CN114106265B - Copolymer, preparation method thereof, aerogel composition and interface coating - Google Patents
Copolymer, preparation method thereof, aerogel composition and interface coating Download PDFInfo
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- CN114106265B CN114106265B CN202111551952.9A CN202111551952A CN114106265B CN 114106265 B CN114106265 B CN 114106265B CN 202111551952 A CN202111551952 A CN 202111551952A CN 114106265 B CN114106265 B CN 114106265B
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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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
- C08F283/124—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes on to polysiloxanes having carbon-to-carbon double bonds
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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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
Abstract
The invention provides a copolymer, a preparation method thereof, an aerogel composition and an interface coating, wherein the copolymer is formed by taking a hydrophobic oligomer as a main chain and hydrophilic molecules as branched chains, and the hydrophobic oligomer is formed by condensing acryloxypropyl trimethoxy silane, epoxyhexyl silane and amino silane; the copolymer, aerogel composition and interface coating provided by the invention have excellent performance, good interlayer binding force, good adhesiveness and high application value.
Description
Technical Field
The invention belongs to the field of high polymer materials, and relates to a copolymer, a preparation method thereof, an aerogel composition and an interface coating.
Background
Aerogel refers to a nanoscale porous solid material formed by replacing the liquid phase in the gel with a gas by a certain drying mode through a sol-gel method. The aerogel has good application in the aspects of heat insulation materials, energy storage devices and coatings.
CN104788925a discloses a composite tackifier for polyester composite material, preparation and application, the composite tackifier is composed of 3-methacryloxypropyl trimethoxy silane, silane by-product and secondary processed product made of silane by-product, the product can effectively improve the mechanical strength of polyester composite material; when the modified polypropylene resin is used for producing polyester artificial stone, 92 parts by mass of 400-mesh quartz powder, 8 parts by mass of unsaturated resin and 0.46 part by mass of composite tackifier are used for curing for 1 hour at 100 ℃, and the bending strength of the formed artificial stone is improved by 5.5 percent and reaches 44.71MPa compared with a product prepared from 3-methacryloxypropyl trimethoxy silane with the same proportion in a similar formula; the elastic modulus is improved by 2.5 percent and reaches 29.23GPa, and the composite material has the advantages of no toxicity, safety, environmental protection and low price. The product cannot be added to aerogel and paint products, and the adhesion between substrates cannot be improved.
The existing aerogel products usually adopt hydrophobic aerogel powder, have good water conveying effect, water resisting effect and heat insulating effect, but have poor adhesive force, and have weak interlayer bonding force with a conventional hydrophilic substrate and a surface layer, so how to further develop products with good interlayer bonding force on the basis of the hydrophobic aerogel has important significance for improving the performance of the aerogel products.
Disclosure of Invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a copolymer, a method of making the same, and aerogel compositions and interfacial coatings.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a copolymer formed by condensing acryloxypropyl trimethoxysilane, epoxysilane and aminosilane with a hydrophobic oligomer as a main chain and a hydrophilic molecule as a branched chain.
In the invention, the polymer formed by condensing three substances of the acryloxypropyl trimethoxy silane, the epoxy silane and the amino silane is used as a hydrophobic main chain framework, so that the effect of forming good binding force with the hydrophobic aerogel is achieved.
The copolymer provided by the invention can be added into aerogel and paint products to increase the hydrophilicity and lipophilicity of a system, thereby improving the adhesive force between hydrophobic aerogel and common hydrophilic base materials.
The CAS number of the acryloxypropyl trimethoxysilane is 4369-14-6; epoxysilane, 3-glycidoxypropyl trimethoxysilane, CAS number 2530-83-8.
Preferably, the hydrophilic molecule is a hydrophilic molecule having unsaturation.
Preferably, in the hydrophilic molecule having unsaturation, the unsaturation is provided by the chemical structure of any one or at least two of: a carbon-carbon double bond, a carbon-carbon triple bond, a carbon-nitrogen double bond, a carbon-nitrogen triple bond, a carbon-oxygen double bond, a carbon-sulfur double bond, or a cycloalkane.
In the present invention, hydrophilic molecules having unsaturation typically have unreacted chemical bonds that are capable of reacting with bonds in the hydrophobic oligomer to join.
Preferably, the hydrophilic molecule having unsaturation includes a hydrophilic molecule having an allyl structure or a hydrophilic molecule having a propenyl structure;
preferably, the hydrophilic molecule having unsaturation comprises any one or a combination of at least two of sodium allylsulfonate, methacrylic acid, methylolacrylamide, or acrylamide.
Preferably, the copolymer has a structure represented by formula I:
wherein R is 1 、R 2 、R 3 The values of x, y and z are independently 1 to 10, for example, 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10, etc., and the values of p, q, m, n are independently 10 to 1000, for example, 10, 100, 300, 600, 800 or 1000, etc.
According to the copolymer provided by the invention, the hydrophobic main chain is taken as a framework, and the branched chain can be well combined with acrylic emulsion in the interface coating, so that the copolymer is uniformly and stably dispersed in the coating.
In a second aspect, the present invention provides a process for the preparation of a copolymer as described in the first aspect, the process comprising the steps of: the copolymer is obtained by reacting, in the presence of a photoinitiator, 50 to 80 parts by weight (for example, 50 parts, 55 parts, 60 parts, 65 parts, 70 parts, 75 parts, 80 parts, etc.) of acryloxypropyl trimethoxysilane, 10 to 20 parts by weight (for example, 10 parts, 12 parts, 15 parts, 18 parts, 20 parts, etc.), 20 to 30 parts by weight (for example, 20 parts, 22 parts, 24 parts, 25 parts, 28 parts, 30 parts, etc.), and 1 to 10 parts by weight (for example, 1 part, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, etc.) of an aminosilane.
Preferably, the dual initiator comprises a component a and a component B, the component a being a combination of hydrogen peroxide and t-butyl hydroperoxide, the component B being a combination of clomazone and ascorbic acid.
Preferably, the temperature of the reaction is 40 to 60 ℃. Preferably, the reaction temperature is generally below 50 ℃.
In a third aspect, the present invention provides an aerogel composition comprising the copolymer of the first aspect.
Preferably, the aerogel composition further comprises the following components: any one or a combination of at least two of aerogel powder, emulsion, film forming auxiliary agent, wetting agent, defoamer, bactericide, thickener or water.
Preferably, the aerogel composition comprises the following components in parts by weight:
wherein the emulsion may be an acrylic emulsion; the film forming aid may be alcohol ester twelve; the wetting agent can be Loonggrun NS2125, defoamer Tego Foamex 825, bactericide chloromethyl isothiazolinone, methyl isothiazolinone, octyl isothiazolinone, benzisothiazolinone, etc.; the thickener can be polyurethane thickener RM-2020NPR, polyurethane thickener RM-8W, etc. These materials are all commercially available.
According to the aerogel composition provided by the invention, through the addition of the copolymer, excellent adhesive force between the aerogel coating with strong hydrophobicity and the substrate and the surface coating can be provided, the compatibility of the hydrophobic aerogel powder in the aerogel composition of the whole aqueous system can be greatly improved, the addition amount of the hydrophobic aerogel powder in the formula is increased, and the heat preservation and heat insulation performance of the composition is improved.
In a fourth aspect, the present invention provides an interfacial coating comprising a copolymer as described in the first aspect.
Preferably, the interface coating further comprises the following components: any one or a combination of at least two of acrylic emulsion, film forming aid, thickener, antifreeze, bactericide, pH regulator or water.
Preferably, the interface coating comprises the following components in parts by weight:
according to the interface coating provided by the invention, through the addition of the copolymer, firm combination can be formed between the hydrophobic main chain and the surface of the hydrophobic aerogel, and excellent interlayer binding force can be formed by utilizing perfect combination of the hydrophilic copolymerization branched chain and the hydrophilic surface coating.
The weight part of the copolymer may be 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, or the like. In the present invention, the content of the copolymer is specified, if the weight part of the copolymer is too high, the hydrophilic part thereof is too much to lower the water resistance, alkali resistance, and the hydrophobic part is too much to lower the adhesion of the interfacial coating to the upper layer thereof having hydrophilicity; on the other hand, if the content of the copolymer is too low, the overall adhesion of the interfacial coating is lowered and the performance is lowered. The preferable weight content is controlled within the above range.
The hydrophilic copolymerization branched chain of the copolymer also forms good combination with the acrylic emulsion in the interface coating, so that the copolymer is uniformly dispersed and stable in the coating.
The weight part of the acrylic emulsion may be 40 parts, 45 parts, 50 parts, 55 parts, 60 parts, or the like. The acrylic emulsion also plays a role in adjusting the adhesive force, and if the content of the acrylic emulsion is too small, the adhesive force of the interface coating is reduced; if the content of the acrylic emulsion is too high, the cost of the interface coating is too high, which is unfavorable for practical application.
The film forming auxiliary agent can be 3 parts, 4 parts or 5 parts by weight, and the specific components can be alcohol ester twelve and the like of the film forming auxiliary agent. In the invention, the film forming additive is properly adjusted according to the glass transition temperature of the acrylic emulsion.
The weight part of the thickener may be 2 parts, 3 parts, etc. The specific components can be polyurethane thickener RM-2020NPR, polyurethane thickener RM-8W, etc. The thickener of the present invention mainly plays a role in adjusting viscosity, and generally, a proper amount is required.
The antifreezing aid can be 2 parts, 2.5 parts or 3 parts by weight, and the specific components can be the antifreezing aid FT-100, propylene glycol and the like. The antifreezing auxiliary agent not only can play a role in resisting freeze thawing, but also can adjust the integral adhesive force of the interface coating. If the content of the anti-freezing auxiliary agent is too low, although the adhesive force of the interface coating is not affected, the anti-freezing and thawing properties of the interface coating are poor; if the content of the antifreezing auxiliary agent is too high, the adhesive force and the water resistance of the interface coating are reduced, the content of volatile organic compounds is high, and the environmental protection effect is poor.
The bactericide may be 0.5 part, 0.7 part, 0.8 part or 1 part by weight, and the specific components may be chloromethyl isothiazolinone, methyl isothiazolinone, octyl isothiazolinone, benzisothiazolinone, etc.
The pH regulator may be 0.5 part, 0.7 part, 0.8 part or 1 part by weight, etc., and the specific components may be 2-amino-2-methyl-1-propanol, sodium hydroxide, ammonia water, etc.
The water may be 25 parts, 28 parts, 30 parts, 35 parts, 40 parts, or the like by weight.
Compared with the prior art, the invention has the beneficial effects that:
according to the copolymer provided by the invention, the polymer formed by condensing three substances of the acryloxypropyl trimethoxy silane, the epoxy silane and the amino silane is used as a hydrophobic main chain skeleton, so that the effect of forming good binding force with hydrophobic aerogel is achieved. It can be added to aerogel and paint products to increase the hydrophilicity and lipophilicity of the system, thereby improving the adhesion between the hydrophobic aerogel and the common hydrophilic substrate.
According to the aerogel composition provided by the invention, through the addition of the copolymer, excellent adhesive force between the aerogel coating with strong hydrophobicity and the substrate and the surface coating can be provided, the compatibility of the hydrophobic aerogel powder in the aerogel composition of the whole aqueous system can be greatly improved, the addition amount of the hydrophobic aerogel powder in the formula is increased, and the heat preservation and heat insulation performance of the composition is improved.
According to the interface coating provided by the invention, through the addition of the copolymer, firm combination can be formed between the hydrophobic main chain and the surface of the hydrophobic aerogel, and excellent interlayer binding force can be formed by utilizing perfect combination of the hydrophilic copolymerization branched chain and the hydrophilic surface coating.
Detailed Description
In order to better illustrate the present invention, the technical solution is easy to understand, and the present invention is further described in detail below.
In the following examples of the present invention, the amount of the initiator to be used is not particularly limited, and may be controlled according to actual needs by those skilled in the art.
Example 1
This example provides a copolymer prepared by the following method:
under the condition that a combination of hydrogen peroxide and tertiary butyl hydroperoxide and a combination of sodium metasilicate and ascorbic acid are adopted as double initiators, 60 parts of acryloxypropyl trimethoxy silane, 15 parts of epoxy silane and 25 parts of amino silane are reacted with 5 parts of sodium allylsulfonate at a temperature of 40 ℃ to obtain a copolymer with a weight average molecular weight of 15000.
Example 2
This example provides a copolymer prepared by the following method:
under the condition that a combination of hydrogen peroxide and tertiary butyl hydroperoxide and a combination of sodium metasilicate and ascorbic acid are adopted as double initiators, 50 parts of acryloxypropyl trimethoxy silane, 10 parts of epoxy silane and 30 parts of amino silane are reacted with 8 parts of methylol acrylamide at the temperature of 60 ℃ to obtain a copolymer with the weight average molecular weight of 20000.
Example 3
This example provides a copolymer prepared by the following method:
under the condition that a combination of hydrogen peroxide and tertiary butyl hydroperoxide and a combination of sodium silicate and ascorbic acid are adopted as double initiators, 80 parts of acryloxypropyl trimethoxy silane, 20 parts of epoxy silane and 20 parts of amino silane are reacted with 10 parts of acrylamide at a temperature of 50 ℃ to obtain a copolymer with a weight average molecular weight of 5000.
Example 4
The embodiment provides an aerogel composition, which comprises the following components in parts by weight:
example 5
The embodiment provides an aerogel composition, which comprises the following components in parts by weight:
example 6
The embodiment provides an aerogel composition, which comprises the following components in parts by weight:
performance testing of aerogel compositions provided in examples 4-6
When the aerogel composition of examples 4-6 is used, the emulsion paint can be well combined with the surface of the aerogel composition, the construction is easy, the feeding is uniform, and the coating and the adhesion are not abnormal.
And (3) testing: the adhesion of the exterior wall latex paints to the aerogel compositions of examples 4 to 6 was rated 0 according to GB/T9286 cross-hatch test of paint films of colored paint and varnish.
Example 7
The embodiment provides an interface coating
Example 8
The embodiment provides an interface coating
Example 9
The embodiment provides an interface coating
Examples 7-9 were provided as interface coatings and performance tests were performed under the following conditions:
when the conventional coating such as the common aqueous acrylic latex paint is applied to the surface of the aerogel, the common aqueous coating is difficult to attach to the surface of the aerogel due to extremely strong surface hydrophobicity, is difficult to feed and easy to slip during construction, can be well combined with the surface of the aerogel when the interface coating is used, is easy to construct, is uniform in feeding, forms a continuous and uniform interface layer after being dried, can be used for constructing the conventional coating again according to normal requirements on the interface layer, and has no abnormality in brushing and attaching.
And (3) testing: the interfacial coatings of examples 7-9 were tested according to GB/T9286 cross-hatch test of paint films of colored paint and varnish to have an adhesion of 0 grade to aerogel and the exterior wall latex paint was tested according to the adhesion of 0 grade to the interfacial coating.
Comparative example 1
The comparative example differs from example 4 only in that the copolymer prepared in example 1 was not included in the comparative example, and an aerogel composition was prepared. According to the GB/T9286 cross-cut test of paint films of colored paint and varnish, the adhesive force between the aerogel composition and the outer wall emulsion paint is 2 grades, the aerogel powder is poorly dispersed in the composition, the whole composition is poor in state, and the stability is poor.
Comparative example 2
The comparative example differs from example 4 only in that the acrylic emulsion is not included in the comparative example, and an aerogel composition is prepared. Because of the lack of the main binding component, the aerogel composition has no strength, no adhesive force and can not form a film.
Comparative example 3
The difference between this comparative example and example 7 is that the interfacial coating provided in this comparative example does not contain the copolymer prepared in example 1, and an interfacial coating was prepared.
The hydrophilic interface coating prepared in this way has poor adhesion with the surface of the aerogel, sagging and dripping similar to lotus leaf effect caused by ineffective wetting and spreading can occur during construction, the hydrophilic interface coating can not be uniformly coated on the surface of the aerogel, and the hydrophilic interface coating can not be well combined with the next coating.
Comparative example 4
The difference between this comparative example and example 7 is that the interfacial coating provided by this comparative example does not contain the copolymer prepared in example 1, but instead is an equivalent amount of hydrophobic alkylphenol ethoxylate.
Although the adhesive force between the prepared hydrophobic interface coating and the surface of the hydrophobic aerogel has a certain effect, the adhesive force can cause sagging and dripping similar to lotus leaf effect caused by ineffective wetting and spreading during the next construction, and the adhesive force can not be uniformly coated and adhered on the surface of the interface coating, so that the effect of the interface coating is lost.
Comparative example 5
The comparative example differs from example 7 only in that the copolymer in the comparative example was 7 parts by weight and the water was 35 parts by weight, to prepare an interface coating material. According to GB/T9286 cross-cut test of paint films of colored paint and varnish, the adhesive force between the interface paint and aerogel is 1 level, and the adhesive force between the outer wall emulsion paint and the interface paint is 1 level. This is because the content of the copolymer is too small, and it is difficult for the hydrophobic main chain skeleton to form a good binding force with the aerogel.
Comparative example 6
The comparative example differs from example 7 only in that the copolymer in the comparative example was 19 parts by weight and the water was 37 parts by weight, to prepare an interface coating material. According to GB/T9286 cross-cut test of paint films of colored paint and varnish, the adhesive force between the interface paint and aerogel is 1 level, and the adhesive force between the outer wall emulsion paint and the interface paint is 1 level. Due to the excessive content of the copolymer, the hydrophobic effect of the copolymer is too strong, and the overall adhesion is reduced.
Comparative example 7
The comparative example was different from example 7 only in that 32 parts by weight of the acrylic emulsion in the comparative example was used, and the interface coating material was prepared in the same manner as in example 7. The adhesive force of the interface paint and the aerogel is 1 level according to GB/T9286 cross-cut test of colored paint and varnish film, and the adhesive force of the external wall emulsion paint and the interface paint is 1 level.
Comparative example 8
The comparative example differs from example 7 only in that 7 parts by weight of the antifreeze additive in the comparative example was used, and the balance was the same as example 7 to prepare an interface coating. The adhesive force of the interface coating is reduced due to the excessively high consumption of the antifreezing auxiliary agent, the adhesive force of the interface coating and aerogel is 2-grade according to the test of GB/T9286 cross-cut test of colored paint and varnish film, and the adhesive force of the external wall emulsion paint and the interface coating is 2-grade.
The detailed process equipment and process flow of the present invention are described by the above embodiments, but the present invention is not limited to, i.e., it does not mean that the present invention must be practiced depending on the detailed process equipment and process flow. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
Claims (5)
1. A copolymer, characterized in that the copolymer is formed by taking a hydrophobic oligomer as a main chain and hydrophilic molecules as branched chains, wherein the hydrophobic oligomer is formed by condensing acryloxypropyl trimethoxysilane, epoxy silane and aminosilane;
the hydrophilic molecule is any one or a combination of at least two of sodium allylsulfonate, methacrylic acid, methylol acrylamide or acrylamide;
the preparation method of the copolymer comprises the following steps:
in the presence of a double initiator, the copolymer is obtained by reacting acryloxypropyl trimethoxy silane, epoxy silane and amino silane with hydrophilic molecules, wherein the weight part of the acryloxypropyl trimethoxy silane is 50-80 parts, the weight part of the epoxy silane is 10-20 parts, the weight part of the amino silane is 20-30 parts, and the weight part of the hydrophilic molecules is 1-10 parts.
2. The copolymer of claim 1, wherein the dual initiator comprises a component a and a component B, the component a being a combination of hydrogen peroxide and t-butyl hydroperoxide and the component B being a combination of clomazone and ascorbic acid.
3. The copolymer of claim 1, wherein the temperature of the reaction is 40-60 ℃.
4. An aerogel composition, characterized in that the aerogel composition comprises the following components:
5. the interface coating is characterized by comprising the following components in parts by weight:
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| CA2724803C (en) * | 2009-12-30 | 2013-04-23 | Rohm And Haas Company | Elastomeric roof coatings with adhesion to weathered thermoplastic polyolefin (tpo) roofing membranes |
| BR112017013725B1 (en) * | 2014-12-31 | 2022-01-04 | Akzo Nobel Coatings International B.V. | COATING COMPOSITION BASED ON ORGANIC SOLVENT AND COATED METALLIC SUBSTRATE |
| CN107922738A (en) * | 2015-09-01 | 2018-04-17 | 日立化成株式会社 | Sol composition and aeroge |
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| CN112852229A (en) * | 2020-12-31 | 2021-05-28 | 上海中南建筑材料有限公司 | Aerogel heat-insulation thick middle coating, heat-insulation finish paint, aerogel heat-insulation heat-preservation coating system for buildings and preparation method thereof |
| CN114133770B (en) * | 2021-12-17 | 2022-07-29 | 上海中南建筑材料有限公司 | Heat-preservation and decoration integrated aerogel coating composition and preparation method and application thereof |
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| JPH08100135A (en) * | 1994-09-28 | 1996-04-16 | Dainippon Toryo Co Ltd | Binder composition for water-based inorganic-organic composite type coating agent |
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| JP2012116961A (en) * | 2010-12-01 | 2012-06-21 | Kaneka Corp | One pack composition |
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