CN118496738A - Flame-retardant high-insulation epoxy composite material and preparation method thereof - Google Patents
Flame-retardant high-insulation epoxy composite material and preparation method thereof Download PDFInfo
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- CN118496738A CN118496738A CN202410932820.8A CN202410932820A CN118496738A CN 118496738 A CN118496738 A CN 118496738A CN 202410932820 A CN202410932820 A CN 202410932820A CN 118496738 A CN118496738 A CN 118496738A
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 239000003063 flame retardant Substances 0.000 title claims abstract description 77
- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 239000004593 Epoxy Substances 0.000 title claims abstract description 50
- 238000009413 insulation Methods 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 28
- 239000012745 toughening agent Substances 0.000 claims abstract description 26
- 239000000945 filler Substances 0.000 claims abstract description 17
- 239000013530 defoamer Substances 0.000 claims abstract description 13
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 238000001125 extrusion Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 238000012216 screening Methods 0.000 claims description 7
- CLFRCXCBWIQVRN-UHFFFAOYSA-N 2,5-dihydroxybenzaldehyde Chemical compound OC1=CC=C(O)C(C=O)=C1 CLFRCXCBWIQVRN-UHFFFAOYSA-N 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- BSYJHYLAMMJNRC-UHFFFAOYSA-N 2,4,4-trimethylpentan-2-ol Chemical compound CC(C)(C)CC(C)(C)O BSYJHYLAMMJNRC-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000005054 phenyltrichlorosilane Substances 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- ORVMIVQULIKXCP-UHFFFAOYSA-N trichloro(phenyl)silane Chemical compound Cl[Si](Cl)(Cl)C1=CC=CC=C1 ORVMIVQULIKXCP-UHFFFAOYSA-N 0.000 claims description 3
- YSWBFLWKAIRHEI-UHFFFAOYSA-N 4,5-dimethyl-1h-imidazole Chemical group CC=1N=CNC=1C YSWBFLWKAIRHEI-UHFFFAOYSA-N 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 239000012065 filter cake Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 3
- 238000000576 coating method Methods 0.000 abstract description 5
- 239000000843 powder Substances 0.000 abstract description 5
- 239000003822 epoxy resin Substances 0.000 description 11
- 229920000647 polyepoxide Polymers 0.000 description 11
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical field of powder coatings, and discloses a flame-retardant high-insulation epoxy composite material and a preparation method thereof. The flame-retardant high-insulation epoxy composite material comprises A, B components, wherein the component A comprises the following components in parts by weight: 70-90 parts of bisphenol A epoxy resin, 30-40 parts of filler, 2-3 parts of flatting agent, 2-3 parts of accelerator, 0.7-1.2 parts of defoamer and 5-8 parts of flame retardant toughening agent; the component B is 6.5-8.5 parts of accelerated dicyandiamide curing agent. The flame-retardant high-insulation epoxy composite material prepared by the invention has good mechanical property, flame retardance and insulativity, and has good application prospect.
Description
Technical Field
The invention belongs to the technical field of powder coating, and particularly relates to a flame-retardant high-insulation epoxy composite material and a preparation method thereof.
Background
The powder coating is a solid powder synthetic resin coating composed of solid resin, pigment, filler, auxiliary agent and the like. Unlike common solvent type paint and water paint, the powder paint has dispersion medium of air rather than solvent and water. The epoxy resin (EP) has the characteristics of no solvent pollution, 100% film formation, low energy consumption and the like, and is widely applied to various fields of electronics, coatings, adhesives and the like due to the excellent mechanical properties, good corrosion resistance and excellent adhesion capability. However, in view of the rapid development of communication technology, the demand for epoxy resins (EP) has arisen for complementary properties such as excellent thermal properties, low relative dielectric constant, low dissipation factor, flame retardancy, etc. Accordingly, there is an urgent need for an epoxy composite material having good flame retardancy and insulation properties, which has solved the above problems.
Disclosure of Invention
The invention aims to provide a flame-retardant high-insulation epoxy composite material and a preparation method thereof, which are used for solving the technical problems of poor flame retardance and insulation of the epoxy composite material in the prior art.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the technical scheme provided by the invention is as follows:
In a first aspect, the invention provides a flame-retardant high-insulation epoxy composite material, which comprises A, B components, wherein the component A comprises the following components in parts by weight: 70-90 parts of bisphenol A epoxy resin, 30-40 parts of filler, 2-3 parts of flatting agent, 2-3 parts of accelerator, 0.7-1.2 parts of defoamer and 5-8 parts of flame retardant toughening agent; the component B is 6.5-8.5 parts of accelerated dicyandiamide curing agent.
Preferably, the preparation method of the flame retardant toughening agent comprises the following steps:
S1, adding 12.9-26g of para-aminotrifluorotoluene and 11-22g of 2, 5-dihydroxybenzaldehyde into 100-200mL of ethanol, stirring for 3-5h, filtering, washing filter residues with ethanol for 3-5 times, adding the filter residues into 200-400mL of ethanol, heating at 75-85 ℃ for 30-50min, adding 17.3-34.6g of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide at 75-85 ℃, continuously stirring for 20-28h, filtering while the mixture is hot, washing filter cakes with ethanol for 3-5 times, and finally vacuum drying at 55-65 ℃ for 24-36h to obtain an intermediate;
The structural formula of the intermediate is as follows:
Wherein, mass spectrometry analysis is carried out on the intermediate, HRMS (ESI) m/z:483.08 (100.0%), 484.09 (27.4%), 485.09 (4.5%).
S2, adding 14.5-29g of the intermediate and 4.1-8.2g of triethylamine into 50-100mL of N, N-dimethylformamide under the atmosphere of nitrogen to obtain a mixed solution; then 2.8-5.6g of phenyl trichlorosilane is dissolved in 40-80mL of tetrahydrofuran, and is slowly added into the mixed solution through a instillation funnel, stirred at room temperature for 2-4h, stirred at 45-55 ℃ for 1-3h, filtered, rotary evaporated at 85-95 ℃ and finally dried in vacuum at 85-95 ℃ for 20-28h, thus obtaining the flame retardant toughening agent.
The structural formula of the flame retardant toughening agent is as follows:
Preferably, the filler is compounded by titanium dioxide, silicon micropowder and light calcium carbonate in a mass ratio of (10-12): (3-5): (3-4).
Preferably, the accelerator is dimethylimidazole.
Preferably, the defoamer is a polyoxyethylene polyoxypropylene alcohol amine ether defoamer.
Preferably, the curing agent is an accelerated dicyandiamide curing agent.
Preferably, the leveling agent is a PV88 leveling agent.
In a second aspect, the invention also provides a preparation method of the flame-retardant high-insulation epoxy composite material, which comprises the following steps:
Adding 70-90 parts of bisphenol A epoxy resin, 30-40 parts of filler, 2-3 parts of flatting agent, 2-3 parts of accelerator, 0.7-1.2 parts of defoamer and 5-8 parts of flame retardant toughening agent into a mixer for premixing, and then adopting a double screw extruder for mixing extrusion, cooling, tabletting, crushing, grinding and screening after extrusion to prepare a component A; 6.5-8.5 parts of accelerating dicyandiamide curing agent;
and (2) uniformly mixing the component A and the component B to obtain the flame-retardant high-insulation epoxy composite material.
The heating temperature of the extruder is 90-110 ℃.
Preferably, the D50 particle size of the flame-retardant high-insulation epoxy composite material is 30-40 mu m.
In summary, due to the adoption of the technical scheme, the beneficial effects of the invention are as follows:
1. The fluorine functional group in the flame retardant toughening agent prepared by the invention can reduce the surface tension of the flame retardant high-insulation epoxy composite material, enhance the hydrophobicity and reduce the water content, thereby reducing the dielectric constant and the dielectric loss; meanwhile, the increase of free volume provided by the intramolecular cavity of the flame retardant toughening agent reduces the density of polarized molecules, si-C bonds reduce the polarizability of matrix resin, the dielectric constant and dielectric loss of the flame retardant high-insulation epoxy composite material are reduced cooperatively, and the insulating property of the flame retardant high-insulation epoxy composite material is improved cooperatively with insulating filler.
2. The flame retardant toughening agent is thermally decomposed in a gas phase to generate phosphorus-containing free radicals, wherein the phosphorus-containing free radicals comprise PO2 </SUB > and PO </SUB >, the combustion free radicals are captured, the combustible hydrocarbon is reduced, and meanwhile, the flame retardant toughening agent is decomposed to generate nonflammable gas, comprising NH 3, N 2 and HF, and has flame retardant effect in the gas phase; the flame retardant toughening agent is thermally decomposed in the condensed phase to generate phosphoric acid derivatives, so that the development of an expanded carbon layer is promoted, and the P and Si elements promote the flame retardant high-insulation epoxy composite material to form a continuous and compact hybrid carbon layer in the combustion process, so that the combustion in the condensed phase is effectively hindered; the synergistic flame retardance of P, N, si elements enhances the gas phase and condensed phase flame retardance, so that the flame-retardant high-insulation epoxy composite material achieves the balance of fire safety and smoke suppression.
3. According to the invention, the impact strength of the flame-retardant high-insulation epoxy composite material is improved by increasing the free volume of the flame-retardant toughening agent and increasing the Si-O flexible bond, and the flame-retardant toughening agent is uniformly distributed in the matrix resin through covalent bonds and hydrogen bonds formed between terminal hydroxyl groups and the epoxy resin, so that the interface binding force with the epoxy resin is enhanced; meanwhile, the addition of the rigid groups improves the tensile strength and the bending strength of the flame-retardant high-insulation epoxy composite material; the combined action of rich rigid groups, si-O flexible chain segments, increased free volume and good interface bonding is cooperated with the composite filler to improve the strength and toughness of the flame-retardant high-insulation epoxy composite material.
4. The flame-retardant high-insulation epoxy composite material prepared by the invention has the advantages of high solid content, safety, environmental protection, good film forming property, 500 mu m of one film forming, capability of meeting the performance requirement of single spraying, excellent wear resistance, high Shore hardness, annual average friction loss of only 0.012 percent, excellent water resistance, capability of keeping performance under the conditions of long-term high humidity or soaking water, good adhesiveness, capability of being effectively attached to the outside of equipment, no peeling and falling off, excellent flame resistance and excellent insulating property.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a preparation process of the flame retardant high insulation epoxy composite material of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described 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
The embodiment discloses a preparation method of a flame retardant toughening agent, which comprises the following steps:
S1, adding 19.5g of para-aminotrifluorotoluene and 15.5g of 2, 5-dihydroxybenzaldehyde into 150mL of ethanol, stirring for 4 hours, filtering, washing filter residues with ethanol for 4 times, adding the filter residues into 300mL of ethanol, heating at 80 ℃ for 40 minutes, adding 26g of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide at 80 ℃, continuously stirring for 24 hours, filtering while the mixture is hot, washing the filter residues with ethanol for 4 times, and finally drying in vacuum at 60 ℃ for 30 hours to obtain an intermediate;
S2, adding 21.8g of intermediate and 6.2g of triethylamine into 75mL of N, N-dimethylformamide under nitrogen atmosphere to obtain a mixed solution; then 4.2g of phenyl trichlorosilane is dissolved in 60mL of tetrahydrofuran, and is slowly added into the mixed solution through a dropping funnel, stirred at room temperature for 3h, then stirred at 50 ℃ for 2h, filtered, and rotary evaporated at 90 ℃, and finally vacuum dried at 90 ℃ for 24h, thus obtaining the flame retardant toughening agent.
Example 2
Referring to fig. 1, the embodiment discloses a preparation method of a flame-retardant high-insulation epoxy composite material, which comprises the following steps:
adding 80g of bisphenol A type epoxy resin, 35g of filler, 2.5g of flatting agent, 2.5g of accelerator, 0.9g of defoaming agent and 7g of flame retardant toughening agent into a mixer for premixing, and then adopting a double-screw extruder for mixing extrusion at 100 ℃, cooling, tabletting, crushing, grinding and screening after extrusion to prepare a component A; 7.5g of accelerating dicyandiamide curing agent;
and (2) uniformly mixing the component A and the component B to obtain the flame-retardant high-insulation epoxy composite material.
Example 3
Referring to fig. 1, the embodiment discloses a preparation method of a flame-retardant high-insulation epoxy composite material, which comprises the following steps:
Adding 70g of bisphenol A type epoxy resin, 40g of filler, 2g of flatting agent, 3g of accelerator, 0.7g of defoamer and 8g of flame retardant toughening agent into a mixer for premixing, then adopting a double-screw extruder for mixing extrusion at 90 ℃, and cooling, tabletting, crushing, grinding and screening after extrusion to prepare a component A; the component B is 8.5g of accelerated dicyandiamide curing agent;
and (2) uniformly mixing the component A and the component B to obtain the flame-retardant high-insulation epoxy composite material.
Example 4
Referring to fig. 1, the embodiment discloses a preparation method of a flame-retardant high-insulation epoxy composite material, which comprises the following steps:
Adding 90g of bisphenol A type epoxy resin, 30g of filler, 3g of flatting agent, 2g of accelerator, 1.2g of defoamer and 5g of flame retardant toughening agent into a mixer for premixing, then adopting a double screw extruder for mixing extrusion at 90-110 ℃, and cooling, tabletting, crushing, grinding and screening after extrusion to prepare a component A; 6.5-8.5g of accelerating dicyandiamide curing agent;
and (2) uniformly mixing the component A and the component B to obtain the flame-retardant high-insulation epoxy composite material.
Example 5
Referring to fig. 1, the embodiment discloses a preparation method of a flame-retardant high-insulation epoxy composite material, which comprises the following steps:
Adding 75g of bisphenol A type epoxy resin, 48g of filler, 2.2g of flatting agent, 2.8g of accelerator, 0.8g of defoamer and 7g of flame retardant toughening agent into a mixer for premixing, and then adopting a double-screw extruder for mixing extrusion at 95 ℃, cooling, tabletting, crushing, grinding and screening after extrusion to prepare a component A; the component B is 8g of accelerating dicyandiamide curing agent;
and (2) uniformly mixing the component A and the component B to obtain the flame-retardant high-insulation epoxy composite material.
Example 6
Referring to fig. 1, the embodiment discloses a preparation method of a flame-retardant high-insulation epoxy composite material, which comprises the following steps:
Adding 85g of bisphenol A type epoxy resin, 32g of filler, 2.8g of flatting agent, 2.2g of accelerator, 1.1g of defoamer and 6g of flame retardant toughening agent into a mixer for premixing, and then adopting a double-screw extruder for mixing extrusion at 105 ℃, cooling, tabletting, crushing, grinding and screening after extrusion to prepare a component A; the component B is 7g of accelerating dicyandiamide curing agent;
and (2) uniformly mixing the component A and the component B to obtain the flame-retardant high-insulation epoxy composite material.
Comparative example 1
Comparative example 1 compared with example 2, comparative example 1 was free of flame retardant toughening agent added during the preparation of flame retardant high insulation epoxy composite material, and the other conditions were unchanged.
Comparative example 2
Comparative example 2 in comparison with example 2, comparative example 2 was free of filler added during the preparation of the flame retardant highly insulating epoxy composite material, and the other conditions were unchanged.
Experimental example
The performance of the flame retardant high insulation epoxy composite materials prepared in examples 2-6 and comparative examples 1-2, respectively, was tested as A, B, C, D, E, F, G, and the AB component was stirred uniformly during the test (spraying vertical height was more than 10m, ethanol diluent was added to the material, in principle 90-100mL/kg was added), the air valve was opened, the air pressure was adjusted (tank air pressure represents 0.3, air outlet air pressure represents 0.2), and the spray head was about 10-15cm from the spray point. The spray head is not kept for too long in spraying, and in principle, the spray head is sprayed back and forth, the residence time in one point is not more than 2s, and the test standard and the test result are shown in table 1:
As shown in the test results of Table 1, the flame-retardant high-insulation epoxy composite material prepared in the embodiment 2 of the invention has good insulativity, mechanical property and flame retardance. As can be seen from the comparison of the comparative example 1 and the example 2, the flame retardant toughening agent is added in the invention, so that the insulativity, the mechanical property and the flame retardant property of the flame retardant high-insulation epoxy composite material can be improved; as can be seen from the comparison of the comparative example 2 and the example 3, the addition of the filler in the invention can improve the insulativity, the mechanical property and the flame retardant property of the flame retardant high-insulation epoxy composite material.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (9)
1. The flame-retardant high-insulation epoxy composite material is characterized by comprising A, B components, wherein the component A comprises the following components in parts by weight: 70-90 parts of bisphenol A epoxy resin, 30-40 parts of filler, 2-3 parts of flatting agent, 2-3 parts of accelerator, 0.7-1.2 parts of defoamer and 5-8 parts of flame retardant toughening agent; the component B is 6.5-8.5 parts of accelerated dicyandiamide curing agent.
2. The flame retardant high insulation epoxy composite of claim 1, wherein the method of preparing the flame retardant toughening agent comprises the steps of:
S1, adding 12.9-26g of para-aminotrifluorotoluene and 11-22g of 2, 5-dihydroxybenzaldehyde into 100-200mL of ethanol, stirring for 3-5h, filtering, washing filter residues with ethanol for 3-5 times, adding the filter residues into 200-400mL of ethanol, heating at 75-85 ℃ for 30-50min, adding 17.3-34.6g of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide at 75-85 ℃, continuously stirring for 20-28h, filtering while the mixture is hot, washing filter cakes with ethanol for 3-5 times, and finally vacuum drying at 55-65 ℃ for 24-36h to obtain an intermediate;
s2, adding 14.5-29g of the intermediate and 4.1-8.2g of triethylamine into 50-100mL of N, N-dimethylformamide under the atmosphere of nitrogen to obtain a mixed solution; then 2.8-5.6g of phenyl trichlorosilane is dissolved in 40-80mL of tetrahydrofuran, and is slowly added into the mixed solution through a instillation funnel, stirred at room temperature for 2-4h, stirred at 45-55 ℃ for 1-3h, filtered, rotary evaporated at 85-95 ℃ and finally dried in vacuum at 85-95 ℃ for 20-28h, thus obtaining the flame retardant toughening agent.
3. The flame-retardant high-insulation epoxy composite material according to claim 1, wherein the filler is compounded by titanium dioxide, silicon micropowder and light calcium carbonate in a mass ratio of (10-12): 3-5): 3-4.
4. The flame retardant high insulation epoxy composite of claim 1, wherein the accelerator is dimethylimidazole.
5. The flame retardant high insulation epoxy composite of claim 1, wherein the defoamer is a polyoxyethylene polyoxypropylene alcohol amine ether defoamer.
6. The flame retardant high insulation epoxy composite of claim 1, wherein the curing agent is an accelerated dicyandiamide type curing agent.
7. The flame retardant high insulation epoxy composite of claim 1, wherein the leveling agent is a PV88 leveling agent.
8. A method of preparing a flame retardant highly insulating epoxy composite material according to any one of claims 1 to 7, comprising the steps of:
Adding 70-90 parts of bisphenol A epoxy resin, 30-40 parts of filler, 2-3 parts of flatting agent, 2-3 parts of accelerator, 0.7-1.2 parts of defoamer and 5-8 parts of flame retardant toughening agent into a mixer for premixing, and then adopting a double screw extruder for mixing extrusion, cooling, tabletting, crushing, grinding and screening after extrusion to prepare a component A; 6.5-8.5 parts of accelerating dicyandiamide curing agent;
and (2) uniformly mixing the component A and the component B to obtain the flame-retardant high-insulation epoxy composite material.
9. The method for preparing a flame retardant high insulation epoxy composite material according to claim 8, wherein the heating temperature of the extruder is 90-110 ℃; the D50 particle size of the flame-retardant high-insulation epoxy composite material is 30-40 mu m.
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| CN103059516A (en) * | 2013-01-08 | 2013-04-24 | 天津市凯华绝缘材料有限公司 | Fast-cure epoxy powder composition |
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| EP3272795A1 (en) * | 2016-07-21 | 2018-01-24 | Guangdong Guangshan New Materials Co., Ltd. | Flame retardant resin composition, thermosetting resin composition, composite metal substrate and flame retardant electronic material |
| CN110760244A (en) * | 2019-11-20 | 2020-02-07 | 应急管理部四川消防研究所 | An epoxy-based steel structure fireproof coating |
| CN116948494A (en) * | 2023-06-20 | 2023-10-27 | 广东傲博新材料有限公司 | Insulating flame-retardant and corrosion-resistant powder coating for batteries and preparation method thereof |
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| CN103059516A (en) * | 2013-01-08 | 2013-04-24 | 天津市凯华绝缘材料有限公司 | Fast-cure epoxy powder composition |
| CN104789106A (en) * | 2015-03-30 | 2015-07-22 | 广西吉宽太阳能设备有限公司 | Water-soluble polyurethane flame-retardant coating and preparation method thereof |
| EP3272795A1 (en) * | 2016-07-21 | 2018-01-24 | Guangdong Guangshan New Materials Co., Ltd. | Flame retardant resin composition, thermosetting resin composition, composite metal substrate and flame retardant electronic material |
| CN110760244A (en) * | 2019-11-20 | 2020-02-07 | 应急管理部四川消防研究所 | An epoxy-based steel structure fireproof coating |
| CN116948494A (en) * | 2023-06-20 | 2023-10-27 | 广东傲博新材料有限公司 | Insulating flame-retardant and corrosion-resistant powder coating for batteries and preparation method thereof |
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