CN113698888B - High-temperature-resistant high-molecular industrial adhesive tape and preparation process thereof - Google Patents
High-temperature-resistant high-molecular industrial adhesive tape and preparation process thereof Download PDFInfo
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- CN113698888B CN113698888B CN202111126520.3A CN202111126520A CN113698888B CN 113698888 B CN113698888 B CN 113698888B CN 202111126520 A CN202111126520 A CN 202111126520A CN 113698888 B CN113698888 B CN 113698888B
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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
- C09J7/29—Laminated material
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
- C08G73/1071—Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
- 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
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- 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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- 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
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
- C09J7/403—Adhesives in the form of films or foils characterised by release liners characterised by the structure of the release feature
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/124—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present on both sides of the carrier, e.g. double-sided adhesive tape
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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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/41—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the carrier layer
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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
- C09J2479/00—Presence of polyamine or polyimide
- C09J2479/08—Presence of polyamine or polyimide polyimide
- C09J2479/086—Presence of polyamine or polyimide polyimide in the substrate
Abstract
A high-temperature-resistant high-molecular industrial adhesive tape and a preparation process thereof are provided, wherein the adhesive tape comprises a base material and a silica gel layer; the base material is prepared by adopting a composite polyimide film, the silica gel layer is prepared by coating silica gel on two sides of the base material, and the outer surface of the silica gel layer is covered with a release film; the composite polyimide film is formed by compounding a modified polyimide film, a pure polyimide film and a modified polyimide film from top to bottom; the modified polyimide film is prepared by preparing a polyamic acid solution from modified nano titanium dioxide and m-phenylenediamine, 4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride through in-situ polymerization, and then carrying out thermal imidization on the polyamic acid solution. The high-temperature-resistant high-molecular industrial adhesive tape and the preparation process thereof adopt the composite polyimide film as a base material, the silica gel is coated on the two sides, the release film is coated on the outer surface of the silica gel layer, and the formulation design of each component is reasonable, so that the adhesive tape has high-temperature resistance, improved hydrophobicity, simple preparation process and wide application prospect.
Description
Technical Field
The invention belongs to the technical field of adhesive tapes, and particularly relates to a high-temperature-resistant high-molecular industrial adhesive tape and a preparation process thereof.
Background
The adhesive tape consists of two parts of base material and adhesive, and has one adhesive layer coated on the surface to connect two or more unconnected objects together. The earliest adhesives were of animal and vegetable origin, rubber being the major component of adhesives in the nineteenth century, and various polymers have been widely used in modern times. The adhesive can adhere things because of the bonding between the molecules and the molecules of the articles to be connected, and the bonding can firmly adhere the molecules together.
The adhesive tape can be divided into: high temperature adhesive tape, double sided adhesive tape, insulating tape, special adhesive tape, pressure sensitive adhesive tape, die cut adhesive tape, different effects are suitable for different industry demands. The adhesive tape used in the high-temperature working environment is mainly used for electronic industry, and the temperature resistance is usually between 120 and 260 ℃ and is commonly used for paint spraying, baking paint leather processing, coating shielding and fixing in the electronic part manufacturing process, printed circuit board and high-temperature treatment shielding. In order to further improve the high temperature resistance of the adhesive tape, a high temperature resistant high molecular industrial adhesive tape and a preparation process thereof are required to be developed.
Disclosure of Invention
The invention aims to: in order to overcome the defects, the invention aims to provide the high-temperature-resistant high-molecular industrial adhesive tape and the preparation process thereof, and the adhesive tape is reasonable in structural design, takes a composite polyimide film as a base material, coats silica gel on two sides, coats a release film on the outer surface of the silica gel layer, protects the silica gel layer from pollution, and is reasonable in formula design, so that the adhesive tape has high-temperature resistance, improved in hydrophobicity, simple in preparation process and wide in application prospect.
The invention aims at realizing the following technical scheme:
a high-temperature-resistant high-molecular industrial adhesive tape, which comprises a base material and a silica gel layer; the base material is prepared by adopting a composite polyimide film, the silica gel layer is prepared by coating silica gel on two sides of the base material, and the outer surface of the silica gel layer is covered with a release film; the composite polyimide film is formed by compounding a modified polyimide film, a pure polyimide film and a modified polyimide film from top to bottom; the modified polyimide film is prepared by preparing polyamide acid solution from modified nano titanium dioxide and m-phenylenediamine, 4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride through in-situ polymerization, and then thermally imidizing the polyamide acid solution; wherein the molar ratio of the m-phenylenediamine to the 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride is 1:1.02, and the addition amount of the modified nano titanium dioxide is 5-7% of the total weight of the m-phenylenediamine and the 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride; the silica gel mainly comprises the following components in parts by weight: 40-50 parts of polymethyl silane, 40-50 parts of tetramethyl tetravinyl cyclotetrasiloxane, 30-40 parts of boron carbide powder, 15-20 parts of glass powder and 10-15 parts of nano silicon dioxide; the release film comprises a substrate and a release layer attached to the surface of the substrate, wherein the release layer is a thin layer formed by a surfactant, and the release layer in the release film is in contact with the silica gel layer.
The high-temperature high-molecular industrial adhesive tape has reasonable structural design, takes the composite polyimide film as a base material, coats silica gel on two sides, coats a release film on the outer surface of the silica gel layer, and protects the silica gel layer from pollution.
The modified polyimide film is prepared by taking m-phenylenediamine and 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride as monomers, adding modified nano titanium dioxide and adopting an in-situ polymerization method, wherein the bond energy of Ti-O bond of the modified nano titanium dioxide is extremely high, the thermal performance of polyimide can be remarkably improved, the thermal stability of the modified polyimide film is greatly improved by detecting the modified polyimide film through methods of thermal loss, differential scanning calorimeter and the like, the glass transition temperature is improved to a certain extent by adding the modified nano titanium dioxide, the thermal loss temperature at 5% can be improved by 45 ℃ compared with that of the pure polyimide film at the highest, the thermal loss temperature at 10% can be improved by 32 ℃ compared with that of the pure polyimide film at the highest, and the decomposition temperature at the maximum decomposition rate is improved by 14 ℃. In addition, the pure polyimide film has poor hydrophobicity due to the existence of hydrophilic groups in the molecular structure, the contact angle is 55.23 degrees, the water absorption rate is 3.56 percent, the modified nano titanium dioxide is added to improve the hydrophobicity of the modified polyimide film, the contact angle of the modified polyimide film can be improved by 92.12 degrees at most, and the water absorption rate is reduced to 1.65 percent at most.
Because the modified nano titanium dioxide is added, the mechanical property of the modified polyimide film is slightly lower than that of the pure polyimide film, the modified polyimide film, the pure polyimide film and the modified polyimide film are compounded into the composite polyimide film, the composite polyimide film has a three-layer structure, the mechanical property of the composite polyimide film is better than that of the modified polyimide film, the composite polyimide film is basically the same as that of the pure polyimide film, the thermal stability and the glass transition temperature of the composite polyimide film are higher than those of the single-layer modified polyimide film, the thermal weight loss temperature of the composite polyimide film at 5% can be improved by 5 ℃ at the maximum than that of the modified polyimide film, the thermal weight loss temperature at 10% can be improved by 3 ℃ at the maximum than that of the pure polyimide film, and the decomposition temperature at the maximum decomposition rate is improved by 3 ℃. The contact angle of the composite polyimide film can be increased by 93.23 degrees at most, and the water absorption is reduced to 1.46 percent at most.
The silica gel is prepared from polymethyl silane and tetramethyl tetravinyl cyclotetrasiloxane serving as raw materials, boron carbide powder, glass powder and nano silicon dioxide serving as fillers, and is rich in Si-H and CH=CH2 active groups and has high temperature resistance and bonding performance. Under the high temperature condition, the melt of the boron carbide powder has excellent melt flow property, crack holes generated by high temperature of the silica gel layer can be effectively repaired, so that the silica gel layer keeps high compactness, the interface bonding strength of the silica gel layer and a base material can be improved by the boron carbide powder and the glass powder, the high temperature bonding property of the adhesive tape is enhanced, nano silicon dioxide can react to form borosilicate glass, and the high temperature property of the silica gel layer is further improved.
Further, in the high-temperature-resistant high-molecular industrial adhesive tape, the thickness of the base material is 0.021mm, and the thicknesses of the modified polyimide film and the pure polyimide film are both 0.007 and mm; the thickness of the silica gel layer is 0.03 and mm, and the thickness of the release film is 0.012 and mm.
Further, the high-temperature-resistant high-molecular industrial adhesive tape is characterized in that the surfactant is an anionic surfactant or a nonionic surfactant or is obtained by compounding the anionic surfactant with the nonionic surfactant; the HLB value of the surfactant is 10-20.
The substrate may be a film-like resin substrate, or a film having a grid shape or special stripes on the surface, such as an acrylic resin film, a phenol resin film, an epoxy resin film, a polycarbonate resin film, a polybutylene terephthalate resin film, a polyester resin film, and a polyethylene film. The anionic surfactant may be sodium stearate, sodium dodecylbenzenesulfonate, sodium oleoyloxyethane sulfonate, succinic acid diester sulfonate, sodium dibutylnaphthalene sulfonate, sodium p-methoxyfatty amidobenzenesulfonate, sodium lauryl sulfate, fatty alcohol polyoxyethylene ether sulfate, oleyl sulfate, didecyl phosphate diester salt, alkyl alcohol polyoxyethylene ether phosphate, sodium dodecylsulfate, sodium oleate, potassium oleate, etc., and the nonionic surfactant may be diethylene glycol monolaurate, octylphenol polyoxyethylene ether, nonylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ester, castor oil polyoxyethylene ether, sorbitan fatty acid ester, polyoxyethylene monooleate, triethanolamine oleic soap, polyoxyethylene sorbitan fatty acid ester, etc.
The invention also relates to a preparation process of the high-temperature-resistant high-molecular industrial adhesive tape, which comprises the following steps of:
(1) The polymethyl silane and tetramethyl tetravinyl cyclotetrasiloxane are put into a reactor, the reaction temperature is set at 100-110 ℃, and the reaction is carried out for 2-3 hours under the protection of inert atmosphere, so as to obtain a liquid precursor; adding boron carbide powder, glass powder and nano silicon dioxide into the liquid precursor, and stirring the mixture to be uniform by a stirrer to obtain silica gel;
(2) Coating a surface active agent on the surface of a substrate to form a release layer, and drying to remove a solvent to form the release layer to obtain a release film; and (3) coating silica gel on two sides of the composite polyimide film by a coating machine, standing for 10-20min, placing between 2 release films, enabling the release layers to be in contact with the silica gel, rolling and compounding, placing into an oven, heating at a speed of 5 ℃/min, solidifying for 0.5-1h at a temperature of 80-100 ℃ to enable the release films, the silica gel and the composite polyimide film to be completely solidified, preserving heat for 10-20min, and naturally cooling to room temperature to obtain the adhesive tape.
Further, the preparation process of the high-temperature-resistant high-molecular industrial adhesive tape comprises the following steps of:
(1) Dissolving the modified nano titanium dioxide in DMF solvent, and performing ultrasonic dispersion for 1-2h under water bath;
(2) Adding m-phenylenediamine, stirring, adding 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride in a small quantity mode for multiple times after the m-phenylenediamine is completely dissolved, and continuously stirring for 3-4 hours to obtain a reaction liquid I;
(3) Dispersing the reaction liquid I in water bath for 20-30min, placing the reaction liquid I in a vacuum drying oven, vacuumizing the reaction liquid I to remove bubbles in the reaction liquid I, and then scraping a film on a uniform dust-free clean glass plate of the reaction liquid I at a uniform speed from bottom to top through a film scraping machine, wherein the height of a push rod of the film scraping machine is 0.007 mm;
(4) Placing the scraped film in a vacuum drying oven for solidification, vacuumizing and preserving heat at 80 ℃ for 1.0-2.0 h to obtain a first layer of modified polyimide film; pouring a second reaction solution on the basis of the modified polyimide film of the first layer, scraping the film at a constant speed from bottom to top by a film scraping machine, wherein the height of a push rod of the film scraping machine is 0.007 and mm, then placing the film in a vacuum drying oven for solidification, vacuumizing and preserving heat at 80 ℃ for 1.0-2.0 h to obtain a pure polyimide film of the second layer; pouring a first reaction solution on the basis of a pure polyimide film of the second layer, scraping a film at a constant speed from bottom to top by a film scraping machine, wherein the height of a push rod of the film scraping machine is 0.007 mm, and then placing the film in a vacuum drying oven for thermal imidization to obtain a modified polyimide film of a third layer;
(5) And after the thermal imidization process is finished, naturally cooling, taking out the glass plate, placing the glass plate in cold water, and waiting for the composite polyimide film attached to the glass plate to naturally fall off, thus obtaining the composite polyimide film.
Further, the preparation process of the high-temperature-resistant high-molecular industrial adhesive tape comprises the following steps of: the initial temperature of the vacuum drying oven is set to 80 ℃, the interior of the vacuum drying oven is continuously vacuumized, then the temperature is raised to 120 ℃, the temperature is raised to 45 ℃ each time from 120 ℃, and each temperature gradient is kept for 0.5h, and the whole process lasts for 4-5h; taking out the cooled glass plate, transferring the cooled glass plate into a blast drying box, preserving heat for 50min from 250 ℃, and raising the temperature to 280 ℃ and preserving heat for 30min.
Further, the preparation process of the high-temperature-resistant high-molecular industrial adhesive tape, the preparation of the second reaction liquid, comprises the following steps: adding m-phenylenediamine into DMF solvent, continuously bubbling N2 into the solution for 10min, stirring until the m-phenylenediamine is completely dissolved under the protection of N2, adding 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride in a small quantity mode for multiple times, stirring until the 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride is completely dissolved, and stirring for 4-5h at room temperature to obtain reaction liquid II; and (3) carrying out ultrasonic dispersion on the first reaction liquid for 20-30min in a water bath, putting the first reaction liquid into a vacuum drying box, and vacuumizing the second reaction liquid to remove bubbles in the reaction liquid.
Further, in the preparation process of the high-temperature-resistant high-molecular industrial adhesive tape, the preparation of the modified nano titanium dioxide comprises the following steps: dispersing nano titanium dioxide particles in distilled water for 1-2 hours, freezing the nano titanium dioxide particles dispersed in the distilled water into ice, transferring the ice into a freeze dryer for continuous 20-36 hours for freeze drying, and then placing the ice into a drying tower for standby; putting the nano titanium dioxide particles into an oven, and preserving heat for 1-2h at 100 ℃; adding KH570 silane coupling agent into absolute ethanol solvent, stirring uniformly, adding the nano titanium dioxide particles, performing ultrasonic treatment in water bath at 40-50 ℃, condensing and refluxing, and continuously stirring for reaction for 4 hours to obtain a reaction solution III; and centrifuging the reaction liquid by a centrifugal machine, separating the modified nano titanium dioxide from the liquid, cleaning the modified nano titanium dioxide by using absolute ethyl alcohol for multiple times, and air-drying to obtain the modified nano titanium dioxide.
The nano titanium dioxide particles are easy to agglomerate due to the self structural characteristics, and through the treatment, the agglomeration effect of the nano titanium dioxide particles can be reduced, and the dispersion effect of the nano titanium dioxide particles in a polyimide matrix can be improved.
Compared with the prior art, the invention has the following beneficial effects:
(1) The high-temperature-resistant high-molecular industrial adhesive tape disclosed by the invention has reasonable structural design, is prepared by taking a composite polyimide film as a base material, coating silica gel on two sides, and coating a release film on the outer surface of the silica gel layer to protect the silica gel layer and prevent pollution; wherein, the thermal stability and the glass transition temperature of the composite polyimide film are higher than those of a single-layer modified polyimide film, the hydrophobicity is better than that of the modified polyimide film, and the composite polyimide film is basically the same as that of a pure polyimide film; the modified polyimide film is prepared by taking m-phenylenediamine and 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride as monomers and adding modified nano titanium dioxide through an in-situ polymerization method, and the heat performance of polyimide can be obviously improved due to extremely high bond energy of Ti-O bond of the modified nano titanium dioxide, and the hydrophobicity of the modified polyimide film is improved due to the addition of the modified nano titanium dioxide; the silica gel is prepared by taking polymethyl silane and tetramethyl tetravinyl cyclotetrasiloxane as raw materials and boron carbide powder, glass powder and nano silicon dioxide as fillers, and is rich in Si-H and CH=CH2 active groups and has high temperature resistance and bonding performance;
(2) The high-temperature-resistant high-molecular industrial adhesive tape and the preparation process thereof provided by the invention are simple in preparation process, high in flexibility and wide in application prospect.
Detailed Description
In the following, examples 1-5 are described in detail in connection with experimental data, and it is apparent that the embodiments described are only some, but not all, examples of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
The following examples provide a high temperature resistant polymeric industrial tape comprising a substrate, a layer of silica gel; the base material is prepared by adopting a composite polyimide film, the silica gel layer is prepared by coating silica gel on two sides of the base material, and the outer surface of the silica gel layer is covered with a release film; the composite polyimide film is formed by compounding a modified polyimide film, a pure polyimide film and a modified polyimide film from top to bottom; the modified polyimide film is prepared by preparing polyamide acid solution from modified nano titanium dioxide and m-phenylenediamine, 4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride through in-situ polymerization, and then thermally imidizing the polyamide acid solution; wherein the molar ratio of the m-phenylenediamine to the 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride is 1:1.02, and the addition amount of the modified nano titanium dioxide is 5-7% of the total weight of the m-phenylenediamine and the 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride; the silica gel mainly comprises the following components in parts by weight: 40-50 parts of polymethyl silane, 40-50 parts of tetramethyl tetravinyl cyclotetrasiloxane, 30-40 parts of boron carbide powder, 15-20 parts of glass powder and 10-15 parts of nano silicon dioxide; the release film comprises a substrate and a release layer attached to the surface of the substrate, wherein the release layer is a thin layer formed by a surfactant, and the release layer in the release film is in contact with the silica gel layer.
Further, the thickness of the base material is 0.021mm, and the thickness of the modified polyimide film and the pure polyimide film are both 0.007 and mm; the thickness of the silica gel layer is 0.03 and mm, and the thickness of the release film is 0.012 and mm.
Further, the surfactant is an anionic surfactant or a nonionic surfactant, or is obtained by compounding the anionic surfactant and the nonionic surfactant; the HLB value of the surfactant is 10-20.
Example 1
The preparation of the single-layer modified polyimide film comprises the following steps:
(1) The molar ratio of the m-phenylenediamine to the 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride is 1:1.02, the addition amount of the modified nano titanium dioxide is 6 percent of the total weight of the m-phenylenediamine and the 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride, the modified nano titanium dioxide is dissolved in DMF solvent, and the modified nano titanium dioxide is dispersed for 2 hours in water bath in an ultrasonic way;
(2) Adding m-phenylenediamine, stirring, adding 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride in a small quantity mode for multiple times after the m-phenylenediamine is completely dissolved, and continuously stirring for 4 hours to obtain a reaction solution I;
(3) Dispersing the reaction liquid in water bath for 30min, placing the reaction liquid in a vacuum drying oven, vacuumizing the reaction liquid to remove bubbles in the reaction liquid, and then scraping the reaction liquid on a uniform dust-free clean glass plate at a uniform speed from bottom to top through a film scraping machine, wherein the height of a push rod of the film scraping machine is 0.021 mm;
(4) Placing the mixture in a vacuum drying oven for thermal imidization, setting the initial temperature of the vacuum drying oven to 80 ℃, continuously vacuumizing the interior of the vacuum drying oven, then heating to 120 ℃, starting from 120 ℃, heating to 45 ℃ each time, and preserving heat for 0.5h by each temperature gradient, wherein the whole process lasts for 4.5h; taking out the cooled glass plate, transferring the cooled glass plate into a blast drying oven, preserving heat for 50min from 250 ℃, and preserving heat for 30min from 280 ℃;
(5) And after the thermal imidization process is finished, naturally cooling, taking out the glass plate, placing the glass plate in cold water, and waiting for the modified polyimide film attached to the glass plate to naturally fall off, thus obtaining the single-layer modified polyimide film.
Wherein, the preparation of the modified nano titanium dioxide comprises the following steps: dispersing nano titanium dioxide particles in distilled water for 1.5 hours, freezing the nano titanium dioxide particles dispersed in the distilled water into ice, transferring the ice into a freeze dryer for 24 hours for freeze drying, and then placing the ice into a drying tower for standby; putting the nano titanium dioxide particles into a baking oven, and preserving heat for 2 hours at 100 ℃; adding KH570 silane coupling agent into absolute ethanol solvent, stirring uniformly, adding the nano titanium dioxide particles, performing ultrasonic treatment in water bath at 50 ℃, condensing and refluxing, and continuously stirring for reaction for 4 hours to obtain a reaction solution III; and centrifuging the reaction liquid by a centrifugal machine, separating the modified nano titanium dioxide from the liquid, cleaning the modified nano titanium dioxide by using absolute ethyl alcohol for multiple times, and air-drying to obtain the modified nano titanium dioxide.
Example 2
The preparation of the composite polyimide film comprises the following steps:
(1) The molar ratio of the m-phenylenediamine to the 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride is 1:1.02, the addition amount of the modified nano titanium dioxide is 6.5 percent of the total weight of the m-phenylenediamine and the 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride, the modified nano titanium dioxide is dissolved in DMF solvent, and the modified nano titanium dioxide is dispersed for 2.5 hours under water bath in an ultrasonic manner;
(2) Adding m-phenylenediamine, stirring, adding 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride in a small quantity mode for multiple times after the m-phenylenediamine is completely dissolved, and continuously stirring for 3 hours to obtain a reaction solution I;
(3) Dispersing the reaction liquid in water bath for 25min, placing the reaction liquid in a vacuum drying oven, vacuumizing the reaction liquid to remove bubbles in the reaction liquid, and then scraping the reaction liquid on a uniform dust-free clean glass plate at a uniform speed from bottom to top through a film scraping machine, wherein the height of a push rod of the film scraping machine is 0.007 and mm;
(4) Placing the scraped film in a vacuum drying oven for solidification, vacuumizing and preserving heat at 80 ℃ for 2.0 h to obtain a first layer of modified polyimide film; pouring a second reaction solution on the basis of the modified polyimide film of the first layer, scraping the film at a constant speed from bottom to top by a film scraping machine, wherein the height of a push rod of the film scraping machine is 0.007 and mm, then placing the film in a vacuum drying oven for solidification, vacuumizing and preserving heat at 80 ℃ for 1.0h to obtain a pure polyimide film of the second layer; pouring a first reaction solution on the basis of a pure polyimide film of the second layer, scraping a film at a constant speed from bottom to top by a film scraping machine, wherein the height of a push rod of the film scraping machine is 0.007 mm, and then placing the film in a vacuum drying oven for thermal imidization to obtain a modified polyimide film of a third layer;
(5) Placing the mixture in a vacuum drying oven for thermal imidization, setting the initial temperature of the vacuum drying oven to 80 ℃, continuously vacuumizing the interior of the vacuum drying oven, then heating to 120 ℃, starting from 120 ℃, heating to 45 ℃ each time, and preserving heat for 0.5h by each temperature gradient, wherein the whole process lasts for 4.5h; taking out the cooled glass plate, transferring the glass plate into a blast drying oven, preserving heat for 50min from 250 ℃, heating to 280 ℃ and preserving heat for 30min, taking out the glass plate after the thermal imidization process is finished, placing the glass plate into cold water, and waiting for the natural falling of the composite polyimide film attached to the glass plate to obtain the composite polyimide film.
Wherein, the preparation of the modified nano titanium dioxide comprises the following steps: dispersing nano titanium dioxide particles in distilled water for 1.5 hours, freezing the nano titanium dioxide particles dispersed in the distilled water into ice, transferring the ice into a freeze dryer for 24 hours for freeze drying, and then placing the ice into a drying tower for standby; putting the nano titanium dioxide particles into a baking oven, and preserving heat for 2 hours at 100 ℃; adding KH570 silane coupling agent into absolute ethanol solvent, stirring uniformly, adding the nano titanium dioxide particles, performing ultrasonic treatment in water bath at 50 ℃, condensing and refluxing, and continuously stirring for reaction for 4 hours to obtain a reaction solution III; and centrifuging the reaction liquid by a centrifugal machine, separating the modified nano titanium dioxide from the liquid, cleaning the modified nano titanium dioxide by using absolute ethyl alcohol for multiple times, and air-drying to obtain the modified nano titanium dioxide.
The preparation of the second reaction liquid comprises the following steps: adding m-phenylenediamine into DMF solvent, continuously bubbling N2 into the solution for 10min, stirring until the m-phenylenediamine is completely dissolved under the protection of N2, adding 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride in a mode of a plurality of times in a small quantity, wherein the molar ratio of the m-phenylenediamine to the 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride is 1:1.02, stirring until the 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride is completely dissolved, and stirring for 4h at room temperature to obtain a reaction solution II; and (3) performing ultrasonic dispersion on the first reaction liquid for 30min in a water bath, putting the first reaction liquid into a vacuum drying box, and vacuumizing the second reaction liquid to remove bubbles in the reaction liquid.
Comparative example 1
The preparation of the pure polyimide film comprises the following steps:
(1) Adding m-phenylenediamine into DMF solvent, continuously bubbling N2 into the solution for 10min, stirring until the m-phenylenediamine is completely dissolved under the protection of N2, adding 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride in a mode of a plurality of times in a small quantity, wherein the molar ratio of the m-phenylenediamine to the 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride is 1:1.02, stirring until the 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride is completely dissolved, and stirring for 4h at room temperature to obtain a reaction solution II; dispersing the first reaction liquid in water bath for 30min, placing the first reaction liquid in a vacuum drying oven, and vacuumizing the second reaction liquid to remove bubbles in the reaction liquid;
(2) Uniformly scraping a film from bottom to top on a uniform dust-free clean glass plate of the reaction liquid II by a film scraping machine, wherein the height of a push rod of the film scraping machine is 0.021 and mm;
(3) Placing the mixture in a vacuum drying oven for thermal imidization, setting the initial temperature of the vacuum drying oven to 80 ℃, continuously vacuumizing the interior of the vacuum drying oven, then heating to 120 ℃, starting from 120 ℃, heating to 45 ℃ each time, and preserving heat for 0.5h by each temperature gradient, wherein the whole process lasts for 4.5h; taking out the cooled glass plate, transferring the cooled glass plate into a blast drying oven, preserving heat for 50min from 250 ℃, and preserving heat for 30min from 280 ℃;
(5) And after the thermal imidization process is finished, naturally cooling, taking out the glass plate, placing the glass plate in cold water, and waiting for the modified polyimide film attached to the glass plate to naturally fall off, thus obtaining the pure polyimide film.
Example 3
The preparation of the silica gel comprises the following steps:
the mass ratio of the polymethyl silane to the tetramethyl tetravinyl cyclotetrasiloxane is 1:1, the polymethyl silane and the tetramethyl tetravinyl cyclotetrasiloxane are placed into a reactor, the reaction temperature is set at 105 ℃, and under the protection of inert atmosphere, the mixture is stirred to be uniform through a stirrer, and the reaction is carried out for 3 hours, so that the silica gel I is obtained.
Example 4
The preparation of the silica gel comprises the following steps:
the silica gel mainly comprises the following components in parts by weight: 40 parts of polymethyl silane, 40 parts of tetramethyl tetravinyl cyclotetrasiloxane, 30 parts of boron carbide powder, 15 parts of glass powder and 1 part of nano silicon dioxide, and placing the polymethyl silane and the tetramethyl tetravinyl cyclotetrasiloxane into a reactor, wherein the reaction temperature is set at 110 ℃, and reacting for 3 hours under the protection of inert atmosphere to obtain a liquid precursor; adding boron carbide powder, glass powder and nano silicon dioxide into the liquid precursor, and stirring the mixture to be uniform by a stirrer to obtain silica gel II.
The high-temperature adhesive property of the silica gel is the reference basis for the most reaction of the temperature resistance of the silica gel, the silica gel I prepared in the example 3 and the silica gel II prepared in the example 4 are coated on two sides of the composite polyimide film prepared in the example 2 by a coating machine, are placed in an oven after being stood for 20min, are heated at a speed of 5 ℃/min, are cured for 1.0h at a temperature of 90 ℃, so that the silica gel and the composite polyimide film are completely cured, are naturally cooled to room temperature after being kept for 20min, and are subjected to shear strength test under different temperatures in an air atmosphere to obtain a sample 1 and a sample 2.
The shear strength of the sample 1 at 200 ℃ is 11.3MPa, the shear strength of the sample 1 at 400 ℃ is 13.8MPa, when the test temperature is increased to 600 ℃, the shear strength of the sample 1 is reduced to 5.1MPa, when the test temperature is further increased to 800 ℃, the sample 1 directly falls off in the test process, which is probably because the volume shrinkage of the sample 1 in the pyrolysis process is large during high-temperature treatment, the residual stress caused by the volume shrinkage is difficult to diffuse and transfer out due to the too fast heating rate, so that the stress is too concentrated, and the silica gel is cracked on the composite polyimide film; the shear strength of sample 2 at 200 ℃ is 10.1MPa, the shear strength of sample 2 at 400 ℃ is 12.9MPa, the shear strength of sample 2 is reduced to 9.5MPa when the test temperature is increased to 600 ℃, and the shear strength of sample 2 is reduced to 8.7MPa when the test temperature is increased to 800 ℃; when the test temperature was raised to 1000 ℃, the shear strength of sample 2 was reduced to 7.7 MPa. The above results indicate that the sample is better than sample 1 in the high temperature range (. Gtoreq.600 ℃).
Example 5
The preparation process of the high-temperature-resistant high-molecular industrial adhesive tape comprises the following steps of:
the silica gel prepared in example 3 and example 4 is coated on both sides of the composite polyimide film prepared in example 2 by a coating machine, and after standing for 20min, the composite polyimide film is placed between 2 release films, so that the release layers are contacted with the silica gel, then subjected to calendaring and compounding, placed into an oven, heated at a speed of 5 ℃/min, cured for 1.0h at a temperature of 90 ℃ to enable the release films, the silica gel and the composite polyimide film to be completely cured, and naturally cooled to room temperature after heat preservation for 20min to obtain the adhesive tape.
The preparation process of the release film comprises the following steps: uniformly mixing 50g of octyl phenol polyoxyethylene ether OP-13 (HLB value is 14), 50g of sodium dodecyl benzene sulfonate (HLB value is 10.6) and 600g of water to obtain a surfactant solution, coating the surfactant solution on the surface of a PET film (thickness is 0.075 mm), baking at 60 ℃ for 40min until the water volatilizes completely to form a release layer, cooling to room temperature to obtain a release film, wherein the amount of surfactant on the release film is 0.25g/m < 2 >, and the HLB value after the surfactant is compounded is 12.3.
And (3) effect verification:
the single-layer modified polyimide films, composite polyimide films, and pure polyimide films obtained in example 1, example 2, comparative example 1, and example 3 were examined.
Among them, by performing thermogravimetric-differential scanning calorimetric analysis and contact angle test, water absorption test and mechanical property test on the single-layer modified polyimide film, composite polyimide film, and pure polyimide film obtained in example 1, example 2, and comparative example 1, it was possible to obtain: the single-layer modified polyimide film of example 1 has the advantages that the thermal stability of example 1 is greatly improved due to the addition of the modified nano titanium dioxide, the glass transition temperature is improved to a certain extent, the temperature of 5% thermal weight loss is 45 ℃ higher than that of the pure polyimide film of comparative example 1, the temperature of 10% thermal weight loss is 32 ℃ higher than that of the pure polyimide film, and the decomposition temperature at the maximum decomposition rate is 14 ℃. In addition, the pure polyimide film of comparative example 1 had poor hydrophobicity due to the presence of hydrophilic groups inside its molecular structure, a contact angle of 55.23 ° and a water absorption of 3.56%, and the addition of modified nano titanium dioxide improved the hydrophobicity of the single-layer modified polyimide film of example 1, a contact angle of 92.12 ° and a water absorption of 1.65%. The composite polyimide film of example 2 has a three-layer structure, has better mechanical properties than the single-layer modified polyimide film of example 1, is substantially the same as the pure polyimide film of comparative example 1, and has higher thermal stability and glass transition temperature than the single-layer modified polyimide film of example 1, the composite polyimide film of example 2 has a 5% thermal weight loss temperature increased by 5 ℃ than the single-layer modified polyimide film of example 1, and a 10% thermal weight loss temperature increased by 3 ℃ than the pure polyimide film, and a decomposition temperature increased by 3 ℃ at the maximum decomposition rate. The composite polyimide film of example 2 was 93.23 deg., and the water absorption was 1.46%.
There are many ways in which the invention may be practiced, and what has been described above is merely a preferred embodiment of the invention. It should be noted that the above examples are only for illustrating the present invention and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that modifications may be made without departing from the principles of the invention, and such modifications are intended to be within the scope of the invention.
Claims (7)
1. The high-temperature-resistant high-molecular industrial adhesive tape is characterized by comprising a base material and a silica gel layer; the base material is prepared by adopting a composite polyimide film, the silica gel layer is prepared by coating silica gel on two sides of the base material, and the outer surface of the silica gel layer is covered with a release film; the composite polyimide film is formed by compounding a modified polyimide film, a pure polyimide film and a modified polyimide film from top to bottom; the modified polyimide film is prepared by preparing polyamide acid solution from modified nano titanium dioxide and m-phenylenediamine, 4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride through in-situ polymerization, and then thermally imidizing the polyamide acid solution; wherein the molar ratio of the m-phenylenediamine to the 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride is 1:1.02, and the addition amount of the modified nano titanium dioxide is 5-7% of the total weight of the m-phenylenediamine and the 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride; the silica gel mainly comprises the following components in parts by weight: 40-50 parts of polymethyl silane, 40-50 parts of tetramethyl tetravinyl cyclotetrasiloxane, 30-40 parts of boron carbide powder, 15-20 parts of glass powder and 10-15 parts of nano silicon dioxide; the release film comprises a substrate and a release layer attached to the surface of the substrate, wherein the release layer is a thin layer formed by a surfactant, and the release layer in the release film is in contact with the silica gel layer; the preparation of the modified nano titanium dioxide comprises the steps of dispersing nano titanium dioxide particles in distilled water for 1-2 hours in an ultrasonic manner, freezing the nano titanium dioxide particles dispersed in the distilled water into ice, transferring the ice into a freeze dryer for continuous 20-36 hours for freeze drying, and then placing the ice into a drying tower for standby; putting the nano titanium dioxide particles into an oven, and preserving heat for 1-2h at 100 ℃; adding KH570 silane coupling agent into absolute ethanol solvent, stirring uniformly, adding the nano titanium dioxide particles, performing ultrasonic treatment in water bath at 40-50 ℃, condensing and refluxing, and continuously stirring for reaction for 4 hours to obtain a reaction solution III; and centrifuging the reaction liquid by a centrifugal machine, separating the modified nano titanium dioxide from the liquid, cleaning the modified nano titanium dioxide by using absolute ethyl alcohol for multiple times, and air-drying to obtain the modified nano titanium dioxide.
2. The high-temperature resistant high-molecular industrial adhesive tape according to claim 1, wherein the thickness of the base material is 0.021mm, and the thickness of the modified polyimide film and the pure polyimide film is 0.007 mm; the thickness of the silica gel layer is 0.03 and mm, and the thickness of the release film is 0.012 and mm.
3. The high-temperature-resistant high-molecular industrial adhesive tape according to claim 1, wherein the surfactant is an anionic surfactant or a nonionic surfactant or is obtained by compounding the anionic surfactant with the nonionic surfactant; the HLB value of the surfactant is 10-20.
4. A process for preparing a high temperature resistant industrial tape according to any one of claims 1 to 3, comprising the steps of:
the polymethyl silane and tetramethyl tetravinyl cyclotetrasiloxane are put into a reactor, the reaction temperature is set at 100-110 ℃, and the reaction is carried out for 2-3 hours under the protection of inert atmosphere, so as to obtain a liquid precursor; adding boron carbide powder, glass powder and nano silicon dioxide into the liquid precursor, and stirring the mixture to be uniform by a stirrer to obtain silica gel;
coating a surface active agent on the surface of a substrate to form a release layer, and drying to remove a solvent to form the release layer to obtain a release film; and (3) coating silica gel on two sides of the composite polyimide film by a coating machine, standing for 10-20min, placing between 2 release films, enabling the release layers to be in contact with the silica gel, rolling and compounding, placing into an oven, heating at a speed of 5 ℃/min, solidifying for 0.5-1h at a temperature of 80-100 ℃ to enable the release films, the silica gel and the composite polyimide film to be completely solidified, preserving heat for 10-20min, and naturally cooling to room temperature to obtain the adhesive tape.
5. The process for preparing a high-temperature resistant high-molecular industrial adhesive tape according to claim 4, wherein the preparation of the composite polyimide film comprises the following steps:
dissolving the modified nano titanium dioxide in DMF solvent, and performing ultrasonic dispersion for 1-2h under water bath;
adding m-phenylenediamine, stirring, adding 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride in a small quantity mode for multiple times after the m-phenylenediamine is completely dissolved, and continuously stirring for 3-4 hours to obtain a reaction liquid I;
dispersing the reaction liquid I in water bath for 20-30min, placing the reaction liquid I in a vacuum drying oven, vacuumizing the reaction liquid I to remove bubbles in the reaction liquid I, and then scraping a film on a uniform dust-free clean glass plate of the reaction liquid I at a uniform speed from bottom to top through a film scraping machine, wherein the height of a push rod of the film scraping machine is 0.007 mm;
placing the scraped film in a vacuum drying oven for solidification, vacuumizing and preserving heat at 80 ℃ for 1.0-2.0 h to obtain a first layer of modified polyimide film; pouring a second reaction solution on the basis of the modified polyimide film of the first layer, scraping the film at a constant speed from bottom to top by a film scraping machine, wherein the height of a push rod of the film scraping machine is 0.007 and mm, then placing the film in a vacuum drying oven for solidification, vacuumizing and preserving heat at 80 ℃ for 1.0-2.0 h to obtain a pure polyimide film of the second layer; pouring a first reaction solution on the basis of a pure polyimide film of the second layer, scraping a film at a constant speed from bottom to top by a film scraping machine, wherein the height of a push rod of the film scraping machine is 0.007 mm, and then placing the film in a vacuum drying oven for thermal imidization to obtain a modified polyimide film of a third layer;
and after the thermal imidization process is finished, naturally cooling, taking out the glass plate, placing the glass plate in cold water, and waiting for the composite polyimide film attached to the glass plate to naturally fall off, thus obtaining the composite polyimide film.
6. The process for preparing a high-temperature resistant industrial adhesive tape according to claim 5, wherein the thermal imidization comprises the following steps: the initial temperature of the vacuum drying oven is set to 80 ℃, the interior of the vacuum drying oven is continuously vacuumized, then the temperature is raised to 120 ℃, the temperature is raised to 45 ℃ each time from 120 ℃, and each temperature gradient is kept for 0.5h, and the whole process lasts for 4-5h; taking out the cooled glass plate, transferring the cooled glass plate into a blast drying box, preserving heat for 50min from 250 ℃, and raising the temperature to 280 ℃ and preserving heat for 30min.
7. The process for preparing the high-temperature-resistant high-molecular industrial adhesive tape according to claim 5, wherein the preparation of the second reaction liquid comprises the following steps: adding m-phenylenediamine into DMF solvent, continuously bubbling N2 into the solution for 10min, stirring until the m-phenylenediamine is completely dissolved under the protection of N2, adding 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride in a small quantity mode for multiple times, stirring until the 4,4'- (4, 4' -isopropyl diphenoxy) diphthalic anhydride is completely dissolved, and stirring for 4-5h at room temperature to obtain reaction liquid II; and (3) carrying out ultrasonic dispersion on the first reaction liquid for 20-30min in a water bath, putting the first reaction liquid into a vacuum drying box, and vacuumizing the second reaction liquid to remove bubbles in the reaction liquid.
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