CN102796281B - Heat resistant filling material used for brominated modified epoxy copper clad laminate and brominated epoxy resin composition used for copper clad laminate - Google Patents
Heat resistant filling material used for brominated modified epoxy copper clad laminate and brominated epoxy resin composition used for copper clad laminate Download PDFInfo
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- CN102796281B CN102796281B CN201210292545.5A CN201210292545A CN102796281B CN 102796281 B CN102796281 B CN 102796281B CN 201210292545 A CN201210292545 A CN 201210292545A CN 102796281 B CN102796281 B CN 102796281B
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Abstract
The invention relates to a heat resistant filling material used for a modified brominated epoxy copper clad laminate and a brominated epoxy resin composition used for the copper clad laminate. The heat resistant filling material used for the modified epoxy copper clad laminate is a hydrotalcite particle, which is an anionic layered compound, and can be mineral or synthesized. The brominated epoxy resin composition used for the copper clad laminate includes brominated epoxy resin, a curing agent, a curing accelerator, a solvent and the heat resistant filling material, which is a hydrotalcite particle with a particle size D50 of 0.01micrometer-10micrometers. The dosage of the hydrotalcite particle accounts for 0.01-10% of the total weight of a brominated epoxy resin composition solid containing the hydrotalcite particle.
Description
Technical field
The present invention relates to copper-clad plate field, particularly relate to a kind of thermotolerance filler for the copper-clad plate of bromination modified epoxy and the brominated epoxy resin composition for copper-clad plate.
Background technology
Traditional fire-retardant printed electronic circuit copper-clad laminate, is mainly adopted brominated epoxy resin, is realized the anti-flaming function of sheet material by bromine.On July 1st, 2006, two parts of environmental protection instructions " about scrapping electric/electronic device instruction " of European Union and " ROHS " are formally implemented.The formal enforcement of European Union two instruction indicates that global electronic industry enters the pb-free solder epoch, due to the raising of pb-free solder temperature, to the heat resistant requirements also corresponding raising of copper-clad plate.Because the bond energy of carbon-bromine key is lower, most of bromide fire retardant decomposes at 200 to 300 DEG C, improves the focus technology problem that copper-clad plate thermotolerance becomes industry research.
Improve by adding filler the common method that copper-clad plate thermotolerance is industry, filler has mineral filler and organic filler two class, and conventional mineral filler has aluminum oxide, magnesium oxide or zinc oxide etc.Hydrotalcite is a kind of novel inorganic filling material, and hydrotalcite lamellar compound (LDHs) is anion type laminated compound, has certain weakly alkaline, and has the feature such as the exchangeability of interlayer ion and the Modulatory character of grain size distribution; Two-dimensional layer inorganics hydrotalcite has the functions such as fire-retardant, smoke elimination, filling, is a kind of BACN of efficient, Halogen, nontoxic, low cigarette.But using little for the research of hydrotalcite lamellar compound as applying filler in copper-clad plate field, the research of applying the thermotolerance of its raising copper-clad plate is just less.
Summary of the invention
The object of the present invention is to provide a kind of thermotolerance filler for the copper-clad plate of modification brominated epoxy, this thermotolerance filler is hydrotalcite particles, by the interpolation of hydrotalcite particles, the thermotolerance of modified brominated epoxy copper-clad plate is significantly improved.
Another object of the present invention is to provide a kind of brominated epoxy resin composition for copper-clad plate, it comprises brominated epoxy resin and makes an addition to the thermotolerance filler hydrotalcite particles in brominated epoxy resin, and the thermotolerance of the copper-clad plate using this brominated epoxy resin composition to make significantly improves.
For achieving the above object, the invention provides a kind of thermotolerance filler for the copper-clad plate of modification brominated epoxy, described thermotolerance filler is hydrotalcite particles, and its general formula is: M
k+mn
n+p(OH)
2a
z y-xH
2o, wherein,
M is any 1+ or 2+ positively charged ion and combination thereof;
N is any 3+ or 4+ positively charged ion and combination thereof;
K is the single molar fraction sum of 1+ positively charged ion;
M is the single molar fraction sum of 2+ positively charged ion;
N is the single molar fraction sum of 3+ positively charged ion;
P is the single molar fraction sum of 4+ positively charged ion;
And k or m can be zero, but both at the most one be zero, and n or p can be zero, but both at the most one be zero, and k+m+n+p=1;
A
z y-be electric charge be y
-with any negatively charged ion that molar fraction is z, more than one y
-the combination of negatively charged ion, in general formula, the scope of k+2m+3n+4p-2-zy=0, x is 1-100;
The example of above formula cationic M has Mg
2+, Ni
2+, Co
2+, Zn
2+, Cu
2+, Ca
2+, Sr
2+, the example of suitable positively charged ion N has: Al
3+, Cr
3+, Fe
3+, Sc
3+, Ti
4+or Sn
4+;
Preferred divalent cation is Mg
2+, Zn
2+, Cu
2+or the combination of these ions, or with the combination of other divalent cation;
Negatively charged ion A can be inorganic or organic anion; Preferred inorganic anion is CO
3 2-, NO
3 -, OH
-, Cl
-, SO
4 2-; The example of organic anion is carboxylic acid ion, as citric acid and stearic acid.
Described hydrotalcite particles for for anion type laminated compound, can be mineral also can be synthesis.It has the exchangeability of laminate structure and interlayer ion, and this interlayer structure and interlayer ion exchangeability make it can absorb and exchange small molecules and the ion of bromine, thus improves the thermotolerance of composition.
The particle diameter D of described hydrotalcite particles
50for 0.01um ~ 10um.
Described hydrotalcite particles is obtained by hydrotalcite lamellar compound.
Described hydrotalcite lamellar compound is at least one in hydrotalcite, houghite and pillared hydrotalcite.
The present invention also provides a kind of brominated epoxy resin composition for copper-clad plate, comprise brominated epoxy resin, solidifying agent, curing catalyst, solvent and thermotolerance filler, described thermotolerance filler is hydrotalcite particles, and the consumption of described hydrotalcite particles is that this contains the 0.01-10% of the composition epoxy resin total weight of solids of hydrotalcite particles.
The general formula of described hydrotalcite particles is: M
k+mn
n+p(OH)
2a
z y-xH
2o, wherein,
M is any 1+ or 2+ positively charged ion and combination thereof;
N is any 3+ or 4+ positively charged ion and combination thereof;
K is the single molar fraction sum of 1+ positively charged ion;
M is the single molar fraction sum of 2+ positively charged ion;
N is the single molar fraction sum of 3+ positively charged ion;
P is the single molar fraction sum of 4+ positively charged ion;
And k or m can be zero, but both at the most one be zero, and n or p can be zero, but both at the most one be zero, and k+m+n+p=1;
A
z y-be electric charge be y
-with any negatively charged ion that molar fraction is z, more than one y
-the combination of negatively charged ion, in general formula, the scope of k+2m+3n+4p-2-zy=0, x is 1-100;
The example of above formula cationic M has Mg
2+, Ni
2+, Co
2+, Zn
2+, Cu
2+, Ca
2+, Sr
2+, the example of suitable positively charged ion N has: Al
3+, Cr
3+, Fe
3+, Sc
3+, Ti
4+or Sn
4+;
Preferred divalent cation is Mg
2+, Zn
2+, Cu
2+or the combination of these ions, or with the combination of other divalent cation;
Negatively charged ion A can be inorganic or organic anion; Preferred inorganic anion is CO
3 2-, NO
3 -, OH
-, Cl
-, SO
4 2-; The example of organic anion is carboxylic acid ion, as citric acid and stearic acid.
Described hydrotalcite particles for for anion type laminated compound, can be mineral also can be synthesis.
The particle diameter D of described hydrotalcite particles
50for 0.01um ~ 10um.
Described hydrotalcite particles is obtained by hydrotalcite lamellar compound, and described hydrotalcite lamellar compound is at least one in hydrotalcite, houghite and pillared hydrotalcite.
Beneficial effect of the present invention: the thermotolerance filler for the copper-clad plate of bromination modified epoxy of the present invention, it is hydrotalcite particles, by making to contain a certain amount of hydrotalcite particles in copper-clad plate, can significantly improve the thermotolerance of copper-clad plate; Brominated epoxy resin composition for copper-clad plate of the present invention, comprise brominated epoxy resin and make an addition to the hydrotalcite particles in brominated epoxy resin, and the thermally stratified layer time of the copper-clad plate using this brominated epoxy resin composition to make rises appreciably, heat decomposition temperature significantly improves, thus improve its thermotolerance, and be conducive to its scale operation, reduce costs.
In order to further understand feature of the present invention and technology contents, refer to following detailed description for the present invention.
Embodiment
The invention provides a kind of thermotolerance filler for the copper-clad plate of modification brominated epoxy, described thermotolerance filler is hydrotalcite particles, and its general formula is: M
k+mn
n+p(OH)
2a
z y-xH
2o
Wherein,
M is any 1+ or 2+ positively charged ion and combination thereof;
N is any 3+ or 4+ positively charged ion and combination thereof;
K is the single molar fraction sum of 1+ positively charged ion;
M is the single molar fraction sum of 2+ positively charged ion;
N is the single molar fraction sum of 3+ positively charged ion;
P is the single molar fraction sum of 4+ positively charged ion;
And k or m can be zero, but both at the most one be zero, and n or p can be zero, but both at the most one be zero, and k+m+n+p=1;
A
z y-be electric charge be y
-with any negatively charged ion that molar fraction is z, more than one y
-the combination of negatively charged ion, in general formula, the scope of k+2m+3n+4p-2-zy=0, x is 1-100;
The example of above formula cationic M has Mg
2+, Ni
2+, Co
2+, Zn
2+, Cu
2+, Ca
2+, Sr
2+, the example of suitable positively charged ion N has: Al
3+, Cr
3+, Fe
3+, Sc
3+, Ti
4+or Sn
4+;
Preferred divalent cation is Mg
2+, Zn
2+, Cu
2+or the combination of these ions, or with the combination of other divalent cation;
Negatively charged ion A can be inorganic or organic anion; Preferred inorganic anion is CO
3 2-, NO
3 -, OH
-, Cl
-, SO
4 2-; The example of organic anion is carboxylic acid ion, as citric acid and stearic acid.
Described hydrotalcite particles has the exchangeability of laminate structure and interlayer ion, and this interlayer structure and interlayer ion exchangeability make it can absorb and exchange molecular bromine and ion in brominated epoxy resin composition.Two-dimensional layer inorganics hydrotalcite has the functions such as fire-retardant, smoke elimination, filling, is a kind of BACN of efficient, Halogen, nontoxic, low cigarette, in copper-clad plate, therefore adds a certain amount of hydrotalcite particles, can improve the thermotolerance of copper-clad plate.
Described hydrotalcite particles is anion type laminated compound, can be mineral also can be synthesis, typical hydrotalcite-based compound is Mg
6a1
2(OH)
16cO
34H
2o, is one of naturally occurring laminated clay ore deposit, finds before and after 1842 in Sweden.
The particle diameter D of hydrotalcite particles described in the present invention
50for 0.01um ~ 10um.
Described hydrotalcite particles is obtained by hydrotalcite lamellar compound.Described hydrotalcite nonwoven fabric from filaments can adopt natural mineral, also can pass through chemosynthesis.
Described hydrotalcite lamellar compound is at least one in hydrotalcite, houghite and pillared hydrotalcite.Described hydrotalcite lamellar compound is anion type laminated compound, lamellar compound refer to there is laminate structure, a compounds that interlayer ion has interchangeability, there is certain weakly alkaline.Owing to being made up of the metal oxide of two kinds of different price types between hydrotalcite lamellar compound laminate, so be also called layered bi-metal oxide compound (being called for short LDH).
The present invention also provides a kind of brominated epoxy resin composition for copper-clad plate, and comprise brominated epoxy resin and make an addition to the hydrotalcite particles in brominated epoxy resin, its general formula is: M
k+mn
n+p(OH)
2a
z y-xH
2o, wherein,
M is any 1+ or 2+ positively charged ion and combination thereof;
N is any 3+ or 4+ positively charged ion and combination thereof;
K is the single molar fraction sum of 1+ positively charged ion;
M is the single molar fraction sum of 2+ positively charged ion;
N is the single molar fraction sum of 3+ positively charged ion;
P is the single molar fraction sum of 4+ positively charged ion;
And k or m can be zero, but both at the most one be zero, and n or p can be zero, but both at the most one be zero, and k+m+n+p=1;
A
z y-be electric charge be y
-with any negatively charged ion that molar fraction is z, more than one y
-the combination of negatively charged ion, in general formula, the scope of k+2m+3n+4p-2-zy=0, x is 1-100;
The example of above formula cationic M has Mg
2+, Ni
2+, Co
2+, Zn
2+, Cu
2+, Ca
2+, Sr
2+, the example of suitable positively charged ion N has: Al
3+, Cr
3+, Fe
3+, Sc
3+, Ti
4+or Sn
4+;
Preferred divalent cation is Mg
2+, Zn
2+, Cu
2+or the combination of these ions, or with the combination of other divalent cation;
Negatively charged ion A can be inorganic or organic anion; Preferred inorganic anion is CO
3 2-, NO
3 -, OH
-, Cl
-, SO
4 2-; The example of organic anion is carboxylic acid ion, as citric acid and stearic acid.
Described hydrotalcite particles for for anion type laminated compound, can be mineral also can be synthesis, typical hydrotalcite-based compound is Mg
6a1
2(OH)
16cO
34H
2o, is one of naturally occurring laminated clay ore deposit, finds before and after 1842 in Sweden.
The particle diameter D of hydrotalcite particles described in the present invention
50for 0.01um ~ 10um.
Described hydrotalcite particles is obtained by hydrotalcite lamellar compound, and described hydrotalcite lamellar compound is at least one in hydrotalcite, houghite and pillared hydrotalcite.
Using above-mentioned brominated epoxy resin composition to prepare described copper-clad plate can adopt ordinary method to prepare: the glue each component of brominated epoxy resin composition of the present invention being hybridly prepared into solids content 65-75%, with glasscloth if electron glass fiber cloth is containing being dipped in glue, then drying, semicure, drying condition can be: 170 DEG C/5-8 minute, make bonding sheet, with this bonding sheet number open superimposed after, be covered with Copper Foil in its one or both sides, this copper-clad plate obtained after thermocompressor lamination.Described modification brominated epoxy copper-clad plate lamination need meet following requirement: 1, the temperature rise rate of lamination, and the heat-up rate usually when material temperature 80-160 DEG C should control at 1.0-3.0 DEG C/min; 2, the pressure of lamination is arranged, and outer material temperature applies full pressure 80 ~ 100 DEG C time, and full pressure pressure is about 300psi; 3, during solidification, control material temperature at 175-200 DEG C, and be incubated 40-90min.
The copper-clad plate of above-mentioned making comprises: several mutual superimposed bonding sheets and the Copper Foil be overlaid on these superimposed bonding sheet one or both sides, and this bonding sheet comprises base-material and by the dry postadhesion of impregnation brominated epoxy resin composition thereon.Described base-material adopts natural fiber, organic synthetic fibers or inorganic fibre, as glasscloth.Copper Foil adopts electrolytic copper foil or rolled copper foil.Described Copper Foil also can adopt the replacements such as nickel foil, aluminium foil or SUS paper tinsel.
Illustrate in detail the present invention by the following examples and describe, described embodiment brominated epoxy resin composite formula is in table 1, table 2.Wherein copper-clad plate covers obtained double face copper by the Copper Foil of 8 bonding sheets and two ounce (35um is thick), and obtained copper-clad plate characteristic data is in table 3, table 4.
Table 1. brominated epoxy resin composite formula 1
| Component (weight part) | Embodiment 1 | Embodiment 2 | Comparative example 1 | Comparative example 2 |
| Brominated epoxy resin DER530 | 100 | 100 | 100 | 100 |
| DICY | 3.0 | 3.0 | 3.0 | 3.0 |
| Glyoxal ethyline | 0.10 | 0.10 | 0.10 | 0.10 |
| Hydrotalcite particles | 1 | 5 | 0 | 20 |
| Dimethyl formamide | In right amount | In right amount | In right amount | In right amount |
| Solids content (%) | 65 | 65 | 65 | 65 |
Table 2. brominated epoxy resin composite formula 2
Table 3. modification brominated epoxy copper-clad plate characteristic data 1
Table 4. modification brominated epoxy copper-clad plate characteristic data 2
The testing method of above characteristic is as follows:
(1), second-order transition temperature (Tg): according to dsc (DSC), measure according to the DSC method of IPC-TM-650 2.4.25 defined.
(2), stripping strength (PS): according to " after the thermal stresses " experiment condition in IPC-TM-650 2.4.8 method, test the stripping strength of metallic cover layer.
(3), incendivity: measure according to UL 94 vertical combustion.
(4), the thermally stratified layer time T-260, T288: measure according to IPC-TM-650 2.4.24.1 method.
(5), heat decomposition temperature Td: measure according to IPC-TM-650 2.4.26 method.
From the Comparative result of table 3, table 4, compared to the copper-clad plate of comparative example 1-3 not containing hydrotalcite particles, the thermally stratified layer time containing the copper-clad plate of the embodiment 1-4 of hydrotalcite particles rises appreciably, and heat decomposition temperature significantly improves, therefore the thermotolerance of the copper-clad plate of embodiment improves.
In sum, the thermotolerance filler for the copper-clad plate of bromination modified epoxy of the present invention is hydrotalcite particles, and the thermotolerance of the copper-clad plate containing this hydrotalcite particles significantly improves; Separately, brominated epoxy resin composition for copper-clad plate of the present invention, by adding a certain amount of hydrotalcite particles in brominated epoxy resin composition, improve the performances such as the thermotolerance of brominated epoxy resin composition, thus improve the thermotolerance using its copper-clad plate made.
The above, for the person of ordinary skill of the art, can make other various corresponding change and distortion according to technical scheme of the present invention and technical conceive, and all these change and be out of shape the protection domain that all should belong to the claims in the present invention.
Claims (6)
1. the brominated epoxy resin composition for copper-clad plate, it is characterized in that, comprise brominated epoxy resin, solidifying agent, curing catalyst, solvent and thermotolerance filler, described thermotolerance filler is hydrotalcite particles, and the consumption of described hydrotalcite particles is that this contains the 0.01-10% of the brominated epoxy resin composition solid gross weight of hydrotalcite particles;
The particle diameter D of described hydrotalcite particles
50for 0.01um ~ 10um.
2., as claimed in claim 1 for the brominated epoxy resin composition of copper-clad plate, it is characterized in that, the general formula of described hydrotalcite particles is: M
k+mn
n+p(OH)
2a
z y-xH
2o
Wherein,
M is any 1+ or 2+ positively charged ion and combination thereof;
N is any 3+ or 4+ positively charged ion and combination thereof;
K is the single molar fraction sum of 1+ positively charged ion;
M is the single molar fraction sum of 2+ positively charged ion;
N is the single molar fraction sum of 3+ positively charged ion;
P is the single molar fraction sum of 4+ positively charged ion;
And k or m can be zero, but both at the most one be zero, and n or p can be zero, but both at the most one be zero, and k+m+n+p=1;
A
z y-be electric charge be y
-with any negatively charged ion that molar fraction is z, more than one y
-the combination of negatively charged ion, in general formula, the scope of k+2m+3n+4p-2-zy=0, x is 1-100;
Above formula cationic M is Mg
2+or Ni
2+, Co
2+, Zn
2+, Cu
2+, Ca
2+, Sr
2+, suitable positively charged ion N is Al
3+or Cr
3+, Fe
3+, Sc
3+, Ti
4+or Sn
4+.
3., as claimed in claim 1 for the brominated epoxy resin composition of copper-clad plate, it is characterized in that, preferred divalent cation is Mg
2+, Zn
2+, Cu
2+or the combination of these ions, or with the combination of other divalent cation.
4., as claimed in claim 1 for the brominated epoxy resin composition of copper-clad plate, it is characterized in that, negatively charged ion A is inorganic or organic anion; Inorganic anion is CO
3 2-, NO
3 -, OH
-, Cl
-, SO
4 2-; Organic anion is carboxylic acid ion.
5., as claimed in claim 1 for the brominated epoxy resin composition of copper-clad plate, it is characterized in that, described hydrotalcite particles is anion type laminated compound, can be mineral also can be synthesis.
6. as claimed in claim 1 for the brominated epoxy resin composition of copper-clad plate, it is characterized in that, described hydrotalcite particles is obtained by hydrotalcite lamellar compound, and described hydrotalcite lamellar compound is at least one in hydrotalcite, houghite and pillared hydrotalcite.
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|---|---|---|---|
| CN201210292545.5A CN102796281B (en) | 2012-08-16 | 2012-08-16 | Heat resistant filling material used for brominated modified epoxy copper clad laminate and brominated epoxy resin composition used for copper clad laminate |
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|---|---|---|---|
| CN201210292545.5A CN102796281B (en) | 2012-08-16 | 2012-08-16 | Heat resistant filling material used for brominated modified epoxy copper clad laminate and brominated epoxy resin composition used for copper clad laminate |
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| CN103555002B (en) * | 2013-11-05 | 2015-06-10 | 重庆市锦艺硅材料开发有限公司 | Inorganic filler for copper-clad plate and preparation method of filler |
| CN112266576A (en) * | 2020-11-04 | 2021-01-26 | 纽宝力精化(广州)有限公司 | Brominated epoxy resin composition for paper substrate |
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| CN101376735B (en) * | 2008-09-26 | 2011-11-30 | 广东生益科技股份有限公司 | Halogen-free flame-proof epoxy resin composition and bonding sheet and copper clad laminate prepared thereby |
| CN102079875B (en) * | 2010-12-18 | 2013-01-02 | 广东生益科技股份有限公司 | High-heat-resistance halogen-free phosphorus-free thermosetting resin composition, and bonding sheet and copper foil-coated laminated board made of same |
| CN102492261B (en) * | 2011-11-14 | 2014-06-04 | 上海南亚覆铜箔板有限公司 | Adhesive for producing common Tg lead-free copper foil-coated plates and preparation method for adhesive |
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