CN111037942B - Preparation process of explosion-proof and radiation-proof double-layer composite mobile phone protective film - Google Patents
Preparation process of explosion-proof and radiation-proof double-layer composite mobile phone protective film Download PDFInfo
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C69/00—Combinations of shaping techniques not provided for in a single one of main groups B29C39/00 - B29C67/00, e.g. associations of moulding and joining techniques; Apparatus therefore
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- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
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Abstract
The invention discloses a preparation process of an explosion-proof and radiation-proof double-layer composite mobile phone protective film, which comprises a fingerprint-proof layer and a radiation-proof base material layer, and comprises the following steps: firstly, preparing a radiation-proof base material layer; secondly, preparing an anti-fingerprint layer; thirdly, compounding one side of the radiation-proof base material layer and the fingerprint-proof layer through an adhesive to obtain the explosion-proof and radiation-proof double-layer composite mobile phone protective film; the composite film is prepared by combining the polyether-ether-ketone film and the graphene oxide/silicon nitride particles, so that the compatibility of a polymer and a particle component on a molecular level can be improved, the graphene oxide/silicon nitride composite film is endowed with good radiation protection performance and antibacterial performance, and the graphene oxide/silicon nitride composite particles can endow the film with excellent wear resistance.
Description
Technical Field
The invention belongs to the technical field of mobile phone protective films, and particularly relates to a preparation process of an explosion-proof and radiation-proof double-layer composite mobile phone protective film.
Background
The mobile phone film is also called as mobile phone beauty film and mobile phone protective film, is a cold mounting film which can be used for mounting the surface of the body of a mobile phone, a screen and other tangible objects, has various types, and can be divided into the following films according to the purposes: a mobile phone screen protective film and a mobile phone body protective film; the functions from the original simple scratch-resistant protective film to the push-out functional protective film series can be divided into: a peep-proof film, a mirror film, an AR film, a frosted film, a high-cleanness film, a scratch-proof protective film, a 3D film, a mobile phone body scratch-proof protective film, a diamond film, a toughened film and the like; however, in the normal use process of the mobile phone, traces and fingerprint lines can be left by touching the mobile phone with hands, the frequently touched surface is usually easily polluted by fingerprints, grease on skin, sweat and cosmetics, and the accumulation of the fingerprints on the surface of the touch screen not only seriously affects the visual definition and the visual sense of the mobile phone, but also causes the readability of the touch panel to be rapidly reduced and the usability of the mobile phone to be reduced; and with the daily use of the mobile phone becoming more and more extensive, the generated radiation can also cause damage to the human body.
The Chinese patent invention CN105450801A discloses a composite mobile phone protective film, which comprises a scratch-proof layer on the uppermost layer, a waterproof layer in the middle layer and a substrate layer on the lowermost layer, wherein the scratch-proof layer is made of toughened glass, the scratch-proof layer accounts for 34-35% of the total weight of the composite mobile phone protective film, the waterproof layer accounts for 31-35% of the total weight of the composite mobile phone protective film, and the substrate layer accounts for 30-33% of the total weight of the composite mobile phone protective film.
Disclosure of Invention
In order to overcome the technical problems, the invention provides a preparation process of an explosion-proof and radiation-proof double-layer composite mobile phone protective film.
The technical problems to be solved by the invention are as follows:
(1) the graphene has super van der waals force and conjugate acting force, a three-dimensional structure is easily formed, so that the graphene has poor dispersibility in an organic phase and an aqueous phase solvent, and composite particles prepared from the graphene and silicon nitride have poor stability and cannot be prepared into a film through the composite particles;
(2) the compatibility of the traditional graphene and a high polymer is poor at a molecular level, and a composite film prepared from the traditional graphene and a polyether-ether-ketone film cannot have excellent radiation-proof performance and antibacterial performance and cannot endow the composite film with excellent wear-resistant performance.
The purpose of the invention can be realized by the following technical scheme:
a preparation process of an explosion-proof and radiation-proof double-layer composite mobile phone protective film comprises a fingerprint-proof layer and a radiation-proof base material layer, and comprises the following steps:
firstly, preparing a radiation-proof base material layer:
step S1, weighing the following raw materials in parts by weight: 5-10 parts of graphene oxide/silicon nitride composite particles, 2-5 parts of butadiene, 10-15 parts of styrene, 10-20 parts of acrylate, 5-10 parts of dimethyl silicone oil, 25-30 parts of ethylene glycol, 1-5 parts of KH550, 0.2-0.8 part of lauroyl peroxide, 3-5 parts of polyether-ether-ketone powder, 15-25 parts of acetonitrile and 0.1-0.3 part of PEG 400;
step S2, dissolving the polyetheretherketone powder in acetonitrile, adding PEG400, stirring at a constant speed for 15min, casting to form a film, drying at 60 ℃ for 5h, cooling to room temperature, and immersing in water for taking down to obtain a polyetheretherketone film;
step S3, adding butadiene, styrene and acrylic ester into a beaker, mixing, adding ethylene glycol, magnetically stirring for 15min to obtain a mixed solution, adding the graphene oxide/silicon nitride composite particles, the simethicone and the mixed solution into deionized water, carrying out ultrasonic treatment for 2h, controlling the ultrasonic power to be 800w, and adding KH550 to obtain a membrane solution;
step S4, adding the polyether-ether-ketone film prepared in the step S2 into the film liquid prepared in the step S3, adding lauroyl peroxide, introducing nitrogen to discharge air, and reacting for 5 hours to obtain a graphene oxide/silicon nitride composite film;
step S5, drying and cutting the prepared graphene oxide/silicon nitride composite film to obtain the radiation-proof base material layer;
the preparation method comprises the steps of firstly preparing a polyether-ether-ketone film, then preparing a film-forming agent by mixing butadiene, styrene, acrylic ester and the like, using ethylene glycol as an organic solvent, preparing a graphene oxide/silicon nitride film solution under the condition that lauroyl peroxide is used as an initiator, and finally preparing the graphene oxide/silicon nitride composite film by using the polyether-ether-ketone film and the film solution.
Step two, preparing the fingerprint-proof layer:
(1) mixing polydimethylsiloxane and a curing agent to prepare a mixture, adding a hydrophobic material, pouring the mixture onto a substrate, and curing for 2 hours at 90 ℃ to prepare a polydimethylsiloxane film, wherein the weight ratio of the polydimethylsiloxane to the curing agent to the hydrophobic material is controlled to be 10: 1: 0.1;
(2) etching the polydimethylsiloxane film for 2min, then ultrasonically drying for 1h at 70 ℃ to obtain an anti-fingerprint film, and cutting the film to obtain the anti-fingerprint layer;
and thirdly, compounding one side of the radiation-proof base material layer and the fingerprint-proof layer through an adhesive to obtain the explosion-proof and radiation-proof double-layer composite mobile phone protective film.
Firstly, preparing a polydimethylsiloxane film, then etching the polydimethylsiloxane film to enable the surface of the polydimethylsiloxane film to generate a micro-nano rough structure, controlling the wettability of sweat on the surface of the polydimethylsiloxane film by etching for 2min to realize the fingerprint prevention effect, and further enhancing the fingerprint prevention performance of the film by adding tridecafluorooctyltrimethoxysilane in the preparation process.
Further, the graphene oxide/silicon nitride composite particles are prepared by the following method:
(1) adding graphene into a round-bottom flask, adding sodium nitrate and 98% concentrated sulfuric acid by mass, stirring for 15min in an ice bath at 3 ℃, adding potassium chlorate, continuously stirring for 30min, heating in a water bath at 40 ℃, reacting for 3h, adding deionized water, placing under an oil bath at 80 ℃, reacting for 30min, adding 20% hydrogen peroxide water by volume, and continuously reacting for 10min, wherein the weight ratio of the graphene to the sodium nitrate to the 98% concentrated sulfuric acid to the potassium chlorate to the 20% hydrogen peroxide water is controlled to be 1: 0.5: 20: 0.1: 3;
(2) adding silicon nitride into deionized water, carrying out magnetic stirring at the rotating speed of 250r/min, adding the graphene oxide solution prepared in the step (1), continuously stirring and carrying out ultrasonic treatment for 30min, then transferring to a hydrothermal kettle, reacting at 100 ℃ for 10h, then filtering, washing a filter cake with absolute ethyl alcohol, dispersing in the absolute ethyl alcohol after washing for three times, adding oleic acid, stirring at the rotating speed of 450r/min and refluxing for 20min, cooling, centrifuging and washing to prepare the graphene oxide/silicon nitride composite particles, wherein the weight ratio of silicon nitride to graphene oxide to oleic acid is controlled to be 1: 0.2: 0.05.
The method comprises the following steps that (1) superstrong van der Waals force and conjugate acting force exist among graphene, a three-dimensional structure is easy to form, and the dispersibility of the graphene in an organic phase and an aqueous phase solvent is poor, graphene oxide is prepared from the graphene under the action of potassium chlorate, 20% hydrogen peroxide water solution and the like, the graphene oxide can be dispersed in water and can also be dispersed in the organic solvent, and rich oxygen-containing functional groups are added on the surface of the graphene oxide, so that the graphene oxide is not easy to agglomerate; and (2) preparing a composite particle by using graphene oxide and silicon nitride, wherein the graphene oxide is flaky in a system and can coat the silicon nitride, the silicon nitride is in a spindle shape under the coating effect of the graphene oxide and the effect of self free energy, then oleic acid is added, a large number of hydroxyl groups exist on the surface of the graphene oxide and can perform esterification reaction with carboxyl groups on the oleic acid, oleic acid molecules are grafted on the surface of the graphene oxide, the surface of the graphene oxide is covered, the distance between the graphene oxides is further increased, the silicon nitride is better mixed with the graphene oxide, and the prepared graphene oxide/silicon nitride composite particle has excellent stability and can endow the finally prepared composite film with excellent wear resistance.
Further, the thickness of the radiation-proof substrate layer and the thickness of the fingerprint-proof layer are 0.10-0.15 mm.
Further, the adhesive in the third step is one or two of water-based plastic-plastic composite adhesive and pressure-sensitive adhesive.
Furthermore, the hydrophobic material in the second step is one or more of tridecafluorooctyltrimethoxysilane, heptadecafluorodecyltriethoxysilane and dodecafluoroheptylpropyltrimethoxysilane.
The invention has the beneficial effects that:
(1) the invention relates to an explosion-proof and radiation-proof double-layer composite mobile phone protective film, which comprises a fingerprint-proof layer and a radiation-proof base material layer, wherein the protective film is used for a mobile phone back shell, the radiation-proof base material layer is a graphene oxide/silicon nitride composite film, a polyether-ether-ketone film is prepared in the preparation process of the film, a film forming agent is prepared by mixing butadiene, styrene, acrylic ester and the like, ethylene glycol is used as an organic solvent, a graphene oxide/silicon nitride film solution is prepared under the condition that lauroyl peroxide is used as an initiator, the graphene oxide/silicon nitride composite film is prepared by the polyether-ether-ketone film and the film solution, the polyether-ether-ketone film and the graphene oxide/silicon nitride particles are combined in the film to prepare a composite film, and the compatibility of a polymer and a particle component on a molecular level can be improved, the graphene oxide/silicon nitride composite film has good radiation-proof performance and antibacterial performance, and the graphene oxide/silicon nitride composite particles can endow the film with excellent wear-resistant performance; in the preparation process of the anti-fingerprint layer, a polydimethylsiloxane film is prepared firstly, then the polydimethylsiloxane film is etched, so that a micro-nano rough structure is generated on the surface of the polydimethylsiloxane film, the wettability of sweat on the surface of the polydimethylsiloxane film can be controlled by the etching time of 2min, and the anti-fingerprint effect is realized, and the anti-fingerprint performance of the film can be further enhanced by adding tridecafluorooctyl trimethoxy silane as a hydrophobic material in the preparation process, so that the technical problems that the traditional graphene and high polymer have poor compatibility on the molecular level, and a composite film prepared from the graphene and a polyether-ether-ketone film does not have excellent radiation resistance and antibacterial performance and cannot endow the composite film with excellent wear resistance are solved;
(2) in the preparation process, in the step (1), graphene is used for preparing graphene oxide under the action of potassium chlorate, 20% hydrogen peroxide water solution and the like, the graphene oxide can be dispersed in water and can also be dispersed in an organic solvent, and rich oxygen-containing functional groups are added on the surface of the graphene oxide, so that the graphene oxide/silicon nitride composite particles are not easy to agglomerate; step (2) preparing a composite particle by using graphene oxide and silicon nitride, wherein the graphene oxide is flaky in a system and can wrap the silicon nitride, the silicon nitride is in a spindle shape under the wrapping effect of the graphene oxide and the effect of self free energy, then oleic acid is added, a large number of hydroxyl groups exist on the surface of the graphene oxide and can perform esterification reaction with carboxyl groups on the oleic acid, oleic acid molecules are grafted on the surface of the graphene oxide, the surface of the graphene oxide is covered, the distance between the graphene oxides is further increased, the silicon nitride is better mixed with the graphene oxide, the prepared graphene oxide/silicon nitride composite particle has excellent stability, the excellent wear resistance of the finally prepared composite film can be endowed, the problem that van der Waals force and conjugate force exist between the graphene is solved, and a three-dimensional structure is easily formed, the dispersibility of the graphene oxide in organic phase and aqueous phase solvents is poor, and the composite particles prepared from the graphene and the silicon nitride have poor stability and cannot be prepared into films.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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 protection scope of the present invention.
Example 1
A preparation process of an explosion-proof and radiation-proof double-layer composite mobile phone protective film comprises a fingerprint-proof layer and a radiation-proof base material layer, and comprises the following steps:
firstly, preparing a radiation-proof base material layer:
step S1, weighing the following raw materials in parts by weight: 5 parts of graphene oxide/silicon nitride composite particles, 2 parts of butadiene, 10 parts of styrene, 10 parts of acrylate, 5 parts of dimethyl silicone oil, 25 parts of ethylene glycol, 1 part of KH550, 0.2 part of lauroyl peroxide, 3 parts of polyether-ether-ketone powder, 15 parts of acetonitrile and 0.1 part of PEG 400;
step S2, dissolving the polyetheretherketone powder in acetonitrile, adding PEG400, stirring at a constant speed for 15min, casting to form a film, drying at 60 ℃ for 5h, cooling to room temperature, and immersing in water for taking down to obtain a polyetheretherketone film;
step S3, adding butadiene, styrene and acrylic ester into a beaker, mixing, adding ethylene glycol, magnetically stirring for 15min to obtain a mixed solution, adding the graphene oxide/silicon nitride composite particles, the simethicone and the mixed solution into deionized water, carrying out ultrasonic treatment for 2h, controlling the ultrasonic power to be 800w, and adding KH550 to obtain a membrane solution;
step S4, adding the polyether-ether-ketone film prepared in the step S2 into the film liquid prepared in the step S3, adding lauroyl peroxide, introducing nitrogen to discharge air, and reacting for 5 hours to obtain a graphene oxide/silicon nitride composite film;
step S5, drying and cutting the prepared graphene oxide/silicon nitride composite film to obtain the radiation-proof base material layer;
step two, preparing the fingerprint-proof layer:
(1) mixing polydimethylsiloxane and vinyl triamine to prepare a mixture, adding tridecafluorooctyltrimethoxysilane, pouring the mixture onto a substrate, curing the mixture for 2 hours at 90 ℃ to prepare a polydimethylsiloxane film, and controlling the weight ratio of the polydimethylsiloxane to the vinyl triamine to the tridecafluorooctyltrimethoxysilane to be 10: 1: 0.1;
(2) etching the polydimethylsiloxane film for 2min, then ultrasonically drying for 1h at 70 ℃ to obtain an anti-fingerprint film, and cutting the film to obtain the anti-fingerprint layer;
and thirdly, compounding one side of the radiation-proof base material layer and the fingerprint-proof layer through an adhesive to obtain the explosion-proof and radiation-proof double-layer composite mobile phone protective film.
The graphene oxide/silicon nitride composite particles are prepared by the following method:
(1) adding graphene into a round-bottom flask, adding sodium nitrate and 98% concentrated sulfuric acid, stirring for 15min in an ice bath at 3 ℃, adding potassium chlorate, continuously stirring for 30min, heating in a water bath at 40 ℃, reacting for 3h, adding deionized water, placing under an oil bath at 80 ℃, reacting for 30min, adding 20% aqueous hydrogen peroxide, continuously reacting for 10min, oxidizing the graphene solution, and controlling the weight ratio of the graphene, the sodium nitrate, the 98% concentrated sulfuric acid, the potassium chlorate and the 20% aqueous hydrogen peroxide to be 1: 0.5: 20: 0.1: 3;
(2) adding silicon nitride into deionized water, carrying out magnetic stirring at the rotating speed of 250r/min, adding the graphene oxide solution prepared in the step (1), continuously stirring and carrying out ultrasonic treatment for 30min, then transferring to a hydrothermal kettle, reacting at 100 ℃ for 10h, then filtering, washing a filter cake with absolute ethyl alcohol, dispersing in the absolute ethyl alcohol after washing for three times, adding oleic acid, stirring at the rotating speed of 450r/min and refluxing for 20min, cooling, centrifuging and washing to prepare the graphene oxide/silicon nitride composite particles, wherein the weight ratio of silicon nitride to graphene oxide to oleic acid is controlled to be 1: 0.2: 0.05.
Example 2
A preparation process of an explosion-proof and radiation-proof double-layer composite mobile phone protective film comprises a fingerprint-proof layer and a radiation-proof base material layer, and comprises the following steps:
firstly, preparing a radiation-proof base material layer:
step S1, weighing the following raw materials in parts by weight: 8 parts of graphene oxide/silicon nitride composite particles, 3 parts of butadiene, 12 parts of styrene, 14 parts of acrylate, 6 parts of dimethyl silicone oil, 26 parts of ethylene glycol, 3 parts of KH550, 0.4 part of lauroyl peroxide, 4 parts of polyether ether ketone powder, 18 parts of acetonitrile and 0.2 part of PEG 400;
step S2, dissolving the polyetheretherketone powder in acetonitrile, adding PEG400, stirring at a constant speed for 15min, casting to form a film, drying at 60 ℃ for 5h, cooling to room temperature, and immersing in water for taking down to obtain a polyetheretherketone film;
step S3, adding butadiene, styrene and acrylic ester into a beaker, mixing, adding ethylene glycol, magnetically stirring for 15min to obtain a mixed solution, adding the graphene oxide/silicon nitride composite particles, the simethicone and the mixed solution into deionized water, carrying out ultrasonic treatment for 2h, controlling the ultrasonic power to be 800w, and adding KH550 to obtain a membrane solution;
step S4, adding the polyether-ether-ketone film prepared in the step S2 into the film liquid prepared in the step S3, adding lauroyl peroxide, introducing nitrogen to discharge air, and reacting for 5 hours to obtain a graphene oxide/silicon nitride composite film;
step S5, drying and cutting the prepared graphene oxide/silicon nitride composite film to obtain the radiation-proof base material layer;
the following procedure was as in example 1.
Example 3
A preparation process of an explosion-proof and radiation-proof double-layer composite mobile phone protective film comprises a fingerprint-proof layer and a radiation-proof base material layer, and comprises the following steps:
firstly, preparing a radiation-proof base material layer:
step S1, weighing the following raw materials in parts by weight: 8 parts of graphene oxide/silicon nitride composite particles, 4 parts of butadiene, 14 parts of styrene, 18 parts of acrylate, 8 parts of dimethyl silicone oil, 28 parts of ethylene glycol, 4 parts of KH550, 0.6 part of lauroyl peroxide, 4 parts of polyether ether ketone powder, 22 parts of acetonitrile and 0.2 part of PEG 400;
step S2, dissolving the polyetheretherketone powder in acetonitrile, adding PEG400, stirring at a constant speed for 15min, casting to form a film, drying at 60 ℃ for 5h, cooling to room temperature, and immersing in water for taking down to obtain a polyetheretherketone film;
step S3, adding butadiene, styrene and acrylic ester into a beaker, mixing, adding ethylene glycol, magnetically stirring for 15min to obtain a mixed solution, adding the graphene oxide/silicon nitride composite particles, the simethicone and the mixed solution into deionized water, carrying out ultrasonic treatment for 2h, controlling the ultrasonic power to be 800w, and adding KH550 to obtain a membrane solution;
step S4, adding the polyether-ether-ketone film prepared in the step S2 into the film liquid prepared in the step S3, adding lauroyl peroxide, introducing nitrogen to discharge air, and reacting for 5 hours to obtain a graphene oxide/silicon nitride composite film;
step S5, drying and cutting the prepared graphene oxide/silicon nitride composite film to obtain the radiation-proof base material layer;
the following procedure was as in example 1.
Example 4
A preparation process of an explosion-proof and radiation-proof double-layer composite mobile phone protective film comprises a fingerprint-proof layer and a radiation-proof base material layer, and comprises the following steps:
firstly, preparing a radiation-proof base material layer:
step S1, weighing the following raw materials in parts by weight: 10 parts of graphene oxide/silicon nitride composite particles, 5 parts of butadiene, 15 parts of styrene, 20 parts of acrylate, 10 parts of dimethyl silicone oil, 30 parts of ethylene glycol, 5 parts of KH550, 0.8 part of lauroyl peroxide, 5 parts of polyether-ether-ketone powder, 25 parts of acetonitrile and 0.3 part of PEG 400;
step S2, dissolving the polyetheretherketone powder in acetonitrile, adding PEG400, stirring at a constant speed for 15min, casting to form a film, drying at 60 ℃ for 5h, cooling to room temperature, and immersing in water for taking down to obtain a polyetheretherketone film;
step S3, adding butadiene, styrene and acrylic ester into a beaker, mixing, adding ethylene glycol, magnetically stirring for 15min to obtain a mixed solution, adding the graphene oxide/silicon nitride composite particles, the simethicone and the mixed solution into deionized water, carrying out ultrasonic treatment for 2h, controlling the ultrasonic power to be 800w, and adding KH550 to obtain a membrane solution;
step S4, adding the polyether-ether-ketone film prepared in the step S2 into the film liquid prepared in the step S3, adding lauroyl peroxide, introducing nitrogen to discharge air, and reacting for 5 hours to obtain a graphene oxide/silicon nitride composite film;
step S5, drying and cutting the prepared graphene oxide/silicon nitride composite film to obtain the radiation-proof base material layer;
the following procedure was as in example 1.
Comparative example 1
Compared with example 1, the preparation method of the comparative example is as follows without adding the graphene oxide/silicon nitride composite particles:
firstly, preparing a radiation-proof base material layer:
step S1, weighing the following raw materials in parts by weight: 5 parts of butadiene, 15 parts of styrene, 20 parts of acrylate, 10 parts of dimethyl silicone oil, 30 parts of ethylene glycol, 5 parts of KH550, 0.8 part of lauroyl peroxide, 5 parts of polyether-ether-ketone powder, 25 parts of acetonitrile and 0.3 part of PEG 400;
step S2, dissolving the polyetheretherketone powder in acetonitrile, adding PEG400, stirring at a constant speed for 15min, casting to form a film, drying at 60 ℃ for 5h, cooling to room temperature, and immersing in water for taking down to obtain a polyetheretherketone film;
step S3, adding butadiene, styrene and acrylic ester into a beaker, mixing, adding ethylene glycol, magnetically stirring for 15min to obtain a mixed solution, adding dimethyl silicone oil and the mixed solution into deionized water, carrying out ultrasonic treatment for 2h, controlling the ultrasonic power to be 800w, and adding KH550 to obtain a membrane solution;
step S4, adding the polyether-ether-ketone film prepared in the step S2 into the film liquid prepared in the step S3, adding lauroyl peroxide, introducing nitrogen to discharge air, and reacting for 5 hours to obtain a graphene oxide/silicon nitride composite film;
step S5, drying and cutting the prepared composite film to obtain the radiation-proof base material layer;
the following procedure was as in example 1.
Comparative example 2
The comparative example is a mobile phone protective film.
The results of the performance tests performed on examples 1-4 and comparative examples 1-2 are shown in the following table:
fingerprint detection prevention: marking on the panel by using a marking pen, and then wiping and observing residual marks;
from the above table, it can be seen that the tensile strengths of examples 1-4 are 2950-2) The elongation at break is 245-; comparative examples 1-2 tensile Strength of 2120-2) In between 180-. Therefore, the polymer and the particle components can be improved by combining the polyether-ether-ketone film with the graphene oxide/silicon nitride particles to prepare the composite filmThe compatibility on the molecular level endows the graphene oxide/silicon nitride composite film with good radiation protection performance and antibacterial performance, and the graphene oxide/silicon nitride composite particles can endow the film with excellent wear resistance.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (5)
1. The preparation process of the explosion-proof and radiation-proof double-layer composite mobile phone protective film is characterized in that the protective film comprises a fingerprint-proof layer and a radiation-proof base material layer, and the preparation process of the protective film comprises the following steps:
firstly, preparing a radiation-proof base material layer:
step S1, weighing the following raw materials in parts by weight: 5-10 parts of graphene oxide/silicon nitride composite particles, 2-5 parts of butadiene, 10-15 parts of styrene, 10-20 parts of acrylate, 5-10 parts of dimethyl silicone oil, 25-30 parts of ethylene glycol, 1-5 parts of KH550, 0.2-0.8 part of lauroyl peroxide, 3-5 parts of polyether-ether-ketone powder, 15-25 parts of acetonitrile and 0.1-0.3 part of PEG 400;
step S2, dissolving the polyetheretherketone powder in acetonitrile, adding PEG400, stirring at a constant speed for 15min, casting to form a film, drying at 60 ℃ for 5h, cooling to room temperature, and immersing in water for taking down to obtain a polyetheretherketone film;
step S3, adding butadiene, styrene and acrylic ester into a beaker, mixing, adding ethylene glycol, magnetically stirring for 15min to obtain a mixed solution, adding the graphene oxide/silicon nitride composite particles, the simethicone and the mixed solution into deionized water, carrying out ultrasonic treatment for 2h, controlling the ultrasonic power to be 800w, and adding KH550 to obtain a membrane solution;
step S4, adding the polyether-ether-ketone film prepared in the step S2 into the film liquid prepared in the step S3, adding lauroyl peroxide, introducing nitrogen to discharge air, and reacting for 5 hours to obtain a graphene oxide/silicon nitride composite film;
step S5, drying and cutting the prepared graphene oxide/silicon nitride composite film to obtain the radiation-proof base material layer;
step two, preparing the fingerprint-proof layer:
(1) mixing polydimethylsiloxane and a curing agent to prepare a mixture, adding a hydrophobic material, pouring the mixture onto a substrate, and curing for 2 hours at 90 ℃ to prepare a polydimethylsiloxane film, wherein the weight ratio of the polydimethylsiloxane to the curing agent to the hydrophobic material is controlled to be 10: 1: 0.1;
(2) etching the polydimethylsiloxane film for 2min, then ultrasonically drying for 1h at 70 ℃ to obtain an anti-fingerprint film, and cutting the film to obtain the anti-fingerprint layer;
and thirdly, compounding one side of the radiation-proof base material layer and the fingerprint-proof layer through an adhesive to obtain the explosion-proof and radiation-proof double-layer composite mobile phone protective film.
2. The preparation process of the explosion-proof and radiation-proof double-layer composite mobile phone protective film according to claim 1, wherein the graphene oxide/silicon nitride composite particles are prepared by the following method:
(1) adding graphene into a round-bottom flask, adding sodium nitrate and 98% concentrated sulfuric acid, stirring for 15min in an ice bath at 3 ℃, adding potassium chlorate, continuously stirring for 30min, heating in a water bath at 40 ℃, reacting for 3h, adding deionized water, placing under an oil bath at 80 ℃, reacting for 30min, adding 20% aqueous hydrogen peroxide, continuously reacting for 10min, oxidizing the graphene solution, and controlling the weight ratio of the graphene, the sodium nitrate, the 98% concentrated sulfuric acid, the potassium chlorate and the 20% aqueous hydrogen peroxide to be 1: 0.5: 20: 0.1: 3;
(2) adding silicon nitride into deionized water, carrying out magnetic stirring at the rotating speed of 250r/min, adding the graphene oxide solution prepared in the step (1), continuously stirring and carrying out ultrasonic treatment for 30min, then transferring to a hydrothermal kettle, reacting at 100 ℃ for 10h, then filtering, washing a filter cake with absolute ethyl alcohol, dispersing in the absolute ethyl alcohol after washing for three times, adding oleic acid, stirring at the rotating speed of 450r/min and refluxing for 20min, cooling, centrifuging and washing to prepare the graphene oxide/silicon nitride composite particles, wherein the weight ratio of silicon nitride to graphene oxide to oleic acid is controlled to be 1: 0.2: 0.05.
3. The preparation process of the explosion-proof and radiation-proof double-layer composite mobile phone protective film according to claim 1, wherein the thicknesses of the radiation-proof substrate layer and the fingerprint-proof layer are 0.10-0.15 mm.
4. The process for preparing an explosion-proof and radiation-proof double-layer composite mobile phone protective film according to claim 1, wherein the adhesive in the third step is one or both of a water-based plastic-plastic composite adhesive and a pressure-sensitive adhesive.
5. The process for preparing an explosion-proof and radiation-proof double-layer composite mobile phone protective film according to claim 1, wherein in the second step, the hydrophobic material is one or more of tridecafluorooctyltrimethoxysilane, heptadecafluorodecyltriethoxysilane and dodecafluoroheptylpropyltrimethoxysilane.
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| CN203528006U (en) * | 2013-11-06 | 2014-04-09 | 尹凯 | Mobile phone screen protecting film |
| CN105694358B (en) * | 2016-04-08 | 2019-03-22 | 天津工业大学 | Sulfonated polyether-ether-ketone-sulfoxidation graphene hybridized film and preparation and application |
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