CN107698936A - Fire-retardant epoxy resin composition, fire-retardant epoxy resin material and preparation method thereof - Google Patents
Fire-retardant epoxy resin composition, fire-retardant epoxy resin material and preparation method thereof Download PDFInfo
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- CN107698936A CN107698936A CN201710723960.4A CN201710723960A CN107698936A CN 107698936 A CN107698936 A CN 107698936A CN 201710723960 A CN201710723960 A CN 201710723960A CN 107698936 A CN107698936 A CN 107698936A
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- Prior art keywords
- epoxy resin
- fire
- retardant
- retardant epoxy
- resin composition
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- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 146
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 141
- 239000003063 flame retardant Substances 0.000 title claims abstract description 88
- 239000000203 mixture Substances 0.000 title claims abstract description 60
- 239000000463 material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 81
- 239000011256 inorganic filler Substances 0.000 claims abstract description 27
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 27
- -1 tertiary amine compounds Chemical class 0.000 claims description 30
- 239000007822 coupling agent Substances 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 25
- 239000000843 powder Substances 0.000 claims description 14
- 239000004593 Epoxy Substances 0.000 claims description 13
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Natural products P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 13
- 229910000410 antimony oxide Inorganic materials 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 239000001301 oxygen Substances 0.000 claims description 12
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims description 12
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 229920001568 phenolic resin Polymers 0.000 claims description 9
- 239000005011 phenolic resin Substances 0.000 claims description 9
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 8
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 8
- 235000021355 Stearic acid Nutrition 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 8
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 8
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 8
- 239000008117 stearic acid Substances 0.000 claims description 8
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 7
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 6
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 6
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 230000004927 fusion Effects 0.000 claims description 4
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 claims description 3
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- 239000004640 Melamine resin Substances 0.000 claims description 3
- 235000021314 Palmitic acid Nutrition 0.000 claims description 3
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 3
- 235000013539 calcium stearate Nutrition 0.000 claims description 3
- 239000008116 calcium stearate Substances 0.000 claims description 3
- 235000019359 magnesium stearate Nutrition 0.000 claims description 3
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 claims description 3
- SCWKRWCUMCMVPW-UHFFFAOYSA-N phenyl n-methylcarbamate Chemical compound CNC(=O)OC1=CC=CC=C1 SCWKRWCUMCMVPW-UHFFFAOYSA-N 0.000 claims description 3
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 2
- 125000001246 bromo group Chemical group Br* 0.000 claims description 2
- HGPXWXLYXNVULB-UHFFFAOYSA-M lithium stearate Chemical compound [Li+].CCCCCCCCCCCCCCCCCC([O-])=O HGPXWXLYXNVULB-UHFFFAOYSA-M 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims 1
- 230000008025 crystallization Effects 0.000 claims 1
- LCDFWRDNEPDQBV-UHFFFAOYSA-N formaldehyde;phenol;urea Chemical compound O=C.NC(N)=O.OC1=CC=CC=C1 LCDFWRDNEPDQBV-UHFFFAOYSA-N 0.000 claims 1
- 150000002460 imidazoles Chemical class 0.000 claims 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 15
- 238000005538 encapsulation Methods 0.000 abstract description 6
- 229920006015 heat resistant resin Polymers 0.000 abstract description 3
- 230000001568 sexual effect Effects 0.000 abstract description 3
- 206010002368 Anger Diseases 0.000 abstract 1
- 238000004040 coloring Methods 0.000 description 20
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 235000012771 pancakes Nutrition 0.000 description 11
- 238000001125 extrusion Methods 0.000 description 10
- 239000006229 carbon black Substances 0.000 description 9
- 235000019504 cigarettes Nutrition 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 235000013312 flour Nutrition 0.000 description 5
- 229920003986 novolac Polymers 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 239000001993 wax Substances 0.000 description 5
- VOOLKNUJNPZAHE-UHFFFAOYSA-N formaldehyde;2-methylphenol Chemical compound O=C.CC1=CC=CC=C1O VOOLKNUJNPZAHE-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 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 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 150000002118 epoxides Chemical class 0.000 description 3
- 238000004898 kneading Methods 0.000 description 3
- 239000012188 paraffin wax Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 229910000000 metal hydroxide Inorganic materials 0.000 description 2
- 150000004692 metal hydroxides Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- USFPINLPPFWTJW-UHFFFAOYSA-N tetraphenylphosphonium Chemical compound C1=CC=CC=C1[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 USFPINLPPFWTJW-UHFFFAOYSA-N 0.000 description 2
- DCXXMTOCNZCJGO-UHFFFAOYSA-N tristearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- NCIAGQNZQHYKGR-UHFFFAOYSA-N naphthalene-1,2,3-triol Chemical class C1=CC=C2C(O)=C(O)C(O)=CC2=C1 NCIAGQNZQHYKGR-UHFFFAOYSA-N 0.000 description 1
- ODGAOXROABLFNM-UHFFFAOYSA-N polynoxylin Chemical compound O=C.NC(N)=O ODGAOXROABLFNM-UHFFFAOYSA-N 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
Abstract
The present invention relates to encapsulation field, in particular to a kind of fire-retardant epoxy resin composition, fire-retardant epoxy resin material and preparation method thereof.The fire-retardant epoxy resin composition, including：Epoxy resin 2~20%；Curing agent 5~10%；Inorganic filler 70~85%；And fire retardant 1~20%, mutually compatibility produces synergy between each raw material.The fire-retardant epoxy resin material of preparation, by adjusting the ratio of fire retardant, while heat-resistant resin system is selected, the purpose that 500 600 DEG C of anti-flammability of composition epoxy resin, heat-resisting sexual satisfaction flames of angers occur when reaching resistive short.It can be widely used for power and insure the encapsulation of resistance.Its preparation method is simple and easy, and feasibility is strong.
Description
Technical field
The present invention relates to Electronic Packaging field, in particular to a kind of fire-retardant epoxy resin composition, fire-retardant type ring
Oxygen resin material and preparation method thereof.
Background technology
In electrical equipment circuitry, resistance is one of conventional electronic device, when short trouble, which occurs, for circuit excessively stream occurs, electricity
The temperature that resistance is particularly insured in resistance can be increased to 500-600 DEG C within a very short time, reach UL-94V-0 marks even if at this moment using
The resistance of accurate composition epoxy resin encapsulation also can pyrolytic smoke occurs and with naked light phenomenon, easily cause burning,
In the presence of very big potential safety hazard.
The content of the invention
The first object of the present invention is to provide a kind of fire-retardant epoxy resin composition solve circuit and short trouble occurs
When there is excessively stream, the problem of resistance easily causes burning.
The second object of the present invention is to provide a kind of preparation method of fire-retardant epoxy resin material, and preparation method is simple
Easy, feasibility is high.
The third object of the present invention is to provide a kind of fire-retardant epoxy resin material solve circuit generation short trouble and go out
During existing excessively stream, the problem of resistance easily causes burning.
In order to realize the above-mentioned purpose of the present invention, spy uses following technical scheme：
A kind of fire-retardant epoxy resin composition, by percentage to the quality, including：Epoxy resin 2~20%；Curing agent 5
~10%；Inorganic filler 70~85%；And fire retardant 1~20%, wherein, epoxy resin is selected from structure such as Formulas I or structure
Epoxy resin as described in Formula II：
Wherein, n is 1-10 positive integer.
A kind of preparation method of fire-retardant epoxy resin material, comprises the following steps：By epoxy resin, curing agent, inorganic
After filler and fire retardant mix, in 20-120 DEG C of mixing, wherein, by percentage to the quality, epoxy resin 2~20%；Solidification
Agent 5~10%；Inorganic filler 70~85%, epoxy resin are selected from epoxy resin of the structure such as Formulas I or structure as described in Formula II：
Wherein n is 1-10 positive integer.
A kind of fire-retardant epoxy resin material, it is prepared into by the preparation method of above-mentioned fire-retardant epoxy resin material
Arrive.
Compared with prior art, beneficial effects of the present invention are：
Fire-retardant epoxy resin composition provided by the invention, including：Epoxy resin 2~20%；Curing agent 5~10%；
Inorganic filler 70~85%；And fire retardant 1~20%, mutually compatibility produces synergy between each raw material.Pass through regulation
The ratio of fire retardant, while select heat-resistant resin system, the fire-retardant epoxy resin material of preparation, ring when reaching resistive short
The purpose that 500-600 DEG C of anti-flammability of epoxy resin composition, heat-resisting sexual satisfaction flames of anger occur.It can be widely used for power and insurance
The encapsulation of resistance.
The preparation method of fire-retardant epoxy resin material provided by the invention, by 2~20% epoxy resin；5~10%
Curing agent；70~85% inorganic filler and 1~20% fire retardant are after mixing, in 20-120 DEG C of mixing, you can with
The fire-retardant epoxy resin material is made.Preparation method is simple and easy, and feasibility is strong.
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.It is unreceipted specific in embodiment
Condition person, the condition suggested according to normal condition or manufacturer are carried out.Agents useful for same or the unreceipted production firm person of instrument, it is
The conventional products that can be obtained by commercially available purchase.
The present embodiment provides a kind of fire-retardant epoxy resin composition：
The fire-retardant epoxy resin composition by percentage to the quality, including：Epoxy resin 2~20%；Curing agent 5~
10%；Inorganic filler 70~85%；And fire retardant 1~20%.
Further, above-mentioned epoxy resin is selected from epoxy resin of the structure such as Formulas I or structure as described in Formula II：
Wherein, n is 1-10 positive integer.
In an optional embodiment of the invention, above-mentioned epoxy resin selection o-cresol formaldehyde type epoxy resin or more officials
The mixture of type epoxy resin or o-cresol formaldehyde type epoxy resin and polyfunctional group type epoxy resin composition can be rolled into a ball.
Further, curing agent includes linear phenol-aldehyde resin, phenyl methylcarbamate linear phenol-aldehyde resin, monohydroxy or dihydroxy naphthols
At least one of urea formaldehyde, dicyclopentadiene type phenolic resin, amido phenolic resin, melamine resin resin.
Further, above-mentioned fire retardant includes brominated epoxy resin, antimony oxide.
Further, above-mentioned fire retardant also includes other metal hydroxides.In an optional embodiment of the invention,
Metal hydroxides can select aluminium hydroxide.
By adjusting the flame-retardant system ratio of brominated epoxy resin and antimony oxide, while select heat-resistant resin body
System, the purpose that 500-600 DEG C of anti-flammability of composition epoxy resin, heat-resisting sexual satisfaction flames of anger occur when reaching resistive short.
Further, inorganic filler includes powdered quartz powder, fusion SiO 2 powder, spherical titanium dioxide
At least one of Si powder, ball-aluminium oxide powder.
Further, the composition epoxy resin also includes：
Accelerator 0.1~1%；Coupling agent 0.1~1%；Releasing agent 0.1~1%；And colouring agent 0.1~1%.
By adding accelerator, coupling agent, releasing agent and colouring agent in the feed, can further improve whole
The performance of individual composition epoxy resin.Mutual compatibility between each raw material, synergy is produced, further increasing whole ring
The combination property of epoxy resin composition.
Further, accelerator includes glyoxaline compound, glyoxaline compound, tertiary amine compounds, organic phosphine
At least two in compound.
Specifically, in an optional embodiment of the invention, above-mentioned accelerator can select glyoxaline compound and uncle
What the compound accelerant or selection tertiary amine compounds and organic phosphine compound that aminated compounds is mixed to form were mixed to form
The compound accelerant that compound accelerant or selection glyoxaline compound and organic phosphine compound are mixed to form.
In other optional embodiments of the invention, above-mentioned the choice of accelerator glyoxaline compound, tertiary amine compounds
And the compound accelerant that three kinds of accelerator of machine phosphine compound are mixed to form.
By from compound accelerant, can more preferably drip performance effect, and then improve whole fire-retardant epoxy resin combination
The performance of thing.
Further, coupling agent includes γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane (KH-560), gamma-amino
At least one of propyl-triethoxysilicane (KH-550), γ-mercaptan aminopropyl trimethoxysilane (KH-580).It is preferred that
Ground, above-mentioned coupling agent selection γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane (KH-560).
It should be noted that when above-mentioned coupling agent selects a variety of coupling agents, according to can fit between multiple compounds
The mixture of ratio composition.
Further, releasing agent is selected from native paraffin, synthetic wax, stearic acid, palmitic acid, zinc stearate, calcium stearate, tristearin
At least one of sour lithium and magnesium stearate.
Specifically, in an optional embodiment of the invention, when above-mentioned releasing agent selects native paraffin, bar wax is selected.Or
When the above-mentioned releasing agent of person selects synthetic wax, synthetic wax selection Tissuemat E.
By adding releasing agent in above-mentioned raw material, can help successfully to divide the product of curing molding from mould
Leave and, so as to obtain smooth product, and ensure that mould is used for multiple times.
Further, colouring agent is selected from carbon black.
It should be understood that above-mentioned colouring agent can select other common colorings applicatory of this area according to actual conditions
Agent.
Some embodiments of the present invention also provide a kind of preparation method of fire-retardant epoxy resin material, including following step
Suddenly：
Comprise the following steps：
By percentage to the quality, by 2~20% above-mentioned epoxy resin；5~10% above-mentioned curing agent；70~85%
After mixing, in 20-120 DEG C of mixing, the flame retardant type epoxy is made in the above-mentioned fire retardant of above-mentioned inorganic filler and 1~20%
Resin material.
Further, in above-mentioned mixing step, concretely 20-30 DEG C, 50-80 DEG C, 90-110 DEG C of temperature or
90-120 DEG C, preferably 60-90 DEG C；Time is 0.5-3 hours, concretely 0.5-1.5 hours or 1-1.5 hours, preferably 0.5-
1 hour.
In concrete operations, above-mentioned each raw material components can be mixed in proportion, heat and be kneaded on kneading machine, obtain
Dispersed mixture, cooling, after crushing, cake is bought on pancake making machine, obtain the resistance encapsulating material of required size.
It should be understood that above-mentioned kneading machine can select the kneading machine of the roller of various materials three commonly used in the art or two rollers.
Some embodiments of the present invention also provide a kind of fire-retardant epoxy resin material, pass through above-mentioned flame retardant type epoxy
The preparation method of resin material is prepared.
By the fire-retardant epoxy resin materials application in the encapsulation of power and insurance resistance, its higher anti-flammability can
Effectively improve whole power and insure the security of the encapsulation of resistance, be effectively prevented from the individual potential safety hazard of naked light.Work as circuit
When excessively stream occurs in generation short trouble, resistance will not also trigger naked light to burn.
The feature and performance of the present invention are described in further detail with reference to embodiments：
Embodiment 1
A kind of fire-retardant epoxy resin composition that the present embodiment provides, by percentage to the quality, including：Epoxy resin
2%；Curing agent 5%；Inorganic filler 85%；Fire retardant 7.6%；Accelerator 0.1%；Coupling agent 0.1%；Releasing agent 0.1%；With
And colouring agent 0.1%.Wherein, epoxy resin, purchased from Japanese Dainippon Ink Chemicals's (trade name：N-670-EXP-S, epoxide equivalent：
200g/eq).Curing agent selects linear phenol-aldehyde resin.Inorganic filler selects preparing spherical SiO 2 powder.Fire retardant selects bromo ring
Oxygen tree fat and antimony oxide.The choice of accelerator glyoxaline compound and tertiary amine compounds.Coupling agent selects γ-(2,3- rings
The oxygen of oxygen third) propyl trimethoxy silicane.Releasing agent is selected from native paraffin.Colouring agent selects carbon black.
The fire-retardant epoxy resin material that the present embodiment provides is prepared：By above-mentioned raw materials according to above-mentioned quality hundred
After dividing than mixing, the mixing extrusion under the conditions of 20 DEG C, obtains dispersed composition epoxy resin in an extruder, cool down,
Crush.Cake is bought on pancake making machine, obtains the composition epoxy resin of required size.
Embodiment 2
A kind of fire-retardant epoxy resin composition that the present embodiment provides, by percentage to the quality, including：Epoxy resin
10%；Curing agent 10%；Inorganic filler 70%；Fire retardant 6%；Accelerator 1%；Coupling agent 1%；Releasing agent 1%；And coloring
Agent 1%.Wherein, epoxy resin, purchased from Japanese DIC Co., Ltd. (trade name：N-670-EXP-S, epoxide equivalent：200g/
eq).Curing agent selects phenyl methylcarbamate linear phenol-aldehyde resin and monohydroxy or dihydroxy naphthlene phenolic resin.Inorganic filler selective freezing type
SiO 2 powder and fusion SiO 2 powder.Fire retardant selects brominated epoxy resin and antimony oxide.Accelerator is selected
Select tertiary amine compounds and organic phosphine compound.Coupling agent selects γ aminopropyltriethoxy silane.Releasing agent, which is selected from, to be closed
Into wax and stearic acid.Colouring agent selects carbon black.
The fire-retardant epoxy resin material that the present embodiment provides is prepared：By above-mentioned raw materials according to above-mentioned quality hundred
After dividing than mixing, the mixing extrusion under the conditions of 80 DEG C, obtains dispersed composition epoxy resin in an extruder, cool down,
Crush.Cake is bought on pancake making machine, obtains the composition epoxy resin of required size.
Embodiment 3
A kind of fire-retardant epoxy resin composition that the present embodiment provides, by percentage to the quality, including：Epoxy resin
20%；Curing agent 5%；Inorganic filler 70%；Fire retardant 4.2%；Accelerator 0.2%；Coupling agent 0.2%；Releasing agent 0.2%；
And colouring agent 0.2%.Wherein, epoxy resin, purchased from Japanese Dainippon Ink Chemicals's (trade name：N-670-EXP-S, epoxy are worked as
Amount：200g/eq).Curing agent selects dicyclopentadiene type phenolic resin.Inorganic filler selects ball-aluminium oxide powder.Fire retardant
Select brominated epoxy resin and antimony oxide.The choice of accelerator glyoxaline compound and organic phosphine compound.Coupling agent selects
Select γ-mercaptan aminopropyl trimethoxysilane.Releasing agent is selected from zinc stearate, calcium stearate, lithium stearate and magnesium stearate.
Colouring agent selects carbon black.
The fire-retardant epoxy resin material that the present embodiment provides is prepared：By above-mentioned raw materials according to above-mentioned quality hundred
After dividing than mixing, the mixing extrusion under the conditions of 110 DEG C, obtains dispersed composition epoxy resin in an extruder, cool down,
Crush.Cake is bought on pancake making machine, obtains the composition epoxy resin of required size.
Embodiment 4
A kind of fire-retardant epoxy resin composition that the present embodiment provides, by percentage to the quality, including：Epoxy resin
7.8%；Curing agent 6%；Inorganic filler 84%；Fire retardant 1%；Accelerator 0.3%；Coupling agent 0.2%；Releasing agent 0.3%；With
And colouring agent 0.4%.Wherein, epoxy resin, purchased from Japanese Dainippon Ink Chemicals's (trade name：N-670-EXP-S, epoxide equivalent：
200g/eq).Curing agent selects amido phenolic resin and melamine resin resin.Inorganic filler selects fusion dioxy
SiClx powder and preparing spherical SiO 2 powder.Fire retardant selects brominated epoxy resin and antimony oxide.The choice of accelerator tertiary amine
Class compound and organic phosphine compound.Coupling agent selects γ-mercaptan aminopropyl trimethoxysilane and γ-(2,3- epoxies third
Oxygen) propyl trimethoxy silicane.Releasing agent is selected from stearic acid and palmitic acid.Colouring agent selects carbon black.
The fire-retardant epoxy resin material that the present embodiment provides is prepared：By above-mentioned raw materials according to above-mentioned quality hundred
After dividing than mixing, the mixing extrusion under the conditions of 105 DEG C, obtains dispersed composition epoxy resin in an extruder, cool down,
Crush.Cake is bought on pancake making machine, obtains the composition epoxy resin of required size.
Embodiment 5
A kind of fire-retardant epoxy resin composition that the present embodiment provides, by percentage to the quality, including：Epoxy resin
4.1%；Curing agent 5%；Inorganic filler 70%；Fire retardant 20%；Accelerator 0.3%；Coupling agent 0.2%；Releasing agent 0.3%；
And colouring agent 0.1%.Wherein, epoxy resin, purchased from Japanese Dainippon Ink Chemicals's (trade name：N-670-EXP-S, epoxy are worked as
Amount：200g/eq).Curing agent selects monohydroxy or dihydroxy naphthlene phenolic resin.Inorganic filler selects clinkering crystal formation silicon dioxide powder
End and ball-aluminium oxide powder.Fire retardant selects brominated epoxy resin and antimony oxide.The choice of accelerator tertiary amine compounds
With organic phosphine compound.Coupling agent selects γ-mercaptan aminopropyl trimethoxysilane.Releasing agent is selected from stearic acid.Colouring agent
Select carbon black.
The fire-retardant epoxy resin material that the present embodiment provides is prepared：By above-mentioned raw materials according to above-mentioned quality hundred
After dividing than mixing, the mixing extrusion under the conditions of 95 DEG C, obtains dispersed composition epoxy resin in an extruder, cool down,
Crush.Cake is bought on pancake making machine, obtains the composition epoxy resin of required size.
Embodiment 6
A kind of fire-retardant epoxy resin composition that the present embodiment provides, by percentage to the quality, including：Epoxy resin
9.8%；Curing agent 6.1%；Inorganic filler 70%；Fire retardant 12.5%；Accelerator 0.5%；Coupling agent 0.4%；Releasing agent
0.4%；And colouring agent 0.3%.Wherein, epoxy resin, including o-cresol formaldehyde type epoxy resin (N-670) 5.2%；It is multifunctional
Group's type epoxy resin (EPPN-502H) 4.6%.Curing agent selects novolac curing agent (PF-8012).Inorganic filler selects
Clinkering crystal formation silica flour.Fire retardant selects brominated epoxy resin and antimony oxide.The choice of accelerator tertiary amine compounds and have
Machine phosphine compound.Coupling agent selects γ-(oxygen of 2,3- epoxies third) propyl trimethoxy silicane.Releasing agent is selected from stearic acid.
Toner selects carbon black.
The fire-retardant epoxy resin material that the present embodiment provides is prepared：By above-mentioned raw materials according to above-mentioned quality hundred
After dividing than mixing, the mixing extrusion under the conditions of 100 DEG C, obtains dispersed composition epoxy resin in an extruder, cool down,
Crush.Cake is bought on pancake making machine, obtains the composition epoxy resin of required size.
Embodiment 7
A kind of fire-retardant epoxy resin composition that the present embodiment provides, by percentage to the quality, including：Epoxy resin
4.8%；Curing agent 7.6%；Inorganic filler 70%；Fire retardant 16%；Accelerator 0.5%；Coupling agent 0.4%；Releasing agent
0.4%；And colouring agent 0.3%.Wherein, epoxy resin, including o-cresol formaldehyde type epoxy resin (N-670) 1.8%；It is multifunctional
Group's type epoxy resin (EPPN-502H) 3%.Curing agent selects novolac curing agent (PF-8012).Inorganic filler selection is molten
Crystal type silica flour.Fire retardant selects brominated epoxy resin and antimony oxide.The choice of accelerator tertiary amine compounds and organic
Phosphine compound.Coupling agent selects γ-(oxygen of 2,3- epoxies third) propyl trimethoxy silicane.Releasing agent is selected from stearic acid.Coloring
Agent selects carbon black.
The fire-retardant epoxy resin material that the present embodiment provides is prepared：By above-mentioned raw materials according to above-mentioned quality hundred
After dividing than mixing, the mixing extrusion under the conditions of 100 DEG C, obtains dispersed composition epoxy resin in an extruder, cool down,
Crush.Cake is bought on pancake making machine, obtains the composition epoxy resin of required size.
Embodiment 8
A kind of fire-retardant epoxy resin composition that the present embodiment provides, by percentage to the quality, including：Polyfunctional group type
Epoxy resin (EPPN-502H) 2.8%；Curing agent 5.6%；Inorganic filler 70%；Fire retardant 20%；Accelerator 0.5%；Coupling
Agent 0.4%；Releasing agent 0.4%；And colouring agent 0.3%.Wherein, curing agent selects novolac curing agent (PF-8012).Nothing
Machine Fillers selection clinkering crystal formation silica flour.Fire retardant selection brominated epoxy resin, antimony oxide and aluminium hydroxide.Accelerator
Select tertiary amine compounds and organic phosphine compound.Coupling agent selects γ-(oxygen of 2,3- epoxies third) propyl trimethoxy silicane.
Releasing agent is selected from stearic acid.Colouring agent selects carbon black.
The fire-retardant epoxy resin material that the present embodiment provides is prepared：By above-mentioned raw materials according to above-mentioned quality hundred
After dividing than mixing, the mixing extrusion under the conditions of 100 DEG C, obtains dispersed composition epoxy resin in an extruder, cool down,
Crush.Cake is bought on pancake making machine, obtains the composition epoxy resin of required size.
Comparative example 1
The preparation of epoxide resin material, raw material are selected from the component of following percetage by weight：O-cresol formaldehyde type epoxy resin (N-
670) 15%；Novolac curing agent (PF-8012) 7.4%；Crystal type silica flour 75%；Brominated epoxy resin 1%；Promote
Agent (TPP+DBU) 0.5%；Coupling agent (KH-560) 0.4%；Releasing agent (AC316A) 0.4%；Colouring agent (MA-600)
0.3%.
By the said components mixing extrusion under the conditions of 100 DEG C in an extruder, dispersed epoxy composite is obtained
Thing, cooling, crush.Cake is bought on pancake making machine, obtains the composition epoxy resin of required size.
Comparative example 2
The preparation of epoxide resin material, raw material are selected from the component of following percentage：O-cresol formaldehyde type epoxy resin (N-670)
15%；Novolac curing agent (PF-8012) 7.4%；Crystal type silica flour 75%；Antimony oxide 1%；Accelerator (TPP+
DBU) 0.5%；Coupling agent (KH-560) 0.4%；Releasing agent (AC316A) 0.4%；Colouring agent (MA-600) 0.3%.
By the said components mixing extrusion under the conditions of 100 DEG C in an extruder, dispersed epoxy composite is obtained
Thing, cooling, crush.Cake is bought on pancake making machine, obtains the composition epoxy resin of required size.
Experimental example
The epoxide resin material provided embodiment 1-8 and comparative example 1-2, detects its combustibility.
Testing program：
Flammability is evaluated：Gained composition epoxy resin is prepared into the batten of 80*10*4mm sizes, added on electric furnace
Heat, observe combustion case.
Evaluation criterion：When resistance in the short-circuit state, smoke phenomenon can occur in composition epoxy resin burning, but can not
To there is naked light phenomenon.
Experimental result is as follows：
Embodiment 1：Smokelessly, the flames of anger
Embodiment 2：There are cigarette, the flames of anger
Embodiment 3：There are cigarette, the flames of anger
Embodiment 4：Smokelessly, the flames of anger
Embodiment 5：There are cigarette, the flames of anger
Embodiment 6：There are cigarette, the flames of anger
Embodiment 7：There are cigarette, the flames of anger
Embodiment 8：Smokelessly, the flames of anger
Comparative example 1：There is cigarette, have naked light
Comparative example 2：There is cigarette, have naked light
It should be understood that although being illustrated with specific embodiment and being described the present invention, but will be appreciated that without departing substantially from this hair
Many other change and modification can be made in the case of bright spirit and scope.It is, therefore, intended that will in appended right
Ask including belonging to all such changes and modifications in the scope of the invention.
Claims (10)
- A kind of 1. fire-retardant epoxy resin composition, it is characterised in that by percentage to the quality, including：Epoxy resin 2~ 20%；Curing agent 5~10%；Inorganic filler 70~85%；And fire retardant 1~20%, wherein, the epoxy resin is selected from knot Epoxy resin of the structure such as Formulas I or structure as described in Formula II：Wherein, n is 1-10 positive integer.
- 2. fire-retardant epoxy resin composition according to claim 1, it is characterised in that the curing agent includes line style phenol Urea formaldehyde, phenyl methylcarbamate linear phenol-aldehyde resin, monohydroxy or dihydroxy naphthlene phenolic resin, dicyclopentadiene type phenolic resin, amino At least one of phenolic resin, melamine resin resin.
- 3. fire-retardant epoxy resin composition according to claim 2, it is characterised in that the inorganic filler includes crystallization At least one in type SiO 2 powder, fusion SiO 2 powder, preparing spherical SiO 2 powder, ball-aluminium oxide powder Kind.
- 4. fire-retardant epoxy resin composition according to claim 3, it is characterised in that the fire retardant includes bromo ring Oxygen tree fat and antimony oxide.
- 5. fire-retardant epoxy resin composition according to claim 1, it is characterised in that by percentage to the quality, described Composition epoxy resin also includes：
- 6. fire-retardant epoxy resin composition according to claim 5, it is characterised in that the accelerator includes imidazoles At least two in compound, tertiary amine compounds, organic phosphine compound.
- 7. fire-retardant epoxy resin composition according to claim 5, it is characterised in that the coupling agent include γ-(2, The oxygen of 3- epoxies third) propyl trimethoxy silicane, γ aminopropyltriethoxy silane, γ-mercaptan aminopropyl trimethoxysilane At least one of.
- 8. fire-retardant epoxy resin composition according to claim 5, it is characterised in that the releasing agent includes natural At least one of wax, synthetic wax, stearic acid, palmitic acid, zinc stearate, calcium stearate, lithium stearate and magnesium stearate.
- 9. a kind of preparation method of fire-retardant epoxy resin material, it is characterised in that comprise the following steps：After epoxy resin, curing agent, inorganic filler and fire retardant are mixed, in 20-120 DEG C of mixing, wherein, with quality percentage Than meter, the epoxy resin 2~20%；The curing agent 5~10%；The inorganic filler 70~85%, the fire retardant 1~ 20%, the epoxy resin is selected from epoxy resin of the structure such as Formulas I or structure as described in Formula II：Wherein n is 1-10 positive integer.
- 10. a kind of fire-retardant epoxy resin material, it is characterised in that it is by fire-retardant epoxy resin as claimed in claim 9 The preparation method of material is prepared.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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Application publication date: 20180216 |