CN102504614A - Organic modified silica sol - Google Patents
Organic modified silica sol Download PDFInfo
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- CN102504614A CN102504614A CN2011103613969A CN201110361396A CN102504614A CN 102504614 A CN102504614 A CN 102504614A CN 2011103613969 A CN2011103613969 A CN 2011103613969A CN 201110361396 A CN201110361396 A CN 201110361396A CN 102504614 A CN102504614 A CN 102504614A
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- Prior art keywords
- silicon sol
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- modified silicon
- properties
- correcting agent
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- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical class O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 title abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003960 organic solvent Substances 0.000 claims abstract description 13
- 239000008187 granular material Substances 0.000 claims abstract description 7
- -1 siloxanes Chemical class 0.000 claims description 19
- 150000001335 aliphatic alkanes Chemical group 0.000 claims description 13
- 125000004432 carbon atom Chemical group C* 0.000 claims description 8
- 239000007822 coupling agent Substances 0.000 claims description 7
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 125000000524 functional group Chemical group 0.000 claims description 3
- 239000004215 Carbon black (E152) Substances 0.000 claims description 2
- 125000001153 fluoro group Chemical group F* 0.000 claims description 2
- 229930195733 hydrocarbon Natural products 0.000 claims description 2
- 150000002430 hydrocarbons Chemical class 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 238000000576 coating method Methods 0.000 abstract description 13
- 229920005989 resin Polymers 0.000 abstract description 9
- 239000011347 resin Substances 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 6
- 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
- 239000007788 liquid Substances 0.000 abstract description 3
- 239000005871 repellent Substances 0.000 abstract 2
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 24
- 150000003376 silicon Chemical class 0.000 description 22
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 15
- 229910052710 silicon Inorganic materials 0.000 description 15
- 239000010703 silicon Substances 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 239000000243 solution Substances 0.000 description 13
- 239000011248 coating agent Substances 0.000 description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 9
- 239000007787 solid Substances 0.000 description 9
- 239000003921 oil Substances 0.000 description 8
- 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
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000006185 dispersion Substances 0.000 description 7
- 239000012530 fluid Substances 0.000 description 7
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 4
- YQGOWXYZDLJBFL-UHFFFAOYSA-N dimethoxysilane Chemical compound CO[SiH2]OC YQGOWXYZDLJBFL-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 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
- 239000000047 product Substances 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
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000001723 curing Methods 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- GAURFLBIDLSLQU-UHFFFAOYSA-N diethoxy(methyl)silicon Chemical compound CCO[Si](C)OCC GAURFLBIDLSLQU-UHFFFAOYSA-N 0.000 description 2
- PKTOVQRKCNPVKY-UHFFFAOYSA-N dimethoxy(methyl)silicon Chemical compound CO[Si](C)OC PKTOVQRKCNPVKY-UHFFFAOYSA-N 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
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 125000000962 organic group Chemical group 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 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
- WXUAQHNMJWJLTG-UHFFFAOYSA-N 2-methylbutanedioic acid Chemical class OC(=O)C(C)CC(O)=O WXUAQHNMJWJLTG-UHFFFAOYSA-N 0.000 description 1
- YEYKMVJDLWJFOA-UHFFFAOYSA-N 2-propoxyethanol Chemical compound CCCOCCO YEYKMVJDLWJFOA-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000003848 UV Light-Curing Methods 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
- 238000004821 distillation Methods 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
- 239000012467 final product Substances 0.000 description 1
- 238000009998 heat setting Methods 0.000 description 1
- 238000010438 heat treatment Methods 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
- 238000005374 membrane filtration Methods 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
- 238000002156 mixing Methods 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
- 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
- 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
- 238000010792 warming Methods 0.000 description 1
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 have special nature, silicon sol has obtained in fields such as fiber, fabric, papermaking, coating, caking agent, pottery, medicine, precision castings using widely.
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 the hard coat film of molding synthetic resin surfaces such as forming 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 scratch resistance performance also should have the characteristic of water and oil repellant, and the product that therefore has the organic solvent silicasol of special purpose arises at the historic moment.
The transparent cured film of this type will add silicon sol usually in order to reach good performance in extraordinary resin film forming curing system; And the surface exists the silicon oxide particle of hydroxyl in resin system, can to assemble because of the effect of hydroxyl; Cause film performance uneven, can occur many coating disadvantages simultaneously.Through 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 tetraethoxy (TEOS) alcoholysis method synthetic silicon sol has been carried out the organic solvent type silicon sol that modification obtains with the siloxanes coupling agent that contains single or a plurality of alkane, has good storage stability but it does not have the characteristic of water and oil repellant.
Use the class coating material that contains the coupling agent modified organic silicon sol of single fluorohydrocarbon type siloxane in the disclosed technology of WO03/102089; Since the water and oil repellant characteristic of its modification group can cause with mixed with resin after the solution package stability poor, the outward appearance of filming has such as disadvantages of filming such as bar road, spots.
Summary of the invention
Technical problem to be solved by this invention provides the organically-modified silicon sol of a kind of solvent-borne type, and it should have good dispersiveness and stable 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 technical scheme below the present invention has adopted:
A kind of organically-modified silicon sol; It is made up of silica dioxide granule, organic solvent and properties-correcting agent; Said organically-modified silicon sol contains the silica dioxide granule of 17～22% mass percents, contains the organic solvent of 63～82.5% mass percents, contains the properties-correcting agent of 0.5～15% mass percent.
Above-mentioned organically-modified silicon sol, said properties-correcting agent are a kind of silicone compounds of hydrocarbon compoud containing fluorine group.
Above-mentioned organically-modified silicon sol, said properties-correcting agent are the two functional group's siloxanes coupling agents that contain fluorohydrocarbon group and alkane group.
Above-mentioned organically-modified silicon sol, said properties-correcting agent structural formula is:
In the formula: R
1Expression:
Or
, wherein n is 1～10 integer;
R
2Expression carbonatoms 1～10 alkane and aromatic hydrocarbons;
R
3The alkane of expression carbonatoms 1～3.
Above-mentioned organically-modified silicon sol, said n are 3～6 integers, R
2Expression carbonatoms 2～5 alkane.
The organically-modified silicon sol of solvent-borne type provided by the invention has suitable median size, and the outward appearance clear has good stability.Good dispersiveness and stable is arranged in the cured film coating fluid of resin system, can eliminate various relevant coating disadvantages, have excellent water and oil repellant performance simultaneously.
Embodiment
Basic colloidal sol among the present invention is the solution that forms the silica dioxide granule with collosol property with compound of silicate class hydrolysis, polymerization.
Properties-correcting agent is the two functional group's siloxanes coupling agents that contain fluorohydrocarbon group and alkane group among the present invention, and its primary structure does
, R wherein
1For
(n is 1 ~ 10 integer in the formula) or
(n is 1 ~ 10 integer in the formula), R
2Be carbonatoms 1～120 alkane and aromatic hydrocarbons, R
3Alkane for carbonatoms 1～3.The siloxanes coupling that contains fluorohydrocarbon and alkane simultaneously is grafted on the particle of silicon dioxide gel, and two organic groups play external water and oil repellant effect respectively, and internal and affine the playing of resin is easy to disperse and stable effect.
Organic solvent can be a hydrophilic solvent, like alcohol, ether, ketone, ester etc.: also can be non-hydrophilic solvent like benzene series, esters of acrylic acid.
The organically-modified silicon sol of solvent-borne type provided by the invention can prepare through following step:
1. reaction: with alkoxide process alkylsiloxane is hydrolyzed and condensation in alcohol, water, alkaline solution, to obtain the reaction solution of silicon sol.
2. modification: in above-mentioned silicon sol solution, add the two functional silanes coupling agents that contain fluorohydrocarbon and alkane, carry out organically-modified.
3. concentrate: the reaction solution in the step 2 is concentrated.
4. displacement: liquid concentrator is carried out solvent exchange, make silicon sol have 17% or the silica concentration of higher weight percent.
The organoalkoxysilane that uses in the alkoxide process of step 1 is like 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 usually, and its consumption is relevant according to the particle diameter of required preparation colloidal sol, and temperature of reaction is 15-50 ℃ and is advisable.
The coupling agent that adds in the 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 the step 3 is that the heating under normal pressure or the decompression concentrates, and also can adopt the mode of membrane-concentrated.
The not special restriction of the organic solvent that uses in the step 4 is generally used Virahol, propyl carbinol, methyl ethyl ketone, MIBK, propylene glycol monomethyl ether, ethylene glycol propyl ether, ETHYLE ACETATE, toluene etc.Substitute mode is the normal pressure displacement, and the boiling point that head temperature reaches the organic solvent of displacement use gets final product.Moisture content preferably can reach 0.1-1.0% below 5.0% in the colloidal sol.
The general solid content of organically-modified silicon sol is 15-30%.
The application of organically-modified silicon sol in hardened coating film generally is directly to join in the functional resin of UV curing or thermofixation 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 ℃.Under this temperature, drip the mixing solutions of tetraethoxy (TEOS) 275g and ethanol 173g, reacting liquid temperature is controlled at 25 ± 3 ℃ of scopes, drips time 60-80 minute.Insulation reaction obtained silicon sol solution after 8 hours.
Embodiment 1
2.4g trifluoro propyl methyldiethoxysilane is joined in the basic silicon sol solution of 2300g 50 ℃ of insulation reaction 5 hours as properties-correcting agent (account for colloidal sol weight 0.5%).Concentration of reaction solution is to 590g under the decompression.With methyl ethyl ketone second alcohol and water in the distillation substitutional solution under keeping the constant situation of strength of solution, the boiling point (79.5 ℃) that head temperature reaches methyl ethyl ketone is a terminal point to normal pressure down.Cool to room temperature, use the 3um membrane filtration, obtain the organically-modified silicon sol of methyl ethyl ketone solution dispersive solid content 17%.
Embodiment 2
As properties-correcting agent (account for colloidal sol weight 2%), use MIBK to be dispersion solvent in 7.3g trifluoro propyl octyl group dimethoxy silane, operate according to the technology of embodiment 1.Obtain the organically-modified silicon sol of MIBK dispersive solid content 22%.
Embodiment 3
As properties-correcting agent (account for colloidal sol weight 10%), use MIBK to be dispersion solvent with 36.4g ten trifluoro octyl group methyldiethoxysilane, operate according to the technology of embodiment 1.Obtain the organically-modified silicon sol of MIBK dispersive solid content 22%.
Embodiment 4
As properties-correcting agent (account for colloidal sol weight 8%), use propylene glycol monomethyl ether to be dispersion agent with 32g difluoro ethyl propyl octyl group dimethoxy silane, operate according to the technology of embodiment 1.Obtain the organically-modified silicon sol of propylene glycol monomethyl ether dispersive solid content 20%.
Embodiment 5
As properties-correcting agent (account for colloidal sol weight 4%), use propylene glycol monomethyl ether to be dispersion agent with 18.8g hexafluoro butyl propyl group methyl dimethoxysilane, operate according to the technology of embodiment 1.Obtain the organically-modified silicon sol of propylene glycol monomethyl ether dispersive solid content 17%.
Embodiment 6
As properties-correcting agent (account for colloidal sol weight 15%), use methyl ethyl ketone to be dispersion agent with 54.5g ten difluoro heptyl propyl group methyl dimethoxysilanes, operate according to the technology of embodiment 1.Obtain methyl ethyl ketone dispersive solid content 22% organically-modified silicon sol.
Comparative Examples 1
As properties-correcting agent (account for colloidal sol weight 4%), use propylene glycol monomethyl ether to be dispersion agent with the 18.8g methyltrimethoxy silane, operate according to the technology of embodiment 1.Obtain the organically-modified silicon sol of propylene glycol monomethyl ether dispersive solid content 17%.
Comparative Examples 2
As properties-correcting agent (account for colloidal sol weight 4%), use methyl ethyl ketone to be dispersion agent with 14.5g ten trifluoro octyl group Trimethoxy silanes, operate according to the technology of embodiment 1.Obtain the organically-modified silicon sol of methyl ethyl ketone dispersive solid content 22%.
Test Example 1
Situation of the particle diameter of the organically-modified silica sol granule that Test Example 1-6 and Comparative Examples 1,2 are obtained, silica concentration, moisture, aggregation etc. detects.The result is as shown in table 1.
Wherein: particle diameter (nm) is that silicon sol was recorded specific surface area a (m with the BET method after under 125 ℃ dry 5 hours
2/ g), (2727/a) calculates through formula; Silica concentration is after under 125 ℃ dry 5 hours, to record silicon sol; Moisture is recorded by the karl-Fischer method moisture content tester; The aggregation situation adopts range estimation.
Table 1
Test Example 2
With organically-modified silicon sol join be uniformly dispersed in the UV cured film coating fluid after, observe it in the dispersiveness of coating fluid and the stability of coating fluid.Film the water and oil repellant performance that test is filmed after solidifying and apparent.The result is as shown in table 2.
The prescription of coating fluid is: 13.0 parts of EM265 (double pentaerythritol methacrylate, Changxing chemistry ltd), 6185B (aliphatic urethane acrylate prepolymer; Changxing chemistry ltd) 7.0 parts, 1.0 parts in 184 (initiator, Tianjin proud son of heaven chemical industry ltds); 2.0 parts of BYK377 (polydimethylsiloxaneskeleton skeleton flow agent, Bi Ke chemical company), 38.7 parts of MIBKs; 15.0 parts of methyl-succinates, 23.3 parts of Virahols, 30.0 parts of organically-modified silicon sol.
The dispersiveness of coating fluid, stability and the outward appearance situation of filming range estimation, 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 of POWEREACH JC2000C1/IT survey meter.Refuse the oily test solution that uses of testing and be n-hexadecane.
Table 2
Claims (5)
1. organically-modified silicon sol; It is made up of silica dioxide granule, organic solvent and properties-correcting agent; It is characterized in that; Said organically-modified silicon sol contains the silica dioxide granule of 17～22% mass percents, contains the organic solvent of 63～82.5% mass percents, contains the properties-correcting agent of 0.5～15% mass percent.
2. according to the said organically-modified silicon sol of claim 1, it is characterized in that being that said properties-correcting agent is a kind of silicone compounds of hydrocarbon compoud containing fluorine group.
3. according to the said organically-modified silicon sol of claim 2, it is characterized in that being that said properties-correcting agent is the two functional group's siloxanes coupling agents that contain fluorohydrocarbon group and alkane group.
4. according to the said organically-modified silicon sol of claim 3, it is characterized in that said properties-correcting agent structural formula is:
In the formula: R
1Expression:
Or
, wherein n is 1～10 integer;
R
2Expression carbonatoms 1～10 alkane and aromatic hydrocarbons;
R
3The alkane of expression carbonatoms 1～3.
5. according to the said organically-modified silicon sol of claim 4, it is characterized in that said n is 3～6 integer, R
2Expression carbonatoms 2～5 alkane.
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|---|---|---|---|
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| CN103773236A (en) * | 2014-01-17 | 2014-05-07 | 浙江大学 | Method for preparing waterproof and oilproof ceramic coating on surface of base material |
| CN106811957A (en) * | 2016-12-08 | 2017-06-09 | 苏州榕绿纳米科技有限公司 | A kind of preparation method of the super hydrophobic surface for for emulsion separate |
| 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 |
| CN109651544A (en) * | 2018-12-10 | 2019-04-19 | 怀化学院 | Hydrophobic nano-silica modified polyacrylate dispersion liquid and preparation method thereof |
| CN110105872A (en) * | 2019-03-12 | 2019-08-09 | 超为科技（北京）有限公司 | A kind of hydrophobic transparent conductive nano coating composition and its coating of preparation |
| CN115746703A (en) * | 2022-11-21 | 2023-03-07 | 东莞市雄驰电子有限公司 | Method for preparing photocureable coating composition and coating based on epoxy fluorobenzene silicone resin and application of photocureable coating composition and coating |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103773236A (en) * | 2014-01-17 | 2014-05-07 | 浙江大学 | Method for preparing waterproof and oilproof ceramic coating on surface of base material |
| 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 |
| CN106811957A (en) * | 2016-12-08 | 2017-06-09 | 苏州榕绿纳米科技有限公司 | A kind of preparation method of the super hydrophobic surface for for emulsion separate |
| 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 |
| CN109651544A (en) * | 2018-12-10 | 2019-04-19 | 怀化学院 | Hydrophobic nano-silica modified polyacrylate dispersion liquid and preparation method thereof |
| CN109651544B (en) * | 2018-12-10 | 2021-05-04 | 怀化学院 | Hydrophobic nano silicon dioxide modified polyacrylate dispersion liquid and preparation method thereof |
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| CN115746703A (en) * | 2022-11-21 | 2023-03-07 | 东莞市雄驰电子有限公司 | Method for preparing photocureable coating composition and coating based on epoxy fluorobenzene silicone resin and application of photocureable coating composition and coating |
| CN115746703B (en) * | 2022-11-21 | 2023-11-10 | 东莞市雄驰电子有限公司 | Photo-curing coating composition prepared based on epoxy fluorobenzene silicone resin, coating method and application |
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