CN102504614B - Organic modified silica sol - Google Patents
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- CN102504614B CN102504614B CN201110361396.9A CN201110361396A CN102504614B CN 102504614 B CN102504614 B CN 102504614B CN 201110361396 A CN201110361396 A CN 201110361396A CN 102504614 B CN102504614 B CN 102504614B
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- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical class O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 4
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 22
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims description 22
- 229940043265 methyl isobutyl ketone Drugs 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- -1 trifluoro propyl octyl group Chemical group 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 17
- 239000006185 dispersion Substances 0.000 claims description 17
- 229910052710 silicon Inorganic materials 0.000 claims description 17
- 239000010703 silicon Substances 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 11
- 238000009413 insulation Methods 0.000 claims description 6
- YQGOWXYZDLJBFL-UHFFFAOYSA-N dimethoxysilane Chemical compound CO[SiH2]OC YQGOWXYZDLJBFL-UHFFFAOYSA-N 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 4
- 230000006837 decompression Effects 0.000 claims description 4
- GAURFLBIDLSLQU-UHFFFAOYSA-N diethoxy(methyl)silicon Chemical compound CCO[Si](C)OCC GAURFLBIDLSLQU-UHFFFAOYSA-N 0.000 claims description 3
- 238000005374 membrane filtration Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 15
- 238000000576 coating method Methods 0.000 abstract description 13
- 239000003960 organic solvent Substances 0.000 abstract description 11
- 229920005989 resin Polymers 0.000 abstract description 9
- 239000011347 resin Substances 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 7
- 239000000377 silicon dioxide Substances 0.000 abstract description 5
- 239000007888 film coating Substances 0.000 abstract description 4
- 238000009501 film coating Methods 0.000 abstract description 4
- 239000008187 granular material Substances 0.000 abstract description 4
- 239000005871 repellent Substances 0.000 abstract 2
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 24
- 239000000243 solution Substances 0.000 description 14
- 239000011248 coating agent Substances 0.000 description 11
- 238000000034 method Methods 0.000 description 11
- 150000001335 aliphatic alkanes Chemical class 0.000 description 10
- 239000003921 oil Substances 0.000 description 9
- 239000002904 solvent Substances 0.000 description 8
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 description 7
- 239000012530 fluid Substances 0.000 description 7
- 239000007822 coupling agent Substances 0.000 description 6
- 125000004432 carbon atom Chemical group C* 0.000 description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 150000004703 alkoxides Chemical class 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- PKTOVQRKCNPVKY-UHFFFAOYSA-N dimethoxy(methyl)silicon Chemical compound CO[Si](C)OC PKTOVQRKCNPVKY-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- GFTRQZRJGBJAKX-UHFFFAOYSA-N ethoxy-methyl-propyl-(2,2,2-trifluoroethoxy)silane Chemical compound FC(CO[Si](OCC)(C)CCC)(F)F GFTRQZRJGBJAKX-UHFFFAOYSA-N 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical group CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 125000000962 organic group Chemical group 0.000 description 2
- PXFBZOLANLWPMH-UHFFFAOYSA-N 16-Epiaffinine Natural products C1C(C2=CC=CC=C2N2)=C2C(=O)CC2C(=CC)CN(C)C1C2CO PXFBZOLANLWPMH-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- YEYKMVJDLWJFOA-UHFFFAOYSA-N 2-propoxyethanol Chemical compound CCCOCCO YEYKMVJDLWJFOA-UHFFFAOYSA-N 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- MUXOBHXGJLMRAB-UHFFFAOYSA-N Dimethyl succinate Chemical class COC(=O)CCC(=O)OC MUXOBHXGJLMRAB-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- APZPSKFMSWZPKL-UHFFFAOYSA-N [3-hydroxy-2,2-bis(hydroxymethyl)propyl] 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC(CO)(CO)CO APZPSKFMSWZPKL-UHFFFAOYSA-N 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 125000005376 alkyl siloxane group Chemical group 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000012769 display material Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 238000009998 heat setting Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000005495 investment casting Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- GOWYWDDPOBCVFH-UHFFFAOYSA-N methoxy-methyl-propyl-(trifluoromethoxy)silane Chemical compound FC(O[Si](OC)(C)CCC)(F)F GOWYWDDPOBCVFH-UHFFFAOYSA-N 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
- Silicon Compounds (AREA)
Abstract
Organic modified silica sol comprises the following components by mass percent: 17 to 22 percent of silica granules, 63 to 82.5 percent of organic solvent, and 0.5 to 15 percent of modifying agent. The organic modified silica sol has an appropriate average particle diameter, is clear and transparent in appearance and excellent in stability, has excellent dispersivity and stability in the hard film coating liquid of a resin system, can eliminate disadvantages of various related coatings, and meanwhile has excellent water-repellent and oil-repellent properties.
Description
Technical field
The present invention relates to a kind of silicon sol of modification.
Background technology
SiO
2colloidal sol is polymer amorphous Si O
2the colloidal solution of microparticulate in solvent.Owing to having special character, silicon sol is widely used in fields such as fiber, fabric, papermaking, coating, caking agent, pottery, medicine, precision castings.
Silicon sol can be divided into water silica sol and organic solvent silicasol according to the difference of solvent property, and organic solvent silicasol is mainly used in forming the hard coat film of the molding synthetic resin surfaces such as lens, bottle, film, sheet.The surface coatings of these series products such as liquid crystal display material, eyeglass and electrical apparatus product not only requires high adhesion strength also should have the characteristic of water and oil repellant, and the product therefore with the organic solvent silicasol of special purpose arises at the historic moment.
This class transparency cured film will add silicon sol conventionally in order to reach good performance in Special Resin film forming curing system, and surface exists the silicon oxide particle of hydroxyl can to assemble because of the effect of hydroxyl in resin system, cause film performance inequality, there will be many coating disadvantages simultaneously.By the SiO to organic solvent silicasol
2the suitable organic group of microparticle surfaces grafting just can be eliminated the various bad phenomenon that general silicon sol occurs in resin system.
Japanese Patent TOHKEMY 2004091220 discloses the synthetic silicon sol of tetraethoxy (TEOS) the alcoholysis method siloxanes coupling agent that contains single or multiple alkane has been carried out to the organic solvent type silicon sol that modification obtains, and has good storage stability but it does not have the characteristic of water and oil repellant.
In the disclosed technology of WO03/102089, use the class coating material that contains the coupling agent modified organic silicon sol of single fluorohydrocarbon type siloxane, due to the water and oil repellant characteristic of its modified group can cause with mixed with resin after solution package stability poor, the outward appearance of film has film disadvantages such as bar road, spot.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of solvent-borne type organic modified silica sol, and it should have good dispersiveness and stability in the cured film coating fluid of resin system, can eliminate various relevant coating disadvantages, has excellent water and oil repellant performance simultaneously.
For achieving the above object, the present invention has adopted following technical scheme:
A kind of organic modified silica sol, it is made up of silica dioxide granule, organic solvent and properties-correcting agent, described organic modified silica sol is containing the silica dioxide granule of 17～22% mass percents, containing the organic solvent of 63～82.5% mass percents, containing the properties-correcting agent of 0.5～15% mass percent.
Above-mentioned organic modified silica sol, described properties-correcting agent is a kind of silicone compounds of hydrocarbon compoud containing fluorine group.
Above-mentioned organic modified silica sol, described properties-correcting agent is the two functional group's siloxanes coupling agents that contain fluorohydrocarbon group and alkane group.
Above-mentioned organic modified silica sol, described structure of modifier formula is:
In formula: R
1represent:
or
, wherein n is 1～10 integer;
R
2represent carbonatoms 1～10 alkane and aromatic hydrocarbons;
R
3represent the alkane of carbonatoms 1～3.
Above-mentioned organic modified silica sol, described n is 3～6 integer, R
2represent carbonatoms 2～5 alkane.
Solvent-borne type organic modified silica sol provided by the invention has suitable median size, and outward appearance clear, has good stability.In the cured film coating fluid of resin system, there are good dispersiveness and stability, can eliminate various relevant coating disadvantages, there is excellent water and oil repellant performance simultaneously.
Embodiment
Basic colloidal sol in the present invention is the solution that forms the silica dioxide granule with collosol property with compound of silicate class hydrolysis, polymerization.
In the present invention, properties-correcting agent is the two functional group's siloxanes coupling agents that contain fluorohydrocarbon group and alkane group, and its primary structure is
, wherein R
1for
(in formula, n is 1 ~ 10 integer) or
(in formula, n is 1 ~ 10 integer), R
2for carbonatoms 1～120 alkane and aromatic hydrocarbons, R
3for the alkane of carbonatoms 1～3.The siloxanes coupling that simultaneously contains fluorohydrocarbon and alkane is grafted on the particle of silicon dioxide gel, and two organic groups play respectively external water and oil repellant effect, and internal and resin is affine plays dispersion and the stable effect of being easy to.
Organic solvent can be hydrophilic solvent, as alcohol, ether, ketone, ester etc.: can be also non-hydrophilic solvent as benzene series, esters of acrylic acid.
Solvent-borne type organic modified silica sol provided by the invention can be prepared by following step:
1. reaction: alkylsiloxane is hydrolyzed and condensation in alcohol, water, alkaline solution with alkoxide process, to obtain the reaction solution of silicon sol.
2. modification: add the two functional silanes coupling agents that contain fluorohydrocarbon and alkane in above-mentioned silicon sol solution, carry out organically-modified.
3. concentrated: the reaction solution in step 2 is concentrated.
4. displacement: concentrated solution is carried out to solvent exchange, make silicon sol have 17% or the silica concentration of higher weight percent.
The organoalkoxysilane using in the alkoxide process of step 1 as: tetramethoxy-silicane (TMOS), tetraethoxysilane (TEOS) can be methyl alcohol, ethanol, Virahol, propyl carbinol etc. as the alcohol of solvent.Water is pure water or redistilled water.Basic catalyst uses ammoniacal liquor conventionally, and its consumption is according to the required interrelation of particle size of preparing colloidal sol, and temperature of reaction is 15-50 DEG C and is advisable.
The coupling agent adding in step 2 comprises trifluoro propyl methyl dimethoxysilane, trifluoro propyl methyldiethoxysilane, trifluoro propyl octyl group dimethoxy silane, difluoro ethyl propyl octyl group dimethoxy silane, hexafluoro butyl propyl group methyl dimethoxysilane, ten difluoro heptyl propyl group methyl dimethoxysilanes, ten trifluoro octyl group methyl dimethoxysilanes, ten trifluoro octyl group methyldiethoxysilane etc.
Concentrated mode in step 3 is that the heating under normal pressure or decompression is concentrated, also can adopt the mode of membrane concentration.
The organic solvent using in step 4 is not particularly limited, and generally uses Virahol, propyl carbinol, methyl ethyl ketone, methyl iso-butyl ketone (MIBK), propylene glycol monomethyl ether, ethylene glycol propyl ether, ethyl acetate, toluene etc.Substitute mode is normal pressure displacement, and head temperature reaches the boiling point of the organic solvent of displacement use.In colloidal sol, moisture content, below 5.0%, preferably can reach 0.1-1.0%.
The general solid content of organic modified silica sol is 15-30%.
The application of organic modified silica sol in hardened coating film, be generally directly join that UV solidifies or the functional resin of thermofixation in, curing of coating.
Be described further below in conjunction with specific embodiment.
The preparation of basic colloidal sol:
Pure water 190g, 26% ammoniacal liquor 26g, ethanol 1734g are mixed, be warming up to 25 DEG C.At this temperature, drip the mixing solutions of tetraethoxy (TEOS) 275g and ethanol 173g, reacting liquid temperature is controlled at 25 ± 3 DEG C of scopes, time for adding 60-80 minute.Insulation reaction obtained silicon sol solution after 8 hours.
Embodiment 1
Using 2.4g trifluoro propyl methyldiethoxysilane as properties-correcting agent, (account for colloidal sol weight 0.5%) joins in the basic silicon sol solution of 2300g, 50 DEG C of insulation reaction 5 hours.The lower concentration of reaction solution of decompression is to 590g.Under normal pressure, distill the second alcohol and water in substitutional solution with methyl ethyl ketone in the situation that reservation strength of solution is constant, the boiling point (79.5 DEG C) that head temperature reaches methyl ethyl ketone is terminal.Cool to room temperature, use 3um membrane filtration, obtain the organic modified silica sol of the solid content 17% of methyl ethyl ketone Solution Dispersion.
Embodiment 2
Using 7.3g trifluoro propyl octyl group dimethoxy silane as properties-correcting agent (account for colloidal sol weight 2%), with methyl iso-butyl ketone (MIBK) be dispersion solvent, operate according to the technique of embodiment 1.Obtain the organic modified silica sol of the solid content 22% of methyl iso-butyl ketone (MIBK) dispersion.
Embodiment 3
Using 36.4g ten trifluoro octyl group methyldiethoxysilane as properties-correcting agent (account for colloidal sol weight 10%), with methyl iso-butyl ketone (MIBK) be dispersion solvent, operate according to the technique of embodiment 1.Obtain the organic modified silica sol of the solid content 22% of methyl iso-butyl ketone (MIBK) dispersion.
Embodiment 4
Using 32g difluoro ethyl propyl octyl group dimethoxy silane as properties-correcting agent (account for colloidal sol weight 8%), with propylene glycol monomethyl ether be dispersion agent, operate according to the technique of embodiment 1.Obtain the organic modified silica sol of the solid content 20% of propylene glycol monomethyl ether dispersion.
Embodiment 5
Using 18.8g hexafluoro butyl propyl group methyl dimethoxysilane as properties-correcting agent (account for colloidal sol weight 4%), with propylene glycol monomethyl ether be dispersion agent, operate according to the technique of embodiment 1.Obtain the organic modified silica sol of the solid content 17% of propylene glycol monomethyl ether dispersion.
Embodiment 6
Using 54.5g ten difluoro heptyl propyl group methyl dimethoxysilanes as properties-correcting agent (account for colloidal sol weight 15%), with methyl ethyl ketone be dispersion agent, operate according to the technique of embodiment 1.Obtain solid content 22% organic modified silica sol that methyl ethyl ketone disperses.
Comparative example 1
Using 18.8g methyltrimethoxy silane as properties-correcting agent (account for colloidal sol weight 4%), with propylene glycol monomethyl ether be dispersion agent, operate according to the technique of embodiment 1.Obtain the organic modified silica sol of the solid content 17% of propylene glycol monomethyl ether dispersion.
Comparative example 2
Using 14.5g ten trifluoro octyl group Trimethoxy silanes as properties-correcting agent (account for colloidal sol weight 4%), with methyl ethyl ketone be dispersion agent, operate according to the technique of embodiment 1.Obtain the organic modified silica sol of the solid content 22% of methyl ethyl ketone dispersion.
Test example 1
Situation of the particle diameter of the organic modified silica sol particle that test example 1-6 and comparative example 1,2 are obtained, silica concentration, moisture, aggregation etc. detects.Result is as shown in table 1.
Wherein: particle diameter (nm) is that silicon sol is recorded to specific surface area a(m by BET method after dry 5 hours at 125 DEG C
2/ g), calculate by formula (2727/a); Silica concentration is that silicon sol is recorded after dry 5 hours at 125 DEG C; Moisture is recorded by karl-Fischer method moisture content tester; Aggregation situation adopts range estimation.
Table 1
。
Test example 2
After organic modified silica sol is joined and is uniformly dispersed in UV cured film coating fluid, observe it in the dispersiveness of coating fluid and the stability of coating fluid.Film, the water and oil repellant performance of test film and apparent after solidifying.Result is as shown in table 2.
The formula of coating fluid is: EM265(double pentaerythritol methacrylate, Changxing Chemical Co., Ltd.) 13.0 parts, 6185B (aliphatic urethane acrylate prepolymer, Changxing Chemical Co., Ltd.) 7.0 parts, 184(initiator, Tianjin proud son of heaven Chemical Co., Ltd.) 1.0 parts, BYK377 (polydimethylsiloxaneskeleton skeleton flow agent, Bi Ke chemical company) 2.0 parts, 38.7 parts of methyl iso-butyl ketone (MIBK), 15.0 parts of dimethyl succinates, 23.3 parts of Virahols, 30.0 parts of organic modified silica sols.
The outward appearance situation range estimation of dispersiveness, stability and the film of coating fluid, visual observation according to fine or not situation be divided into excellent, good, can, differ from four grades.The contact angle of water and oil repellant characteristic is measured with quiet contact angle/interfacial tension survey meter of POWEREACH JC2000C1.The test solution of refusing oil test use is n-hexadecane.
Table 2
Claims (2)
1. an organic modified silica sol, is characterized in that, described basic colloidal sol is prepared as follows:
Pure water 190g, 26% ammoniacal liquor 26g, ethanol 1734g are mixed, be warming up to 25 DEG C; At this temperature, drip the mixing solutions of tetraethoxy 275g and ethanol 173g, reacting liquid temperature is controlled at 25 ± 3 DEG C of scopes, time for adding 60-80 minute, and insulation reaction obtains basic colloidal sol after 8 hours;
Modification is carried out as follows:
Using 7.3g trifluoro propyl octyl group dimethoxy silane as properties-correcting agent, join in the basic silicon sol solution of 2300g, 50 DEG C of insulation reaction 5 hours, the lower concentration of reaction solution of decompression is to 590g; Under normal pressure, distill the second alcohol and water in substitutional solution by methyl iso-butyl ketone (MIBK) in the situation that reservation strength of solution is constant, the boiling point that head temperature reaches methyl iso-butyl ketone (MIBK) is terminal; Cool to room temperature, with 3 μ m membrane filtrations, obtain the organic modified silica sol of the solid content 22% of methyl isobutyl ketone solution dispersion;
In described organic modified silica sol, moisture content is 0.43%.
2. an organic modified silica sol, is characterized in that, described basic colloidal sol is prepared as follows:
Pure water 190g, 26% ammoniacal liquor 26g, ethanol 1734g are mixed, be warming up to 25 DEG C; At this temperature, drip the mixing solutions of tetraethoxy 275g and ethanol 173g, reacting liquid temperature is controlled at 25 ± 3 DEG C of scopes, time for adding 60-80 minute, and insulation reaction obtains basic colloidal sol after 8 hours;
Modification is carried out as follows:
Using 36.4g ten trifluoro octyl group methyldiethoxysilane as properties-correcting agent, join in the basic silicon sol solution of 2300g, 50 DEG C of insulation reaction 5 hours, the lower concentration of reaction solution of decompression is to 590g; Under normal pressure, distill the second alcohol and water in substitutional solution by methyl iso-butyl ketone (MIBK) in the situation that reservation strength of solution is constant, the boiling point that head temperature reaches methyl iso-butyl ketone (MIBK) is terminal; Cool to room temperature, with 3 μ m membrane filtrations, obtain the organic modified silica sol of the solid content 22% of methyl isobutyl ketone solution dispersion;
In described organic modified silica sol, moisture content is 0.45%.
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|---|---|---|---|
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| CN103773236B (en) * | 2014-01-17 | 2016-02-03 | 浙江大学 | A kind of method preparing waterproof and oilproof type ceramic coating at substrate surface |
| CN106811957B (en) * | 2016-12-08 | 2019-08-27 | 苏州榕绿纳米科技有限公司 | A kind of preparation method of the super hydrophobic surface for lotion separation |
| CN108641416A (en) * | 2018-04-16 | 2018-10-12 | 奥普家居股份有限公司 | A kind of manufacturing method of Nanometer dustproof coating and its application |
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