CN109266211A - Organopolysiloxane super hydrophobic coating and preparation method thereof - Google Patents
Organopolysiloxane super hydrophobic coating and preparation method thereof Download PDFInfo
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- CN109266211A CN109266211A CN201810990412.2A CN201810990412A CN109266211A CN 109266211 A CN109266211 A CN 109266211A CN 201810990412 A CN201810990412 A CN 201810990412A CN 109266211 A CN109266211 A CN 109266211A
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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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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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
- C09D5/08—Anti-corrosive paints
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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
- C09D5/1656—Antifouling paints; Underwater paints characterised by the film-forming substance
- C09D5/1662—Synthetic film-forming substance
- C09D5/1675—Polyorganosiloxane-containing compositions
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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
- C09D5/1687—Use of special 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
- C09D5/18—Fireproof paints including high temperature resistant paints
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Paints Or Removers (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The present invention relates to chemical field, a kind of organopolysiloxane super hydrophobic coating and preparation method thereof, the molecular formula of organosilan precursor in the coating are as follows: R are disclosed3Si‑X‑SiR3, the X in the formula is CnH2nChain radicals, wherein n be 2,4,6,8,10 or 12, R Cl, OCH3Or OCH2CH3.Preparation method includes the following steps the following steps are included: being R by a certain proportion of molecular formula at room temperature3Si‑X‑SiR3Organosilane precursors and after dimethyl silicone polymer is mixed evenly, be added photoacid generator, after stirring and dissolving, film forming sprayed in substrate；It is placed in 10 ~ 60min of irradiation under LED light lamp, obtains the organopolysiloxane super hydrophobic coating.Compared with existing super-hydrophobic coat technology of preparing, this method is easy to operate, polymerization speed is fast, without using organic solvent, and energy conservation and environmental protection has a vast market foreground.
Description
Technical field
The present invention relates to technical field of paint preparation, in particular to a kind of organopolysiloxane super hydrophobic coating and its preparation
Method.
Background technique
Super-hydrophobic coating material is widely paid close attention to due to its special surface non wettability by people, automatically cleaning,
The fields such as antifouling, anti-icing, anticorrosion, drag reduction have broad application prospects.
There are many preparation method of super-hydrophobic coat at present, and a large amount of different type super-hydrophobic coats are prepared out.But needle
To practical application, most preparation methods of report need special equipment, complicated process, and use in preparation process
A large amount of volatile organic solvents, cause it to be only applicable to laboratory research.In addition, conventional polymer polymer coating by
It is easy to lose superhydrophobic characteristic when heat, outdoor application, causes the stability of material not good enough, it is difficult to industrial applications.
Summary of the invention
Goal of the invention: aiming at the problems existing in the prior art, the present invention provides a kind of super-hydrophobic painting of organopolysiloxane
Material and preparation method thereof, polysiloxane backbone are not easy to be decomposed by ultraviolet light and ozone, have good thermal stability, weather-proof energy
Power, and this method is easy to operate, polymerization speed is fast, without using any solvent, energy conservation and environmental protection.
Technical solution: the present invention provides a kind of organopolysiloxane super hydrophobic coating, body before organosilan in the coating
The molecular formula of body are as follows: R3Si-X-SiR3, the X in the formula is CnH2nChain radicals, wherein n is 2,4,6,8,10 or 12, and R is
Cl、OCH3Or OCH2CH3。
The present invention also provides a kind of preparation methods of organopolysiloxane super hydrophobic coating, comprising the following steps: room temperature
Under, it is R by a certain proportion of molecular formula3Si-X-SiR3Organosilane precursors mixed with dimethyl silicone polymer, stirring is mixed
After closing uniformly, photoacid generator is added, after stirring and dissolving, film forming is sprayed in substrate；It is placed under lamp and irradiates preset time, obtain institute
State organopolysiloxane super hydrophobic coating；It is R in the molecular formula3Si-X-SiR3Organosilane precursors in, the X in formula is
CnH2nChain radicals, wherein n be 2,4,6,8,10 or 12, R Cl, OCH3Or OCH2CH3。
Preferably, the mass ratio between the organosilane precursors and the dimethyl silicone polymer is 2 ~ 10:1.
Preferably, the organosilane precursors, the dimethyl silicone polymer and the light produce the matter between sour machine
Amount is than being 1 ~ 10:1:0.05 ~ 0.5.
Preferably, the dimethyl silicone polymer is methoxyl group OCH3Sealing end, average molecular weight 550g/mol.
Preferably, the lamp is the light emitting diode with specific wavelength, wavelength 320nm, 365nm or 405nm.
Preferably, the power of the light emitting diode is 0.1 ~ 20mW/cm2；It is preferred that 0.5mW/cm2、2mW/cm2、5mW/
cm2、10mW/cm2。
Preferably, the photoacid generator is diphenyl iodine hexafluorophosphate (DH), 4- isobutyl phenenyl -4'- methyl
Phenyl-iodide hexafluorophosphate (I250), 2- methyl-α-[2- [[the third sulfonyl] imines] -3 (2H)-thenylidene-benzene acetonitrile
(PAG103), diphenyl-(4- phenyl sulphur) phenyl sulfonium hexafluorophosphate (UV6992) or 4- octyloxy diphenyl iodine hexafluoro antimony
Hydrochlorate (OPHA).
Preferably, the substrate is glass, silicon wafer, tinplate, aluminium alloy, polycarbonate, filter paper or woven fabric.
Preferably, the preset time irradiated under the lamp be 10 ~ 60min, preferably 15min, 30min, 45min or
60min。
The utility model has the advantages that organosilane precursors, dimethyl silicone polymer are directly mixed with photoacid generator and are stirred in the present invention
After mixing uniformly, sprays in substrate and obtain organosilicon liquid coating；Then illumination photodissociation photoacid generator generates super acids initiation and has
Si-Cl, SiOCH in machine silane precursor3Or SiOCH2CH3Hydrolysis-condensation reaction to get the super-hydrophobic painting of organopolysiloxane
Layer.Wherein, the SiOCH that dimethyl silicone polymer passes through sealing end3Si-Cl, SiOCH in group and organosilane precursors3Or
SiOCH2CH3Copolycondensation is hydrolyzed, is present in organopolysiloxane skeleton, due to its low-surface-energy characteristic, in conjunction with coating
The coarse structure on surface, so that resulting organopolysiloxane has ultra-hydrophobicity.
Preparation method provided by the invention compared with prior art, need to only be simply mixed organosilane precursors and light produces acid
Agent, without using solvent, and in the case where no illumination, formula solution is highly stable；The preparation of coating only needs simple optical
According to 10 ~ 60min, has many advantages, such as substrate that is environmentally protective, being simple and efficient, can be widely applied to unlike material；In the present invention
Super-hydrophobic coat has that heat-resisting, weather resistance is excellent, self-cleaning material, in terms of with wide application before
Scape.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph and water contact angle figure on 2 floating coat surface of embodiment.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.
Embodiment 1:
By bis- (trichlorine silicon substrate) hexane (Cl of 1,6-3Si-C6H12-SiCl3) 9g and polydimethylsiloxane 1g is uniformly mixed, then
4- isobutyl phenenyl -4'- aminomethyl phenyl iodine hexafluorophosphate (I250) 0.2g is added, is sprayed into substrate after being completely dissolved
Film, the LED lamplight of 320nm shine 10min, and the power of LED is 20 mW/cm2, organopolysiloxane super-hydrophobic coat is obtained, as a result
It is shown in Table 1.
Embodiment 2:
By bis- (front three oxygen silicon base) the hexane [(CH of 1,6-3O)3Si-C6H12-Si(OCH3)3] 7.5g and polydimethylsiloxane 2.5g
It is uniformly mixed, adds 2- methyl-α-[2- [[the third sulfonyl] imines] -3 (2H)-thenylidene-benzene acetonitrile
(PAG103) 0.05g sprays film forming in substrate after being completely dissolved, the LED lamplight of 405nm shines 30min, and the power of LED is
0.5 mW/cm2, organopolysiloxane super-hydrophobic coat is obtained, the results are shown in Table 1.The scanning electron microscope (SEM) photograph of the coating surface of the coating
It is as shown in Figure 1 with water contact angle figure, it is seen that the rough surface of obtained organopolysiloxane super-hydrophobic coat, water contact angle
156°。
Embodiment 3:
By bis- (front three oxygen silicon base) the ethane [(CH of 1,2-3O)3Si-C2H4-Si(OCH3)3] 8g and polydimethylsiloxane 2g stirring it is mixed
It closes uniformly, adds 4- octyloxy diphenyl iodine hexafluoro antimonate (OPHA) 0.1g, be sprayed into substrate after being completely dissolved
Film, the LED lamplight of 365nm shine 30min, and the power of LED is 2 mW/cm2, organopolysiloxane super-hydrophobic coat is obtained, as a result
It is shown in Table 1.
Embodiment 4:
By bis- (front three oxygen silicon base) the octane [(CH of 1,8-3O)3Si-C8H16-Si(OCH3)3] 7g and polydimethylsiloxane 3g stirring
It is uniformly mixed, adds 2- methyl-α-[2- [[the third sulfonyl] imines] -3 (2H)-thenylidene-benzene acetonitrile (PAG103)
0.1g sprays film forming in substrate after being completely dissolved, the LED lamplight of 405nm shines 30min, and the power of LED is 0.5 mW/cm2,
Organopolysiloxane super-hydrophobic coat is obtained, the results are shown in Table 1.
Embodiment 5:
By bis- (front three oxygen silicon base) certain herbaceous plants with big flowers the alkane [(CH of 1,10-3O)3Si-C10H20-Si(OCH3)3] 6g and polydimethylsiloxane 4g stirs
It mixes uniformly mixed, adds 2- methyl-α-[2- [[the third sulfonyl] imines] -3 (2H)-thenylidene-benzene acetonitrile (PAG103)
0.2g sprays film forming in substrate after being completely dissolved, the LED lamplight of 405nm shines 30min, and the power of LED is 5 mW/cm2, obtain
To organopolysiloxane super-hydrophobic coat, 1 the results are shown in Table.
Embodiment 6:
By bis- (three ethoxy silicon substrates) the dodecane [(CH of 1,12-3CH2O)3Si-C12H24-Si(OCH2CH3)3] 6.5g and poly dimethyl
Silane 3.5g is uniformly mixed, and adds 2- methyl-α-[2- [[the third sulfonyl] imines] -3 (2H)-thenylidene-benzene second
Nitrile (PAG103) 0.5g sprays film forming in substrate after being completely dissolved, the LED lamplight of 405nm shines 60min, and the power of LED is 10
mW/cm2, a kind of organopolysiloxane super-hydrophobic coat is obtained, the results are shown in Table 1.
1 organopolysiloxane super-hydrophobic coat water contact angle test result of table
Note: contact angle test produces DSA25 type full-automatic video contact angle measurement using Kr ü ss company of Germany, and row of making even is surveyed
The average value of examination three times.
The technical concepts and features of above embodiment only to illustrate the invention, its object is to allow be familiar with technique
People cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
The equivalent transformation or modification that Spirit Essence is done, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of organopolysiloxane super hydrophobic coating, which is characterized in that the molecular formula of organosilan precursor in the coating are as follows:
R3Si-X-SiR3, the X in the formula is CnH2nChain radicals, wherein n be 2,4,6,8,10 or 12, R Cl, OCH3Or
OCH2CH3。
2. a kind of preparation method of organopolysiloxane super hydrophobic coating as described in claim 1, which is characterized in that including with
Lower step:
It at room temperature, is R by a certain proportion of molecular formula3Si-X-SiR3Organosilane precursors and dimethyl silicone polymer it is mixed
It closes, after being uniformly mixed, photoacid generator is added, after stirring and dissolving, film forming is sprayed in substrate；It is placed in when irradiating default under lamp
Between, obtain the organopolysiloxane super hydrophobic coating；
It is R in the molecular formula3Si-X-SiR3Organosilane precursors in, X in formula is CnH2nChain radicals, wherein n
It is 2,4,6,8,10 or 12, R Cl, OCH3Or OCH2CH3。
3. organopolysiloxane super hydrophobic coating according to claim 2 and preparation method thereof, which is characterized in that described to have
Mass ratio between machine silane precursor and the dimethyl silicone polymer is 2 ~ 10:1.
4. the preparation method of organopolysiloxane super hydrophobic coating according to claim 2, which is characterized in that described organic
It is 1 ~ 10:1:0.05 ~ 0.5 that silane precursor, the dimethyl silicone polymer and the light, which produce the mass ratio between sour machine,.
5. the preparation method of organopolysiloxane super hydrophobic coating according to claim 2, which is characterized in that described poly- two
Methylsiloxane is methoxyl group OCH3Sealing end, average molecular weight 550g/mol.
6. organopolysiloxane super hydrophobic coating according to claim 2 and preparation method thereof, which is characterized in that described
Lamp is the light emitting diode with specific wavelength, wavelength 320nm, 365nm or 405nm.
7. the preparation method of organopolysiloxane super hydrophobic coating according to claim 6, which is characterized in that described to shine
The power of diode is 0.1 ~ 20mW/cm2。
8. the preparation method of organopolysiloxane super hydrophobic coating, feature according to any one of claim 2 to 7 exist
In the photoacid generator is diphenyl iodine hexafluorophosphate (DH), 4- isobutyl phenenyl -4'- aminomethyl phenyl iodine hexafluoro phosphorus
Hydrochlorate, 2- methyl-α-[2- [[the third sulfonyl] imines] -3 (2H)-thenylidene-benzene acetonitrile, diphenyl-(4- phenyl sulphur) benzene
Base sulfonium hexafluorophosphate or 4- octyloxy diphenyl iodine hexafluoro antimonate.
9. the preparation method of organopolysiloxane super hydrophobic coating, feature according to any one of claim 2 to 7 exist
In the substrate is glass, silicon wafer, tinplate, aluminium alloy, polycarbonate, filter paper or woven fabric.
10. the preparation method of organopolysiloxane super hydrophobic coating, feature according to any one of claim 2 to 7
It is, the preset time irradiated under the lamp is 10 ~ 60min.
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Cited By (6)
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| CN110205020A (en) * | 2019-05-29 | 2019-09-06 | 福建好优新材料有限公司 | A kind of automobile chassis automatically cleaning protective agent and preparation method thereof |
| CN110444568A (en) * | 2019-07-31 | 2019-11-12 | 武汉华星光电半导体显示技术有限公司 | Organic LED display panel and preparation method thereof, display device |
| CN111978861A (en) * | 2020-09-01 | 2020-11-24 | 淮阴工学院 | Preparation method of phenyl polysiloxane super-hydrophobic coating |
| CN111978862A (en) * | 2020-09-01 | 2020-11-24 | 淮阴工学院 | Preparation method of polysiloxane super-hydrophobic coating |
| CN112029325A (en) * | 2020-09-01 | 2020-12-04 | 淮阴工学院 | Preparation method of polyacrylate super-hydrophobic coating |
| CN113088190A (en) * | 2019-11-21 | 2021-07-09 | 淮阴工学院 | Preparation method of fluorine-containing organopolysiloxane self-cleaning coating |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110205020A (en) * | 2019-05-29 | 2019-09-06 | 福建好优新材料有限公司 | A kind of automobile chassis automatically cleaning protective agent and preparation method thereof |
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| CN112029325A (en) * | 2020-09-01 | 2020-12-04 | 淮阴工学院 | Preparation method of polyacrylate super-hydrophobic coating |
| CN111978862B (en) * | 2020-09-01 | 2021-08-17 | 淮阴工学院 | Preparation method of polysiloxane super-hydrophobic coating |
| CN111978861B (en) * | 2020-09-01 | 2021-11-23 | 淮阴工学院 | Preparation method of phenyl polysiloxane super-hydrophobic coating |
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