CN113372814A - Cage-shaped polysilsesquioxane-based super-hydrophilic functional coating and preparation method thereof - Google Patents
Cage-shaped polysilsesquioxane-based super-hydrophilic functional coating and preparation method thereof Download PDFInfo
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- 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
- C09D183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
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- 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
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
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- 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
- C08G77/38—Polysiloxanes modified by chemical after-treatment
- C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
- C08G77/388—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing nitrogen
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/66—Additives characterised by particle size
- C09D7/67—Particle size smaller than 100 nm
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Abstract
The invention discloses a super-hydrophilic functional coating based on cage-shaped polysilsesquioxane, wherein a precursor solution of the super-hydrophilic functional coating comprises main body resin, hydrophilic nano silicon dioxide particles and a solvent; the main resin is a main resin with alkoxy prepared by the reaction of epoxy cage polysilsesquioxane and secondary amino siloxane. The precursor solution of the super-hydrophilic functional coating comprises main resin, hydrophilic nano silicon dioxide particles and a solvent. The main resin with alkoxy reaction functional groups is prepared by adopting the reaction of epoxy cage polysilsesquioxane and secondary amino siloxane, and the super-hydrophilic coating which has certain surface roughness and hydroxyl hydrophilic groups on the surface is prepared by utilizing the nano-size effect of the cage polysilsesquioxane and the size effect of hydrophilic nano-silica by matching with hydrophilic nano-silica particles, wherein the water contact angle is less than 5 degrees. Meanwhile, the existence of the cage-shaped polysilsesquioxane can effectively promote the dispersion effect of the nano silicon dioxide.
Description
Technical Field
The invention belongs to the technical field of super-hydrophilic materials, and particularly relates to a super-hydrophilic functional coating based on cage-shaped polysilsesquioxane and a preparation method thereof.
Background
Surface wettability is one of the important characteristics of solid surfaces, and research progress is always focused and favored by researchers. The degree of wetting of a solid surface by a liquid is generally characterized by a Contact Angle (CA), and when the contact angle between water and the solid surface is less than 5 °, the surface is considered to be a super-hydrophilic surface, and the degree of hydrophilicity is determined by the structure and chemical composition of the surface of the coating. The super-hydrophilic surface has good wetting property, so that water can be instantly spread and quickly evaporated, water drops are prevented from being bonded and staying on the surface, the effects of blocking and isolating dirt can be achieved, and the effect of easily cleaning oil, dirt and the like can be realized.
The applicant researches and discovers that the prior art has the following problems:
currently, existing superhydrophilic coatings are mostly achieved by introducing hydrophilic nanoparticles. Such as a super-hydrophilic film based on titanium dioxide photocatalysis, a surfactant coated super-hydrophilic surface. The titanium dioxide super-hydrophilic coating with a single component does not show hydrophilicity any more after the irradiation of an ultraviolet lamp is removed, but the long-acting property of the titanium dioxide super-hydrophilic coating cannot be ensured indoors, so that the application range of the titanium dioxide super-hydrophilic coating is limited. Surfactants tend to run off and are not resistant to wiping and solvents.
On the other hand, many super-hydrophilic coatings with silica nanoparticles introduced therein need high-temperature treatment, for example, chinese patent publication No. CN200610113975.0 discloses a super-hydrophilic self-cleaning anti-fog coating, and the technical scheme is that after electrostatic assembly, high-temperature sintering is performed to form a coarse super-surface to realize the super-hydrophilic coating, and the preparation conditions are harsh.
With the development of society, the super-hydrophilic coating will be more and more favored by the market with its excellent self-cleaning property. Therefore, it is desirable to provide a novel superhydrophilic coating.
Disclosure of Invention
The invention aims to solve the technical problems and provides a super-hydrophilic functional coating based on cage-shaped polysilsesquioxane and a preparation method thereof.
In order to solve the problems, the invention is realized according to the following technical scheme:
in a first aspect, the invention provides a super-hydrophilic functional coating based on cage-like polysilsesquioxane, which is characterized in that:
the precursor solution of the super-hydrophilic functional coating comprises main body resin, hydrophilic nano silicon dioxide particles and a solvent;
the main resin is a main resin with alkoxy prepared by the reaction of epoxy cage polysilsesquioxane and secondary amino siloxane.
With reference to the first aspect, the present invention further provides an embodiment 1 of the first aspect, wherein a mass ratio of the nano silica particles to the host resin is 2 to 8:1, and a mass of the solvent is 50 to 95% of a total mass.
In combination with the first aspect, the present disclosure also provides embodiment 2 of the first aspect, wherein the molar ratio of the epoxy cage polysilsesquioxane to the secondary aminosiloxane is from 1: 8.
in combination with the first aspect, the present invention further provides a 3 rd embodiment of the first aspect, where the epoxy cage polysilsesquioxane is one or two of glycidyl ether oxypropyl cage polysilsesquioxane and epoxy cyclohexyl ethyl cage polysilsesquioxane, and a particle size of the epoxy cage polysilsesquioxane is 1 to 3 nm.
In combination with the first aspect, the present invention also provides embodiment 4 of the first aspect, wherein the secondary aminosiloxane is one or more of N-butyl-3-aminopropyltrimethoxysilane, N-butyl-3-aminopropyltriethoxysilane, bis- [3- (trimethoxy silicon) -propyl ] -amine, bis- [3- (triethoxy silicon) -propyl ] -amine, 3-anilinopropyltrimethoxysilane, 3- (phenylamino) propyltriethoxysilane, 3- (N-cyclohexylamine) propyltrimethoxysilane and 3- (N-cyclohexylamine) propylmethyldimethoxysilane.
With reference to the first aspect, the present invention further provides a 5 th embodiment of the first aspect, wherein the hydrophilic nanosilica particles have a particle size of 5 to 100 nm.
With reference to the first aspect, the present invention further provides a 6 th embodiment of the first aspect, wherein the hydrophilic nano-silica particles are one or both of liquid silica sol and powdered silica.
In combination with the first aspect, the present disclosure also provides a 7 th embodiment of the first aspect, wherein the solvent is one or both of ethanol and isopropanol.
In a second aspect, the present invention also provides a preparation method of a super-hydrophilic functional coating based on cage-like polysilsesquioxane, for preparing the super-hydrophilic functional coating of the first aspect, the preparation method comprising the following steps:
(1) adding epoxy cage polysilsesquioxane and a solvent into a container, adding secondary amino siloxane with the molar ratio of 8 times of that of the epoxy cage polysilsesquioxane and the solvent under the stirring state, and reacting for later use after a period of time;
wherein, the main body resin with alkoxy is prepared by the reaction of epoxy cage polysilsesquioxane and secondary amino siloxane;
(2) adding hydrophilic nano silicon dioxide into a container, and stirring uniformly to obtain a precursor solution of the super-hydrophilic functional coating based on the cage-shaped polysilsesquioxane;
(3) and coating the precursor solution on the surface of a substrate, and reacting for 24 hours at room temperature to obtain the super-hydrophilic functional coating.
Compared with the prior art, the invention has the beneficial effects that:
(1) the precursor solution of the super-hydrophilic functional coating comprises main resin, hydrophilic nano silicon dioxide particles and a solvent. The main resin with alkoxy reaction functional groups is prepared by adopting the reaction of epoxy cage polysilsesquioxane and secondary amino siloxane, and the super-hydrophilic coating which has certain surface roughness and hydroxyl hydrophilic groups on the surface is prepared by utilizing the nano-size effect of the cage polysilsesquioxane and the size effect of hydrophilic nano-silica by matching with hydrophilic nano-silica particles, wherein the water contact angle is less than 5 degrees. Meanwhile, the existence of the cage-shaped polysilsesquioxane can effectively promote the dispersion effect of the nano silicon dioxide.
(2) The main resin with alkoxy can realize normal temperature moisture curing under the promotion action of tertiary amino, effectively overcomes the technical problem of harsh preparation conditions of the conventional super-hydrophilic coating, does not need to add other catalysts or promoters, and can prepare the super-hydrophilic functional coating simply, quickly and rapidly.
Drawings
Embodiments of the invention are described in further detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a schematic representation of the caged polysilsesquioxane-based superhydrophilic functional coating of the present invention.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Referring to fig. 1, a schematic diagram of a super-hydrophilic functional coating according to the present invention is shown. The precursor solution of the super-hydrophilic functional coating based on the cage-shaped polysilsesquioxane comprises main body resin, hydrophilic nano silicon dioxide particles and a solvent; the main resin is a main resin with alkoxy prepared by the reaction of epoxy cage polysilsesquioxane and secondary amino siloxane.
Wherein the mass ratio of the nano silicon dioxide particles to the main resin is 2-8: 1, and the mass of the solvent is 50-95% of the total mass. The molar ratio of the epoxy cage polysilsesquioxane to the secondary amino siloxane is 1: 8.
in a preferred implementation, the epoxy cage-shaped polysilsesquioxane is one or two of glycidyl ether oxypropyl cage-shaped polysilsesquioxane and epoxy cyclohexyl ethyl cage-shaped polysilsesquioxane, and the particle size of the epoxy cage-shaped polysilsesquioxane is 1-3 nm. The invention utilizes the nanometer size effect of the cage-shaped polysilsesquioxane and the size effect of the hydrophilic nanometer silicon dioxide to prepare the super-hydrophilic coating which has certain surface roughness and hydroxyl hydrophilic groups on the surface, and the water contact angle is less than 5 degrees. Meanwhile, the existence of the cage-shaped polysilsesquioxane can effectively promote the dispersion effect of the nano silicon dioxide.
In a preferred embodiment, the secondary aminosilicone is one or more of N-N-butyl-3-aminopropyltrimethoxysilane, N-N-butyl-3-aminopropyltriethoxysilane, bis- [3- (trimethoxy silicon) -propyl ] -amine, bis- [3- (triethoxy silicon) -propyl ] -amine, 3-anilinopropyltrimethoxysilane, 3- (phenylamino) propyltriethoxysilane, 3- (N-cyclohexylamine) propyltrimethoxysilane and 3- (N-cyclohexylamine) propylmethyldimethoxysilane.
In the present invention, under the repeated research and experiment of the applicant, the secondary amino siloxane is creatively selected because the secondary amino siloxane only contains one active hydrogen, and the reaction with the epoxy group of the epoxy cage polysilsesquioxane is 1-to-1 reaction, so that the crosslinking type polymer can not be generated through crosslinking. Also, by introducing a secondary aminosiloxane, the reaction of the amino group and the epoxy group produces a moisture curable oligomer with siloxy groups, and the tertiary amino group of the final system can act as an accelerator for the moisture cure of siloxy groups.
And the applicant researches and discovers that if other raw materials are adopted for reaction, such as primary amino, a cross-linked polymer is generated, so that the subsequent process cannot be carried out, and the super-hydrophilic coating cannot be prepared.
In the present invention, the hydrophilic nano-silica particles preferably have a particle size of 5 to 100 nm. The hydrophilic nano silicon dioxide particles are one or two of liquid silica sol and powder silicon dioxide.
Meanwhile, the adopted solvent is an environment-friendly solvent and can be one or two of ethanol and isopropanol.
The invention discloses a preparation method of a super-hydrophilic functional coating based on cage-shaped polysilsesquioxane, which comprises the following steps:
adding a certain amount of epoxy cage polysilsesquioxane into a container, then adding a certain amount of solvent, adding 8 times of mol ratio of secondary amino siloxane under a stirring state, reacting for a while for later use, and reacting the epoxy cage polysilsesquioxane with the secondary amino siloxane to obtain main body resin with alkoxy; adding hydrophilic nano silicon dioxide into a container, and stirring uniformly to obtain a precursor solution of the super-hydrophilic functional coating based on the cage-shaped polysilsesquioxane; and coating the precursor solution on the surface of a substrate, and reacting for 24 hours at room temperature to obtain the super-hydrophilic functional coating.
The super-hydrophilic coating can be suitable for products such as glass, stainless steel, plastics and the like which need to realize self-cleaning or antifogging.
Example 1
60g of ethanol was added to a 500ml two-necked flask, and glycidoxypropyl caged polysilsesquioxane was added under stirring6g, then 9.8g N-n-butyl-3-aminopropyltrimethoxysilane is added, after 24 hours of room temperature reaction, 33g of wound-healing hydrophilic silicon dioxide (A), (B), (C) and (D) are added200) And uniformly stirring to obtain a precursor solution with solid content of about 45%.
The precursor is easily coated on the surface of the substrate by a spraying method, the super-hydrophilic coating is obtained after curing for 24 hours at room temperature, and the water contact angle of the super-hydrophilic coating is detected to be 4 degrees.
Example 2
200g of ethanol was added to a 500ml two-necked flask, and glycidoxypropyl caged polysilsesquioxane was added under stirring5g, then 7.6g of 3- (phenylamino) propylmethoxysilane, reacting at room temperature for 24h, then 63g of Yingchuang hydrophilic silica (a)380) And stirring uniformly to obtain a precursor solution with the solid content of about 27 percent.
The precursor is easily coated on the surface of the substrate by a spraying method, and the super-hydrophilic coating is obtained after curing for 24 hours at room temperature, and the water contact angle of the super-hydrophilic coating is 3 degrees through detection.
Example 3
300g of ethanol was added to a 500ml two-necked flask, and epoxy cyclohexyl ethyl cage polysilsesquioxane was added under stirring8g, then 12.5g N-n-butyl-3-aminopropyltriethoxysilane is added, after 24 hours of room temperature reaction, 143.5g of wound-healing hydrophilic silicon dioxide (A), (B) and (C)130) And uniformly stirring to obtain a precursor solution with the solid content of about 35 percent.
Coating the precursor solution on the surface of a substrate by a spraying method, curing at room temperature for 24 hours to obtain the super-hydrophilic coating, and detecting that the water contact angle of the super-hydrophilic coating is 2 degrees.
Example 4
300g of ethanol was added to a 500ml two-necked flask, and epoxy cyclohexyl ethyl cage polysilsesquioxane was added under stirring5g, then 9.6g of bis- [3- (trimethoxy-silicon) -propyl ] are added]Amine, reacting at room temperature for 24 hours, adding 87.6g of wound-healing hydrophilic silica (c) ((C))150) And uniformly stirring to obtain a precursor solution with solid content of about 25 percent.
Coating the precursor solution on the surface of a substrate by a spraying method, curing at room temperature for 24 hours to obtain the super-hydrophilic coating, and detecting that the water contact angle of the super-hydrophilic coating is 3 degrees.
Comparative example 1
100g of ethanol was added to a 500ml two-necked flask, and epoxy cyclohexyl ethyl cage polysilsesquioxane was added under stirring8g, then 12.5g N-n-butyl-3-aminopropyltriethoxysilane was addedAnd reacting at room temperature for 24 hours to obtain a precursor solution with the solid content of about 17 percent.
Coating the precursor solution on the surface of a substrate by a spraying method, curing for 24 hours at room temperature to obtain a coating, and detecting that the water contact angle of the coating is 20 degrees.
Comparative example 2
60g of ethanol was added to a 500ml two-necked flask, and glycidoxypropyl caged polysilsesquioxane was added under stirring6g, then 9.8g N-n-butyl-3-aminopropyltrimethoxysilane is added, after 24 hours of room temperature reaction, 16g of wound-healing hydrophilic silicon dioxide (A), (B), (C) and (C) are added200) And uniformly stirring to obtain a precursor solution with the solid content of about 35 percent.
Coating the precursor solution on the surface of a substrate by a spraying method, curing for 24 hours at room temperature to obtain a coating, and detecting that the water contact angle of the coating is 10 degrees.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, so that any modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (9)
1. A super-hydrophilic functional coating based on cage-shaped polysilsesquioxane is characterized in that:
the precursor solution of the super-hydrophilic functional coating comprises main body resin, hydrophilic nano silicon dioxide particles and a solvent;
the main resin is a main resin with alkoxy prepared by the reaction of epoxy cage polysilsesquioxane and secondary amino siloxane.
2. The caged polysilsesquioxane-based superhydrophilic functional coating of claim 1, wherein:
the mass ratio of the nano silicon dioxide particles to the main resin is 2-8: 1, and the mass of the solvent is 50-95% of the total mass.
3. The caged polysilsesquioxane-based superhydrophilic functional coating of claim 2, wherein:
the molar ratio of the epoxy cage polysilsesquioxane to the secondary amino siloxane is 1: 8.
4. the caged polysilsesquioxane-based superhydrophilic functional coating of claim 3, wherein:
the epoxy cage-shaped polysilsesquioxane is one or two of glycidol ether oxypropyl cage-shaped polysilsesquioxane and epoxy cyclohexyl ethyl cage-shaped polysilsesquioxane, and the particle size of the epoxy cage-shaped polysilsesquioxane is 1-3 nm.
5. The caged polysilsesquioxane-based superhydrophilic functional coating of claim 3, wherein:
the secondary amino siloxane is one or more of N-N-butyl-3-aminopropyltrimethoxysilane, N-N-butyl-3-aminopropyltriethoxysilane, bis- [3- (trimethoxy silicon) -propyl ] -amine, bis- [3- (triethoxy silicon) -propyl ] -amine, 3-anilinopropyltrimethoxysilane, 3- (phenylamino) propyltriethoxysilane, 3- (N-cyclohexylamine) propyltrimethoxysilane and 3- (N-cyclohexylamine) propylmethyldimethoxysilane.
6. The caged polysilsesquioxane-based superhydrophilic functional coating of claim 1, wherein:
the particle size of the hydrophilic nano silicon dioxide particles is 5-100 nm.
7. The caged polysilsesquioxane-based superhydrophilic functional coating of claim 6, wherein:
the hydrophilic nano silicon dioxide particles are one or two of liquid silica sol and powder silicon dioxide.
8. The caged polysilsesquioxane-based superhydrophilic functional coating of claim 1, wherein:
the solvent is one or two of ethanol and isopropanol.
9. A preparation method of a super-hydrophilic functional coating based on cage-shaped polysilsesquioxane is characterized by comprising the following steps:
(1) adding epoxy cage polysilsesquioxane and a solvent into a container, adding secondary amino siloxane with the molar ratio of 8 times of that of the epoxy cage polysilsesquioxane and the solvent under the stirring state, and reacting for later use after a period of time;
wherein, the main body resin with alkoxy is prepared by the reaction of epoxy cage polysilsesquioxane and secondary amino siloxane;
(2) adding hydrophilic nano silicon dioxide into a container, and stirring uniformly to obtain a precursor solution of the super-hydrophilic functional coating based on the cage-shaped polysilsesquioxane;
(3) and coating the precursor solution on the surface of a substrate, and reacting for 24 hours at room temperature to obtain the super-hydrophilic functional coating.
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CN113897135A (en) * | 2021-11-29 | 2022-01-07 | 广东晟毅新材料科技有限公司 | Super-hydrophilic anti-fog coating and preparation method thereof |
CN114774900A (en) * | 2022-04-13 | 2022-07-22 | 沈阳化工大学 | Method for increasing surface roughness of steel wire for rubber hose by adopting self-roughening process |
CN114774900B (en) * | 2022-04-13 | 2023-12-29 | 沈阳化工大学 | Method for increasing surface roughness of steel wire for rubber tube by adopting self-roughening process |
CN116554477A (en) * | 2023-01-29 | 2023-08-08 | 武汉中科先进材料科技有限公司 | POSS modified polymer, preparation method thereof and super-hydrophilic coating containing POSS modified polymer |
CN116554477B (en) * | 2023-01-29 | 2024-01-30 | 武汉中科先进材料科技有限公司 | POSS modified polymer, preparation method thereof and super-hydrophilic coating containing POSS modified polymer |
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