CN102838894B - Preparation method for high performance coating - Google Patents
Preparation method for high performance coating Download PDFInfo
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- CN102838894B CN102838894B CN201110170247.4A CN201110170247A CN102838894B CN 102838894 B CN102838894 B CN 102838894B CN 201110170247 A CN201110170247 A CN 201110170247A CN 102838894 B CN102838894 B CN 102838894B
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- 239000011248 coating agent Substances 0.000 title claims abstract description 64
- 238000000576 coating method Methods 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 239000000945 filler Substances 0.000 claims abstract description 7
- 239000000049 pigment Substances 0.000 claims abstract description 7
- -1 orthosilicate organic ester Chemical class 0.000 claims abstract description 4
- 238000007599 discharging Methods 0.000 claims abstract description 3
- 239000002253 acid Substances 0.000 claims description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 16
- 229920005989 resin Polymers 0.000 claims description 15
- 239000011347 resin Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 8
- 239000001117 sulphuric acid Substances 0.000 claims description 8
- 235000011149 sulphuric acid Nutrition 0.000 claims description 8
- 125000000217 alkyl group Chemical group 0.000 claims description 6
- 239000012752 auxiliary agent Substances 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 125000004432 carbon atom Chemical group C* 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 5
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000000306 component Substances 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- ZUEKXCXHTXJYAR-UHFFFAOYSA-N tetrapropan-2-yl silicate Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)OC(C)C ZUEKXCXHTXJYAR-UHFFFAOYSA-N 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 20
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 13
- 239000000377 silicon dioxide Substances 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000725 suspension Substances 0.000 abstract description 2
- 239000010419 fine particle Substances 0.000 abstract 2
- 239000000654 additive Substances 0.000 abstract 1
- 230000000996 additive effect Effects 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000004806 packaging method and process Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 11
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 10
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 description 10
- 239000006185 dispersion Substances 0.000 description 9
- 229960001866 silicon dioxide Drugs 0.000 description 9
- 239000002105 nanoparticle Substances 0.000 description 7
- 239000003973 paint Substances 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- 229920001577 copolymer Polymers 0.000 description 6
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical group FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 description 6
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 6
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 6
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 5
- 229940043232 butyl acetate Drugs 0.000 description 5
- 239000013530 defoamer Substances 0.000 description 5
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 239000012046 mixed solvent Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 229920006243 acrylic copolymer Polymers 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 2
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- MLFHJEHSLIIPHL-UHFFFAOYSA-N isoamyl acetate Chemical compound CC(C)CCOC(C)=O MLFHJEHSLIIPHL-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
- 229940043265 methyl isobutyl ketone Drugs 0.000 description 2
- 239000005543 nano-size silicon particle Substances 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 235000019260 propionic acid Nutrition 0.000 description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound 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
- 238000012360 testing method Methods 0.000 description 2
- VPBZZPOGZPKYKX-UHFFFAOYSA-N 1,2-diethoxypropane Chemical compound CCOCC(C)OCC VPBZZPOGZPKYKX-UHFFFAOYSA-N 0.000 description 1
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 1
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 239000004812 Fluorinated ethylene propylene Substances 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- 229920006172 Tetrafluoroethylene propylene Polymers 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019445 benzyl alcohol Nutrition 0.000 description 1
- 229960004217 benzyl alcohol Drugs 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- HQQADJVZYDDRJT-UHFFFAOYSA-N ethene;prop-1-ene Chemical group C=C.CC=C HQQADJVZYDDRJT-UHFFFAOYSA-N 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 229940093499 ethyl acetate Drugs 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 229940117955 isoamyl acetate Drugs 0.000 description 1
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000006224 matting agent Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920009441 perflouroethylene propylene Polymers 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 229920003987 resole Polymers 0.000 description 1
- 238000007665 sagging Methods 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
Abstract
The present invention relates to a preparation method for a high performance coating containing a SixOx-1(OH)y(OR)z alcosol. Specific steps of the preparation method comprise: adding an alcohol solution to an orthosilicate organic ester Si(OR)4 in a dropwise manner under stirring to obtain an alcosol containing a substance having a structure formula of SixOx-1(OH)y(OR)Z, mixing the SixOx-1(OH)y(OR)z alcosol, a film-forming component, a pigment, a filler and an additive in a solvent, and carrying out material discharging and packaging. According to the high performance coating of the present invention, silicon dioxide exists in the form of condensed SixOx-1(OH)y(OR)z fine particles with a particle size of about 1-10 nm, and has good compatibility with the coating solvent, such that the particles can be uniformly dispersed in the coating, and problems of poor suspension stability, poor thixotropy, not high finish, and the like of the raw materials are solved well, wherein the condensed SixOx-1(OH)y(OR)z fine particles are not completely hydrolyzed.
Description
Technical field
The present invention relates to a kind of preparation method for coating, relate more specifically to contain Si
xo
x-1(OH)
y(OR)
zthe preparation method of the high-performance coating of alcosol.
Background technology
Nano silicon adds in coating, both can coating have good hardness and scratch resistance, can keep again the film transparency simultaneously.Improve the scrub resistance, intensity, hardness of coating etc.; Take into account and improve the anti-ultraviolet aging experimental performance of coating, significantly reduce time of drying, and the suspension stability that raw material exists is poor, thixotropy is poor, smooth finish is not high etc., and problem is also well solved.
At present, the nanoparticle in nano paint often directly adds in resin matrix with the form of auxiliary agent.Because the particle diameter of nano silicon is little, specific surface energy is large, and it is very easy to reunite or can be dispersed in coating by pigment, filler embedding in coating.
Summary of the invention
The object of the invention is to solve above-mentioned deficiency, a kind of preparation method of high-performance coating is provided.The technical scheme that realizes the object of the invention is: a kind of preparation method of high-performance coating, comprises the following steps:
1) under stirring, Organic Alcohol is mixed into positive Alkoxysilanes Si (OR) is housed
4reactor in, then drip diluted acid or diluted alkaline to solution, temperature of reaction is controlled to room temperature with circulated refrigerated water, stir 10-20min, obtain that to contain structural formula be Si
xo
x-1(OH)
y(OR)
zthe alcosol of sol particles, wherein:
X is greater than 0 integer;
Z is greater than 0 integer;
2x-2=y+z; With
R represents to have the straight or branched alkyl of 2-9 carbon atom, preferably has the straight or branched alkyl of 3-6 carbon atom, more preferably ethyl;
2) by Si
xo
x-1(OH)
y(OR)
zalcosol, film-forming components, pigment and filler and auxiliary agent mix in solvent;
3) discharging, packing.
The preparation method of above-mentioned high-performance coating, positive Alkoxysilanes Si (OR) in described step 1)
4for tetraethoxy, positive isopropyl silicate, a kind of in the positive silicon ester of the tetrabutyl.
The preparation method of above-mentioned high-performance coating, in described step 1), Organic Alcohol is the one in ethanol, propyl alcohol or butanols.
The preparation method of above-mentioned high-performance coating, in described step 1), diluted acid is dilute hydrochloric acid or dilute sulphuric acid, and diluted alkaline is weak ammonia, and the volumetric molar concentration of dilute hydrochloric acid or dilute sulphuric acid or weak ammonia is: 0.001-1mol/L, preferred: 0.01-0.5mol/L, more preferably: 0.05-0.1mol/L.
The preparation method of above-mentioned high-performance coating, in described step 1), in positive Alkoxysilanes and diluted acid or diluted alkaline, the mol ratio of water is 1:0.1-5, is preferably 1:0.2-4, more preferably 1:0.3-3.
The preparation method of above-mentioned high-performance coating, in described step 1), diluted acid or diluted alkaline rate of addition are 0.2-8ml/min, are preferably 0.3-6ml/min, more preferably 0.5-3ml/min.
The preparation method of above-mentioned high-performance coating, Si in described step 1)
xo
x-1(OH)
y(OR)
zthe structural formula of alcosol is Si
xo
x-1(OH)
y(OR)
zthe particle diameter of sol particles be 1-10nm.
The present invention has positive effect:
(1) preparation method of the present invention is simple, easy to operate; (2) the accurate control of the rate of addition by diluted acid or diluted alkaline effectively realizes and suppresses the too fast object of hydrolysis.Sol particles particle diameter yardstick is controlled below 10nm, and size distribution is relatively even, Si
xo
x-1(OH)
y(OR)
zcolloidal sol stable performance, do not reunite.
Embodiment
Coating of the present invention comprises following component: A) Si
xo
x-1(OH)
y(OR)
zalcosol, wherein: x is greater than 0 integer; Z is greater than 0 integer; 2x-2=y+z; Represent to have the straight or branched alkyl of 2-9 carbon atom with R, preferably there is the straight or branched alkyl of 3-6 carbon atom, more preferably ethyl; And B) film-forming components; Wherein in the Si of silicon-dioxide
xo
x-1(OH)
y(OR)
zthe weight ratio of alcosol and film-forming components is 1:15-85, is preferably 1:20-65, more preferably 1:25-50.
Si
xo
x-1(OH)
y(OR)
zalcosol is added drop-wise to Organic Alcohol in positive Alkoxysilanes and makes under stirring, and wherein in positive Alkoxysilanes and diluted acid or diluted alkaline, the mol ratio of water is 1:0.1-5, is preferably 1:0.2-4, more preferably 1:0.3-3; Rate of addition is 0.2-8ml/min, is preferably 0.3-6ml/min, more preferably 0.5-3ml/min.Stirring velocity is generally 200-250rpm, for example 200rpm or 250rpm.Organic Alcohol is ethanol, propyl alcohol or butanols, drips and conventionally carries out at normal temperatures.The Si of described alcosol
xo
x-1(OH)
y(OR)
zthe particle diameter of minuteness particle is 1-10nm, for example 1-6nm or 3-9nm.
The film-forming components using in coating of the present invention can be known to those skilled in the art any film-forming components, the example is fluorocarbon resin, urethane resin, Synolac, thermosetting acrylic resin, resol, nitro-cotton, chlorinated rubber, pitch, modified rosin resin, thermoplastic acrylic resin etc.Being preferably membrane component is fluorocarbon resin.Be well known to those skilled in the art for fluorocarbon resin of the present invention, the example is fluorinated ethylene propylene, polyvinylidene difluoride (PVDF), vinylidene fluoride-hexafluoropropylene copolymer, hexafluoropropylene (HFP)/tetrafluoroethylene (TFE)-vinylidene fluoride copolymers, tetrafluoroethylene propylene copolymer, tetrafluoroethylene-vinylidene-acrylic copolymer etc.Preferably the present invention's fluorocarbon resin used is selected from polyvinylidene difluoride (PVDF), vinylidene fluoride-hexafluoropropylene copolymer, hexafluoropropylene (HFP)/tetrafluoroethylene (TFE)-vinylidene fluoride copolymers, tetrafluoroethylene-vinylidene-acrylic copolymer.
Coating of the present invention also comprises solvent.Solvent for use is common solvent or its mixture, includes but not limited to that aromatic hydrocarbons is as dimethylbenzene, toluene etc.; Ester class is as ethyl acetate, butylacetate, Isoamyl Acetate FCC etc.; Alcohols is as butanols, isopropylcarbinol, phenylcarbinol etc.; Ethers is as ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, propylene glycol diethyl ether etc.; Ketone is as methyl iso-butyl ketone (MIBK), methyl phenyl ketone, isophorone etc.Those skilled in the art can be according to the present invention coating desired properties as the amount of definite solvent for use such as coating property.
Coating of the present invention also can comprise other component known to those skilled in the art, for example pigment; Filler, such as talcum powder, calcium carbonate, barium sulfate, silicon-dioxide etc.; Auxiliary agent, for example defoamer, wetting agent, dispersion agent, emulsifying agent, anti-settling agent, stablizer, anti skinning agent, flow agent, siccative, anti-sagging agent, softening agent, matting agent, fire retardant, mould inhibitor, sterilant, trapping agent etc.Those skilled in the art can be according to the present invention coating desired properties determine concrete kind and the consumption thereof of other component used as bactericidal property etc.
By the Si making as mentioned above
xo
x-1(OH)
y(OR)
zalcosol, film-forming components, optional pigment and filler and optional auxiliary agent mix and obtain coating of the present invention in solvent, wherein in the Si of silicon-dioxide
xo
x-1(OH)
y(OR)
zthe weight ratio of alcosol and film-forming components is 1:15-85, is preferably 1:20-65, more preferably 1:25-50.
Used film forming component, solvent and optional pigment, filler and the auxiliary agent using are all described above.
The coating of the present invention making as mentioned above can be sealed, and preserve in dry environment.Certainly, for coating of the present invention, preferably now-making-now-using.
Can be by any appropriate method known to those skilled in the art by application of paints of the present invention in material surface to be coated, such as roller coat, spraying, dip-coating, brushing, blade coating etc.By after described application of paints is on material surface to be coated, optionally under existing, weak acid makes the Si in film
xo
x-1(OH)
y(OR)
zminuteness particle is further hydrolyzed, and wherein weak acid can be for example formic acid, acetic acid, propionic acid or oxalic acid, and its concentration is 0.1-10 % by weight, is preferably 0.5-6 % by weight.In further hydrolytic process, due to Si
xo
x-1(OH)
y(OR)
zminuteness particle is dispersed and be substantially fixed in film, and the condensation degree that is therefore hydrolyzed gained Nano particles of silicon dioxide can not improve substantially, continues to remain about 1-10nm, obtains thus Nano particles of silicon dioxide and is uniformly distributed final coating therein.
(embodiment 1)
Tetraethoxy is added in reactor, then, under the stirring velocity of 250rpm, ethanol is added in reactor, the dilute hydrochloric acid that drips 0.05mol/L with the rate of addition of 3ml/min is again in reactor, dropwising rear continuation stirs 15 minutes, temperature of reaction kettle is controlled at 20 ℃ with circulated refrigerated water, obtains by Si
2o (OH)
2(OR)
4, Si
3o
2(OH)
2(OR)
6, Si
3o
2(OH)
3(OR)
5the water white Si of sol particles composition
xo
x-1(OH)
y(OR)
zalcosol mixture.Particle size analyzer measuring result shows gained Si
xo
x-1(OH)
y(OR)
zthe Si of alcosol
xo
x-1(OH)
y(OR)
zthe particle diameter of minuteness particle is 1-6nm.Polyvinylidene difluoride (PVDF) is dispersed in the mixed solvent that the weight ratio of dimethylbenzene, butylacetate and isophorone is 7:2:1 and forms fluorocarbon resin dispersion system, and its solid content is 40 % by weight.By gained Si
xo
x-1(OH)
y(OR)
zalcosol adds in fluorocarbon resin dispersion system, then adds defoamer (commercially available, German Bi Ke BYK-141), and flow agent (commercially available, German Bi Ke BYK-333) also mixes acquisition coating of the present invention.It is the film of approximately 30 microns that gained paint spay-coating is obtained to thickness on steel, after coating surface is dry, is 1.5%(weight by concentration) acetic acid aqueous solution be sprayed on film, and film is placed in envrionment conditions, so that Si wherein
xo
x-1(OH)
y(OR)
zminuteness particle is further hydrolyzed into Nano particles of silicon dioxide.Final gained coating is tested, and acquired results is in table 1.
(embodiment 2)
Silicic acid four isopropyl esters are added in reactor, then, under the stirring velocity of 200rpm, propyl alcohol is added in reactor, the dilute hydrochloric acid that drips 0.06mol/L with the rate of addition of 6ml/min is again in reactor, dropwising rear continuation stirs 10 minutes, temperature of reaction kettle is controlled at 20 ℃ with circulated refrigerated water, obtains by Si
2o (OH)
2(OR)
4, Si
3o
2(OH)
2(OR)
6, Si
3o
2(OH)
3(OR)
5the water white Si of sol particles composition
xo
x-1(OH)
y(OR)
zalcosol mixture.Particle size analyzer measuring result shows gained Si
xo
x-1(OH)
y(OR)
zthe Si of alcosol
xo
x-1(OH)
y(OR)
zthe particle diameter of minuteness particle is 2-8nm.2.32kg vinylidene fluoride-hexafluoropropylene copolymer is dispersed in the mixed solvent that the weight ratio of dimethylbenzene, butylacetate and isophorone is 7:2:1 and forms fluorocarbon resin dispersion system, and its solid content is 40 % by weight.By gained Si
xo
x-1(OH)
y(OR)
zalcosol adds in fluorocarbon resin dispersion system, then adds defoamer (commercially available, German Bi Ke BYK-141), and flow agent (commercially available, German Bi Ke BYK-333) also mixes acquisition coating of the present invention.It is the film of approximately 30 microns that gained paint spay-coating is obtained to thickness on steel, after coating surface is dry, is 6%(weight by concentration) aqueous formic acid be sprayed on film, and film is placed in envrionment conditions, so that Si wherein
xo
x-1(OH)
y(OR)
zminuteness particle is further hydrolyzed into Nano particles of silicon dioxide.Final gained coating is tested, and acquired results is in table 1.
(embodiment 3)
Positive silicic acid four butyl ester is added in reactor, then, under the stirring velocity of 250rpm, propyl alcohol is added in reactor, drip 0.1mol/L dilute hydrochloric acid in reactor with the rate of addition of 0.3ml/min again, dropwising rear continuation stirs 20 minutes, temperature of reaction kettle is controlled at 20 ℃ with circulated refrigerated water, obtains by Si
2o (OH)
2(OR)
4, Si
3o
2(OH)
2(OR)
6, Si
3o
2(OH)
3(OR)
5the water white Si of sol particles composition
xo
x-1(OH)
y(OR)
zalcosol mixture.Particle size analyzer measuring result shows gained Si
xo
x-1(OH)
y(OR)
zthe Si of alcosol
xo
x-1(OH)
y(OR)
zthe particle diameter of minuteness particle is 1-10nm.Hexafluoropropylene (HFP)/tetrafluoroethylene (TFE)-vinylidene fluoride copolymers is dispersed in the mixed solvent that the volume ratio of dimethylbenzene, butylacetate and isophorone is 7:2:1 and forms fluorocarbon resin dispersion system, and its solid content is 40 % by weight.By gained Si
xo
x-1(OH)
y(OR)
zalcosol adds in fluorocarbon resin dispersion system, then adds defoamer (commercially available, German Bi Ke BYK-141), and flow agent (commercially available, German Bi Ke BYK-333) also mixes acquisition coating of the present invention.It is the film of approximately 30 microns that gained paint spay-coating is obtained to thickness on steel, after coating surface is dry, is 0.6%(weight by concentration) oxalic acid aqueous solution be sprayed on film, and film is placed in envrionment conditions, so that Si wherein
xo
x-1(OH)
y(OR)
zminuteness particle is further hydrolyzed into Nano particles of silicon dioxide.Final gained coating is tested, and acquired results is in table 1.
(embodiment 4)
Silicic acid four isopropyl esters are added in reactor, then, under the stirring velocity of 200rpm, butanols is added in reactor, the dilute hydrochloric acid that drips 0.07mol/L with the rate of addition of 0.5ml/min is again in reactor, dropwising rear continuation stirs 20 minutes, temperature of reaction kettle is controlled at 20 ℃ with circulated refrigerated water, obtains by Si
2o (OH)
2(OR)
4, Si
3o
2(OH)
2(OR)
6, Si
3o
2(OH)
3(OR)
5the water white Si of sol particles composition
xo
x-1(OH)
y(OR)
zalcosol mixture.Particle size analyzer measuring result shows gained Si
xo
x-1(OH)
y(OR)
zthe Si of alcosol
xo
x-1(OH)
y(OR)
zthe particle diameter of minuteness particle is 3-9nm.Tetrafluoroethylene-vinylidene-acrylic copolymer is dispersed in the mixed solvent that the volume ratio of dimethylbenzene, butylacetate and isophorone is 7:2:1 and forms fluorocarbon resin dispersion system, and its solid content is 40 % by weight.By gained Si
xo
x-1(OH)
y(OR)
zalcosol adds in fluorocarbon resin dispersion system, then adds defoamer (commercially available, German Bi Ke BYK-141), and flow agent (commercially available, German Bi Ke BYK-333) also mixes acquisition coating of the present invention.It is the film of approximately 30 microns that gained paint spay-coating is obtained to thickness on steel, after coating surface is dry, is 2%(weight by concentration) the propionic acid aqueous solution be sprayed on film, and film is placed in envrionment conditions, so that Si wherein
xo
x-1(OH)
y(OR)
zminuteness particle is further hydrolyzed into Nano particles of silicon dioxide.Final gained coating is tested, and acquired results is in table 1.
Performance test
Test event: resistance to wiping examination performance, uvioresistant
Test result: as shown in table 1 below
Table 1
| ? | The outward appearance of coating | Resistance to wiping examinationPerformance improves multiple | The uvioresistant time (h) |
| Embodiment 1 | Smooth | 9 | 600 |
| Embodiment 2 | Smooth | 4 | 350 |
| Embodiment 3 | Smooth | 11 | 660 |
| Embodiment 4 | Smooth | 7 | 450 |
Table 1 shows by coating gained coatingsurface of the present invention smooth, and shows the scrub resistance, intensity, hardness etc. that improve coating; Take into account the anti-ultraviolet aging experimental performance that improves coating.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a preparation method for high-performance coating, said method comprising the steps of:
1) under stirring, Organic Alcohol is mixed into positive Alkoxysilanes Si (OR) is housed
4reactor in, then drip diluted acid or diluted alkaline to solution, temperature of reaction is controlled to room temperature with circulated refrigerated water, stir 10-20min, obtain that to contain structural formula be Si
xo
x-1(OH)
x-1(OR)
x-1the alcosol of sol particles, hereinafter referred to as Si
xo
x-1(OH)
y(OR)
zalcosol, wherein:
X is greater than 0 integer;
Z is greater than 0 integer;
2x-2=y+z; With
R represents to have the straight or branched alkyl of 2-9 carbon atom;
2) by Si
xo
x-1(OH)
y(OR)
zalcosol, film-forming components, pigment and filler and auxiliary agent mix in solvent;
3) discharging, packing;
Positive Alkoxysilanes Si (OR) in described step 1)
4for tetraethoxy, positive isopropyl silicate, a kind of in the positive silicon ester of the tetrabutyl;
In described step 1), in positive Alkoxysilanes and diluted acid or diluted alkaline, the mol ratio of water is 1:0.1-5;
In described step 1), diluted acid or diluted alkaline rate of addition are 0.2-8ml/min;
In described step 1), Organic Alcohol is the one in ethanol, propyl alcohol or butanols;
In described step 1), diluted acid is dilute hydrochloric acid or dilute sulphuric acid, and diluted alkaline is weak ammonia, and the volumetric molar concentration of dilute hydrochloric acid or dilute sulphuric acid or weak ammonia is: 0.001-1mol/L;
In described step 1), film-forming components is fluorocarbon resin.
2. the preparation method of high-performance coating according to claim 1, is characterized in that: in described step 1), R represents to have the straight or branched alkyl of 2-6 carbon atom.
3. the preparation method of high-performance coating according to claim 1, is characterized in that: in described step 1), R represents ethyl.
4. the preparation method of high-performance coating according to claim 1, is characterized in that: in described step 1), diluted acid is dilute hydrochloric acid or dilute sulphuric acid, and diluted alkaline is weak ammonia, and the volumetric molar concentration of dilute hydrochloric acid or dilute sulphuric acid or weak ammonia is: 0.01-0.5mol/L.
5. the preparation method of high-performance coating according to claim 1, is characterized in that: in described step 1), diluted acid is dilute hydrochloric acid or dilute sulphuric acid, and diluted alkaline is weak ammonia, and the volumetric molar concentration of dilute hydrochloric acid or dilute sulphuric acid or weak ammonia is: 0.05-0.1mol/L.
6. the preparation method of high-performance coating according to claim 1, is characterized in that: in step 1), in positive Alkoxysilanes and diluted acid or diluted alkaline, the mol ratio of water is 1:0.2-4.
7. the preparation method of high-performance coating according to claim 1, is characterized in that: in step 1), in positive Alkoxysilanes and diluted acid or diluted alkaline, the mol ratio of water is 1:0.3-3.
8. the preparation method of high-performance coating according to claim 1, is characterized in that: in step 1), diluted acid or diluted alkaline rate of addition are 0.3-6ml/min.
9. the preparation method of high-performance coating according to claim 1, is characterized in that: in step 1), diluted acid or diluted alkaline rate of addition are 0.5-3ml/min.
10. the preparation method of high-performance coating according to claim 1, is characterized in that: Si in step 1)
xo
x-1(OH)
y(OR)
zthe structural formula of alcosol is Si
xo
x-1(OH)
y(OR)
zthe particle diameter of sol particles be 1-10nm.
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| CN106634563B (en) * | 2016-11-09 | 2020-10-23 | 科派股份有限公司 | Nontoxic anticorrosion mildew-proof nano coating and preparation and application methods thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87107834A (en) * | 1986-10-03 | 1988-07-27 | Ppg工业公司 | Organo-siloxane/metal oxide coating |
| US5035745A (en) * | 1990-06-29 | 1991-07-30 | Ppg Industries, Inc. | Ion-exchanged abrasion resistant coatings |
| CN101368066A (en) * | 2008-10-13 | 2009-02-18 | 南京大学 | Organosilane zinc-rich paint |
| CN101985536A (en) * | 2010-10-25 | 2011-03-16 | 江苏考普乐新材料股份有限公司 | Fluorocarbon paint and preparation method thereof |
| CN102079949A (en) * | 2010-12-22 | 2011-06-01 | 李志� | Preparation method of nanometer aerogel heat-insulation coating |
-
2011
- 2011-06-23 CN CN201110170247.4A patent/CN102838894B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87107834A (en) * | 1986-10-03 | 1988-07-27 | Ppg工业公司 | Organo-siloxane/metal oxide coating |
| US5035745A (en) * | 1990-06-29 | 1991-07-30 | Ppg Industries, Inc. | Ion-exchanged abrasion resistant coatings |
| CN101368066A (en) * | 2008-10-13 | 2009-02-18 | 南京大学 | Organosilane zinc-rich paint |
| CN101985536A (en) * | 2010-10-25 | 2011-03-16 | 江苏考普乐新材料股份有限公司 | Fluorocarbon paint and preparation method thereof |
| CN102079949A (en) * | 2010-12-22 | 2011-06-01 | 李志� | Preparation method of nanometer aerogel heat-insulation coating |
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