CN114605762B - Nanometer zirconia dispersion liquid, preparation method and application - Google Patents
Nanometer zirconia dispersion liquid, preparation method and application Download PDFInfo
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- CN114605762B CN114605762B CN202210422098.4A CN202210422098A CN114605762B CN 114605762 B CN114605762 B CN 114605762B CN 202210422098 A CN202210422098 A CN 202210422098A CN 114605762 B CN114605762 B CN 114605762B
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 247
- 239000006185 dispersion Substances 0.000 title claims abstract description 100
- 239000007788 liquid Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- -1 acryloyloxy Chemical group 0.000 claims abstract description 43
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 31
- 239000011347 resin Substances 0.000 claims abstract description 31
- 229920005989 resin Polymers 0.000 claims abstract description 31
- 239000002245 particle Substances 0.000 claims abstract description 26
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 14
- 125000003118 aryl group Chemical group 0.000 claims abstract description 13
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 12
- 125000003545 alkoxy group Chemical group 0.000 claims abstract description 11
- 125000000753 cycloalkyl group Chemical group 0.000 claims abstract description 10
- 239000003995 emulsifying agent Substances 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 17
- 239000002904 solvent Substances 0.000 claims description 17
- 239000012788 optical film Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 125000003277 amino group Chemical group 0.000 claims description 9
- ITCAUAYQCALGGV-XTICBAGASA-M sodium;(1r,4ar,4br,10ar)-1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylate Chemical compound [Na+].C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C([O-])=O ITCAUAYQCALGGV-XTICBAGASA-M 0.000 claims description 8
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- 150000001412 amines Chemical class 0.000 claims description 4
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- JMGZBMRVDHKMKB-UHFFFAOYSA-L disodium;2-sulfobutanedioate Chemical compound [Na+].[Na+].OS(=O)(=O)C(C([O-])=O)CC([O-])=O JMGZBMRVDHKMKB-UHFFFAOYSA-L 0.000 claims description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Natural products OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims 2
- 235000010290 biphenyl Nutrition 0.000 claims 1
- 239000004305 biphenyl Substances 0.000 claims 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 13
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 abstract description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 abstract description 6
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract description 5
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 abstract description 5
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 4
- 239000001257 hydrogen Substances 0.000 abstract description 4
- 230000003287 optical effect Effects 0.000 abstract description 3
- 125000005373 siloxane group Chemical group [SiH2](O*)* 0.000 abstract description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 abstract description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 abstract description 2
- KIQKWYUGPPFMBV-UHFFFAOYSA-N diisocyanatomethane Chemical compound O=C=NCN=C=O KIQKWYUGPPFMBV-UHFFFAOYSA-N 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 20
- 239000000243 solution Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- QNAYBMKLOCPYGJ-UHFFFAOYSA-N D-alpha-Ala Natural products CC([NH3+])C([O-])=O QNAYBMKLOCPYGJ-UHFFFAOYSA-N 0.000 description 8
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 description 8
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 6
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 6
- 125000003396 thiol group Chemical group [H]S* 0.000 description 6
- GSJNBCZKEUYYLK-UHFFFAOYSA-N [phenoxy(phenyl)methyl] prop-2-enoate Chemical compound C=1C=CC=CC=1C(OC(=O)C=C)OC1=CC=CC=C1 GSJNBCZKEUYYLK-UHFFFAOYSA-N 0.000 description 4
- GCTPMLUUWLLESL-UHFFFAOYSA-N benzyl prop-2-enoate Chemical compound C=CC(=O)OCC1=CC=CC=C1 GCTPMLUUWLLESL-UHFFFAOYSA-N 0.000 description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- PKMSXGVLJHFQHJ-UHFFFAOYSA-N (2-phenylphenyl)methyl prop-2-enoate Chemical compound C=CC(=O)OCC1=CC=CC=C1C1=CC=CC=C1 PKMSXGVLJHFQHJ-UHFFFAOYSA-N 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 3
- 125000003710 aryl alkyl group Chemical group 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 3
- LLAPDLPYIYKTGQ-UHFFFAOYSA-N 1-aminoethyl Chemical group C[CH]N LLAPDLPYIYKTGQ-UHFFFAOYSA-N 0.000 description 2
- VAZQKPWSBFZARZ-UHFFFAOYSA-N 2-(2-phenylphenoxy)ethyl prop-2-enoate Chemical compound C=CC(=O)OCCOC1=CC=CC=C1C1=CC=CC=C1 VAZQKPWSBFZARZ-UHFFFAOYSA-N 0.000 description 2
- CDOUZKKFHVEKRI-UHFFFAOYSA-N 3-bromo-n-[(prop-2-enoylamino)methyl]propanamide Chemical compound BrCCC(=O)NCNC(=O)C=C CDOUZKKFHVEKRI-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 125000003342 alkenyl group Chemical group 0.000 description 2
- 125000004202 aminomethyl group Chemical group [H]N([H])C([H])([H])* 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 2
- 235000019329 dioctyl sodium sulphosuccinate Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 235000019260 propionic acid Nutrition 0.000 description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical group O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 2
- 125000001424 substituent group Chemical group 0.000 description 2
- 125000000542 sulfonic acid group Chemical group 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 125000003944 tolyl group Chemical group 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- QBYIENPQHBMVBV-HFEGYEGKSA-N (2R)-2-hydroxy-2-phenylacetic acid Chemical compound O[C@@H](C(O)=O)c1ccccc1.O[C@@H](C(O)=O)c1ccccc1 QBYIENPQHBMVBV-HFEGYEGKSA-N 0.000 description 1
- LGEJUGBHYJDUJO-UHFFFAOYSA-N 1,1'-biphenyl;methyl prop-2-enoate Chemical compound COC(=O)C=C.C1=CC=CC=C1C1=CC=CC=C1 LGEJUGBHYJDUJO-UHFFFAOYSA-N 0.000 description 1
- YCEZZDNWLVQCRU-UHFFFAOYSA-N 1,2-diaminoethyl Chemical group N[CH]CN YCEZZDNWLVQCRU-UHFFFAOYSA-N 0.000 description 1
- 125000006083 1-bromoethyl group Chemical group 0.000 description 1
- 125000001478 1-chloroethyl group Chemical group [H]C([H])([H])C([H])(Cl)* 0.000 description 1
- 125000004066 1-hydroxyethyl group Chemical group [H]OC([H])([*])C([H])([H])[H] 0.000 description 1
- 125000000094 2-phenylethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- COLNVLDHVKWLRT-QMMMGPOBSA-N L-phenylalanine Chemical compound OC(=O)[C@@H](N)CC1=CC=CC=C1 COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 description 1
- IWYDHOAUDWTVEP-UHFFFAOYSA-N R-2-phenyl-2-hydroxyacetic acid Natural products OC(=O)C(O)C1=CC=CC=C1 IWYDHOAUDWTVEP-UHFFFAOYSA-N 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 125000005370 alkoxysilyl group Chemical group 0.000 description 1
- 125000005103 alkyl silyl group Chemical group 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 125000001204 arachidyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 125000005997 bromomethyl group Chemical group 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 125000004218 chloromethyl group Chemical group [H]C([H])(Cl)* 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 125000006165 cyclic alkyl group Chemical group 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 125000001511 cyclopentyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C1([H])[H] 0.000 description 1
- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001183 hydrocarbyl group Chemical group 0.000 description 1
- 125000004029 hydroxymethyl group Chemical group [H]OC([H])([H])* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 229960002510 mandelic acid Drugs 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000001421 myristyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000003136 n-heptyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 125000004368 propenyl group Chemical group C(=CC)* 0.000 description 1
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000005415 substituted alkoxy group Chemical group 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 125000000101 thioether group Chemical group 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/08—Homopolymers or copolymers of acrylic acid esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/175—Amines; Quaternary ammonium compounds containing COOH-groups; Esters or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/41—Compounds containing sulfur bound to oxygen
- C08K5/42—Sulfonic acids; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2244—Oxides; Hydroxides of metals of zirconium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a nano zirconia dispersion liquid, a preparation method and application thereof, and relates to the technical field of optical resins. The nano zirconia dispersion liquid comprises nano zirconia, resin and a capping agent, wherein the R structure in the capping agent is at least one selected from alkyl, alkoxy, carbonyl, acryloyloxy, aromatic ring, double bond, cycloalkyl, methylene, isocyanate, mercapto, amino, carboxyl and hydroxyl; x is selected from at least one of amino, hydroxyl and siloxy; the Y structure is selected from at least one of hydrogen, carboxyl, hydroxyl, sulfonic acid, phosphoric acid, and siloxane groups. According to the nano zirconia dispersion liquid, the electron donor group is introduced to the surface of the nano zirconia by the capping agent, so that the thickness of an electric double layer around nano zirconia particles is increased, repulsive force among the particles is increased, and the stability of the nano zirconia dispersion liquid is improved. The nanometer zirconia dispersion liquid has stable index smaller than 1.2 after being kept stand for 12 months in normal temperature and light shading condition, and has good stability.
Description
Technical Field
The invention relates to the technical field of optical resins, in particular to a nano zirconia dispersion liquid, a preparation method and application.
Background
In recent years, a resin-type zirconia dispersion liquid obtained by combining a zirconia particle dispersion with a transparent resin or a film has been used well in the optical field. For example, optical films such as brightness enhancement films prepared from zirconia resin dispersions can be used in LCD displays to increase the brightness and clarity of the screen.
To enable dispersion of zirconia nanoparticles in a resin matrix or for use in fully formulated compositions, one approach is a solvent-free process, in which zirconia powder aggregate particles are reduced in size, surface treated, and compounded into a resin by a mechanical grinding process (e.g., milling) without the aid of a solvent. Although this method avoids the use of solvents, the agglomeration of particles is severe and the stability of the dispersion is not as good as expected.
Another method is an organic solvent-based method in which an organic solvent (usually a water-miscible solvent) is mixed with water in a certain ratio, and after the particles are treated, the water and the organic solvent are removed to obtain a resin-based zirconia dispersion, and although this method has a certain advantage in terms of dispersibility of the particles as compared with a solvent-free method, there is a problem that dispersion stability of the dispersion is poor, such as a phenomenon that the zirconia dispersion is deteriorated in light transmittance, becomes cloudy in a system, and even a phenomenon that zirconia small particles are precipitated occurs, and furthermore, a large amount of use of the organic solvent is necessarily accompanied with pollution to the environment and hazard to the human body, and is disadvantageous for cost reduction and mass production.
In view of this, the present invention has been made.
Disclosure of Invention
The invention aims to provide a nano zirconia dispersion liquid so as to solve the technical problems of serious particle agglomeration, poor stability and easy environmental pollution of the zirconia dispersion liquid in the prior art.
In order to achieve the above object of the present invention, the following technical solutions are specifically adopted:
the first aspect of the invention provides a nano zirconia dispersion comprising nano zirconia, a resin and a capping agent;
the structure of the capping agent is as follows:
wherein R is selected from C 1 -C 20 Substituted or unsubstituted alkyl, C 1 -C 20 Substituted or unsubstitutedAt least one of a substituted alkoxy group, a carbonyl group, a substituted or unsubstituted acryloyloxy group, a substituted or unsubstituted aromatic ring, a substituted or unsubstituted double bond, a substituted or unsubstituted cycloalkyl group, a methylene group, an isocyanate group, a mercapto group, an amino group, a carboxyl group, and a hydroxyl group.
X is selected from at least one of amino, hydroxyl and substituted or unsubstituted siloxy.
Y is selected from at least one of hydrogen, carboxyl, hydroxyl, sulfonic acid group, phosphoric acid group and substituted or unsubstituted siloxane group.
Alternatively, R is selected from C 1 -C 12 Substituted or unsubstituted alkyl, C 1 -C 12 At least one of a substituted or unsubstituted alkoxy group, a carbonyl group, a substituted or unsubstituted acryloyloxy group, a substituted or unsubstituted aromatic ring, a substituted or unsubstituted double bond, a substituted or unsubstituted cycloalkyl group, a methylene group, an isocyanate group, a mercapto group, an amino group, a carboxyl group, and a hydroxyl group.
Preferably, R is selected from C 1 -C 4 Substituted or unsubstituted alkyl, C 1 -C 4 At least one of a substituted or unsubstituted alkoxy group, a carbonyl group, a substituted or unsubstituted acryloyloxy group, a substituted or unsubstituted aromatic ring, a substituted or unsubstituted double bond, a substituted or unsubstituted cycloalkyl group, a methylene group, an isocyanate group, a mercapto group, an amino group, a carboxyl group, and a hydroxyl group.
Optionally, the addition amount of the capping agent is 3-25% of the mass of the nano zirconia.
Optionally, the particle size of the nano zirconia is 1-40nm.
Preferably, the nano zirconia is present in an amount of 50wt.% to 70wt.%.
Optionally, an emulsifier is also included.
Preferably, the emulsifier comprises at least one of polyoxyethylene fatty amine, sodium abietate, dioctyl sodium sulfosuccinate and polyoxyethylene lauryl ether.
Optionally, the addition amount of the emulsifier is 1-12% of the mass of the nano zirconia.
In a second aspect, the present invention provides a method for preparing a nano zirconia dispersion, comprising the steps of: preparing a first solution from a capping agent and an optional emulsifier, adding a nano zirconia solution into the first solution, and finally adding resin to obtain the nano zirconia dispersion.
Optionally, the resin comprises at least one of phenoxybenzyl acrylate, biphenylmethanol acrylate, benzyl acrylate, or ortho-phenylphenoxyethyl acrylate.
Preferably, the solvent of the first solution comprises water.
Preferably, the solvent of the nano zirconia solution comprises water.
Optionally, the method further comprises the step of adding resin to remove solvent to obtain the nano zirconia dispersion liquid.
Preferably, the solvent is removed by evaporation.
In a third aspect, the present invention provides the use of the nano zirconia dispersion in the preparation of an optical film.
Compared with the prior art, the invention has at least the following beneficial effects:
according to the nano zirconia dispersion liquid, the electron donor group is introduced to the surface of the nano zirconia by the capping agent, so that the thickness of an electric double layer around nano zirconia particles is increased, repulsive force among the particles is increased, and the stability of the nano zirconia dispersion liquid is improved. The nanometer zirconia dispersion liquid has stable index smaller than 1.2 after being kept stand for 12 months in normal temperature and light shading condition, and has good stability.
The preparation method of the nano zirconia dispersion liquid provided by the invention has the advantages of simple process, low cost, green and pollution-free preparation process, no need of complex dispersing equipment and capability of preparing the zirconia dispersion liquid with high stability.
The application of the nano zirconia dispersion liquid in the preparation of the optical film provides dispersion liquid with good stability for the optical film, and the prepared optical film has good uniformity, and can greatly improve the refractive index of the optical film and the performance of the film.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to embodiments and examples, but it will be understood by those skilled in the art that the following embodiments and examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The first aspect of the invention provides a nano zirconia dispersion comprising nano zirconia, a resin and a capping agent;
the structure of the capping agent is as follows:
wherein R is selected from C 1 -C 20 Substituted or unsubstituted alkyl, C 1 -C 20 At least one of a substituted or unsubstituted alkoxy group, a carbonyl group, a substituted or unsubstituted acryloyloxy group, a substituted or unsubstituted aromatic ring, a substituted or unsubstituted double bond, a substituted or unsubstituted cycloalkyl group, a methylene group, an isocyanate group, a mercapto group, an amino group, a carboxyl group, and a hydroxyl group;
x is selected from at least one of amino, hydroxyl and substituted or unsubstituted siloxy;
y is selected from at least one of hydrogen, carboxyl, hydroxyl, sulfonic acid group, phosphoric acid group and substituted or unsubstituted siloxane group.
It is known from DLVO electric double layer theory that when two charged zirconia particles are close to each other, electric double layers around the particles overlap each other, electric double layers deform, repulsive force is generated between the particles, meanwhile, van der waals attraction force acts between the two particles, and when repulsive force between the particles is greater than van der waals attraction force between the particles, stability of the particles is greatly improved, and macroscopic appearance is that the zirconia dispersion liquid is stable in dispersion. Therefore, the X structure in the capping agent of the present invention introduces electron donor groups into zirconia to increase the thickness of the electric double layer around the particles, and to increase the repulsive force between the particles, thereby improving the stability of the zirconia dispersion.
According to the nano zirconia dispersion liquid, the electron donor group is introduced to the surface of the nano zirconia by the capping agent, so that the thickness of an electric double layer around nano zirconia particles is increased, repulsive force among the particles is increased, and the stability of the nano zirconia dispersion liquid is improved. The nanometer zirconia dispersion liquid has stable index smaller than 1.2 after being kept stand for 12 months in normal temperature and light shading condition, and has good stability.
In some embodiments of the invention, C 1 -C 20 Substituted or unsubstituted alkyl groups, suitable short groups include straight, branched or cyclic alkyl, alkenyl, aryl and aralkyl groups. Particular exemplary groups include straight chain alkyl groups such as methyl, ethyl, propyl, butyl, pentyl, hexyl, heptyl, octyl, decyl, dodecyl, tetradecyl, hexadecyl, octadecyl, and eicosyl; branched alkyl groups such as isopropyl, isobutyl, tert-butyl, tert-hexyl and 2-ethylhexyl; cyclic alkyl groups such as cyclopentyl and cyclohexyl; alkenyl groups such as vinyl, allyl, and propenyl; aryl groups such as phenyl and tolyl; and aralkyl groups such as benzyl. Some or all of the hydrogen atoms on the hydrocarbyl group may be substituted, with suitable substituents including: alkoxy groups such as methoxy, ethoxy and (iso) propoxy: halogen atoms such as fluorine, chlorine, bromine and iodine; cyano group; an amino group; c (C) 6 -C 18 Aryl groups such as phenyl and tolyl; c (C) 7 -C 18 Aralkyl groups such as benzyl and phenethyl; an ester group; an ether group; an acyl group; a thioether group; alkylsilyl, and alkoxysilyl groups, as well as combinations of the foregoing.
In some embodiments of the invention, C 1 -C 20 Substituted or unsubstituted alkoxy is a group represented by-OM, M is typically but not limited to methyl, ethyl, propyl, isopropyl, n-butyl, sec-butyl, isobutyl, tert-butyl, n-pentyl, n-hexyl, n-heptyl, n-octyl, hydroxymethyl, 1-hydroxyethyl, 2-hydroxyisobutyl, 1, 2-dihydroxyethyl, 1, 3-dihydroxyisopropyl, 2, 3-dihydroxytert-butyl, 1,2, 3-trihydroxypropyl, chloromethyl, 1-chloroethyl, 2-chloroisobutyl, 1, 2-dichloroethyl, 1, 3-dichloroisopropyl, 2, 3-dichlorotert-butyl, 1,2, 3-tri-Chloropropyl, bromomethyl, 1-bromoethyl, 2-bromoisobutyl, 1, 2-dibromoethyl, 1, 3-dibromoisopropyl, 2, 3-dibromo-tert-butyl, 1,2, 3-tribromopropyl, iodomethyl, 1-iodoethyl, 2-iodoisobutyl, 1, 2-diiodoethyl, 1, 3-diiodoisopropyl, 2, 3-diiodotert-butyl, 1,2, 3-triiodopropyl, aminomethyl, 1-aminoethyl, 2-aminoisobutyl, 1, 2-diaminoethyl, 1, 3-diaminoisopropyl, 2, 3-diaminotert-butyl, 1,2, 3-triaminopropyl, aminomethyl or 1-aminoethyl.
In some embodiments of the invention, X is typically but not limited to an amine group, a hydroxyl group, a substituted or unsubstituted siloxy group.
In some embodiments of the invention, Y is typically, but not limited to, hydrogen, carboxyl, hydroxyl, sulfonic acid, phosphoric acid, substituted or unsubstituted siloxy.
In the substituted or unsubstituted group of the present invention, the substituent is typically but not limited to halogen, benzene ring, alkyl, hydroxyl or carboxyl.
Alternatively, R is selected from C 1 -C 12 Substituted or unsubstituted alkyl, C 1 -C 12 At least one of a substituted or unsubstituted alkoxy group, a carbonyl group, a substituted or unsubstituted acryloyloxy group, a substituted or unsubstituted aromatic ring, a substituted or unsubstituted double bond, a substituted or unsubstituted cycloalkyl group, a methylene group, an isocyanate group, a mercapto group, an amino group, a carboxyl group, and a hydroxyl group.
Preferably, R is selected from C 1 -C 4 Substituted or unsubstituted alkyl, C 1 -C 4 At least one of a substituted or unsubstituted alkoxy group, a carbonyl group, a substituted or unsubstituted acryloyloxy group, a substituted or unsubstituted aromatic ring, a substituted or unsubstituted double bond, a substituted or unsubstituted cycloalkyl group, a methylene group, an isocyanate group, a mercapto group, an amino group, a carboxyl group, and a hydroxyl group.
Optionally, the addition amount of the capping agent is 3-25% of the mass of the nano zirconia.
When the addition amount of the capping agent is less than 3%, the stability of the nano zirconia dispersion liquid is not greatly improved; when the addition amount of the capping agent is more than 25%, the stability improving effect on the nano zirconia dispersion is not great and the cost is increased.
In some embodiments of the present invention, the capping agent is typically added in an amount of, but not limited to, 3%, 5%, 7%, 9%, 11%, 13%, 15%, 17%, 19%, 21%, 23% or 25% by mass of the nano zirconia.
Optionally, the particle size of the nano zirconia is 1nm-40nm.
Preferably, the nano zirconia is present in an amount of 50wt.% to 70wt.%.
When the content of the nano zirconia is lower than 50 wt%, the content of the nano zirconia is too low, which is not beneficial to saving the cost; when the content of nano zirconia is higher than 70wt.%, the stability of the nano zirconia dispersion may be negatively affected.
Optionally, an emulsifier is also included.
In some embodiments of the present invention, an amount of an emulsifier is added to the system, and the synergistic effect between the capping agent and the emulsifier is utilized to further increase the stability of the zirconia resin dispersion.
Preferably, the emulsifier comprises at least one of polyoxyethylene fatty amine, sodium abietate, dioctyl sodium sulfosuccinate and polyoxyethylene lauryl ether.
Optionally, the addition amount of the emulsifier is 1-12% of the mass of the nano zirconia.
In some embodiments of the invention, the emulsifier is typically added in an amount of, but not limited to, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11% or 12% by mass of the nano zirconia.
In a second aspect, the present invention provides a method for preparing a nano zirconia dispersion, comprising the steps of: preparing a first solution from a capping agent and an optional emulsifier, adding a nano zirconia solution into the first solution, and finally adding resin to obtain the nano zirconia dispersion.
The preparation method of the nano zirconia dispersion liquid provided by the invention has the advantages of simple process, low cost, green and pollution-free preparation process, no need of complex dispersing equipment and capability of preparing the zirconia dispersion liquid with high stability.
Optionally, the resin comprises at least one of phenoxybenzyl acrylate, biphenylmethanol acrylate, benzyl acrylate, or ortho-phenylphenoxyethyl acrylate.
In some embodiments of the present invention, the resin is typically, but not limited to, phenoxybenzyl acrylate, biphenylmethanol acrylate, benzyl acrylate, or ortho-phenylphenoxyethyl acrylate.
The English abbreviations of phenoxybenzyl acrylate, biphenyl methanol acrylate, benzyl acrylate, and o-phenylphenoxyethyl acrylate in the resin are respectively referred to as PBA, BPMA, BZA, OPPEA, and O-phenylphenoxyethyl acrylate, respectively.
Preferably, the solvent of the first solution comprises water.
Preferably, the solvent of the nano zirconia solution comprises water.
In some preferred embodiments of the invention, water is used as a solvent, so that the organic solvent component is not added in the preparation process, the whole preparation process is green and pollution-free, and the problem that the cost is increased due to the large-scale use of the organic solvent, which is unfavorable for industrial production, is solved.
Optionally, the method further comprises removing the solvent after adding the resin to obtain the nano zirconia dispersion liquid.
Preferably, the solvent is removed by evaporation.
In a third aspect, the present invention provides the use of the nano zirconia dispersion in the preparation of an optical film.
The application of the nano zirconia dispersion liquid in the preparation of the optical film provides dispersion liquid with good stability for the optical film, and the prepared optical film has good uniformity, and can greatly improve the refractive index of the optical film and the performance of the film.
The invention is further illustrated by the following specific examples and comparative examples, however, it should be understood that these examples are for the purpose of illustration only in greater detail and should not be construed as limiting the invention in any way. The raw materials used in the examples and comparative examples of the present invention were conducted under conventional conditions or conditions recommended by the manufacturer, without specifying the specific conditions. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
The embodiment provides a nano zirconia dispersion liquid, which specifically comprises the following steps:
1. firstly, preparing nano zirconia into an aqueous solution for later use.
2. Adding alpha-aminopropionic acid with 15% of nano zirconia mass and sodium abietate with 1% of nano zirconia mass serving as an emulsifier into water, wherein the addition amount of the water is 3 times of the mass of the alpha-aminopropionic acid and the sodium abietate, and uniformly dispersing the materials by using magnetic stirring for 20min to obtain a first solution.
3. And (3) adding the nano zirconium oxide aqueous solution obtained in the step (1) into the first solution for capping treatment, adding PBA into the obtained solution after the reaction is finished, and then removing solvent water by rotary evaporation to obtain PBA-type nano zirconium oxide dispersion.
Example 2
The present embodiment provides a nano zirconia dispersion, which is different from embodiment 1 in that the addition amount of sodium abietate in step 2 is 6% of the mass of nano zirconia, and the other raw materials and steps are the same as embodiment 1, and are not described herein.
Example 3
The present embodiment provides a nano zirconia dispersion, which is different from embodiment 1 in that the addition amount of sodium abietate in step 2 is 12% of the mass of nano zirconia, and the other raw materials and steps are the same as embodiment 1, and are not described here again.
Example 4
The present embodiment provides a nano zirconia dispersion, which is different from embodiment 2 in that the addition amount of α -aminopropionic acid in step 2 is 3% of the mass of nano zirconia, and the other raw materials and steps are the same as those in embodiment 2, and are not described herein.
Example 5
The present embodiment provides a nano zirconia dispersion, which is different from embodiment 2 in that the addition amount of α -aminopropionic acid in step 2 is 25% of the mass of nano zirconia, and the rest of the raw materials and steps are the same as those in embodiment 2, and are not described herein.
Example 6
The present embodiment provides a nano zirconia dispersion, which is different from embodiment 2 in that the capping agent in step 2 is phenylalanine, and the other raw materials and steps are the same as those in embodiment 2, and are not described herein.
Example 7
The present embodiment provides a nano zirconia dispersion, which is different from embodiment 2 in that the capping agent in step 2 is a-hydroxy- [1, 1-biphenyl ] -4-acetic acid, and the other raw materials and steps are the same as those in embodiment 2, and are not described herein.
Example 8
The present embodiment provides a nano zirconia dispersion, which is different from embodiment 2 in that the capping agent in step 2 is mandelic acid, and the other raw materials and steps are the same as those in embodiment 2, and are not described herein.
Example 9
The present embodiment provides a nano zirconia dispersion, which is different from embodiment 2 in that the emulsifier in step 2 is polyoxyethylene fatty amine, and the other raw materials and steps are the same as those in embodiment 2, and are not described herein.
Example 10
The present embodiment provides a nano zirconia dispersion, which is different from embodiment 2 in that the emulsifier in step 2 is diisooctyl sodium sulfosuccinate, and the other raw materials and steps are the same as those in embodiment 2, and are not described herein.
Example 11
The present embodiment provides a nano zirconia dispersion, which is different from embodiment 2 in that the emulsifier in step 2 is polyoxyethylene lauryl ether, and the other raw materials and steps are the same as those in embodiment 2, and are not described herein.
Example 12
The present embodiment provides a nano zirconia dispersion, which is different from embodiment 2 in that the resin in step 3 is BPMA, and the other raw materials and steps are the same as those in embodiment 2, and are not described herein.
Example 13
The present embodiment provides a nano zirconia dispersion, which is different from embodiment 2 in that the resin in step 3 is BZA, and the other raw materials and steps are the same as those in embodiment 2, and are not described herein.
Example 14
The difference between the nano zirconia dispersion liquid provided in this embodiment and embodiment 2 is that the resin in step 3 is OPPEA, and the other raw materials and steps are the same as those in embodiment 2, and are not described here again.
Example 15
The present embodiment provides a nano zirconia dispersion, unlike in embodiment 2, no emulsifier is added in step 2, and the rest of the raw materials and steps are the same as those in embodiment 2, and are not described here again.
Example 16
The present embodiment provides a nano zirconia dispersion, which is different from embodiment 2 in that the addition amount of α -aminopropionic acid in step 2 is 35% of the mass of nano zirconia, and the other raw materials and steps are the same as those in embodiment 2, and are not described herein.
Example 17
The present embodiment provides a nano zirconia dispersion, which is different from embodiment 2 in that the addition amount of sodium abietate in step 2 is 20% of the mass of nano zirconia, and the other raw materials and steps are the same as those in embodiment 2, and are not described herein.
Example 18
The present example provides a nano zirconia resin dispersion, which is different from example 17 in that the amount of α -aminopropionic acid added in step 2 is 35% of the mass of nano zirconia, and the other raw materials and steps are the same as those in example 17, and are not described here again.
Comparative example 1
This comparative example provides a nano zirconia resin type dispersion, which is different from example 2 in that α -aminopropionic acid is replaced with propionic acid, and the other raw materials and steps are the same as those of example 2, and are not described here again.
Comparative example 2
This comparative example provides a nano zirconia resin dispersion, unlike example 2, in which no α -aminopropionic acid was added, the remaining raw materials and steps are the same as example 2, and no detailed description is given here.
Test examples
The stability index measurements were carried out on the nano zirconia dispersions obtained in examples 1 to 18 and comparative examples 1 to 2.
Standing conditions: and standing for 12 months at normal temperature in dark place.
As can be seen from the formula (1), when the dispersion stability index was 1, that is, the transmittance of the dispersion at 725nm was not changed before and after standing, that is, the dispersion stability was excellent, a larger dispersion stability index indicates a poorer dispersion stability.
The stability index obtained by the test is shown in table 1.
TABLE 1 stability index data table for dispersions
| Concentration/wt.% | Dispersion stability index | |
| Example 1 | 60wt.％ | 1.17 |
| Example 2 | 60wt.％ | 1.02 |
| Example 3 | 60wt.％ | 1.08 |
| Example 4 | 60wt.％ | 1.2 |
| Example 5 | 60wt.％ | 1.1 |
| Example 6 | 60wt.％ | 1.06 |
| Example 7 | 60wt.％ | 1.15 |
| Example 8 | 60wt.％ | 1.08 |
| Example 9 | 60wt.％ | 1.06 |
| Example 10 | 60wt.％ | 1.13 |
| Example 11 | 60wt.％ | 1.1 |
| Example 12 | 60wt.％ | 1.03 |
| Example 13 | 60wt.％ | 1.03 |
| Example 14 | 60wt.％ | 1.04 |
| Example 15 | 60wt.％ | 1.32 |
| Example 16 | 60wt.％ | 1.31 |
| Example 17 | 60wt.％ | 1.34 |
| Example 18 | 60wt.％ | 1.42 |
| Comparative example 1 | 60wt.％ | 1.36 |
| Comparative example 2 | 60wt.％ | - |
As can be seen from table 1, in example 2, compared with comparative example 1, the capping agent propionic acid in comparative example 1 does not contain an electron donor group, and its resin type dispersion stability index is 1.36, which is much higher than the corresponding parameter (1.02) in example 2, indicating that the introduction of the electron donor group can increase the repulsive force between particles, playing an important role in maintaining the dispersion stability. In example 15 and comparative example 2, the stability index of the resin type dispersion was inferior to that of example 2 without adding the emulsifier and the capping agent, respectively, and the PBA type dispersion prepared in comparative example 2 even exhibited the phenomenon of zirconia precipitation, which suggests that the capping agent and the emulsifier have a synergistic effect in maintaining the stability of the dispersion. In addition, the content of capping agent and emulsifier has a great influence on achieving dispersion stability and dispersion preparation, and the amount should be controlled in a reasonable range, otherwise the opposite effect is achieved, and the cost is increased, which is fully demonstrated in examples 1,2 and 3, examples 2, 4 and 5, and examples 16, 17 and 18. Meanwhile, in examples 2, 6, 7, 8, the stability index of the PBA-type dispersion liquid was greatly different due to the difference in the types of capping agents, which suggests that the difference in the structures of the different capping agents resulted in the difference in the influence of the electron donor groups thereof on the structure of the electric double layer, so that the stability of the dispersion liquid was also different. Similarly, in examples 2, 9, 10, 11, there was a large difference in the stability index of the PBA-type dispersion due to the difference in the types of the emulsifiers, which indicated that the different emulsifiers were different in the ability to improve the stability of the dispersion.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (11)
1. The nanometer zirconia dispersion liquid is characterized by comprising nanometer zirconia, resin, an emulsifying agent and a capping agent;
the addition amount of the emulsifier is 1-12% of the mass of the nano zirconia; the addition amount of the capping agent is 3% -25% of the mass of the nano zirconia;
the resin is at least one of biphenyl methyl alcohol acrylic ester, benzyl acrylic ester or o-phenyl phenoxyethyl acrylic ester;
the structure of the capping agent is as follows:
；
wherein R is selected from C 1 -C 20 Substituted or unsubstituted alkyl, C 1 -C 20 At least one of a substituted or unsubstituted alkoxy group, a substituted or unsubstituted aromatic ring, a substituted or unsubstituted double bond, and a substituted or unsubstituted cycloalkyl group;
x is an amino group; y is carboxyl.
2. The nano zirconia dispersion according to claim 1, wherein R is selected from C 1 -C 12 Substituted or unsubstituted alkyl, C 1 -C 12 At least one of a substituted or unsubstituted alkoxy group, a substituted or unsubstituted aromatic ring, a substituted or unsubstituted double bond, and a substituted or unsubstituted cycloalkyl group.
3. The nano zirconia dispersion according to claim 1, wherein R is selected from C 1 -C 4 Substituted or unsubstituted alkyl, C 1 -C 4 At least one of a substituted or unsubstituted alkoxy group, a substituted or unsubstituted aromatic ring, a substituted or unsubstituted double bond, and a substituted or unsubstituted cycloalkyl group.
4. The nano zirconia dispersion according to claim 1, wherein the particle size of the nano zirconia is 1nm to 40nm.
5. The nano zirconia dispersion according to claim 1, wherein the content of the nano zirconia is 50wt.% to 70wt.%.
6. The nano-zirconia dispersion according to claim 1, wherein the emulsifier comprises at least one of polyoxyethylene fatty amine, sodium abietate, diisooctyl sodium sulfosuccinate, polyoxyethylene lauryl ether.
7. A method for preparing the nano zirconia dispersion according to any one of claims 1 to 6, comprising the steps of: preparing a first solution from a capping agent and an emulsifying agent, adding a nano zirconia solution into the first solution, and finally adding resin to obtain the nano zirconia dispersion liquid.
8. The method of preparing according to claim 7, wherein the solvent of the first solution comprises water;
the solvent of the nano zirconia solution comprises water.
9. The method of claim 7, further comprising removing the solvent after adding the resin to obtain the nano zirconia dispersion.
10. The method of claim 9, wherein the solvent is removed by evaporation.
11. Use of the nano zirconia dispersion according to any one of claims 1 to 6 or the nano zirconia dispersion prepared by the preparation method according to any one of claims 7 to 10 for preparing an optical film.
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| CN114249956A (en) * | 2020-09-24 | 2022-03-29 | 凯斯科技股份有限公司 | Surface-modified metal oxide nanoparticle dispersion composition, method for producing same, film composition, and optical film |
| CN113773691A (en) * | 2021-09-13 | 2021-12-10 | 山东国瓷功能材料股份有限公司 | Nano zirconium oxide dispersion liquid, preparation method thereof, monomer dispersion liquid and optical film |
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