CN109384967A - A kind of high thermal conductivity boron nitride/native rubber composite material and preparation method thereof - Google Patents
A kind of high thermal conductivity boron nitride/native rubber composite material and preparation method thereof Download PDFInfo
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- CN109384967A CN109384967A CN201811248742.0A CN201811248742A CN109384967A CN 109384967 A CN109384967 A CN 109384967A CN 201811248742 A CN201811248742 A CN 201811248742A CN 109384967 A CN109384967 A CN 109384967A
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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
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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
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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
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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
- 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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- 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
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Abstract
The invention discloses a kind of high thermal conductivity boron nitride/native rubber composite materials and preparation method thereof, the composite material includes natural rubber matrix, vulcanizing agent and modified boron nitride nanosheet, wherein the modification to boron nitride nanosheet are as follows: form poly- (catechol/polyamines) (PCPA) layer in the auto polymerization of boron nitride nanosheet surface using catechol and polyamines.Then nanometer sheet surface second functionalization is realized using the functional group reactions on the catechol base, amino and silane coupling agent on the surface PCPA, form modified boron nitride nanosheet.Above-mentioned modified boron nitride nanosheet is added in natural rubber matrix, the rubber composite material for having both high thermal conductivity coefficient and excellent mechanical properties is prepared into.The method of the present invention is high-efficient, at low cost, reaction condition is mild, easy to operate, effectively increases the heating conduction and mechanical performance of natural rubber, can be widely applied to Electronic Packaging field.
Description
Technical field
The invention belongs to technical field of polymer, and in particular to a kind of high thermal conductivity boron nitride/native rubber composite material and
Preparation method.
Background technique
With the fast development of the high-tech areas such as Aeronautics and Astronautics, electric, health care, rubber part is made
Higher and higher with service life and thermal stability requirement, the heating conduction of rubber is increasingly taken seriously.In numerous rubber matrix materials
In material, natural rubber is because having good insulating properties, air-tightness and biggish tensile strength and elongation at break, and source
The extensively extensive concern by researchers.But natural rubber is the non-conductor of heat, therefore is frequently necessary to lead using filling
The method of hot filler is prepared into heat-conductive composite material, to improve the heating conduction of rubber.Usually used heat filling is inorganic
Filler, but it can differ larger with the surface of organic natural rubber, interfacial combined function between the two is poor, leads to inorganic lead
Hot filler is easy to reunite in natural rubber matrix, and interface resistance increases, and the heating conduction of composite material improves not significant.It is multiple simultaneously
Poor interfacial combined function makes the mechanical properties decrease of composite material significant in condensation material, so that heat-conductivity rubber composite material
Actual use critical constraints.Therefore, it is necessary to be modified to inorganic heat filling surface, to improve it in rubber matrix
Dispersion performance and interfacial combined function, to effectively improve the heating conduction and mechanical performance of composite material.
A kind of Chinese patent application " preparation method of vertical orientation boron nitride/high polymer insulating heat-conduction material " (patent Shen
Number 201611218918.9) nitrogen that surface modification is prepared using dopamine auto polymerization and silane coupler modified method please be proposed
Change boron nanometer sheet, then the boron nitride nanosheet of this surface modification is coated among two layers of polymers, utilizes hot-pressing technique
Above-mentioned trilaminate material is pressed into certain thickness thermally conductive film.Pellicular cascade at block or is finally wound into a circle
Cylinder.Thermal conductivity in prepared insulating heat-conductive composite material face with higher, but composite material preparation process is complicated, step
It is rapid cumbersome, while the price of dopamine is more expensive, limits its extensive application industrially.Chinese patent application is " a kind of
Novel graphene modification heat conductive rubber " (number of patent application 201710831380.7) proposes a kind of side of new modified graphene
Method.Graphene oxide is obtained using Hummers method first, then disperses graphene oxide in silver ammino solution, adds grape
Sugar restores anion, obtains modified graphene-silver nano particle composite material, is added in rubber matrix, shows
The thermal coefficient for having landed rubber composite material high.But the preparation condition of rubber composite material is harsh, preparation process is complicated, breaks
It splits elongation and is remarkably decreased (< 10%).
Summary of the invention
It is an object of the present invention to provide a kind of high thermal conductivity boron nitride/native rubber composite materials and preparation method thereof.
The present invention provides a kind of method of modifying of boron nitride nanosheet, and modified boron nitride nanosheet is added to naturally
In rubber matrix, high thermal conductivity boron nitride/native rubber composite material is prepared.Using catechol and polyamines in boron nitride nanometer
The auto polymerization of piece surface forms poly- (catechol/polyamines) (PCPA) layer.Then using the catechol base on the surface PCPA, amino and
Functional group reactions on silane coupling agent realize its surface second functionalization, form the boron nitride nanosheet of surface modification.By institute
The modification boron nitride nanosheet of preparation is filled into natural rubber matrix, its dispersibility in rubber matrix can be significantly improved
Can, to significantly improve the heating conduction and mechanical performance of rubber composite material.This method is easy to operate, economic and environment-friendly, efficiently
When section, prepared product can be applied to dielectric electronic package field.
The specific technical solution of the present invention is a kind of high thermal conductivity boron nitride/native rubber composite material, which is characterized in that
Including natural rubber matrix, vulcanizing agent and boron nitride nanosheet.Wherein:
Natural rubber matrix: 100 mass parts
Vulcanizing agent: 2-8 mass parts
Modified boron nitride nanosheet: 10-200 mass parts
Further, vulcanizing agent used is traditional sulphur system, including sulphur, zinc oxide and stearic acid.
Further, the catechol and polyamines that modified boron nitride nanosheet is low cost are in boron nitride nanosheet surface autohemagglutination
Conjunction forms poly- (catechol/polyamines) (PCPA) layer.Then catechol base, amino and the silane coupling agent on the surface PCPA are utilized
On functional group reactions realize its surface second functionalization, form the boron nitride nanosheet of surface modification.The polyamine compounds
For one of ethylenediamine, five amine of tetrem diyl, penta tetramine of season and three second tetramines or a variety of；The silane coupling agent be KH560,
KH570's or Si69 is one or more.
Further, the modified boron nitride heat filling preparation method the following steps are included:
1) appropriate trishydroxymethylaminomethane is added in 100ml deionized water, adjusting pH value is 7-10, is prepared into molten
Liquid 1.
2) by quality be 1-2g catechol and quality be 0.5-1g polyamines be added in solution 1, be prepared into solution
2。
3) boron nitride nanosheet that quality is 50-200g is added slowly in solution 2, while prepared mixing is molten
Liquid is placed in constant temperature blender with magnetic force, sets bath temperature as 30-40 DEG C, sets mixing speed as 400-500r/min, permanent
Temperature reaction 6-10h, is prepared into solution 3.
4) temperature of solution 3 is increased to 50-70 DEG C, then adds the silane coupled of mass fraction 1%-15% thereto
Agent, isothermal reaction 6-8h are prepared into solution 4.
5) solution 4 is filtered, is washed with deionized 3-5 times, in drying in oven, obtain modified boron nitride nanometer
Piece.
Further, the modified boron nitride nanosheet uniform particle sizes, size 100-800nm, boron nitride nanosheet is through repairing
Adorn the unformed layer of rear surface deposition 2-6nm.
Further, the preparation method of the composite material is modified boron nitride nanosheet and natural rubber in two-roll mill
On be kneaded, melting temperature be 25-40 DEG C, be kneaded uniformly after place 7-24h, vulcanized using process control tablet press machine,
Controlling Tooling Fabrication Area temperature is 120-160 DEG C, and the tabletting time is 0.5-2h, and pressure 15-25MPa obtains the natural of high thermal conductivity coefficient
Rubber composite material.Above-mentioned obtained high thermal conductivity boron nitride/native rubber composite material thermal coefficient is 0.39-1.21W/
MK, dielectric constant 3.09-3.81, elasticity modulus 1.58-9.47MPa, elongation at break 467-629%.
Advantageous effect of the invention are as follows: the preparation method of high thermal conductivity boron nitride/native rubber composite material provided by the invention,
It selects PCPA method of modifying relative to poly-dopamine modified lithium method, there is higher efficiency and more inexpensive advantage.PCPA simultaneously
Chemical bonds between the silane coupling agent of surface grafting can provide between inorganic heat filling and rubber molecule, so that composite material
Dispersion performance be improved significantly, so that the heating conduction of composite material and mechanical property are significantly improved, and keep compared with
Low dielectric constant.
Specific embodiment
Below by embodiment, the present invention is further described, but not as limiting the scope of the invention.
Embodiment 1
(1) 2.8g catechol and 1.6g tetra- (second diyl) five amine are added in 100ml deionized water, using three hydroxyl first
Base aminomethane solid (Tris) adjust aqueous solution to PH be 8 after, addition 50g boron nitride, under room temperature, with 400r/min's
Stirring rate is stirred to react 6h.
(2) bath temperature is increased to 70 DEG C, and 0.5g silane coupling agent KH560 is added, is stirred with the mixing speed of 400r/min
5h is mixed, reaction is washed with deionized to neutrality after stopping, and is filtered, vacuum drying obtains modified boron nitride nanosheet.
(3) by the natural rubber of 100 mass parts, room temperature modeling is practiced on a mill, and it is modified that 50 mass parts are made in step (2)
Boron nitride nanosheet is added gradually in natural rubber, is then gradually added into 3 mass parts sulphur, and cutter is kneaded, beats triangle bag, make
Mixing it is uniform.
(4) it is kneaded after parking for 24 hours, pressure 15MPa is set on vulcanizing press, vulcanizes 60min at 150 DEG C, is obtained
High thermal conductivity boron nitride/native rubber composite material.
(5) heating conduction and Mechanics Performance Testing, test are carried out to obtained modification boron nitride/native rubber composite material
It the results are shown in Table one.Using the DXF-500 model conductometer test material thermal coefficient of TA company, the U.S., rubber composite material is obtained
Thermal coefficient be shown in Table one.At room temperature with German Novochtrol Alpha-A impedance instrument test composite material, under 1kHz
Dielectric constant is shown in Table one.According to national standard GB/T 528-2009, using the microcomputer controlled electronic of model U.S. Instron 3366
The stress-strain diagram of universal testing machine sample, obtains elongation at break and tensile strength, and test result is shown in Table one.
Embodiment 2
The preparation method is the same as that of Example 1, the difference is that the amount of modified boron nitride nanosheet is 200 mass parts, test result is shown in
Table one.
Embodiment 3
The preparation method is the same as that of Example 1, the difference is that four (second diyl) five amine in modifying agent are changed to penta tetramine of season, tests
It the results are shown in Table one.
Embodiment 4
Preparation method is with embodiment 3, the difference is that the amount of modified boron nitride nanosheet is 200 mass parts, test result is shown in
Table one.
Embodiment 5
Preparation method is with embodiment 2, the difference is that the quality of catechol is 2g, the quality of four (second diyl) five amine is
1g, test result are shown in Table one.
Embodiment 6
Preparation method is with embodiment 4, the difference is that the quality of catechol is 1.5g, the quality of ethylenediamine is 1g, test
It the results are shown in Table one.
Embodiment 7
The preparation method is the same as that of Example 1, the difference is that silane coupling agent is KH570, test result is shown in Table one.
Embodiment 8
Preparation method is with embodiment 4, the difference is that silane coupling agent is KH570, test result is shown in Table one.
Embodiment 9
The preparation method is the same as that of Example 1, the difference is that silane coupling agent is silicon 69, test result is shown in Table one.
Embodiment 10: preparation method is with embodiment 4, the difference is that silane coupling agent is silicon 69, test result is shown in Table one.
Comparative example 1
The preparation method is the same as that of Example 1, the difference is that not adding high thermal conductivity filler grain, test result is shown in Table one.
Comparative example 2
The preparation method is the same as that of Example 1, the difference is that adding the unmodified boron nitride nanosheet of 50 mass parts, test result is shown in Table
One.
Comparative example 3
Preparation method is with embodiment 2, the difference is that the unmodified boron nitride nanosheet of 200 mass parts of addition, test result
It is shown in Table one.
Table one
As can be seen from Table I, modified boron nitride nanosheet is added in natural rubber matrix to mention significantly
The heating conduction of high natural rubber, maximum thermal coefficient have reached 1.21W/mK, and 12 times of about pure natural rubber,
At this time the elongation at break of natural rubber and tensile strength have it is significant must improve, and keep lower dielectric constant, Ke Yiying
For electronic material encapsulation field.
As described above, describing the invention in detail, it is clear that as long as essentially without inventive point of the invention is detached from
And effect, obvious variations to those skilled in the art, also it is all included in the scope of protection of the present invention.
Claims (8)
1. a kind of high thermal conductivity boron nitride/native rubber composite material characterized by comprising
Natural rubber matrix: 100 mass parts
Vulcanizing agent: 2-5 mass parts
Modified boron nitride nanosheet: 10-200 mass parts.
2. composite material according to claim 1, it is characterised in that: the vulcanizing agent is sulphur system, the sulphur body
System is sulphur, zinc oxide and stearic acid.
3. the preparation method of composite material described in claim 1, which comprises the following steps:
1) trishydroxymethylaminomethane aqueous solution 1 is prepared；
2) aqueous solution 1 is added in catechol and polyamine compounds, forms solution 2；
3) boron nitride nanosheet is added in solution 2；Solution 3 is formed, is formed in boron nitride nanosheet surface auto polymerization poly-
(catechol/polyamines) (PCPA) layer；
4) solution 3 is heated, heats silane coupling agent, form solution 4, realize secondary function on the boron nitride nanosheet surface
Change；
5) solution 4 is filtered, obtains modified boron nitride nanosheet.
4. method according to claim 3, which is characterized in that the polyamine compounds are ethylenediamine, five amine of tetrem diyl, season
One of penta tetramine and three second tetramines are a variety of；The silane coupling agent is the one or more of KH560, KH570 or Si69.
5. method according to claim 3, which is characterized in that
Appropriate trishydroxymethylaminomethane is added in 100ml deionized water in step 1), adjusting pH value is 7-10, is prepared into
Solution 1；
In step 2) by quality be 1-2g catechol and quality be 0.5-1g polyamine compounds be added in solution 1, make
For at solution 2；
The boron nitride nanosheet that quality is 50-200g is added in solution 2 in step 3), while by prepared mixed solution
It is placed in constant temperature blender with magnetic force, sets bath temperature as 30-40 DEG C, set mixing speed as 400-500r/min, constant temperature
6-10h is reacted, solution 3 is prepared into；
The temperature of solution 3 is heated to 50-70 DEG C in step 4), the silane for then adding mass fraction 1%-15% thereto is even
Join agent, isothermal reaction 5-8h is prepared into solution 4；
Solution 4 is filtered in step 5), gains are washed with deionized 3-5 times, in drying in oven, obtain modified nitrogen
Change boron nanometer sheet.
6. method according to claim 3, which is characterized in that the modified boron nitride nanosheet uniform particle sizes, size are
100-800nm, unformed layer of the boron nitride nanosheet through modification rear surface deposition 2-6nm.
7. method according to claim 3, which is characterized in that further include steps of
6) modified boron nitride nanosheet obtained by step 5) is kneaded with natural rubber；
7) step 6) gains are vulcanized, obtains the native rubber composite material of high thermal conductivity coefficient.
8. method according to claim 7, which is characterized in that
It is kneaded on the double roll mill in step 6), melting temperature is 25-40 DEG C, places 24-32h after being kneaded uniformly；
Is vulcanized in step 7) using process control tablet press machine, control Tooling Fabrication Area temperature is 120 DEG C -160 DEG C, and the tabletting time is
0.5-2h, pressure 15-25MPa.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110144067A (en) * | 2019-06-11 | 2019-08-20 | 三力士股份有限公司 | A kind of preparation method of the heat-conductive composite material of natural rubber |
| CN110862592A (en) * | 2019-11-28 | 2020-03-06 | 北京石油化工学院 | Alumina/carboxylic butyronitrile composite material and preparation method thereof |
| CN111484654A (en) * | 2020-05-11 | 2020-08-04 | 徐工集团工程机械有限公司 | Heat conduction rubber material and rubber track |
| CN111499935A (en) * | 2020-05-22 | 2020-08-07 | 中北大学 | Modified graphene oxide/natural rubber high-thermal-conductivity composite material |
| CN111892753A (en) * | 2020-08-18 | 2020-11-06 | 华东理工大学 | Preparation method of modified hexagonal boron nitride heat-conducting film |
| CN115028891A (en) * | 2022-06-10 | 2022-09-09 | 安徽建筑大学 | Flame-retardant heat-conducting agent, preparation method thereof and application thereof in rubber composite material |
| CN115505267A (en) * | 2022-09-23 | 2022-12-23 | 山东大学 | Method for preparing silicon rubber gasket for electronic packaging heat dissipation by using high-phenyl-content methyl vinyl phenyl silicon rubber |
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| CN106953051A (en) * | 2017-03-10 | 2017-07-14 | 厦门益舟新能源科技有限公司 | A kind of ceramic diaphragm of in-situ preparation compound binding agent and its preparation method and application |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110144067A (en) * | 2019-06-11 | 2019-08-20 | 三力士股份有限公司 | A kind of preparation method of the heat-conductive composite material of natural rubber |
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| CN110862592A (en) * | 2019-11-28 | 2020-03-06 | 北京石油化工学院 | Alumina/carboxylic butyronitrile composite material and preparation method thereof |
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| CN111499935A (en) * | 2020-05-22 | 2020-08-07 | 中北大学 | Modified graphene oxide/natural rubber high-thermal-conductivity composite material |
| CN111892753A (en) * | 2020-08-18 | 2020-11-06 | 华东理工大学 | Preparation method of modified hexagonal boron nitride heat-conducting film |
| CN111892753B (en) * | 2020-08-18 | 2022-08-23 | 华东理工大学 | Preparation method of modified hexagonal boron nitride heat-conducting film |
| CN115028891A (en) * | 2022-06-10 | 2022-09-09 | 安徽建筑大学 | Flame-retardant heat-conducting agent, preparation method thereof and application thereof in rubber composite material |
| CN115505267A (en) * | 2022-09-23 | 2022-12-23 | 山东大学 | Method for preparing silicon rubber gasket for electronic packaging heat dissipation by using high-phenyl-content methyl vinyl phenyl silicon rubber |
| CN115505267B (en) * | 2022-09-23 | 2023-05-23 | 山东大学 | Method for preparing silicone rubber gasket for electronic packaging and heat dissipation by using methyl vinyl phenyl silicone rubber with high phenyl content |
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