CN111647370A - Adhesive film for bonding rubber materials and using method thereof - Google Patents
Adhesive film for bonding rubber materials and using method thereof Download PDFInfo
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- CN111647370A CN111647370A CN202010448619.4A CN202010448619A CN111647370A CN 111647370 A CN111647370 A CN 111647370A CN 202010448619 A CN202010448619 A CN 202010448619A CN 111647370 A CN111647370 A CN 111647370A
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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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
- C09J11/04—Non-macromolecular additives inorganic
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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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- 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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/21—Paper; Textile fabrics
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/144—Alcohols; Metal alcoholates
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
- D06M13/5135—Unsaturated compounds containing silicon atoms
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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
- C09J2463/00—Presence of epoxy resin
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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
- C09J2477/00—Presence of polyamide
- C09J2477/006—Presence of polyamide in the substrate
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The adhesive film for bonding the rubber material comprises a framework base material and an adhesive, wherein the adhesive is soaked into the interior and the exterior of the framework base material, the adhesive is prepared by mixing a polysiloxane modified epoxy resin body, a low molecular weight polyamide curing agent and hydrophilic white carbon black, the mass ratio of the polysiloxane modified epoxy resin body to the low molecular weight polyamide curing agent to the hydrophilic white carbon black is 100:40-55:5-7, and the mass ratio of the framework base material to the adhesive is 1: 33-37. The glue film is used for on-site manufacture or used after being refrigerated and stored after being manufactured. The adhesive film is used for bonding the nitrile rubber, the flowing of the adhesive is avoided in the bonding process, the thixotropy is good, the operation period of the adhesive coating process is prolonged, the difficulty coefficient of the adhesive coating process is reduced, the adhesive coating workload is reduced, and the adhesive coating is uniform.
Description
Technical Field
The invention relates to the field of adhesive films, in particular to an adhesive film for bonding rubber materials and a using method thereof.
Background
The heat insulating layer of the rocket motor shell and the heat insulating layer of the explosive column are both made of nitrile rubber, and the two layers of nitrile rubber are required to be bonded by the process. The prior art is that glue is coated on the heat insulation layer of the explosive column, and then the explosive column is pushed in place to bond the explosive column and the heat insulation layer of the shell. Because the used adhesive has high viscosity, poor flow and thixotropy at normal temperature, high difficulty coefficient during actual gluing, large workload and uneven gluing; the glue can be cured at normal temperature, and the operation period is short, so that a glue film needs to be manufactured for the adhesion of the nitrile rubber.
For the special environment of nitrile rubber bonding inside the shell of the rocket engine, the following requirements also exist for the adhesive film: the adhesive film and the nitrile rubber have good system adaptability, do not generate chemical reactions such as corrosion and the like with the nitrile rubber, and the material performance is insensitive to the change of the environmental temperature and humidity; the adhesive film has good adaptability and filling capability to uneven bonding surfaces; the adhesive film manufacturing time is short, the operation cycle of the manufactured adhesive film process is more than 2 hours and the curing cycle is less than 72 hours under the conditions of normal temperature (20 ℃) and normal pressure. In view of this, the technical scheme of adhesive film development is proposed, aims at solving the problems of gumming, uneven gumming, long operation period and the like.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides the adhesive film for bonding the rubber material, which has good system adaptability with the nitrile rubber, does not generate chemical reactions such as corrosion and the like with the nitrile rubber, has insensitive material performance to environmental temperature and humidity changes, and reduces the gluing difficulty in the process of bonding the nitrile rubber.
An adhesive film for bonding rubber materials comprises a framework base material and an adhesive, wherein the adhesive is soaked into the interior and the exterior of the framework base material and comprises a polysiloxane modified epoxy resin body, a low molecular weight polyamide curing agent and hydrophilic white carbon black which are mixed to prepare the adhesive film,
the mass ratio of the polysiloxane modified epoxy resin body to the low molecular weight polyamide curing agent to the hydrophilic white carbon black is 100:40-55: 5-7.
Further, the mass ratio of the polysiloxane modified epoxy resin body, the low molecular weight polyamide curing agent and the hydrophilic white carbon black is 100:45: 6.
Furthermore, the molecular structural formula of the polysiloxane modified epoxy resin body is prepared by coupling and condensing a linear organic silicon modified epoxy group and a hyperbranched epoxy group through a silane coupling agent, and is a bead chain-shaped hyperbranched macromolecular structural formula:
namely, it is
n is 20-1000, R1 is epoxyalkyl, R2 is alkyl or hyperbranched epoxy.
Specific R1 is epoxypropyl, epoxyethyl or epoxybutyl, or other epoxyalkyl.
The hyperbranched epoxy group structure is as follows:
one or a combination of more than one;
in the structural formula of the five hyperbranched epoxy groups, "o" represents an oxygen atom, the inflection point of each line segment represents a carbon atom, and the tail end of each line segment has an epoxy group, or the tail end of each line segment has two epoxy groups, or the tail end of each line segment has four epoxy groups, or the tail end of each line segment has eight epoxy groups, or the tail end of each line segment has sixteen epoxy groups.
Wherein the low molecular weight polyamide curing agent is one or more of Zhenjiang Danbao 650, stannless phoenix 650 and Shuntian polyamide epoxy curing agent 650; the hydrophilic white carbon black is one of American cabot hydrophilic gas phase white carbon black M-512 nanometer silicon dioxide, German waker white carbon black N20 hydrophilic gas phase silicon dioxide, Yuanjiang brand YJ2#, cabot CAB-O-SIL TS-530, German Gusai A380 gas phase white carbon black and Yingchu AEROSIL 200.
Further, the polysiloxane modified epoxy resin body comprises a reaction stock solution prepared from 82-90 parts by mass of linear organosilicon modified epoxy resin CRE-2501 and 10-18 parts by mass of hyperbranched epoxy resin CRE-2502, and a silane coupling agent in an amount of 0.5-2 parts by mass is added into the reaction stock solution to react to prepare the polysiloxane modified epoxy resin body. The silane coupling agent is 0.5-2 parts by mass based on 100 parts by mass of the reaction stock solution.
Further, the mass ratio of the skeleton base material to the adhesive is 1: 33-37.
Furthermore, the skeleton base material is a compressible polyamide fiber porous fabric, the aperture is 1-5mm, and the density is 1.05-1.25g/cm3The porosity is 90-97%, and the viscosity of the adhesive is 104-130 cps.
Further, the framework base material is a framework base material A or a framework base material B;
the diameter of the polyamide fiber of the framework substrate A is 350-500 mu m, and the strength is 78-85 MPa; correspondingly, the aperture of the framework substrate A, namely the polyamide fiber porous fabric, is 3-5mm, and the porosity is 90-95%;
the diameter of the polyamide fiber of the framework substrate B is 100-300 mu m, and the strength is 75-80 MPa; correspondingly, the aperture of the polyamide fiber porous fabric of the framework substrate B is 1-3mm, and the porosity is 95-97%.
Further, the apparent density of the skeleton base material B is 0.03-0.035g/cm3Compression rate of 85-88.5%, compression rebound rate of 75-82%, compression modulus14.5-15.7Mpa。
Further, the skeleton base material B is prepared by modification, and the modification method comprises the following steps:
s1, soaking the polyamide fiber porous fabric (the original skeleton base material for short) of the skeleton base material B in a closed container containing ethanol in an environment with the temperature of 20 +/-5 ℃ and the humidity of not higher than 70%, taking out the polyamide fiber porous fabric after soaking, draining, putting the polyamide fiber porous fabric in an oven, baking and taking out the polyamide fiber porous fabric;
s2, soaking the dried original skeleton substrate in a surface treating agent, taking out the original skeleton substrate after soaking, draining, placing the original skeleton substrate in an oven for baking, and taking out the original skeleton substrate to obtain a skeleton substrate B, wherein the surface treating agent is a pure water solution containing gamma-acryloyloxypropyltrimethoxysilane.
Further, in step S1, the purity of the ethanol is 95%, the time for soaking the original skeleton base material in the ethanol is 20-28h, the original skeleton base material is taken out and naturally drained for 3-8min, the baking temperature in the oven is 55-65 ℃, and the baking time is 100-140 min;
in step S2, the dried original skeleton base material is soaked in the surface treating agent for 20-28h, and is naturally drained for 3-8min after being taken out; placing the substrate in an oven at 55-65 ℃ for baking for 140min, raising the temperature to 85-95 ℃ for further baking for 200min, closing the oven, and naturally cooling the oven to room temperature to obtain the framework substrate B.
Further, in step S2, the mass fraction of gamma-acryloxypropyltrimethoxysilane in the surface treatment agent is 2.0 ± 0.05%.
Furthermore, the outer surface of the framework substrate A or the framework substrate B is coated with two pieces of release paper, and the two pieces of release paper are respectively coated on the front surface and the back surface of the outer surface of the framework substrate A or the framework substrate B.
Further, the adhesive film for bonding the rubber material is used in a field manufacturing mode or used after being refrigerated and stored after being manufactured.
The adhesive film for bonding the rubber material has the following characteristics:
1. the defects of the traditional gluing process are avoided, the nitrile rubber is bonded through the adhesive film, the glue does not flow in the bonding process, the thixotropy is good, the operation period of the gluing process is prolonged, the difficulty coefficient of the gluing process is reduced, the gluing workload is reduced, and the gluing is uniform;
2. the nitrile rubber is bonded through the adhesive film, so that the use amount of operators and adhesives is reduced, the production cost is reduced, and the adhesive film can be prepared in advance, so that the operation period in the bonding process is shortened and the production efficiency is improved compared with manual gluing and bonding;
3. the adhesive film has good system adaptability with nitrile rubber, does not generate chemical reactions such as corrosion and the like with the nitrile rubber, has good adaptability and filling capacity to uneven pasting surfaces, has good flexibility and good adaptability to thickness compression, and can meet the pasting requirements of different gaps;
4. the adhesive film has short curing time, reduces subsequent bonding time, improves the whole charging efficiency, has good aging performance, high tensile strength and peel strength of the body and excellent bonding performance;
5. the adhesive film can be used after being manufactured on site or after being refrigerated and stored after being manufactured, and the flexibility of use is good.
Detailed Description
The technical solutions in the embodiments of the present invention will be described below clearly and completely in connection with the embodiments of the present invention, and it is obvious 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 scope of the protection of the present invention.
Example 1:
an adhesive film for bonding rubber materials comprises a framework base material and an adhesive, wherein the adhesive is soaked into the interior and the exterior of the framework base material and comprises a polysiloxane modified epoxy resin body, a low molecular weight polyamide curing agent and hydrophilic white carbon black which are mixed to prepare the adhesive film,
in this example, the mass ratio of the polysiloxane modified epoxy resin body, the low molecular weight polyamide curing agent, and the hydrophilic white carbon black is 100:45: 6.
The molecular structural formula of the polysiloxane modified epoxy resin body is prepared by coupling and condensing linear organic silicon modified epoxy group CRE-2501 and hyperbranched epoxy group CRE-2502 through a silane coupling agent (vinyl trimethoxy silane) to form a bead chain hyperbranched high molecular structural formula:
namely, it is
Linear silicone-modified epoxy groups, that is, polysiloxane segments are composed of n ═ 200 linear silicone-modified epoxy groups, another example is n ═ 20, yet another example is n ═ 1000, R1 is epoxyalkyl, in this example R1 is epoxypropyl, R2 is methyl alkyl (50), a combination of three hyperbranched epoxy groups (50 each), each structure being distributed at intervals; in another embodiment, the number and structural distribution of each of the alkyl groups and hyperbranched epoxy groups are random. Compared with another embodiment, where n is 20 and yet another embodiment, where n is 1000, R2 has similar structure but different molecular weights.
The preparation method of the polysiloxane modified epoxy resin body comprises the following steps: adding 86.2 parts of linear organic silicon modified epoxy resin into a reaction kettle according to mass fraction, heating to 80 ℃, stirring for 15min, adding 13.8 parts of hyperbranched epoxy resin, continuously stirring for 20min to obtain reaction stock solution, and then reacting the reaction stock solutionAdding 0.5 part of silane coupling agent (vinyl trimethoxy silane) into the solution, stirring for 90min, naturally cooling to 50 ℃, and discharging. In particular, 0.5 parts by mass of the silane coupling agent (vinyltrimethoxysilane) was based on the mass of the reaction liquid obtained. The viscosity of the linear organosilicon modified epoxy resin is 60000cps, and the density of the linear organosilicon modified epoxy resin is 1.08g/cm3Epoxy value of 0.30mol/100g, and the product is light yellow transparent liquid; the viscosity of the hyperbranched epoxy resin is 40000cps, and the density of the hyperbranched epoxy resin is 1.00g/cm3Epoxy value of 0.62mol/100g, and is light yellow transparent liquid; the silane coupling agent (vinyltrimethoxysilane) had a density of 0.93g/cm3It is colorless transparent liquid.
After the polysiloxane modified epoxy resin body is prepared by the method, the skeleton base material is selected to prepare the adhesive film. The skeleton base material is compressible polyamide fiber porous fabric with a structure similar to steel wire ball-shaped three-dimensional fabric and a density of 1.2g/cm3The porosity is 92%, i.e. the percentage of the total volume occupied by the pores of the skeletal substrate, and the viscosity of the adhesive is 110 cps.
In this embodiment, the skeleton substrate is a skeleton substrate a, and the polyamide fiber of the skeleton substrate a has a diameter of 420um and a strength of 78 MPa; correspondingly, the aperture of the polyamide fiber porous fabric of the framework base material A is 3-5mm, the aperture is an irregular shape formed in the space range of the polyamide fiber, the mass ratio of the framework base material A to the adhesive is 1:35, and the thickness of the manufactured adhesive film is 6 mm.
The adopted low molecular weight polyamide curing agent is Zhenjiangdan 650, the hydrophilic white carbon black is American cabot hydrophilic gas phase white carbon black M-512 nanometer silicon dioxide, and the preparation process is as follows:
q1, mixing, namely stirring and mixing the polysiloxane modified epoxy resin body, the low molecular weight polyamide curing agent and the hydrophilic white carbon black according to the mass ratio of 100:45:6, wherein the stirring mode is machine stirring, and the stirring speed is 800r/min, so as to prepare the adhesive;
q2, gum dipping, namely respectively gluing adhesives on the upper surface and the lower surface of the framework substrate A, and then wrapping the framework substrate A by using release paper;
q3, glue film forming, namely placing the wrapped framework substrate into a forming tool, and compressing the framework substrate into a block shape through the forming tool to obtain the glue film.
In another embodiment, during gum dipping, an adhesive is coated on one surface of the framework substrate, the adhesive does not completely permeate the framework substrate, most of the framework substrate is in a surface dry state, and particularly, the bottom surface of the framework substrate does not have a glue solution. The thickness of the framework substrate is 6mm, the penetration thickness of the adhesive is about 2mm, and the residual adhesive liquid of the single-sided demoulding paper is more. After the double-sided adhesive is coated, the interlayer of the framework substrate is free of the adhesive, the surfaces of the upper layer and the lower layer are provided with more adhesives, the thickness of the framework substrate is 6mm, the penetration thickness of the glue solution is about 2mm, and the residual glue solution of the double-sided release paper is more. After further improvement, an adhesive is coated on the single surface of the framework substrate, the edge of the release paper is folded and then pressed, the penetration thickness of the adhesive is about 4mm, for the framework substrate with 6mm, the surface of 2mm at the bottom of the framework substrate is free of the adhesive, and the residual adhesive liquid of the release paper on the contact surface of the release paper and the adhesive is less. In conclusion, by adopting the method in the application, the glue dipping consistency of the adhesive and the framework base material is good, the glue dipping amount in the framework base material and the uniformity of the adhesive in the framework base material are ensured, the residual glue solution on the release paper is less, and the utilization rate of the adhesive is improved.
The skeleton substrate A has high strength, thick pore diameter of the material, rough surface, poor flexibility, compressibility, small pore space and difficult gum dipping. After the glue film is manufactured, the glue film is not easy to bend and difficult to compress and cannot be well adhered to an adaptive arc-shaped surface, the outside of the manufactured glue film is coated with demolding paper, glue overflow in compression molding can be prevented, meanwhile, the glue film is convenient to transport, the glue film can be directly conveyed to an adhering site after the manufacturing is completed, one demolding paper is firstly torn off during adhering, then the glue film is aligned with the vertical edge of the medicine block to be adhered, and then the glue film is uniformly rolled and adhered to the molded surface of the medicine block along the surface of the medicine block by using a cylindrical hollow rod. After the adhesive film is completely paved, the adhesive film is repeatedly pasted with a round bar for three times, so that the adhesive film is firmly pasted with the nitrile rubber outside the molded surface of the medicine block. And tearing off the other surface of the demoulding paper along the surface of the glue film, bonding the nitrile rubber with the other surface, and driving three rows of 14 studs in a broken line shape in the upper half area of the glue film in order to prevent the glue film from sliding down under the action of gravity, wherein the driving depth is about 8 mm. In another embodiment, the prepared adhesive film is stored in a cold storage mode for two days at the temperature of minus 14 ℃, and then the adhesive film is conveyed to a pasting site, so that a good bonding effect can be achieved.
The adhesive film is adopted for pasting, and compared with the traditional manual gluing pasting, the advantages are as shown in the following table 1:
TABLE 1
| Pasting mode | Cycle of pasting operation | Gummosis | Amount of glue used | Glue overflow amount | Operator personnel | Preparation in advance |
| Manual gluing and sticking | Long and long | Severe gummosis | Big (a) | Big (a) | Multiple purpose | Whether or not |
| Glue film paste | Short length | Glue does not flow | Small | Small | 3 persons | Can store |
Example 2:
an adhesive film for bonding rubber materials comprises a framework base material and an adhesive, wherein the adhesive is soaked into the interior and the exterior of the framework base material and comprises a polysiloxane modified epoxy resin body, a low molecular weight polyamide curing agent and hydrophilic white carbon black which are mixed to prepare the adhesive film,
in this example, the ratio of the polysiloxane-modified epoxy resin body, the low molecular weight polyamide curing agent, and the hydrophilic white carbon black is 100:55:7 by mass.
The molecular structural formula of the polysiloxane modified epoxy resin body is prepared by coupling and condensing linear organic silicon modified epoxy group CRE-2501 and hyperbranched epoxy group CRE-2502 through a silane coupling agent (vinyl trimethoxy silane) to form a bead chain hyperbranched high molecular structural formula:
namely, it is
Linear silicone-modified epoxy groups, that is, a polysiloxane segment is composed of n ═ 500 linear silicone-modified epoxy groups, R1 is an epoxyalkyl group, in this example, R1 is an epoxypropyl group, R2 is an ethyl group (100), a combination of four hyperbranched epoxy groups (100 each), each structure being distributed at intervals; in another embodiment, the number and structural distribution of each of the alkyl groups and hyperbranched epoxy groups are random.
The mass ratio of the skeleton base material to the adhesive is 1: 37.
The skeleton base material is a compressible polyamide fiber porous fabric with the aperture of 1-5mm and the density of 1.15g/cm3The porosity is 90% -97%, and the viscosity of the adhesive is 126 cps.
The framework base material is a framework base material B; the diameter of the polyamide fiber of the framework substrate B is 100-300 mu m, and the strength is 75-80 MPa; correspondingly, the pore diameter of the polyamide fiber porous fabric of the framework substrate B is 1-3mm, and the porosity is 95%.
The apparent density of the skeleton base material B is 0.033g/cm3The compression ratio was 87%, the compression rebound ratio was 77%, and the compression modulus was 14.5 MPa.
The skeleton base material B is prepared by modification, in this example, the size of the skeleton base material B is 1200mm × 1500mm × 6mm, and the modification method includes the following steps:
s1, soaking the polyamide fiber porous fabric of the framework substrate B, namely the original framework substrate, in a closed container containing ethanol at the temperature of 20 +/-5 ℃ and the humidity of not higher than 70%, taking out the fabric after soaking, draining, putting the fabric in an oven, baking and taking out the fabric;
s2, soaking the dried original skeleton substrate in a surface treating agent, taking out the original skeleton substrate after soaking, draining, placing the original skeleton substrate in an oven for baking, and taking out the original skeleton substrate to obtain a skeleton substrate B, wherein the surface treating agent is a pure water solution containing gamma-acryloyloxypropyltrimethoxysilane.
In the step S1, the purity of 8Kg of ethanol is 95%, the time for soaking the original skeleton base material in the ethanol is 24h, the original skeleton base material is taken out and naturally drained for 5min, the baking temperature in an oven is 60 ℃, and the baking time is 120 min;
in step S2, the dried original skeleton base material is soaked in the surface treating agent for 24h, and is naturally drained for 5min after being taken out; and (3) placing the substrate in a 60 ℃ oven for baking for 120min, raising the temperature to 90 ℃, continuing baking for 180min, closing the oven, and naturally cooling the oven to room temperature to obtain the framework substrate B.
In step S2, the mass fraction of gamma-acryloyloxypropyltrimethoxysilane in the surface treatment agent is 2.0 ± 0.05%.
Compared with the skeleton base material A, the skeleton base material B modified by the method has the advantages of equivalent strength, thinner material aperture of the skeleton, smooth surface, good flexibility, easier compression, larger pore space, easy gum dipping and higher gum absorption amount. The preparation method of the adhesive film comprises the following steps:
q1, mixing, namely stirring and mixing the polysiloxane modified epoxy resin body, the low molecular weight polyamide curing agent and the hydrophilic white carbon black according to the mass ratio of 100:55:7, wherein the stirring mode is machine stirring, and the stirring rotating speed is 800r/min, so as to obtain the adhesive;
q2, gum dipping, namely respectively gluing adhesives on the upper surface and the lower surface of the framework substrate B, and then wrapping the framework substrate B by using release paper;
q3, forming an adhesive film, namely placing the wrapped framework substrate B into a forming tool, and compressing the framework substrate B into a block shape through the forming tool to obtain the adhesive film.
Glue film forming tool comprises fixed plate subassembly, movable plate subassembly, cylinder. When the mold is used, the adhesive film on the side of the demolding paper is placed on the fixing plate, the adhesive film is flat and upward, the edge of the demolding paper is folded downward, and the center of the demolding paper is symmetrically placed. After the standard placement, the fixed plate resets, the movable plate moves downwards, pressure is applied, the compression force is 7850N, the compression distance is 1mm, and the compression time is 5 minutes.
The relevant test data of the adhesive films made of the framework base materials A and B are shown in the following table:
TABLE 2 comparison of tensile Strength test of adhesive films made from skeleton substrates A and B
TABLE 3 comparison of peel strength test for adhesive films made of skeleton substrates A and B
TABLE 4 comparison of tear Strength test of adhesive films made from skeleton substrates A and B
Through tests on tensile strength, tearing strength and peeling strength, the adhesive film strength of the framework base material B is obviously improved compared with that of an adhesive film made of the framework base material A. After the adhesive film is prepared, the adhesive and the framework base material B are integrated, so that the interaction force is stronger, the flexibility of the adhesive film is better, the adhesive film is easier to compress, and the adhesive film can be well suitable for the arc-shaped surface to be adhered.
Example 3:
an adhesive film for bonding rubber materials comprises a framework base material and an adhesive, wherein the adhesive is soaked into the interior and the exterior of the framework base material and comprises a polysiloxane modified epoxy resin body, a low molecular weight polyamide curing agent and hydrophilic white carbon black which are mixed to prepare the adhesive film,
in this example, the mass ratio of the polysiloxane modified epoxy resin body, the low molecular weight polyamide curing agent, and the hydrophilic white carbon black is 100:40: 5.
The molecular structural formula of the polysiloxane modified epoxy resin body is prepared into a bead chain hyperbranched high molecular structural formula by coupling and condensing linear organosilicon modified epoxy group CRE-2501 and hyperbranched epoxy group CRE-2502 through a silane coupling agent, wherein a polysiloxane chain segment consists of n 730 linear organosilicon modified epoxy groups, R1 is epoxyalkyl, in the embodiment, R1 is epoxybutyl, R2 is alkyl or hyperbranched epoxy group,
namely, it is
The epoxy groups are linear organosilicon modified epoxy groups, namely a polysiloxane chain segment is composed of n-730 linear organosilicon modified epoxy groups, R1 is an epoxy group, in the embodiment, R1 is propylene oxide, R2 is methyl alkyl (180), and a combination of five hyperbranched epoxy groups (110 in each), and each structure is distributed at intervals; in another embodiment, the number and structural distribution of each of the alkyl groups and hyperbranched epoxy groups are random.
The mass ratio of the skeleton base material to the adhesive is 1: 34.
The skeleton base material is a compressible polyamide fiber porous fabric with the aperture of 1-5mm and the density of 1.20g/cm3The porosity is 90% -97%, and the viscosity of the adhesive is 110 cps.
The framework base material is a framework base material B; the polyamide fiber of the framework substrate B has the diameter of 220um and the strength of 78 MPa; correspondingly, the polyamide fiber porous fabric of the framework substrate B has the pore diameter of 1-3mm and the porosity of 94%.
The apparent density of the skeleton base material B is 0.033g/cm3The compression ratio was 87%, the compression rebound ratio was 80%, and the compression modulus was 15.2 MPa.
The skeleton base material B is prepared by modification, in this example, the size of the skeleton base material B is 300mm × 6mm, and the modification method includes the following steps:
s1, soaking the polyamide fiber porous fabric of the framework substrate B, namely the original framework substrate, in a closed container containing ethanol at the temperature of 20 +/-5 ℃ and the humidity of not higher than 70%, taking out the fabric after soaking, draining, putting the fabric in an oven, baking and taking out the fabric;
s2, soaking the dried original skeleton substrate in a surface treating agent, taking out the original skeleton substrate after soaking, draining, placing the original skeleton substrate in an oven for baking, and taking out the original skeleton substrate to obtain a skeleton substrate B, wherein the surface treating agent is a pure water solution containing gamma-acryloyloxypropyltrimethoxysilane.
In the step S1, the purity of the ethanol is 95%, the time for soaking the original skeleton base material in the ethanol is 20 hours, the original skeleton base material is taken out and naturally drained for 4 minutes, the baking temperature in an oven is 55 ℃, and the baking time is 105 minutes;
in step S2, the dried original skeleton base material is soaked in the surface treating agent for 22h, and is taken out and naturally drained for 4 min; and (3) placing the substrate in an oven at 55 ℃ for baking for 110min, raising the temperature to 85 ℃, continuing baking for 170min, closing the oven, and naturally cooling the oven to room temperature to obtain the framework substrate B.
In another embodiment, in step S1, the ethanol has a mass of 8Kg and a purity of 95%, the original skeleton substrate is soaked in the ethanol for 27 hours, and is taken out and naturally drained for 7 minutes, the baking temperature in the oven is 63 ℃, and the baking time is 130 minutes; in step S2, soaking the dried original skeleton base material in the surface treating agent for 28h, taking out and naturally draining for 8 min; and (3) placing the substrate in an oven at 60 ℃ for baking for 180min, raising the temperature to 92 ℃, continuing baking for 190min, closing the oven, and naturally cooling the oven to room temperature to obtain the framework substrate B.
In step S2, the mass fraction of gamma-acryloyloxypropyltrimethoxysilane in the surface treatment agent is 2.0 ± 0.05%.
Compared with the skeleton base material A, the skeleton base material B modified by the method has the advantages of equivalent strength, thinner material aperture of the skeleton, smooth surface, good flexibility, easier compression, larger pore space, easy gum dipping and higher gum absorption amount. The preparation method of the adhesive film comprises the following steps:
q1, mixing the adhesive, namely stirring and mixing the polysiloxane modified epoxy resin body, the low molecular weight polyamide curing agent and the hydrophilic white carbon black in a mass ratio of 100:40:5 in a machine stirring manner by adopting a star-shaped stirring wheel at a stirring speed of 850r/min to prepare the adhesive;
q2, gum dipping, namely respectively gluing adhesives on the upper surface and the lower surface of the framework substrate B, and then wrapping the framework substrate B by using release paper;
q3, forming an adhesive film, namely placing the wrapped framework substrate B into a forming tool, and compressing the framework substrate B into a block shape through the forming tool to obtain the adhesive film.
The prepared adhesive film is used as it is or after being frozen for storage, and the specific conditions are as follows:
TABLE 5 film parameters for production
For the ready-to-use adhesive film, 335kg was directly loaded after three days of curing, and debonding occurred for 66 hours.
TABLE 6 refrigeration storage of film parameters
And for the adhesive film refrigerated at the temperature of-14 ℃ for 2 days, after the adhesive film is solidified for three days, 180kg is loaded, the adhesive film is not debonded and is continuously loaded for three days, 140kg is continuously loaded, the adhesive film is not debonded and is continuously loaded for one day, 120kg is continuously loaded, and debonding occurs after 8 hours, so that the adhesive film refrigerated is better in service performance.
Claims (10)
1. An adhesive film for bonding rubber materials is characterized by comprising a framework base material and an adhesive, wherein the adhesive is soaked into the interior and the exterior of the framework base material and comprises a polysiloxane modified epoxy resin body, a low molecular weight polyamide curing agent and hydrophilic white carbon black which are mixed to prepare the adhesive film,
the mass ratio of the polysiloxane modified epoxy resin body to the low molecular weight polyamide curing agent to the hydrophilic white carbon black is 100:40-55: 5-7.
2. The adhesive film for bonding rubber materials according to claim 1, wherein the mass ratio of the skeleton base material to the adhesive is 1: 33-37.
3. The adhesive film according to claim 1 or 2, wherein the skeleton base material is a compressible polyamide fiber porous fabric with a pore size of 1-5mm and a density of 1.05-1.25g/cm3The porosity is 90-97%, and the viscosity of the adhesive is 104-130 cps.
4. The adhesive film for bonding rubber materials according to claim 3, wherein the skeleton base material is a skeleton base material A or a skeleton base material B;
the diameter of the polyamide fiber of the framework substrate A is 350-500 mu m, and the strength is 78-85 MPa; correspondingly, the aperture of the framework substrate A, namely the polyamide fiber porous fabric, is 3-5mm, and the porosity is 90-95%;
the diameter of the polyamide fiber of the framework substrate B is 100-300 mu m, and the strength is 75-80 MPa; correspondingly, the pore diameter of the polyamide fiber porous fabric of the framework substrate B is 1-3mm, and the porosity is 95-97%.
5. The adhesive film for bonding rubber materials as claimed in claim 4, wherein the skeleton base material B has an apparent density of 0.03-0.035g/cm3The compression rate is 85-88.5%, the compression rebound rate is 75-82%, and the compression modulus is 14.5-15.7 MPa.
6. The adhesive film for bonding rubber materials according to claim 5, wherein the skeleton base material B is prepared by modification, and the modification method comprises the following steps:
s1, soaking the polyamide fiber porous fabric of the framework substrate B, namely the original framework substrate, in a closed container containing ethanol at the temperature of 20 +/-5 ℃ and the humidity of not higher than 70%, taking out the fabric after soaking, draining, putting the fabric in an oven, baking and taking out the fabric;
s2, soaking the dried original skeleton substrate in a surface treating agent, taking out the original skeleton substrate after soaking, draining, placing the original skeleton substrate in an oven for baking, and taking out the original skeleton substrate to obtain a skeleton substrate B, wherein the surface treating agent is a pure water solution containing gamma-acryloyloxypropyltrimethoxysilane.
7. The adhesive film for bonding rubber materials as claimed in claim 6, wherein in step S1, the ethanol has a purity of 95%, the original skeleton is soaked in ethanol for 20-28h, and then naturally drained for 3-8min, the baking temperature in the oven is 55-65 ℃ and the baking time is 100-140 min;
in step S2, the dried original skeleton base material is soaked in the surface treating agent for 20-28h, and is naturally drained for 3-8min after being taken out; placing the substrate in an oven at 55-65 ℃ for baking for 140min, raising the temperature to 85-95 ℃ for further baking for 200min, closing the oven, and naturally cooling the oven to room temperature to obtain the framework substrate B.
8. The adhesive film for bonding rubber materials according to claim 7, wherein in step S2, the mass fraction of gamma-acryloxypropyltrimethoxysilane in the surface treatment agent is 2.0 ± 0.05%.
9. The adhesive film for bonding rubber materials according to any one of claims 1 to 2 and 4 to 5, wherein the outer surface of the framework substrate A or B is coated with two pieces of release paper, and the two pieces of release paper are respectively coated on the front surface and the back surface of the outer surface of the framework substrate A or B.
10. The use method of the adhesive film according to claims 1-9, wherein the adhesive film is used in situ or after being refrigerated and stored.
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| CN1670109A (en) * | 2005-05-11 | 2005-09-21 | 李洁华 | Modified epoxy resin adhesive and its preparation process |
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| CN109181607A (en) * | 2018-11-23 | 2019-01-11 | 深圳市欧科力科技有限公司 | A kind of construction material epoxy adhesive and preparation method thereof |
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| CN1670109A (en) * | 2005-05-11 | 2005-09-21 | 李洁华 | Modified epoxy resin adhesive and its preparation process |
| CN101475731A (en) * | 2009-01-06 | 2009-07-08 | 中国科学院广州化学研究所 | Epoxy resin composite material added with modified polysiloxane and preparation thereof |
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