CN107177162A - A kind of conductive phenol formaldehyde resin of copper powder hollow glass microballoon blending and modifying and preparation method thereof - Google Patents
A kind of conductive phenol formaldehyde resin of copper powder hollow glass microballoon blending and modifying and preparation method thereof Download PDFInfo
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- CN107177162A CN107177162A CN201710451443.6A CN201710451443A CN107177162A CN 107177162 A CN107177162 A CN 107177162A CN 201710451443 A CN201710451443 A CN 201710451443A CN 107177162 A CN107177162 A CN 107177162A
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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
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/10—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with phenol
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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
- C08K3/02—Elements
- C08K3/04—Carbon
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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
- C08K3/02—Elements
- C08K3/08—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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
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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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/28—Glass
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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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
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
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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
- C08K3/28—Nitrogen-containing compounds
- C08K2003/282—Binary compounds of nitrogen with aluminium
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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
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
Abstract
The invention discloses a kind of preparation method of the conductive phenol formaldehyde resin of copper powder hollow glass microballoon blending and modifying, it is characterised in that KH550 is dissolved in ethanol solution, and the filler added after drying, heating water bath magnetic agitation obtains surface treatment heat-conductive insulation filling；KH550 is added into graphene oxide, is placed in ice-water bath, ultrasound is peeled off, and is uniformly dispersed, catalyst is added, magnetic agitation is reacted under oil bath；It is then dispersed in acetone, sonic oscillation, adds attapulgite, continues ultrasonically treated, evaporate solvent acetone, obtain composite reinforcement；Sodium hydroxide solution is hydrogenated with into hollow glass microballoon, immersion treatment, plus absolute ethyl alcohol, KH550, stirring is stirred；Copper powder and phenol, formalin are added in reactor, heating water bath adds above resulting material, is stirred by rotating magneton, constant temperature backflow polymerization is cooled to room temperature, depressurizes suction filtration, elevated cure shaping.
Description
Technical field
The present invention relates to art of printed circuit boards, and in particular to a kind of conduction of copper powder-hollow glass microballoon blending and modifying
The preparation method of phenolic resin.
Background technology
With developing rapidly for electronic information technology, electronic circuit it is also proposed with the performance of printed circuit board (PCB) (PCB)
Higher requirement.The electronic equipment that volume is frivolous and power consumption is larger is just perplexed from birth by heating problem, and PCB is as each
The bridge and carrier of heater members, be always strengthen equipment cooling research emphasis, the excellent baseplate material of heat conductivility and
The even heat distribution that the PCB of good radiating structure can produce heater members, strengthens radiating efficiency, reduces expensive device
Fire damage.
The content of the invention
The present invention solves the technical problem of provide a kind of conductive phenolic aldehyde of copper powder-hollow glass microballoon blending and modifying
The preparation method of resin, the phenolic resin prepared according to the technique has good electric conductivity, thermal conductivity and fracture toughness.
The technical problems to be solved by the invention are realized using following technical scheme：
The preparation method of the conductive phenol formaldehyde resin of a kind of copper powder-hollow glass microballoon blending and modifying, it is characterised in that by following step
It is rapid to carry out：
A. the surface treatment of filler：
4-7 parts by weight aluminium nitride, 3-6 parts by weight silicon powder fillers are placed in 150-160 DEG C of baking oven and dry 2-3h, by 1-2 weights
Measure part KH550 1:5-10 is dissolved in ethanol solution, the filler added after drying, the magnetic agitation 1-2h under 70-80 DEG C of water-bath,
Stand cooling, filtering, 85-95 DEG C of drying is complete, grind；
B. the partial reduction and modification of graphene oxide：
0.1-0.2 parts by weight KH550 are added into 2-4 parts by weight graphene oxides, is placed in ice-water bath, uses supersonic cell powder
Broken machine ultrasound peels off 1-2h, is uniformly dispersed, adds 0.5-1 part by weight of catalyst, under 70-80 DEG C of oil bath, magnetic agitation reaction
5-6h, filtering, alcohol are washed 3-5 times, are placed in 80-90 DEG C of convection oven and are dried complete, mechanical lapping crushing；
Then 1:5-10 is scattered in acetone, sonic oscillation 1-2h, adds 3-5 parts by weight attapulgites, continues ultrasonically treated 1-
2h, mixed liquor is placed in open-top receptacle in 70-80 DEG C of lasting stirring, solvent acetone is evaporated, composite reinforcement is made；
C. the surface treatment of hollow glass microballoon：
Into 2-4 parts by weight hollow glass microballoons 1:5-10 adds sodium hydroxide solution, stirs immersion treatment 4-6h, suction filtration, water
Neutrality is washed till, after 90-100 DEG C is fully dried, 1:3-5 adds absolute ethyl alcohol, adds 0.1-0.2 parts by weight silane couplers
KH550, stirs 3-4h, filtering, 80-90 DEG C of drying are completely；
D. the preparation of conductive phenol formaldehyde resin：
3-5 parts by weight copper powder and 10-15 parts by weight of phenol, 40-60 parts by weight of formaldehyde solution are added in reactor, hydroxide is used
Sodium solution adjusts pH to be 13-14, is reacted in 70-80 DEG C of water-bath, resulting material in a, b, c is added, by rotating magneton
Be stirred, heated at constant temperature backflow polymerization 4-5h is cooled to room temperature, depressurizes suction filtration, be warming up to 140-150 DEG C of solidification 2-3h into
Type.
Wherein, the concentration of ethanol solution described in step a is 90-95%.Catalyst described in step b is N, N,- two hexamethylenes
Base carbodiimide.The mass fraction of sodium hydroxide solution described in step c is 10-15%.Sodium hydroxide solution described in step d
Mass fraction be 30-35%, formalin concentration be 40-45%.
The present invention reaction mechanism and have the beneficial effect that：
Hollow glass microballoon is surface-treated with Silane coupling agent KH550, improves its compatibility with matrix, it is modified with
Aluminium nitride, silicon powder filler hydridization filled phenolic resin, collaboration improve the thermal conductivity of composite；With KH550 to graphite oxide
Alkene carries out partial reduction and functional modification, obtains modified graphene, the amino of coupling agent and the epoxy of surface of graphene oxide
Group there occurs nucleophilic substitution；Again by solwution method, attapulgite particle is set to be adsorbed in the way of Hydrogenbond in oxidation
Graphene film layer surface, obtains composite reinforcement, improves the mechanical property, fracture toughness and heat endurance of composite；With
Copper powder, formalin, phenol are raw material, and blending is prepared for conductive phenol formaldehyde resin.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment
A kind of preparation method of the conductive phenol formaldehyde resin of copper powder-hollow glass microballoon blending and modifying, it is characterised in that by with
Lower step is carried out：
A. the surface treatment of filler：
4kg aluminium nitride, 3kg silicon powder fillers are placed in 150-160 DEG C of baking oven and dry 2h, by 1kg KH550 1:10 are dissolved in second
In alcoholic solution, the filler added after drying, the magnetic agitation 1h under 70-80 DEG C of water-bath stands cooling, filtering, 85-95 DEG C of drying
Completely, grind；
B. the partial reduction and modification of graphene oxide：
0.1kg KH550 are added into 2kg graphene oxides, are placed in ice-water bath, are peeled off with ultrasonic cell disruptor ultrasound
1h, is uniformly dispersed, and adds 0.5kg catalyst, under 70-80 DEG C of oil bath, magnetic agitation reaction 5h, and filtering, alcohol are washed 3 times, is placed in
Complete, mechanical lapping is dried in 80-90 DEG C of convection oven to crush；
Then 1:10 are scattered in acetone, sonic oscillation 1h, add 3kg attapulgites, continue ultrasonically treated 1h, mixed liquor is put
In 70-80 DEG C of lasting stirring in open-top receptacle, solvent acetone is evaporated, composite reinforcement is made.
C. the surface treatment of hollow glass microballoon：
Into 4kg hollow glass microballoons 1:10 add sodium hydroxide solutions, stir immersion treatment 4h, suction filtration, are washed to neutrality,
After 90-100 DEG C is fully dried, 1:5 add absolute ethyl alcohol, add 0.1kg Silane coupling agent KH550s, stir 3h, filtering, 80-90
DEG C dry complete；
D. the preparation of conductive phenol formaldehyde resin：
5kg copper powders and 15kg phenol, 60kg formalins are added in reactor, adjust pH to be 13-14 with sodium hydroxide solution,
Reacted in 70-80 DEG C of water-bath, add resulting material in a, b, c, be stirred by rotating magneton, heated at constant temperature backflow
It polymerize 4h, is cooled to room temperature, depressurize suction filtration, is warming up to 140-150 DEG C of solidification 2h shaping.
Wherein, the concentration of ethanol solution described in step a is 90%.Catalyst described in step b is N, N,- dicyclohexyl
Carbodiimide.The mass fraction of sodium hydroxide solution described in step c is 15%.The quality of sodium hydroxide solution described in step d
Fraction is 35%, and formalin concentration is 40%.
Claims (6)
1. a kind of conductive phenol formaldehyde resin of copper powder-hollow glass microballoon blending and modifying, it is characterised in that：
KH550 is dissolved in ethanol solution, the filler added after drying, heating water bath magnetic agitation must be surface-treated heat conduction exhausted
Edge filler；KH550 is added into graphene oxide, is placed in ice-water bath, ultrasound is peeled off, and is uniformly dispersed, catalyst is added, in oil
The lower magnetic agitation reaction of bath；It is then dispersed in acetone, sonic oscillation, adds attapulgite, continues ultrasonically treated, evaporate molten
Agent acetone, obtains composite reinforcement；It is hydrogenated with sodium hydroxide solution into hollow glass microballoon, stirs immersion treatment, plus absolute ethyl alcohol,
KH550, stirring；Copper powder and phenol, formalin are added in reactor, heating water bath adds above resulting material, passes through rotation
Turn magneton to be stirred, constant temperature backflow polymerization is cooled to room temperature, depressurizes suction filtration, elevated cure shaping.
2. a kind of preparation method of the conductive phenol formaldehyde resin of copper powder-hollow glass microballoon blending and modifying, it is characterised in that：
A. the surface treatment of filler：
4-7 parts by weight aluminium nitride, 3-6 parts by weight silicon powder fillers are placed in 150-160 DEG C of baking oven and dry 2-3h, by 1-2 weights
Measure part KH550 1:5-10 is dissolved in ethanol solution, the filler added after drying, the magnetic agitation 1-2h under 70-80 DEG C of water-bath,
Stand cooling, filtering, 85-95 DEG C of drying is complete, grind；
B. the partial reduction and modification of graphene oxide：
0.1-0.2 parts by weight KH550 are added into 2-4 parts by weight graphene oxides, is placed in ice-water bath, uses supersonic cell powder
Broken machine ultrasound peels off 1-2h, is uniformly dispersed, adds 0.5-1 part by weight of catalyst, under 70-80 DEG C of oil bath, magnetic agitation reaction
5-6h, filtering, alcohol are washed 3-5 times, are placed in 80-90 DEG C of convection oven and are dried complete, mechanical lapping crushing；
Then 1:5-10 is scattered in acetone, sonic oscillation 1-2h, adds 3-5 parts by weight attapulgites, continues ultrasonically treated 1-
2h, mixed liquor is placed in open-top receptacle in 70-80 DEG C of lasting stirring, solvent acetone is evaporated, composite reinforcement is made；
C. the surface treatment of hollow glass microballoon：
Into 2-4 parts by weight hollow glass microballoons 1:5-10 adds sodium hydroxide solution, stirs immersion treatment 4-6h, suction filtration, water
Neutrality is washed till, after 90-100 DEG C is fully dried, 1:3-5 adds absolute ethyl alcohol, adds 0.1-0.2 parts by weight silane couplers
KH550, stirs 3-4h, filtering, 80-90 DEG C of drying are completely；
D. the preparation of conductive phenol formaldehyde resin：
3-5 parts by weight copper powder and 10-15 parts by weight of phenol, 40-60 parts by weight of formaldehyde solution are added in reactor, hydroxide is used
Sodium solution adjusts pH to be 13-14, is reacted in 70-80 DEG C of water-bath, resulting material in a, b, c is added, by rotating magneton
Be stirred, heated at constant temperature backflow polymerization 4-5h is cooled to room temperature, depressurizes suction filtration, be warming up to 140-150 DEG C of solidification 2-3h into
Type.
3. a kind of preparation side of the conductive phenol formaldehyde resin of copper powder-hollow glass microballoon blending and modifying according to claim 2
Method, it is characterised in that the concentration of ethanol solution described in step a is 90-95%.
4. a kind of preparation side of the conductive phenol formaldehyde resin of copper powder-hollow glass microballoon blending and modifying according to claim 2
Method, it is characterised in that catalyst described in step b is N, N,- dicyclohexylcarbodiimide.
5. a kind of preparation side of the conductive phenol formaldehyde resin of copper powder-hollow glass microballoon blending and modifying according to claim 2
Method, it is characterised in that the mass fraction of sodium hydroxide solution described in step c is 10-15%.
6. a kind of preparation side of the conductive phenol formaldehyde resin of copper powder-hollow glass microballoon blending and modifying according to claim 2
Method, it is characterised in that the mass fraction of sodium hydroxide solution described in step d is 35-40%, formalin concentration is 40-45%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710451443.6A CN107177162A (en) | 2017-06-15 | 2017-06-15 | A kind of conductive phenol formaldehyde resin of copper powder hollow glass microballoon blending and modifying and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710451443.6A CN107177162A (en) | 2017-06-15 | 2017-06-15 | A kind of conductive phenol formaldehyde resin of copper powder hollow glass microballoon blending and modifying and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114649123A (en) * | 2022-04-11 | 2022-06-21 | 贝迪斯电子有限公司 | Manufacturing method of high-temperature-resistant flame-retardant precise metal film resistor |
| CN116948408A (en) * | 2023-08-24 | 2023-10-27 | 广州市文逸通讯设备有限公司 | Wear-resistant heat-dissipation mobile phone protective shell material and preparation process thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114649123A (en) * | 2022-04-11 | 2022-06-21 | 贝迪斯电子有限公司 | Manufacturing method of high-temperature-resistant flame-retardant precise metal film resistor |
| CN116948408A (en) * | 2023-08-24 | 2023-10-27 | 广州市文逸通讯设备有限公司 | Wear-resistant heat-dissipation mobile phone protective shell material and preparation process thereof |
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Application publication date: 20170919 |