CN111647188A - Flexible environment-friendly high-temperature-resistant protective film and preparation method thereof - Google Patents

Flexible environment-friendly high-temperature-resistant protective film and preparation method thereof Download PDF

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CN111647188A
CN111647188A CN202010511425.4A CN202010511425A CN111647188A CN 111647188 A CN111647188 A CN 111647188A CN 202010511425 A CN202010511425 A CN 202010511425A CN 111647188 A CN111647188 A CN 111647188A
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fiber
parts
temperature
core layer
protective film
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CN111647188B (en
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潘炜
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Anhui Liumai New Material Technology Co ltd
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Ningbo Liumai New Material Technology Co ltd
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    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
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Abstract

The invention relates to the technical field of film manufacturing, in particular to a flexible environment-friendly high-temperature-resistant protective film and a preparation method thereof, wherein the protective film comprises a basic core layer and an infrared reflecting layer; the material is prepared from aromatic polyamide fiber, nano copper oxide, nano zinc sulfide, perfluoroalkyl polyether, phenolic resin modified neoprene, polytetrafluoroethylene, polybenzimidazole fiber, basalt fiber, nano silicon dioxide, chlorohydrin rubber, o-cresol formaldehyde epoxy resin, methyl silicone rubber, polyurethane modified epoxy resin and sulfur trioxide. The film disclosed by the invention is subjected to multilayer treatment, so that the hierarchy of the whole film is clear, the heat conduction effect can be reduced, the heat absorption of the whole film is reduced through multilayer reflection of external radiation, the film has better high-temperature tolerance and heat insulation effect, the compatibility of a manufacturing link and the environment is good, and the environment suitability is better.

Description

Flexible environment-friendly high-temperature-resistant protective film and preparation method thereof
Technical Field
The invention relates to the technical field of film manufacturing, in particular to a flexible environment-friendly high-temperature-resistant protective film and a preparation method thereof.
Background
A film made of organic high molecular polymer. With the development of petroleum industry and science and technology, the application field of polymer films is continuously expanded, and the original packaging films are developed into intelligent polymer films, polymer functional films and the like. The polymer membrane is applied to the fields of nuclear fuel and metal extraction, gas separation, seawater desalination, ultrapure water preparation, sewage and waste treatment, artificial organ manufacturing, medicine, food, agriculture, chemical industry and the like by virtue of excellent performance. However, the polymer film in the prior art is rarely studied under high heat use, and the polymer film is often simply mixed and coagulated in the production process, and it is difficult to develop the excellent performance of the polymer film. For example, a heat insulation plastic film with the patent number of CN201310658538.7 and a production method thereof, which consists of an acid-doped polymethacrylate film and a nano tin dioxide crystalline heat insulation layer deposited on the surface of the film, so that the heat insulation effect of the film adhered to the surface of glass is good, the plastic film has soft texture and high strength, but the high temperature resistant effect interval is narrow, and the high strength of the film can not be exerted under special environment; for example, CN201510600862.2 is a high temperature resistant isolation film and a method for preparing the same, the silicone rubber coated on the substrate provides good wettability and physical entanglement with the nonwoven fabric, and after the cross-linking agent is cured, the overall strength is high and the flexibility is good, but the heat insulation of the film is simple, and the use effect is poor only by using high temperature resistant materials under continuous high temperature.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a flexible environment-friendly high-temperature-resistant protective film and a preparation method thereof, which are used for improving the use of the film under high-temperature strength and improving the use effect of the film under extreme conditions, and the specific technical scheme is as follows:
a flexible environment-friendly high-temperature-resistant protective film comprises a basic core layer and an infrared reflecting layer; the mass ratio of the basic core layer to the infrared reflecting layer is (5-8) to 0.1; the infrared reflecting layer is prepared from the following raw materials in parts by mass: 3-5 parts of aromatic polyamide fiber, 0.1-0.3 part of nano copper oxide, 0.1-0.3 part of nano zinc sulfide, 0.01-0.05 part of perfluoroalkyl polyether, 15-25 parts of phenolic resin modified neoprene and 5-15 parts of polytetrafluoroethylene.
Further, the basic core layer is composed of the following raw materials in parts by mass: 8-10 parts of polybenzimidazole fiber, 0.2-0.5 part of basalt fiber, 0.5-1 part of nano silicon dioxide, 10-15 parts of chlorohydrin rubber, 18-22 parts of o-cresol formaldehyde epoxy resin, 5-8 parts of methyl silicone rubber, 25-30 parts of polyurethane modified epoxy resin and 0.02-0.05 part of sulfur trioxide.
Further, the aromatic polyamide fiber is one or more of poly-p-phenylene terephthamide fiber and poly-m-phenylene isophthalamide fiber.
Further, the fineness of the aromatic polyamide fiber is 0.1mm-0.8 mm.
Furthermore, the fineness of the polybenzimidazole fiber is 0.1mm-0.8 mm.
The preparation method of the flexible environment-friendly high-temperature-resistant protective film comprises the following steps:
(1) modification of basalt fibers:
heating the basalt fiber to 120 ℃ in vacuum, introducing steam for heating for 10-20min, introducing sulfur trioxide, heating to 200 ℃ in vacuum, performing ultrasonic treatment for 15-25min, reducing the temperature to 60-80 ℃, and drying the basalt fiber in vacuum to constant weight; the mass ratio of the water vapor to the basalt fibers is 1: 10;
(2) mixing a basic core layer:
heating polybenzimidazole fiber, nano-silica, epichlorohydrin rubber and methyl silicone rubber to 240 ℃ in vacuum equipment, mixing uniformly, and adding modified basalt fiber;
(3) shaping a basic core layer:
adding the o-cresol formaldehyde epoxy resin into the mixture obtained in the last step, fully and uniformly mixing, adding the polyurethane modified epoxy resin, dissolving and stirring, pouring the molten mass into a mold, and cooling and molding to obtain a basic core layer;
(4) infrared reflecting layer adhesion
Heating aromatic polyamide fiber, nano copper oxide, nano zinc sulfide, perfluoroalkyl polyether and phenolic resin modified neoprene to 180-class temperature and 200 ℃, uniformly mixing, spraying the mixture on the surface of a basic core layer, and spraying a layer of fused polytetrafluoroethylene.
Compared with the prior art, the invention has the technical effects that:
the film is subjected to multilayer treatment, the base core layer and the infrared reflecting layer are arranged, so that the whole film is distinct in level, the heat conduction effect can be reduced, the heat absorption of the whole film is reduced through multilayer reflection by external radiation, and the film has better high-temperature tolerance and heat insulation effect. In addition, the compactness of the infrared reflecting layer is improved by selecting the raw materials of the basic core layer and the infrared reflecting layer and spraying and mixing the aromatic polyamide fiber, the phenolic resin modified neoprene and the polytetrafluoroethylene.
According to the invention, the high stability of the aromatic polyamide fiber and the high viscosity of the phenolic resin modified neoprene are utilized to increase the mixing degree of the nano copper oxide and the nano zinc sulfide and promote the dispersion of the nano copper oxide and the nano zinc sulfide, so that the stability of the infrared reflecting layer under strong light is higher, the film condensation degree of the infrared reflecting layer is enhanced, the better stress characteristic is realized on the microstructure, the molecular constraint effect is enhanced, and the macro effect of fracture resistance is improved; and the forbidden bandwidths of the nano copper oxide and the nano zinc sulfide are 0.5-3.1eV, are closer to the forbidden bandwidths of near infrared rays and visible light, have high refractive index, and have higher reflection effect on the near infrared rays.
In addition, the basalt fiber in the basic core layer is modified by using sulfur trioxide at high temperature, the basalt fiber is etched by sulfuric acid formed by high-efficiency diffusion of high-temperature water vapor carrying trace sulfur trioxide by utilizing the characteristic that the basalt fiber contains active metals such as calcium and the like, the surface modification of the basalt fiber is accelerated under the action of ultrasonic waves, so that the contact area of the basalt fiber and the sulfuric acid is wider, the surface roughness of the basalt fiber is higher, the bonding effect of the basalt fiber, silicon rubber and polyurethane modified epoxy resin is strengthened, the agglomeration of the basalt fiber and the silicon rubber is improved under the action of the silicon dioxide, the stability of the basic core layer at high temperature is enhanced, the bonding degree of the basic core layer and the infrared reflecting layer is improved, the film is integrally layered but structurally integrated, the mechanical effect is unified, the integral resistance is better, the basic core layer has lower temperature under the cladding of the infrared reflecting layer, the membrane has a wider high-temperature buffer area at high temperature, is beneficial to exerting better structural performance at high temperature and has better resistance; and no serious pollution emission is caused in the manufacturing process, so that the method is extremely environment-friendly.
According to the invention, polytetrafluoroethylene is sprayed on the surface, the characteristic of high melting point of the polytetrafluoroethylene is utilized, the surface of the mixture of aromatic polyamide fiber, nano copper oxide, nano zinc sulfide, perfluoroalkyl polyether and phenolic resin modified chloroprene rubber is ablated by spraying, the surface tightening of the whole infrared reflecting layer is promoted, the strength and the high temperature resistance of the surface of the protective film are enhanced, the penetration of external heat is reduced, and the surface deformation generated by ablation is utilized to increase the infrared reflecting area, so that the whole protective film has good application effect at high temperature and low temperature, the reflection of the nano copper oxide and the nano zinc sulfide in the film to infrared rays is ensured, and meanwhile, the flexibility of the film at low temperature is improved.
The tensile strength of the protective film prepared by the method exceeds 5.28Mpa, and the elongation at break exceeds 200.53%. When the room temperature is 25 ℃, the film is attached to a glass plate, the other surface of the film is irradiated by a 1000W iodine tungsten lamp, the irradiation distance is 0.5m, the temperature of the glass plate is lower than 29.68 ℃ in 30min and lower than 33.12 ℃ in 60min, and the film has a very good high-temperature isolation effect.
Detailed Description
The technical solution of the present invention is further defined below with reference to the specific embodiments, but the scope of the claims is not limited to the description.
Example 1
A flexible environment-friendly high-temperature-resistant protective film comprises a basic core layer and an infrared reflecting layer; the mass ratio of the basic core layer to the infrared reflecting layer is 8: 0.1; the infrared reflecting layer is prepared from the following raw materials in parts by mass: 5 parts of aromatic polyamide fiber, 0.3 part of nano copper oxide, 0.3 part of nano zinc sulfide, 0.05 part of perfluoroalkyl polyether, 25 parts of phenolic resin modified neoprene and 15 parts of polytetrafluoroethylene; the aromatic polyamide fiber is poly-p-phenylene terephthamide fiber; the fineness of the aromatic polyamide fiber is 0.8 mm; the basic core layer is composed of the following raw materials in parts by mass: 10 parts of polybenzimidazole fiber, 0.5 part of basalt fiber, 0.2 part of nano silicon dioxide, 15 parts of chlorohydrin rubber, 22 parts of o-cresol formaldehyde epoxy resin, 8 parts of methyl silicone rubber, 30 parts of polyurethane modified epoxy resin and 0.05 part of sulfur trioxide; the fineness of the polybenzimidazole fiber is 0.8 mm.
The preparation method of the flexible environment-friendly high-temperature-resistant protective film comprises the following steps:
(1) modification of basalt fibers:
heating basalt fiber to 120 ℃ in vacuum, introducing steam for heating for 20min, introducing sulfur trioxide, heating to 200 ℃, performing ultrasonic treatment for 25min, reducing the temperature to 80 ℃, and drying the basalt fiber to constant weight in vacuum; the mass ratio of the water vapor to the basalt fibers is 1: 10;
(2) mixing a basic core layer:
heating polybenzimidazole fiber, nano silicon dioxide, chlorohydrin rubber and methyl silicone rubber to 220 ℃ in vacuum equipment, mixing uniformly, and adding modified basalt fiber;
(3) shaping a basic core layer:
adding the o-cresol formaldehyde epoxy resin into the mixture obtained in the last step, fully and uniformly mixing, adding the polyurethane modified epoxy resin, dissolving and stirring, pouring the molten mass into a mold, and cooling and molding to obtain a basic core layer;
(4) infrared reflecting layer adhesion
Heating aromatic polyamide fiber, nano copper oxide, nano zinc sulfide, perfluoroalkyl polyether and phenolic resin modified neoprene adhesive to 200 ℃, uniformly mixing, spraying the mixture on the surface of a basic core layer, and spraying a layer of fused polytetrafluoroethylene.
Example 2
A flexible environment-friendly high-temperature-resistant protective film comprises a basic core layer and an infrared reflecting layer; the mass ratio of the basic core layer to the infrared reflecting layer is 5: 0.1; the infrared reflecting layer is prepared from the following raw materials in parts by mass: 3 parts of aromatic polyamide fiber, 0.1 part of nano copper oxide, 0.1 part of nano zinc sulfide, 0.01 part of perfluoroalkyl polyether, 15 parts of phenolic resin modified neoprene and 5 parts of polytetrafluoroethylene; the aromatic polyamide fiber is polyisophthaloyl metaphenylene diamine fiber; the fineness of the aromatic polyamide fiber is 0.8 mm; the basic core layer is composed of the following raw materials in parts by mass: 10 parts of polybenzimidazole fiber, 0.5 part of basalt fiber, 0.2 part of nano silicon dioxide, 15 parts of chlorohydrin rubber, 22 parts of o-cresol formaldehyde epoxy resin, 8 parts of methyl silicone rubber, 30 parts of polyurethane modified epoxy resin and 0.05 part of sulfur trioxide; the fineness of the polybenzimidazole fiber is 0.8 mm.
The preparation method of the flexible environment-friendly high-temperature-resistant protective film comprises the following steps:
(1) modification of basalt fibers:
heating basalt fiber to 120 ℃ in vacuum, introducing steam for heating for 20min, introducing sulfur trioxide, heating to 180 ℃, performing ultrasonic treatment for 15min, reducing the temperature to 60 ℃, and drying the basalt fiber to constant weight in vacuum; the mass ratio of the water vapor to the basalt fibers is 1: 10;
(2) mixing a basic core layer:
heating polybenzimidazole fiber, nano silicon dioxide, chlorohydrin rubber and methyl silicone rubber to 240 ℃ in vacuum equipment, mixing uniformly, and adding modified basalt fiber;
(3) shaping a basic core layer:
adding the o-cresol formaldehyde epoxy resin into the mixture obtained in the last step, fully and uniformly mixing, adding the polyurethane modified epoxy resin, dissolving and stirring, pouring the molten mass into a mold, and cooling and molding to obtain a basic core layer;
(4) infrared reflecting layer adhesion
Heating aromatic polyamide fiber, nano copper oxide, nano zinc sulfide, perfluoroalkyl polyether and phenolic resin modified neoprene adhesive to 180 ℃, uniformly mixing, spraying the mixture on the surface of a basic core layer, and spraying a layer of fused polytetrafluoroethylene.
Example 3
A flexible environment-friendly high-temperature-resistant protective film comprises a basic core layer and an infrared reflecting layer; the mass ratio of the basic core layer to the infrared reflecting layer is 7: 0.1; the infrared reflecting layer is prepared from the following raw materials in parts by mass: 4 parts of aromatic polyamide fiber, 0.23 part of nano copper oxide, 0.13 part of nano zinc sulfide, 0.03 part of perfluoroalkyl polyether, 18 parts of phenolic resin modified neoprene and 11 parts of polytetrafluoroethylene; the aromatic polyamide fiber is formed by mixing poly (p-phenylene terephthalamide) fiber and poly (m-phenylene isophthalamide) fiber according to the mass ratio of 1: 1; the fineness of the aromatic polyamide fiber is 0.5 mm; the basic core layer is composed of the following raw materials in parts by mass: 9 parts of polybenzimidazole fiber, 0.4 part of basalt fiber, 1 part of nano silicon dioxide, 13 parts of chlorohydrin rubber, 19 parts of o-cresol formaldehyde epoxy resin, 7 parts of methyl silicone rubber, 28 parts of polyurethane modified epoxy resin and 0.02 part of sulfur trioxide; the fineness of the polybenzimidazole fiber is 0.8 mm.
The preparation method of the flexible environment-friendly high-temperature-resistant protective film comprises the following steps:
(1) modification of basalt fibers:
heating basalt fiber to 110 ℃ in vacuum, introducing steam for 18min, introducing sulfur trioxide, heating to 199 ℃, performing ultrasonic treatment for 19min, reducing the temperature to 75 ℃, and drying the basalt fiber to constant weight in vacuum; the mass ratio of the water vapor to the basalt fibers is 1: 10;
(2) mixing a basic core layer:
heating polybenzimidazole fiber, nano silicon dioxide, chlorohydrin rubber and methyl silicone rubber to 230 ℃ in vacuum equipment, mixing uniformly, and adding modified basalt fiber;
(3) shaping a basic core layer:
adding the o-cresol formaldehyde epoxy resin into the mixture obtained in the last step, fully and uniformly mixing, adding the polyurethane modified epoxy resin, dissolving and stirring, pouring the molten mass into a mold, and cooling and molding to obtain a basic core layer;
(4) infrared reflecting layer adhesion
Heating aromatic polyamide fiber, nano copper oxide, nano zinc sulfide, perfluoroalkyl polyether and phenolic resin modified neoprene to 190 ℃, uniformly mixing, spraying the mixture on the surface of a basic core layer, and spraying a layer of fused polytetrafluoroethylene.
Comparative example
Comparative example 1 The difference from the embodiment 1 is that the raw materials do not contain nano copper oxide;
comparative example 2 The difference from the embodiment 1 is that the raw materials do not contain nano zinc sulfide;
comparative example 3 The difference from example 1 is that the starting material was preparedDoes not contain polyfluortetraethylene;
comparative example 4 The difference from the embodiment 1 is that the basalt fiber is not contained in the raw materials for making;
comparative example 5 The difference from the embodiment 1 is that the basalt fiber is not modified in the raw materials;
comparative example 6 The difference from the embodiment 1 is that the nano silicon dioxide is not added in the step (2) in the preparation raw material;
comparative example 7 The difference from example 1 is that no sulfur trioxide is added in step (1);
comparative example 8 The difference from example 1 is that no ultrasonic treatment was performed in step (1);
comparative example 9 According to patent No. CN 201810673134.8.
Test examples
Respectively treating the films prepared in the examples 1-3 and the comparative examples 1-8 for 5 hours in a heat preservation box at 150 ℃, and detecting the tensile strength and the elongation at break of the films; the films were attached to a glass plate at room temperature of 25 deg.C, one side of the film was irradiated with a 1000W tungsten-iodine lamp at an irradiation distance of 0.5m, and the heat insulating effect of each film was evaluated by detecting the temperature of the glass plate at 30min and 60 min.
Figure BDA0002528451260000081
Figure BDA0002528451260000091
As can be seen from the table, the film of the present invention has better tensile strength and elongation at break after high temperature treatment, and has better high temperature resistance; after irradiation, the temperature of the film-thickness glass plate is lower, and the temperature rising speed is slow, so that the film has better heat insulation effect.

Claims (6)

1. The flexible environment-friendly high-temperature-resistant protective film is characterized by comprising a basic core layer and an infrared reflecting layer; the mass ratio of the basic core layer to the infrared reflecting layer is (5-8) to 0.1; the infrared reflecting layer is prepared from the following raw materials in parts by mass: 3-5 parts of aromatic polyamide fiber, 0.1-0.3 part of nano copper oxide, 0.1-0.3 part of nano zinc sulfide, 0.01-0.05 part of perfluoroalkyl polyether, 15-25 parts of phenolic resin modified neoprene and 5-15 parts of polytetrafluoroethylene.
2. The flexible environment-friendly high-temperature-resistant protective film as claimed in claim 1, wherein the basic core layer is composed of the following raw materials in parts by mass: 8-10 parts of polybenzimidazole fiber, 0.2-0.5 part of basalt fiber, 0.5-1 part of nano silicon dioxide, 10-15 parts of chlorohydrin rubber, 18-22 parts of o-cresol formaldehyde epoxy resin, 5-8 parts of methyl silicone rubber, 25-30 parts of polyurethane modified epoxy resin and 0.02-0.05 part of sulfur trioxide.
3. The flexible environment-friendly high-temperature-resistant protective film according to claim 1, wherein the aromatic polyamide fiber is one or more of poly (p-phenylene terephthalamide) fiber and poly (m-phenylene isophthalamide) fiber.
4. The flexible environment-friendly high-temperature-resistant protective film according to claim 1, wherein the fineness of the aromatic polyamide fiber is 0.1mm to 0.8 mm.
5. The flexible environment-friendly high temperature resistant protective film according to claim 1, wherein the fineness of the polybenzimidazole fiber is 0.1mm to 0.8 mm.
6. The flexible environment-friendly high-temperature-resistant protective film according to claim 1, which is prepared by the following steps:
(1) modification of basalt fibers:
heating the basalt fiber to 120 ℃ in vacuum, introducing steam for heating for 10-20min, introducing sulfur trioxide, heating to 200 ℃ in vacuum, performing ultrasonic treatment for 15-25min, reducing the temperature to 60-80 ℃, and drying the basalt fiber in vacuum to constant weight; the mass ratio of the water vapor to the basalt fibers is 1: 10;
(2) mixing a basic core layer:
heating polybenzimidazole fiber, nano-silica, epichlorohydrin rubber and methyl silicone rubber to 240 ℃ in vacuum equipment, mixing uniformly, and adding modified basalt fiber;
(3) shaping a basic core layer:
adding the o-cresol formaldehyde epoxy resin into the mixture obtained in the last step, fully and uniformly mixing, adding the polyurethane modified epoxy resin, dissolving and stirring, pouring the molten mass into a mold, and cooling and molding to obtain a basic core layer;
(4) infrared reflecting layer adhesion
Heating aromatic polyamide fiber, nano copper oxide, nano zinc sulfide, perfluoroalkyl polyether and phenolic resin modified neoprene to 180-class temperature and 200 ℃, uniformly mixing, spraying the mixture on the surface of a basic core layer, and spraying a layer of fused polytetrafluoroethylene.
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