CN102585440B - High-CTI (comparative tracking index) halogen-free flame retardant resin composition for copper-clad laminate - Google Patents
High-CTI (comparative tracking index) halogen-free flame retardant resin composition for copper-clad laminate Download PDFInfo
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Abstract
The invention discloses a high-CTI (comparative tracking index) halogen-free flame retardant resin composition for a copper-clad laminate. The composition comprises the following components in parts by weight: 30-70 parts of polyepoxy resin, 1-5 part of curing agent, 0.01-1 parts of curing promoter, and 20-60 parts of filler. The resin composition disclosed by the invention remains high heat resistance while being endued with a high CTI value. The resin composition disclosed by the invention not only contains phosphorus epoxy resin, but also is added with some tough epoxy resins, so that the processing characteristics are greatly improved. The copper-clad laminate fabricated with the resin composition disclosed by the invention has the characteristics of high heat resistance, high CTI value, no halogen, good processing characteristics and the like.
Description
Technical field
The present invention relates to the high CTI value halogen free flame-retardant type resin combination for copper clad foil substrate.
Background technology
Along with scientific and technical develop rapidly, the formation that large-scale industry is integrated causes the infringement that can't remedy to mankind itself's living environment, and is very urgent thereby environment protection becomes.In recent years, the electronic technology develop rapidly, electronic product is serious day by day to the influence that environment produces, electronic waste product particularly, present most electronic products are halogen flame retardant, after the halogen burning, not only the amount of being fuming is big, and the smell is awful, and can produce the very strong hydrogen halide of corrodibility.According to another bibliographical information, the time can produce Dioxins at halogen-containing fire retardant at Pintsch process and burning in recent years, carcinogenic substances such as diphenylene-oxide, " about scrapping the electric/electronic device instruction " and " using the objectionable impurities instruction about restriction in electric/electronic device " have been put into effect in Europe, electronic product must not contain lead (Lead) after requiring on July in 2006 1, cadmium (Cadmium), mercury (Mercury), sexavalent chrome six kinds of materials such as (Hexavalent Chromium), Japan is the relevant decree of corresponding proposition halogen-free flameproof also, special SONY proposes all to adopt the Halogen material, therefore the baseplate material of developing halogen-free flame-retardant is imperative, has become the focus of industry.
On the other hand, human lives's security more and more extensively is subjected to the concern of society.For improving the safe reliability of electronic product, special in the insulating material that uses under the wet environment condition (as motor, electrical equipment etc.) safe reliability, exploitation high-insulativity product assurance electronic product safe reliability is exactly an important developing direction in recent years.The CTI value that the macromolecular material copper-clad plate is tested (Comparative Tracking Index), refer to material surface to be able to take 50 electrolytic solution (0.1% aqueous ammonium chloride solution) and do not form the maximum voltage value of tracking, it weighs the insulation safety performance of this material to a certain extent, this value is more high, the insulativity that represents material is more good, and (CTI 〉=600V is 0 grade; 400V≤CTI＜600V is 1 grade; 250V≤CTI＜400V is 2 grades; 175V≤CTI＜250V is 3 grades; 100V≤CTI＜175V is 4 grades; CTI＜100V is 5 grades), therefore high CTI product (CTI is more than 600V) has become electron trade researchdevelopment trend.
In recent years the high CTI sheet material of some mainly is the CEM-3 material, but since electric relevant industries implementation is unleaded, the hot environment of product application requires also correspondingly improving constantly, thermotolerance to material proposes new requirement, therefore the CEM-3 material reaches above requirement just has some unable to do what one wishes, and also there is the bad problem of thermotolerance in the FR4 sheet material of more existing high CTI, this kind sheet material generally all is to use ATH(aluminium hydroxide) CTI is provided, but ATH adds and can produce stable on heating decline, and ATH adds less the fire-retardant requirement that do not reach again.
Summary of the invention
The object of the present invention is to provide the high CTI value halogen free flame-retardant type resin combination for copper clad foil substrate.
The technical solution used in the present invention is:
Be used for the high CTI value halogen free flame-retardant type resin combination of copper clad foil substrate, contain following parts by weight of component: 30～70 parts of poly epoxy resins, 1～5 part in solidifying agent, 0.01～1 part of curing catalyst, 20～60 parts of fillers.
Preferably, said composition contains following parts by weight of component: 40～60 parts of poly epoxy resins, 1.5～3 parts in solidifying agent, 0.05～0.5 part of curing catalyst, 25～55 parts of fillers.
Preferably, poly epoxy resin is the bifunctional epoxy resin, novolac epoxy, at least a in the phosphorous epoxy resin.
Preferably, described bifunctional epoxy resin is at least a in bisphenol A type epoxy resin, the bisphenol f type epoxy resin;
Described novolac epoxy is at least a in phenol phenol aldehyde type epoxy resin, ortho-cresol phenolic aldehyde type Resins, epoxy, the bisphenol A-type novolac epoxy;
Described phosphorous epoxy resin is 9, the 10-dihydro-9-oxy is assorted-and the DOPO modified epoxy), 10-(2 10-phospho hetero phenanthrene-10-oxide modifying Resins, epoxy (is called for short:, the 5-dihydroxy phenyl)-9, the 10-dihydro-9-oxy is assorted-and the DOPO-HQ modified epoxy), 10-(2 10-phospho hetero phenanthrene-10-oxide modifying Resins, epoxy (is called for short:, 9-dihydroxyl naphthyl)-9, the 10-dihydro-9-oxy is assorted-and 10-phospho hetero phenanthrene-10-oxide modifying Resins, epoxy (is called for short: at least a the DOPO-NQ modified epoxy).
Preferably, said composition contains following parts by weight of component: 30～40 parts of phosphorous epoxy resins, 5～10 parts of bifunctional epoxy resins, 5～10 parts of novolac epoxys, 1.5～3 parts in solidifying agent, 0.05～0.5 part of curing catalyst, 25～55 parts of fillers.
Preferably, said composition contains following parts by weight of component: 30～39 parts of phosphorous epoxy resins, 10～21 parts of bifunctional epoxy resins, 1.5～3 parts in solidifying agent, 0.05～0.5 part of curing catalyst, 25～55 parts of fillers.
Preferably, said composition contains following parts by weight of component: 30～49 parts of phosphorous epoxy resins, 10～21 parts of novolac epoxys, 1.5～3 parts in solidifying agent, 0.05～0.5 part of curing catalyst, 25～55 parts of fillers.
Preferably, filler is made up of aluminium hydroxide, boehmite; Or filler is made up of silicon-dioxide, aluminium hydroxide, boehmite.
Preferably, the particle diameter of filler is 1～5 μ m.
Preferably, the weight proportion of aluminium hydroxide is 10～25 parts.
Preferably, the weight proportion of boehmite is 10～50 parts.
Preferably, solidifying agent is Dyhard RU 100.
Preferably, curing catalyst is any in glyoxal ethyline, 2-ethyl-4-methylimidazole, 2-ethyl imidazol(e), 2-phenylimidazole, undecyl imidazole, the benzyldimethylamine.
Boehmite of the present invention also claims the hydration Alpha-alumina.
The invention has the beneficial effects as follows:
Resin combination of the present invention has been endowed high CTI value when keeping high heat resistance, resin combination of the present invention not only has phosphorous epoxy resin, some tough epoxy resins have also been added, improve processing characteristics greatly, adopt imidazoles as curing catalyst simultaneously, can control the speed of response of the course of processing.
The copper clad foil substrate that resin combination of the present invention is made has the thermotolerance height, CTI value height, halogen, and characteristic such as good processability.
The flame retardant effect of resin combination of the present invention is mainly provided by the phosphorus in the phosphorous epoxy resin, filler boehmite, aluminium hydroxide, makes system reach the requirement of Halogen.
The present invention just can reach taking into account of system thermotolerance and high CTI value by the ratio of adjustment system boehmite and aluminium hydroxide, and since its hardness, therefore to add this filler than little many of silicon-dioxide also less to the processing influence of subsequent substrate.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment, but be not limited thereto.
Boehmite, particle diameter are 1～5 μ m, and model: 613L is available from prosperous source, Bangbu quartz material company limited;
Aluminium hydroxide, particle diameter are 1～5 μ m, model: H-42M, the clear and production of Japan;
Silicon-dioxide, particle diameter are 1～5 μ m, model: DB1003, and the East China Sea silicon powder is produced;
Undecyl imidazole changes into available from Japanese four countries;
The DOPO modified epoxy, model: PE-315, the massfraction of phosphorus are 3.6%, available from Taiwan Jinyi Chemicals Co., Ltd.;
Bisphenol A type epoxy resin, model 901 is available from Hongchang Electronic Material Inustry Co., Ltd., Guangzhou;
The bisphenol A-type novolac epoxy, model: 3180, available from Korea S kolon company;
The DOPO-NQ modified epoxy, model: YEP-220 is available from wide mountain, Quzhou chemical industry company limited;
The DOPO-HQ modified epoxy, model: G261 is available from Yixing ancient cooking vessel wound company;
Bisphenol f type epoxy resin, model: 201, available from Hongchang Electronic Material Inustry Co., Ltd., Guangzhou.
Embodiment 1
A kind of high CTI value halogen free flame-retardant type resin combination contains following parts by weight of component: 39 parts of DOPO modified epoxies, 21 parts of bisphenol A type epoxy resins, 2 parts of Dyhard RU 100s, 0.3 part of undecyl imidazole, 10 parts in aluminium hydroxide, 28 parts of boehmites.
Embodiment 2
A kind of high CTI value halogen free flame-retardant type resin combination contains following parts by weight of component: 39 parts of DOPO modified epoxies, 21 parts of bisphenol-A phenolic type Resins, epoxy, 2 parts of Dyhard RU 100s, 0.2 part of undecyl imidazole, 19 parts in aluminium hydroxide, 19 parts of boehmites.
Embodiment 3
A kind of high CTI value halogen free flame-retardant type resin combination contains following parts by weight of component: 31.5 parts of DOPO modified epoxies, 17 parts of bisphenol-A phenolic type Resins, epoxy, 1.5 parts of Dyhard RU 100s, 0.5 part of undecyl imidazole, 20 parts in aluminium hydroxide, 30 parts of boehmites.
Embodiment 4
A kind of high CTI value halogen free flame-retardant type resin combination contains following parts by weight of component: 30 parts of DOPO-NQ modified epoxies, 5 parts of bisphenol f type epoxy resins, 5 parts of ortho-cresol phenolic aldehyde type Resins, epoxy, 3 parts of Dyhard RU 100s, 0.05 part of 2-ethyl imidazol(e), 25 parts in aluminium hydroxide, 30 parts of boehmites.
Embodiment 5
A kind of high CTI value halogen free flame-retardant type resin combination contains following parts by weight of component: 35 parts of DOPO-HQ modified epoxies, 8 parts of bisphenol f type epoxy resins, 8 parts of phenol phenol aldehyde type epoxy resins, 1.5 parts of Dyhard RU 100s, 0.3 part of 2-ethyl-4-methylimidazole, 20 parts in aluminium hydroxide, 10 parts of boehmites.
Embodiment 6
A kind of high CTI value halogen free flame-retardant type resin combination contains following parts by weight of component: 40 parts of DOPO-HQ modified epoxies, 10 parts of bisphenol A type epoxy resins, 10 parts of ortho-cresol phenolic aldehyde type Resins, epoxy, 2 parts of Dyhard RU 100s, 0.5 part of 2-phenylimidazole, 10 parts in aluminium hydroxide, 15 parts of boehmites.
Embodiment 7
A kind of high CTI value halogen free flame-retardant type resin combination contains following parts by weight of component: 30 parts of DOPO-NQ modified epoxies, 1 part of Dyhard RU 100,1 part of 2-ethyl-4-methylimidazole, 10 parts in aluminium hydroxide, 10 parts of boehmites.
Embodiment 8
A kind of high CTI value halogen free flame-retardant type resin combination contains following parts by weight of component: 35 parts of phenol phenol aldehyde type epoxy resins, 35 parts of bisphenol f type epoxy resins, 5 parts of Dyhard RU 100s, 0.01 part of benzyldimethylamine, 10 parts in aluminium hydroxide, 50 parts of boehmites.
Embodiment 9
A kind of high CTI value halogen free flame-retardant type resin combination contains following parts by weight of component: 30 parts of DOPO-NQ modified epoxies, 15 parts of bisphenol A type epoxy resins, 1.5 parts of Dyhard RU 100s, 0.05 part of 2-ethyl imidazol(e), 25 parts in aluminium hydroxide, 30 parts of boehmites.
Embodiment 10
A kind of high CTI value halogen free flame-retardant type resin combination contains following parts by weight of component: 35 parts of DOPO modified epoxies, 10 parts of bisphenol f type epoxy resins, 3 parts of Dyhard RU 100s, 0.5 part of 2-ethyl-4-methylimidazole, 15 parts in aluminium hydroxide, 10 parts of boehmites.
Embodiment 11
A kind of high CTI value halogen free flame-retardant type resin combination contains following parts by weight of component: 30 parts of DOPO-HQ modified epoxies, 18 parts of phenol phenol aldehyde type epoxy resins, 3 parts of Dyhard RU 100s, 0.5 part of 2-phenylimidazole, 15 parts in aluminium hydroxide, 10 parts of boehmites.
Embodiment 12
A kind of high CTI value halogen free flame-retardant type resin combination contains following parts by weight of component: 34 parts of DOPO-HQ modified epoxies, 10 parts of ortho-cresol phenolic aldehyde type Resins, epoxy, 1.5 parts of Dyhard RU 100s, 0.05 part of 2-phenylimidazole, 25 parts in aluminium hydroxide, 30 parts of boehmites.
Comparative Examples 1
A kind of resin combination contains following parts by weight of component: 39 parts of DOPO modified epoxies, 21 parts of bisphenol A type epoxy resins, 2 parts of Dyhard RU 100s, 0.3 part of undecyl imidazole, 38 parts in aluminium hydroxide.
Comparative Examples 2
A kind of resin combination contains following parts by weight of component: 39 parts of DOPO modified epoxies, 21 parts of bisphenol A type epoxy resins, 2 parts of Dyhard RU 100s, 0.3 part of undecyl imidazole, 38 parts of boehmites.
Comparative Examples 3
A kind of resin combination contains following parts by weight of component: 39 parts of DOPO modified epoxies, 21 parts of bisphenol A type epoxy resins, 2 parts of Dyhard RU 100s, 0.3 part of undecyl imidazole, 38 parts of silicon-dioxide.
The moulding process of copper clad foil substrate comprises the steps:
1. resin combination is prepared into the thermoset glue:
1) under the room temperature, in proportion container, adds resin combination (except the filler), solvent and thinner, stir, add filler, stirred 6 hours, get glue;
2) sampling, the test glue is controlled its gel time at the gel time of 170 ℃ of hot plates between 200～300 seconds by the addition of curing catalyst, gets the thermoset glue.
With dimethyl formamide DMF, pimelinketone, butanone, propylene glycol monomethyl ether, propylene glycol monomethyl ether amyl acetate etc. or its combination as solvent, with acetone, butanone or its combination as thinner.
2. impregnation:
To soak the adhesive plaster of above-mentioned thermoset glue by vertical or horizontal type impregnation machine, by conditions such as control extruding wheel speed, linear speed, wind-warm syndrome and furnace temperature, make prepreg;
Be example with vertical impregnation machine:
The proportion of glue: 1.10～1.20;
Extruding wheel speed :-1.8～-2.5 ± 0.1 M/min;
Main line speed: 5～14 M/min;
Wind-warm syndrome: 130～160 ℃;
Furnace temperature: 140～180 ℃.
Make prepreg by above condition.
3. compacting:
After the prepreg that cuts and Copper Foil combined, put into the vacuum hotpressing machine, compacting obtaining copper clad foil substrate.
Temperature formula: 130 ℃/30min+160 ℃/30min+180 ℃/20min+210 ℃/180min
Pressure formula: 20Kgfcm-2/30min+50Kgfcm
-2/ 15min+95Kgfcm
-2/ 150min+20Kgfcm
-2/ 65min
Vacuum is set: 30mmHg/130min+760mmHg/130min
With the copper clad foil substrate of the resin combination of embodiment 1～8 and Comparative Examples 1～3 preparation, The performance test results sees Table 1 and table 2.As seen from table, resin combination of the present invention can be prepared into resistance toheat and resistance to flame can be good, the copper clad foil substrate of CTI excellent performance, and the processing characteristics of this substrate is preferable, content of halogen and fire-retardant also all in standard range.More as can be known, the aluminium hydroxide in the component of the present invention and boehmite play an important role to the good performance of covering the Copper Foil base by embodiment 1 and Comparative Examples 1～3 data.
The copper clad foil substrate of the resin combination preparation of embodiment 4～8, The performance test results sees Table 2.As seen from table, compared with the test result of embodiment 4～6 by embodiment in the table 1 1～3,7～8, the copper clad foil substrate CTI performance of the resin combination of embodiment 4～6 preparation is more excellent as can be known.
More than the performance test methods of every index as follows:
A. second-order transition temperature: according to differential scanning calorimetry, measure according to the DSC method of IPC-TM-650 2.4.25 defined;
B.CTI(relative discharge tracking index): the method according to GB/T 4207-84 defined is tested;
C. difficult to burn: according to the test of UL94 method regulation;
D. anti-immersed solder: whether the sample (base material of 10cm * 10cm) sample kept 2 hours in 121 ℃, the pressure cooking treatment unit of 105Kpa after is immersed in 30 seconds in the tin stove that is heated to 260 ℃, change with visual inspection;
E. processibility: sample (base material of 28cm * 28cm) is holed, and the abrasion situation of drill point is compared the processing characteristics of base material before and after the comparison boring;
F. content of halogen: measure according to JPCA-ES-01-2003 " without halide copper-clad plate test method ", adopt the content of halogen of oxygen flask combustion method and ion-chromatographic determination veneer sheet.
Claims (5)
1. be used for the high CTI value halogen free flame-retardant type resin combination of copper clad foil substrate, contain following parts by weight of component: 30～70 parts of poly epoxy resins, 1～5 part in solidifying agent, 0.01～1 part of curing catalyst, 20～60 parts of fillers;
Described solidifying agent is Dyhard RU 100;
Described curing catalyst is any in glyoxal ethyline, 2-ethyl-4-methylimidazole, 2-ethyl imidazol(e), 2-phenylimidazole, undecyl imidazole, the benzyldimethylamine;
Described filler is made up of 10～25 weight part aluminium hydroxides, 10～50 weight part boehmites.
2. high CTI value halogen free flame-retardant type resin combination according to claim 1, it is characterized in that: said composition contains following parts by weight of component: 40～60 parts of poly epoxy resins, 1.5～3 parts in solidifying agent, 0.05～0.5 part of curing catalyst, 25～55 parts of fillers.
3. high CTI value halogen free flame-retardant type resin combination according to claim 1 and 2 is characterized in that: at least a in bifunctional epoxy resin, novolac epoxy, the phosphorous epoxy resin of poly epoxy resin.
4. high CTI value halogen free flame-retardant type resin combination according to claim 3 is characterized in that:
Described bifunctional epoxy resin is at least a in bisphenol A type epoxy resin, the bisphenol f type epoxy resin;
Described novolac epoxy is at least a in phenol phenol aldehyde type epoxy resin, ortho-cresol phenolic aldehyde type Resins, epoxy, the bisphenol A-type novolac epoxy;
Described phosphorous epoxy resin is 9, the 10-dihydro-9-oxy is assorted-10-phospho hetero phenanthrene-10-oxide modifying Resins, epoxy, 10-(2, the 5-dihydroxy phenyl)-9, the 10-dihydro-9-oxy is assorted-10-phospho hetero phenanthrene-10-oxide modifying Resins, epoxy, 10-(2,9-dihydroxyl naphthyl)-9, the 10-dihydro-9-oxy is assorted-at least a in 10-phospho hetero phenanthrene-10-oxide modifying Resins, epoxy.
5. high CTI value halogen free flame-retardant type resin combination according to claim 1 and 2, it is characterized in that: the particle diameter of filler is 1～5 μ m.
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| CN110872430A (en) * | 2019-11-29 | 2020-03-10 | 陕西生益科技有限公司 | High CTI resin composition, prepreg, laminated board and metal foil-clad laminated board |
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