CN107083088A - A kind of organic fluorine silicon hybrid inorganic silicate coating and its preparation method and application - Google Patents
A kind of organic fluorine silicon hybrid inorganic silicate coating and its preparation method and application Download PDFInfo
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- CN107083088A CN107083088A CN201710348126.1A CN201710348126A CN107083088A CN 107083088 A CN107083088 A CN 107083088A CN 201710348126 A CN201710348126 A CN 201710348126A CN 107083088 A CN107083088 A CN 107083088A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
- C09D1/02—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates
- C09D1/04—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates with organic additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/10—Esters
- C08F120/22—Esters containing halogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/42—Introducing metal atoms or metal-containing groups
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1606—Antifouling paints; Underwater paints characterised by the anti-fouling agent
- C09D5/1637—Macromolecular compounds
Abstract
The invention belongs to technical field of paint preparation, a kind of organic fluorine silicon hybrid inorganic silicate coating is disclosed.The coating is made up of the component of following parts by weight meter：100 parts of inorganic silicic acid salting liquid；1~30 part of organic fluorinated silicone polymer emulsion；1~30 part of organic fluorinated silicone inorganic hybrid polymer emulsion；5~50 parts of water；0.5~5 part of defoamer；0.5~5 part of dispersant；0.05~5 part of levelling agent；10~60 parts of filler.The invention also discloses its preparation method.Organic fluorine silicon hybrid inorganic silicate coating of the present invention has good pliability, water resistance, resistance to acids and bases, alkali resistance 48h is without exception, abrasion resistance (1200 times without show-through), it is effective prevent coating cracking in use, come off, dry linting the problems such as, had a wide range of applications in hydrophobic, the high antifouling building inside and outside wall field of height.
Description
Technical field
The invention belongs to inorganic silicate paint field, more particularly to a kind of organic fluorine silicon hybrid inorganic silicate coating and
Its preparation method and application.
Background technology
At present, commercially available inorganic silicate coating is usually using inorganic silicate as film forming matter, and inorganic silicate has
Abundant raw material, pollution-free, high temperature resistant and it is ageing-resistant the advantages of, meet Contemporary Architecture material energy-conservation and environmental protection requirement.Although nothing
Machine coating has many advantages, such as, but due to having many trickle cavities in coating, with the extension of use time, building table
Dust, the organic matter in face etc. are constantly deposited, and this can cause the decorative effect of coating to substantially reduce.And with urban skyscraper
Development, the presence of pollutant brings negative effect to the cleaning of building.It is all these all to have impact on inorganic silicate coating
Large-scale application.
Organic fluorinated silicone polymer has low-surface-energy, high thermal stability, chemical inertness (acid and alkali-resistance, solvent resistance) etc. excellent
Point, is widely used in fields such as coating, marine anti-pollution, fabric finishing agents.The coating of organic fluorinated silicone modified mistake is in film forming
When, wherein fluoroalkane group and siloxane group can be migrated to the surface of film, significantly reduced the surface energy of film, played thin
Water automatically cleaning effect.And organic fluorinated silicone polymer is generally oil-soluble polymers, it is difficult to be added in aqueous coating system.
The content of the invention
To solve the shortcoming and deficiency of above-mentioned prior art, primary and foremost purpose of the invention is to provide a kind of Organic fluoride sila
Change inorganic silicate coating.The present invention is by adding organic fluorinated silicone polymer emulsion, organic fluorinated silicone-inorganic hybrid polymer emulsion
Enter into coating, so as to reach high hydrophobic, high antifouling effect, meet need of the inorganic silicate coating in building inner-outer wall
Ask.
Another object of the present invention is to provide the preparation method of above-mentioned organic fluorine silicon hybrid inorganic silicate coating.
It is still another object of the present invention to provide the application of above-mentioned organic fluorine silicon hybrid inorganic silicate coating.
The purpose of the present invention is realized by following proposal：
A kind of organic fluorine silicon hybrid inorganic silicate coating, is made up of the component of following parts by weight：
The sodium silicate aqueous solution and/or modulus that the described preferred modulus of inorganic silicic acid salting liquid is 1.0~6.0 be 1.0~
6.0 potassium silicate aqueous solution.
Described organic fluorinated silicone polymer emulsion is made by following steps：80~100 parts by weight water, 3~6 parts by weight are cloudy
Ionic emulsifying agent, the mixing of 2~4 parts by weight nonionic emulsifiers, nitrogen protection add 1~50 parts by weight fluorochemical monomer, 2~10
Parts by weight mercaptosilane coupling agents, quickly stir 0.5~2h pre-emulsifications, then 0.5~3.0 parts by weight initiator of addition, 70~
90 DEG C of 2~9h of reaction, obtain organic fluorinated silicone polymer emulsion；
Described anion emulsifier is lauryl sodium sulfate, dodecyl sodium sulfate, neopelex, ten
At least one of six alkyl benzene sulphonates or octadecyl benzenesulfonic acid；
Described nonionic emulsifier is polyoxyethylene alkyl ether, alkylphenol-polyethenoxy base ether or polyoxyethylene sorbitol
At least one of acid anhydride stearate；
Described fluorochemical monomer be trifluoroethyl methacrylate, Hexafluorobutyl mathacrylate, hexafluorobutyl acrylate,
At least one of dodecafluoroheptyl methacrylate or the trifluoro monooctyl ester of methacrylic acid ten；
Described mercaptosilane coupling agents are mercaptopropyl trimethoxysilane and/or mercaptopropyltriethoxysilane；
Described initiator is ammonium persulfate and/or potassium peroxydisulfate.
Obtained organic fluorinated silicone-inorganic hybrid polymer has structure shown in formula I：
Wherein R1For hydrogen or methyl, RfFor the alkyl of 1~6 fluorine-containing carbon atom, n is 4~2000.
Described organic fluorinated silicone-inorganic hybrid polymer emulsion is made by following steps：In the organic of 88~170 parts by weight
1~20 parts by weight organosiloxane and 0.5~10.0 part by weight of catalyst, 30~60 DEG C of stirrings are added in silicon-fluorine polymer thing emulsion
0.5~6.0h is reacted, that is, obtains organic fluorinated silicone-inorganic hybrid polymer emulsion；
Described organosiloxane is tetraethyl orthosilicate, methyl silicate, MTMS, methyl triethoxy
At least one of silane, dimethyldimethoxysil,ne or dimethyldiethoxysilane；
Described catalyst is acid or base catalyst, and described acidic catalyst is hydrochloric acid and/or acetic acid, described
Base catalyst is at least one of ammoniacal liquor, sodium hydroxide, potassium hydroxide or 2- amino-2-methyl propyl alcohol；
Obtained organic fluorinated silicone polymer has the structure as shown in formula II：
Wherein R1For hydrogen or methyl, R2For methyl or ethyl, RfFor the alkyl of 1~6 fluorine-containing carbon atom, n is 4~
2000。
In the composition of raw materials of organic fluorine silicon hybrid inorganic silicate coating of the present invention, described defoamer refers to mineral oils
Defoamer and/or polysiloxane-based defoamer；Described dispersant refers in acrylates, polyacrylate or carboxylic acid sodium salt extremely
Few one kind；Described levelling agent refers to acrylic compounds levelling agent；Described filler refers to precipitated calcium carbonate, titanium dioxide, silica
At least one of or titanium dioxide.
The preparation method of above-mentioned organic fluorine silicon hybrid inorganic silicate coating, is comprised the steps of：
By inorganic silicic acid salting liquid, water, organic fluorinated silicone polymer emulsion and organic fluorinated silicone-inorganic hybrid polymer emulsion,
Once be added in reactor, at 30~80 DEG C react 2~10 hours, be cooled to after room temperature, obtain organic fluorine silicon hybrid without
Machine silicate solutions；Then defoamer, dispersant, levelling agent are added, after stirring, filler is added, is uniformly dispersed, produce
To organic fluorine silicon hybrid inorganic silicate coating.
The organic fluorine silicon hybrid inorganic silicate coating of the present invention can be applied in high hydrophobic, high antifouling building inside and outside wall
On.
The present invention mechanism be：A kind of organic fluorinated silicone polymer emulsion is prepared for by emulsion polymerization first, then had
The method of machine silicon-fluorine polymer thing emulsion situ generation inorganic phase is prepared for a kind of organic fluorinated silicone-inorganic hybrid polymer emulsion,
The organic fluorinated silicone polymer emulsion and organic fluorinated silicone-inorganic hybrid polymer emulsion is recycled to be prepared for a kind of hydrophobic, Gao Fang of height
Dirty inorganic silicate coating.Using its long side chain fluoro-containing group effective mobility to coating surface, improve the water resistance, resistance to of coating
Staining therefore prepared coating not only has weatherability, water resistance, resistance to acids and bases, can also solve coating in construction
Ftracture, come off, dry linting the problems such as, and with excellent high hydrophobicity and high soil resistance.
The present invention has the following advantages and beneficial effect relative to prior art：
(1) present invention is prepared for a kind of organic fluorinated silicone polymer emulsion by emulsion polymerization first, then miscellaneous by molecule
Change technology is prepared for a kind of organic fluorinated silicone-inorganic hybrid polymer emulsion, and hydridization is further then carried out with inorganic silicate obtains
To the hybrid solution with high hydrophobicity energy, and by the use of the hydridization solution as main film forming substance, it have developed a kind of high thin
Water, high antifouling organic fluorine silicon hybrid inorganic silicate coating.
(2) long side chain fluoro-containing group is contained in organic fluorine silicon hybrid inorganic silicate coating of the present invention, in coating
In film forming procedure, long side chain moves to coating surface, effectively improves contact angle on surface of coating (between 105~145 °) so that system
Standby organic fluorine silicon hybrid inorganic silicate coating has high hydrophobic, high antifouling effect.
(3) organic fluorine silicon hybrid inorganic silicate coating of the present invention has water resistance, resistance to acids and bases, alkali resistance
48h is without exception, abrasion resistance (1200 times without show-through), effectively prevent the cracking of coating, come off, dry linting the problems such as.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Embodiment 1
The preparation of organic fluorine silicon hybrid inorganic silicate coating, comprises the following steps：
(1) preparation of organic fluorinated silicone polymer emulsion
80g deionized waters, 3g are added in the reaction vessel equipped with thermometer, condenser pipe, agitator and nitrogen access tube
Dodecyl sodium sulfate, 2g alkylphenol-polyethenoxy base ethers, stirs at 70 DEG C, then adds 5g methacrylic acid trifluoro second
Ester and 1g mercaptopropyl trimethoxysilanes, quick stirring pre-emulsification 30min, add 0.5g ammonium persulfates and (are dissolved in 10g deionizations
In water), air cooling discharges after reacting 9h at 70 DEG C.
(2) preparation of organic fluorinated silicone-inorganic hybrid polymer emulsion：
2g methyl silicates and 8g ammoniacal liquor, 30 DEG C of stirring reaction 5h are added in the emulsion obtained by step (1), that is, are had
Machine fluorine silicon-inorganic hybrid polymer emulsion.
(3) sodium silicate aqueous solution, 5 parts by weight water, 5 parts by weight organic fluorinated silicone polymer that 100 parts by weight moduluses are 1.5 are taken
Emulsion and 5 parts by weight organic fluorinated silicone-inorganic hybrid polymer emulsion, are once added in reactor, small in reaction 2 at 30 DEG C
When, it is cooled to after room temperature, obtains organic fluorinated silicone-inorganic hybridization silicate solutions；Then 0.5 parts by weight mineral oils froth breaking is added
Agent, 0.5 parts by weight of acrylic acid dipersant, 0.1 parts by weight propylene acids levelling agent, after stirring, add 10 parts by weight
Precipitated calcium carbonate, is uniformly dispersed, you can obtain the organic fluorine silicon hybrid inorganic silicate coating.
The coating is subjected to film with flush coater, carries out testing its performance according to JGT26-2002 standards.Test result is such as
Under：Surface drying time 1.8h；Workability：Brushing second is accessible；Appearance of film is normal；Alkali resistance 48h is without exception；Washability
Property：2000 times without show-through；Contrast ratio：0.95, stain resistance is 4% (≤15%, reach the II levels standard in JGT26-2002),
Contact angle：110°.
Embodiment 2
The preparation of organic fluorine silicon hybrid inorganic silicate coating, comprises the following steps：
(1) preparation of organic fluorinated silicone polymer emulsion
100g deionized waters, 4g are added in the reaction vessel equipped with thermometer, condenser pipe, agitator and nitrogen access tube
Dodecyl sodium sulfate, 2g alkylphenol-polyethenoxy base ethers, stirs at 80 DEG C, then adds 10g methacrylic acid hexafluoros
Butyl ester and 2g mercaptopropyl trimethoxysilanes, quick stirring pre-emulsification 30min, add 1g ammonium persulfates and (are dissolved in 10g deionizations
In water), air cooling discharges after reacting 6h at 80 DEG C.
(2) preparation of organic fluorinated silicone-inorganic hybrid polymer emulsion：
5g tetraethyl orthosilicates and 4g ammoniacal liquor, 60 DEG C of stirring reaction 0.5h are added in the emulsion obtained by step (1), that is, are obtained
Organic fluorinated silicone-inorganic hybrid polymer emulsion.
(3) sodium silicate aqueous solution, 5 parts by weight water, 30 parts by weight the organic fluorinated silicones polymerization that 100 parts by weight moduluses are 1.5 are taken
Thing emulsion and 5 parts by weight organic fluorinated silicone-inorganic hybrid polymer emulsion, are once added in reactor, in reacting 10 at 30 DEG C
Hour, it is cooled to after room temperature, obtains organic fluorinated silicone-inorganic hybridization silicate solutions；Then 1 parts by weight mineral oils froth breaking is added
Agent, 1 parts by weight of acrylic acid dipersant, 0.1 parts by weight propylene acids levelling agent, after stirring, add 20 parts by weight two
Silica, is uniformly dispersed, you can obtain the organic fluorine silicon hybrid inorganic silicate coating.
The coating is subjected to film with flush coater, carries out testing its performance according to JGT26-2002 standards.Test result is such as
Under：Surface drying time 1.5h；Workability：Brushing second is accessible；Appearance of film is normal；Alkali resistance 48h is without exception；Washability
Property：2000 times without show-through；Contrast ratio：0.95, stain resistance is 3% (≤15%, reach the II levels standard in JGT26-2002),
Contact angle：125°.
Embodiment 3
The preparation of organic fluorine silicon hybrid inorganic silicate coating, comprises the following steps：
(1) preparation of organic fluorinated silicone polymer emulsion
100g deionized waters, 6g are added in the reaction vessel equipped with thermometer, condenser pipe, agitator and nitrogen access tube
Dodecyl sodium sulfate, 4g alkylphenol-polyethenoxy base ethers, stirs at 90 DEG C, then adds 50g methacrylic acids 12
Fluorine heptyl ester and 10g mercaptopropyltriethoxysilanes, quick stirring pre-emulsification 1h, add 3g potassium peroxydisulfates and (are dissolved in 10g deionizations
In water), air cooling discharges after reacting 3h at 90 DEG C.
(2) preparation of organic fluorinated silicone-inorganic hybrid polymer emulsion：
20g MTESs and 5g sodium hydroxides, 30 DEG C of stirring reactions are added in the emulsion obtained by step (1)
6h, that is, obtain organic fluorinated silicone-inorganic hybrid polymer emulsion.
(3) potassium silicate aqueous solution, 50 parts by weight water, 15 parts by weight organic fluorinated silicone polymer that 100 parts by weight moduluses are 6 are taken
Emulsion and 15 parts by weight organic fluorinated silicone-inorganic hybrid polymer emulsion, are once added in reactor, small in reaction 2 at 80 DEG C
When, it is cooled to after room temperature, obtains organic silicon-fluorine-inorganic hybridization silicate solutions；Then 3 parts by weight silicone antifoams are added
Agent, 3 parts by weight of acrylic acid dipersants, 2 parts by weight propylene acids levelling agents, after stirring, add 10 parts by weight lightweights
Calcium carbonate, 20 parts by weight of titanium dioxide, 10 parts by weight of silica, are uniformly dispersed, you can obtain the organic fluorine silicon hybrid without
Machine silicate paint.
The coating is subjected to film with flush coater, carries out testing its performance according to JGT26-2002 standards.Test result is such as
Under：Surface drying time 0.6h；Workability：Brushing second is accessible；Appearance of film is normal；Alkali resistance 48h is without exception；Washability
Property：2000 times without show-through；Contrast ratio：0.97, stain resistance be 1.5% (≤15%, reach that II levels in JGT26-2002 are marked
It is accurate), contact angle：140°.
Embodiment 4
The preparation of organic fluorine silicon hybrid inorganic silicate coating, comprises the following steps：
(1) preparation of organic fluorinated silicone polymer emulsion：
80g deionized waters, 3g are added in the reaction vessel equipped with thermometer, condenser pipe, agitator and nitrogen access tube
Neopelex, 2g polyoxyethylene alkyl ethers stir at 80 DEG C, then add the trifluoro of 20g methacrylic acids ten
Monooctyl ester and 4g mercaptopropyltriethoxysilanes, quick stirring pre-emulsification 30min, add 1g potassium peroxydisulfates and (are dissolved in 10g deionizations
In water), air cooling discharges after reacting 3h at 80 DEG C.
(2) preparation of organic fluorinated silicone-inorganic hybrid polymer emulsion：
10g MTMSs and 5g potassium hydroxide, 60 DEG C of stirring reactions are added in the emulsion obtained by step (1)
3h, that is, obtain organic fluorinated silicone-inorganic hybrid polymer emulsion.
(3) potassium silicate aqueous solution, 20 parts by weight water, 10 parts by weight organic fluorinated silicone polymer that 100 parts by weight moduluses are 3 are taken
Emulsion and 25 parts by weight organic fluorinated silicone-inorganic hybrid polymer emulsion, are once added in reactor, small in reaction 5 at 60 DEG C
When, it is cooled to after room temperature, obtains organic silicon-fluorine-inorganic hybridization silicate solutions；Then 5 parts by weight silicone antifoams are added
Agent, 5 parts by weight of acrylic acid dipersants, 4 parts by weight propylene acids levelling agents, after stirring, add 30 parts by weight dioxies
Change titanium, 20 parts by weight of silica, be uniformly dispersed, you can obtain the organic fluorine silicon hybrid inorganic silicate coating.
The coating is subjected to film with flush coater, carries out testing its performance according to JGT26-2002 standards.Test result is such as
Under：Surface drying time 1h；Workability：Brushing second is accessible；Appearance of film is normal；Alkali resistance 48h is without exception；Washability
Property：2000 times without show-through；Contrast ratio：0.98, stain resistance be 1.0% (≤15%, reach that II levels in JGT26-2002 are marked
It is accurate), contact angle：145°.
Embodiment 5
The preparation of organic fluorine silicon hybrid inorganic silicate coating, comprises the following steps：
(1) preparation of organic fluorinated silicone polymer emulsion：
100g deionized waters, 4g are added in the reaction vessel equipped with thermometer, condenser pipe, agitator and nitrogen access tube
Dodecyl sodium sulfate, 3g alkylphenol-polyethenoxy base ethers, stirs at 80 DEG C, then adds 30g hexafluorobutyl acrylates
With 6g mercaptopropyltriethoxysilanes, quick stirring pre-emulsification 45min adds 3g potassium peroxydisulfates and (is dissolved in 10g deionized waters
In), air cooling discharges after reacting 6h at 80 DEG C.
(2) preparation of organic fluorinated silicone-inorganic hybrid polymer emulsion：
15g dimethyldiethoxysilanes and 5g acetic acid, 50 DEG C of stirring reactions are added in the emulsion obtained by step (1)
4h, that is, obtain organic fluorinated silicone-inorganic hybrid polymer emulsion.
(3) sodium silicate aqueous solution, 20 weights that sodium silicate aqueous solution, 30 parts by weight moduluses that 50 parts by weight moduluses are 1 are 3 are taken
Measure sodium silicate aqueous solution, 30 parts by weight water and 30 parts by weight organic fluorinated silicone-inorganic hybrid polymer emulsion, one that part modulus is 2
It is secondary to be added in reactor, in being reacted 6 hours at 50 DEG C, it is cooled to after room temperature, obtains organic fluorinated silicone-inorganic hybridization silicate molten
Liquid；Then 3 parts by weight mineral oil defoaming agents, 3 parts by weight of acrylic acid dipersants, 5 parts by weight propylene acids levelling agents are added,
After stirring, 30 parts by weight titanium dioxides are added, are uniformly dispersed, you can obtained the organic fluorine silicon hybrid inorganic silicate and apply
Material.
The coating is subjected to film with flush coater, carries out testing its performance according to JGT26-2002 standards.Test result is such as
Under：Surface drying time 1.2h；Workability：Brushing second is accessible；Appearance of film is normal；Alkali resistance 48h is without exception；Washability
Property：2000 times without show-through；Contrast ratio：0.96, stain resistance is 2% (≤15%, reach the II levels standard in JGT26-2002),
Contact angle：135°
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by above-described embodiment of the invention
Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of organic fluorine silicon hybrid inorganic silicate coating, it is characterised in that：It is made up of the component of following parts by weight：
Described organic fluorinated silicone polymer emulsion is made by following steps：By 80~100 parts by weight water, 3~6 parts by weight anion
Emulsifying agent, the mixing of 2~4 parts by weight nonionic emulsifiers, nitrogen protection add 1~50 parts by weight fluorochemical monomer, 2~10 weight
Part mercaptosilane coupling agents, quickly stir 0.5~2h pre-emulsifications, then add 0.5~3.0 parts by weight initiator, 70~90 DEG C
2~9h is reacted, organic fluorinated silicone polymer emulsion is obtained；
Described organic fluorinated silicone-inorganic hybrid polymer emulsion is made by following steps：In the organic fluorinated silicone of 88~170 parts by weight
1~20 parts by weight organosiloxane and 0.5~10.0 part by weight of catalyst, 30~60 DEG C of stirring reactions are added in polymer emulsion
0.5~6.0h, that is, obtain organic fluorinated silicone-inorganic hybrid polymer emulsion.
2. organic fluorine silicon hybrid inorganic silicate coating according to claim 1, it is characterised in that：
Described anion emulsifier is lauryl sodium sulfate, dodecyl sodium sulfate, neopelex, hexadecane
At least one of base benzene sulfonic acid or octadecyl benzenesulfonic acid；
Described nonionic emulsifier is that polyoxyethylene alkyl ether, alkylphenol-polyethenoxy base ether or polyoxyethylene sorbitol acid anhydride are hard
At least one of resin acid ester；
Described fluorochemical monomer is trifluoroethyl methacrylate, Hexafluorobutyl mathacrylate, hexafluorobutyl acrylate, methyl
At least one of dodecafluorhe-ptylacrylate or the trifluoro monooctyl ester of methacrylic acid ten；
Described mercaptosilane coupling agents are mercaptopropyl trimethoxysilane and/or mercaptopropyltriethoxysilane；
Described initiator is ammonium persulfate and/or potassium peroxydisulfate.
3. organic fluorine silicon hybrid inorganic silicate coating according to claim 1, it is characterised in that：
Described organosiloxane is tetraethyl orthosilicate, methyl silicate, MTMS, methyltriethoxy silane
At least one of alkane, dimethyldimethoxysil,ne or dimethyldiethoxysilane；
Described catalyst is acid or base catalyst, and described acidic catalyst is hydrochloric acid and/or acetic acid, described alkalescence
Catalyst is at least one of ammoniacal liquor, sodium hydroxide, potassium hydroxide or 2- amino-2-methyl propyl alcohol.
4. organic fluorine silicon hybrid inorganic silicate coating according to claim 1, it is characterised in that：Described inorganic silicic acid
Salting liquid is the potassium silicate aqueous solution that the sodium silicate aqueous solution and/or modulus that modulus is 1.0~6.0 are 1.0~6.0.
5. organic fluorine silicon hybrid inorganic silicate coating according to claim 1, it is characterised in that：Described defoamer refers to
Mineral oil defoaming agent and/or polysiloxane-based defoamer.
6. organic fluorine silicon hybrid inorganic silicate coating according to claim 1, it is characterised in that：Described dispersant refers to
At least one of acrylates, polyacrylate or carboxylic acid sodium salt.
7. organic fluorine silicon hybrid inorganic silicate coating according to claim 1, it is characterised in that：Described levelling agent refers to
Acrylic compounds levelling agent.
8. organic fluorine silicon hybrid inorganic silicate coating according to claim 1, it is characterised in that：Described filler refers to gently
At least one of matter calcium carbonate, titanium dioxide, silica or titanium dioxide.
9. the preparation method of the organic fluorine silicon hybrid inorganic silicate coating described in claim any one of 1-8, it is characterised in that
Comprise the steps of：
By inorganic silicic acid salting liquid, water, organic fluorinated silicone polymer emulsion and organic fluorinated silicone-inorganic hybrid polymer emulsion, once
It is added in reactor, in being reacted 2~10 hours at 30~80 DEG C, is cooled to after room temperature, obtains organic fluorine silicon hybrid inorganic silicon
Acid salt solution；Then defoamer, dispersant, levelling agent are added, after stirring, filler is added, is uniformly dispersed, that is, had
Machine fluorine silicon hybridization inorganic silicate coating.
10. the organic fluorine silicon hybrid inorganic silicate coating described in claim any one of 1-8 is in high hydrophobic, high antifouling building
Application in inner-outer wall.
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| CN107779090A (en) * | 2017-10-18 | 2018-03-09 | 厦门固克涂料集团有限公司 | Coating of the compound organic fluorinated silicone of inorganic silicic acid lithium potassium solution and preparation method thereof |
| CN108084751A (en) * | 2017-12-21 | 2018-05-29 | 中科院广州化学有限公司 | A kind of fluorine-containing titanium colloidal sol, inorganic silicate coating and preparation method thereof |
| CN108752590A (en) * | 2018-04-25 | 2018-11-06 | 中科广化（重庆）新材料研究院有限公司 | A kind of long-chain siloxy flucride siloxane lotion and its modified inorganic silicate coating and preparation method thereof |
| CN109503846A (en) * | 2018-11-29 | 2019-03-22 | 中科院广州化学有限公司南雄材料生产基地 | A kind of titaniferous colloidal sol organosiloxane hybridisation emulsion and modified Portland coating |
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| CN115044259A (en) * | 2022-05-27 | 2022-09-13 | 昆明璋润涂装工程有限公司 | Micro cement coating and construction method thereof |
| CN115627086A (en) * | 2022-09-29 | 2023-01-20 | 广州先进技术研究所 | High-temperature-resistant wide-spectrum super-lyophobic coating and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2019062083A1 (en) * | 2017-09-28 | 2019-04-04 | 洛阳尖端技术研究院 | Superhydrophobic coating layer, preparation method therefor and application thereof |
| CN107779090A (en) * | 2017-10-18 | 2018-03-09 | 厦门固克涂料集团有限公司 | Coating of the compound organic fluorinated silicone of inorganic silicic acid lithium potassium solution and preparation method thereof |
| CN108084751A (en) * | 2017-12-21 | 2018-05-29 | 中科院广州化学有限公司 | A kind of fluorine-containing titanium colloidal sol, inorganic silicate coating and preparation method thereof |
| CN108752590A (en) * | 2018-04-25 | 2018-11-06 | 中科广化（重庆）新材料研究院有限公司 | A kind of long-chain siloxy flucride siloxane lotion and its modified inorganic silicate coating and preparation method thereof |
| CN108752590B (en) * | 2018-04-25 | 2021-08-13 | 中科广化（重庆）新材料研究院有限公司 | Long-chain silicon-oxygen-based fluorine-containing siloxane emulsion, modified inorganic silicate coating thereof and preparation method thereof |
| CN109503846A (en) * | 2018-11-29 | 2019-03-22 | 中科院广州化学有限公司南雄材料生产基地 | A kind of titaniferous colloidal sol organosiloxane hybridisation emulsion and modified Portland coating |
| CN115044259A (en) * | 2022-05-27 | 2022-09-13 | 昆明璋润涂装工程有限公司 | Micro cement coating and construction method thereof |
| CN115627086A (en) * | 2022-09-29 | 2023-01-20 | 广州先进技术研究所 | High-temperature-resistant wide-spectrum super-lyophobic coating and preparation method thereof |
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