dried variable transmittance film, a bus bar capable of applying electricity to both transparent conductive film substrates was installed, and a power supply and a switch were connected to the two bus bars to prepare a variable transmittance film.
하기 표 1에 실시예 1 내지 3에서 사용한 재료 및 Hansen 용해도 파라미터를 나타내었다.Table 1 below shows the materials and Hansen solubility parameters used in Examples 1 to 3.
[실시 예 4 내지 6][Examples 4 to 6]
이소펜틸아세테이트에 분산된 폴리요오드 분극입자(10 wt%)를 액상의 비극성 분산안정제와 고르게 혼합한 후 이소펜틸아세테이트를 건조하여 분극입자 현탁액(분극입자:분산안정제=6:94)을 형성하였다. 극성의 액상 고분자 수지용 반응성 올리고머와 분극입자 현탁액을 혼합(올리고머:현탁액=1:0.8)한 후 위의 혼합용액에 개시제로 2,2-azobisisobutyronitrile을 반응성 올리고머 양의 0.8w% 고르게 혼합한 다음, 투명 전도막이 코팅된 기판 위에 코팅하고, 반응성 올리고머를 65℃에서 중합함으로써 상분리에 의해 분극입자 현탁액이 액적으로 분산된 투과도 가변 필름을 제조하였다.Polyiodine polarized particles (10 wt%) dispersed in isopentyl acetate were evenly mixed with a liquid non-polar dispersion stabilizer, and then the isopentyl acetate was dried to form a polarized particle suspension (polarized particles:dispersion stabilizer = 6:94). After mixing the reactive oligomer for polar liquid polymer resin and the polarized particle suspension (oligomer: suspension = 1:0.8), 2,2-azobisisobutyronitrile as an initiator was mixed evenly with 0.8w% of the amount of the reactive oligomer in the above mixed solution, A variable transmittance film in which the polarized particle suspension was dispersed in droplets was prepared by phase separation by coating on a substrate coated with a transparent conductive film and polymerizing a reactive oligomer at 65° C.
하기 표 2에 실시예 4 내지 6에서 사용한 재료 및 Hansen 용해도 파라미터를 나타내었다.Table 2 below shows the materials and Hansen solubility parameters used in Examples 4 to 6.
[시험 예 1 내지 6][Test Examples 1 to 6]
상기 실시예 1 내지 6에서 만들어진 투과도 가변필름 위에 다른 투명전도막을 부착하고, 양 쪽의 투명 전도막 기판에 전기를 인가할 수 있는 버스바를 설치한 다음, 두 버스바에 전원 및 스위치를 연결하고. 전기 인가 전후(off/110V)에 대하여 투과도를 변화를 UV/VIS spectrophotometer를 이용하여 가시광선 영역의 투과율(380-770㎚)을 확인하였으며, 그 결과를 하기 표 3에 나타내었다.Attach another transparent conductive film on the variable transmittance film made in Examples 1 to 6, install a bus bar capable of applying electricity to both transparent conductive film substrates, and then connect power and a switch to the two bus bars. Transmittance (380-770 nm) in the visible ray region was confirmed using a UV/VIS spectrophotometer to change transmittance before and after electric application (off/110V), and the results are shown in Table 3 below.
Claims (12)
상기 결합부는 하기 [화학식 1] 내지 [화학식 4]에서 선택된 어느 하나의 것으로 표시되는 화합물이고,
[화학식 1] [화학식 2]
[화학식 3] [화학식 4]
(상기 화학식 1 내지 4에서, X는 N, O, F 또는 S이고, m은 2 내지 20 사이의 정수이며, n은 1 내지 5 사이의 정수이다)
상기 용해부는 하기 [화학식 5] 내지 [화학식 9]에서 선택된 어느 하나의 것으로 표시되는 화합물인 것을 특징으로 하는 분극입자 현탁액.
[화학식 5] [화학식 6]
[화학식 7] [화학식 8]
[화학식 9]
(상기 화학식 5 내지 9에서, o는 30 내지 200 사이의 정수이며, p는 4 내지 15 사이의 정수이다)A polarized particle suspension containing a liquid dispersion stabilizer consisting of an anchoring group and a solubilizing group,
The binding portion is a compound represented by any one selected from the following [Formula 1] to [Formula 4],
[Formula 1] [Formula 2]
[Formula 3] [Formula 4]
(In Formulas 1 to 4, X is N, O, F or S, m is an integer between 2 and 20, and n is an integer between 1 and 5)
The dissolving part is a polarized particle suspension, characterized in that the compound represented by any one selected from the following [Formula 5] to [Formula 9].
[Formula 5] [Formula 6]
[Formula 7] [Formula 8]
[Formula 9]
(In Chemical Formulas 5 to 9, o is an integer between 30 and 200, and p is an integer between 4 and 15)
(II) 고분자 수지를 용매에 용해하여 고분자 수지 용액을 얻는 단계;
(III) 상기 분극입자 현탁액과 고분자 수지 용액을 혼합하는 단계; 및
(IV) 상기 혼합용액을 투명전도막이 코팅된 기판 위에 코팅하고 용매를 건조함으로써 상분리에 의해 분극입자 현탁액이 액적으로 분산된 고형의 필름을 형성하는 단계;를 포함하는 투과도 가변 필름의 제조방법.(I) uniformly mixing the polarized particles dispersed in isopentyl acetate with the liquid dispersion stabilizer according to claim 1 and then drying the isopentyl acetate to form a polarized particle suspension;
(II) dissolving the polymer resin in a solvent to obtain a polymer resin solution;
(III) mixing the polarized particle suspension with a polymer resin solution; and
(IV) coating the mixed solution on a transparent conductive film-coated substrate and drying the solvent to form a solid film in which the polarized particle suspension is dispersed in droplets by phase separation; Method for producing a variable transmittance film comprising.
(ii) 상기 분극입자 현탁액과 반응성 올리고머를 혼합하는 단계; 및
(iii) 상기 혼합용액을 투명전도막이 코팅된 기판 위에 코팅하고 반응성 올리고머를중합함으로써 상분리에 의해 분극입자 현탁액이 액적으로 분산된 고형의 필름을 형성하는 단계;를 포함하는 투과도 가변 필름의 제조방법.(i) uniformly mixing the polarized particles dispersed in isopentyl acetate with the liquid dispersion stabilizer according to claim 1 and then drying the isopentyl acetate to form a polarized particle suspension;
(ii) mixing the polarized particle suspension with a reactive oligomer; and
(iii) forming a solid film in which the polarized particle suspension is dispersed in droplets by phase separation by coating the mixed solution on a substrate coated with a transparent conductive film and polymerizing a reactive oligomer;
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| KR920011659A (en) | 1990-12-14 | 1992-07-24 | 강진구 | Robot Return to Origin |
| KR930702534A (en) | 1990-08-31 | 1993-09-09 | 레나토 스가르비 | Antibiotic GE1655 Complex and its Factors A, B and C |
| KR20170093000A (en) * | 2016-02-04 | 2017-08-14 | 동우 화인켐 주식회사 | Colored photosensitive resin composition and color filter using the same |
| JP2019056126A (en) * | 2013-11-04 | 2019-04-11 | ルブリゾル アドバンスド マテリアルズ， インコーポレイテッド | Acrylic dispersants with fused aromatic imide anchor groups |
| KR102151969B1 (en) * | 2019-12-11 | 2020-09-04 | 주식회사 지투비 | Method for manufacturing light valve windows and light valve windows manufactured thereby |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR930702534A (en) | 1990-08-31 | 1993-09-09 | 레나토 스가르비 | Antibiotic GE1655 Complex and its Factors A, B and C |
| KR920011659A (en) | 1990-12-14 | 1992-07-24 | 강진구 | Robot Return to Origin |
| JP2019056126A (en) * | 2013-11-04 | 2019-04-11 | ルブリゾル アドバンスド マテリアルズ， インコーポレイテッド | Acrylic dispersants with fused aromatic imide anchor groups |
| KR20170093000A (en) * | 2016-02-04 | 2017-08-14 | 동우 화인켐 주식회사 | Colored photosensitive resin composition and color filter using the same |
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