CN106751475A - A kind of halogen-free resin composition and its prepreg being made and copper-clad plate - Google Patents
A kind of halogen-free resin composition and its prepreg being made and copper-clad plate Download PDFInfo
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- CN106751475A CN106751475A CN201611057429.XA CN201611057429A CN106751475A CN 106751475 A CN106751475 A CN 106751475A CN 201611057429 A CN201611057429 A CN 201611057429A CN 106751475 A CN106751475 A CN 106751475A
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- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
- B32B15/092—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising epoxy resins
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
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- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
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- 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
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5313—Phosphinic compounds, e.g. R2=P(:O)OR'
-
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2311/00—Metals, their alloys or their compounds
- B32B2311/12—Copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2363/00—Epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
- C08J2363/04—Epoxynovolacs
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- 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
- 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
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- 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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
The present invention relates to a kind of halogen-free resin composition and its prepreg being made and copper-clad plate, including following component：100 parts of non-halogen non-phosphate epoxy resin, 2 50 parts of curing agent, 0.1 3 parts of curing accelerator, 15 28 parts of fire retardant, 35 55 parts of solvent, resin combination process is simple of the invention, low production cost.It is free of halogen element, can reach " green " fire-retardant effect, the characteristics of have CTI >=600V high, high-peeling strength >=1.90N/mm according to copper-clad plate obtained in the present invention.
Description
Technical field
The present invention relates to a kind of halogen-free resin composition and its prepreg being made and copper-clad plate, belong to copper-clad plate manufacture
Technical field.
Background technology
It is well known that traditional the fire-retardant of copper-clad plate depends on brominated epoxy resin and its synergist-antimony oxide always,
Indispensable role is occupied in composite-based copper clad plate, fire-retardant one is sharp as being solved in copper-clad plate developer's hand
Device.But as research finds that halogen-antimony is fire-retardant to have been found to have harmfulness to health and environment.Therefore new ring is developed
Protect Non-halogen Flame Retardant Technology and have become trend of the times.The country's more widespread practice is to use phosphorous epoxy resin at present, is utilized
Produced segregation phosphoric acid strong dehydration and incarbonization, reaches fire-retardant effect after phasphorus-containing polymer burning.But phosphorous ring
Oxygen tree fat price general charged is higher, so that its cost is greatly improved.
Dialkyl hypophosphorous acid aluminium is a kind of new green environment protection add phosphorus containing flame retardant developed in recent years, relative to it
His additive flame retardant, its flame retarding efficiency and CTI values are higher.The present invention uses dialkyl hypophosphorous acid aluminium and aluminium hydroxide, titanium white
Powder carries out compounding mixing, reaches the purpose of Green Flammability.
The content of the invention
The deficiency that the present invention exists for existing environment friendly halogen-free fireproof technology, there is provided a kind of halogen-free resin composition and its system
Into prepreg and copper-clad plate.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：
A kind of halogen-free resin composition, by weight, including following component：
Further, the fire retardant is aluminium hydroxide, titanium dioxide, the mixture of dialkyl phosphinic acid aluminium.
Further, aluminium hydroxide, titanium dioxide, the part by weight of dialkyl phosphinic acid aluminium three are (5- in the fire retardant
10)：(2-8)：(3-10), the particle diameter of the aluminium hydroxide is 3-5 μm, and the particle diameter of dialkyl phosphinic acid aluminium is 5-20 μm.
Further, the non-halogen non-phosphate epoxy resin is bisphenol A type epoxy resin or novolac epoxy resin.
Further, described curing agent be linear phenolic resin, 4,4- diaminodiphenyl-methanes, methyl hexahydrophthalic anhydride,
One or more in dicyandiamide, 4,4- DADPSs of mixture.
Further, described curing accelerator is in 2-methylimidazole, 2-ethyl-4-methylimidazole, 2- phenylimidazoles
Any one.
Further, described solvent is dimethylformamide, acetone, MEK, glycol monoethyl ether, cyclohexanone, the third two
One kind in alcohol monomethyl ether, ethanol, toluene.
The beneficial effects of the invention are as follows：
1) dialkyl hypophosphorous acid aluminium is free of halogen element, with aluminium hydroxide, titanium dioxide can be reached after compounding mixes " green
The fire-retardant effect of color ".
2) present invention uses cheap base epoxy resin bisphenol A type epoxy resin or novolac epoxy resin, production
Low cost.
3) the characteristics of there is CTI >=600V high, high-peeling strength >=1.90N/mm according to copper-clad plate obtained in the present invention.
The present invention is also claimed the prepreg and copper-clad plate prepared using halogen-free resin composition of the invention.
Specific embodiment
Principle of the invention and feature are described below in conjunction with example, example is served only for explaining the present invention, and
It is non-for limiting the scope of the present invention.
Embodiment 1：
A kind of halogen-free resin composition, by weight, including following component：100 parts of (epoxies of bisphenol A type epoxy resin
Value 0.18-0.22), 18 parts of linear phenolic resin, 0.1 part of 2-ethyl-4-methylimidazole, 5 parts of aluminium hydroxide, 8 parts of titanium dioxide, two
10 parts of ethyl hypo-aluminum orthophosphate, 35 parts of MEK.
Embodiment 2：
A kind of halogen-free resin composition, by weight, including following component：100 parts of (epoxies of bisphenol A type epoxy resin
Value 0.51-0.54), 25 parts of linear phenolic resin, 0.16 part of 2-methylimidazole, 10 parts of aluminium hydroxide, 8 parts of titanium dioxide, diethyl
10 parts of hypo-aluminum orthophosphate, 40 parts of MEK, are blended resin glue.
Embodiment 3：
A kind of halogen-free resin composition, by weight, including following component：100 parts of (epoxide numbers of novolac epoxy resin
0.51-0.54), 50 parts of 4,4- DADPSs, 3 parts of 2- phenylimidazoles, 10 parts of aluminium hydroxide, 2 parts of titanium dioxide, methyl cyclohexane
3 parts of base phosphinic acids aluminium, 15 parts of dimethylformamide, 25 parts of propylene glycol monomethyl ether is blended resin glue.
Embodiment 4：
A kind of halogen-free resin composition, by weight, including following component：100 parts of (epoxide numbers of novolac epoxy resin
0.51-0.54), 2 parts of dicyandiamide, 0.20 part of 2-methylimidazole, 10 parts of aluminium hydroxide, 5 parts of titanium dioxide, diethyl hypo-aluminum orthophosphate 7
Part, 35 parts of dimethylformamide, 20 parts of toluene are blended resin glue.
Above-mentioned halogen-free resin composition can be prepared using conventional preparation method, first by hard resin and admittedly
Agent dissolves in a solvent, stirs to after being completely dissolved, and adds liquid resin and curing accelerator, stirs, and adds hydrogen
Aluminum oxide, titanium dioxide, dialkyl phosphinic acid aluminium, with obtaining final product resin adhesive liquid after mulser emulsion dispersion after stirring；
Gained glue is coated in glass cloth surface by gluing machine, by regulation speed, compression roller gap, wind-warm syndrome, furnace temperature
Etc. condition, that is, desired prepreg is obtained, control resin content is in 39%-48%.It is above-mentioned several to be taken according to thickness requirement
Prepreg, is superimposed together, and Copper Foil is covered with its one side or two sides, is put between two steel plates, the hot pressing in vacuum press,
So as to be pressed into copper-clad plate.
In an embodiment of the present invention, described copper-clad plate is to use above-mentioned eight prepregs and two copper of 35 μ m-thicks
Paper tinsel is superimposed together, by vacuum press in 175 ± 5 DEG C, 35 ± 5kgf/cm2Under the conditions of hot pressing 90min, cooling, obtain final product
1.61/1 copper-clad plate.Then the copper-clad plate performance is tested, concrete outcome is shown in Table 1.
Table 1：The performance test data of embodiment 1-4 gained copper-clad plates
| Detection project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Peel strength (N/mm) | 1.90 | 1.97 | 2.00 | 1.90 |
| CTI | 600 | 600 | 600 | 600 |
| Anti-flammability | FV0 | FV0 | FV0 | FV0 |
| Content of halogen | 0.06 | 0.04 | 0.04 | 0.06 |
| Punching | It is excellent | It is excellent | It is excellent | It is excellent |
Note：
(1) CTI relative discharges tracking index：Method according to GB/T 4207-84 defineds is tested.
(2) flammability：Determined according to UL94 vertical combustions.
(3) content of halogen is according to JPCA-ES-01-2003《Halogen-free type copper-clad plate method of testing》Detection, is burnt using flask
Formula gas assimilating method and ion chromatograph determine the content of halogen of copper-clad plate.
Compared with prior art, the important performance such as anti-flammability, CTI, peel strength reaches for copper-clad plate obtained by the present invention
To or more than generic copper-clad plate performance indications, and low production cost, due to not containing halogen in dipping glue, can subtract
Few its in manufacture and crosses generation pernicious gas health of human body is caused damage using process.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all it is of the invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (10)
1. a kind of halogen-free resin composition, it is characterised in that by weight, including following component：
2. halogen-free resin composition according to claim 1, it is characterised in that the fire retardant is aluminium hydroxide, titanium white
The mixture of powder, dialkyl phosphinic acid aluminium.
3. halogen-free resin composition according to claim 2, it is characterised in that aluminium hydroxide, titanium white in the fire retardant
Powder, the part by weight of dialkyl phosphinic acid aluminium three are (5-10)：(2-8)：(3-10).
4. halogen-free resin composition according to claim 1 and 2, it is characterised in that the particle diameter of the aluminium hydroxide is 3-5
μm, the particle diameter of dialkyl phosphinic acid aluminium is 5-20 μm.
5. halogen-free resin composition according to claim 1 and 2, it is characterised in that the non-halogen non-phosphate epoxy resin is
Bisphenol A type epoxy resin or novolac epoxy resin.
6. halogen-free resin composition according to claim 1 and 2, it is characterised in that described curing agent is novolac
One or more in resin, 4,4- diaminodiphenyl-methanes, methyl hexahydrophthalic anhydride, dicyandiamide, 4,4- DADPSs
Mixture.
7. halogen-free resin composition according to claim 1 and 2, it is characterised in that described curing accelerator is 2- first
Any one in base imidazoles, 2-ethyl-4-methylimidazole, 2- phenylimidazoles.
8. halogen-free resin composition according to claim 1 and 2, it is characterised in that described solvent is dimethyl formyl
One kind in amine, acetone, MEK, glycol monoethyl ether, cyclohexanone, propylene glycol monomethyl ether, ethanol, toluene.
9. the prepreg that a kind of halogen-free resin composition as any one of claim 1-8 is prepared.
10. the copper-clad plate that a kind of prepreg as claimed in claim 9 is prepared.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611057429.XA CN106751475B (en) | 2016-11-26 | 2016-11-26 | A kind of halogen-free resin composition and its manufactured prepreg and copper-clad plate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611057429.XA CN106751475B (en) | 2016-11-26 | 2016-11-26 | A kind of halogen-free resin composition and its manufactured prepreg and copper-clad plate |
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| Publication Number | Publication Date |
|---|---|
| CN106751475A true CN106751475A (en) | 2017-05-31 |
| CN106751475B CN106751475B (en) | 2019-03-15 |
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| CN201611057429.XA Active CN106751475B (en) | 2016-11-26 | 2016-11-26 | A kind of halogen-free resin composition and its manufactured prepreg and copper-clad plate |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1847352A (en) * | 2005-04-13 | 2006-10-18 | 信越化学工业株式会社 | Flame retardant adhesive composition, and adhesive sheet, coverlay film and flexible copper-clad laminate using same |
| CN102241872A (en) * | 2011-06-28 | 2011-11-16 | 江汉大学 | Aluminum methylcyclohexyl phosphinate/epoxy resin flame-retardant composite material |
| JP2012025917A (en) * | 2010-07-27 | 2012-02-09 | Panasonic Electric Works Co Ltd | Halogen-free epoxy resin composition, coverlay film, bonding sheet, prepreg and laminate for printed wiring board |
| CN104610704A (en) * | 2015-01-28 | 2015-05-13 | 清远市普塞呋磷化学有限公司 | Halogen-free flame retardant anhydride cured epoxy resin composition |
-
2016
- 2016-11-26 CN CN201611057429.XA patent/CN106751475B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1847352A (en) * | 2005-04-13 | 2006-10-18 | 信越化学工业株式会社 | Flame retardant adhesive composition, and adhesive sheet, coverlay film and flexible copper-clad laminate using same |
| JP2012025917A (en) * | 2010-07-27 | 2012-02-09 | Panasonic Electric Works Co Ltd | Halogen-free epoxy resin composition, coverlay film, bonding sheet, prepreg and laminate for printed wiring board |
| CN102241872A (en) * | 2011-06-28 | 2011-11-16 | 江汉大学 | Aluminum methylcyclohexyl phosphinate/epoxy resin flame-retardant composite material |
| CN104610704A (en) * | 2015-01-28 | 2015-05-13 | 清远市普塞呋磷化学有限公司 | Halogen-free flame retardant anhydride cured epoxy resin composition |
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Address after: 265400 No.268, Guoda Road, Zhaoyuan City, Yantai City, Shandong Province Patentee after: Shandong Jinbao Electronics Co.,Ltd. Address before: 265400 No. 128, Wenquan Road, Zhaoyuan, Shandong, Yantai Patentee before: SHANDONG JINBAO ELECTRONICS Co.,Ltd. |
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