CN110387210B - EB (Epstein-Barr) curing-based adhesive and preparation method of mica tape with same - Google Patents
EB (Epstein-Barr) curing-based adhesive and preparation method of mica tape with same Download PDFInfo
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- CN110387210B CN110387210B CN201910699574.5A CN201910699574A CN110387210B CN 110387210 B CN110387210 B CN 110387210B CN 201910699574 A CN201910699574 A CN 201910699574A CN 110387210 B CN110387210 B CN 110387210B
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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
- 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
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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
- 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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- 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
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
-
- 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
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B9/047—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material made of fibres or filaments
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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
- C09J183/00—Adhesives 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; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
- C09J183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
-
- 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
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/10—Inorganic fibres
- B32B2262/101—Glass fibres
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention relates to an EB (Epstein-Barr) curing-based adhesive which comprises, by mass, 30-50% of acrylate modified silicone oil, 10-30% of vinyl silicone oil, 10-30% of an acrylate diluent monomer and 5-10% of a coupling agent; the preparation method comprises the following steps: s1, preparing an adhesive solution, immersing the alkali-free glass cloth in the adhesive solution, and forming an adhesive layer on the surface of the alkali-free glass cloth through a dip coating process; s2, compounding the alkali-free glass cloth with the adhesive layer and mica paper together, and uniformly permeating for 45S to obtain a mica tape; and S3, carrying out electron beam irradiation on the mica tape, and rolling and slitting after the irradiation is finished. The EB curing adhesive does not need any volatile solvent, the solid content of the adhesive is 100%, and VOC (volatile organic compounds) is not discharged; the EB is adopted to cure the mica tape without baking, so that the heat generated during curing is very low, and the energy is saved; the invention has high production efficiency, and the production speed can reach 20m/min or even higher.
Description
Technical Field
The invention relates to the technical field of mica tape preparation, in particular to an EB (Epstein-Barr) curing-based adhesive and a preparation method of a mica tape with the EB curing-based adhesive.
Background
The mica tape is an insulating material formed by baking, drying and cutting reinforcing materials such as mica paper, glass fiber cloth and the like together with a proper adhesive, has excellent high-temperature resistance and combustion resistance, has good flexibility in a normal state, and is suitable for fire-resistant insulating layers of various fire-resistant electromagnetic cables and coils; at present, the method for producing mica tapes in China is to prepare a mica tape adhesive solution by using a solvent and resin, compound the mica tape adhesive solution with mica paper after impregnating a reinforcing material, remove the solvent by heating, roll and cut the mica tape adhesive solution (referred to as impregnation gluing or wet gluing process). Because the mica paper has strong adhesive absorption capacity, when the impregnation gluing process is adopted, most of the liquid adhesive can penetrate into the mica paper layers to fill the gaps among the mica sheets, and the other part of the adhesive forms a continuous and uniform adhesive film on the interface of the glass cloth reinforcing material and the mica paper.
The preparation of the mica tape needs a large amount of toluene solvent to dilute the glue and then meets the requirements of the gluing process, the recovery rate of the toluene solvent in the production process is only about 70 percent, so the toluene can be inevitably volatilized into the atmosphere and cause serious pollution to the environment, and in addition, the toluene belongs to flammable and explosive liquid and has great threat to the health of operators and personal safety; meanwhile, the mica tape needs to be baked in an oven with the length of 30 meters in the manufacturing process, the energy consumption is high, the occupied area is large, the linear speed of the mica tape is generally 10m/min due to the limitations of the dip-coating speed and the baking speed, and the efficiency is low.
Disclosure of Invention
The invention aims to solve the technical problem of providing an EB curing-based adhesive which has no VOC volatilization, small facility floor area and can improve the preparation speed and a preparation method of a mica tape with the EB curing-based adhesive.
The technical scheme adopted by the invention for solving the technical problems is as follows: an EB curing-based adhesive comprises the following components in percentage by mass,
more specifically, the acrylate functional group of the acrylate modified silicone oil is one or more of monofunctional, bifunctional and trifunctional.
More specifically, the viscosity of the acrylate modified silicone oil is between 100 and 5000 cps.
More specifically, the vinyl silicone oil contains 8-15% of vinyl.
More specifically, the viscosity of the vinyl silicone oil is 300-5000 cps.
More specifically, the acrylate diluent monomer is one or a mixture of isobornyl acrylate, isobornyl methacrylate, 2-ethylhexyl acrylate and 3,3, 5-trimethylcyclohexyl acrylate.
More specifically, the coupling agent adopts one or more of a coupling agent containing an acrylate functional group or a coupling agent containing a vinyl functional group.
More specifically, the coupling agent containing acrylate functional group comprises 3-trimethoxy silane acrylate propyl ester and methacryloxypropyl trimethoxy silane; the coupling agent containing vinyl functional groups comprises vinyl tributyrinoxime silane and vinyl trimethoxy silane.
A preparation method of the adhesive mica tape based on EB curing comprises the following steps,
s1, preparing an adhesive solution, immersing the alkali-free glass cloth in the adhesive solution, and forming an adhesive layer on the surface of the alkali-free glass cloth through a dip coating process;
s2, compounding the alkali-free glass cloth with the adhesive layer and the mica paper together, and enabling the mixture to uniformly permeate for 45 seconds to obtain a mica tape;
s3, performing electron beam irradiation on the mica tape in a nitrogen atmosphere with oxygen concentration lower than 200ppm, and winding and cutting after the irradiation is completed.
More specifically, in the step S3, the irradiation height of the electron beam irradiation is 20mm, the mica tape conveying speed is 25m/min, the electron beam energy is 500kev, and the electron beam curing dose is 50 kgy.
The invention has the beneficial effects that: 1. the EB curing adhesive does not need any volatile solvent, the solid content of the adhesive is 100%, VOC (volatile organic compounds) cannot be discharged into the air, and the safety and the body health of workers cannot be influenced; 2. the EB is adopted to cure the mica tape without baking, so that the heat generated during curing is very low, the energy consumption is low, and the energy is saved; 3. the production efficiency of the invention is high, the production speed of the traditional mica tape production process is 10m/min because of the limitation of the area of the field, and the production speed of the EB curing mica tape can reach 20m/min or even higher.
Detailed Description
The present invention is described in detail below.
An EB curing-based adhesive comprises the following components in percentage by mass,
the acrylate modified silicone oil comprises acrylate functional groups with single functionality, double functionality and tri-functionality, wherein the acrylate functional groups can only comprise single functionality, double functionality or tri-functionality, and can also be combined by two or more of the single functionality, the double functionality and the tri-functionality; the viscosity of the acrylate modified silicone oil is controlled to be 100-5000 cps.
The vinyl silicone oil contains 8-15% of vinyl (calculated by methyl vinyl silicone chain units); the viscosity of the vinyl silicone oil is 300-5000 cps.
The acrylate diluent monomer is one of isobornyl acrylate, isobornyl methacrylate, 2-ethylhexyl acrylate and 3,3, 5-trimethylcyclohexyl acrylate, or two or more of isobornyl acrylate, isobornyl methacrylate, 2-ethylhexyl acrylate and 3,3, 5-trimethylcyclohexyl acrylate; it has good solubility and dilutability.
The coupling agent is one or a mixture of more of a coupling agent containing acrylate functional groups or a coupling agent containing vinyl functional groups; the coupling agent containing acrylate functional group comprises 3-trimethoxy silane acrylate propyl ester and methacryloxypropyl trimethoxy silane; the coupling agent containing vinyl functional group includes vinyl tributyrinoxime silane and vinyl trimethoxy silane.
The mica tape is prepared by the adhesive according to the preparation method,
s1, preparing an adhesive solution, immersing the alkali-free glass cloth in the adhesive solution, and forming an adhesive layer on the surface of the alkali-free glass cloth through a dip coating process;
s2, compounding the alkali-free glass cloth with the adhesive layer and the mica paper together, and enabling the mixture to uniformly permeate for 45 seconds to obtain a mica tape;
s3, performing electron beam irradiation on the mica tape in a nitrogen atmosphere with oxygen concentration lower than 200ppm, and winding and cutting after the irradiation is completed.
The following is an example of the preparation of a mica tape according to the above preparation method.
Example 1
D1 preparation of adhesive solution based on EB curing
40kg of monofunctional acrylate modified silicone oil, 15kg of vinyl silicone oil with a vinyl content of 8%, 20kg of isobornyl acrylate and 5kg of 3-trimethoxy silane acrylic acrylate were put into a reaction vessel and mixed for 20 minutes to prepare an adhesive solution based on EB curing.
D2 preparation of mica tape
23g/m2The alkali-free glass cloth is dipped into glue filled with an adhesive solution based on EB curingIn the tank, an adhesive layer is formed on the surface of the alkali-free glass cloth by a dip coating process, and the alkali-free glass cloth with the adhesive layer is mixed with 165g/m2Compounding natural gold mica paper, and uniformly permeating for 45s to obtain the mica tape.
D3 EB curing mica tape
Carrying out electron beam irradiation on the mica tape obtained in the step D2 in a nitrogen atmosphere with oxygen concentration lower than 200ppm, wherein the irradiation height of the electron beam irradiation is 20mm, the conveying speed of the mica tape is 25m/min, the energy of the electron beam is 500kev, and the curing dose of the electron beam is 50 kgy; and (5) winding and cutting after the irradiation is finished to obtain a finished product.
Example 2
D1 preparation of adhesive solution based on EB curing
20kg of monofunctional acrylate modified silicone oil and 15kg of bifunctional acrylate modified silicone oil are taken, 10kg of vinyl silicone oil with the vinyl content of 8%, 20kg of 2-ethylhexyl acrylate and 5kg of methacryloxypropyl trimethoxy silane are put into a reaction vessel for mixing, and the time is controlled to be 20 minutes, so that the adhesive solution based on EB curing is prepared.
D2 preparation of mica tape
23g/m2The alkali-free glass cloth is immersed into a glue tank filled with an adhesive solution based on EB curing, an adhesive layer is formed on the surface of the alkali-free glass cloth through a dip coating process, and the alkali-free glass cloth with the adhesive layer and 165g/m are mixed2Compounding natural gold mica paper, and uniformly permeating for 45s to obtain the mica tape.
D3 EB curing mica tape
Carrying out electron beam irradiation on the mica tape obtained in the step D2 in a nitrogen atmosphere with oxygen concentration lower than 200ppm, wherein the irradiation height of the electron beam irradiation is 20mm, the conveying speed of the mica tape is 25m/min, the energy of the electron beam is 500kev, and the curing dose of the electron beam is 50 kgy; and (5) winding and cutting after the irradiation is finished to obtain a finished product.
Example 3
D1 preparation of adhesive solution based on EB curing
30kg of monofunctional acrylate modified silicone oil, 5kg of bifunctional acrylate modified silicone oil and 5kg of trifunctional acrylate modified silicone oil are taken, 15kg of vinyl silicone oil with the vinyl content of 8%, 20kg of 3,3, 5-trimethylcyclohexyl acrylate and 8kg of vinyltrimethoxysilane are taken and put into a reaction vessel for mixing, and the time is controlled to be 20 minutes, so that the adhesive solution based on EB curing is prepared.
D2 preparation of mica tape
23g/m2The alkali-free glass cloth is immersed into a glue tank filled with an adhesive solution based on EB curing, an adhesive layer is formed on the surface of the alkali-free glass cloth through a dip coating process, and the alkali-free glass cloth with the adhesive layer and 165g/m are mixed2Compounding natural gold mica paper, and uniformly permeating for 45s to obtain the mica tape.
D3 EB curing mica tape
Carrying out electron beam irradiation on the mica tape obtained in the step D2 in a nitrogen atmosphere with oxygen concentration lower than 200ppm, wherein the irradiation height of the electron beam irradiation is 20mm, the conveying speed of the mica tape is 25m/min, the energy of the electron beam is 500kev, and the curing dose of the electron beam is 50 kgy; and (5) winding and cutting after the irradiation is finished to obtain a finished product.
Example 4
D1 preparation of adhesive solution based on EB curing
30kg of monofunctional acrylate modified silicone oil, 10kg of bifunctional acrylate modified silicone oil and 5kg of trifunctional acrylate modified silicone oil are taken, 20kg of vinyl silicone oil with the vinyl content of 10%, 25kg of isoborneol methacrylate and 10kg of vinyl tributyrinoxime silane are put into a reaction vessel for mixing, and the time is controlled to be 20 minutes, so that the adhesive solution based on EB curing is prepared.
D2 preparation of mica tape
23g/m2The alkali-free glass cloth is immersed into a glue tank filled with an adhesive solution based on EB curing, an adhesive layer is formed on the surface of the alkali-free glass cloth through a dip coating process, and the alkali-free glass cloth with the adhesive layer and 165g/m are mixed2Compounding natural gold mica paper, and uniformly permeating for 45s to obtain the mica tape.
D3 EB curing mica tape
Carrying out electron beam irradiation on the mica tape obtained in the step D2 in a nitrogen atmosphere with oxygen concentration lower than 200ppm, wherein the irradiation height of the electron beam irradiation is 20mm, the conveying speed of the mica tape is 25m/min, the energy of the electron beam is 500kev, and the curing dose of the electron beam is 50 kgy; and (5) winding and cutting after the irradiation is finished to obtain a finished product.
The performance of the mica tape manufactured in a common way is tested and compared with the performance of the 4 examples, and the comparison result is as follows:
as can be seen from the 4 embodiments and the proportion, the performance of the mica tape prepared by the preparation method is basically consistent with that of the mica tape prepared by the prior art, and the performance of the mica tape can reach that of the traditional mica tape.
In conclusion, the EB curing adhesive disclosed by the invention does not need any volatile solvent, the solid content of the adhesive is 100%, VOC (volatile organic compounds) cannot be discharged into the air, and the safety and the body health of workers cannot be influenced; the EB is adopted to cure the mica tape without baking, so that the heat generated during curing is very low, the energy consumption is low, and the energy is saved; the production efficiency of the invention is high, the production speed of the traditional mica tape production process is 10m/min because of the limitation of the area of the field, and the production speed of the EB curing mica tape can reach 20m/min or even higher.
It is to be emphasized that: the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and all simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (9)
1. A preparation method of an EB curing-based adhesive mica tape is characterized in that the adhesive comprises the following components in percentage by mass,
30-50% of acrylate modified silicone oil;
10-30% of vinyl silicone oil;
10-30% of an acrylate diluent monomer;
5-10% of a coupling agent;
the steps of the preparation method are as follows,
s1, preparing an adhesive solution, immersing the alkali-free glass cloth in the adhesive solution, and forming an adhesive layer on the surface of the alkali-free glass cloth through a dip coating process;
s2, compounding the alkali-free glass cloth with the adhesive layer and the mica paper together, and enabling the mixture to uniformly permeate for 45 seconds to obtain a mica tape;
s3, performing electron beam irradiation on the mica tape in a nitrogen atmosphere with oxygen concentration lower than 200ppm, and winding and cutting after the irradiation is completed.
2. The method for preparing the EB-curing-based adhesive mica tape according to claim 1, wherein the acrylate functional group of the acrylate modified silicone oil is one or more of monofunctional, bifunctional and trifunctional.
3. The method for preparing the mica tape based on the EB curing adhesive according to claim 2, wherein the viscosity of the acrylate modified silicone oil is 100 to 5000 cps.
4. The method for preparing the adhesive mica tape based on EB curing according to claim 1, wherein the vinyl silicone oil contains 8-15% of vinyl.
5. The method for preparing the EB curing based adhesive mica tape according to claim 4, wherein the viscosity of the vinyl silicone oil is 300 to 5000 cps.
6. The method for preparing the EB curing-based adhesive mica tape according to claim 1, wherein the acrylate diluent monomer is one or more of isobornyl acrylate, isobornyl methacrylate, 2-ethylhexyl acrylate, and 3,3, 5-trimethylcyclohexyl acrylate.
7. The method for preparing the EB-curing-based adhesive mica tape according to claim 1, wherein the coupling agent is one or more of a coupling agent containing acrylate functional groups or a coupling agent containing vinyl functional groups.
8. The method for preparing the EB-curing-based adhesive mica tape according to claim 7, wherein the acrylate functional group-containing coupling agent is 3-trimethoxy silane propyl acrylate or methacryloxypropyl trimethoxy silane; the coupling agent containing vinyl functional groups is vinyl tributyrinoxime silane or vinyl trimethoxy silane.
9. The method for preparing mica tape with adhesive based on EB curing as claimed in claim 1, wherein the irradiation height of electron beam irradiation in step S3 is 20mm, the mica tape conveying speed is 25m/min, the electron beam energy is 500kev, and the electron beam curing dose is 50 kgy.
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| CN112159642A (en) * | 2020-09-25 | 2021-01-01 | 中广核达胜加速器技术有限公司 | Adhesive, preparation method and curing method of flame-retardant glass fiber tape |
| CN112625646A (en) * | 2020-12-15 | 2021-04-09 | 上海瑞且盟材料科技有限公司 | Mica tape adhesive based on electron beam curing and preparation process thereof |
| CN113470906A (en) * | 2021-05-24 | 2021-10-01 | 中广核新奇特(扬州)电气有限公司 | Production process of electron beam curing mica tape |
| CN113681915A (en) * | 2021-07-15 | 2021-11-23 | 中广核新奇特(扬州)电气有限公司 | Preparation method for producing double-sided film reinforced mica tape in electron beam curing mode |
| CN114843050A (en) * | 2022-06-02 | 2022-08-02 | 中广核达胜加速器技术有限公司 | Method for rapidly preparing mica tapes in batches |
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| CN101432357A (en) * | 2006-05-01 | 2009-05-13 | 出光兴产株式会社 | Optical semiconductor sealing material |
| CN105632660A (en) * | 2014-10-30 | 2016-06-01 | 株洲时代新材料科技股份有限公司 | High-thermal-conductivity dry mica tape and preparation method therefor |
| CN106147695A (en) * | 2016-06-29 | 2016-11-23 | 佛山市幸多新材料有限公司 | Quick cured silicone glue of one 1 to 1 double-component and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101432357A (en) * | 2006-05-01 | 2009-05-13 | 出光兴产株式会社 | Optical semiconductor sealing material |
| CN105632660A (en) * | 2014-10-30 | 2016-06-01 | 株洲时代新材料科技股份有限公司 | High-thermal-conductivity dry mica tape and preparation method therefor |
| CN106147695A (en) * | 2016-06-29 | 2016-11-23 | 佛山市幸多新材料有限公司 | Quick cured silicone glue of one 1 to 1 double-component and preparation method thereof |
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