CN114106265A - 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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- CN114106265A CN114106265A CN202111551952.9A CN202111551952A CN114106265A CN 114106265 A CN114106265 A CN 114106265A CN 202111551952 A CN202111551952 A CN 202111551952A CN 114106265 A CN114106265 A CN 114106265A
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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
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Abstract
The invention provides a copolymer, a preparation method thereof, an aerogel composition and an interface coating, wherein the copolymer is formed by taking hydrophobic oligomer as a main chain and hydrophilic molecules as branched chains, and the hydrophobic oligomer is formed by condensing acryloxypropyltrimethoxysilane, epoxyhexylsilane and aminosilane; the copolymer, the aerogel composition and the interface coating provided by the invention have the advantages of excellent performance, good interlayer binding force, good adhesion 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 is a nano-scale porous solid material formed by replacing liquid phase in gel with gas by a certain drying way 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 and its preparation and application, the composite tackifier is composed of 3-methacryloxypropyl trimethoxy silane, silane by-product and secondary processed product made from silane by-product, the product can effectively improve the mechanical strength of polyester composite material; when the polyester artificial stone is used for producing polyester artificial stones, 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, and the curing time is 1 hour at 100 ℃, so that the bending strength of the formed artificial stones is improved by 5.5% and reaches 44.71MPa compared with that of products prepared by using 3-methacryloxypropyltrimethoxysilane with the same proportion and 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 into aerogel and coating products, and cannot improve the adhesive force between base materials.
The existing aerogel product is usually selected from hydrophobic aerogel powder, has good water delivery effect, water-resistant effect and heat insulation effect, but is generally poor in adhesive force, and weaker in interlayer bonding force with conventional hydrophilic substrates and surface layers, so that the product with good interlayer bonding force is further developed on the basis of the hydrophobic aerogel, and the aerogel product has important significance in improving the performance of the aerogel product.
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 preparing the same, and an aerogel composition and an interface coating.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a copolymer, wherein the copolymer is formed by using a hydrophobic oligomer as a main chain and using a hydrophilic molecule as a branch chain, and the hydrophobic oligomer is formed by condensing acryloxypropyltrimethoxysilane, epoxy silane and aminosilane.
According to the invention, a polymer formed by condensing acryloxypropyltrimethoxysilane, epoxy silane and aminosilane is used as a hydrophobic main chain skeleton, so that an effect of forming a good bonding force with hydrophobic aerogel is achieved.
The copolymer provided by the invention can be added into aerogel and coating products to increase the hydrophilicity and lipophilicity of a system, so that the adhesive force between the hydrophobic aerogel and a common hydrophilic base material is improved.
The CAS number of the acryloxypropyltrimethoxysilane is 4369-14-6; the epoxysilane is 3-glycidoxypropyltrimethoxysilane with 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: carbon-carbon double bonds, carbon-carbon triple bonds, carbon-nitrogen double bonds, carbon-nitrogen triple bonds, carbon-oxygen double bonds, carbon-sulfur double bonds, or cycloalkanes.
In the present invention, the hydrophilic molecules having unsaturation generally have unreacted chemical bonds that can react with and become attached to the bonds in the hydrophobic oligomer.
Preferably, the hydrophilic molecule having unsaturation includes a hydrophilic molecule having an allyl structure or a hydrophilic molecule having an acryl 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 the structure shown in formula I:
wherein R is1、R2、R3Independently selected from any one of acryloxypropyltrimethoxysilane, epoxy silane and amino silane, the values of x, y and z are independently 1-10, for example, 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10, and the like, p, q, m,The value of n is independently 10 to 1000, and may be, for example, 10, 100, 300, 600, 800, 1000, or the like.
The copolymer provided by the invention takes the hydrophobic main chain as a skeleton, and the branched chain can form good combination 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 preparing a copolymer as described in the first aspect, the process comprising the steps of: the copolymer is obtained by reacting acryloxypropyltrimethoxysilane, epoxysilane and aminosilane with hydrophilic molecules in the presence of a dual initiator, wherein the acryloxypropyltrimethoxysilane is 50-80 parts (for example, 50 parts, 55 parts, 60 parts, 65 parts, 70 parts, 75 parts or 80 parts) by weight, the epoxysilane is 10-20 parts (for example, 10 parts, 12 parts, 15 parts, 18 parts or 20 parts) by weight, the aminosilane is 20-30 parts (for example, 20 parts, 22 parts, 24 parts, 25 parts, 28 parts or 30 parts) by weight, and the hydrophilic molecules are 1-10 parts (for example, 1 part, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts or 10 parts) by weight.
Preferably, the diinitiator includes component a which is a combination of hydrogen peroxide and t-butyl hydroperoxide and component B which is a combination of sodium formaldehyde sulfoxylate and ascorbic acid.
Preferably, the reaction temperature is 40-60 ℃. 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: aerogel powder, emulsion, film forming auxiliary agent, wetting agent, defoaming agent, bactericide, thickening agent or water or the combination of at least two of the substances.
Preferably, the aerogel composition comprises the following components in parts by weight:
wherein the emulsion may be an acrylic emulsion; the film forming additive can be alcohol ester twelve; the wetting agent can be Loongrun NS2125, antifoaming agent Tego Foamex 825, bactericide chloromethyl isothiazolinone, methyl isothiazolinone, octyl isothiazolinone, benzisothiazolone, etc.; the thickener can be polyurethane thickener RM-2020NPR, polyurethane thickener RM-8W, etc. These substances are commercially available.
The aerogel composition provided by the invention can provide excellent adhesive force between the aerogel coating with strong hydrophobicity and the substrate and the surface coating through adding the copolymer, can greatly improve the compatibility of the hydrophobic aerogel powder in the aerogel composition of the whole aqueous system, increases the addition amount of the hydrophobic aerogel powder in the formula, and improves the heat insulation performance of the composition.
In a fourth aspect, the present invention provides an interfacial coating comprising the copolymer of the first aspect.
Preferably, the interface coating further comprises the following components: any one or the combination of at least two of acrylic emulsion, film forming auxiliary agent, thickening agent, antifreezing agent, bactericide, pH regulator or water.
Preferably, the interface coating comprises the following components in parts by weight:
the interface coating provided by the invention can form firm combination with the hydrophobic aerogel surface through the hydrophobic main chain of the interface coating by adding the copolymer, and can form excellent interlayer combination force by utilizing the perfect combination of the hydrophilic copolymerization branched chain and the hydrophilic surface coating.
The weight parts 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, and if the weight part of the copolymer is too high, the hydrophilic portion is too much to lower the water resistance and alkali resistance, while the hydrophobic portion is too much to lower the adhesion of the interfacial coating to the topcoat coating having hydrophilicity thereon; if the content of the copolymer is too low, the overall adhesion of the interface coating is reduced, and the performance is reduced. The preferable weight content is controlled within the above range.
The hydrophilic copolymeric branches of the copolymer also form a good bond with the acrylic emulsion in the interfacial coating, making the copolymer uniformly and stably dispersed in the coating.
The acrylic emulsion may be present in an amount of 40 parts, 45 parts, 50 parts, 55 parts, 60 parts, or the like by weight. The acrylic emulsion also has the function of 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 not favorable for practical use.
The film forming aid can be 3 parts, 4 parts or 5 parts by weight, and the specific components can be film forming aid alcohol ester twelve and the like. In the invention, the film-forming assistant is properly adjusted according to the glass transition temperature of the acrylic emulsion.
The weight portion of the thickener may be 2 parts, 3 parts, etc. The concrete components can be thickeners such as polyurethane thickener RM-2020NPR, polyurethane thickener RM-8W and the like. The thickener of the present invention mainly functions to adjust viscosity, and generally, it is sufficient if it is used in an appropriate amount.
The anti-freezing auxiliary agent can be 2 parts, 2.5 parts or 3 parts by weight, and the specific components can be anti-freezing auxiliary agent FT-100, propylene glycol and the like. The anti-freezing auxiliary agent not only can play a role in freeze thawing resistance, but also can adjust the overall 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 influenced, the freeze-thaw resistance of the interface coating is poor; if the content of the anti-freezing 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 environment-friendly effect is poor.
The bactericide may be 0.5 part, 0.7 part, 0.8 part, 1 part, etc., and the specific component 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, and the specific components may be 2-amino-2-methyl-1-propanol, sodium hydroxide, ammonia water, etc.
The weight parts of water may be 25 parts, 28 parts, 30 parts, 35 parts, 40 parts, or the like.
Compared with the prior art, the invention has the beneficial effects that:
the copolymer provided by the invention takes a polymer formed by condensing acryloxypropyltrimethoxysilane, epoxy silane and aminosilane as a hydrophobic main chain skeleton, so that the effect of forming good bonding force with hydrophobic aerogel is achieved. The hydrophilic aerogel can be added into aerogel and coating products to increase the hydrophilicity and lipophilicity of a system, so that the adhesive force between the hydrophobic aerogel and a common hydrophilic base material is improved.
The aerogel composition provided by the invention can provide excellent adhesive force between the aerogel coating with strong hydrophobicity and the substrate and the surface coating through adding the copolymer, can greatly improve the compatibility of the hydrophobic aerogel powder in the aerogel composition of the whole aqueous system, increases the addition amount of the hydrophobic aerogel powder in the formula, and improves the heat insulation performance of the composition.
The interface coating provided by the invention can form firm combination with the hydrophobic aerogel surface through the hydrophobic main chain of the interface coating by adding the copolymer, and can form excellent interlayer combination force by utilizing the perfect combination of the hydrophilic copolymerization branched chain and the hydrophilic surface coating.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions, the present invention is further described in detail below.
In the following examples of the present invention, the amount of the initiator may be enough to enable the reaction system to react, and the amount of the initiator may be controlled by those skilled in the art according to actual needs, and is not particularly limited herein.
Example 1
This example provides a copolymer prepared by the following method:
60 parts of acryloxypropyltrimethoxysilane, 15 parts of epoxysilane and 25 parts of aminosilane were reacted with 5 parts of sodium allylsulfonate at a temperature of 40 ℃ under the condition that a combination of hydrogen peroxide and tert-butyl hydroperoxide, a combination of sodium formaldehyde sulfoxylate and ascorbic acid were used as a diinitiator to obtain a copolymer with a weight average molecular weight of 15000.
Example 2
This example provides a copolymer prepared by the following method:
a copolymer having a weight-average molecular weight of 20000 was obtained by reacting 50 parts of acryloxypropyltrimethoxysilane, 10 parts of epoxysilane and 30 parts of aminosilane with 8 parts of methylolacrylamide at a temperature of 60 ℃ using a combination of hydrogen peroxide and t-butyl hydroperoxide and a combination of sodium formaldehyde sulfoxylate and ascorbic acid as a dual initiator.
Example 3
This example provides a copolymer prepared by the following method:
80 parts of acryloxypropyltrimethoxysilane, 20 parts of epoxysilane and 20 parts of aminosilane are reacted with 10 parts of acrylamide at the temperature of 50 ℃ under the condition that a combination of hydrogen peroxide and tert-butyl hydroperoxide and a combination of sodium formaldehyde sulfoxylate and ascorbic acid are used as a double initiator to obtain a copolymer, and the weight-average molecular weight is 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:
the aerogel compositions provided in examples 4 to 6 were subjected to performance testing
When the conventional coating such as the common water-based acrylic emulsion paint is applied to the surface of the common aerogel, the common emulsion paint is difficult to attach to the surface of the common aerogel due to the extremely strong surface hydrophobicity, the feeding is difficult and the common aerogel is easy to slip during construction, and when the aerogel compositions of the examples 4 to 6 are 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 attachment are not abnormal.
And (3) testing: the adhesion of the exterior wall latex paints tested in GB/T9286 "test for marking test of paint films of paints and varnishes" and the aerogel compositions of examples 4 to 6 were all of grade 0.
Example 7
This example provides an interfacial coating
Example 8
This example provides an interfacial coating
Example 9
This example provides an interfacial coating
The interfacial coatings provided in examples 7-9 were tested for performance under the following conditions:
when the conventional coating such as common water-based acrylic emulsion paint is applied to the surface of the aerogel, the common water-based coating is difficult to attach to the surface of the aerogel due to extremely strong surface hydrophobicity, the loading is difficult and the aerogel is easy to slip during construction, the interface coating can be well combined with the surface of the aerogel during use, the construction is easy, the loading is uniform, a continuous and uniform interface layer is formed after drying, the conventional coating can be constructed on the interface layer according to normal requirements, and the conventional coating is not abnormal during coating and attachment.
And (3) testing: the adhesion between the interface coating and the aerogel in examples 7-9 was rated 0 and the adhesion between the exterior wall latex paint and the interface coating was rated 0 as tested in GB/T9286 "test for drawing checks on paint films of colored paints and varnishes".
Comparative example 1
This comparative example differs from example 4 only in that the copolymer prepared in example 1 was not included in this comparative example and an aerogel composition was prepared. According to GB/T9286 marking test of paint film of colored paint and varnish, the adhesion force of the aerogel composition and the external wall latex paint is 2 grade, the aerogel powder is poorly dispersed in the composition, and the whole composition has poor state and poor stability.
Comparative example 2
This comparative example differs from example 4 only in that no acrylic emulsion was included in this comparative example and an aerogel composition was prepared. Because of the lack of main bonding components, the aerogel composition has no strength, no adhesive force and can not form a film.
Comparative example 3
This comparative example differs from example 7 in that it provides an interfacial coating that does not contain the copolymer prepared in example 1, and is prepared to provide an interfacial coating.
The hydrophilic interface coating prepared in the way has poor adhesive force with the surface of the aerogel, and during construction, sagging and dripping similar to lotus leaf effect caused by ineffective wetting and spreading can occur, so that the hydrophilic interface coating can not be uniformly coated on the surface of the aerogel and can not be well combined with the next coating.
Comparative example 4
This comparative example differs from example 7 in that it provides an interfacial coating that does not contain the copolymer prepared in example 1, but instead replaces it with an equivalent amount of hydrophobic alkylphenol ethoxylate.
Although the adhesion force between the hydrophobic interface coating and the surface of the hydrophobic aerogel prepared in the way has a certain effect, due to the strong hydrophobicity of the hydrophobic interface coating, the hydrophobic interface coating can sag and drip due to the lotus leaf effect similar to the lotus leaf effect generated by ineffective wetting and spreading in the next construction, and the hydrophobic interface coating 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
This comparative example differs from example 7 only in that an interfacial coating was prepared with 7 parts by weight of copolymer and 35 parts by weight of water in this comparative example. According to GB/T9286, the test shows that the adhesion between the interface coating and the aerogel is grade 1, and the adhesion between the external wall emulsion paint and the interface coating is grade 1. 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 bonding force with the aerogel.
Comparative example 6
This comparative example differs from example 7 only in that 19 parts by weight of the copolymer and 37 parts by weight of water were used in this comparative example to prepare an interfacial coating. According to GB/T9286, the test shows that the adhesion between the interface coating and the aerogel is grade 1, and the adhesion between the external wall emulsion paint and the interface coating is grade 1. Due to the excessive content of the copolymer, the hydrophobic effect of the copolymer is too strong, and the overall adhesive force is reduced.
Comparative example 7
The comparative example is different from example 7 only in that the acrylic emulsion in the comparative example is 32 parts by weight, and the interfacial coating is prepared in the same manner as in example 7. Because the addition amount of the acrylic emulsion is insufficient, the cohesive force of the interface coating is insufficient, the integral adhesive force is reduced, the adhesive force of the interface coating and the aerogel is 1 grade according to GB/T9286 marking test of colored paint and varnish paint film, and the adhesive force of the exterior wall latex paint and the interface coating is 1 grade.
Comparative example 8
The comparative example is different from example 7 only in that the anti-freezing additive in the comparative example is 7 parts by weight, and the balance is the same as example 7 to prepare the interface coating. The adhesion of the interface coating is reduced due to the excessively high dosage of the anti-freezing auxiliary agent, and the adhesion of the interface coating and aerogel is 2 grade and the adhesion of the exterior wall latex paint and the interface coating is 2 grade according to GB/T9286 test of grid test of paint films of colored paint and varnish.
The present invention is illustrated by the above-mentioned examples, but the present invention is not limited to the above-mentioned detailed process equipment and process flow, i.e. it is not meant to imply that the present invention must rely on the above-mentioned detailed process equipment and process flow to be practiced. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (12)
1. The copolymer is characterized in that the copolymer is formed by taking a hydrophobic oligomer as a main chain and taking a hydrophilic molecule as a branch chain, and the hydrophobic oligomer is formed by condensing acryloxypropyltrimethoxysilane, epoxy silane and aminosilane.
2. The copolymer of claim 1, wherein the hydrophilic molecule is a hydrophilic molecule having unsaturation.
3. The copolymer of claim 1 or 2, wherein the hydrophilic molecule having unsaturation is provided by the chemical structure of any one or at least two of: carbon-carbon double bonds, carbon-carbon triple bonds, carbon-nitrogen double bonds, carbon-nitrogen triple bonds, carbon-oxygen double bonds, carbon-sulfur double bonds or cycloalkanes;
preferably, the hydrophilic molecule having unsaturation includes a hydrophilic molecule having an allyl structure or a hydrophilic molecule having an acryl 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.
4. The copolymer of any one of claims 1-3, wherein the copolymer has a structure according to formula I:
wherein R is1、R2、R3Independently selected from any one of acryloxypropyltrimethoxysilane, epoxy silane or aminosilane, the values of x, y and z are independently 1-10, and the values of p, q, m and n are independently 10-1000.
5. Process for the preparation of a copolymer according to any one of claims 1 to 4, characterized in that it comprises the following steps: in the presence of a dual initiator, acryloxypropyltrimethoxysilane, epoxy silane and aminosilane react with hydrophilic molecules to obtain the copolymer, wherein the acryloxypropyltrimethoxysilane is 50-80 parts by weight, the epoxy silane is 10-20 parts by weight, the aminosilane is 20-30 parts by weight, and the hydrophilic molecules are 1-10 parts by weight.
6. The method of claim 5, wherein the diinitiator comprises component A which is a combination of hydrogen peroxide and t-butyl hydroperoxide, and component B which is a combination of sodium formaldehyde sulfoxylate and ascorbic acid;
preferably, the reaction temperature is 40-60 ℃.
7. An aerogel composition, comprising the copolymer of any of claims 1-4.
8. The aerogel composition of claim 7, further comprising the following components: aerogel powder, emulsion, film forming auxiliary agent, wetting agent, defoaming agent, bactericide, thickening agent or water or the combination of at least two of the substances.
9. The aerogel composition according to claim 8 or 9, comprising the following components in parts by weight:
10. an interfacial coating, comprising the copolymer of any of claims 1-4.
11. The interface coating of claim 10, further comprising the following components: any one or the combination of at least two of acrylic emulsion, film forming auxiliary agent, thickening agent, antifreezing agent, bactericide, pH regulator or water.
12. The interface coating of claim 10 or 11, comprising the following components in parts by weight:
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