CN108752590A - A kind of long-chain siloxy flucride siloxane lotion and its modified inorganic silicate coating and preparation method thereof - Google Patents
A kind of long-chain siloxy flucride siloxane lotion and its modified inorganic silicate coating and preparation method thereof Download PDFInfo
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- CN108752590A CN108752590A CN201810378067.7A CN201810378067A CN108752590A CN 108752590 A CN108752590 A CN 108752590A CN 201810378067 A CN201810378067 A CN 201810378067A CN 108752590 A CN108752590 A CN 108752590A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/24—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen halogen-containing groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
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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
- 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, disclose a kind of long-chain siloxy flucride siloxane lotion and its modified inorganic silicate coating and preparation method.The emulsion modified inorganic silicate coating of long-chain siloxy flucride siloxane is grouped as by the group of following parts by weight meter：100 parts of inorganic silicic acid salting liquid；2~30 parts of long-chain siloxy flucride siloxane lotion；10~50 parts of water；0.5~4 part of antifoaming agent；0.5~4 part of dispersant；0.1~4 part of levelling agent；100~200 parts of filler.Invention additionally discloses preparation methods.Roller coating can be used in inorganic silicate coating of the present invention, the techniques such as spraying and brushing, surface contact angle is up to 100~145 °, water resistance, resistance to acid and alkali, wherein alkali resistance 48h is without exception, and abrasion resistance (1200 times without show-through), it effective the problems such as preventing coating cracking in use, falling off, lose powder, is had a wide range of applications in high hydrophobic, the 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 long-chain siloxy flucride siloxane lotion and its
Modified inorganic silicate coating and preparation method.
Background technology
Currently, commercially available inorganic silicate coating is using inorganic silicate as film forming matter, while inorganic silicate has
Raw material sources are abundant, high temperature resistant, it is ageing-resistant and pollution-free the advantages that, meet the energy saving and environmentally friendly requirement of Contemporary Architecture material.Though
So inorganic silicate coating has many advantages, such as, but due to having many subtle cavities in coating, with prolonging for usage time
Long, dust, organic matter of building surface etc. constantly deposit, this can substantially reduce the decorative effect of coating.And with city height
The development of layer building, the presence of pollutant bring negative effect to the cleaning of building.It is all these all to affect inorganic silicon
The large-scale application of phosphate coating material.
Organosilicon, the functions segment such as Organic fluoride are introduced in inorganic silicate coating, due to introduced in molecule bond energy compared with
Big Si-O keys and C-F keys, can be greatly reduced the surface energy of coating, and floor height waterproof, the high performances such as antifouling are applied to assign.Often
The organosilicon containing reactive functional groups seen, organic fluorine monomer are based on silane coupling agent.Organosilicon or Organic fluoride is used alone
Silane coupler modified inorganic silicate coating has the following disadvantages, such as usually its strand is shorter, and modified effect is unknown
It is aobvious；And hydrolysising group activity is larger in silane coupling agent, easily reacts between each other and crosslinks entanglement, steady so as to cause it
It is qualitative poor.If organosilicon and Organic fluoride are carried out modified inorganic silicate coating in a manner of physical mixed between the two, exist
The poor problem of its compatibility.Therefore, if long chain silicone segment and fluorine-containing can simultaneously be introduced in modifier body construction
Group can then improve compatibility between the two and its modified effect.
Invention content
To solve the disadvantage that the above-mentioned prior art and deficiency, the primary purpose of the present invention is that providing a kind of long-chain siloxy
Flucride siloxane lotion and preparation method thereof.Another object of the present invention is to provide a kind of long-chain siloxy flucride siloxane breasts
Liquid modified inorganic silicate coating and preparation method thereof.
The purpose of the present invention is realized by following proposal：
A kind of long-chain siloxy flucride siloxane lotion, the long-chain siloxy flucride siloxane lotion have such as I institute of formula
The chemical structural formula shown：
Wherein, R1、R2Be methyl alkoxy, ethyl alkoxy, hydroxyl orRfIt is that there is 1~8
Carbon atom contains fluoroalkyl group, n1、n2It is the natural number that 4-2000 interior energies are divided exactly by 4.
Preferably, the solid content of the lotion is 20%-50%.
A kind of preparation method of long-chain siloxy flucride siloxane lotion, includes the following steps, by 80-160 parts of water, 2-6
Part anion emulsifier, 2-4 parts of nonionic emulsifiers and 6-40 parts of octamethylcy-clotetrasiloxanes are added in reactor, in nitrogen
Under protection, 4-10h is reacted at 60-90 DEG C, 10-40 parts of small molecule flucride siloxanes is added, reacts 2- at 65-90 DEG C
10h obtains long-chain siloxy flucride siloxane lotion.
Preferably, the anion emulsifier is dodecyl benzene sulfonic acid, cetyl benzenesulfonic acid or octadecyl benzene sulphur
At least one of acid.
Preferably, the nonionic emulsifier is alkylphenol-polyethenoxy base ether, polyoxyethylene alkyl ether or polyoxyethylene
At least one of sorbitan tristearate.
Preferably, the small molecule flucride siloxane is trifluoro propyl trimethoxy silane, trifluoro propyl triethoxysilicane
Alkane, hexafluoro butyl propyl trimethoxy silicane, ten difluoro heptyl propyl trimethoxy silicanes, ten trifluoro octyl trimethoxy silicon
In alkane, tridecafluoro-n-octyltriethoxysilane, 17 fluorine ruthenium trimethoxysilanes, 17 fluorine ruthenium triethoxysilanes extremely
Few one kind.
A kind of emulsion modified inorganic silicate coating of long-chain siloxy flucride siloxane is grouped by the group of following parts by weight
At：
Preferably, the sodium silicate aqueous solution and/or modulus that the modulus of the inorganic silicic acid salting liquid is 1.0~6.0 are 1.0
~6.0 potassium silicate aqueous solution.
Preferably, the antifoaming agent refers to mineral oil defoaming agent and/or polysiloxane-based antifoaming agent；The dispersant refers to third
At least one of olefin(e) acid salt, carboxylic acid sodium salt or polyacrylate；The levelling agent refers to acrylic compounds levelling agent；The filler refers to
At least one of titanium dioxide, titanium dioxide, silica or precipitated calcium carbonate.
A kind of preparation method of the emulsion modified inorganic silicate coating of long-chain siloxy flucride siloxane, including following step
Suddenly：Inorganic silicic acid salting liquid, water, long-chain siloxy flucride siloxane lotion are added in reactor, stirred evenly；Then plus
Enter antifoaming agent, dispersant, levelling agent, after stirring evenly, add filler, room temperature disperses 3-12h, uniformly to get to described
The emulsion modified inorganic silicate coating of long-chain siloxy flucride siloxane.
The present invention mechanism be：
The long-chain siloxy flucride siloxane lotion that the present invention uses by and meanwhile introduce the organosilicon of long-chain and containing fluorine-based
Group, makes its effective mobility to coating surface, improves water resistance, the stain resistant of coating, therefore prepared coating not only has
Weatherability, water resistance, resistance to acid and alkali, the problems such as the cracking of coating in construction can also be solved, fall off, lose powder, and with excellent
Different high hydrophobicity and high soil resistance.
The present invention compared with the existing technology, has the following advantages and advantageous effect：
(1) present invention a kind of long-chain siloxy flucride siloxane lotion is prepared for by emulsion polymerization first, then with nothing
Machine silicate further carries out hydridization and obtains the hybrid solution with high hydrophobicity energy, and using the hydridization solution as main
Film forming matter has developed a kind of high hydrophobic, high antifouling inorganic silicate coating.
(2) have containing long-chain in the emulsion modified inorganic silicate coating of long-chain siloxy flucride siloxane of the present invention
Machine silicon and fluoro-containing group, in coating film forming procedure, fluoro-containing group moves to coating surface, effectively improves contact angle on surface of coating
(100 °~145 °) so that the inorganic silicate coating of preparation has the effect of high hydrophobic, high antifouling.
(3) the emulsion modified inorganic silicate coating of long-chain siloxy flucride siloxane of the present invention has water resistance,
Resistance to acid and alkali, alkali resistance 48h is without exception, abrasion resistance (1200 times without show-through), can effectively prevent the cracking of coating, fall off,
The problems such as picking.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Embodiment 1
(1) preparation of long-chain siloxy flucride siloxane lotion
80g deionized waters, 2g ten are added in the reaction vessel being passed through equipped with thermometer, blender, condenser pipe and nitrogen
Dialkyl benzene sulfonic acids, 2g alkylphenol-polyethenoxy base ethers, 10g octamethylcy-clotetrasiloxanes react 9h at 70 DEG C, are then added
15g trifluoro propyl trimethoxy silanes react air-cooled discharging after 9h at 75 DEG C, obtain long-chain siloxy flucride siloxane breast
Liquid, solid content 26%.
(2) preparation of the emulsion modified inorganic silicate coating of long-chain siloxy flucride siloxane
Take the sodium silicate aqueous solution, 10 parts by weight water, the 4 fluorine-containing silica of parts by weight long-chain siloxy that 100 parts by weight moduluses are 2
Alkane lotion, is once added in reaction kettle, stirs evenly；Then 0.5 parts by weight mineral oil defoaming agent, 0.5 parts by weight are added
Acrylates dispersant, 0.2 parts by weight propylene acids levelling agent, after stirring evenly, add 100 parts by weight precipitated calcium carbonates,
Room temperature disperses 3h, is uniformly dispersed, you can obtains the 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：0.94, stain resistance is 4% (≤15%, reach the II grades standard in JGT26-2002),
Contact angle：105°.
Embodiment 2
(1) preparation of long-chain siloxy flucride siloxane lotion
100g deionized waters, 4g ten are added in the reaction vessel being passed through equipped with thermometer, blender, condenser pipe and nitrogen
Six alkyl benzene sulphonates, 3g polyoxyethylene alkylethers, 20g octamethylcy-clotetrasiloxanes react 6h at 80 DEG C, are then added
10g hexafluoro butyl propyl trimethoxy silicanes react air-cooled discharging after 4h at 80 DEG C, obtain long-chain siloxy flucride siloxane
Lotion, solid content 27%.
(2) preparation of the emulsion modified inorganic silicate coating of long-chain siloxy flucride siloxane
Take the potassium silicate aqueous solution, 20 parts by weight water, 10 parts by weight long-chain siloxy fluorine silicons that 100 parts by weight moduluses are 3
Oxygen alkane lotion, is once added in reaction kettle, stirs evenly；Then the polysiloxane-based antifoaming agent of 1 parts by weight, 1 parts by weight are added
Polyacrylic acid dipersant, 1.5 parts by weight propylene acids levelling agents, after stirring evenly, add 150 parts by weight of silica,
Room temperature disperses 4h, is uniformly dispersed, you can obtains the 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：0.96, stain resistance be 3.5% (≤15%, reach II grades in JGT26-2002 and mark
It is accurate), contact angle：125°.
Embodiment 3
(1) preparation of long-chain siloxy flucride siloxane lotion
120g deionized waters, 5g ten are added in the reaction vessel being passed through equipped with thermometer, blender, condenser pipe and nitrogen
Six alkyl benzene sulphonates, 4g polyoxyethylene alkylethers, 40g octamethylcy-clotetrasiloxanes react 4h at 90 DEG C, are then added
17 fluorine ruthenium trimethoxysilanes of 20g react air-cooled discharging after 2h at 90 DEG C, obtain long-chain siloxy flucride siloxane breast
Liquid, solid content 36%.
(2) preparation of the emulsion modified inorganic silicate coating of long-chain siloxy flucride siloxane
Take the potassium silicate aqueous solution, 50 parts by weight water, 30 parts by weight long-chain siloxy fluorine silicons that 100 parts by weight moduluses are 6
Oxygen alkane lotion, is once added in reaction kettle, stirs evenly；Then 4 parts by weight mineral oil defoaming agents, 3 parts by weight third are added
Olefin(e) acid dipersant, 4 parts by weight propylene acids levelling agents after stirring evenly, add 200 parts by weight titanium dioxides, room temperature dispersion
12h is uniformly dispersed, you can obtains the 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 1.2h；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：0.98, stain resistance is 2% (≤15%, reach the II grades standard in JGT26-2002),
Contact angle：145°.
Embodiment 4
(1) preparation of long-chain siloxy flucride siloxane lotion
100g deionized waters, 4g ten are added in the reaction vessel being passed through equipped with thermometer, blender, condenser pipe and nitrogen
Eight alkyl benzene sulphonates, 3g polyoxyethylene sorbitol acid anhydride stearates, 30g octamethylcy-clotetrasiloxanes react 8h, so at 75 DEG C
15g trifluoro propyls trimethoxy silane and ten difluoro heptyl propyl trimethoxy silicanes of 10g are added afterwards, after reacting 6h at 75 DEG C
Air-cooled discharging obtains long-chain siloxy flucride siloxane lotion, solid content 38%.
(2) preparation of the emulsion modified inorganic silicate coating of long-chain siloxy flucride siloxane
Take the sodium silicate aqueous solution that 50 parts by weight moduluses are 4 and the sodium silicate aqueous solution that 50 parts by weight moduluses are 6,30 weight
Part water, 20 parts by weight long-chain siloxy flucride siloxane lotions, are once added in reaction kettle, stir evenly；Then 1 weight is added
Measure part mineral oil defoaming agent and the polysiloxane-based antifoaming agent of 2 parts by weight, 2 parts by weight of acrylic acid dipersants, 2 parts by weight propylene
Acids levelling agent after stirring evenly, adds the silica of 100 parts by weight of titanium dioxide and 50 parts by weight, and room temperature disperses 6h,
It is uniformly dispersed, you can obtain the 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：0.96, stain resistance is 3% (≤15%, reach the II grades standard in JGT26-2002),
Contact angle：135°.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of long-chain siloxy flucride siloxane lotion, which is characterized in that the long-chain siloxy flucride siloxane lotion tool
Just like chemical structural formula shown in formula I：
Wherein, R1、R2Be methyl alkoxy, ethyl alkoxy, hydroxyl orRfIt is that there is 1~8 carbon original
Son contains fluoroalkyl group, n1、n2It is the natural number that 4-2000 interior energies are divided exactly by 4.
2. long-chain siloxy flucride siloxane lotion according to claim 1, which is characterized in that the solid content of the lotion
For 20%-50%.
3. a kind of preparation method of long-chain siloxy flucride siloxane lotion, which is characterized in that include the following steps, by 80-160
Part water, 2-6 parts of anion emulsifiers, 2-4 parts of nonionic emulsifiers and 6-40 parts of octamethylcy-clotetrasiloxanes are added to reactor
In, under nitrogen protection, 4-10h is reacted at 60-90 DEG C, 10-40 parts of small molecule flucride siloxanes is added, in 65-90 DEG C
Lower reaction 2-10h obtains long-chain siloxy flucride siloxane lotion.
4. preparation method according to claim 3, which is characterized in that the anion emulsifier is detergent alkylate sulphur
At least one of acid, cetyl benzenesulfonic acid or octadecyl benzenesulfonic acid.
5. preparation method according to claim 3, which is characterized in that the nonionic emulsifier is alkylphenol-polyethenoxy
At least one of base ether, polyoxyethylene alkyl ether or polyoxyethylene sorbitol acid anhydride stearate.
6. preparation method according to claim 3, which is characterized in that the small molecule flucride siloxane is trifluoro propyl three
Methoxy silane, trifluoro propyl triethoxysilane, hexafluoro butyl propyl trimethoxy silicane, ten difluoro heptyl propyl trimethoxies
Base silane, ten trifluoro octyl trimethoxy silanes, tridecafluoro-n-octyltriethoxysilane, 17 fluorine ruthenium trimethoxysilanes,
At least one of 17 fluorine ruthenium triethoxysilanes.
7. a kind of emulsion modified inorganic silicate coating of long-chain siloxy flucride siloxane, which is characterized in that be by following weight
The group of part is grouped as：
8. coating according to claim 7, which is characterized in that the modulus of the inorganic silicic acid salting liquid is 1.0~6.0
The potassium silicate aqueous solution that sodium silicate aqueous solution and/or modulus are 1.0~6.0.
9. coating according to claim 7, which is characterized in that the antifoaming agent refers to mineral oil defoaming agent and/or poly- silicon
Oxygen alkanes antifoaming agent；The dispersant refers at least one of acrylates, carboxylic acid sodium salt or polyacrylate；The levelling agent
Refer to acrylic compounds levelling agent；The filler refers at least one of titanium dioxide, titanium dioxide, silica or precipitated calcium carbonate.
10. a kind of preparation method of the emulsion modified inorganic silicate coating of long-chain siloxy flucride siloxane, which is characterized in that packet
Include the following steps：Inorganic silicic acid salting liquid, water, long-chain siloxy flucride siloxane lotion are added in reactor, stirring is equal
It is even；Then antifoaming agent, dispersant, levelling agent is added, after stirring evenly, adds filler, room temperature disperses 3-12h, uniformly to get
To the emulsion modified inorganic silicate coating of long-chain siloxy flucride siloxane.
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|---|---|---|---|---|
| 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 |
| CN112316844A (en) * | 2020-10-30 | 2021-02-05 | 广东风华高新科技股份有限公司 | Surface modification solution and application thereof |
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