CN102875968A - Flame-retardation enhanced epoxy plastic sheet material and its preparation method - Google Patents
Flame-retardation enhanced epoxy plastic sheet material and its preparation method Download PDFInfo
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- CN102875968A CN102875968A CN2011101923867A CN201110192386A CN102875968A CN 102875968 A CN102875968 A CN 102875968A CN 2011101923867 A CN2011101923867 A CN 2011101923867A CN 201110192386 A CN201110192386 A CN 201110192386A CN 102875968 A CN102875968 A CN 102875968A
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- 239000000463 material Substances 0.000 title claims abstract description 57
- 239000004593 Epoxy Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000002985 plastic film Substances 0.000 title abstract 4
- 239000003063 flame retardant Substances 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 239000000835 fiber Substances 0.000 claims abstract description 7
- 239000003822 epoxy resin Substances 0.000 claims abstract description 6
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 40
- 229920005989 resin Polymers 0.000 claims description 20
- 239000011347 resin Substances 0.000 claims description 20
- 239000004033 plastic Substances 0.000 claims description 19
- 229920003023 plastic Polymers 0.000 claims description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 12
- 229920001971 elastomer Polymers 0.000 claims description 11
- 239000005060 rubber Substances 0.000 claims description 11
- LSWYGACWGAICNM-UHFFFAOYSA-N 2-(prop-2-enoxymethyl)oxirane Chemical compound C=CCOCC1CO1 LSWYGACWGAICNM-UHFFFAOYSA-N 0.000 claims description 10
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 10
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical group CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 10
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000009413 insulation Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 claims description 9
- 239000003365 glass fiber Substances 0.000 claims description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- 239000004902 Softening Agent Substances 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 229920000459 Nitrile rubber Polymers 0.000 claims description 7
- NTXGQCSETZTARF-UHFFFAOYSA-N buta-1,3-diene;prop-2-enenitrile Chemical compound C=CC=C.C=CC#N NTXGQCSETZTARF-UHFFFAOYSA-N 0.000 claims description 7
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 7
- 230000000979 retarding effect Effects 0.000 claims description 6
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 claims description 6
- 229940015043 glyoxal Drugs 0.000 claims description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-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
- 150000001412 amines Chemical class 0.000 claims description 4
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical group C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 4
- 229920001897 terpolymer Polymers 0.000 claims description 4
- DROMNWUQASBTFM-UHFFFAOYSA-N dinonyl benzene-1,2-dicarboxylate Chemical compound CCCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCCC DROMNWUQASBTFM-UHFFFAOYSA-N 0.000 claims description 3
- KMOUUZVZFBCRAM-OLQVQODUSA-N (3as,7ar)-3a,4,7,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1C=CC[C@@H]2C(=O)OC(=O)[C@@H]21 KMOUUZVZFBCRAM-OLQVQODUSA-N 0.000 claims description 2
- CMQUQOHNANGDOR-UHFFFAOYSA-N 2,3-dibromo-4-(2,4-dibromo-5-hydroxyphenyl)phenol Chemical compound BrC1=C(Br)C(O)=CC=C1C1=CC(O)=C(Br)C=C1Br CMQUQOHNANGDOR-UHFFFAOYSA-N 0.000 claims description 2
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 2
- 239000004709 Chlorinated polyethylene Substances 0.000 claims description 2
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 2
- FQYUMYWMJTYZTK-UHFFFAOYSA-N Phenyl glycidyl ether Chemical compound C1OC1COC1=CC=CC=C1 FQYUMYWMJTYZTK-UHFFFAOYSA-N 0.000 claims description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 2
- AWMVMTVKBNGEAK-UHFFFAOYSA-N Styrene oxide Chemical compound C1OC1C1=CC=CC=C1 AWMVMTVKBNGEAK-UHFFFAOYSA-N 0.000 claims description 2
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 claims description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical group [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004917 carbon fiber Substances 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 239000000470 constituent Substances 0.000 claims description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical group O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 2
- WHHGLZMJPXIBIX-UHFFFAOYSA-N decabromodiphenyl ether Chemical compound BrC1=C(Br)C(Br)=C(Br)C(Br)=C1OC1=C(Br)C(Br)=C(Br)C(Br)=C1Br WHHGLZMJPXIBIX-UHFFFAOYSA-N 0.000 claims description 2
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims description 2
- OEIWPNWSDYFMIL-UHFFFAOYSA-N dioctyl benzene-1,4-dicarboxylate Chemical compound CCCCCCCCOC(=O)C1=CC=C(C(=O)OCCCCCCCC)C=C1 OEIWPNWSDYFMIL-UHFFFAOYSA-N 0.000 claims description 2
- 229960001545 hydrotalcite Drugs 0.000 claims description 2
- 229910001701 hydrotalcite Inorganic materials 0.000 claims description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 2
- 239000000347 magnesium hydroxide Substances 0.000 claims description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 2
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000391 magnesium silicate Substances 0.000 claims description 2
- 229910052919 magnesium silicate Inorganic materials 0.000 claims description 2
- 235000019792 magnesium silicate Nutrition 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 239000010445 mica Substances 0.000 claims description 2
- 229910052618 mica group Inorganic materials 0.000 claims description 2
- 229920003986 novolac Polymers 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 229920006122 polyamide resin Polymers 0.000 claims description 2
- 229920000137 polyphosphoric acid Polymers 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- DCRSYTGOGMAXIA-UHFFFAOYSA-N zinc;oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4].[Zn+2] DCRSYTGOGMAXIA-UHFFFAOYSA-N 0.000 claims description 2
- 238000012545 processing Methods 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 3
- 230000004048 modification Effects 0.000 abstract description 3
- 239000003085 diluting agent Substances 0.000 abstract 1
- 239000000945 filler Substances 0.000 abstract 1
- 239000004615 ingredient Substances 0.000 abstract 1
- 239000004014 plasticizer Substances 0.000 abstract 1
- 239000012747 synergistic agent Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 26
- 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 8
- AQPHBYQUCKHJLT-UHFFFAOYSA-N 1,2,3,4,5-pentabromo-6-(2,3,4,5,6-pentabromophenyl)benzene Chemical group BrC1=C(Br)C(Br)=C(Br)C(Br)=C1C1=C(Br)C(Br)=C(Br)C(Br)=C1Br AQPHBYQUCKHJLT-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000011161 development Methods 0.000 description 5
- 235000011837 pasties Nutrition 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 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
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention belongs to the technical field of high-molecular material modification and processing and discloses a flame-retardation enhanced epoxy plastic sheet material and its preparation method. The epoxy plastic sheet material comprises the following ingredients of: by weight, 100 parts of epoxy resin, 5-20 parts of a plasticizer, 3-15 parts of a flexibilizer, 80-150 parts of reinforced fibers, 0-100 parts of a filler, 8-15 parts of a diluent, 15-30 parts of a fire retardant, 3-8 parts of a flame-retardation synergistic agent and 5-18 parts of a curing agent. In comparison with the prior art, the flame-retardation enhanced epoxy plastic sheet material provided by the invention has advantages of strong strength, good toughness, impact resistance, long service life, low cost, flame retardation and good flame resistance, is easy to process, and can meet the criteria at V-0 level of UL-94. The material provided by the invention can be widely applied in many national economical fields such as automobile, building sheet material and the like.
Description
Technical field
The invention belongs to polymer modification and processing technique field, relate to a kind of epoxy plastics sheet material and preparation method thereof.
Background technology
Along with the development of automotive industry, the auto output steady-state growth of China, the automobile consumption scale is increasingly huge.Show according to China Association for Automobile Manufacturers's distributing data, China's output reached 934.51 ten thousand in 2008, and the automobile sales volume reaches 938.05 ten thousand.Although global economic crisis has been brought the automobile industry of various countries and has been had a strong impact on; but domestic automobile producer responds actively, and adds the support of government policy, recently the automobile sales volume bottom out of China; from overall trend, the automotive industry of China will keep the situation that grows continuously and fast.When the progress of automobile and relevant industries brought huge opportunity, automotive industry also was faced with huge challenge.The development of automobile and relevant industries is day by day obvious on the impact of the aspects such as social energy resource supply, environment protection, and the pressure of the energy-saving and emission-reduction that therefore will bear also increases increasingly.In automobile industry, the testing model that is not related to sheet metal part or plastic paste and assembly subassembly, except minority is worked the profile with aluminium alloy, major part is with the pasty state lumbering resin profile of working, this pasty state lumbering resin is take the Resins, epoxy synthetic materials as the basis, and the weakness of existing pasty state lumbering resin is: weave construction is soft, wear no resistance, fragility is large, the life-span is short, flame retardant resistance is undesirable.
Development along with production technology, people's novel material that begins one's study, the another kind of novel material of replacing pasty state lumbering resin---polyurethane(s) plastic plate appearance, its excellent property: good toughness, wear resistance are high, easy processing, dense structure, cause user's very big interest, obtained at present customer's approval, the user who makes testing model of this material is also more and more.But this material is imported materials and items, and price is high, and cost is large, is unfavorable for popularizing and promoting the development of automotive industry.
Summary of the invention
The object of the invention is to for the defective of prior art and a kind of flame-retardant reinforced epoxy plastics sheet material is provided, this plastic plate excellent property and cost are low.
Another object of the present invention provides above-mentioned flame-retardant reinforced epoxy plastics preparation of plates method.
The present invention is achieved through the following technical solutions above-mentioned purpose:
A kind of epoxy plastics sheet material, it comprises following component and weight part:
100 parts of Resins, epoxy,
5～20 parts in softening agent,
3～15 parts of toughner,
80～150 parts of fortifying fibres,
0～00 part of weighting agent,
8～15 parts of thinners,
15～30 parts of fire retardants,
3～8 parts of fire retarding synergists,
5～18 parts in solidifying agent.
Described Resins, epoxy is selected from bisphenol A type epoxy resin, novolac epoxy or tricyanic epoxy resin, and described per kilogram Resins, epoxy contains the oxirane value of 4.3～5.1 equivalents, fugitive constituent≤1%, in order to reach above-mentioned requirements, select that room temperature hardening, dimensional stabilizing, intensity are high, thermal expansivity circlet epoxy resins.
Described softening agent is selected from dioctyl phthalate (DOP), dibutyl phthalate, Dinonylphthalate or dioctyl terephthalate.
Described toughner is selected from polyamide resin, butadiene-acrylonitrile rubber or terpolymer EP rubber.
Described fortifying fibre is selected from glass fibre, carbon fiber or fibrous magnesium silicate.
Described weighting agent is selected from silica powder, mica powder, calcium carbonate or titanium dioxide; And the granularity of described silica powder is greater than 270 orders, whiteness 85-90.
Described thinner is selected from pimelinketone, dimethylbenzene, vinylbenzene, styrene oxide, phenyl glycidyl ether or glycidyl allyl ether.
Described fire retardant is selected from trimeric cyanamide, melamine cyanurate, coating polyphosphoric acid amine, magnesium hydroxide, aluminium hydroxide, decabromodiphenyl oxide, tetrabromo-bisphenol, chlorinatedpolyethylene or clorafin.
Described fire retarding synergist is selected from calcium oxide, aluminum oxide, boron trioxide, titanium oxide zinc oxide, magnesium oxide, silicon oxide, zinc borate, hydrotalcite or antimonous oxide.
Described solidifying agent is selected from a kind of in quadrol, diethylenetriamine-propylene oxide phenyl ether affixture, isophthalic triamine, Tetra hydro Phthalic anhydride or the glyoxal ethyline; The amine value of described solidifying agent diethylenetriamine-propylene oxide phenyl ether affixture is 680～720.
A kind of above-mentioned flame-retardant reinforced epoxy plastics preparation of plates method may further comprise the steps:
(1) takes by weighing according to the above ratio each raw material, Resins, epoxy, softening agent, toughner, fortifying fibre, weighting agent, thinner are added in the reactor, stir;
(2) fire retardant and fire retarding synergist are joined in the mixture of preparation in the step (1), be heated to 80～100 ℃, and stir to occurring without solid particulate; Add again solidifying agent, stirring and evenly mixing;
(3) feed liquid for preparing is stirred under vacuum, degassed;
(4) place forming mould to be cured the material after degassed again, release after 3～4 hours, die temperature is 80～100 ℃; Again with the constant temperature insulation 1.5～2.5 hours under 55～65 ℃ of temperature of above-mentioned sheet material after release.
The whipping temp of described step (1) is 70～80 ℃, and churning time is 8～12 minutes.
The vacuum tightness of described step (3) is 9.0～10.0 * 10
4Pa, stirring velocity 160～200r/min, the degassed time is 10-15 minute.
The present invention compared with prior art has following advantage and beneficial effect:
1, high and good toughness, shock-resistant, easy processing of flame-retardant reinforced epoxy plastics timber intensity provided by the present invention, the V-0 grade standard that the life-span is long and cost is low, fire-retardant fireproof can reach well UL-94.
2, material provided by the present invention can be widely used in numerous national economy fields such as automobile industry, building board.And this material cost is cheap, performance is high, can promote developing rapidly of automobile industry etc., satisfies the needs of social development.
Embodiment
Below in conjunction with specific embodiment, aforesaid flame-retardant reinforced epoxy plastics sheet material is described in further detail.
Adopt GB (GB) to measure the properties of material among the embodiment, if no special instructions, the umber of component is parts by weight.
Embodiment 1
, stirred 10 minutes under 70 ℃ of conditions in 100 parts of Resins, epoxy, 8 parts of dioctyl phthalate (DOP)s, 5 parts of terpolymer EP rubbers, 100 parts in glass fibre, 30 parts of silica powders, 10 parts of adding reactors of glycidyl allyl ether by recipe ratio;
In 20 parts of clorafins, 5 parts of addings of antimonous oxide said mixture, be heated to 80 ℃, and stir to occurring without solid particulate; Add again 9 parts of diethylenetriamines-propylene oxide phenyl ether affixture, stirring and evenly mixing;
(vacuum tightness is 9.5*10 under vacuum with the feed liquid for preparing
4Pa) stir stirring velocity 180r/min, degassed 12 minutes; Place forming mould to be cured the material after degassed again, release after 3.5 hours, die temperature is 90 ℃;
Again with the constant temperature insulation 2 hours under 55 ℃ of temperature of above-mentioned sheet material after release.Gained sheet material is processed into test bars by the standard test requirement, tests its performance and list in the table 1.
Embodiment 2
, stirred 8 minutes under 75 ℃ of conditions in 100 parts of Resins, epoxy, 14 parts of dibutyl phthalates, 8 parts of butadiene-acrylonitrile rubbers, 80 parts in glass fibre, 20 parts in calcium carbonate, 12 parts of adding reactors of glycidyl allyl ether by recipe ratio;
In 15 parts of decabromodiphenyl oxides, 6 parts of addings of zinc borate said mixture, be heated to 85 ℃, and stir to occurring without solid particulate; Add again 5 parts of glyoxal ethylines, stirring and evenly mixing;
(vacuum tightness is 9.2*10 under vacuum with the feed liquid for preparing
4Pa) stir stirring velocity 170r/min, degassed 10 minutes; Place forming mould to be cured the material after degassed again, release after 3 hours, die temperature is 80 ℃;
Again with the constant temperature insulation 1.5 hours under 60 ℃ of temperature of above-mentioned sheet material after release.Gained sheet material is processed into test bars by the standard test requirement, tests its performance and list in the table 1.
Embodiment 3
, stirred 8 minutes under 80 ℃ of conditions in 100 parts of Resins, epoxy, 6 parts of Dinonylphthalates, 4 parts of terpolymer EP rubbers, 120 parts in glass fibre, 60 parts in calcium carbonate, 8 parts of adding reactors of glycidyl allyl ether by recipe ratio;
In 20 parts of tetrabromo-bisphenols, 6 parts of addings of antimonous oxide said mixture, be heated to 95 ℃, and stir to occurring without solid particulate; Add again 10 parts of diethylenetriamines-propylene oxide phenyl ether affixture, stirring and evenly mixing;
(vacuum tightness is 10.0*10 under vacuum with the feed liquid for preparing
4Pa) stir stirring velocity 160r/min, degassed 14 minutes; Place forming mould to be cured the material after degassed again, release after 3 hours, die temperature is 100 ℃;
Again with the constant temperature insulation 2 hours under 65 ℃ of temperature of above-mentioned sheet material after release.Gained sheet material is processed into test bars by the standard test requirement, tests its performance and list in the table 1.
Embodiment 4
, stirred 12 minutes under 75 ℃ of conditions in 100 parts of Resins, epoxy, 15 parts of dibutyl phthalates, 10 parts of butadiene-acrylonitrile rubbers, 100 parts in glass fibre, 10 parts of adding reactors of glycidyl allyl ether by recipe ratio;
In 28 parts of decabromodiphenyl oxides, 8 parts of addings of antimonous oxide said mixture, be heated to 100 ℃, and stir to occurring without solid particulate; Add again 18 parts of glyoxal ethylines, stirring and evenly mixing;
(vacuum tightness is 9.5*10 under vacuum with the feed liquid for preparing
4Pa) stir stirring velocity 200r/min, degassed 10 minutes; Place forming mould to be cured the material after degassed again, release after 3.5 hours, die temperature is 85 ℃;
Again with the constant temperature insulation 2.5 hours under 55 ℃ of temperature of above-mentioned sheet material after release.Gained sheet material is processed into test bars by the standard test requirement, tests its performance and list in the table 1.
Embodiment 5
, stirred 10 minutes under 80 ℃ of conditions in 100 parts of Resins, epoxy, 18 parts of dioctyl phthalate (DOP)s, 15 parts of butadiene-acrylonitrile rubbers, 150 parts in glass fibre, 100 parts of silica powders, 15 parts of adding reactors of glycidyl allyl ether by recipe ratio;
In 25 parts of decabromodiphenyl oxides, 6 parts of addings of zinc borate said mixture, be heated to 90 ℃, and stir to occurring without solid particulate; Add again 15 parts of diethylenetriamines-propylene oxide phenyl ether affixture, stirring and evenly mixing;
(vacuum tightness is 10.0*10 under vacuum with the feed liquid for preparing
4Pa) stir stirring velocity 180r/min, degassed 15 minutes; Place forming mould to be cured the material after degassed again, release after 3.5 hours, die temperature is 95 ℃;
Again with the constant temperature insulation 1.5 hours under 65 ℃ of temperature of above-mentioned sheet material after release.Gained sheet material is processed into test bars by the standard test requirement, tests its performance and list in the table 1.
Comparative example 1
Do not add softening agent, toughner, all the other are with embodiment 5., stirred 10 minutes under 80 ℃ of conditions in 100 parts of Resins, epoxy, 150 parts in glass fibre, 100 parts of silica powders, 15 parts of adding reactors of glycidyl allyl ether by recipe ratio;
In 25 parts of decabromodiphenyl oxides, 6 parts of addings of zinc borate said mixture, be heated to 90 ℃, and stir to occurring without solid particulate; Add again 15 parts of diethylenetriamines-propylene oxide phenyl ether affixture, stirring and evenly mixing;
(vacuum tightness is 10.0*10 under vacuum with the feed liquid for preparing
4Pa) stir stirring velocity 180r/min, degassed 15 minutes; Place forming mould to be cured the material after degassed again, release after 3.5 hours, die temperature is 95 ℃;
Again with the constant temperature insulation 1.5 hours under 65 ℃ of temperature of above-mentioned sheet material after release.Gained sheet material is processed into test bars by the standard test requirement, tests its performance and list in the table 1.
Comparative example 2
Do not add fortifying fibre, all the other are with embodiment 5., stirred 10 minutes under 80 ℃ of conditions in 100 parts of Resins, epoxy, 18 parts of dioctyl phthalate (DOP)s, 15 parts of butadiene-acrylonitrile rubbers, 100 parts of silica powders, 15 parts of adding reactors of glycidyl allyl ether by recipe ratio;
In 25 parts of decabromodiphenyl oxides, 6 parts of addings of zinc borate said mixture, be heated to 90 ℃, and stir to occurring without solid particulate; Add again 15 parts of diethylenetriamines-propylene oxide phenyl ether affixture, stirring and evenly mixing;
(vacuum tightness is 10.0*10 under vacuum with the feed liquid for preparing
4Pa) stir stirring velocity 180r/min, degassed 15 minutes; Place forming mould to be cured the material after degassed again, release after 3.5 hours, die temperature is 95 ℃;
Again with the constant temperature insulation 1.5 hours under 65 ℃ of temperature of above-mentioned sheet material after release.Gained sheet material is processed into test bars by the standard test requirement, tests its performance and list in the table 1.
Comparative example 3
Do not add fire retardant, all the other are with embodiment 4., stirred 12 minutes under 75 ℃ of conditions in 100 parts of Resins, epoxy, 15 parts of dibutyl phthalates, 10 parts of butadiene-acrylonitrile rubbers, 100 parts in glass fibre, 10 parts of adding reactors of glycidyl allyl ether by recipe ratio;
In 28 parts of decabromodiphenyl oxides, 8 parts of addings of antimonous oxide said mixture, be heated to 100 ℃, and stir to occurring without solid particulate; Add again 18 parts of glyoxal ethylines, stirring and evenly mixing;
(vacuum tightness is 9.5*10 under vacuum with the feed liquid for preparing
4Pa) stir stirring velocity 200r/min, degassed 10 minutes; Place forming mould to be cured the material after degassed again, release after 3.5 hours, die temperature is 85 ℃;
Again with the constant temperature insulation 2.5 hours under 55 ℃ of temperature of above-mentioned sheet material after release.Gained sheet material is processed into test bars by the standard test requirement, tests its performance and list in the table 1.
By every data in the table 1 as can be known, the over-all properties of embodiment 4,5 products obtained therefroms is better, satisfies the performance requriements of product.Do not add softening agent in the Comparative Examples 1, toughner significantly reduces sheet bending intensity, shock strength, fragility is large, be difficult for processing, do not reach the performance requriements of product; Do not add fortifying fibre in the Comparative Examples 2, make the tensile strength decrease of sheet material, can not satisfy the product mechanical property requirements; Do not add fire retardant in the Comparative Examples 3, make the oxygen index of sheet material sample very low, flame retardant effect does not reach the V-0 grade standard of UL-94.
Table 1
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.The person skilled in the art obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not breaking away from the improvement that category of the present invention makes and revise all should be within protection scope of the present invention.
Claims (10)
1. epoxy plastics sheet material, it is characterized in that: it comprises following component and weight part:
100 parts of Resins, epoxy,
5～20 parts in softening agent,
3～15 parts of toughner,
80～150 parts of fortifying fibres,
0～100 part of weighting agent,
8～15 parts of thinners,
15～30 parts of fire retardants,
3～8 parts of fire retarding synergists,
5～18 parts in solidifying agent.
2. epoxy plastics sheet material according to claim 1, it is characterized in that: described Resins, epoxy is selected from bisphenol A type epoxy resin, novolac epoxy or tricyanic epoxy resin, and described per kilogram Resins, epoxy contains the oxirane value of 4.3～5.1 equivalents, fugitive constituent≤1%.
3. epoxy plastics sheet material according to claim 1, it is characterized in that: described softening agent is selected from dioctyl phthalate (DOP), dibutyl phthalate, Dinonylphthalate or dioctyl terephthalate; Or described toughner is selected from polyamide resin, butadiene-acrylonitrile rubber or terpolymer EP rubber.
4. epoxy plastics sheet material according to claim 1, it is characterized in that: described fortifying fibre is selected from glass fibre, carbon fiber or fibrous magnesium silicate; Or described weighting agent is selected from silica powder, mica powder, calcium carbonate or titanium dioxide, and the granularity of described silica powder is greater than 270 orders, whiteness 85-90.
5. epoxy plastics sheet material according to claim 1, it is characterized in that: described thinner is selected from pimelinketone, dimethylbenzene, vinylbenzene, styrene oxide, phenyl glycidyl ether or glycidyl allyl ether.
6. epoxy plastics sheet material according to claim 1, it is characterized in that: described fire retardant is selected from trimeric cyanamide, melamine cyanurate, coating polyphosphoric acid amine, magnesium hydroxide, aluminium hydroxide, decabromodiphenyl oxide, tetrabromo-bisphenol, chlorinatedpolyethylene or clorafin.
7. epoxy plastics sheet material according to claim 1, it is characterized in that: described fire retarding synergist is selected from calcium oxide, aluminum oxide, boron trioxide, titanium oxide zinc oxide, magnesium oxide, silicon oxide, zinc borate, hydrotalcite or antimonous oxide; Or described solidifying agent is selected from a kind of in quadrol, diethylenetriamine-propylene oxide phenyl ether affixture, isophthalic triamine, Tetra hydro Phthalic anhydride or the glyoxal ethyline, and the amine value of described solidifying agent diethylenetriamine-propylene oxide phenyl ether affixture is 680～720.
8. above-mentioned epoxy plastics preparation of plates method is characterized in that: may further comprise the steps:
(1) takes by weighing each raw material in ratio claimed in claim 1, Resins, epoxy, softening agent, toughner, fortifying fibre, weighting agent, thinner are added in the reactor, stir;
(2) fire retardant and fire retarding synergist are joined in the mixture of preparation in the step (1), be heated to 80～100 ℃, and stir to occurring without solid particulate; Add again solidifying agent, stirring and evenly mixing;
(3) feed liquid for preparing is stirred under vacuum, degassed;
(4) place forming mould to be cured the material after degassed again, release after 3～4 hours, die temperature is 80～100 ℃; Again with the constant temperature insulation 1.5～2.5 hours under 55～65 ℃ of temperature of above-mentioned sheet material after release.
9. preparation method according to claim 8, it is characterized in that: the whipping temp of described step (1) is 70～80 ℃, churning time is 8～12 minutes.
10. preparation method according to claim 8, it is characterized in that: the vacuum tightness of described step (3) is 9.0～10.0 * 10
4Pa, stirring velocity 160～200r/min, the degassed time is 10-15 minute.
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