CN108641653A - A method of preparing epoxy resin-matrix high heat conductive insulating composite glue solution with modified nitridation aluminum-boron nitride-nitrile rubber - Google Patents
A method of preparing epoxy resin-matrix high heat conductive insulating composite glue solution with modified nitridation aluminum-boron nitride-nitrile rubber Download PDFInfo
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- CN108641653A CN108641653A CN201810487020.4A CN201810487020A CN108641653A CN 108641653 A CN108641653 A CN 108641653A CN 201810487020 A CN201810487020 A CN 201810487020A CN 108641653 A CN108641653 A CN 108641653A
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- epoxy resin
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- boron nitride
- high heat
- nitrile rubber
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of methods preparing epoxy resin-matrix high heat conductive insulating composite glue solution with modified aluminium nitride boron nitride nitrile rubber, it is characterized in that, by deionized water NaOH tune pH, Cetyltrimethylammonium bromide and boron nitride is added, condensing reflux stirs, heating reaction filters, washing, is dried in vacuo to obtain organic modification of surface boron nitride powder；Filler grain aluminium nitride is heated in vacuum drying chamber, is then added in silane coupling agent hydrolyzate, is stirred in water bath with thermostatic control, is filtered, air blast in drying box is put into and dries, be ground up, sieved；Nitrile rubber mixing is added into epoxy resin to stir evenly, heating stirring obtains toughening-modifiedepoxy resin, vacuumizing and defoaming, front gained modified filler is added, stirs evenly, instills antifoaming agent, high-speed stirred, curing agent is added, vacuum defoamation keeps the temperature glue in vacuum drying chamber, it is in thick to carry out precuring to glue, obtains epoxy resin-matrix high heat conductive insulating composite glue solution.
Description
Technical field
The present invention relates to resin arts, and in particular to a kind of to prepare asphalt mixtures modified by epoxy resin with modified nitridation aluminum-boron nitride-nitrile rubber
The method of aliphatic radical high heat conductive insulating composite glue solution.
Background technology
As basis material, epoxy resin has good biodegradability, and density is low, usage time is long, excellent
It the advantages that electrochemistry and mechanical property, plays an important role in the composite.They be widely used in aerospace,
The fields such as military affairs.But epoxy resin limit oxygen index is very low, easily burns, sustained combustion and smoke amount is big after catching fire.Closely
A little years reduce fire hazard to improve the fire-retardant performance of composite material, and fire retarding epoxide resin is more and more concerned especially to navigate
There is an urgent need to non-toxic, environmental friendly fire proofings in the fields such as sky, space flight, military affairs.
Epoxy resin has many advantages, such as that adhesive property is good, easy processing molding, is widely used in electronic apparatus, aerospace etc.
In technology, but it is combustible material, once being ignited, the mechanical property of composite material will be caused to reduce rapidly, therefore to ring
The technical barrier in flame-retardant modified always this field of oxygen resin.Carbon fiber because of it with high intensity, proportion is small, thermally expands system
The performances such as small are counted, one of main reinforcement fibres of advanced composite material are become.Carbon nanotube has because of its unique structure
A kind of good thermal conductivity, it is considered to be ideal flame-retardant additive.
Invention content
The invention mainly solves the technical problem of providing a kind of ring is prepared with modified nitridation aluminum-boron nitride-nitrile rubber
The method of epoxy resin-based high heat conductive insulating composite glue solution has excellent according to epoxy resin-matrix composite glue solution prepared by the technique
High heat conductive insulating performance.
A kind of side preparing epoxy resin-matrix high heat conductive insulating composite glue solution with modified nitridation aluminum-boron nitride-nitrile rubber
Method, which is characterized in that carry out according to the following steps：
（1）The preparation of organic modification of surface boron nitride powder：
With NaOH tune pH it is 8.5-9.5 by 200-300 parts of deionized waters, Cetyltrimethylammonium bromide and 20-30 parts is added
Boron nitride, condensing reflux stirring, reacts 4-5h at 80-83 DEG C, filters, washes 2-3 times, and 20- is dried in vacuo in 80-83 DEG C
For 24 hours, organic modification of surface boron nitride powder is obtained；
（2）The drying process of filler and surface are modified：
20-30 parts of filler grain aluminium nitride are heated into 1-2h in 120-123 DEG C of vacuum drying chamber, are then added to silane coupled
In agent hydrolyzate, 2-3h is stirred in 70-72 DEG C of water bath with thermostatic control, is filtered, and is put into air blast in drying box and is dried, 200 mesh are crossed in grinding
Sieve；
（3）The preparation of high heat conductive insulating composite glue solution：
14-16 parts of nitrile rubber mixing are added into 95-105 parts of epoxy resin, stirs evenly, heats and stir at 140-142 DEG C
2-3h is mixed, toughening-modifiedepoxy resin is obtained, gained modified filler in (1), (2), stirring is added in vacuumizing and defoaming 2-3 times
Uniformly, antifoaming agent is instilled, 5-6 parts of curing agent are added in high-speed stirred 2-3h, and glue is dried in vacuo by vacuum defoamation at 40-42 DEG C
15-20min is kept the temperature in case, it is in thick to carry out precuring to glue, obtains epoxy resin-matrix high heat conductive insulating composite glue solution.
Wherein, step（1）Middle NaOH concentration is 0.1-0.2mol/L, a concentration of 0.5- of Cetyltrimethylammonium bromide
0.6g/L。
Step（2）It is middle that Silane coupling agent KH550 is dissolved in absolute ethyl alcohol, it is even to be made into the silane that mass concentration is 1-2%
Join agent hydrolyzate.
The reaction mechanism of the present invention is as follows：
Organic modification, nitridation are carried out to boron nitride micron film using cationic surfactant Cetyltrimethylammonium bromide
Boron surface modification improves wellability of the epoxy resin to boron nitride, and nitridation boron surface improves itself and epoxy resin-matrix
Interface performance and Miscibility, the composite glue solution thermal coefficient prepared with modified boron nitride are high；Pass through Silane coupling agent KH550
Filler aluminium nitride is surface-treated, the binder course of inorganic phase-silane coupling agent-organic phase can be formed, improves polymer
With the adhesive strength between inorganic material interface；Using epoxy resin as matrix, nitrile rubber carries out toughening modifying to matrix, can be improved
Matrix and intergranular wetability and the workability of glue, prepare the compound inslation glue of high heat conduction.
Specific implementation mode
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention be easy to understand, tie below
Specific embodiment is closed, the present invention is further explained.
Embodiment
A kind of side preparing epoxy resin-matrix high heat conductive insulating composite glue solution with modified nitridation aluminum-boron nitride-nitrile rubber
Method, which is characterized in that carry out according to the following steps：
（1）The preparation of organic modification of surface boron nitride powder：
With NaOH tune pH it is 8.5-9.5 by 200kg deionized waters, Cetyltrimethylammonium bromide and 20kg boron nitride is added,
Condensing reflux stirs, and 4h is reacted at 80-83 DEG C, filters, washes 2 times, is dried in vacuo 20h in 80-83 DEG C, obtains surface organic
Modified boron nitride powder；
（2）The drying process of filler and surface are modified：
20kg filler grain aluminium nitride is heated into 1h in 120-123 DEG C of vacuum drying chamber, is then added to silane coupling agent water
It solves in liquid, 2h is stirred in 70-72 DEG C of water bath with thermostatic control, filter, be put into air blast in drying box and dry, 200 mesh sieve is crossed in grinding；
（3）The preparation of high heat conductive insulating composite glue solution：
The mixing of 14kg nitrile rubbers is added into 95kg epoxy resin, stirs evenly, heating stirring 2h, obtains at 140-142 DEG C
To toughening-modifiedepoxy resin, vacuumizing and defoaming 2 times is added gained modified filler in (1), (2), stirs evenly, instillation disappears
5kg curing agent is added in infusion, high-speed stirred 2h, and glue is kept the temperature 20min by vacuum defoamation in 40-42 DEG C of vacuum drying chamber,
It is in thick to carry out precuring to glue, obtains epoxy resin-matrix high heat conductive insulating composite glue solution.
Wherein, step（1）Middle NaOH concentration is 0.1mol/L, a concentration of 0.5g/L of Cetyltrimethylammonium bromide.
Step（2）It is middle that Silane coupling agent KH550 is dissolved in absolute ethyl alcohol, be made into mass concentration be 1% it is silane coupled
Agent hydrolyzate.
Claims (4)
1. a kind of method preparing epoxy resin-matrix high heat conductive insulating composite glue solution with modified nitridation aluminum-boron nitride-nitrile rubber,
It is characterized in that, by deionized water NaOH tune pH, Cetyltrimethylammonium bromide is added and boron nitride, condensing reflux stir
It mixes, heating reaction filters, washing, is dried in vacuo to obtain organic modification of surface boron nitride powder；By filler grain aluminium nitride true
It is heated in empty drying box, is then added in silane coupling agent hydrolyzate, is stirred in water bath with thermostatic control, filtered, be put into drying box
Middle air blast drying, is ground up, sieved；Nitrile rubber mixing is added into epoxy resin, stirs evenly, heating stirring obtains toughening
Modified epoxy resin, vacuumizing and defoaming are added front gained modified filler, stir evenly, instillation antifoaming agent, high-speed stirred,
Curing agent is added, vacuum defoamation keeps the temperature glue in vacuum drying chamber, and it is in thick to carry out precuring to glue, obtains ring
Epoxy resin-based high heat conductive insulating composite glue solution.
2. a kind of epoxy resin-matrix high heat conduction is prepared according to claim 1 with modified nitridation aluminum-boron nitride-nitrile rubber
The method of insulated compound glue, which is characterized in that carry out according to the following steps：
（1）The preparation of organic modification of surface boron nitride powder：
With NaOH tune pH it is 8.5-9.5 by 200-300 parts of deionized waters, Cetyltrimethylammonium bromide and 20-30 parts is added
Boron nitride, condensing reflux stirring, reacts 4-5h at 80-83 DEG C, filters, washes 2-3 times, and 20- is dried in vacuo in 80-83 DEG C
For 24 hours, organic modification of surface boron nitride powder is obtained；
（2）The drying process of filler and surface are modified：
20-30 parts of filler grain aluminium nitride are heated into 1-2h in 120-123 DEG C of vacuum drying chamber, are then added to silane coupled
In agent hydrolyzate, 2-3h is stirred in 70-72 DEG C of water bath with thermostatic control, is filtered, and is put into air blast in drying box and is dried, 200 mesh are crossed in grinding
Sieve；
（3）The preparation of high heat conductive insulating composite glue solution：
14-16 parts of nitrile rubber mixing are added into 95-105 parts of epoxy resin, stirs evenly, heats and stir at 140-142 DEG C
2-3h is mixed, toughening-modifiedepoxy resin is obtained, gained modified filler in (1), (2), stirring is added in vacuumizing and defoaming 2-3 times
Uniformly, antifoaming agent is instilled, 5-6 parts of curing agent are added in high-speed stirred 2-3h, and glue is dried in vacuo by vacuum defoamation at 40-42 DEG C
15-20min is kept the temperature in case, it is in thick to carry out precuring to glue, obtains epoxy resin-matrix high heat conductive insulating composite glue solution.
3. a kind of epoxy resin-matrix high heat conduction is prepared according to claim 2 with modified nitridation aluminum-boron nitride-nitrile rubber
The method of insulated compound glue, which is characterized in that step（1）Middle NaOH concentration is 0.1-0.2mol/L, octadecyl trimethyl
A concentration of 0.5-0.6g/L of ammonium bromide.
4. a kind of epoxy resin-matrix high heat conduction is prepared according to claim 2 with modified nitridation aluminum-boron nitride-nitrile rubber
The method of insulated compound glue, which is characterized in that step（2）It is middle that Silane coupling agent KH550 is dissolved in absolute ethyl alcohol, it is made into
Mass concentration is the silane coupling agent hydrolyzate of 1-2%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810487020.4A CN108641653A (en) | 2018-05-21 | 2018-05-21 | A method of preparing epoxy resin-matrix high heat conductive insulating composite glue solution with modified nitridation aluminum-boron nitride-nitrile rubber |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810487020.4A CN108641653A (en) | 2018-05-21 | 2018-05-21 | A method of preparing epoxy resin-matrix high heat conductive insulating composite glue solution with modified nitridation aluminum-boron nitride-nitrile rubber |
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| Publication Number | Publication Date |
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| CN108641653A true CN108641653A (en) | 2018-10-12 |
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| CN201810487020.4A Withdrawn CN108641653A (en) | 2018-05-21 | 2018-05-21 | A method of preparing epoxy resin-matrix high heat conductive insulating composite glue solution with modified nitridation aluminum-boron nitride-nitrile rubber |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113136158A (en) * | 2021-04-22 | 2021-07-20 | 深圳市图特美高分子材料有限公司 | Solvent-free environment-friendly flame-retardant adhesive film and preparation method thereof |
| CN116477585A (en) * | 2023-03-10 | 2023-07-25 | 四川大学 | Method for improving water resistance of aluminum nitride powder |
-
2018
- 2018-05-21 CN CN201810487020.4A patent/CN108641653A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113136158A (en) * | 2021-04-22 | 2021-07-20 | 深圳市图特美高分子材料有限公司 | Solvent-free environment-friendly flame-retardant adhesive film and preparation method thereof |
| CN116477585A (en) * | 2023-03-10 | 2023-07-25 | 四川大学 | Method for improving water resistance of aluminum nitride powder |
| CN116477585B (en) * | 2023-03-10 | 2024-02-23 | 四川大学 | Method for improving water resistance of aluminum nitride powder |
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Application publication date: 20181012 |