CN114702783A - Transparent glass fiber mobile phone cover plate and preparation method thereof - Google Patents

Transparent glass fiber mobile phone cover plate and preparation method thereof Download PDF

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CN114702783A
CN114702783A CN202210310218.1A CN202210310218A CN114702783A CN 114702783 A CN114702783 A CN 114702783A CN 202210310218 A CN202210310218 A CN 202210310218A CN 114702783 A CN114702783 A CN 114702783A
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glass fiber
cover plate
mobile phone
phone cover
taking
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CN114702783B (en
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张宗权
何辉春
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Huizhou Zongsheng Electronic Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00Compositions of epoxy resins; Compositions of derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/4007Curing agents not provided for by the groups C08G59/42 - C08G59/66
    • C08G59/4014Nitrogen containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular 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
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1039Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors comprising halogen-containing substituents
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular 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
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1042Copolyimides derived from at least two different tetracarboxylic compounds or two different diamino compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular 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
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1075Partially aromatic polyimides
    • C08G73/1078Partially aromatic polyimides wholly aromatic in the diamino moiety

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
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  • Reinforced Plastic Materials (AREA)
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Abstract

The invention discloses a transparent glass fiber mobile phone cover plate and a preparation method thereof. The cover plate has excellent mechanical property and water resistance, has excellent integral light transmission, and can be used as a mobile phone cover plate. The method has reasonable process design and proper component proportion, and the prepared mobile phone cover plate not only has higher mechanical property of strength, but also has excellent surface water resistance, lower water absorption and better light transmittance, can be widely applied to the fields of mobile phone cover plates, electronic product cover plates, shells and the like, and has higher practicability.

Description

Transparent glass fiber mobile phone cover plate and preparation method thereof
Technical Field
The invention relates to the technical field of glass fiber cover plates, in particular to a transparent glass fiber mobile phone cover plate and a preparation method thereof.
Background
Glass fiber (original English name: glass fiber) is an inorganic non-metallic material with excellent performance, and has the advantages of good insulativity, strong heat resistance, good corrosion resistance and high mechanical strength, but has the defects of brittleness and poor wear resistance. Glass fibers are commonly used as reinforcing materials in composite materials, electrical and thermal insulation materials, circuit substrates, and other various fields of the national economy.
At present, when a mobile phone cover plate is manufactured, epoxy resin glue is coated on two sides of continuous glass fiber cloth through a reinforcing layer, and multiple layers of epoxy resin glue are hot pressed after curing to obtain a glass fiber laminated plate.
In order to solve the technical problem, a transparent glass fiber mobile phone cover plate and a preparation method thereof are disclosed.
Disclosure of Invention
The invention aims to provide a transparent glass fiber mobile phone cover plate and a preparation method thereof, which aim to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
a preparation method of a transparent glass fiber mobile phone cover plate comprises the following steps:
(1) taking graphene oxide, bismuth trichloride and N, N-dimethylformamide, carrying out ultrasonic dispersion for 30-40 min to obtain a mixed solution, adding the mixed solution, stirring for 30-40 h at 25-30 ℃, filtering, washing and drying in vacuum to obtain aminated graphene;
taking aminated graphene and absolute ethyl alcohol, and performing ultrasonic dispersion for 30-40 min to obtain a graphene dispersion liquid; soaking the continuous glass fiber cloth into the graphene dispersion liquid, performing ultrasonic dispersion for 5-10 min, and performing vacuum drying to obtain pretreated glass fiber cloth;
(2) uniformly mixing dopamine, polyethyleneimine and Tris buffer solution, adding pretreated glass fiber cloth, depositing for 4-6h at 25-30 ℃, taking out, washing with deionized water, and drying in vacuum to obtain a pretreated substrate;
(3) taking diethylenetriamine and deionized water, and uniformly mixing to obtain a solution A; uniformly mixing heptafluorobutyric acid and deionized water, slowly dropwise adding the mixture into the solution A, stirring for reaction for 2-3 hours, and performing rotary evaporation to remove water to obtain fluorinated diethylenetriamine;
preheating 2, 2' -bis (trifluoromethyl) diaminobiphenyl and hexafluoro dianhydride at 140-150 ℃ for 20-24 hours respectively; taking preheated 2,2 ' -bis (trifluoromethyl) diaminobiphenyl and N, N-dimethylacetamide, uniformly stirring, adding hexafluoro dianhydride and dicyclohexyl-3, 4,3 ', 4' -tetracarboxylic dianhydride, introducing nitrogen, and stirring for 10-12 hours in a nitrogen environment to obtain polyamic acid;
(4) taking polyamic acid, epoxy resin and fluorinated diethylenetriamine, and uniformly mixing at 30-35 ℃ to obtain a resin glue solution;
coating resin glue solution on two sides of the pretreated substrate, heating to 100-110 ℃ at a heating rate of 5-6 ℃/min, and curing to obtain a prepreg;
and taking a plurality of layers of prepreg, performing hot-pressing compounding, cutting and shaping to obtain the cover plate.
According to an optimized scheme, in the step (1), the concentration of the graphene dispersion liquid is 0.3 g/L; the mass ratio of the continuous glass fiber cloth to the graphene dispersion liquid is 1: 8.
according to an optimized scheme, in the step (1), the mass ratio of the graphene oxide to the bismuth trichloride to the 1, 6-hexanediamine is 10: 1: 5.
in an optimized scheme, in the step (3), the molar ratio of the diethylenetriamine to the heptafluorobutyric acid is 2: 1.
according to an optimized scheme, in the resin glue solution in the step (4), the mass ratio of the epoxy resin, the polyamic acid and the fluorinated diethylenetriamine is 100: 22: 15.
according to an optimized scheme, in the step (4), the pretreatment matrix accounts for 45-50 wt% of the mass of the prepreg.
In a more optimized scheme, in the step (3), the molar ratio of the 2, 2' -bis (trifluoromethyl) diaminobiphenyl to the hexafluoro dianhydride is 1: 1, the molar ratio of the dicyclohexyl-3, 4,3 ', 4' -tetracarboxylic dianhydride to the hexafluoro dianhydride is 1: 20.
according to an optimized scheme, the mobile phone cover plate is prepared by the preparation method of the transparent glass fiber mobile phone cover plate.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a transparent glass fiber mobile phone cover plate and a preparation method thereof. The cover plate has excellent mechanical property and water resistance, has excellent integral light transmission, and can be used as a mobile phone cover plate.
This application at first carries out the preliminary treatment to continuous glass fiber cloth, carries out amination to graphite alkene earlier, again with its load to the glass fiber surface, its aim at: on one hand, the graphene oxide is loaded on the surface of the continuous glass fiber cloth, so that the continuous glass fiber cloth can be enhanced, the mechanical property of the continuous glass fiber cloth is improved, and the strength and the mechanical property of a subsequent mobile phone cover plate are enhanced; on the other hand, the load of the graphene oxide can also enhance the adhesive force between the continuous glass fiber cloth and the subsequent polydopamine layer.
On the basis of the scheme, 1, 6-hexamethylene diamine is selected during the amination treatment of the graphene oxide, and the proper alkyl chain length aliphatic diamine is selected during the grafting, so that the dispersibility of the graphene on the surface of the glass fiber cloth can be improved, but when the alkyl chain length is too long, the deposition and the attachment of the polydopamine are influenced, so that the 1, 6-hexamethylene diamine is selected as the most preferable scheme in the alkyl aliphatic diamine.
After the continuous glass fiber cloth is pretreated, the continuous glass fiber cloth is immersed in a mixed solution of dopamine, polyethyleneimine and Tris buffer solution for autopolymerization and deposition, the amount of each component is limited, and the deposition time is 4-6h, so that: in the scheme, the transparency and the light transmittance of the mobile phone cover plate need to be ensured, and the color of the mobile phone cover plate can influence the light transmittance of a product as the polymerization time of dopamine is increased; the deposition time is too short, the polydopamine layer is used as a connecting transition layer between the resin glue layer and the continuous glass fiber cloth, and the effect of improving the adhesive force between the resin glue layer and the continuous glass fiber cloth is reduced; therefore, the scheme limits the amount of each component and ensures that the deposition time is 4-6h, so as to ensure that the effective adhesion between the continuous glass fiber cloth and the resin glue solution can be realized, and the light transmittance of the transparent cover plate can be ensured.
Meanwhile, the scheme also limits the components of the resin glue solution, the scheme takes the mixture of the fluorinated diethylenetriamine and the polyamide acid as the curing agent, and the mixture is added into the epoxy resin to form the resin glue solution, and the technical effect realized by the step is as follows: on one hand, fluorine groups are introduced in the adjustment of the curing agent, so that the water resistance of the epoxy resin can be improved, and the water absorption rate is reduced; on the other hand, the polyamic acid is prepared from 2,2 ' -bis (trifluoromethyl) diaminobiphenyl, hexafluoro dianhydride and dicyclohexyl-3, 4,3 ', 4' -tetracarboxylic dianhydride which are used as raw materials to prepare a product containing a fluorine group and a biphenyl six-membered ring structure.
The invention discloses a transparent glass fiber mobile phone cover plate and a preparation method thereof, the process design is reasonable, the component proportion is proper, the prepared mobile phone cover plate not only has higher mechanical property of strength, but also has excellent surface water resistance, lower water absorption and better light transmittance, can be widely applied to the fields of mobile phone cover plates, electronic product cover plates, shells and the like, and has higher practicability.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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 method of a transparent glass fiber mobile phone cover plate comprises the following steps:
(1) taking graphene oxide, bismuth trichloride and N, N-dimethylformamide, and carrying out ultrasonic dispersion for 30min to obtain a mixed solution, wherein the concentration of the graphene oxide in the mixed solution is 0.1 g/mL; adding 1, 6-hexanediamine, stirring for 40h at 25 ℃, filtering, washing, and drying in vacuum to obtain aminated graphene; the mass ratio of the graphene oxide to the bismuth trichloride to the 1, 6-hexanediamine is 10: 1: 5.
taking aminated graphene and absolute ethyl alcohol, and performing ultrasonic dispersion for 30min to obtain a graphene dispersion liquid; the concentration of the graphene dispersion liquid is 0.3 g/L; soaking continuous glass fiber cloth into the graphene dispersion liquid, performing ultrasonic dispersion for 5min, wherein the ultrasonic power is 600W, and performing vacuum drying to obtain pretreated glass fiber cloth; the mass ratio of the continuous glass fiber cloth to the graphene dispersion liquid is 1: 8.
(2) uniformly mixing dopamine, polyethyleneimine and Tris buffer solution to obtain a mixed solution; adding pretreated glass fiber cloth, depositing for 6h at 25 ℃, taking out, washing with deionized water, and drying in vacuum to obtain a pretreated matrix; the weight ratio of the pretreated glass fiber cloth to the mixed solution is 1: 10; the concentration of dopamine in the mixed solution is 2mg/mL, and the concentration of polyethyleneimine in the mixed solution is 2 mg/mL.
(3) Taking diethylenetriamine and deionized water, and uniformly mixing to obtain a solution A; uniformly mixing heptafluorobutyric acid and deionized water, slowly dripping into the solution A, stirring for reaction for 2 hours, and performing rotary evaporation to remove water to obtain fluorinated diethylenetriamine;
the molar ratio of the diethylenetriamine to the heptafluorobutyric acid is 2: 1.
preheating 2,2 '-bis (trifluoromethyl) diaminobiphenyl and hexafluoro-dianhydride at 140 ℃ for 24 hours respectively, uniformly stirring the preheated 2, 2' -bis (trifluoromethyl) diaminobiphenyl and N, N-dimethylacetamide at the rotating speed of 300r/min, adding hexafluoro-dianhydride and dicyclohexyl-3, 4,3 ', 4' -tetracarboxylic dianhydride, introducing nitrogen, and stirring for 10 hours in a nitrogen environment to obtain polyamic acid;
the molar ratio of the 2, 2' -bis (trifluoromethyl) diaminobiphenyl to the hexafluorodianhydride is 1: 1, the molar ratio of the dicyclohexyl-3, 4,3 ', 4' -tetracarboxylic dianhydride to the hexafluoro dianhydride is 1: 20.
(4) taking polyamic acid, epoxy resin and fluorinated diethylenetriamine, and uniformly mixing at 30 ℃ to obtain a resin glue solution; the mass ratio of the epoxy resin to the polyamic acid to the fluorinated diethylenetriamine is 100: 22: 15.
coating resin glue solution on two sides of the pretreated substrate, heating to 100 ℃ at a heating rate of 5 ℃/min, and curing to obtain a prepreg; the pretreatment matrix accounts for 50 wt% of the mass of the prepreg.
And taking the three layers of prepregs, performing hot-press compounding, cutting and shaping to obtain the cover plate.
Example 2:
a preparation method of a transparent glass fiber mobile phone cover plate comprises the following steps:
(1) taking graphene oxide, bismuth trichloride and N, N-dimethylformamide, and carrying out ultrasonic dispersion for 35min to obtain a mixed solution, wherein the concentration of the graphene oxide in the mixed solution is 0.1 g/mL; adding 1, 6-hexanediamine, stirring for 35h at 28 ℃, filtering, washing, and drying in vacuum to obtain aminated graphene; the mass ratio of the graphene oxide to the bismuth trichloride to the 1, 6-hexanediamine is 10: 1: 5.
taking aminated graphene and absolute ethyl alcohol, and performing ultrasonic dispersion for 35min to obtain a graphene dispersion liquid; the concentration of the graphene dispersion liquid is 0.3 g/L; soaking continuous glass fiber cloth into the graphene dispersion liquid, performing ultrasonic dispersion for 8min, wherein the ultrasonic power is 600W, and performing vacuum drying to obtain pretreated glass fiber cloth; the mass ratio of the continuous glass fiber cloth to the graphene dispersion liquid is 1: 8.
(2) uniformly mixing dopamine, polyethyleneimine and Tris buffer solution to obtain a mixed solution; adding pretreated glass fiber cloth, depositing for 5h at 28 ℃, taking out, washing with deionized water, and drying in vacuum to obtain a pretreated matrix; the weight ratio of the pretreated glass fiber cloth to the mixed solution is 1: 10; the concentration of dopamine in the mixed solution is 2mg/mL, and the concentration of polyethyleneimine in the mixed solution is 2 mg/mL.
(3) Taking diethylenetriamine and deionized water, and uniformly mixing to obtain a solution A; uniformly mixing heptafluorobutyric acid and deionized water, slowly dripping into the solution A, stirring for reaction for 2-3h, and removing water by rotary evaporation to obtain fluorinated diethylenetriamine;
the molar ratio of the diethylenetriamine to the heptafluorobutyric acid is 2: 1.
preheating 2,2 '-bis (trifluoromethyl) diaminobiphenyl and hexafluoro-dianhydride at 145 ℃ for 22 hours respectively, uniformly stirring the preheated 2, 2' -bis (trifluoromethyl) diaminobiphenyl and N, N-dimethylacetamide at the rotating speed of 350r/min, adding hexafluoro-dianhydride and dicyclohexyl-3, 4,3 ', 4' -tetracarboxylic dianhydride, introducing nitrogen, and stirring for 11 hours in a nitrogen environment to obtain polyamic acid;
the molar ratio of the 2, 2' -bis (trifluoromethyl) diaminobiphenyl to the hexafluorodianhydride is 1: 1, the molar ratio of the dicyclohexyl-3, 4,3 ', 4' -tetracarboxylic dianhydride to the hexafluoro dianhydride is 1: 20.
(4) taking polyamic acid, epoxy resin and fluorinated diethylenetriamine, and uniformly mixing at 32 ℃ to obtain a resin glue solution; the mass ratio of the epoxy resin to the polyamic acid to the fluorinated diethylenetriamine is 100: 22: 15.
coating resin glue solution on two sides of the pretreated substrate, heating to 105 ℃ at a heating rate of 5 ℃/min, and curing to obtain a prepreg; the pretreatment matrix accounts for 50 wt% of the mass of the prepreg.
And taking the three layers of prepregs, performing hot-pressing compounding, and cutting and shaping to obtain the cover plate.
Example 3:
a preparation method of a transparent glass fiber mobile phone cover plate comprises the following steps:
(1) taking graphene oxide, bismuth trichloride and N, N-dimethylformamide, and carrying out ultrasonic dispersion for 40min to obtain a mixed solution, wherein the concentration of the graphene oxide in the mixed solution is 0.1 g/mL; adding 1, 6-hexanediamine, stirring for 30h at 30 ℃, filtering, washing, and drying in vacuum to obtain aminated graphene; the mass ratio of the graphene oxide to the bismuth trichloride to the 1, 6-hexanediamine is 10: 1: 5.
taking aminated graphene and absolute ethyl alcohol, and performing ultrasonic dispersion for 40min to obtain a graphene dispersion liquid; the concentration of the graphene dispersion liquid is 0.3 g/L; soaking continuous glass fiber cloth into the graphene dispersion liquid, performing ultrasonic dispersion for 10min, wherein the ultrasonic power is 600W, and performing vacuum drying to obtain pretreated glass fiber cloth; the mass ratio of the continuous glass fiber cloth to the graphene dispersion liquid is 1: 8.
(2) uniformly mixing dopamine, polyethyleneimine and Tris buffer solution to obtain a mixed solution; adding pretreated glass fiber cloth, depositing for 4h at 30 ℃, taking out, washing with deionized water, and drying in vacuum to obtain a pretreated matrix; the weight ratio of the pretreated glass fiber cloth to the mixed solution is 1: 10; the concentration of dopamine in the mixed solution is 2mg/mL, and the concentration of polyethyleneimine in the mixed solution is 2 mg/mL.
(3) Taking diethylenetriamine and deionized water, and uniformly mixing to obtain a solution A; uniformly mixing heptafluorobutyric acid and deionized water, slowly dripping into the solution A, stirring for reaction for 3 hours, and performing rotary evaporation to remove water to obtain fluorinated diethylenetriamine;
the molar ratio of the diethylenetriamine to the heptafluorobutyric acid is 2: 1.
preheating 2,2 '-bis (trifluoromethyl) diaminobiphenyl and hexafluoro dianhydride at 150 ℃ for 20 hours respectively, uniformly stirring the preheated 2, 2' -bis (trifluoromethyl) diaminobiphenyl and N, N-dimethylacetamide at the rotating speed of 400r/min, adding hexafluoro dianhydride and dicyclohexyl-3, 4,3 ', 4' -tetracarboxylic dianhydride, introducing nitrogen, and stirring for 12 hours in a nitrogen environment to obtain polyamic acid;
the molar ratio of the 2, 2' -bis (trifluoromethyl) diaminobiphenyl to the hexafluorodianhydride is 1: 1, the molar ratio of the dicyclohexyl-3, 4,3 ', 4' -tetracarboxylic dianhydride to the hexafluoro dianhydride is 1: 20.
(4) taking polyamic acid, epoxy resin and fluorinated diethylenetriamine, and uniformly mixing at 35 ℃ to obtain a resin glue solution; the mass ratio of the epoxy resin to the polyamic acid to the fluorinated diethylenetriamine is 100: 22: 15.
coating resin glue solution on two sides of the pretreated substrate, heating to 110 ℃ at a heating rate of 5 ℃/min, and curing to obtain a prepreg; the pretreatment matrix accounts for 50 wt% of the mass of the prepreg.
And taking the three layers of prepregs, performing hot-pressing compounding, and cutting and shaping to obtain the cover plate.
Comparative example 1: in the comparative example 1, in which a control experiment was carried out on the basis of example 3, fluorinated diethylenetriamine was not introduced, and the rest of the procedure was identical.
A preparation method of a transparent glass fiber mobile phone cover plate comprises the following steps:
(1) taking graphene oxide, bismuth trichloride and N, N-dimethylformamide, and carrying out ultrasonic dispersion for 40min to obtain a mixed solution, wherein the concentration of the graphene oxide in the mixed solution is 0.1 g/mL; adding 1, 6-hexanediamine, stirring for 30h at 30 ℃, filtering, washing, and drying in vacuum to obtain aminated graphene; the mass ratio of the graphene oxide to the bismuth trichloride to the 1, 6-hexanediamine is 10: 1: 5.
taking aminated graphene and absolute ethyl alcohol, and performing ultrasonic dispersion for 40min to obtain a graphene dispersion liquid; the concentration of the graphene dispersion liquid is 0.3 g/L; soaking continuous glass fiber cloth into the graphene dispersion liquid, performing ultrasonic dispersion for 10min, wherein the ultrasonic power is 600W, and performing vacuum drying to obtain pretreated glass fiber cloth; the mass ratio of the continuous glass fiber cloth to the graphene dispersion liquid is 1: 8.
(2) uniformly mixing dopamine, polyethyleneimine and Tris buffer solution to obtain a mixed solution; adding pretreated glass fiber cloth, depositing for 4h at 30 ℃, taking out, washing with deionized water, and drying in vacuum to obtain a pretreated matrix; the weight ratio of the pretreated glass fiber cloth to the mixed solution is 1: 10; the concentration of dopamine in the mixed solution is 2mg/mL, and the concentration of polyethyleneimine in the mixed solution is 2 mg/mL.
(3) Preheating 2,2 '-bis (trifluoromethyl) diaminobiphenyl and hexafluoro dianhydride at 150 ℃ for 20 hours respectively, uniformly stirring the preheated 2, 2' -bis (trifluoromethyl) diaminobiphenyl and N, N-dimethylacetamide at the rotating speed of 400r/min, adding hexafluoro dianhydride and dicyclohexyl-3, 4,3 ', 4' -tetracarboxylic dianhydride, introducing nitrogen, and stirring for 12 hours in a nitrogen environment to obtain polyamic acid;
the molar ratio of the 2, 2' -bis (trifluoromethyl) diaminobiphenyl to the hexafluoro dianhydride is 1: 1, the molar ratio of the dicyclohexyl-3, 4,3 ', 4' -tetracarboxylic dianhydride to the hexafluoro dianhydride is 1: 20.
(4) taking polyamide acid and epoxy resin, and uniformly mixing at 35 ℃ to obtain a resin glue solution; the mass ratio of the epoxy resin to the polyamic acid is 100: 37.
coating resin glue solution on two sides of the pretreated substrate, heating to 110 ℃ at a heating rate of 5 ℃/min, and curing to obtain a prepreg; the pretreatment matrix accounts for 50 wt% of the mass of the prepreg.
And taking the three layers of prepregs, performing hot-pressing compounding, and cutting and shaping to obtain the cover plate.
Comparative example 2: in comparative example 2, in which a control experiment was performed on the basis of example 3, fluorinated diethylenetriamine and polyamic acid were not introduced, only 4,4' -diaminodiphenylsulfone was added, and the remaining steps were identical.
A preparation method of a transparent glass fiber mobile phone cover plate comprises the following steps:
(1) taking graphene oxide, bismuth trichloride and N, N-dimethylformamide, and performing ultrasonic dispersion for 40min to obtain a mixed solution, wherein the concentration of the graphene oxide in the mixed solution is 0.1 g/mL; adding 1, 6-hexanediamine, stirring for 30 hours at 30 ℃, filtering, washing, and drying in vacuum to obtain aminated graphene; the mass ratio of the graphene oxide to the bismuth trichloride to the 1, 6-hexanediamine is 10: 1: 5.
taking aminated graphene and absolute ethyl alcohol, and performing ultrasonic dispersion for 40min to obtain a graphene dispersion liquid; the concentration of the graphene dispersion liquid is 0.3 g/L; soaking continuous glass fiber cloth into the graphene dispersion liquid, performing ultrasonic dispersion for 10min, wherein the ultrasonic power is 600W, and performing vacuum drying to obtain pretreated glass fiber cloth; the mass ratio of the continuous glass fiber cloth to the graphene dispersion liquid is 1: 8.
(2) uniformly mixing dopamine, polyethyleneimine and Tris buffer solution to obtain a mixed solution; adding pretreated glass fiber cloth, depositing at 30 ℃ for 4h, taking out, washing with deionized water, and vacuum drying to obtain a pretreated matrix; the weight ratio of the pretreated glass fiber cloth to the mixed solution is 1: 10; the concentration of dopamine in the mixed solution is 2mg/mL, and the concentration of polyethyleneimine in the mixed solution is 2 mg/mL.
(3) Uniformly mixing 4,4' -diamino diphenyl sulfone and epoxy resin at 35 ℃ to obtain a resin glue solution; the mass ratio of the epoxy resin to the 4,4' -diamino diphenyl sulfone is 100: 15.
coating resin glue solution on two sides of the pretreated substrate, heating to 110 ℃ at a heating rate of 5 ℃/min, and curing to obtain a prepreg; the pretreatment matrix accounts for 50 wt% of the mass of the prepreg.
And taking the three layers of prepregs, performing hot-pressing compounding, and cutting and shaping to obtain the cover plate.
Comparative example 3: a control experiment was performed on the basis of example 3, with a polydopamine deposition time of 8h in comparative example 3.
A preparation method of a transparent glass fiber mobile phone cover plate comprises the following steps:
(1) taking graphene oxide, bismuth trichloride and N, N-dimethylformamide, and carrying out ultrasonic dispersion for 40min to obtain a mixed solution, wherein the concentration of the graphene oxide in the mixed solution is 0.1 g/mL; adding 1, 6-hexanediamine, stirring for 30h at 30 ℃, filtering, washing, and drying in vacuum to obtain aminated graphene; the mass ratio of the graphene oxide to the bismuth trichloride to the 1, 6-hexanediamine is 10: 1: 5.
taking aminated graphene and absolute ethyl alcohol, and performing ultrasonic dispersion for 40min to obtain a graphene dispersion liquid; the concentration of the graphene dispersion liquid is 0.3 g/L; soaking continuous glass fiber cloth into the graphene dispersion liquid, performing ultrasonic dispersion for 10min, wherein the ultrasonic power is 600W, and performing vacuum drying to obtain pretreated glass fiber cloth; the mass ratio of the continuous glass fiber cloth to the graphene dispersion liquid is 1: 8.
(2) uniformly mixing dopamine, polyethyleneimine and Tris buffer solution to obtain a mixed solution; adding pretreated glass fiber cloth, precipitating for 8h at 30 ℃, taking out, washing with deionized water, and vacuum drying to obtain a pretreated matrix; the weight ratio of the pretreated glass fiber cloth to the mixed solution is 1: 10; the concentration of dopamine in the mixed solution is 2mg/mL, and the concentration of polyethyleneimine in the mixed solution is 2 mg/mL.
(3) Taking diethylenetriamine and deionized water, and uniformly mixing to obtain a solution A; uniformly mixing heptafluorobutyric acid and deionized water, slowly dripping into the solution A, stirring for reaction for 3 hours, and performing rotary evaporation to remove water to obtain fluorinated diethylenetriamine;
the molar ratio of the diethylenetriamine to the heptafluorobutyric acid is 2: 1.
preheating 2,2 '-bis (trifluoromethyl) diaminobiphenyl and hexafluoro dianhydride at 150 ℃ for 20 hours respectively, uniformly stirring the preheated 2, 2' -bis (trifluoromethyl) diaminobiphenyl and N, N-dimethylacetamide at the rotating speed of 400r/min, adding hexafluoro dianhydride and dicyclohexyl-3, 4,3 ', 4' -tetracarboxylic dianhydride, introducing nitrogen, and stirring for 12 hours in a nitrogen environment to obtain polyamic acid;
the molar ratio of the 2, 2' -bis (trifluoromethyl) diaminobiphenyl to the hexafluorodianhydride is 1: 1, the molar ratio of dicyclohexyl-3, 4,3 ', 4' -tetracarboxylic dianhydride to hexafluoro dianhydride is 1: 20.
(4) taking polyamic acid, epoxy resin and fluorinated diethylenetriamine, and uniformly mixing at 35 ℃ to obtain a resin glue solution; the mass ratio of the epoxy resin to the polyamic acid to the fluorinated diethylenetriamine is 100: 22: 15.
coating resin glue solution on two sides of the pretreated substrate, heating to 110 ℃ at a heating rate of 5 ℃/min, and curing to obtain a prepreg; the pretreatment matrix accounts for 50 wt% of the mass of the prepreg.
And taking the three layers of prepregs, performing hot-pressing compounding, and cutting and shaping to obtain the cover plate.
Comparative example 4: a control experiment was performed on the basis of example 3, with a polydopamine deposition time of 10h in comparative example 4.
Comparative example 5: a control experiment was performed on the basis of example 3, and comparative example 5 did not pretreat the surface of the glass fibers.
A preparation method of a transparent glass fiber mobile phone cover plate comprises the following steps:
(1) uniformly mixing dopamine, polyethyleneimine and Tris buffer solution to obtain a mixed solution; adding continuous glass fiber cloth, depositing for 4h at 30 ℃, taking out, washing with deionized water, and drying in vacuum to obtain a pretreated substrate; the weight ratio of the pretreated glass fiber cloth to the mixed solution is 1: 10; the concentration of dopamine in the mixed solution is 2mg/mL, and the concentration of polyethyleneimine in the mixed solution is 2 mg/mL.
(2) Taking diethylenetriamine and deionized water, and uniformly mixing to obtain a solution A; uniformly mixing heptafluorobutyric acid and deionized water, slowly dripping into the solution A, stirring for reaction for 3 hours, and performing rotary evaporation to remove water to obtain fluorinated diethylenetriamine;
the molar ratio of the diethylenetriamine to the heptafluorobutyric acid is 2: 1.
preheating 2,2 '-bis (trifluoromethyl) diaminobiphenyl and hexafluoro dianhydride at 150 ℃ for 20 hours respectively, uniformly stirring the preheated 2, 2' -bis (trifluoromethyl) diaminobiphenyl and N, N-dimethylacetamide at the rotating speed of 400r/min, adding hexafluoro dianhydride and dicyclohexyl-3, 4,3 ', 4' -tetracarboxylic dianhydride, introducing nitrogen, and stirring for 12 hours in a nitrogen environment to obtain polyamic acid;
the molar ratio of the 2, 2' -bis (trifluoromethyl) diaminobiphenyl to the hexafluoro dianhydride is 1: 1, the molar ratio of dicyclohexyl-3, 4,3 ', 4' -tetracarboxylic dianhydride to hexafluoro dianhydride is 1: 20.
(3) taking polyamic acid, epoxy resin and fluorinated diethylenetriamine, and uniformly mixing at 35 ℃ to obtain a resin glue solution; the mass ratio of the epoxy resin to the polyamic acid to the fluorinated diethylenetriamine is 100: 22: 15.
coating resin glue solution on two sides of the pretreated substrate, heating to 110 ℃ at a heating rate of 5 ℃/min, and curing to obtain a prepreg; the pretreatment matrix accounts for 50 wt% of the mass of the prepreg.
And taking the three layers of prepregs, performing hot-pressing compounding, and cutting and shaping to obtain the cover plate.
Comparative example 6: a control experiment was carried out on the basis of example 3, comparative example 6 incorporating 1, 12-diaminododecane.
A preparation method of a transparent glass fiber mobile phone cover plate comprises the following steps:
(1) taking graphene oxide, bismuth trichloride and N, N-dimethylformamide, and carrying out ultrasonic dispersion for 40min to obtain a mixed solution, wherein the concentration of the graphene oxide in the mixed solution is 0.1 g/mL; adding 1, 12-diaminododecane, stirring at 30 ℃ for 30 hours, filtering, washing, and drying in vacuum to obtain aminated graphene; the mass ratio of the graphene oxide to the bismuth trichloride to the 1, 12-diaminododecane is 10: 1: 5.
taking aminated graphene and absolute ethyl alcohol, and performing ultrasonic dispersion for 40min to obtain a graphene dispersion liquid; the concentration of the graphene dispersion liquid is 0.3 g/L; soaking continuous glass fiber cloth into the graphene dispersion liquid, performing ultrasonic dispersion for 10min, wherein the ultrasonic power is 600W, and performing vacuum drying to obtain pretreated glass fiber cloth; the mass ratio of the continuous glass fiber cloth to the graphene dispersion liquid is 1: 8.
(2) uniformly mixing dopamine, polyethyleneimine and Tris buffer solution to obtain a mixed solution; adding pretreated glass fiber cloth, depositing for 4h at 30 ℃, taking out, washing with deionized water, and drying in vacuum to obtain a pretreated matrix; the weight ratio of the pretreated glass fiber cloth to the mixed solution is 1: 10; the concentration of dopamine in the mixed solution is 2mg/mL, and the concentration of polyethyleneimine in the mixed solution is 2 mg/mL.
(3) Taking diethylenetriamine and deionized water, and uniformly mixing to obtain a solution A; uniformly mixing heptafluorobutyric acid and deionized water, slowly dripping into the solution A, stirring for reaction for 3 hours, and performing rotary evaporation to remove water to obtain fluorinated diethylenetriamine;
the molar ratio of the diethylenetriamine to the heptafluorobutyric acid is 2: 1.
preheating 2,2 '-bis (trifluoromethyl) diaminobiphenyl and hexafluoro dianhydride at 150 ℃ for 20 hours respectively, uniformly stirring the preheated 2, 2' -bis (trifluoromethyl) diaminobiphenyl and N, N-dimethylacetamide at the rotating speed of 400r/min, adding hexafluoro dianhydride and dicyclohexyl-3, 4,3 ', 4' -tetracarboxylic dianhydride, introducing nitrogen, and stirring for 12 hours in a nitrogen environment to obtain polyamic acid;
the molar ratio of the 2, 2' -bis (trifluoromethyl) diaminobiphenyl to the hexafluorodianhydride is 1: 1, the molar ratio of the dicyclohexyl-3, 4,3 ', 4' -tetracarboxylic dianhydride to the hexafluoro dianhydride is 1: 20.
(4) taking polyamic acid, epoxy resin and fluorinated diethylenetriamine, and uniformly mixing at 35 ℃ to obtain a resin glue solution; the mass ratio of the epoxy resin to the polyamic acid to the fluorinated diethylenetriamine is 100: 22: 15.
coating resin glue solution on two sides of the pretreated substrate, heating to 110 ℃ at a heating rate of 5 ℃/min, and curing to obtain a prepreg; the pretreatment matrix accounts for 50 wt% of the mass of the prepreg.
And taking the three layers of prepregs, performing hot-pressing compounding, and cutting and shaping to obtain the cover plate.
In the above examples, the continuous glass fiber cloth was E-grade glass fiber cloth with an areal density of 1200g/m2. The graphene oxide sheet diameter was 3 μm.
And (3) detection test:
1. the cover plates prepared in examples 1 to 3 and comparative examples 1 to 6 were weighed, and then soaked in distilled water at 25 ℃ for 24 hours, and after taking out, the surface moisture was absorbed by absorbent paper, and the weight was weighed and compared with the weight before the test to calculate the water absorption rate.
2. The cover plates prepared in examples 1-3 and comparative examples 1-6 were tested for tensile strength according to GB/T1447-. The product size is 2mm × 25mm × 150 mm.
3. The cover plates prepared in examples 1-3 and comparative examples 1-6 were subjected to a transmittance test using an ultraviolet-visible spectrophotometer.
Item Tensile Strength (MPa) 30d tensile Strength (MPa) 24h Water absorption (%) Light transmittance (%)
Example 1 749 736 0.17% >90%
Example 2 752 739 0.17% >90%
Example 3 757 745 0.15% >90%
Comparative example 1 751 742 0.55% /
Comparative example 2 721 713 1.21% /
Comparative example 3 756 748 0.16% 79%
Comparative example 4 759 749 0.14% 72%
Comparative example 5 624 612 0.20% /
Comparative example 6 742 735 0.8% /
And (4) conclusion: the invention discloses a transparent glass fiber mobile phone cover plate and a preparation method thereof, the process design is reasonable, the component proportion is proper, the prepared mobile phone cover plate not only has higher mechanical property of strength, but also has excellent surface water resistance, lower water absorption rate and better light transmittance, can be widely applied to the fields of mobile phone cover plates, electronic product cover plates, shells and the like, and has higher practicability.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (8)

1. A preparation method of a transparent glass fiber mobile phone cover plate is characterized by comprising the following steps: the method comprises the following steps:
(1) taking graphene oxide, bismuth trichloride and N, N-dimethylformamide, carrying out ultrasonic dispersion for 30-40 min to obtain a mixed solution, adding 1, 6-hexanediamine, stirring for 30-40 h at 25-30 ℃, filtering, washing, and carrying out vacuum drying to obtain aminated graphene;
taking aminated graphene and absolute ethyl alcohol, and performing ultrasonic dispersion for 30-40 min to obtain a graphene dispersion liquid; soaking continuous glass fiber cloth into the graphene dispersion liquid, performing ultrasonic dispersion for 5-10 min, and performing vacuum drying to obtain pretreated glass fiber cloth;
(2) uniformly mixing dopamine, polyethyleneimine and Tris buffer solution, adding pretreated glass fiber cloth, depositing for 4-6h at 25-30 ℃, taking out, washing with deionized water, and drying in vacuum to obtain a pretreated substrate;
(3) taking diethylenetriamine and deionized water, and uniformly mixing to obtain a solution A; uniformly mixing heptafluorobutyric acid and deionized water, slowly dripping into the solution A, stirring for reaction for 2-3h, and removing water by rotary evaporation to obtain fluorinated diethylenetriamine;
preheating 2,2 '-bis (trifluoromethyl) diaminobiphenyl and hexafluoro-dianhydride at 140-150 ℃ for 20-24 hours respectively, uniformly stirring the preheated 2, 2' -bis (trifluoromethyl) diaminobiphenyl and N, N-dimethylacetamide, adding hexafluoro-dianhydride and dicyclohexyl-3, 4,3 ', 4' -tetracarboxylic dianhydride, introducing nitrogen, and stirring for 10-12 hours in a nitrogen environment to obtain polyamic acid;
(4) taking polyamic acid, epoxy resin and fluorinated diethylenetriamine, and uniformly mixing at 30-35 ℃ to obtain a resin glue solution;
coating resin glue solution on two sides of the pretreated substrate, heating to 100-110 ℃ at a heating rate of 5-6 ℃/min, and curing to obtain a prepreg;
and taking a plurality of layers of prepreg, performing hot-pressing compounding, cutting and shaping to obtain the cover plate.
2. The method for preparing a transparent glass fiber mobile phone cover plate according to claim 1, wherein the method comprises the following steps: in the step (1), the concentration of the graphene dispersion liquid is 0.3 g/L; the mass ratio of the continuous glass fiber cloth to the graphene dispersion liquid is 1: 8.
3. the method for preparing a transparent glass fiber mobile phone cover plate according to claim 1, wherein the method comprises the following steps: in the step (1), the mass ratio of the graphene oxide to the bismuth trichloride to the 1, 6-hexanediamine is 10: 1: 5.
4. the method for preparing a transparent glass fiber mobile phone cover plate according to claim 1, wherein the method comprises the following steps: in the step (3), the molar ratio of diethylenetriamine to heptafluorobutyric acid is 2: 1.
5. the method for preparing a transparent glass fiber mobile phone cover plate according to claim 1, wherein the method comprises the following steps: in the resin glue solution in the step (4), the mass ratio of the epoxy resin, the polyamic acid and the fluorinated diethylenetriamine is 100: 22: 15.
6. the method for preparing a transparent glass fiber mobile phone cover plate according to claim 1, wherein the method comprises the following steps: in the step (4), the pretreatment matrix accounts for 45-50 wt% of the mass of the prepreg.
7. The method for preparing a transparent glass fiber mobile phone cover plate according to claim 1, wherein the method comprises the following steps: in the step (3), the molar ratio of the 2, 2' -bis (trifluoromethyl) diaminobiphenyl to the hexafluoro dianhydride is 1: 1, the molar ratio of the dicyclohexyl-3, 4,3 ', 4' -tetracarboxylic dianhydride to the hexafluoro dianhydride is 1: 20.
8. the mobile phone cover plate prepared by the preparation method of the transparent glass fiber mobile phone cover plate according to any one of claims 1 to 7.
CN202210310218.1A 2022-03-28 2022-03-28 Transparent glass fiber mobile phone cover plate and preparation method thereof Active CN114702783B (en)

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Publication number Priority date Publication date Assignee Title
CN117153470A (en) * 2023-08-29 2023-12-01 江苏荣宜电缆有限公司 Waterproof anti-aging photovoltaic cable and preparation method thereof

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CN106521687A (en) * 2016-11-10 2017-03-22 过冬 Preparation method of amination graphene oxide reinforced fibers
CN113801354A (en) * 2021-10-07 2021-12-17 惠州市纵胜电子材料有限公司 High-temperature-resistant transparent glass fiber insulating plate and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106521687A (en) * 2016-11-10 2017-03-22 过冬 Preparation method of amination graphene oxide reinforced fibers
CN113801354A (en) * 2021-10-07 2021-12-17 惠州市纵胜电子材料有限公司 High-temperature-resistant transparent glass fiber insulating plate and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117153470A (en) * 2023-08-29 2023-12-01 江苏荣宜电缆有限公司 Waterproof anti-aging photovoltaic cable and preparation method thereof

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