CN113831877B - Modified epoxy resin adhesive and application thereof in hard mica plate - Google Patents
Modified epoxy resin adhesive and application thereof in hard mica plate Download PDFInfo
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- CN113831877B CN113831877B CN202111133116.9A CN202111133116A CN113831877B CN 113831877 B CN113831877 B CN 113831877B CN 202111133116 A CN202111133116 A CN 202111133116A CN 113831877 B CN113831877 B CN 113831877B
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B19/00—Layered products comprising a layer of natural mineral fibres or particles, e.g. asbestos, mica
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
Abstract
The invention discloses a modified epoxy resin adhesive and application thereof in a hard mica plate, wherein the modified epoxy resin adhesive comprises the following components in percentage by weight: 40-80 parts of epoxy resin; 10-21 parts of epoxy-terminated phenyl silicone oil; 20-40 parts of phenolic resin; 0.5-5 parts of silane coupling agent; 3-8 parts of polyvinyl formal aldehyde; 100-220 parts of diluent. The invention solves the problems of brittleness, severe high-temperature degradation, high smoke odor, easy striae, more scraps, low cutting precision and the like of a mica plate prepared from the traditional epoxy resin after solidification, and provides the epoxy resin adhesive for the mica plate.
Description
Technical Field
The invention relates to the field of electrical insulation materials, in particular to a modified epoxy resin adhesive and a butt joint method.
Background
Epoxy resins are a generic term for compounds containing two or more epoxy groups in the molecule, and are one of the three thermosetting resin materials most commonly used in the modern industry. The epoxy resin has the advantages of high mechanical strength, good bonding performance, good chemical property stability, good electrical insulation performance, wide curing temperature range, corrosion resistance and the like, and is widely applied to various aspects of chemical industry, electronic packaging, plastics, paint industry, machinery, national defense, large hydraulic engineering, civil engineering and building industry and the like.
The mica paper is made from mica ore as raw material by chemical or hydraulic breaking pulping. The mica plate is formed by gluing mica paper through a gluing machine, drying, cutting, stacking paper and pressing at high temperature. Mica boards and mica paper are widely applied to a plurality of fields requiring high-temperature insulation, such as industry, aerospace, generator sets, household appliances and the like. In the current-stage mica plate industry, glue is mainly divided into epoxy resin glue and silicone resin glue, and the mica plate is divided into an epoxy plate and a silicone resin plate according to different glue types.
The epoxy resin material has the advantages of high mechanical strength and good bonding performance, plays a unique role in the fields with high strength and high bonding requirements, but the traditional epoxy resin has the defects of high internal stress, easy brittleness, serious high-temperature degradation, easy cracking, chipping, serious high-temperature fuming and the like in cutting due to the special structure of the traditional epoxy resin, and influences the product quality. There is an urgent need for modification studies on epoxy resin materials to provide them with more excellent comprehensive properties.
Disclosure of Invention
The invention aims to solve the problems that a mica plate prepared from the traditional epoxy resin is brittle after solidification, is easily degraded seriously at high temperature, is large in smoke odor at high temperature, is easy to fry in cutting, is more in chips, is low in cutting precision and the like, and provides the epoxy resin adhesive for the mica plate.
In order to achieve the above purpose, the present invention provides the following technical solutions: the modified epoxy resin adhesive is characterized by comprising the following components in parts by weight:
as a preferable scheme of the invention, the epoxy resin is one or a mixture of more of bisphenol A epoxy resin, bisphenol F epoxy resin and bisphenol S epoxy resin; bisphenol a epoxy resins are preferred.
As a preferred scheme of the invention, the epoxy-terminated phenyl trisiloxane is an epoxy-terminated phenyl trisiloxane and has the following structure:
as a preferred embodiment of the present invention, the phenolic resin is a low molecular weight liquid thermosetting phenolic resin.
As a preferable mode of the invention, the silane coupling agent is a silane coupling agent containing an epoxy group in a molecule.
As a preferable scheme of the invention, the silane coupling agent is one or a mixture of more of gamma-glycidoxypropyl trimethoxysilane, beta- (3, 4-epoxycyclohexyl) ethyl trimethoxysilane and glycidoxypropyl methyl diethoxy silane. Gamma-glycidoxypropyl trimethoxysilane is preferred.
As a preferred embodiment of the present invention, the diluent includes alcohols and benzene; the mass ratio of the alcohols to the benzene is 3-5:5-7. The alcohol is preferably ethanol and the benzene is preferably xylene.
As a preferred scheme of the invention, the preparation method of the modified epoxy resin adhesive comprises the following steps:
s1, adding epoxy resin, phenolic resin, epoxy phenyl silicone oil, polyvinyl formal and benzene diluents, which can be toluene or xylene, into a sol kettle, heating to 80-120 ℃, uniformly mixing, and dissolving into a liquid state;
s2, cooling to 20-30 ℃, adding the silane coupling agent and the alcohol diluent, and uniformly stirring.
The invention also provides application of the modified epoxy resin adhesive in the hard mica plate, and the application method comprises the following steps:
uniformly coating modified epoxy resin glue on the surface of mica paper by adopting a coating machine, wherein the glue application amount is 8% -10%;
step two, uniformly passing the coated mica paper through a drying tunnel with the temperature raised at the stage of 50-150 ℃ for about 3-5 min;
and thirdly, cutting the mica paper after the mica paper is discharged from the drying tunnel into required size, stacking the mica paper together according to the thickness requirement, sending the mica paper into a plate vulcanizing machine for hot pressing for 3-5 hours, wherein the hot pressing temperature is 100-250 ℃, the pressure is 1.5-10 MPa, and cooling to room temperature after hot pressing to obtain the hard epoxy mica plate.
Compared with the prior art, the invention has the following beneficial effects: the epoxy phenyl silicone oil at the introduction end in the epoxy resin system can utilize the flexibility of the Si-O bond of the siloxane, so that the internal stress of the epoxy resin is reduced, and the cracking is reduced; meanwhile, the introduction of siloxane can obviously improve the temperature resistance of the epoxy resin and reduce fuming; the silane coupling agent containing epoxy groups can be adopted to form chemical bonds between alkoxy groups in the coupling agent and mica paper, so that the wettability and the adhesiveness of epoxy resin glue on the mica paper are increased; the polyvinyl formal acetal can improve the bonding strength, toughness and wear resistance of the whole glue system.
The mica plate prepared by the invention has the advantages of smooth surface, high strength, no brittleness during cutting, less scraps during cutting, difficult generation of striae (cracks) at cutting positions, no sticking of dies during cutting, and capability of greatly improving cutting precision and product qualification rate.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
60kg of epoxy resin, 12kg of epoxy phenyl silicone oil, 27kg of liquid phenolic resin, 5kg of polyvinyl formal acetal and 84kg of toluene are put into a reaction kettle, stirring and heating are started, the temperature is kept at about 105 ℃ for 1.5h to completely dissolve and uniformly mix the materials, cooling water is started to cool the materials, 126kg of methanol and 2.5kg of gamma-glycidyl ether oxypropyl trimethoxysilane are added into the reaction kettle when the temperature of the materials is reduced to 27+/-3 ℃, stirring is continued for 30min, and the modified epoxy resin adhesive is obtained after discharging.
Example 2
55kg of epoxy resin, 16kg of epoxy phenyl silicone oil, 30kg of liquid phenolic resin, 8kg of polyvinyl formal and 84kg of toluene are put into a reaction kettle, stirring and heating are started, the temperature is kept at about 105 ℃ for 1.5 hours to completely dissolve and uniformly mix the materials, cooling water is started to cool the materials, 126kg of methanol and 3kg of beta- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane are added into the reaction kettle when the temperature of the materials is reduced to 27 ℃ +/-3 ℃, stirring is continued for 30 minutes, and the modified epoxy resin adhesive is obtained after discharging.
Example 3
50kg of epoxy resin, 21kg of epoxy phenyl silicone oil, 30kg of liquid phenolic resin, 7.5kg of polyvinyl formal acetal and 84kg of toluene are put into a reaction kettle, stirring and heating are started, the temperature is kept at about 105 ℃ for 1.5h to completely dissolve and uniformly mix materials, cooling water is started to cool the materials, 126kg of methanol is added into the reaction kettle when the temperature of the materials is reduced to 27+/-3 ℃, 5kg of glycidoxypropyl methyl diethoxy silane is continuously stirred for 30min, and the modified epoxy resin adhesive is obtained after discharging.
Example 4
60kg of epoxy resin, 12kg of epoxy phenyl silicone oil, 27kg of liquid phenolic resin, 5kg of polyvinyl formal acetal and 84kg of dimethylbenzene are put into a reaction kettle, stirring and heating are started, the temperature is kept at about 105 ℃ for 1.5h to completely dissolve and uniformly mix the materials, cooling water is started to cool the materials, 126kg of ethanol and 2.5kg of gamma-glycidyl ether oxypropyl trimethoxysilane are added into the reaction kettle when the temperature of the materials is reduced to 27+/-3 ℃, stirring is continued for 30min, and the modified epoxy resin adhesive is obtained after discharging.
Example 5
55kg of epoxy resin, 12kg of epoxy phenyl silicone oil, 25kg of liquid phenolic resin, 7kg of polyvinyl formal acetal and 84kg of toluene are put into a reaction kettle, stirring and heating are started, the temperature is kept at about 105 ℃ for 1.5h to completely dissolve and uniformly mix materials, cooling water is started to cool the materials, 126kg of methanol and 2.5kg of gamma-glycidyl ether oxypropyl trimethoxysilane are added into the reaction kettle when the temperature of the materials is reduced to 27+/-3 ℃, stirring is continued for 30min, and the modified epoxy resin adhesive is obtained after discharging.
Blank control group
60kg of epoxy resin, 27kg of liquid phenolic resin and 84kg of toluene are put into a reaction kettle, stirring and heating are started, the temperature is kept at about 105 ℃ for 1.5 hours to completely dissolve and uniformly mix materials, cooling water is started to cool the materials, 126kg of methanol is added into the reaction kettle when the temperature of the materials is reduced to 27+/-3 ℃, stirring is continued for 30 minutes, and the modified epoxy resin adhesive is obtained after discharging.
Control group 1
60kg of epoxy resin, 12kg of epoxy phenyl silicone oil, 27kg of liquid phenolic resin, 12kg of polyvinyl formal acetal and 84kg of toluene are put into a reaction kettle, stirring and heating are started, the temperature is kept at about 105 ℃ for 1.5h to completely dissolve and uniformly mix materials, cooling water is started to cool the materials, 126kg of methanol and 2.5kg of gamma-glycidyl ether oxypropyl trimethoxysilane are added into the reaction kettle when the temperature of the materials is reduced to 27+/-3 ℃, stirring is continued for 30min, and the modified epoxy resin adhesive is obtained after discharging.
Control group 2
60kg of epoxy resin, 12kg of epoxy phenyl silicone oil, 27kg of liquid phenolic resin, 1.5kg of polyvinyl formal acetal and 84kg of toluene are put into a reaction kettle, stirring and heating are started, the temperature is kept at about 105 ℃ for 1.5h to completely dissolve and uniformly mix materials, cooling water is started to cool the materials, 126kg of methanol and 2.5kg of gamma-glycidyl ether oxypropyl trimethoxysilane are added into the reaction kettle when the temperature of the materials is reduced to 27+/-3 ℃, stirring is continued for 30min, and the modified epoxy resin adhesive is obtained after discharging.
Control group 3
60kg of epoxy resin, 27kg of liquid phenolic resin, 5kg of polyvinyl formal-aldehyde and 84kg of toluene are put into a reaction kettle, stirring and heating are started, the temperature is kept at about 105 ℃ for 1.5 hours to completely dissolve and uniformly mix the materials, cooling water is started to cool the materials, 126kg of methanol and 2.5kg of gamma-glycidyl ether oxypropyl trimethoxy silane are added into the reaction kettle when the temperature of the materials is reduced to 27+/-3 ℃, stirring is continued for 30 minutes, and discharging is carried out to obtain the modified epoxy resin adhesive.
Control group 4
55kg of epoxy resin, 12kg of epoxy phenyl silicone oil, 25kg of liquid phenolic resin, 12kg of polyvinyl formal acetal and 84kg of toluene are put into a reaction kettle, stirring and heating are started, the temperature is kept at about 105 ℃ for 1.5h to completely dissolve and uniformly mix materials, cooling water is started to cool the materials, 126kg of methanol, 1.5kg of gamma-glycidyl ether oxypropyl trimethoxysilane and 2.5kg of gamma-glycidyl ether oxypropyl trimethoxysilane are added into the reaction kettle when the temperature of the materials is reduced to 27+/-3 ℃, stirring is continued for 30min, and the modified epoxy resin adhesive is obtained after discharging.
Control group 5
55kg of epoxy resin, 12kg of epoxy phenyl silicone oil, 25kg of liquid phenolic resin, 1.5kg of polyvinyl formal acetal and 84kg of toluene are put into a reaction kettle, stirring and heating are started, the temperature is kept at about 105 ℃ for 1.5h to completely dissolve and uniformly mix materials, cooling water is started to cool the materials, 126kg of methanol, 1.5kg of gamma-glycidyl ether oxypropyl trimethoxysilane and 2.5kg of gamma-glycidyl ether oxypropyl trimethoxysilane are added into the reaction kettle when the temperature of the materials is reduced to 27+/-3 ℃, stirring is continued for 30min, and the modified epoxy resin adhesive is obtained after discharging.
Control group 6
55kg of epoxy resin, 25kg of liquid phenolic resin, 7kg of polyvinyl formal and 84kg of toluene are put into a reaction kettle, stirring and heating are started, the temperature is kept at about 105 ℃ for 1.5 hours to completely dissolve and uniformly mix materials, cooling water is started to cool the materials, 126kg of methanol, 1.5kg of gamma-glycidyl ether oxypropyl trimethoxysilane and 2.5kg of gamma-glycidyl ether oxypropyl trimethoxysilane are added into the reaction kettle when the temperature of the materials is reduced to 27 ℃ +/-3 ℃, stirring is continued for 30 minutes, and discharging is carried out to obtain the modified epoxy resin adhesive.
Uniformly coating the modified epoxy resin adhesives prepared in the examples 1-5, the blank control groups and the control groups 1-6 on mica paper through an automatic glue spreader respectively, then enabling the glue solution to pass through a drying tunnel at a speed of 8m/min, and setting the temperature of the drying tunnel in a sectional heating mode: the first section 50 ℃, the second section 80 ℃, the third section 110 ℃, the fourth section 130 ℃ and the fifth section 150 ℃ to obtain the sized mica paper;
cutting the glued mica paper into paper with the length and width of 1.1m, stacking the glued mica paper with the glue facing upwards for 11 layers, placing the paper on a flat vulcanizing machine for hot pressing, wherein the initial temperature of hot pressing is 110 ℃, the temperature is increased by 30 ℃ every 15min, and the maximum temperature is 250 ℃ and the pressure is 10Mpa. Exhausting before each heating in the pressing process, and performing forced cooling to 60 ℃ after pressing to obtain the mica plate.
The hard mica plates prepared in examples 1 to 5, blank control groups and control groups 1 to 6 were subjected to performance test and comparison, and the bending strength was GB/T5019.2-2009 (bending strength and bending modulus); the hard mica material for IEC371-3-3 heating equipment is adopted in the condition of 600 ℃ fuming and foaming; boiling with GB/T5019.2-2009 (folding) for 1.5 hours; the cutting performance is judged by visually observing whether a cutting surface has cracks after a plate is cut by a plate cutting machine, and the occurrence of cracks (striae) can influence cutting precision, so that product flaws are even disqualified;
as shown in table 1.
TABLE 1
The comparison results of the above embodiments show that the modified epoxy resin adhesive can obviously improve the mechanical property, the temperature resistance, the moisture resistance and the cutting processability of the mica plate. Wherein, according to the comparison groups 1-6, the polyvinyl formal acetal can improve the bending strength of the mica plate, and when the polyvinyl formal acetal and the epoxy phenyl silicone oil are added into the epoxy resin according to a certain proportion, the bending strength of the mica plate can be obviously improved, and the performance of the mica plate is further improved.
The invention is not limited to the embodiments described above, but a number of modifications and adaptations can be made by a person skilled in the art without departing from the principle of the invention, which modifications and adaptations are also considered to be within the scope of the invention. What is not described in detail in this specification is prior art known to those skilled in the art.
Claims (8)
1. The modified epoxy resin adhesive is characterized by comprising the following components in parts by weight:
40-80 parts of epoxy resin
10-21 parts of epoxy-terminated phenyl silicone oil
20-40 parts of phenolic resin
Silane coupling agent 0.5-5 parts
3-8 parts of polyvinyl formal aldehyde
100-220 parts of a diluent;
the epoxy-terminated phenyl trisiloxane is characterized in that the epoxy-terminated phenyl trisiloxane has the following structure:
。
2. the modified epoxy resin glue of claim 1, wherein the epoxy resin is one or more of bisphenol a epoxy resin, bisphenol F epoxy resin, bisphenol S epoxy resin.
3. The modified epoxy resin glue of claim 1, wherein the phenolic resin is a low molecular weight liquid thermosetting phenolic resin.
4. The modified epoxy resin glue of claim 1, wherein the silane coupling agent is a silane coupling agent containing an epoxy group in a molecule.
5. The modified epoxy resin adhesive of claim 4, wherein the silane coupling agent is one or a mixture of a plurality of gamma-glycidoxypropyl trimethoxysilane, beta- (3, 4-epoxycyclohexyl) ethyl trimethoxysilane and glycidoxypropyl methyl diethoxysilane.
6. The modified epoxy resin glue of claim 1, wherein the diluent comprises alcohols and benzenes; the mass ratio of the alcohols to the benzene is 3-5:5-7.
7. The modified epoxy resin glue of claim 6, wherein the method for preparing the modified epoxy resin glue comprises the following steps:
s1, adding epoxy resin, phenolic resin, epoxy phenyl silicone oil, polyvinyl formal and benzene diluents into a sol kettle, heating to 80-120 ℃, uniformly mixing, and dissolving into a liquid state;
and S2, cooling to 20-30 ℃, adding the silane coupling agent and the alcohol diluent, and uniformly stirring.
8. The application of the modified epoxy resin adhesive in the hard mica plate as claimed in any one of claims 1 to 7, which is characterized in that the application method is as follows:
uniformly coating modified epoxy resin glue on the surface of mica paper by using a coating machine, wherein the glue application amount is 8% -10%;
step two, uniformly passing the coated mica paper through a drying tunnel with the temperature increased at the stage of 50-150 ℃ for 3-5 minutes;
and thirdly, cutting the mica paper after the mica paper is discharged from the drying channel into required dimensions, stacking the mica paper together according to the thickness requirement, sending the mica paper into a flat vulcanizing machine for hot pressing for 3-5 hours, wherein the hot pressing temperature is 100-250 ℃, the pressure is 1.5-10 MPa, and cooling to room temperature after hot pressing to obtain the hard epoxy mica plate.
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| CN111516282A (en) * | 2020-04-24 | 2020-08-11 | 湖北平安电工材料有限公司 | Preparation method of laminated mica magnetic conduction plate |
| CN112852285A (en) * | 2021-03-01 | 2021-05-28 | 广东欣创新材料科技有限公司 | Manufacturing process of moisture-proof corrosion-resistant UV high-light plate capable of generating negative ions |
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