CN114605762A - Nano zirconium oxide dispersion liquid, preparation method and application - Google Patents
Nano zirconium oxide dispersion liquid, preparation method and application Download PDFInfo
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- CN114605762A CN114605762A CN202210422098.4A CN202210422098A CN114605762A CN 114605762 A CN114605762 A CN 114605762A CN 202210422098 A CN202210422098 A CN 202210422098A CN 114605762 A CN114605762 A CN 114605762A
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- nano zirconia
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- 239000007788 liquid Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 title description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 240
- 239000006185 dispersion Substances 0.000 claims abstract description 106
- -1 acryloyloxy Chemical group 0.000 claims abstract description 51
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 31
- 239000011347 resin Substances 0.000 claims abstract description 29
- 229920005989 resin Polymers 0.000 claims abstract description 29
- 239000002245 particle Substances 0.000 claims abstract description 23
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 19
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 14
- 125000003545 alkoxy group Chemical group 0.000 claims abstract description 12
- 125000003118 aryl group Chemical group 0.000 claims abstract description 12
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims abstract description 12
- 125000000753 cycloalkyl group Chemical group 0.000 claims abstract description 10
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 claims abstract description 10
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 8
- KIQKWYUGPPFMBV-UHFFFAOYSA-N diisocyanatomethane Chemical compound O=C=NCN=C=O KIQKWYUGPPFMBV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 5
- 239000001257 hydrogen Substances 0.000 claims abstract description 5
- 239000003995 emulsifying agent Substances 0.000 claims description 25
- 239000002904 solvent Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 13
- 239000012788 optical film Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 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 9
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims 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 claims description 5
- GCTPMLUUWLLESL-UHFFFAOYSA-N benzyl prop-2-enoate Chemical compound C=CC(=O)OCC1=CC=CC=C1 GCTPMLUUWLLESL-UHFFFAOYSA-N 0.000 claims description 5
- 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 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- 150000001412 amines Chemical class 0.000 claims description 4
- HWQXBVHZYDELQG-UHFFFAOYSA-L disodium 2,2-bis(6-methylheptyl)-3-sulfobutanedioate Chemical compound C(CCCCC(C)C)C(C(C(=O)[O-])S(=O)(=O)O)(C(=O)[O-])CCCCCC(C)C.[Na+].[Na+] HWQXBVHZYDELQG-UHFFFAOYSA-L 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
- 125000000542 sulfonic acid group Chemical group 0.000 claims description 2
- 125000003277 amino group Chemical group 0.000 abstract description 6
- 230000003287 optical effect Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 description 20
- 239000000243 solution Substances 0.000 description 18
- 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 9
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 description 9
- 239000003960 organic solvent Substances 0.000 description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 238000013459 approach Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000000694 effects 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
- 230000008569 process Effects 0.000 description 3
- LLAPDLPYIYKTGQ-UHFFFAOYSA-N 1-aminoethyl Chemical group C[CH]N LLAPDLPYIYKTGQ-UHFFFAOYSA-N 0.000 description 2
- 125000004423 acyloxy group Chemical group 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
- 125000003710 aryl alkyl group Chemical group 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
- 238000003912 environmental pollution Methods 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
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 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
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 description 2
- 238000001556 precipitation Methods 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
- 230000002195 synergetic effect Effects 0.000 description 2
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 125000003396 thiol group Chemical group [H]S* 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
- 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
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 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
- 230000002411 adverse Effects 0.000 description 1
- 125000005370 alkoxysilyl group Chemical group 0.000 description 1
- 125000005103 alkyl silyl group Chemical group 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 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
- 230000008859 change Effects 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
- 238000013329 compounding Methods 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
- 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
- 239000003292 glue 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
- 230000006872 improvement Effects 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
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 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
- 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
- 150000003254 radicals Chemical class 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
- 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, and relates to the technical field of optical resin. The nano zirconia dispersion liquid comprises nano zirconia, resin and a capping agent, wherein the R structure in the capping agent is selected from at least one of alkyl, alkoxy, carbonyl, acryloyloxy, aromatic ring, double bond, cycloalkyl, methylene, isocyanate, sulfydryl, amino, carboxyl and hydroxyl; x is at least one selected from the group consisting of amine group, hydroxyl group and siloxy group; the structure of Y is at least one selected from hydrogen, carboxyl, hydroxyl, sulfonic group, phosphoric group and siloxy. According to the nano-zirconia dispersion liquid provided by the invention, the capping agent introduces the electron donor group to the surface of the nano-zirconia, so that the thickness of an electric double layer around the nano-zirconia particles is increased, the repulsive force among the particles is increased, and the stability of the nano-zirconia dispersion liquid is improved. The dispersion stability index of the nano zirconia dispersion is less than 1.2 after the nano zirconia dispersion is kept stand for 12 months under the condition of normal temperature and light shielding, and the nano zirconia dispersion has better stability.
Description
Technical Field
The invention relates to the technical field of optical resin, in particular to a nano zirconia dispersion liquid, a preparation method and application.
Background
In recent years, a resin-type zirconia dispersion obtained by combining a zirconia particle dispersion with a transparent resin or film has been used favorably in the optical field. Optical films such as brightness enhancement films prepared from zirconia resin type dispersions can be used in LCD displays to increase the brightness and clarity of the screen.
To enable the zirconia nanoparticles to be dispersed in a resin matrix or used in a fully formulated composition, one approach is a solventless approach, reducing the zirconia powder aggregate particle size, surface treating it, and compounding into the resin by a mechanical grinding process (e.g., milling) without the aid of a solvent. Although this method avoids the use of a solvent, the agglomeration of particles is serious and the stability of the dispersion does not achieve the desired effect.
Another method is an organic solvent-based method in which an organic solvent (usually a water-miscible solvent) is mixed with water at a certain ratio, the particles are treated, and then the water and the organic solvent are removed to obtain a resin-based zirconia dispersion, which has advantages in terms of dispersibility of the particles as compared with the solvent-free method, but has problems of poor dispersion stability of the dispersion, such as poor light transmittance of the zirconia dispersion, turbidity of the system, and even precipitation of small zirconia particles when UV glue is prepared, and furthermore, the use of a large amount of the organic solvent entails environmental pollution and harm to human body, and is disadvantageous in terms of cost reduction and mass production.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
One of the purposes of the invention is to provide a nano zirconia dispersion liquid to relieve 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 purpose of the present invention, the following technical solutions are adopted:
the first aspect of the invention provides a nano zirconia dispersion liquid, which comprises nano zirconia, resin and a capping agent;
the structure of the capping agent is as follows:
wherein R is selected from C1-C20Substituted or unsubstituted alkyl, C1-C20At least one of substituted or unsubstituted alkoxy, carbonyl, substituted or unsubstituted acryloyloxy, substituted or unsubstituted aromatic ring, substituted or unsubstituted double bond, substituted or unsubstituted cycloalkyl, methylene, isocyanate group, mercapto, amino, carboxyl and hydroxyl.
X is at least one selected from amine group, hydroxyl group and substituted or unsubstituted siloxy group.
Y is at least one selected from the group consisting of hydrogen, carboxyl, hydroxyl, sulfonic acid group, phosphoric acid group and substituted or unsubstituted siloxy group.
Alternatively, R is selected from C1-C12Substituted or unsubstituted alkyl, C1-C12At least one of substituted or unsubstituted alkoxy, carbonyl, substituted or unsubstituted acryloyloxy, substituted or unsubstituted aromatic ring, substituted or unsubstituted double bond, substituted or unsubstituted cycloalkyl, methylene, isocyanate group, mercapto, amino, carboxyl and hydroxyl.
Preferably, R is selected from C1-C4Substituted or unsubstituted alkyl, C1-C4Substituted or unsubstituted alkoxy, carbonyl, substituted or unsubstituted acryloyloxy, substituted or unsubstituted aromatic ring, substituted or unsubstituted alkoxy, carbonyl, substituted or unsubstituted acyloxy group, carbonyl, or substituted or unsubstituted acyloxy group,At least one of 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 nano zirconia has a particle size of 1-40 nm.
Preferably, the content of the nano zirconia is 50 wt.% to 70 wt.%.
Optionally, an emulsifier is also included.
Preferably, the emulsifier comprises at least one of polyoxyethylene fatty amine, sodium abietate, sodium diisooctyl sulfosuccinate and polyoxyethylene lauryl ether.
Optionally, the addition amount of the emulsifier is 1% -12% of the mass of the nano zirconia.
The second aspect of the present invention provides a method for preparing a nano zirconia dispersion, comprising the steps of: preparing a capping agent and an optional emulsifier into a first solution, adding a nano zirconia solution into the first solution, and finally adding resin to obtain the nano zirconia dispersion liquid.
Optionally, the resin comprises at least one of phenoxybenzyl acrylate, biphenylcarbinol acrylate, benzyl acrylate, or o-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 obtaining the nano zirconia dispersion liquid after adding a resin to remove the solvent.
Preferably, the solvent is removed by evaporation.
The third aspect of the invention provides an application of the nano zirconia dispersion liquid in preparing an optical film.
Compared with the prior art, the invention has at least the following beneficial effects:
according to the nano-zirconia dispersion liquid provided by the invention, the capping agent introduces the electron donor group to the surface of the nano-zirconia, so that the thickness of an electric double layer around the nano-zirconia particles is increased, the repulsive force among the particles is increased, and the stability of the nano-zirconia dispersion liquid is improved. The dispersion stability index of the nano zirconia dispersion is less than 1.2 after the nano zirconia dispersion is kept stand for 12 months under the condition of normal temperature and light shielding, and the nano zirconia dispersion has better 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 dispersion equipment and capability of preparing the high-stability zirconia dispersion liquid.
The application of the nano-zirconia dispersion liquid in preparing the optical film provided by the invention provides the dispersion liquid with better stability for the optical film, the prepared optical film has better uniformity, the refractive index of the optical film can be greatly improved, and the performance of the film is improved.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to embodiments and examples, but those skilled in the art will understand that the following embodiments and examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first aspect of the invention provides a nano zirconia dispersion liquid, which comprises nano zirconia, resin and a capping agent;
the structure of the capping agent is as follows:
wherein R is selected from C1-C20Substituted or unsubstituted alkyl, C1-C20At least one of substituted or unsubstituted alkoxy, carbonyl, substituted or unsubstituted acryloyloxy, substituted or unsubstituted aromatic ring, substituted or unsubstituted double bond, substituted or unsubstituted cycloalkyl, methylene, isocyanate group, mercapto, amino, carboxyl and hydroxyl;
x is at least one selected from amino, hydroxyl and substituted or unsubstituted siloxy;
y is at least one selected from hydrogen, carboxyl, hydroxyl, sulfonic group, phosphoric group and substituted or unsubstituted siloxy.
From DLVO double-layer theory, it is known that when two charged zirconia particles approach each other, the electric double layers around the particles overlap each other, the electric double layers deform, repulsion occurs between the particles, and van der waals attractive force also exists between the two particles. Therefore, the X structure in the capping agent of the invention introduces an electron donor group into the zirconia to increase the thickness of double electric layers around the particles and increase the repulsive force between the particles, thereby improving the stability of the zirconia dispersion.
According to the nano-zirconia dispersion liquid provided by the invention, the capping agent introduces the electron donor group to the surface of the nano-zirconia, so that the thickness of an electric double layer around the nano-zirconia particles is increased, the repulsive force between the particles is increased, and the stability of the nano-zirconia dispersion liquid is improved. The dispersion stability index of the nano zirconia dispersion is less than 1.2 after the nano zirconia dispersion is kept stand for 12 months under the condition of normal temperature and light shielding, and the nano zirconia dispersion has better stability.
In some embodiments of the invention, C1-C20Substituted or unsubstituted alkyl groups, suitable short radicals include straight, branched or cyclic alkyl, alkenyl, aryl and aralkyl groups. Specific 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 radicals, e.g. methoxy, ethoxyAnd (iso) propoxy group: halogen atoms such as fluorine, chlorine, bromine and iodine; a cyano group; an amino group; c6-C18Aryl groups such as phenyl and tolyl; c7-C18Aralkyl groups such as benzyl and phenethyl; an ester group; an ether group; an acyl group; a thioether group; alkylsilyl groups, and alkoxysilyl groups, and combinations of the foregoing.
In some embodiments of the invention, C1-C20The substituted or unsubstituted alkoxy group 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-trichloropropyl, bromomethyl, 1-bromoethyl, 2-bromoisobutyl, 1, 2-dibromoethyl, 1, 3-dibromoisopropyl, 2, 3-dibromotert-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 present 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 groups of the present invention, the substituent is typically, but not limited to, a halogen, a benzene ring, an alkyl group, a hydroxyl group, or a carboxyl group.
Alternatively, R is selected from C1-C12Substituted or unsubstituted alkyl, C1-C12At least one of substituted or unsubstituted alkoxy, carbonyl, substituted or unsubstituted acryloyloxy, substituted or unsubstituted aromatic ring, substituted or unsubstituted double bond, substituted or unsubstituted cycloalkyl, methylene, isocyanate group, mercapto, amino, carboxyl and hydroxyl.
Preferably, R is selected from C1-C4Substituted or unsubstituted alkyl, C1-C4At 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 improvement 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 nano zirconia has a particle size of 1nm to 40 nm.
Preferably, the content of the nano zirconia is 50 wt.% to 70 wt.%.
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 the nano zirconia is higher than 70 wt.%, the stability of the nano zirconia dispersion is negatively affected.
Optionally, an emulsifier is also included.
In some embodiments of the present invention, an amount of emulsifier is added to the system, and the stability of the zirconia resin dispersion is further improved by utilizing the synergistic effect between the capping agent and the emulsifier.
Preferably, the emulsifier comprises at least one of polyoxyethylene fatty amine, sodium abietate, sodium diisooctyl 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 present 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.
The second aspect of 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 dispersion equipment and capability of preparing the high-stability zirconia dispersion liquid.
Optionally, the resin comprises at least one of phenoxybenzyl acrylate, biphenylcarbinol acrylate, benzyl acrylate, or o-phenylphenoxyethyl acrylate.
In some embodiments of the invention, the resin is typically, but not limited to, phenoxybenzyl acrylate, biphenylcarbinol acrylate, benzyl acrylate, or o-phenylphenoxyethyl acrylate.
In the above-mentioned resins, phenoxybenzyl acrylate is abbreviated as PBA, biphenylcarbinol acrylate is abbreviated as BPMA, benzyl acrylate is abbreviated as BZA, and orthophenylphenoxyethyl acrylate is abbreviated as OPPEA.
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 the solvent, so that no organic solvent component is 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 use of the organic solvent, which is not beneficial to 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.
The third aspect of the invention provides an application of the nano zirconia dispersion liquid in preparing an optical film.
The application of the nano-zirconia dispersion liquid in preparing the optical film provided by the invention provides the dispersion liquid with better stability for the optical film, the prepared optical film has better uniformity, the refractive index of the optical film can be greatly improved, and the performance of the film is improved.
The invention is further illustrated by the following specific examples and comparative examples, but it should be understood that these examples are for purposes of illustration only and are not to be construed as limiting the invention in any way. The raw materials used in the examples and comparative examples of the present invention, those having no particular reference to conditions, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
The embodiment provides a nano zirconia dispersion liquid, which specifically comprises the following steps:
1. firstly, preparing the nano zirconia into aqueous solution for later use.
2. Adding alpha-aminopropionic acid accounting for 15% of the mass of the nano zirconia and emulsifier sodium abietate accounting for 1% of the mass of the nano zirconia 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 alpha-aminopropionic acid and the sodium abietate by 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 performing rotary evaporation to remove solvent water to obtain a PBA type nano zirconium oxide dispersion.
Example 2
The present example provides a nano zirconia dispersion, which is different from example 1 in that the addition amount of sodium abietate in step 2 is 6% of the mass of the nano zirconia, and the remaining raw materials and steps are the same as those in example 1, and are not described herein again.
Example 3
The present example provides a nano zirconia dispersion, which is different from example 1 in that the addition amount of sodium abietate in step 2 is 12% of the mass of the nano zirconia, and the remaining raw materials and steps are the same as those in example 1, and are not described herein again.
Example 4
This example provides a nano zirconia dispersion, which is different from example 2 in that the addition amount of the α -aminopropionic acid in step 2 is 3% of the mass of the nano zirconia, and the remaining raw materials and steps are the same as those in example 2, and are not described again here.
Example 5
This example provides a nano zirconia dispersion, which is different from example 2 in that the addition amount of the α -aminopropionic acid in step 2 is 25% of the mass of the nano zirconia, and the remaining raw materials and steps are the same as those in example 2, and are not described again here.
Example 6
This example provides a nano zirconia dispersion, which is different from example 2 in that the capping agent in step 2 is phenylalanine, and the rest of the raw materials and steps are the same as those in example 2, and are not described herein again.
Example 7
This example provides a nano zirconia dispersion, which is different from example 2 in that the capping agent in step 2 is a-hydroxy- [1, 1-biphenyl ] -4-acetic acid, and the rest of the raw materials and steps are the same as those in example 2, and are not described herein again.
Example 8
This example provides a nano zirconia dispersion, which is different from example 2 in that the capping agent in step 2 is mandelic acid, and the rest of the raw materials and steps are the same as those in example 2, and are not described herein again.
Example 9
This example provides a nano zirconia dispersion, which is different from example 2 in that the emulsifier in step 2 is polyoxyethylene fatty amine, and the rest of the raw materials and steps are the same as those in example 2, and are not described again here.
Example 10
The present embodiment provides a nano zirconia dispersion, which is different from embodiment 2 in that the emulsifier in step 2 is sodium diisooctyl sulfosuccinate, and the remaining raw materials and steps are the same as those in embodiment 2, and are not described herein again.
Example 11
This example provides a nano zirconia dispersion, which is different from example 2 in that the emulsifier in step 2 is polyoxyethylene lauryl ether, and the rest of the raw materials and steps are the same as those in example 2, and are not described again here.
Example 12
This example provides a nano zirconia dispersion, which is different from example 2 in that the resin in step 3 is BPMA, and the rest of the raw materials and steps are the same as those in example 2, and are not repeated herein.
Example 13
This example provides a nano zirconia dispersion, which is different from example 2 in that the resin in step 3 is BZA, and the rest of the raw materials and steps are the same as those in example 2, and are not repeated herein.
Example 14
This example provides a nano zirconia dispersion, which is different from example 2 in that the resin in step 3 is OPPEA, and the rest of the raw materials and steps are the same as those in example 2, and are not described herein again.
Example 15
This example provides a nano zirconia dispersion, which is different from example 2 in that an emulsifier is not added in step 2, and the rest of the raw materials and steps are the same as those in example 2, and are not described herein again.
Example 16
This example provides a nano zirconia dispersion, which is different from example 2 in that the addition amount of the α -aminopropionic acid in step 2 is 35% of the mass of the nano zirconia, and the remaining raw materials and steps are the same as those in example 2, and are not described again here.
Example 17
The present example provides a nano zirconia dispersion, which is different from example 2 in that the addition amount of sodium abietate in step 2 is 20% of the mass of the nano zirconia, and the remaining raw materials and steps are the same as those in example 2, and are not described herein again.
Example 18
This 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% by mass of the nano zirconia, and the remaining raw materials and steps are the same as those in example 17 and are not described 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 was replaced with propionic acid, and the remaining raw materials and steps were the same as in example 2 and will not be described again.
Comparative example 2
This comparative example provides a nano zirconia resin-type dispersion, which is different from example 2 in that no α -aminopropionic acid was added, and the remaining raw materials and steps were the same as in example 2, and thus, detailed description thereof is omitted.
Test examples
The nano zirconia dispersions obtained in examples 1 to 18 and comparative examples 1 to 2 were subjected to stability index measurement.
Standing conditions are as follows: standing at normal temperature in dark for 12 months.
As can be seen from formula (1), when the dispersion stability index is 1, i.e., the transmittance of the dispersion at 725nm does not change before and after standing, i.e., the dispersion stability is excellent, the larger the dispersion stability index is, the worse the dispersion stability is.
The stability index obtained from the test is shown in table 1.
TABLE 1 dispersion stability index data Table
| Concentration/wt. -%) | Stability index of dispersion | |
| 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, in comparison with comparative example 1, the capping agent propionic acid in comparative example 1 does not contain an electron donor group, and the resin type dispersion stability index is 1.36, which is much higher than the corresponding parameter (1.02) in example 2, which shows that the introduction of the electron donor group can increase the repulsion between particles, and plays 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, in which the PBA type dispersion prepared in comparative example 2 even showed zirconia precipitation, indicating that the capping agent and the emulsifier have a synergistic effect in maintaining the stability of the dispersion. In addition, the content of the capping agent and the emulsifier has a great influence on the stability of the dispersion and the preparation process of the dispersion, and the amount thereof should be controlled within a reasonable range, otherwise the adverse effect is caused, and the cost is also increased, which is fully demonstrated in examples 1,2 and 3, and examples 2, 4 and 5, and examples 16, 17 and 18. Meanwhile, in examples 2, 6, 7, and 8, the stability indexes of the PBA type dispersions were greatly different depending on the types of capping agents, which indicates that the stability of the dispersions was different since the influence of the electron donor group on the electric double layer structure was different depending on the structure of different capping agents. Similarly, in examples 2, 9, 10, 11, the stability indices of the PBA type dispersions were greatly different due to the different types of emulsifiers, which indicates that the different emulsifiers also have different abilities to improve the stability of the dispersions.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A nano zirconia dispersion is characterized by comprising nano zirconia, resin and a capping agent;
the structure of the capping agent is as follows:
wherein R is selected from C1-C20Substituted or unsubstituted alkyl, C1-C20At least one of substituted or unsubstituted alkoxy, carbonyl, substituted or unsubstituted acryloyloxy, substituted or unsubstituted aromatic ring, substituted or unsubstituted double bond, substituted or unsubstituted cycloalkyl, methylene, isocyanate group, mercapto, amino, carboxyl and hydroxyl;
x is at least one selected from amino, hydroxyl and substituted or unsubstituted siloxy;
y is at least one selected from the group consisting of hydrogen, carboxyl, hydroxyl, sulfonic acid group, phosphoric acid group, substituted and unsubstituted siloxy group.
2. According toThe nano zirconia dispersion of claim 1 wherein R is selected from C1-C12Substituted or unsubstituted alkyl, C1-C12At least one of substituted or unsubstituted alkoxy, carbonyl, substituted or unsubstituted acryloyloxy, substituted or unsubstituted aromatic ring, substituted or unsubstituted double bond, substituted or unsubstituted cycloalkyl, methylene, isocyanate group, mercapto, amino, carboxyl and hydroxyl;
preferably, R is selected from C1-C4Substituted or unsubstituted alkyl, C1-C4At least one of substituted or unsubstituted alkoxy, carbonyl, substituted or unsubstituted acryloyloxy, substituted or unsubstituted aromatic ring, substituted or unsubstituted double bond, substituted or unsubstituted cycloalkyl, methylene, isocyanate group, mercapto, amino, carboxyl and hydroxyl.
3. The nano zirconia dispersion liquid according to claim 1, wherein the addition amount of the capping agent is 3 to 25% by mass of the nano zirconia.
4. The nano zirconia dispersion of claim 1 wherein the nano zirconia has a particle size of 1nm to 40 nm;
preferably, the content of the nano zirconia is 50 wt.% to 70 wt.%.
5. The nano zirconia dispersion of claim 1 further comprising an emulsifier;
preferably, the emulsifier comprises at least one of polyoxyethylene fatty amine, sodium abietate, sodium diisooctyl sulfosuccinate and polyoxyethylene lauryl ether.
6. The nano zirconia dispersion liquid according to claim 5, wherein the amount of the emulsifier added is 1 to 12% by mass of the nano zirconia.
7. A method for preparing the nano zirconia dispersion liquid according to any one of claims 1 to 6, 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.
8. The method of claim 7, wherein the resin comprises at least one of phenoxybenzyl acrylate, biphenylcarbinol acrylate, benzyl acrylate, or o-phenylphenoxyethyl acrylate;
preferably, the solvent of the first solution comprises water;
preferably, the solvent of the nano zirconia solution comprises water.
9. The preparation method according to claim 7, further comprising removing the solvent after adding the resin to obtain the nano zirconia dispersion liquid;
preferably, the solvent is removed by evaporation.
10. Use of the nano zirconia dispersion liquid according to any one of claims 1 to 6 or the nano zirconia dispersion liquid prepared by the preparation method according to any one of claims 7 to 9 in the preparation of an optical film.
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| CN107406530A (en) * | 2015-02-25 | 2017-11-28 | Dic株式会社 | Solidification compound and its solidfied material and optical component |
| 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 |
| 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 |
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| JP2009067949A (en) * | 2007-09-14 | 2009-04-02 | Nippon Shokubai Co Ltd | Resin composition |
| CN107001067A (en) * | 2014-12-12 | 2017-08-01 | Dic株式会社 | The manufacture method of inorganic microparticle-dispersed liquid, solidification compound and its solidfied material comprising the dispersion liquid |
| CN107406530A (en) * | 2015-02-25 | 2017-11-28 | Dic株式会社 | Solidification compound and its solidfied material and optical component |
| 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 |
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