CN114702783B - 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 PDFInfo
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- CN114702783B CN114702783B CN202210310218.1A CN202210310218A CN114702783B CN 114702783 B CN114702783 B CN 114702783B CN 202210310218 A CN202210310218 A CN 202210310218A CN 114702783 B CN114702783 B CN 114702783B
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- 239000003365 glass fiber Substances 0.000 title claims abstract description 93
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- 238000000034 method Methods 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 85
- 229910021389 graphene Inorganic materials 0.000 claims description 67
- 239000004744 fabric Substances 0.000 claims description 59
- 239000000243 solution Substances 0.000 claims description 53
- 239000011259 mixed solution Substances 0.000 claims description 50
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims description 40
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 36
- 239000006185 dispersion Substances 0.000 claims description 36
- 239000007788 liquid Substances 0.000 claims description 36
- 238000002156 mixing Methods 0.000 claims description 36
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 34
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 33
- 229920005989 resin Polymers 0.000 claims description 29
- 239000011347 resin Substances 0.000 claims description 29
- ZPSUIVIDQHHIFH-UHFFFAOYSA-N 3-(trifluoromethyl)-4-[2-(trifluoromethyl)phenyl]benzene-1,2-diamine Chemical group FC(F)(F)C1=C(N)C(N)=CC=C1C1=CC=CC=C1C(F)(F)F ZPSUIVIDQHHIFH-UHFFFAOYSA-N 0.000 claims description 28
- 239000003292 glue Substances 0.000 claims description 28
- 238000001291 vacuum drying Methods 0.000 claims description 28
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 27
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 27
- 239000008367 deionised water Substances 0.000 claims description 26
- 229910021641 deionized water Inorganic materials 0.000 claims description 26
- 239000003822 epoxy resin Substances 0.000 claims description 25
- 229920000647 polyepoxide Polymers 0.000 claims description 25
- 239000000203 mixture Substances 0.000 claims description 23
- 239000004952 Polyamide Substances 0.000 claims description 21
- 239000002253 acid Substances 0.000 claims description 21
- 229920002647 polyamide Polymers 0.000 claims description 21
- 239000000758 substrate Substances 0.000 claims description 21
- 229960003638 dopamine Drugs 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 20
- 229920002873 Polyethylenimine Polymers 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 19
- 238000005406 washing Methods 0.000 claims description 19
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims description 18
- 238000000151 deposition Methods 0.000 claims description 17
- YPJUNDFVDDCYIH-UHFFFAOYSA-N perfluorobutyric acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)F YPJUNDFVDDCYIH-UHFFFAOYSA-N 0.000 claims description 16
- 239000007983 Tris buffer Substances 0.000 claims description 11
- 238000007731 hot pressing Methods 0.000 claims description 11
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 11
- SNHKMHUMILUWSJ-UHFFFAOYSA-N 5-(1,3-dioxo-3a,4,5,6,7,7a-hexahydro-2-benzofuran-5-yl)-3a,4,5,6,7,7a-hexahydro-2-benzofuran-1,3-dione Chemical compound C1CC2C(=O)OC(=O)C2CC1C1CC2C(=O)OC(=O)C2CC1 SNHKMHUMILUWSJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 10
- 238000013329 compounding Methods 0.000 claims description 10
- 238000005520 cutting process Methods 0.000 claims description 10
- 239000011159 matrix material Substances 0.000 claims description 10
- 229920005575 poly(amic acid) Polymers 0.000 claims description 10
- 238000007493 shaping process Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 9
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 238000002390 rotary evaporation Methods 0.000 claims description 8
- 238000002834 transmittance Methods 0.000 abstract description 10
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 238000013461 design Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 239000002352 surface water Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 21
- -1 aliphatic diamine Chemical class 0.000 description 7
- 230000008021 deposition Effects 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 229920001690 polydopamine Polymers 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- MQJKPEGWNLWLTK-UHFFFAOYSA-N Dapsone Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 MQJKPEGWNLWLTK-UHFFFAOYSA-N 0.000 description 3
- QFTYSVGGYOXFRQ-UHFFFAOYSA-N dodecane-1,12-diamine Chemical compound NCCCCCCCCCCCCN QFTYSVGGYOXFRQ-UHFFFAOYSA-N 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 238000005576 amination reaction Methods 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000001153 fluoro group Chemical group F* 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates 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
- C08G59/18—Macromolecules 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
- C08G59/40—Macromolecules 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
- C08G59/4007—Curing agents not provided for by the groups C08G59/42 - C08G59/66
- C08G59/4014—Nitrogen containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1039—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors comprising halogen-containing substituents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1042—Copolyimides derived from at least two different tetracarboxylic compounds or two different diamino compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1075—Partially aromatic polyimides
- C08G73/1078—Partially aromatic polyimides wholly aromatic in the diamino moiety
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Reinforced Plastic Materials (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
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 overall light transmittance, and can be used as a mobile phone cover plate. The invention has reasonable process design and proper component proportion, and the prepared mobile phone cover plate not only has high mechanical property of strength, but also has excellent surface water resistance, low water absorption and good light transmittance, and can be widely applied to the fields of mobile phone cover plates, electronic product cover plates, shells and the like, and has high practicability.
Description
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 (English name: glass fiber) is an inorganic nonmetallic material with excellent performance, and has the advantages of good insulation, strong heat resistance, good corrosion resistance and high mechanical strength, but has the disadvantages of brittle property and poor wear resistance. Glass fibers are commonly used as reinforcing materials in composite materials, electrical and thermal insulation materials, circuit substrates, and the like in various areas of national economy.
When the mobile phone cover plate is prepared at present, a continuous glass fiber cloth is generally used as a reinforcing layer, epoxy resin glue is coated on two sides of the reinforcing layer, and after curing, the reinforcing layer is subjected to multi-layer hot pressing to obtain a glass fiber laminated plate.
Aiming at the situation, we disclose a transparent glass fiber mobile phone cover plate and a preparation method thereof, so as to solve the technical problem.
Disclosure of Invention
The invention aims to provide a transparent glass fiber mobile phone cover plate and a preparation method thereof, which are used for solving 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, performing 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 vacuum drying to obtain aminated graphene;
taking the aminated graphene and absolute ethyl alcohol, and performing ultrasonic dispersion for 30-40 min to obtain graphene dispersion liquid; immersing the continuous glass fiber cloth into graphene dispersion liquid, performing ultrasonic dispersion for 5-10 min, and performing vacuum drying to obtain pretreated glass fiber cloth;
(2) Taking dopamine, polyethylenimine and Tris buffer solution, uniformly mixing, adding pretreated glass fiber cloth, depositing for 4-6 hours at 25-30 ℃, taking out, washing with deionized water, and vacuum drying to obtain a pretreated substrate;
(3) Uniformly mixing diethylenetriamine and deionized water to obtain a solution A; uniformly mixing heptafluorobutyric acid and deionized water, slowly dripping the mixture into the solution A, stirring and reacting for 2-3h, and removing water by rotary evaporation to obtain fluorodiethylenetriamine;
2,2' -di (trifluoromethyl) diaminobiphenyl and hexafluorodianhydride are taken and respectively preheated for 20 to 24 hours at the temperature of 140 to 150 ℃; taking preheated 2,2' -bis (trifluoromethyl) diaminobiphenyl and N, N-dimethylacetamide, uniformly stirring, adding hexafluorodianhydride and dicyclohexyl-3, 4,3',4' -tetracarboxylic dianhydride, introducing nitrogen, and stirring for 10-12 hours under a nitrogen environment to obtain polyamic acid;
(4) Uniformly mixing polyamide acid, epoxy resin and fluorinated diethylenetriamine at 30-35 ℃ to obtain 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 prepreg;
and taking a plurality of layers of prepregs, carrying out hot pressing compounding, and cutting and shaping to obtain the cover plate.
In the more optimized scheme, in the step (1), the concentration of the graphene dispersion liquid is 0.3g/L; the mass ratio of the continuous glass fiber cloth to the graphene dispersion liquid is 1:8.
in the more optimized scheme, in the step (1), the mass ratio of the graphene oxide to the bismuth trichloride to the 1, 6-hexamethylenediamine is 10:1:5.
in a more optimized scheme, in the step (3), the molar ratio of the diethylenetriamine to the heptafluorobutyric acid is 2:1.
in the more optimized scheme, in the resin glue solution in the step (4), the mass ratio of the epoxy resin to the polyamide acid to the fluorinated diethylenetriamine is 100:22:15.
in the more optimized scheme, in the step (4), the pretreatment matrix accounts for 45-50wt% of the mass of the prepreg.
More preferably, in the step (3), the molar ratio of the 2,2' -bis (trifluoromethyl) diaminobiphenyl to the hexafluorodianhydride is 1:1, wherein the molar ratio of dicyclohexyl-3, 4,3',4' -tetrahydric dianhydride to hexafluorodianhydride 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 overall light transmittance, and can be used as a mobile phone cover plate.
The application carries out preliminary treatment to continuous glass fiber cloth at first, carries out the amination to graphene earlier, carries its to glass fiber surface again, its aim at: on one hand, graphene oxide is loaded on the surface of the continuous glass fiber cloth, so that the continuous glass fiber cloth can be reinforced, and the mechanical property of the continuous glass fiber cloth is improved, so that the strength and mechanical property of a follow-up mobile phone cover plate are enhanced; on the other hand, the graphene oxide load can also enhance the adhesive force between the continuous glass fiber cloth and the subsequent polydopamine layer.
Based on the scheme, 1, 6-hexamethylenediamine is selected during amination treatment of graphene oxide, and proper alkyl chain length aliphatic diamine is selected during grafting, so that the dispersibility of graphene on the surface of glass fiber cloth can be improved, but the deposition and adhesion of polydopamine can be influenced when the alkyl chain length is too long, so that 1, 6-hexamethylenediamine is selected as the most preferable scheme in the alkyl aliphatic diamine.
After pretreatment of the continuous glass fiber cloth, the continuous glass fiber cloth is immersed in a mixed solution of dopamine, polyethylenimine and Tris buffer solution for self-polymerization deposition, and the amounts of the components and the deposition time are limited to 4-6h, wherein the aim is that: in the scheme, the transparency and the light transmittance of the mobile phone cover plate are required to be ensured, and the color of the mobile phone cover plate can influence the light transmittance of a product along with the increase of the polymerization time of dopamine; the deposition time is too short, and the polydopamine layer is used as a connecting transition layer between the resin glue layer and the continuous glass fiber cloth, so that 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 the deposition time to be 4-6h, so 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, and adopts the mixture of the fluorodiethylenetriamine and the polyamide acid as the curing agent and adds the curing agent into the epoxy resin to form the resin glue solution, and the technical effects realized by the steps are 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 polyamide acid is prepared from 2,2' -di (trifluoromethyl) diaminobiphenyl, hexafluorodianhydride and dicyclohexyl-3, 4,3',4' -tetracarboxylic dianhydride as raw materials to prepare a product containing fluorine groups and biphenyl six-membered ring structures, and the polyamide acid is used as an epoxy resin curing agent, so that the water resistance of the epoxy resin can be further improved, and the strength and heat resistance of the cured resin are improved, so that the cured resin has excellent mechanical properties and excellent waterproof and moistureproof properties.
The invention discloses a transparent glass fiber mobile phone cover plate and a preparation method thereof, which are reasonable in process design and proper in component proportion, and the prepared mobile phone cover plate not only has high strength mechanical properties, but also is excellent in surface water resistance, low in water absorption and good in light transmittance, and can be widely applied to the fields of mobile phone cover plates, electronic product cover plates, shells and the like, and has high practicability.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the 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 performing ultrasonic dispersion for 30min to obtain a mixed solution, wherein the concentration of the graphene oxide in the mixed solution is 0.1g/mL; adding 1, 6-hexamethylenediamine, stirring for 40 hours at 25 ℃, filtering, washing, and vacuum drying to obtain the aminated graphene; the mass ratio of the graphene oxide to the bismuth trichloride to the 1, 6-hexamethylenediamine is 10:1:5.
taking the aminated graphene and absolute ethyl alcohol, and performing ultrasonic dispersion for 30min to obtain graphene dispersion liquid; the concentration of the graphene dispersion liquid is 0.3g/L; immersing the continuous glass fiber cloth into graphene dispersion liquid, performing ultrasonic dispersion for 5min, performing vacuum drying at an ultrasonic power of 600W to obtain pretreated glass fiber cloth; the mass ratio of the continuous glass fiber cloth to the graphene dispersion liquid is 1:8.
(2) Taking dopamine, polyethylenimine and Tris buffer solution, and uniformly mixing to obtain a mixed solution; adding the pretreated glass fiber cloth, depositing for 6 hours at 25 ℃, taking out, washing with deionized water, and vacuum drying 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 2mg/mL.
(3) Uniformly mixing diethylenetriamine and deionized water to obtain a solution A; uniformly mixing heptafluorobutyric acid and deionized water, slowly dripping the mixture into the solution A, stirring the mixture for reaction for 2 hours, and removing water by rotary evaporation to obtain diethylenetriamine fluoride;
the molar ratio of diethylenetriamine to heptafluorobutyric acid is 2:1.
2,2 '-bis (trifluoromethyl) diaminobiphenyl and hexafluorodianhydride are taken and respectively preheated for 24 hours at 140 ℃, the preheated 2,2' -bis (trifluoromethyl) diaminobiphenyl and N, N-dimethylacetamide are taken and uniformly stirred at the rotating speed of 300r/min, and the hexafluorodianhydride and dicyclohexyl-3, 4,3',4' -tetracarboxylic dianhydride are added, nitrogen is introduced, and the mixture is stirred 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, wherein the molar ratio of dicyclohexyl-3, 4,3',4' -tetrahydric dianhydride to hexafluorodianhydride is 1:20.
(4) Uniformly mixing polyamide acid, epoxy resin and fluorinated diethylenetriamine at 30 ℃ to obtain resin glue solution; the mass ratio of the epoxy resin to the polyamide acid to the fluorinated diethylenetriamine is 100:22:15.
coating resin glue solution on two sides of the pretreated substrate, and heating to 100 ℃ at a heating rate of 5 ℃/min for curing to obtain prepreg; the pretreatment matrix is 50wt% of the mass of the prepreg.
And (5) taking three layers of prepregs, carrying out hot pressing compounding, and 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 performing ultrasonic dispersion for 35min to obtain a mixed solution, wherein the concentration of the graphene oxide in the mixed solution is 0.1g/mL; adding 1, 6-hexamethylenediamine, stirring for 35 hours at 28 ℃, filtering, washing, and vacuum drying to obtain the aminated graphene; the mass ratio of the graphene oxide to the bismuth trichloride to the 1, 6-hexamethylenediamine is 10:1:5.
taking the aminated graphene and absolute ethyl alcohol, and performing ultrasonic dispersion for 35min to obtain graphene dispersion liquid; the concentration of the graphene dispersion liquid is 0.3g/L; immersing the continuous glass fiber cloth into graphene dispersion liquid, performing ultrasonic dispersion for 8min, performing vacuum drying at an ultrasonic power of 600W to obtain pretreated glass fiber cloth; the mass ratio of the continuous glass fiber cloth to the graphene dispersion liquid is 1:8.
(2) Taking dopamine, polyethylenimine and Tris buffer solution, and uniformly mixing to obtain a mixed solution; adding the pretreated glass fiber cloth, depositing for 5 hours at 28 ℃, taking out, washing with deionized water, and vacuum drying 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 2mg/mL.
(3) Uniformly mixing diethylenetriamine and deionized water to obtain a solution A; uniformly mixing heptafluorobutyric acid and deionized water, slowly dripping the mixture into the solution A, stirring the mixture for reaction for 2 to 3 hours, and removing water by rotary evaporation to obtain fluorodiethylenetriamine;
the molar ratio of diethylenetriamine to heptafluorobutyric acid is 2:1.
2,2 '-bis (trifluoromethyl) diaminobiphenyl and hexafluorodianhydride are respectively preheated at 145 ℃ for 22 hours, the preheated 2,2' -bis (trifluoromethyl) diaminobiphenyl and N, N-dimethylacetamide are uniformly stirred at the rotating speed of 350r/min, the hexafluorodianhydride and dicyclohexyl-3, 4,3',4' -tetracarboxylic dianhydride are added, nitrogen is introduced, and the mixture is stirred 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, wherein the molar ratio of dicyclohexyl-3, 4,3',4' -tetrahydric dianhydride to hexafluorodianhydride is 1:20.
(4) Uniformly mixing polyamide acid, epoxy resin and fluorinated diethylenetriamine at 32 ℃ to obtain resin glue solution; the mass ratio of the epoxy resin to the polyamide acid to the fluorinated diethylenetriamine is 100:22:15.
coating resin glue solution on two sides of the pretreated substrate, and heating to 105 ℃ at a heating rate of 5 ℃/min for curing to obtain prepreg; the pretreatment matrix is 50wt% of the mass of the prepreg.
And (5) taking three layers of prepregs, carrying out 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 performing ultrasonic dispersion for 40min to obtain a mixed solution, wherein the concentration of the graphene oxide in the mixed solution is 0.1g/mL; adding 1, 6-hexamethylenediamine, stirring for 30 hours at 30 ℃, filtering, washing, and vacuum drying to obtain the aminated graphene; the mass ratio of the graphene oxide to the bismuth trichloride to the 1, 6-hexamethylenediamine is 10:1:5.
taking the aminated graphene and absolute ethyl alcohol, and performing ultrasonic dispersion for 40min to obtain graphene dispersion liquid; the concentration of the graphene dispersion liquid is 0.3g/L; immersing continuous glass fiber cloth into graphene dispersion liquid, performing ultrasonic dispersion for 10min, performing vacuum drying at an ultrasonic power of 600W to obtain pretreated glass fiber cloth; the mass ratio of the continuous glass fiber cloth to the graphene dispersion liquid is 1:8.
(2) Taking dopamine, polyethylenimine and Tris buffer solution, and uniformly mixing to obtain a mixed solution; adding the pretreated glass fiber cloth, depositing for 4 hours at 30 ℃, taking out, washing with deionized water, and vacuum drying 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 2mg/mL.
(3) Uniformly mixing diethylenetriamine and deionized water to obtain a solution A; uniformly mixing heptafluorobutyric acid and deionized water, slowly dripping the mixture into the solution A, stirring the mixture for reaction for 3 hours, and removing water by rotary evaporation to obtain diethylenetriamine fluoride;
the molar ratio of diethylenetriamine to heptafluorobutyric acid is 2:1.
2,2 '-bis (trifluoromethyl) diaminobiphenyl and hexafluorodianhydride are respectively preheated for 20 hours at 150 ℃, the preheated 2,2' -bis (trifluoromethyl) diaminobiphenyl and N, N-dimethylacetamide are taken and uniformly stirred at the rotation speed of 400r/min, and the hexafluorodianhydride and dicyclohexyl-3, 4,3',4' -tetracarboxylic dianhydride are added, nitrogen is introduced, and the mixture is stirred 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, wherein the molar ratio of dicyclohexyl-3, 4,3',4' -tetrahydric dianhydride to hexafluorodianhydride is 1:20.
(4) Uniformly mixing polyamide acid, epoxy resin and fluorinated diethylenetriamine at 35 ℃ to obtain resin glue solution; the mass ratio of the epoxy resin to the polyamide acid to the fluorinated diethylenetriamine is 100:22:15.
coating resin glue solution on two sides of the pretreated substrate, and heating to 110 ℃ at a heating rate of 5 ℃/min for curing to obtain prepreg; the pretreatment matrix is 50wt% of the mass of the prepreg.
And (5) taking three layers of prepregs, carrying out hot pressing compounding, and cutting and shaping to obtain the cover plate.
Comparative example 1: a control experiment was performed on the basis of example 3, in which no fluorodiethylenetriamine was introduced in comparative example 1, the remaining steps being 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 0.1g/mL; adding 1, 6-hexamethylenediamine, stirring for 30 hours at 30 ℃, filtering, washing, and vacuum drying to obtain the aminated graphene; the mass ratio of the graphene oxide to the bismuth trichloride to the 1, 6-hexamethylenediamine is 10:1:5.
taking the aminated graphene and absolute ethyl alcohol, and performing ultrasonic dispersion for 40min to obtain graphene dispersion liquid; the concentration of the graphene dispersion liquid is 0.3g/L; immersing continuous glass fiber cloth into graphene dispersion liquid, performing ultrasonic dispersion for 10min, performing vacuum drying at an ultrasonic power of 600W to obtain pretreated glass fiber cloth; the mass ratio of the continuous glass fiber cloth to the graphene dispersion liquid is 1:8.
(2) Taking dopamine, polyethylenimine and Tris buffer solution, and uniformly mixing to obtain a mixed solution; adding the pretreated glass fiber cloth, depositing for 4 hours at 30 ℃, taking out, washing with deionized water, and vacuum drying 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 2mg/mL.
(3) 2,2 '-bis (trifluoromethyl) diaminobiphenyl and hexafluorodianhydride are respectively preheated for 20 hours at 150 ℃, the preheated 2,2' -bis (trifluoromethyl) diaminobiphenyl and N, N-dimethylacetamide are taken and uniformly stirred at the rotation speed of 400r/min, and the hexafluorodianhydride and dicyclohexyl-3, 4,3',4' -tetracarboxylic dianhydride are added, nitrogen is introduced, and the mixture is stirred 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, wherein the molar ratio of dicyclohexyl-3, 4,3',4' -tetrahydric dianhydride to hexafluorodianhydride is 1:20.
(4) Uniformly mixing polyamide acid and epoxy resin at 35 ℃ to obtain resin glue solution; the mass ratio of the epoxy resin to the polyamide acid is 100:37.
coating resin glue solution on two sides of the pretreated substrate, and heating to 110 ℃ at a heating rate of 5 ℃/min for curing to obtain prepreg; the pretreatment matrix is 50wt% of the mass of the prepreg.
And (5) taking three layers of prepregs, carrying out hot pressing compounding, and cutting and shaping to obtain the cover plate.
Comparative example 2: a control experiment was performed on the basis of example 3, in which no fluorinated diethylenetriamine or polyamic acid was introduced in comparative example 2, and only 4,4' -diaminodiphenyl sulfone 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 0.1g/mL; adding 1, 6-hexamethylenediamine, stirring for 30 hours at 30 ℃, filtering, washing, and vacuum drying to obtain the aminated graphene; the mass ratio of the graphene oxide to the bismuth trichloride to the 1, 6-hexamethylenediamine is 10:1:5.
taking the aminated graphene and absolute ethyl alcohol, and performing ultrasonic dispersion for 40min to obtain graphene dispersion liquid; the concentration of the graphene dispersion liquid is 0.3g/L; immersing continuous glass fiber cloth into graphene dispersion liquid, performing ultrasonic dispersion for 10min, performing vacuum drying at an ultrasonic power of 600W to obtain pretreated glass fiber cloth; the mass ratio of the continuous glass fiber cloth to the graphene dispersion liquid is 1:8.
(2) Taking dopamine, polyethylenimine and Tris buffer solution, and uniformly mixing to obtain a mixed solution; adding the pretreated glass fiber cloth, depositing for 4 hours at 30 ℃, taking out, washing with deionized water, and vacuum drying 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 2mg/mL.
(3) Mixing 4,4' -diaminodiphenyl sulfone and epoxy resin uniformly at 35 ℃ to obtain resin glue solution; the mass ratio of the epoxy resin to the 4,4' -diaminodiphenyl sulfone is 100:15.
coating resin glue solution on two sides of the pretreated substrate, and heating to 110 ℃ at a heating rate of 5 ℃/min for curing to obtain prepreg; the pretreatment matrix is 50wt% of the mass of the prepreg.
And (5) taking three layers of prepregs, carrying out hot pressing compounding, and cutting and shaping to obtain the cover plate.
Comparative example 3: control experiments were 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 performing ultrasonic dispersion for 40min to obtain a mixed solution, wherein the concentration of the graphene oxide in the mixed solution is 0.1g/mL; adding 1, 6-hexamethylenediamine, stirring for 30 hours at 30 ℃, filtering, washing, and vacuum drying to obtain the aminated graphene; the mass ratio of the graphene oxide to the bismuth trichloride to the 1, 6-hexamethylenediamine is 10:1:5.
taking the aminated graphene and absolute ethyl alcohol, and performing ultrasonic dispersion for 40min to obtain graphene dispersion liquid; the concentration of the graphene dispersion liquid is 0.3g/L; immersing continuous glass fiber cloth into graphene dispersion liquid, performing ultrasonic dispersion for 10min, performing vacuum drying at an ultrasonic power of 600W to obtain pretreated glass fiber cloth; the mass ratio of the continuous glass fiber cloth to the graphene dispersion liquid is 1:8.
(2) Taking dopamine, polyethylenimine and Tris buffer solution, and uniformly mixing to obtain a mixed solution; adding the pretreated glass fiber cloth, depositing for 8 hours at 30 ℃, taking out, washing with deionized water, and vacuum drying 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 2mg/mL.
(3) Uniformly mixing diethylenetriamine and deionized water to obtain a solution A; uniformly mixing heptafluorobutyric acid and deionized water, slowly dripping the mixture into the solution A, stirring the mixture for reaction for 3 hours, and removing water by rotary evaporation to obtain diethylenetriamine fluoride;
the molar ratio of diethylenetriamine to heptafluorobutyric acid is 2:1.
2,2 '-bis (trifluoromethyl) diaminobiphenyl and hexafluorodianhydride are respectively preheated for 20 hours at 150 ℃, the preheated 2,2' -bis (trifluoromethyl) diaminobiphenyl and N, N-dimethylacetamide are taken and uniformly stirred at the rotation speed of 400r/min, and the hexafluorodianhydride and dicyclohexyl-3, 4,3',4' -tetracarboxylic dianhydride are added, nitrogen is introduced, and the mixture is stirred 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, wherein the molar ratio of dicyclohexyl-3, 4,3',4' -tetrahydric dianhydride to hexafluorodianhydride is 1:20.
(4) Uniformly mixing polyamide acid, epoxy resin and fluorinated diethylenetriamine at 35 ℃ to obtain resin glue solution; the mass ratio of the epoxy resin to the polyamide acid to the fluorinated diethylenetriamine is 100:22:15.
coating resin glue solution on two sides of the pretreated substrate, and heating to 110 ℃ at a heating rate of 5 ℃/min for curing to obtain prepreg; the pretreatment matrix is 50wt% of the mass of the prepreg.
And (5) taking three layers of prepregs, carrying out hot pressing compounding, and cutting and shaping to obtain the cover plate.
Comparative example 4: control experiments were performed on the basis of example 3, with a polydopamine deposition time of 10h in comparative example 4.
Comparative example 5: control experiments were performed on the basis of example 3, in which the glass fiber surface was not pretreated in comparative example 5.
A preparation method of a transparent glass fiber mobile phone cover plate comprises the following steps:
(1) Taking dopamine, polyethylenimine and Tris buffer solution, and uniformly mixing to obtain a mixed solution; adding continuous glass fiber cloth, depositing for 4 hours at 30 ℃, taking out, washing with deionized water, and vacuum drying 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 2mg/mL.
(2) Uniformly mixing diethylenetriamine and deionized water to obtain a solution A; uniformly mixing heptafluorobutyric acid and deionized water, slowly dripping the mixture into the solution A, stirring the mixture for reaction for 3 hours, and removing water by rotary evaporation to obtain diethylenetriamine fluoride;
the molar ratio of diethylenetriamine to heptafluorobutyric acid is 2:1.
2,2 '-bis (trifluoromethyl) diaminobiphenyl and hexafluorodianhydride are respectively preheated for 20 hours at 150 ℃, the preheated 2,2' -bis (trifluoromethyl) diaminobiphenyl and N, N-dimethylacetamide are taken and uniformly stirred at the rotation speed of 400r/min, and the hexafluorodianhydride and dicyclohexyl-3, 4,3',4' -tetracarboxylic dianhydride are added, nitrogen is introduced, and the mixture is stirred 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, wherein the molar ratio of dicyclohexyl-3, 4,3',4' -tetrahydric dianhydride to hexafluorodianhydride is 1:20.
(3) Uniformly mixing polyamide acid, epoxy resin and fluorinated diethylenetriamine at 35 ℃ to obtain resin glue solution; the mass ratio of the epoxy resin to the polyamide acid to the fluorinated diethylenetriamine is 100:22:15.
coating resin glue solution on two sides of the pretreated substrate, and heating to 110 ℃ at a heating rate of 5 ℃/min for curing to obtain prepreg; the pretreatment matrix is 50wt% of the mass of the prepreg.
And (5) taking three layers of prepregs, carrying out hot pressing compounding, and cutting and shaping to obtain the cover plate.
Comparative example 6: a control experiment was performed on the basis of example 3, with 1, 12-diaminododecane introduced in comparative example 6.
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 0.1g/mL; adding 1, 12-diaminododecane, stirring for 30 hours at 30 ℃, filtering, washing, and vacuum drying to obtain the aminated graphene; the mass ratio of the graphene oxide to the bismuth trichloride to the 1, 12-diaminododecane is 10:1:5.
taking the aminated graphene and absolute ethyl alcohol, and performing ultrasonic dispersion for 40min to obtain graphene dispersion liquid; the concentration of the graphene dispersion liquid is 0.3g/L; immersing continuous glass fiber cloth into graphene dispersion liquid, performing ultrasonic dispersion for 10min, performing vacuum drying at an ultrasonic power of 600W to obtain pretreated glass fiber cloth; the mass ratio of the continuous glass fiber cloth to the graphene dispersion liquid is 1:8.
(2) Taking dopamine, polyethylenimine and Tris buffer solution, and uniformly mixing to obtain a mixed solution; adding the pretreated glass fiber cloth, depositing for 4 hours at 30 ℃, taking out, washing with deionized water, and vacuum drying 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 2mg/mL.
(3) Uniformly mixing diethylenetriamine and deionized water to obtain a solution A; uniformly mixing heptafluorobutyric acid and deionized water, slowly dripping the mixture into the solution A, stirring the mixture for reaction for 3 hours, and removing water by rotary evaporation to obtain diethylenetriamine fluoride;
the molar ratio of diethylenetriamine to heptafluorobutyric acid is 2:1.
2,2 '-bis (trifluoromethyl) diaminobiphenyl and hexafluorodianhydride are respectively preheated for 20 hours at 150 ℃, the preheated 2,2' -bis (trifluoromethyl) diaminobiphenyl and N, N-dimethylacetamide are taken and uniformly stirred at the rotation speed of 400r/min, and the hexafluorodianhydride and dicyclohexyl-3, 4,3',4' -tetracarboxylic dianhydride are added, nitrogen is introduced, and the mixture is stirred 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, wherein the molar ratio of dicyclohexyl-3, 4,3',4' -tetrahydric dianhydride to hexafluorodianhydride is 1:20.
(4) Uniformly mixing polyamide acid, epoxy resin and fluorinated diethylenetriamine at 35 ℃ to obtain resin glue solution; the mass ratio of the epoxy resin to the polyamide acid to the fluorinated diethylenetriamine is 100:22:15.
coating resin glue solution on two sides of the pretreated substrate, and heating to 110 ℃ at a heating rate of 5 ℃/min for curing to obtain prepreg; the pretreatment matrix is 50wt% of the mass of the prepreg.
And (5) taking three layers of prepregs, carrying out 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/m 2 . The graphene oxide sheet diameter is 3 μm.
Detection test:
1. taking the cover plates prepared in examples 1-3 and comparative examples 1-6, weighing, respectively soaking in distilled water at 25 ℃ for 24 hours, taking out the water absorbing paper to absorb the surface moisture, weighing and comparing the weight with the weight before testing, and calculating the water absorption rate.
2. The cover plates prepared in examples 1 to 3 and comparative examples 1 to 6 were taken, their tensile strength was measured according to GB/T1447-2005, then immersed in distilled water for 30d at 25℃and wiped dry after taking out, and their tensile strength was again measured and recorded. The product dimensions were 2mm by 25mm by 150mm.
3. The cover plates prepared in examples 1 to 3 and comparative examples 1 to 6 were used for light transmittance testing, and an ultraviolet-visible spectrophotometer was used for the testing.
Project | Tensile Strength (MPa) | 30d tensile Strength (MPa) | 24h Water absorption (%) | 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% | / |
Conclusion: the invention discloses a transparent glass fiber mobile phone cover plate and a preparation method thereof, which are reasonable in process design and proper in component proportion, and the prepared mobile phone cover plate not only has high strength mechanical properties, but also is excellent in surface water resistance, low in water absorption and good in light transmittance, and can be widely applied to the fields of mobile phone cover plates, electronic product cover plates, shells and the like, and has high practicability.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. The preparation method of the transparent glass fiber mobile phone cover plate is characterized by comprising the following steps of:
(1) Taking graphene oxide, bismuth trichloride and N, N-dimethylformamide, performing ultrasonic dispersion for 30-40 min to obtain a mixed solution, adding 1, 6-hexamethylenediamine, stirring for 30-40 h at 25-30 ℃, filtering, washing, and performing vacuum drying to obtain aminated graphene;
taking the aminated graphene and absolute ethyl alcohol, and performing ultrasonic dispersion for 30-40 min to obtain graphene dispersion liquid; immersing the continuous glass fiber cloth into graphene dispersion liquid, performing ultrasonic dispersion for 5-10 min, and performing vacuum drying to obtain pretreated glass fiber cloth;
(2) Taking dopamine, polyethylenimine and Tris buffer solution, uniformly mixing, adding pretreated glass fiber cloth, depositing for 4-6 hours at 25-30 ℃, taking out, washing with deionized water, and vacuum drying to obtain a pretreated substrate;
(3) Uniformly mixing diethylenetriamine and deionized water to obtain a solution A; uniformly mixing heptafluorobutyric acid and deionized water, slowly dripping the mixture into the solution A, stirring and reacting for 2-3h, and removing water by rotary evaporation to obtain fluorodiethylenetriamine;
2,2 '-di (trifluoromethyl) diaminobiphenyl and hexafluorodianhydride are respectively preheated for 20-24 hours at 140-150 ℃, the preheated 2,2' -di (trifluoromethyl) diaminobiphenyl and N, N-dimethylacetamide are taken and uniformly stirred, the hexafluorodianhydride and dicyclohexyl-3, 4,3',4' -tetracarboxylic dianhydride are added, nitrogen is introduced, and the mixture is stirred for 10-12 hours in a nitrogen environment, so as to obtain polyamic acid;
(4) Uniformly mixing polyamide acid, epoxy resin and fluorinated diethylenetriamine at 30-35 ℃ to obtain 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 prepreg;
and taking a plurality of layers of prepregs, carrying out hot pressing compounding, and cutting and shaping to obtain the cover plate.
2. The method for preparing the transparent glass fiber mobile phone cover plate according to claim 1, which is characterized in that: in the step (1), the concentration of the graphene dispersion liquid is 0.3g/L; the mass ratio of the continuous glass fiber cloth to the graphene dispersion liquid is 1:8.
3. the method for preparing the transparent glass fiber mobile phone cover plate according to claim 1, which is characterized in that: in the step (1), the mass ratio of the graphene oxide to the bismuth trichloride to the 1, 6-hexamethylenediamine is 10:1:5.
4. the method for preparing the transparent glass fiber mobile phone cover plate according to claim 1, which is characterized in that: in the step (3), the molar ratio of the diethylenetriamine to the heptafluorobutyric acid is 2:1.
5. the method for preparing the transparent glass fiber mobile phone cover plate according to claim 1, which is characterized in that: in the resin glue solution in the step (4), the mass ratio of the epoxy resin to the polyamide acid to the fluorinated diethylenetriamine is 100:22:15.
6. the method for preparing the transparent glass fiber mobile phone cover plate according to claim 1, which is characterized in that: in the step (4), the pretreatment matrix accounts for 45-50wt% of the mass of the prepreg.
7. The method for preparing the transparent glass fiber mobile phone cover plate according to claim 1, which is characterized in that: in the step (3), the molar ratio of the 2,2' -bis (trifluoromethyl) diaminobiphenyl to the hexafluorodianhydride is 1:1, wherein the molar ratio of the dicyclohexyl-3, 4,3',4' -tetrahydric dianhydride to the hexafluorodianhydride is 1:20.
8. a mobile phone cover plate made by the method for making a transparent glass fiber mobile phone cover plate according to any one of claims 1-7.
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