CN112662135A - Epoxy resin insulating board and preparation method thereof - Google Patents
Epoxy resin insulating board and preparation method thereof Download PDFInfo
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- CN112662135A CN112662135A CN202011459618.6A CN202011459618A CN112662135A CN 112662135 A CN112662135 A CN 112662135A CN 202011459618 A CN202011459618 A CN 202011459618A CN 112662135 A CN112662135 A CN 112662135A
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 47
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 43
- IISBACLAFKSPIT-UHFFFAOYSA-N Bisphenol A Natural products C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000012763 reinforcing filler Substances 0.000 claims abstract description 27
- 239000000945 filler Substances 0.000 claims abstract description 25
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 21
- 230000003712 anti-aging effect Effects 0.000 claims abstract description 17
- 230000032683 aging Effects 0.000 claims abstract description 14
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 14
- VXHYVVAUHMGCEX-UHFFFAOYSA-N 2-(2-hydroxyphenoxy)phenol Chemical compound OC1=CC=CC=C1OC1=CC=CC=C1O VXHYVVAUHMGCEX-UHFFFAOYSA-N 0.000 claims abstract description 13
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000011575 calcium Substances 0.000 claims abstract description 13
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 13
- 229920005989 resin Polymers 0.000 claims abstract description 13
- 239000011347 resin Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000002270 dispersing agent Substances 0.000 claims abstract description 5
- 239000013530 defoamer Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 66
- 238000003756 stirring Methods 0.000 claims description 64
- 238000006243 chemical reaction Methods 0.000 claims description 56
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 54
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 41
- ZZTCPWRAHWXWCH-UHFFFAOYSA-N diphenylmethanediamine Chemical compound C=1C=CC=CC=1C(N)(N)C1=CC=CC=C1 ZZTCPWRAHWXWCH-UHFFFAOYSA-N 0.000 claims description 33
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 24
- 238000010992 reflux Methods 0.000 claims description 23
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- 238000009413 insulation Methods 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 17
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 16
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 16
- 229910021389 graphene Inorganic materials 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000012065 filter cake Substances 0.000 claims description 15
- 239000000706 filtrate Substances 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 15
- 239000002518 antifoaming agent Substances 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 12
- 229920000570 polyether Polymers 0.000 claims description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims description 11
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 11
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 10
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 229940040526 anhydrous sodium acetate Drugs 0.000 claims description 9
- 229910052801 chlorine Inorganic materials 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- ASOKPJOREAFHNY-UHFFFAOYSA-N 1-Hydroxybenzotriazole Chemical compound C1=CC=C2N(O)N=NC2=C1 ASOKPJOREAFHNY-UHFFFAOYSA-N 0.000 claims description 8
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- 229960000583 acetic acid Drugs 0.000 claims description 8
- KQNKJJBFUFKYFX-UHFFFAOYSA-N acetic acid;trihydrate Chemical compound O.O.O.CC(O)=O KQNKJJBFUFKYFX-UHFFFAOYSA-N 0.000 claims description 8
- KCXMKQUNVWSEMD-UHFFFAOYSA-N benzyl chloride Chemical compound ClCC1=CC=CC=C1 KCXMKQUNVWSEMD-UHFFFAOYSA-N 0.000 claims description 8
- 229940073608 benzyl chloride Drugs 0.000 claims description 8
- 239000000460 chlorine Substances 0.000 claims description 8
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims description 8
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 claims description 8
- 239000012362 glacial acetic acid Substances 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 229940046892 lead acetate Drugs 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000005543 nano-size silicon particle Substances 0.000 claims description 8
- 239000012286 potassium permanganate Substances 0.000 claims description 8
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 claims description 7
- ZMXYNJXDULEQCK-UHFFFAOYSA-N 2-amino-p-cresol Chemical compound CC1=CC=C(O)C(N)=C1 ZMXYNJXDULEQCK-UHFFFAOYSA-N 0.000 claims description 7
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- 229940018564 m-phenylenediamine Drugs 0.000 claims description 7
- 239000001632 sodium acetate Substances 0.000 claims description 7
- 235000017281 sodium acetate Nutrition 0.000 claims description 7
- 239000004317 sodium nitrate Substances 0.000 claims description 7
- 235000010344 sodium nitrate Nutrition 0.000 claims description 7
- JVERADGGGBYHNP-UHFFFAOYSA-N 5-phenylbenzene-1,2,3,4-tetracarboxylic acid Chemical compound OC(=O)C1=C(C(O)=O)C(C(=O)O)=CC(C=2C=CC=CC=2)=C1C(O)=O JVERADGGGBYHNP-UHFFFAOYSA-N 0.000 claims description 6
- 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 6
- AMLFJZRZIOZGPW-UHFFFAOYSA-N prop-1-en-1-amine Chemical compound CC=CN AMLFJZRZIOZGPW-UHFFFAOYSA-N 0.000 claims description 6
- HWCKGOZZJDHMNC-UHFFFAOYSA-M tetraethylammonium bromide Chemical compound [Br-].CC[N+](CC)(CC)CC HWCKGOZZJDHMNC-UHFFFAOYSA-M 0.000 claims description 6
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000005286 illumination Methods 0.000 claims description 5
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- VVJKKWFAADXIJK-UHFFFAOYSA-N Allylamine Chemical compound NCC=C VVJKKWFAADXIJK-UHFFFAOYSA-N 0.000 claims description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 4
- DCXXMTOCNZCJGO-UHFFFAOYSA-N tristearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 claims description 4
- VBICKXHEKHSIBG-UHFFFAOYSA-N beta-monoglyceryl stearate Natural products CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 claims description 3
- 238000000643 oven drying Methods 0.000 claims description 2
- 235000010265 sodium sulphite Nutrition 0.000 claims description 2
- 229910000365 copper sulfate Inorganic materials 0.000 claims 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims 2
- 239000001257 hydrogen Substances 0.000 abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 7
- 150000008040 ionic compounds Chemical class 0.000 abstract description 2
- 238000006552 photochemical reaction Methods 0.000 abstract description 2
- 239000004593 Epoxy Substances 0.000 abstract 4
- 230000006378 damage Effects 0.000 abstract 1
- 230000003014 reinforcing effect Effects 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- 239000005977 Ethylene Substances 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 238000005034 decoration Methods 0.000 description 3
- 238000009408 flooring Methods 0.000 description 3
- 229940037312 stearamide Drugs 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 description 1
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229930003836 cresol Natural products 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000006193 diazotization reaction Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229940075507 glyceryl monostearate Drugs 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical group [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001788 mono and diglycerides of fatty acids Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Abstract
The invention discloses an epoxy resin insulating board and a preparation method thereof, wherein the insulating floor comprises the following raw materials in parts by weight: 30-50 parts of epoxy bisphenol A type resin, 0.2-0.5 part of dispersant, 0.5-1.5 parts of defoamer, 5-8 parts of anti-aging filler, 8-10 parts of reinforcing filler, 3-5 parts of silicon dioxide and 3-5 parts of calcium powder; this reinforcing filler can make epoxy's toughness reinforcing, this ageing-resistant filler is difficult for appearing from epoxy insulated floor, and ageing-resistant intramolecular hydrogen bond destruction, the hydrogen bond ring is opened and is formed ionic compound, this structure is unstable, can release unnecessary energy with harmless heat energy for reaching stable state, and then make hydrogen bond reconversion, and then protection epoxy insulated floor does not take place photochemical reaction, the effectual ageing resistance that has promoted epoxy insulated panel, this panel is fit for being applied to the substrate of making floor and wallboard.
Description
Technical Field
The invention relates to the technical field of floor preparation, in particular to an epoxy resin insulating plate and a preparation method thereof.
Background
The modern society is developing at a high speed, and various buildings such as bamboo shoots are pulled out after the rain, and the demand of decorative plates and floors for building surfaces is continuously increased. The building decorative board and floor are materials which are paved or coated on the surface of a building to play the roles of decoration and environment beautification, integrate materials, processes, modeling design and aesthetics, are important material bases of building decoration engineering, and the epoxy resin insulation floor gradually enters the sight of people by virtue of excellent performance.
The existing epoxy resin insulation floor is general in moisture and heat resistance, can absorb moisture when used in an environment with large moisture, so that the performance of the floor is reduced, and the surface of the floor is obviously aged after the floor is used for a period of time, so that the service life of the floor is shortened.
Disclosure of Invention
The invention aims to provide an epoxy resin insulating plate and a preparation method thereof.
The technical problems to be solved by the invention are as follows:
the existing epoxy resin insulation floor is general in moisture and heat resistance, can absorb moisture when used in an environment with large moisture, so that the performance of the floor is reduced, and the surface of the floor is obviously aged after the floor is used for a period of time, so that the service life of the floor is shortened.
The purpose of the invention can be realized by the following technical scheme:
an epoxy resin insulation board comprises the following raw materials in parts by weight: 30-50 parts of epoxy bisphenol A type resin, 0.2-0.5 part of dispersant, 0.5-1.5 parts of defoamer, 5-8 parts of anti-aging filler, 8-10 parts of reinforcing filler, 3-5 parts of silicon dioxide and 3-5 parts of calcium powder;
the epoxy resin insulating floor is prepared by the following steps:
step S1: adding epoxy bisphenol A resin into a stirring kettle, stirring at the rotation speed of 300-;
step S2: and (4) adding the mixture prepared in the step S1, the reinforcing filler, the silicon dioxide and the calcium powder into a stirring kettle, stirring for 10-15min at the rotation speed of 800-1000r/min, adding into a mold, and curing at the temperature of 110-120 ℃ to obtain the epoxy resin insulating floor.
Further, the dispersing agent is one or a mixture of more of ethylene bis stearamide, glyceryl tristearate and glyceryl monostearate in any proportion, and the defoaming agent is one of polyether defoaming agent GP, polyether defoaming agent GPE and polyether defoaming agent GPES.
Further, the reinforcing filler is prepared by the following steps:
step A1: adding concentrated sulfuric acid into a reaction kettle, stirring and adding graphite and sodium nitrate under the conditions that the rotating speed is 150-200r/min and the temperature is 1-3 ℃, stirring for 5-10min, adding potassium permanganate, heating to the temperature of 35-40 ℃, reacting for 20-25h, adding distilled water and a hydrogen peroxide solution under the temperature of 80-85 ℃, stirring for 1-1.5h, filtering to remove filtrate, washing a filter cake with deionized water until the pH value is 7, and drying to obtain graphene oxide;
step A2: dissolving bisphenol A in tetrahydrofuran, introducing chlorine, reacting for 20-30min under the condition of illumination, adding potassium carbonate, stirring under the condition of the rotation speed of 150-;
the reaction process is as follows:
step A3: dissolving diaminodiphenylmethane in acetone to obtain diaminodiphenylmethane solution, adding half of the diaminodiphenylmethane solution and the graphene oxide prepared in the step A1 into a reaction kettle, stirring the mixture to be uniform at the rotation speed of 200-300r/min, adding 1-hydroxy benzotriazole, reacting for 5-8h, filtering to remove filtrate, oven drying the filter cake to obtain modified graphene, dispersing the modified graphene in dimethylacetamide, under the conditions that the rotation speed is 150-, and reacting for 8-10h at the temperature of 160 ℃ to obtain the reinforcing filler.
Further, the use amount ratio of the concentrated sulfuric acid, the graphite, the sodium nitrate, the potassium permanganate, the distilled water and the hydrogen peroxide solution in the step A1 is 50mL:2g: 1g: 6g: 15mL of 6mL of concentrated sulfuric acid, 98% of concentrated sulfuric acid by mass, 30% of hydrogen peroxide solution by mass, 1mol of 1: 1mol of 9mL of 2mL of the bisphenol A, chlorine, potassium carbonate and tetraethylammonium bromide in the step A2, 4:1:1 of the formaldehyde, the intermediate 1 and diaminodiphenylmethane in a molar ratio, 20% of the diaminodiphenylmethane solution in the step A3, 10mL of the diaminodiphenylmethane solution, 3g of the graphene oxide and 1-hydroxybenzotriazole in the modified graphene, 0.5g of the modified graphene, 1.5g of the biphenyltetracarboxylic dianhydride, 6mL of the diaminodiphenylmethane solution, the intermediate 2 and the sulfuric acid solution, and 30-35% of the sulfuric acid solution.
Further, the aging-resistant filler is prepared by the following steps:
step B1: adding benzyl chloride into a reaction kettle, stirring and dropwise adding mixed acid under the conditions that the rotation speed is 200-25 ℃ and the temperature is 20-25 ℃ for 1.5h to prepare an intermediate 3, adding the intermediate 3, benzene and aluminum trichloride into the reaction kettle, reacting for 8-12h under the condition that the temperature is 80-85 ℃ to prepare an intermediate 4, adding the intermediate 4, glacial acetic acid and lead acetate trihydrate into the reaction kettle, dropwise adding nitric acid under the condition that the temperature is 100-110 ℃ to react for 5-8h to prepare an intermediate 5, adding the intermediate 5, iron powder and ethanol into the reaction kettle, performing reflux reaction for 3-5h under the condition that the temperature is 80-85 ℃, dropwise adding a hydrochloric acid solution, and continuing to react for 20-30min to prepare an intermediate 6;
the reaction process is as follows:
step B2: adding o-amino-p-cresol, deionized water and concentrated hydrochloric acid into a reaction kettle, adding a dropping liquid under the conditions that the rotation speed is 200-5 ℃ and the temperature is 3-5 ℃ to react for 2-3h to obtain an intermediate 7, adding the intermediate 7 and an anhydrous sodium acetate solution into m-phenylenediamine and hydrochloric acid solution under the temperature of 1-3 ℃, dropping for 20-30min, heating to 25-30 ℃ after dropping, continuing to react for 2-3h to obtain an intermediate 8, dissolving the intermediate 8 into methanol, adding a copper sulfate pentahydrate solution and ammonia water, and performing reflux reaction for 2-3h at the temperature of 110-120 ℃ to obtain an intermediate 9;
the reaction process is as follows:
step B3: dissolving cyanuric chloride in acetone, adding the intermediate 6 and sodium acetate prepared in the step B1, reacting for 3-5h at the rotation speed of 120-150r/min and the temperature of 3-5 ℃, adding the intermediate 9 prepared in the step B2, reacting for 3-5h at the temperature of 40-50 ℃, adding propenyl amine, refluxing for 3-5h at the temperature of 80-90 ℃, adding gamma-mercaptopropyl trimethoxysilane and triethylamine, refluxing for 5-8h at the temperature of 115 ℃ to prepare an intermediate 10, dispersing nano silicon dioxide in an ethanol aqueous solution, adjusting the pH value of the solution to 4-5, adding the intermediate 10, reacting for 3-5h at the temperature of 80-85 ℃, filtering to remove filtrate, and drying the filter cake to obtain the anti-aging filler.
The reaction process is as follows:
further, the dosage mass ratio of the benzyl chloride and the mixed acid in the step B1 is 2:1, the mixed acid is formed by mixing nitric acid with the mass fraction of 97% and sulfuric acid with the mass fraction of 98% in a molar ratio of 2:1, the dosage ratio of the intermediate 3, benzene and aluminum trichloride is 1g:10.2mL:1g, the dosage ratio of the intermediate 4, glacial acetic acid, lead acetate trihydrate and nitric acid is 2.5g:20mL:0.025g:2g, the mass fraction of the nitric acid is 97%, the dosage ratio of the intermediate 5, iron powder, ethanol and hydrochloric acid solution is 2.8g:4.5g:60mL:200mL, hydrochloric acid solution is formed by mixing hydrochloric acid with the mass fraction of 38% and ethanol with the mass fraction of 95% in a volume ratio of 1:9, the dosage ratio of the o-amino-p-cresol, the deionized water, the concentrated hydrochloric acid and the concentrated hydrochloric acid in the step B2 is 1.1g:15mL:2mL:5mL, the concentration of the liquid adding acid is 25%, and the sodium sulfite is added, Mixing copper sulfate pentahydrate and deionized water according to the using amount ratio of 0.7g:0.04g:50mL, wherein the using amount ratio of m-phenylenediamine, a hydrochloric acid solution, an intermediate 7 and an anhydrous sodium acetate solution is 1.08g:20mL:2.3g:10mL, the mass fraction of the anhydrous sodium acetate solution is 40%, the using amount ratio of an intermediate 8, the copper sulfate pentahydrate solution and ammonia water is 1g:3mL:5mL, the mass fraction of the copper sulfate pentahydrate solution is 35%, the mass fraction of the ammonia water is 25%, the molar ratio of the cyanuric chloride, the sodium acetate, the intermediate 6, the intermediate 9, the allylamine and the gamma-mercaptopropyltrimethoxysilane described in the step B3 is 1:1:1:1:1:1, the using amount of triethylamine is 20-30% by mass of the gamma-mercaptopropyltrimethoxysilane, and the using amount ratio of the intermediate 10 and the nano-silica is 1: 5.
A preparation method of an epoxy resin insulating plate comprises the following steps:
step S1: adding epoxy bisphenol A resin into a stirring kettle, stirring at the rotation speed of 300-;
step S2: and (4) adding the mixture prepared in the step S1, the reinforcing filler, the silicon dioxide and the calcium powder into a stirring kettle, stirring for 10-15min at the rotation speed of 800-1000r/min, adding into a mold, and curing at the temperature of 110-120 ℃ to obtain the epoxy resin insulating floor.
The invention has the beneficial effects that: the invention prepares an enhanced filler in the preparation of an epoxy resin insulation board, the enhanced filler takes graphite as a raw material and is oxidized by concentrated sulfuric acid, potassium permanganate and hydrogen peroxide in turn to prepare graphene oxide, bisphenol A is firstly reacted with chlorine to ensure that one hydrogen atom on a methyl group is replaced by a chlorine atom, an intermediate 1 is prepared under the action of potassium carbonate and tetraethylammonium bromide, the intermediate 1, formaldehyde and diaminodiphenylmethane are further reacted to prepare an intermediate 2, the graphene oxide and diaminodiphenylmethane are reacted under the action of 1-hydroxybenzotriazole, carboxyl on the surface of the graphene oxide is condensed with one amino group of the diaminodiphenylmethane to prepare modified graphene, the modified graphene, biphenyl tetracarboxylic dianhydride and diaminodiphenylmethane are subjected to polycondensation, and the intermediate 2 and the carboxyl on the side chain on the surface of the modified graphene are subjected to esterification reaction, preparing a reinforcing filler, mixing the reinforcing filler with epoxy resin, reacting amino groups on molecular chains on the surface of the reinforcing filler with epoxy groups to solidify the epoxy resin, improving the humidity resistance and heat resistance of the epoxy resin, simultaneously adding graphene to enhance the toughness of the epoxy resin, preparing an anti-aging filler, reacting benzyl chloride serving as a raw material to prepare an intermediate 3, reacting the intermediate 3 with benzene to prepare an intermediate 4, reacting the intermediate 4 with glacial acetic acid and lead acetate trihydrate to prepare an intermediate 5, further reacting the intermediate 5 with iron powder to prepare an intermediate 6, performing diazotization on cresol with o-amino groups to prepare an intermediate 7, reacting the intermediate 7 with phenylenediamine to prepare an intermediate 8, further reacting the intermediate 8 to prepare an intermediate 9, and sequentially reacting the intermediate 6, the intermediate 9 and propenyl amine with cyanuric chloride under temperature control, adding gamma-mercaptopropyl trimethoxy silane for reaction to prepare an intermediate 10, mixing the intermediate with nano silicon dioxide, hydrolyzing methoxyl to form silanol and forming hydrogen bonds with hydroxyl on the surface of the nano silicon dioxide to prepare the anti-aging filler, wherein the anti-aging filler is not easy to separate out from the epoxy resin insulation floor, the hydrogen bonds in molecules are destroyed, hydrogen bond rings are opened to form ionic compounds, the structure is unstable, redundant energy can be released by harmless heat energy to achieve a stable state, so that the hydrogen bonds are recovered to the original state, the epoxy resin insulation floor is protected from photochemical reaction, the aging resistance of the epoxy resin insulation board is effectively improved, the board is suitable for being used as a base material of floors and wallboards, and the surface can be pasted with various decoration materials and veneer treatments, such as pasting melamine paper decorative paper, wood veneer, PVC/PP color film, veneer, color film, And ink jet printing.
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
An epoxy resin insulation board comprises the following raw materials in parts by weight: 30 parts of epoxy bisphenol A type resin, 0.2 part of ethylene bis stearamide, 0.5 part of polyether defoaming agent GP, 5 parts of anti-aging filler, 8 parts of reinforcing filler, 3 parts of silicon dioxide and 3 parts of calcium powder;
the epoxy resin insulating floor is prepared by the following steps:
step S1: adding epoxy bisphenol A resin into a stirring kettle, stirring at the rotating speed of 300r/min, adding ethylene-based bis-stearamide, polyether defoaming agent GP and anti-aging filler, and stirring for 1h to prepare a mixture;
step S2: and (4) adding the mixture prepared in the step (S1), the reinforcing filler, the silicon dioxide and the calcium powder into a stirring kettle, stirring for 10min at the rotating speed of 800r/min, adding into a mold, and curing at a high temperature of 110 ℃ to prepare the epoxy resin insulation floor.
The reinforcing filler is prepared by the following steps:
step A1: adding concentrated sulfuric acid into a reaction kettle, stirring and adding graphite and sodium nitrate under the conditions that the rotating speed is 150r/min and the temperature is 1 ℃, stirring for 5min, adding potassium permanganate, heating to the temperature of 35 ℃, reacting for 20h, adding distilled water and a hydrogen peroxide solution under the temperature of 80 ℃, stirring for 1h, filtering to remove filtrate, washing a filter cake with deionized water until the pH value is 7, and drying to obtain graphene oxide;
step A2: dissolving bisphenol A in tetrahydrofuran, introducing chlorine, reacting for 20min under the condition of illumination, adding potassium carbonate, stirring until the potassium carbonate is completely dissolved under the condition of the rotation speed of 150r/min, adding tetraethylammonium bromide, performing reflux reaction for 1h under the condition of the temperature of 110 ℃ to prepare an intermediate 1, adding formaldehyde, chloroform, the intermediate 1 and diaminodiphenylmethane into a reaction kettle, and reacting for 4h under the conditions of the rotation speed of 150r/min and the temperature of 75 ℃ to prepare an intermediate 2;
step A3: dissolving diaminodiphenylmethane in acetone to prepare a diaminodiphenylmethane solution, adding half of the diaminodiphenylmethane solution and the graphene oxide prepared in the step A1 into a reaction kettle, stirring the mixture uniformly at the rotation speed of 200r/min, adding 1-hydroxybenzotriazole, reacting for 5 hours, filtering to remove filtrate, drying a filter cake to prepare modified graphene, dispersing the modified graphene in dimethylacetamide, adding biphenyltetracarboxylic dianhydride and the rest diaminodiphenylmethane solution at the rotation speed of 150r/min and the temperature of 0 ℃, reacting for 45 hours, adding the intermediate 2 prepared in the step A2 and a sulfuric acid solution, and reacting for 8 hours at the temperature of 160 ℃ to prepare the reinforcing filler.
The aging-resistant filler is prepared by the following steps:
step B1: adding benzyl chloride into a reaction kettle, stirring and dropwise adding mixed acid under the conditions that the rotating speed is 200r/min and the temperature is 20 ℃, stirring for 1.5 hours to prepare an intermediate 3, adding the intermediate 3, benzene and aluminum trichloride into the reaction kettle, reacting for 8 hours under the condition that the temperature is 80 ℃ to prepare an intermediate 4, adding the intermediate 4, glacial acetic acid and lead acetate trihydrate into the reaction kettle, dropwise adding nitric acid under the condition that the temperature is 100 ℃ to react for 5 hours to prepare an intermediate 5, adding the intermediate 5, iron powder and ethanol into the reaction kettle, performing reflux reaction for 3 hours under the condition that the temperature is 80 ℃, dropwise adding a hydrochloric acid solution, and continuing to react for 20 minutes to prepare an intermediate 6;
step B2: adding o-amino-p-cresol, deionized water and concentrated hydrochloric acid into a reaction kettle, adding dropwise added liquid under the conditions that the rotating speed is 200r/min and the temperature is 3 ℃ to react for 2 hours to obtain an intermediate 7, adding the intermediate 7 and an anhydrous sodium acetate solution into the m-phenylenediamine and a hydrochloric acid solution under the condition that the temperature is 1 ℃, dropwise adding for 20 minutes, heating to 25 ℃ after dropwise adding, continuing to react for 2 hours to obtain an intermediate 8, dissolving the intermediate 8 in methanol, adding a copper sulfate pentahydrate solution and ammonia water, and performing reflux reaction for 2 hours under the condition that the temperature is 110 ℃ to obtain an intermediate 9;
step B3: dissolving cyanuric chloride in acetone, adding the intermediate 6 and sodium acetate prepared in the step B1, reacting for 3h at the rotation speed of 120r/min and the temperature of 3 ℃, adding the intermediate 9 prepared in the step B2, reacting for 3h at the temperature of 40 ℃, adding propenyl amine, refluxing for 3h at the temperature of 80 ℃, adding gamma-mercaptopropyl trimethoxy silane and triethylamine, refluxing for 5h at the temperature of 115 ℃ to prepare an intermediate 10, dispersing nano silicon dioxide in an ethanol aqueous solution, adjusting the pH value of the solution to be 4, adding the intermediate 10, reacting for 3h at the temperature of 80 ℃, filtering to remove filtrate, and drying a filter cake to prepare the anti-aging filler.
Example 2
An epoxy resin insulation board comprises the following raw materials in parts by weight: 40 parts of epoxy bisphenol A type resin, 0.3 part of ethylene bis stearamide, 1 parts of polyether type defoaming agent GP, 6 parts of anti-aging filler, 9 parts of reinforcing filler, 4 parts of silicon dioxide and 4 parts of calcium powder;
the epoxy resin insulating floor is prepared by the following steps:
step S1: adding epoxy bisphenol A resin into a stirring kettle, stirring at the rotating speed of 300r/min, adding ethylene-based bis-stearamide, polyether defoaming agent GP and anti-aging filler, and stirring for 1.5h to obtain a mixture;
step S2: and (4) adding the mixture prepared in the step (S1), the reinforcing filler, the silicon dioxide and the calcium powder into a stirring kettle, stirring for 15min at the rotating speed of 800r/min, adding into a mold, and curing at a high temperature of 110 ℃ to prepare the epoxy resin insulation floor.
The reinforcing filler is prepared by the following steps:
step A1: adding concentrated sulfuric acid into a reaction kettle, stirring and adding graphite and sodium nitrate under the conditions that the rotating speed is 200r/min and the temperature is 1 ℃, stirring for 10min, adding potassium permanganate, heating to the temperature of 35 ℃, reacting for 25h, adding distilled water and a hydrogen peroxide solution under the temperature of 80 ℃, stirring for 1.5h, filtering to remove filtrate, washing a filter cake with deionized water until the pH value is 7, and drying to obtain graphene oxide;
step A2: dissolving bisphenol A in tetrahydrofuran, introducing chlorine, reacting for 20min under the condition of illumination, adding potassium carbonate, stirring until the potassium carbonate is completely dissolved under the condition of the rotation speed of 200r/min, adding tetraethylammonium bromide, performing reflux reaction for 1.5h under the condition of the temperature of 110 ℃ to prepare an intermediate 1, adding formaldehyde, chloroform, the intermediate 1 and diaminodiphenylmethane into a reaction kettle, and reacting for 4h under the conditions of the rotation speed of 150r/min and the temperature of 80 ℃ to prepare an intermediate 2;
step A3: dissolving diaminodiphenylmethane in acetone to prepare a diaminodiphenylmethane solution, adding half of the diaminodiphenylmethane solution and the graphene oxide prepared in the step A1 into a reaction kettle, stirring the mixture uniformly at the rotation speed of 300r/min, adding 1-hydroxybenzotriazole, reacting for 5 hours, filtering to remove filtrate, drying a filter cake to prepare modified graphene, dispersing the modified graphene in dimethylacetamide, adding biphenyltetracarboxylic dianhydride and the rest diaminodiphenylmethane solution at the rotation speed of 200r/min and the temperature of 0 ℃, reacting for 45 hours, adding the intermediate 2 prepared in the step A2 and a sulfuric acid solution, and reacting for 10 hours at the temperature of 160 ℃ to prepare the reinforcing filler.
The aging-resistant filler is prepared by the following steps:
step B1: adding benzyl chloride into a reaction kettle, stirring and dropwise adding mixed acid under the conditions that the rotating speed is 200r/min and the temperature is 25 ℃, stirring for 1.5 hours to prepare an intermediate 3, adding the intermediate 3, benzene and aluminum trichloride into the reaction kettle, reacting for 12 hours under the condition that the temperature is 80 ℃ to prepare an intermediate 4, adding the intermediate 4, glacial acetic acid and lead acetate trihydrate into the reaction kettle, dropwise adding nitric acid under the condition that the temperature is 100 ℃ to react for 8 hours to prepare an intermediate 5, adding the intermediate 5, iron powder and ethanol into the reaction kettle, carrying out reflux reaction for 5 hours under the condition that the temperature is 80 ℃, dropwise adding a hydrochloric acid solution, and continuing to react for 20 minutes to prepare an intermediate 6;
step B2: adding o-amino-p-cresol, deionized water and concentrated hydrochloric acid into a reaction kettle, adding dropwise added liquid under the conditions that the rotating speed is 300r/min and the temperature is 3 ℃ to react for 3 hours to obtain an intermediate 7, adding the intermediate 7 and an anhydrous sodium acetate solution into the m-phenylenediamine and a hydrochloric acid solution under the condition that the temperature is 1 ℃, dropwise adding for 30 minutes, heating to 25 ℃ after dropwise adding, continuing to react for 3 hours to obtain an intermediate 8, dissolving the intermediate 8 in methanol, adding a copper sulfate pentahydrate solution and ammonia water, and performing reflux reaction for 3 hours under the condition that the temperature is 110 ℃ to obtain an intermediate 9;
step B3: dissolving cyanuric chloride in acetone, adding the intermediate 6 and sodium acetate prepared in the step B1, reacting for 3h at the rotation speed of 120r/min and the temperature of 5 ℃, adding the intermediate 9 prepared in the step B2, reacting for 3h at the temperature of 50 ℃, adding propenyl amine, refluxing for 3h at the temperature of 90 ℃, adding gamma-mercaptopropyl trimethoxy silane and triethylamine, refluxing for 8h at the temperature of 115 ℃ to prepare an intermediate 10, dispersing nano silicon dioxide in an ethanol aqueous solution, adjusting the pH value of the solution to be 4, adding the intermediate 10, reacting for 3h at the temperature of 85 ℃, filtering to remove filtrate, and drying a filter cake to prepare the anti-aging filler.
Example 3
An epoxy resin insulation board comprises the following raw materials in parts by weight: 50 parts of epoxy bisphenol A type resin, 0.5 part of ethylene bis stearamide, 1.5 parts of polyether defoaming agent GP, 8 parts of anti-aging filler, 10 parts of reinforcing filler, 5 parts of silicon dioxide and 5 parts of calcium powder;
the epoxy resin insulating floor is prepared by the following steps:
step S1: adding epoxy bisphenol A resin into a stirring kettle, stirring at the rotating speed of 500r/min, adding ethylene-based bis-stearamide, polyether defoaming agent GP and anti-aging filler, and stirring for 1.5h to obtain a mixture;
step S2: and (4) adding the mixture prepared in the step (S1), the reinforcing filler, the silicon dioxide and the calcium powder into a stirring kettle, stirring for 15min at the rotating speed of 1000r/min, adding into a mold, and curing at high temperature at 120 ℃ to prepare the epoxy resin insulation floor.
The reinforcing filler is prepared by the following steps:
step A1: adding concentrated sulfuric acid into a reaction kettle, stirring and adding graphite and sodium nitrate under the conditions that the rotating speed is 200r/min and the temperature is 3 ℃, stirring for 10min, adding potassium permanganate, heating to 40 ℃, reacting for 25h, adding distilled water and a hydrogen peroxide solution under the condition that the temperature is 85 ℃, stirring for 1.5h, filtering to remove filtrate, washing a filter cake with deionized water until the pH value is 7, and drying to obtain graphene oxide;
step A2: dissolving bisphenol A in tetrahydrofuran, introducing chlorine, reacting for 30min under the condition of illumination, adding potassium carbonate, stirring until the potassium carbonate is completely dissolved under the condition of the rotation speed of 200r/min, adding tetraethylammonium bromide, performing reflux reaction for 1.5h under the condition of the temperature of 120 ℃ to prepare an intermediate 1, adding formaldehyde, chloroform, the intermediate 1 and diaminodiphenylmethane into a reaction kettle, and reacting for 6h under the conditions of the rotation speed of 200r/min and the temperature of 80 ℃ to prepare an intermediate 2;
step A3: dissolving diaminodiphenylmethane in acetone to prepare a diaminodiphenylmethane solution, adding half of the diaminodiphenylmethane solution and the graphene oxide prepared in the step A1 into a reaction kettle, stirring the mixture uniformly at the rotation speed of 300r/min, adding 1-hydroxybenzotriazole, reacting for 8 hours, filtering to remove filtrate, drying a filter cake to prepare modified graphene, dispersing the modified graphene in dimethylacetamide, adding biphenyltetracarboxylic dianhydride and the rest diaminodiphenylmethane solution at the rotation speed of 200r/min and the temperature of 0 ℃, reacting for 50 hours, adding the intermediate 2 prepared in the step A2 and a sulfuric acid solution, and reacting for 10 hours at the temperature of 160 ℃ to prepare the reinforcing filler.
The aging-resistant filler is prepared by the following steps:
step B1: adding benzyl chloride into a reaction kettle, stirring and dropwise adding mixed acid under the conditions that the rotating speed is 300r/min and the temperature is 25 ℃, stirring for 1.5 hours to prepare an intermediate 3, adding the intermediate 3, benzene and aluminum trichloride into the reaction kettle, reacting for 12 hours under the condition that the temperature is 85 ℃ to prepare an intermediate 4, adding the intermediate 4, glacial acetic acid and lead acetate trihydrate into the reaction kettle, dropwise adding nitric acid under the condition that the temperature is 110 ℃ to react for 8 hours to prepare an intermediate 5, adding the intermediate 5, iron powder and ethanol into the reaction kettle, carrying out reflux reaction for 5 hours under the condition that the temperature is 85 ℃, dropwise adding a hydrochloric acid solution, and continuing to react for 30 minutes to prepare an intermediate 6;
step B2: adding o-amino-p-cresol, deionized water and concentrated hydrochloric acid into a reaction kettle, adding dropwise added liquid under the conditions that the rotating speed is 300r/min and the temperature is 5 ℃ to react for 3 hours to obtain an intermediate 7, adding the intermediate 7 and an anhydrous sodium acetate solution into the m-phenylenediamine and a hydrochloric acid solution under the temperature of 3 ℃, dropwise adding for 30 minutes, heating to 30 ℃ after dropwise adding, continuing to react for 3 hours to obtain an intermediate 8, dissolving the intermediate 8 in methanol, adding a copper sulfate pentahydrate solution and ammonia water, and performing reflux reaction for 3 hours under the temperature of 120 ℃ to obtain an intermediate 9;
step B3: dissolving cyanuric chloride in acetone, adding the intermediate 6 and sodium acetate prepared in the step B1, reacting for 5 hours at the rotation speed of 150r/min and the temperature of 5 ℃, adding the intermediate 9 prepared in the step B2, reacting for 5 hours at the temperature of 50 ℃, adding propenyl amine, refluxing for 5 hours at the temperature of 90 ℃, adding gamma-mercaptopropyl trimethoxy silane and triethylamine, refluxing for 8 hours at the temperature of 115 ℃ to prepare an intermediate 10, dispersing nano silicon dioxide in an ethanol aqueous solution, adjusting the pH value of the solution to be 5, adding the intermediate 10, reacting for 5 hours at the temperature of 85 ℃, filtering to remove filtrate, and drying a filter cake to prepare the anti-aging filler.
Comparative example
The comparison example is a common epoxy resin insulation floor in the market.
The epoxy resin insulation floorings manufactured in examples 1 to 3 and the comparative example were subjected to a performance test, the test results of which are shown in table 1 below;
moisture and heat resistance: the epoxy resin floors prepared in examples 1 to 3 and comparative example were tested for mechanical properties, and then the epoxy resin floors were soaked in water at 70 ℃ for 30, 50, 80 hours, and again tested for a decrease in mechanical properties.
Aging resistance: the epoxy resin floors prepared in examples 1 to 3 and comparative example were tested for mechanical properties using a wavelength of 340nm and a pre-irradiation degree of 0.68W/m2The temperature of the blackboard is 60 ℃, and the condensation temperature is 60 ℃; a single cycle process; illuminating for 3h, and blowing for 10 min; the circulation process is repeated continuously, and the total experiment time is 168 h; after aging, the mechanical properties were tested for degradation.
TABLE 1
As can be seen from Table 1, the epoxy resin flooring obtained in examples 1-3 shows no decrease in mechanical strength after being tested for resistance to humidity and heat and aging, while the epoxy resin flooring obtained in comparative example shows a decrease in mechanical strength after being tested for resistance to humidity and heat and aging, indicating that the present invention has excellent resistance to humidity and heat and aging.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (7)
1. An epoxy resin insulation board is characterized in that: the feed comprises the following raw materials in parts by weight: 30-50 parts of epoxy bisphenol A type resin, 0.2-0.5 part of dispersant, 0.5-1.5 parts of defoamer, 5-8 parts of anti-aging filler, 8-10 parts of reinforcing filler, 3-5 parts of silicon dioxide and 3-5 parts of calcium powder;
the epoxy resin insulating floor is prepared by the following steps:
step S1: adding epoxy bisphenol A resin into a stirring kettle, stirring at the rotation speed of 300-;
step S2: and (4) adding the mixture prepared in the step S1, the reinforcing filler, the silicon dioxide and the calcium powder into a stirring kettle, stirring for 10-15min at the rotation speed of 800-1000r/min, adding into a mold, and curing at the temperature of 110-120 ℃ to obtain the epoxy resin insulating floor.
2. The epoxy resin insulating board as claimed in claim 1, wherein: the dispersing agent is one or a mixture of more of ethylene bis stearamide, tristearin and stearic acid monoglyceride in any proportion, and the defoaming agent is one of polyether defoaming agent GP, polyether defoaming agent GPE and polyether defoaming agent GPES.
3. The epoxy resin insulating board as claimed in claim 1, wherein: the reinforcing filler is prepared by the following steps:
step A1: adding concentrated sulfuric acid into a reaction kettle, stirring and adding graphite and sodium nitrate under the conditions that the rotating speed is 150-200r/min and the temperature is 1-3 ℃, stirring for 5-10min, adding potassium permanganate, heating to the temperature of 35-40 ℃, reacting for 20-25h, adding distilled water and a hydrogen peroxide solution under the temperature of 80-85 ℃, stirring for 1-1.5h, filtering to remove filtrate, washing a filter cake with deionized water until the pH value is 7, and drying to obtain graphene oxide;
step A2: dissolving bisphenol A in tetrahydrofuran, introducing chlorine, reacting for 20-30min under the condition of illumination, adding potassium carbonate, stirring under the condition of the rotation speed of 150-;
step A3: dissolving diaminodiphenylmethane in acetone to obtain diaminodiphenylmethane solution, adding half of the diaminodiphenylmethane solution and the graphene oxide prepared in the step A1 into a reaction kettle, stirring the mixture to be uniform at the rotation speed of 200-300r/min, adding 1-hydroxy benzotriazole, reacting for 5-8h, filtering to remove filtrate, oven drying the filter cake to obtain modified graphene, dispersing the modified graphene in dimethylacetamide, under the conditions that the rotation speed is 150-, and reacting for 8-10h at the temperature of 160 ℃ to obtain the reinforcing filler.
4. The epoxy resin insulating board as claimed in claim 3, wherein: the use amount ratio of the concentrated sulfuric acid, the graphite, the sodium nitrate, the potassium permanganate, the distilled water and the hydrogen peroxide solution in the step A1 is 50mL:2g: 1g: 6g: 15mL of 6mL of concentrated sulfuric acid, 98% of concentrated sulfuric acid by mass, 30% of hydrogen peroxide solution by mass, 1mol of 1: 1mol of 9mL of 2mL of the bisphenol A, chlorine, potassium carbonate and tetraethylammonium bromide in the step A2, 4:1:1 of the formaldehyde, the intermediate 1 and diaminodiphenylmethane in a molar ratio, 20% of the diaminodiphenylmethane solution in the step A3, 10mL of the diaminodiphenylmethane solution, 3g of the graphene oxide and 1-hydroxybenzotriazole in the modified graphene, 0.5g of the modified graphene, 1.5g of the biphenyltetracarboxylic dianhydride, 6mL of the diaminodiphenylmethane solution, the intermediate 2 and the sulfuric acid solution, and 30-35% of the sulfuric acid solution.
5. The epoxy resin insulating board as claimed in claim 1, wherein: the aging-resistant filler is prepared by the following steps:
step B1: adding benzyl chloride into a reaction kettle, stirring and dropwise adding mixed acid under the conditions that the rotation speed is 200-25 ℃ and the temperature is 20-25 ℃ for 1.5h to prepare an intermediate 3, adding the intermediate 3, benzene and aluminum trichloride into the reaction kettle, reacting for 8-12h under the condition that the temperature is 80-85 ℃ to prepare an intermediate 4, adding the intermediate 4, glacial acetic acid and lead acetate trihydrate into the reaction kettle, dropwise adding nitric acid under the condition that the temperature is 100-110 ℃ to react for 5-8h to prepare an intermediate 5, adding the intermediate 5, iron powder and ethanol into the reaction kettle, performing reflux reaction for 3-5h under the condition that the temperature is 80-85 ℃, dropwise adding a hydrochloric acid solution, and continuing to react for 20-30min to prepare an intermediate 6;
step B2: adding o-amino-p-cresol, deionized water and concentrated hydrochloric acid into a reaction kettle, adding a dropping liquid under the conditions that the rotation speed is 200-5 ℃ and the temperature is 3-5 ℃ to react for 2-3h to obtain an intermediate 7, adding the intermediate 7 and an anhydrous sodium acetate solution into m-phenylenediamine and hydrochloric acid solution under the temperature of 1-3 ℃, dropping for 20-30min, heating to 25-30 ℃ after dropping, continuing to react for 2-3h to obtain an intermediate 8, dissolving the intermediate 8 into methanol, adding a copper sulfate pentahydrate solution and ammonia water, and performing reflux reaction for 2-3h at the temperature of 110-120 ℃ to obtain an intermediate 9;
step B3: dissolving cyanuric chloride in acetone, adding the intermediate 6 and sodium acetate prepared in the step B1, reacting for 3-5h at the rotation speed of 120-150r/min and the temperature of 3-5 ℃, adding the intermediate 9 prepared in the step B2, reacting for 3-5h at the temperature of 40-50 ℃, adding propenyl amine, refluxing for 3-5h at the temperature of 80-90 ℃, adding gamma-mercaptopropyl trimethoxysilane and triethylamine, refluxing for 5-8h at the temperature of 115 ℃ to prepare an intermediate 10, dispersing nano silicon dioxide in an ethanol aqueous solution, adjusting the pH value of the solution to 4-5, adding the intermediate 10, reacting for 3-5h at the temperature of 80-85 ℃, filtering to remove filtrate, and drying the filter cake to obtain the anti-aging filler.
6. The epoxy resin insulating board as claimed in claim 5, wherein: the dosage mass ratio of the benzyl chloride and the mixed acid in the step B1 is 2:1, the mixed acid is formed by mixing nitric acid with the mass fraction of 97% and sulfuric acid with the mass fraction of 98% in a molar ratio of 2:1, the dosage ratio of the intermediate 3, benzene and aluminum trichloride is 1g:10.2mL:1g, the dosage ratio of the intermediate 4, glacial acetic acid, lead acetate trihydrate and nitric acid is 2.5g:20mL:0.025g:2g, the mass fraction of the nitric acid is 97%, the dosage ratio of the intermediate 5, iron powder, ethanol and hydrochloric acid solution is 2.8g:4.5g:60mL:200mL, the hydrochloric acid solution is formed by mixing hydrochloric acid with the mass fraction of 38% and ethanol with the mass fraction of 95% in a volume ratio of 1:9, the dosage ratio of the o-amino-p-cresol, deionized water, concentrated hydrochloric acid and dropping liquid in the step B2 is 1.1g:15mL:2mL, the concentration of the concentrated hydrochloric acid is 25%, and the sodium sulfite and the dropping liquid is copper sulfate and the copper sulfate, Mixing deionized water with the use amount of 0.7g:0.04g:50mL, mixing m-phenylenediamine, a hydrochloric acid solution, an intermediate 7 and an anhydrous sodium acetate solution with the use amount ratio of 1.08g:20mL:2.3g:10mL, the mass fraction of the anhydrous sodium acetate solution is 40%, the use amount ratio of an intermediate 8, a blue vitriod solution and ammonia water is 1g:3mL:5mL, the mass fraction of the blue vitriod solution is 35%, the mass fraction of the ammonia water is 25%, the use amount molar ratio of cyanuric chloride, sodium acetate, an intermediate 6, an intermediate 9, allylamine and gamma-mercaptopropyltrimethoxysilane described in step B3 is 1:1:1:1:1:1, the use amount of triethylamine is 20-30% of the gamma-mercaptopropyltrimethoxysilane, and the use amount mass ratio of the intermediate 10 and the nano silicon dioxide is 1: 5.
7. The preparation method of the epoxy resin insulation board as claimed in claim 1, wherein the method comprises the following steps: the method specifically comprises the following steps:
step S1: adding epoxy bisphenol A resin into a stirring kettle, stirring at the rotation speed of 300-;
step S2: and (4) adding the mixture prepared in the step S1, the reinforcing filler, the silicon dioxide and the calcium powder into a stirring kettle, stirring for 10-15min at the rotation speed of 800-1000r/min, adding into a mold, and curing at the temperature of 110-120 ℃ to obtain the epoxy resin insulating floor.
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