CN110256956B - Primer for silicon rubber and preparation method thereof - Google Patents
Primer for silicon rubber and preparation method thereof Download PDFInfo
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- CN110256956B CN110256956B CN201910588943.3A CN201910588943A CN110256956B CN 110256956 B CN110256956 B CN 110256956B CN 201910588943 A CN201910588943 A CN 201910588943A CN 110256956 B CN110256956 B CN 110256956B
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
- C09J5/02—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving pretreatment of the surfaces to be joined
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2400/00—Presence of inorganic and organic materials
- C09J2400/10—Presence of inorganic materials
- C09J2400/14—Glass
- C09J2400/143—Glass in the substrate
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2483/00—Presence of polysiloxane
- C09J2483/006—Presence of polysiloxane in the substrate
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Abstract
The invention relates to the field of high polymer sealing materials, in particular to a primer for silicon rubber and a preparation method thereof. The primer for the silicon rubber comprises the following components in parts by weight: 5-20 parts of methoxy silicone resin; 1-10 parts of adhesion promoter; 1-5 parts of silicate ester; 1-5 parts of a silane coupling agent; 1-5 parts of a catalyst; 60-90 parts of a solvent; the adhesion promoter is prepared by reacting epoxy silane and secondary amino silane; the silane coupling agent is selected from vinyl tri-tert-butyl peroxy silane and/or bis- [ gamma- (triethoxy silicon) propyl ] tetrasulfide. The primer for the silicon rubber provided by the invention can improve the adhesion of the single-component silicon rubber on the LOW-E glass surface and can also improve the adhesion of the double-component silicon rubber on the LOW-E glass surface. Experiments show that cohesive failure of the primer for silicon rubber can reach 85% or even 100% when the primer is matched with a single-component silicone adhesive or a two-component silicone adhesive.
Description
Technical Field
The invention relates to the field of high polymer sealing materials, in particular to a primer for silicon rubber and a preparation method thereof.
Background
The heat loss of the outer door and window glass is the main part of the energy consumption of the building, and accounts for more than 50 percent of the energy consumption of the building. Research data has shown that the heat transfer at the inner surface of the glass is mainly radiation, accounting for 58%, which means that the loss of heat energy is reduced by changing the properties of the glass, and the most effective method is to inhibit the radiation at the inner surface. The emissivity of ordinary float glass is as high as 0.84, and can be reduced to below 0.15 after a silver-based low-emissivity film is plated. Therefore, the Low-E glass is used for manufacturing the door and the window of the building, so that the transmission of indoor heat energy to the outdoor space caused by radiation can be greatly reduced, and an ideal energy-saving effect is achieved.
Another significant benefit from the reduction of indoor heat loss is environmental protection. Cold season, CO caused by building heating2、SO2And the emission of harmful gases is an important pollution source. If the Low-E glass is used, fuel consumed by heating can be greatly reduced due to reduction of heat loss, thereby reducing emission of harmful gas.
The heat transfer through the glass is bidirectional, i.e. the heat can be transferred from the room to the outside and vice versa, and is done simultaneously, only with the problem of poor heat transfer. In winter, the indoor temperature is higher than the outdoor temperature, and heat preservation is required. In summer, the indoor temperature is lower than that of the outdoor, and the glass is required to be capable of insulating heat, namely, the outdoor heat is transmitted to the indoor as little as possible. The Low-E glass can meet the requirements of winter and summer, can preserve and insulate heat, and has the effects of environmental protection and Low carbon.
The Low-E glass also has good optical performance and can effectively reduce the reflectivity of visible light. Due to the above characteristics, Low-E glass has been widely used in developed countries.
However, Low-E glass is a film-system product with a surface coated with multiple layers of metal or other compounds. Due to the existence of the film, the adhesive property of the common silicon rubber on the surface of the common silicon rubber is greatly reduced, and interface peeling often occurs, so that the glass is loosened and even falls off.
In order to solve the above problems, it is urgently required to develop a primer for improving the adhesion of silicone rubber on a LOW-E glass surface.
Disclosure of Invention
In view of the above, the technical problem to be solved by the invention is to provide a primer for silicone rubber and a preparation method thereof, and the primer for silicone rubber provided by the invention can improve the adhesion of single-component silicone rubber on a LOW-E glass surface and can also improve the adhesion of double-component silicone rubber on the LOW-E glass surface.
The invention provides a primer for silicon rubber, which comprises the following components in parts by weight:
the adhesion promoter is prepared by reacting epoxy silane and secondary amino silane;
the silane coupling agent is selected from vinyl tri-tert-butyl peroxy silane and/or bis- [ gamma- (triethoxy silicon) propyl ] tetrasulfide.
Preferably, the methoxy silicon resin has a structure shown in formula (I):
in the formula (I), R1Is hydrogen or methyl; r2Is methyl or ethyl; r3Is methyl.
Preferably, the number average molecular weight of the methoxy silicon resin is 500-5000.
Preferably, the epoxy silane is selected from one or more of gamma-glycidoxypropyltrimethoxysilane, 3- (2, 3-glycidoxy) propylmethyldiethoxysilane, 3- (2, 3-glycidoxy) propylmethyldimethoxysilane, gamma-glycidoxypropyltriethoxysilane, beta- (3, 4-epoxycyclohexyl) -ethyltriethoxysilane and beta- (3, 4-epoxycyclohexyl) -ethyltrimethoxysilane;
the secondary aminosilane is selected from one or more of N- (N-butyl) -gamma-aminopropyltrimethoxysilane, N-cyclohexyl-gamma-aminopropylmethyldimethoxysilane, bis (3-trimethoxysilylpropyl) amine, bis- (gamma-trimethoxysilylpropyl) amine, bis (3-triethoxysilylpropyl) amine and N-phenyl-gamma-aminopropyltrimethoxysilane.
Preferably, the silicate is selected from methyl orthosilicate and/or ethyl orthosilicate.
Preferably, the catalyst is selected from one or more of titanate, zirconate and aluminate.
Preferably, the titanate is selected from one or more of isopropyl titanate, butyl titanate, tetrabutyl titanate mixture, polybutyl titanate, tetraisooctyl titanate, tetraethoxy titanium, tetrakis (2-ethylhexanol) titanium, n-propyl titanate, propyldioleate acyloxy (dioctylphosphate acyloxy) titanate, isopropyltris (dioctylphosphate acyloxy) titanate, isopropyltrioleate acyloxy titanate, isopropyltris (dodecylbenzene sulfonic acid) titanate, isopropyltris (dioctylphosphate acyloxy) ethylene titanate and tetraisopropylbis (dioctylphosphite acyloxy) titanate;
the zirconate is selected from one or more of n-butyl zirconate and isobutyl zirconate;
the aluminate is selected from one or more of diisopropyl di (ethyl acetoacetate) aluminate, isopropyl aluminate and diisopropyl di (acetylacetone) aluminate.
Preferably, the solvent is one or more of butyl acetate, propyl acetate, toluene, ethyl acetate and butanone.
The invention also provides a preparation method of the primer for the silicon rubber, which comprises the following steps:
mixing methoxy silicon resin, adhesion promoter, silicate ester, silane coupling agent, catalyst and solvent to obtain the primer for the silane modified adhesive.
Preferably, the mixing is stirring mixing, the mixing temperature is 20-50 ℃, and the mixing time is 5-120 min.
The invention provides a primer for silicon rubber, which comprises the following components in parts by weight: 5-20 parts of methoxy silicone resin; 1-10 parts of adhesion promoter; 1-5 parts of silicate ester; 1-5 parts of a silane coupling agent; 1-5 parts of a catalyst; 60-90 parts of a solvent; the adhesion promoter is prepared by reacting epoxy silane and secondary amino silane; the silane coupling agent is selected from vinyl tri-tert-butyl peroxy silane and/or bis- [ gamma- (triethoxy silicon) propyl ] tetrasulfide. The primer for the silicon rubber provided by the invention can improve the adhesion of the single-component silicon rubber on the LOW-E glass surface and can also improve the adhesion of the double-component silicon rubber on the LOW-E glass surface.
Experimental results show that the cohesive failure of the primer for silicon rubber prepared by the invention can reach 85% or even 100% when the primer is matched with a single-component silicone adhesive or a double-component silicone adhesive. Therefore, the primer for the silicon rubber provided by the invention not only can enable the single-component silicon rubber to have better adhesion on a LOW-E glass surface, but also can enable the double-component silicon rubber to have better adhesion on the LOW-E glass surface.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a primer for silicon rubber, which comprises the following components in parts by weight:
the adhesion promoter is prepared by reacting epoxy silane and secondary amino silane;
the silane coupling agent is selected from vinyl tri-tert-butyl peroxy silane and/or bis- [ gamma- (triethoxy silicon) propyl ] tetrasulfide.
The primer for silicon rubber provided by the invention comprises methoxy silicon resin. The methoxy silicon resin has double methoxy groups, can react and crosslink with metal oxide components in the LOW-E film to form a film structure, and improves the surface flatness. The weight part of the methoxy silicone resin is 5-20 parts. In certain embodiments of the present invention, the weight part of the methoxy silicon resin is 7 parts, 15 parts or 18 parts.
In some embodiments of the present invention, the methoxy silicon resin has a structure represented by formula (i):
in the formula (I), R1Is hydrogen or methyl; r2Is methyl or ethyl; r3Is methyl.
In some embodiments of the invention, the number average molecular weight of the methoxy silicon resin is 500-5000. In certain embodiments, the methoxy silicon resin has a number average molecular weight of 2000, 1500, 4000, or 3000.
The primer for silicon rubber provided by the invention also comprises an adhesion promoter. The adhesion promoter is 1-10 parts by weight. In certain embodiments of the invention, the adhesion promoter is present in 6 parts, 9 parts, or 3 parts by weight.
In certain embodiments of the invention, the adhesion promoter is prepared by reacting an epoxy silane and a secondary amino silane. Specifically, the following may be mentioned: mixing epoxy silane and secondary amino silane, and stirring for 30-60 min at 20-60 ℃ to obtain the adhesion promoter.
In certain embodiments of the present invention, the epoxy silane is selected from one or more of gamma-glycidoxypropyltrimethoxysilane, 3- (2, 3-glycidoxy) propylmethyldiethoxysilane, 3- (2, 3-glycidoxy) propylmethyldimethoxysilane, gamma-glycidoxypropyltriethoxysilane, beta- (3, 4-epoxycyclohexyl) -ethyltriethoxysilane, and beta- (3, 4-epoxycyclohexyl) -ethyltrimethoxysilane.
In certain embodiments of the present invention, the secondary aminosilane is selected from one or more of N- (N-butyl) - γ -aminopropyltrimethoxysilane, N-cyclohexyl- γ -aminopropylmethyldimethoxysilane, bis (3-trimethoxysilylpropyl) amine, bis- (γ -trimethoxysilylpropyl) amine, bis (3-triethoxysilylpropyl) amine, and N-phenyl- γ -aminopropyltrimethoxysilane.
In certain embodiments of the present invention, the mass ratio of the epoxy silane to the secondary amine silane is 23 to 26: 30-35. In certain embodiments, the mass ratio of epoxy silane to secondary amine silane is 23.6: 34. 26: 35. 25: 35 or 26: 30.
the stirring temperature is 20-60 ℃. In certain embodiments of the invention, the temperature of the stirring is ambient temperature, 55 ℃, or 35 ℃. The stirring time is 30-60 min. In certain embodiments of the invention, the time of stirring is 60 min.
The silicon rubber primer also comprises silicate ester. The silicate ester is 1-5 parts by weight. In certain embodiments of the present invention, the silicate is 1 part, 3 parts, or 4 parts by weight.
In certain embodiments of the present invention, the silicate is selected from methyl orthosilicate and/or ethyl orthosilicate.
The primer for silicon rubber provided by the invention also comprises a silane coupling agent. The silane coupling agent is 1-5 parts by weight. In certain embodiments of the present invention, the silane coupling agent is present in an amount of 2 parts, 3 parts, or 4 parts by weight.
In the invention, the silane coupling agent is selected from vinyl tri-tert-butyl peroxy silane and/or bis- [ gamma- (triethoxy silicon) propyl ] tetrasulfide.
The primer for silicon rubber provided by the invention also comprises a catalyst. The catalyst of the invention can accelerate the onset time of the silicon rubber on the LOW-E glass surface. The weight part of the catalyst is 1-5 parts. In certain embodiments of the present invention, the weight portion of the catalyst is 1 part, 2 parts, 4 parts, or 5 parts.
In certain embodiments of the invention, the catalyst is selected from one or more of the group consisting of titanates, zirconates, and aluminates.
The titanate is preferably one or more of isopropyl n-titanate, butyl n-titanate, tetrabutyl titanate mixture, polybutyl titanate, tetraisooctyl titanate, tetraethoxytitanium, tetrakis (2-ethylhexanol) titanium, n-propyl titanate, propyldioleate acyloxy (dioctylphosphate) titanate, isopropyltris (dioctylphosphate) titanate, isopropyltrioleate acyloxy titanate, isopropyltris (dodecylbenzene sulfonic acid) titanate, isopropyltris (dioctylphosphate) ethylene titanate and tetraisopropylbis (dioctylphosphite) titanate.
The zirconate is preferably one or more of n-butyl zirconate and isobutyl zirconate.
The aluminate is preferably one or more of diisopropyl di (ethyl acetoacetate) aluminate, isopropyl aluminate and diisopropyl di (acetylacetone) aluminate.
The primer for silicon rubber provided by the invention also comprises a solvent. The weight part of the solvent is 60-90 parts. In certain embodiments of the present invention, the solvent is present in an amount of 71 parts, 68 parts, 70 parts, 86 parts, or 60 parts by weight.
In certain embodiments of the present invention, the solvent is one or more of butyl acetate, propyl acetate, toluene, ethyl acetate, and butanone.
The invention also provides a preparation method of the primer for silicon rubber, which comprises the following steps:
mixing methoxy silicon resin, adhesion promoter, silicate ester, silane coupling agent, catalyst and solvent to obtain the primer for the silane modified adhesive.
In certain embodiments of the invention, the mixing is stirred mixing. In some embodiments of the present invention, the temperature of the mixing is 20 to 50 ℃. In certain embodiments, the temperature of the mixing is ambient temperature or 50 ℃. In some embodiments of the present invention, the mixing time is 5-120 min. In certain embodiments, the time of mixing is 60min or 90 min.
The source of the above-mentioned raw materials is not particularly limited in the present invention, and may be generally commercially available.
The invention provides a primer for silicon rubber, which comprises the following components in parts by weight: 5-20 parts of methoxy silicone resin; 1-10 parts of adhesion promoter; 1-5 parts of silicate ester; 1-5 parts of a silane coupling agent; 1-5 parts of a catalyst; 60-90 parts of a solvent; the adhesion promoter is prepared by reacting epoxy silane and secondary amino silane; the silane coupling agent is selected from vinyl tri-tert-butyl peroxy silane and/or bis- [ gamma- (triethoxy silicon) propyl ] tetrasulfide. The primer for the silicon rubber provided by the invention can improve the adhesion of the single-component silicon rubber on the LOW-E glass surface and can also improve the adhesion of the double-component silicon rubber on the LOW-E glass surface.
Experimental results show that the cohesive failure of the primer for silicon rubber prepared by the invention can reach 85% or even 100% when the primer is matched with a single-component silicone adhesive or a double-component silicone adhesive. Therefore, the primer for the silicon rubber provided by the invention not only can enable the single-component silicon rubber to have better adhesion on a LOW-E glass surface, but also can enable the double-component silicon rubber to have better adhesion on the LOW-E glass surface.
In order to further illustrate the present invention, the following will describe a silicone rubber primer and a method for preparing the same in detail with reference to examples, but they should not be construed as limiting the scope of the present invention.
The starting materials used in the following examples are all generally commercially available.
Example 1
Preparation of adhesion promoter:
23.6g of gamma-glycidoxypropyltrimethoxysilane and 34g of bis (3-trimethoxysilylpropyl) amine were mixed, and stirred at room temperature for 60 minutes to obtain an adhesion promoter.
Preparation of a primer:
the methoxy silicone resin has a structure shown as a formula (I), wherein R1Is hydrogen; r2Is methyl, R3Is methyl and has a molecular weight of 2000.
Stirring and mixing 15g of the methoxy silicon resin, 6g of the adhesion promoter, 3g of methyl orthosilicate, 1g of n-butyl titanate, 1g of n-butyl zirconate, 3g of vinyl tri-tert-butyl peroxy silane and 71g of propyl acetate for 60min at normal temperature to obtain the primer for silicon rubber.
Comparative example 1
Preparation of adhesion promoter:
23.6g of gamma-glycidoxypropyltrimethoxysilane and 34g of bis (3-trimethoxysilylpropyl) amine were mixed, and stirred at room temperature for 60 minutes to obtain an adhesion promoter.
Preparation of a primer:
the methoxy silicone resin has a structure shown as a formula (I), wherein R1Is hydrogen; r2Is methyl, R3Is methyl and has a molecular weight of 2000.
Stirring and mixing 15g of the methoxy silicon resin, 6g of the adhesion promoter, 3g of methyl orthosilicate, 1g of n-butyl titanate, 1g of n-butyl zirconate, 3g of vinyl trimethoxy silane and 71g of propyl acetate at normal temperature for 60min to obtain the primer for silicon rubber.
Example 2
Preparation of adhesion promoter:
26g of 3- (2, 3-epoxypropoxy) propylmethyldiethoxysilane and 35g of bis (3-triethoxysilylpropyl) amine were mixed, and stirred at 55 ℃ for 60min to obtain an adhesion promoter.
Preparation of a primer:
the methoxy silicone resin has a structure shown as a formula (I), wherein R1Is methyl; r2Is methyl, R3Is methyl and has a molecular weight of 1500.
Stirring and mixing 15g of methoxy silicon resin, 9g of adhesion promoter, 1g of ethyl orthosilicate, 1g of isopropyl aluminate, 3g of isopropyl tris (dioctyl pyrophosphato acyloxy) ethylene titanate, 3g of vinyl tri-tert-butylperoxy silane and 68g of propyl acetate for 60min at normal temperature to obtain the primer for silicon rubber.
Example 3
Preparation of adhesion promoter:
26g of 3- (2, 3-epoxypropoxy) propylmethyldiethoxysilane and 35g of bis (3-triethoxysilylpropyl) amine were mixed, and stirred at 55 ℃ for 60min to obtain an adhesion promoter.
Preparation of a primer:
the methoxy silicone resin has a structure shown as a formula (I), wherein R1Is methyl; r2Is ethyl, R3Is methyl and has a molecular weight of 4000.
Stirring and mixing 15g of methoxy silicon resin, 9g of adhesion promoter, 1g of ethyl orthosilicate, 1g of isopropyl aluminate, 3g of isopropyl tris (dioctyl pyrophosphato acyloxy) ethylene titanate, 4g of bis- [ gamma- (triethoxy silicon) propyl ] tetrasulfide and 70g of propyl acetate at normal temperature for 60min to obtain the primer for silicon rubber.
Example 4
Preparation of adhesion promoter:
25g of 3- (2, 3-glycidoxy) propyl methyl dimethoxy silane and 35g N-phenyl-gamma-aminopropyl trimethoxy silane are mixed and stirred for 60min at 35 ℃ to obtain the adhesion promoter.
Preparation of a primer:
the methoxy silicone resin has a structure shown as a formula (I), wherein R1Is hydrogen; r2Is ethyl, R3Is methyl and has a molecular weight of 4000.
7g of the methoxy silicon resin, 3g of the adhesion promoter, 1g of ethyl orthosilicate, 0.5g of methyl orthosilicate, 0.5g of isopropyl aluminate, 0.5g of isobutyl zirconate, 2g of bis- [ gamma- (triethoxy silicon) propyl ] tetrasulfide and 86g of ethyl acetate are stirred and mixed for 90min at normal temperature to obtain the primer for silicon rubber.
Example 5
Preparation of adhesion promoter:
26g of 3- (2, 3-glycidoxy) propylmethyldimethoxysilane and 30g N-cyclohexyl-. gamma. -aminopropylmethyldimethoxysilane were mixed and stirred at 55 ℃ for 60min to obtain an adhesion promoter.
Preparation of a primer:
the methoxy silicone resin has a structure shown as a formula (I), wherein R1Is methyl; r2Is methyl, R3Is methyl and has a molecular weight of 3000.
18g of the methoxysilicon resin, 9g of the adhesion promoter, 2g of ethyl orthosilicate, 2g of methyl orthosilicate, 2g of n-butyl zirconate, 3g of tetraisopropyl bis (dioctylphosphite acyloxy) titanate, 2g of bis- [ gamma- (triethoxysilyl) propyl ] tetrasulfide, 2g of vinyltri-t-butylperoxysilane, 40g of propyl acetate and 20g of toluene were stirred and mixed at 50 ℃ for 60 minutes to obtain a primer for silicone rubber.
Comparative example 2
Preparation of adhesion promoter:
26g of 3- (2, 3-epoxypropoxy) propylmethyldiethoxysilane and 35g of bis (3-triethoxysilylpropyl) amine were mixed, and stirred at 55 ℃ for 60min to obtain an adhesion promoter.
Preparation of a primer:
the methoxy silicone resin has a structure shown as a formula (I), wherein R1Is methyl; r2Is methyl, R3Is methyl and has a molecular weight of 3000.
Stirring and mixing 15g of the methoxy silicon resin, 9g of the adhesion promoter, 1g of ethyl orthosilicate, 4g of bis- [ gamma- (triethoxy silicon) propyl ] tetrasulfide and 70g of propyl acetate at normal temperature for 60min to obtain the primer for silicon rubber.
Example 6
The adhesion performance of the primers for silicone rubber obtained in examples 1 to 5 and comparative examples 1 to 2 was examined:
and respectively coating the single-component silicone adhesive and the two-component silicone adhesive after the primer for the silicone rubber is coated on the surface of the LOW-E section. The adhesiveness was examined after oxidizing for 28 days at normal temperature. The results are shown in Table 1.
TABLE 1 adhesion Performance test results of the primers for silicon rubber obtained in examples 1 to 5 and comparative examples 1 to 2
| Single-component silicon rubber | Two-component silicon rubber | |
| Example 1 | 100% cohesive failure | 100% cohesive failure |
| Comparative example 1 | Peeling off | 20% cohesive failure |
| Example 2 | 90% cohesive failure | 100% cohesive failure |
| Example 3 | 95% cohesive failure | 100% cohesive failure |
| Example 4 | 85% cohesive failure | 100% cohesive failure |
| Example 5 | 100% cohesive failure | 100% cohesive failure |
| Comparative example 2 | 10% cohesive failure | 30% cohesive failure |
As can be seen from Table 1, the cohesive failure of the primer for silicone rubber prepared by the invention can reach 85% or even 100% when the primer is matched with a single-component silicone adhesive or matched with a two-component silicone adhesive. Therefore, the primer for the silicon rubber provided by the invention not only can enable the single-component silicon rubber to have better adhesion on a LOW-E glass surface, but also can enable the double-component silicon rubber to have better adhesion on the LOW-E glass surface.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. The primer for silicon rubber is characterized by comprising the following components in parts by weight:
the adhesion promoter is prepared by reacting epoxy silane and secondary amino silane;
the silane coupling agent is selected from vinyl tri-tert-butyl peroxy silane and/or bis- [ gamma- (triethoxy silicon) propyl ] tetrasulfide;
the methoxy silicon resin has a structure shown as a formula (I):
in the formula (I), R1Is hydrogen or methyl; r2Is methyl or ethyl; r3Is methyl.
2. The primer coating agent for silicone rubber according to claim 1, wherein the number average molecular weight of the methoxy silicon resin is 500 to 5000.
3. The primer for silicone rubber according to claim 1, wherein the epoxy silane is one or more selected from the group consisting of γ -glycidoxypropyltrimethoxysilane, 3- (2, 3-glycidoxy) propylmethyldiethoxysilane, 3- (2, 3-glycidoxy) propylmethyldimethoxysilane, γ -glycidoxypropyltriethoxysilane, β - (3, 4 epoxycyclohexyl) -ethyltriethoxysilane, and β - (3, 4 epoxycyclohexyl) -ethyltrimethoxysilane;
the secondary aminosilane is selected from one or more of N- (N-butyl) -gamma-aminopropyltrimethoxysilane, N-cyclohexyl-gamma-aminopropylmethyldimethoxysilane, bis (3-trimethoxysilylpropyl) amine, bis- (gamma-trimethoxysilylpropyl) amine, bis (3-triethoxysilylpropyl) amine and N-phenyl-gamma-aminopropyltrimethoxysilane.
4. The primer for silicone rubber according to claim 1, wherein the silicate is selected from methyl orthosilicate and/or ethyl orthosilicate.
5. The primer coating agent for silicone rubber according to claim 1, wherein the catalyst is one or more selected from titanate, zirconate, and aluminate.
6. The primer coating for silicone rubber according to claim 5, wherein the titanate is selected from one or more of isopropyl titanate, butyl titanate, polybutyl titanate, tetraisooctyl titanate, tetraethoxytitanium, tetrakis (2-ethylhexanol) titanium, n-propyl titanate, propyldioleate acyloxy (dioctylphosphonoxy) titanate, isopropyltris (dioctylphosphonoxy) titanate, isopropyltrioleate acyloxy titanate, isopropyltris (dodecylbenzenesulfonic acid) titanate, isopropyltris (dioctylphosphonoxy) ethylene titanate and tetraisopropylbis (dioctylphosphonoxy) titanate;
the zirconate is selected from one or more of n-butyl zirconate and isobutyl zirconate;
the aluminate is selected from one or more of diisopropyl di (ethyl acetoacetate) aluminate, isopropyl aluminate and diisopropyl di (acetylacetone) aluminate.
7. The primer for silicone rubber according to claim 1, wherein the solvent is one or more of butyl acetate, propyl acetate, toluene, ethyl acetate, and methyl ethyl ketone.
8. A method for producing the primer for silicone rubber according to claim 1, comprising the steps of:
mixing methoxy silicon resin, adhesion promoter, silicate ester, silane coupling agent, catalyst and solvent to obtain the primer for the silane modified adhesive.
9. The method according to claim 8, wherein the mixing is stirring mixing, the temperature of the mixing is 20 to 50 ℃, and the time of the mixing is 5 to 120 min.
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| CN111234737B (en) * | 2020-03-11 | 2021-05-28 | 杭州之江新材料有限公司 | Primer, preparation method, bonding method and application |
| CN112625598A (en) * | 2020-12-17 | 2021-04-09 | 成都硅宝科技股份有限公司 | Primer for silicon rubber self-adhesive tape and preparation method thereof |
| CN113717633B (en) * | 2021-05-08 | 2022-07-29 | 杭州师范大学 | Primer for bonding silicon resin thermal protection coating and preparation method and application thereof |
| CN117624604B (en) * | 2024-01-25 | 2024-04-16 | 以诺康医疗科技（苏州）有限公司 | Titanate-silicate oligomer, preparation method thereof, primer containing oligomer and application of primer |
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