CN106496634A - A kind of preparation method of magnesium hydroxide Graphene composite heat-conducting insulating packing - Google Patents
A kind of preparation method of magnesium hydroxide Graphene composite heat-conducting insulating packing Download PDFInfo
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- CN106496634A CN106496634A CN201610895658.2A CN201610895658A CN106496634A CN 106496634 A CN106496634 A CN 106496634A CN 201610895658 A CN201610895658 A CN 201610895658A CN 106496634 A CN106496634 A CN 106496634A
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- graphene oxide
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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
- C08K9/10—Encapsulated 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
- C08K3/02—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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Abstract
The invention belongs to technical field of fine, and in particular to a kind of preparation method of magnesium hydroxide Graphene composite heat-conducting insulating packing.The present invention adds magnesium salt solution with graphene oxide water solution as raw material, by adjusting pH value, makes the magnesium hydroxide that in-situ deposition reaction is obtained on graphene oxide;The magnesium hydroxide graphene oxide hybrid material of above-mentioned gained carries out heat treatment under an inert atmosphere within the temperature range of 150 300 DEG C, make graphene oxide that thermal reduction to occur to a certain extent, that is, obtain magnesium hydroxide Graphene (redox graphene) compounded mix.The filler is added in electric insulating copolymer the thermal conductivity that can improve polymer composites, while remaining electrically isolated from property, also improves the fire resistance of composite to a certain extent.The preparation method has simple to operate, environmental friendliness, it is easy to the features such as large-scale production.
Description
Technical field
The invention belongs to technical field of fine, and in particular to a kind of magnesium hydroxide-Graphene (reduction-oxidation graphite
Alkene) composite heat-conducting insulating packing preparation method.
Background technology
With the high speed development of microelectronics industry, integrated circuit high speed, densification increasingly, therefore it is required that microelectronics material
Material has good heat conductivility.For some fields(Such as LED field), in addition it is also necessary to there is material good electrical insulation capability to come
Prevent electrical short etc..Therefore the material for preparing with good heat-conductivity and insulating has obtained the concern of academia and industrial quarters.Poly-
The advantages of compound material is due to light weight, insulation, simple moulding process to be become supported using most wide electronics at present or encapsulating material.
But for conventional electronic material, due to relatively low thermal conductivity (TC itself<0.3 W/m K), can not meet electronics material
Expect the needs to radiating, it is therefore desirable to which raising thermal conductivity is modified to which.The insulating packing added with high thermal conductivity is to carry
A kind of effective means of high polymer thermal conductivity.Some common ceramic materials such as boron nitride, aluminium nitride, carborundum etc. have very high
Thermal conductivity (TC>100 W/m K), add them into the thermal conductivity that material can be significantly improved in polymer, yet with
Expensive, limit its application industrially.The cheap metal-oxide of other for example magnesium oxide, aluminium oxide,
Zinc oxide etc. also has higher thermal conductivity (TC=10-100 W/m K), and adding them into also can be to a certain extent in polymer
Improve the thermal conductivity of material, but if want to obtain very high thermal conductivity be accomplished by adding substantial amounts of filler (>50 vol %),
This will certainly loss material other performance, such as processing characteristics, mechanical property etc..
Graphene is a kind of new two-dimentional material with carbon element, has high thermal conductivity (TC=5300 W/m K), is added into
The thermal conductivity of material can be significantly increased very much in polymer.The Graphene that content is 5% is added to polypropylene by Fu Qiang et al.
(PP) in find material thermal conductivity reach 0.4 W/m K, be pure PP twice (Colloid. Polym. Sci.2015,
293, 1495).But Graphene also has very high electrical conductivity (EC ~ 6000 S/cm) simultaneously, the therefore addition of Graphene can be big
The big insulating properties for reducing polymer.Have been reported that the heat conduction threshold value for showing material is higher than conductivity threshold, that is to say, that work as addition
When the amount of Graphene can increase substantially the thermal conductivity of material, material is conductive, and this will be unfavorable for Graphene in microelectronics
The application (Chem. Mater. 2015,27,2100) of material.Therefore the heat good in order to play Graphene to greatest extent
Conductance ensures the insulating properties of material simultaneously, and the inorganic filler of insulation is wrapped in graphenic surface to prevent graphene conductive from leading to
The formation on road can realize that aluminium oxide parcel is arrived graphite using sol-gal process by nonconducting purpose Jeong of material conducts heat et al.
Alkene surface is prepared for the compounded mix of alumina-graphite alkene, adds it in polymer, it is found that the thermal conductivity of material has been carried
Height, at the same material holding insulation (Mater. Chem. Phys. 2015,153,291).But, prepare at present insulating packing-
The method of Graphene compounded mix usually needs to use organic solvent, is unfavorable for environmental conservation, and preparation process is more complicated.
Therefore the method for designing simpler, convenient, environmental protection prepares insulating packing-Graphene compounded mix to expanding Graphene in micro- electricity
The application of sub-industry has great significance.
The present invention proposes the preparation side of a kind of magnesium hydroxide-Graphene (redox graphene) composite heat-conducting insulating packing
Method.Its main process includes, adds magnesium salt, by adjusting pH value, make in graphite oxide first in graphene oxide water solution
In-situ deposition magnesium hydroxide on alkene;By magnesium hydroxide obtained above-graphene oxide hybrid material under an inert atmosphere in
Heat treatment is carried out within the temperature range of 200-300 DEG C, is made graphene oxide that thermal reduction to occur to a certain extent, that is, is obtained hydrogen
Magnesium oxide-Graphene (redox graphene) compounded mix.
Content of the invention
It is an object of the invention to propose a kind of simple, convenient, environmental protection to prepare magnesium hydroxide-Graphene composite heat-conducting exhausted
The method of edge filler.
The method for preparing magnesium hydroxide-Graphene composite heat-conducting insulating packing proposed by the present invention, concretely comprises the following steps:
With graphene oxide water solution as raw material, magnesium salt solution is added, by adjusting pH value, in situ heavy on graphene oxide
The magnesium hydroxide that product reaction is obtained;Wherein, graphene oxide is 1 with the mass ratio of magnesium salt:0.1-1:100, preferably 1:1-1:
50;
The magnesium hydroxide of said process gained-graphene oxide hybrid material is put in an inert atmosphere in 150-300 DEG C of temperature
Heat treatment is carried out in the range of degree, is made graphene oxide that thermal reduction to occur to a certain extent, that is, is obtained magnesium hydroxide-Graphene
(redox graphene) compounded mix.
Wherein, magnesium hydroxide is a kind of important inorganic anti-flaming material, can at 300 DEG C stable existence;Graphite oxide
Alkene can occur a certain degree of thermal reduction in this temperature range at 150-300 DEG C, generate Graphene (reduction-oxidation graphite
Alkene).The compounded mix is added in electric insulating copolymer the thermal conductivity that can improve polymer composites, while keeping electricity
Insulating properties, while improve the fire resistance of composite to a certain extent.
In the present invention, described graphene oxide water solution is the graphene oxide suspension being dispersed in water.Oxidation stone
The concentration of black alkene suspension is 0.01-10mg/mL, and preferred concentration is 1-10mg/mL.
In the present invention, described magnesium salt can be the water-soluble salts such as magnesium chloride, magnesium nitrate, magnesium sulfate.Magnesium salt water
The concentration of solution is 0.01-10mg/mL, and preferred concentration is 1-10mg/mL.
In the present invention, the material of described regulation pH value, the mainly water-soluble alkali such as sodium hydroxide, potassium hydroxide, ammonia
Property material.PH value is more than 8, and preferable ph is 8-10.
In the present invention, described heat treatment temperature is magnesium hydroxide stable existence while making graphene oxide that certain journey to occur
Degree thermal reduction forms the temperature of Graphene, generally will be between 150-300 DEG C.
In the present invention, described inert atmosphere can be the non-oxidizing atmospheres such as nitrogen, argon, carbon dioxide.
In the present invention, described heat treatment time, generally in 0.5-10 hours.
In the present invention, described polymer is the polymer of electric insulation, can be thermoplastic polymer and thermosetting polymerization
Thing.
Heretofore described magnesium hydroxide-Graphene (redox graphene) compounded mix, is adding polymer matrix
When body prepares composite, addition is generally the 10-70% (mass content) of composite total amount.
The simple and convenient environmental protection of the preparation method, is suitable for large-scale use.The magnesium hydroxide of preparation-Graphene compounded mix adds
Enter in the polymer of electric insulation and the thermal conductivity and anti-flammability of material can be improved on the premise of insulating properties is kept, in microelectronics
Material Field has broad application prospects.
Specific embodiment
Specifically by the following examples the present invention is further illustrated.
Embodiment 1
5000 mL of graphene oxide water solution of 1 mg/mL is prepared, the magnesium chloride and 1.5 mol/L of 0.75 mol/L is added
Each 1000 ml of sodium hydrate aqueous solution, stirs 2 h, and filtering drying is crushed afterwards, fires 2 h, obtain under 250 DEG C of argon gas atmospheres
Arrive magnesium hydroxide-Graphene (redox graphene) compounded mix.Scanning electron microscope analysis show that magnesium hydroxide is uniformly wrapped in
On Graphene.
It is added in polypropylene (PP, Yangtze petrochemical industry, trade mark F401) matrix, finds when compounded mix mass fraction is
When 50%, the composite of gained keeps insulating properties, and thermal conductivity is 0.38W/m K, is 1.8 times of pure PP (0.21 W/m K),
Oxygen index (OI) (OI) is 28.0 (pure PP is 18.5).
Embodiment 2
Other wherein replace magnesium chloride with magnesium nitrate with embodiment 1.The composite of gained keeps the insulating properties, its thermal conductivity to be
0.41W/m K, oxygen index (OI) are 27.0.
Embodiment 3
Other wherein replace magnesium chloride with magnesium sulfate with embodiment 1.The composite of gained keeps the insulating properties, its thermal conductivity to be
0.4 W/m K, oxygen index (OI) is 26.5.
Embodiment 4
Other wherein replace sodium hydroxide with potassium hydroxide with embodiment 1.The composite of gained keeps insulating properties, its heat conduction
Rate is 0.42 W/m K, and oxygen index (OI) is 27.0.
Embodiment 5
Other wherein replace sodium hydroxide with ammonia with embodiment 1.The composite of gained keeps the insulating properties, its thermal conductivity to be
0.40 W/m K, oxygen index (OI) is 27.0.
Embodiment 6
Other wherein replace argon with nitrogen with embodiment 1.The composite of gained keeps insulating properties, and its thermal conductivity is 0.41
W/m K, oxygen index (OI) are 27.0.
Embodiment 7
Other wherein replace polypropylene with epoxy resin (blue star Wuxi petrochemical industry, trade mark E51) with embodiment 1.The composite wood of gained
Material keeps insulating properties, and its thermal conductivity is 0.38W/m K, and oxygen index (OI) is 27.5.
Embodiment 8
Other wherein replace 250 DEG C with 300 DEG C with embodiment 1.The composite of gained keeps the insulating properties, its thermal conductivity to be
0.41 W/m K, oxygen index (OI) is 27.0.
Embodiment 9
Other wherein replace magnesium chloride, potassium hydroxide to replace sodium hydroxide, carbon dioxide to replace argon with embodiment 1 with magnesium nitrate
Gas.The composite of gained keeps insulating properties, and its thermal conductivity is 0.42 W/m K, and oxygen index (OI) is 27.0.
Claims (8)
1. the preparation method of a kind of magnesium hydroxide-Graphene composite heat-conducting insulating packing, it is characterised in that concretely comprise the following steps:
(1)With graphene oxide water solution as raw material, magnesium salt solution is added, by adjusting pH value, former on graphene oxide
The magnesium hydroxide that position deposition reaction is obtained;Wherein, graphene oxide is 1 with the mass ratio of magnesium salt:0.1-1:100;
(2)The magnesium hydroxide of said process gained-graphene oxide hybrid material is put in an inert atmosphere in 150-300 DEG C
Within the temperature range of carry out heat treatment, make graphene oxide that thermal reduction to occur to a certain extent, that is, obtain magnesium hydroxide-graphite
Alkene compounded mix.
2. preparation method according to claim 1, it is characterised in that described graphene oxide water solution is for being dispersed in water
In graphene oxide suspension, the concentration of graphene oxide suspension is 0.01-10mg/mL;
Described magnesium salt is magnesium chloride, magnesium nitrate or magnesium sulfate water-soluble salts, and the concentration of magnesium salt solution is 0.01-
10mol/L.
3. preparation method according to claim 1 and 2, it is characterised in that the material of described regulation pH value is hydroxide
Sodium, potassium hydroxide or ammonia, pH value are more than 8.
4. preparation method according to claim 3, it is characterised in that described inert atmosphere is nitrogen, argon or dioxy
Change carbon non-oxidizing atmosphere.
5. the preparation method according to claim 1,2 or 4, it is characterised in that described heat treatment time is 0.5-10
Hour.
6. the magnesium hydroxide that preparation method as described in one of claim 1-5 is obtained-Graphene composite heat-conducting insulating packing should
With being that the filler is added in electric insulating copolymer.
7. application according to claim 6, described electric insulating copolymer include thermoplastic polymer and thermosetting polymerization
Thing.
8. application according to claim 7, the addition of described magnesium hydroxide-Graphene composite heat-conducting insulating packing is
The 10-70% of composite gross mass.
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Cited By (7)
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CN108285778A (en) * | 2018-01-25 | 2018-07-17 | 广东工业大学 | A kind of high thermal conductivity paraffin composite phase change material and preparation method thereof |
CN108295829A (en) * | 2018-02-07 | 2018-07-20 | 福建工程学院 | The preparation and application of magnesium hydroxide/redox graphene composite material |
CN109206848A (en) * | 2017-06-30 | 2019-01-15 | 洛阳尖端技术研究院 | A kind of epoxy prepreg and preparation method thereof |
CN109233869A (en) * | 2018-08-09 | 2019-01-18 | 苏州市泽镁新材料科技有限公司 | A kind of preparation method of the high fire-retardance high thermal conductivity composite particles based on magnesium hydroxide |
CN110423379A (en) * | 2019-08-12 | 2019-11-08 | 哈尔滨理工大学 | A kind of magnesium hydroxide/graphene platelet composite flame-retardant agent and preparation method thereof |
WO2022088429A1 (en) * | 2020-10-30 | 2022-05-05 | 歌尔股份有限公司 | Conductive wire material, coil, and apparatus |
WO2022088427A1 (en) * | 2020-10-30 | 2022-05-05 | 歌尔股份有限公司 | Conductive wire, conductive coil, and conductive device |
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Cited By (8)
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CN109206848A (en) * | 2017-06-30 | 2019-01-15 | 洛阳尖端技术研究院 | A kind of epoxy prepreg and preparation method thereof |
CN108285778A (en) * | 2018-01-25 | 2018-07-17 | 广东工业大学 | A kind of high thermal conductivity paraffin composite phase change material and preparation method thereof |
CN108295829A (en) * | 2018-02-07 | 2018-07-20 | 福建工程学院 | The preparation and application of magnesium hydroxide/redox graphene composite material |
CN109233869A (en) * | 2018-08-09 | 2019-01-18 | 苏州市泽镁新材料科技有限公司 | A kind of preparation method of the high fire-retardance high thermal conductivity composite particles based on magnesium hydroxide |
CN110423379A (en) * | 2019-08-12 | 2019-11-08 | 哈尔滨理工大学 | A kind of magnesium hydroxide/graphene platelet composite flame-retardant agent and preparation method thereof |
CN110423379B (en) * | 2019-08-12 | 2021-05-07 | 哈尔滨理工大学 | Magnesium hydroxide/graphene sheet composite flame retardant and preparation method thereof |
WO2022088429A1 (en) * | 2020-10-30 | 2022-05-05 | 歌尔股份有限公司 | Conductive wire material, coil, and apparatus |
WO2022088427A1 (en) * | 2020-10-30 | 2022-05-05 | 歌尔股份有限公司 | Conductive wire, conductive coil, and conductive device |
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Application publication date: 20170315 |