CN108192577A - A kind of fire-retardant graphene flexible membrane of high heat conduction and preparation method thereof - Google Patents
A kind of fire-retardant graphene flexible membrane of high heat conduction and preparation method thereof Download PDFInfo
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- CN108192577A CN108192577A CN201711485232.0A CN201711485232A CN108192577A CN 108192577 A CN108192577 A CN 108192577A CN 201711485232 A CN201711485232 A CN 201711485232A CN 108192577 A CN108192577 A CN 108192577A
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- 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
- 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
- C09K21/00—Fireproofing materials
- C09K21/02—Inorganic materials
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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
- C09K21/00—Fireproofing materials
- C09K21/02—Inorganic materials
- C09K21/04—Inorganic materials containing phosphorus
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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
- C09K21/00—Fireproofing materials
- C09K21/06—Organic materials
Abstract
The invention belongs to heat conductive flame-retarding Material Fields, disclose fire-retardant graphene flexible membrane of a kind of high heat conduction and preparation method thereof.Reducing agent with anti-flammability is introduced to graphene oxide layer surface by way of functionalization or grafting and graphene oxide is restored by the fire-retardant graphene flexible membrane of high heat conduction, is then added filler assembling film forming and is obtained；The mass ratio of the reducing agent and graphene oxide with anti-flammability is 1：1~10, the mass ratio of the reducing agent and filler with anti-flammability is 1~1.2：1.The fire-retardant graphene flexible membrane of the high heat conduction can reach 15W m in the thermal conductivity factor of in-plane‑1K‑1, vertical plane thermal conductivity factor can reach 0.8W m‑1·K‑1, tensile strength reach 35Mpa；In addition its flame retardant property is good, without heat release below 500 DEG C, in 540 DEG C of most high fever release temperature, and peak heat release 37Wg‐1Below.
Description
Technical field
The invention belongs to heat conductive flame-retarding Material Fields, and in particular to a kind of fire-retardant graphene flexible membrane of high heat conduction and its preparation
Method.
Background technology
The progress of modern information technologies promotes electronic device toward intelligent, high frequency and micromation fast development, thus
The energy density of electronic device is caused to increase, at work, heat accumulates rapidly, the temperature of device work is caused to increase, seriously
Influence service life, safety and the user experience of element.It wherein radiates and the safety based on fire prevention consideration is for electricity
The urgent problem to be solved during use of sub- device.
Carbon-based material has efficient heat conductivility, therefore has very big application value in field of radiating.It is but traditional
Carbon-based material such as graphite etc. need the energy consumptions such as high temperature technology that could form a film, and its mechanical property is bad.Graphene is as two
Tie up structural material, on heat dissipation performance have unique advantage, and be used as the derivative of graphene, graphene oxide preparation with
And it is simple in cost, simultaneous oxidation graphene is due to its unique molecular structure, and for its MOLECULE DESIGN, performance improvement provides
Basis.CN103449423A discloses one kind using graphene oxide as raw material, and graphene heat conduction is prepared by techniques such as films
The method of film, the technique are related to the process of inert atmosphere high temperature thermal reduction, and energy consumption is higher, and process is complicated, simultaneously for
Its flame-retarding does not carry out the considerations of effective.
Invention content
The defects of in order to solve the prior art and deficiency, primary and foremost purpose of the invention are to provide a kind of fire-retardant graphite of high heat conduction
Alkene flexible membrane.
Another object of the present invention is to provide the membrane preparation method of the fire-retardant graphene flexible membrane of the high heat conduction.
It is still another object of the present invention to provide the fire-retardant graphene flexible membrane of the high heat conduction as dissipation from electronic devices material
The application of material.
The purpose of the present invention is achieved through the following technical solutions：
A kind of fire-retardant graphene flexible membrane of high heat conduction, by the reduction with anti-flammability by way of functionalization or grafting
Agent is introduced to graphene oxide layer surface and graphene oxide is restored, and then adds filler assembling film forming and obtains；Institute
The mass ratio for stating reducing agent and graphene oxide with anti-flammability is 1：1~10, the reducing agent with anti-flammability is with filling out
The mass ratio of material is 1~1.2：1.
Each raw material dosage proportioning of the present invention can make to form good synergistic effect between filler and graphene oxide, if
Each dosage increases or decreases, then can destroy synergistic effect.If filler is excessive, mechanical property is deteriorated after film forming, reduction of pliability；Also
Former agent is crossed at most can be so that filming performance be deteriorated, and corresponding mechanical property and heat conductivility are declined.
The preparation method of the fire-retardant graphene flexible membrane of high heat conduction, includes the following steps：
(1) to graphene oxide aqueous dispersions add in anti-flammability reducing agent, adjust PH to 8~10, ultrasound 30~
It 90 minutes, is then stirred under the conditions of 50~90 DEG C to being completely dispersed；The reducing agent and graphene oxide with anti-flammability
Mass ratio be 1：1~10；
(2) then add in filler, ultrasonic disperse 30~90 minutes；The quality of the reducing agent and filler with anti-flammability
Than being 1~1.2：1；
(3) last solvent flashing obtains the fire-retardant graphene flexible membrane of the high heat conduction after dry.
Graphene oxide is water-soluble preferably, and ultrasonic disperse is after 30 minutes, and dispersion performance is preferable in aqueous solution, when addition is filled out
Material is stirred and ultrasound, and contact-impact is more abundant between filler and graphene oxide, therefore reacts very fast and greatly shorten
Reaction time.
The present invention does not require the property of graphene oxide, and few layer can pass through to the graphene oxide of multilayer
Conventional method such as Hummers methods or modified Hummers methods are made, and also can directly be commercially available on the market.
Preferably, it is described to be dispersed with stirring the time as 60~150 minutes.
Preferably, the reducing agent with anti-flammability be Modified Citric Acid sodium, it is aluminium, modified gallic acid, dopamine, more
Any one of bar amine derivative, modification of chitosan, POSS, layered metal oxide；The modification refer to by chemistry or
Person's physical method makes compound have anti-flammability.
Preferably, the filler is nano-cellulose, carbon nanotube, nanometer silicon carbide, boron nitride, nanometer hydroxyapatite
In it is one or more.
Preferably, in step (3) at 20~70 DEG C solvent flashing.
Wherein, for above-mentioned using dopamine as the scheme of the reducing agent with anti-flammability, after introducing dopamine, with
Graphene forms the structure of " sandwich ", and in burning, the graphene of superficial layer forms a fine and close carbon-coating as protection
Layer so that it is fire-retardant to reach physics.In addition to this, the hydroxyl on dopamine (tea phenol) has very strong cleaning free radical activity,
The free radical that burning generates can be removed in combustion process, so as to reach flame retardant effect.It therefore, can between dopamine and graphene
To form good physical chemistry flame retardant synergistic effect.And for above-mentioned filler (nano-cellulose, carbon nanotube, nano silicon carbide
It is one or more in silicon, boron nitride and nanometer hydroxyapatite), wherein nano-cellulose, carbon nanotube have high draw ratio,
" bridge " effect can be formed between graphene so that the thermal conducting path in film greatly increases, nanometer silicon carbide and boron nitride
All there is high thermal conductivity, and the filler dosed all has certain flame retardant property, also has in nanometer hydroxyapatite abundant
P elements have excellent flame retardant effect.
The present invention is had the following advantages and advantageous effect relative to the prior art：
(1) flexible membrane prepared by the present invention, preparation process is simple, flexible, has high-termal conductivity and good resistance
Combustion property.
(2) process of flexible membrane prepared by the present invention selects green reduction mode redox graphene.
(3) process of flexible membrane prepared by the present invention, is not related to high temperature, high-pressure process is simple for process, has excellent performance.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Embodiment 1：
Graphene oxide is prepared by modified Hummers, the aqueous dispersions of 5mg/ml is then prepared into, takes above-mentioned oxidation stone
Black alkene solution 70ml adds in 0.35g aluminium, adjusts PH to 8.5, then it is small to be dispersed with stirring 2 under the conditions of 80 DEG C for ultrasound 30 minutes
When.Then 0.3g carbon nanotubes, ultrasonic disperse 30 minutes are added in.It finally pours into mold, at ambient temperature solvent flashing, does
Dry film forming.
Embodiment 2：
Graphene oxide is prepared by modified Hummers, the aqueous dispersions of 8mg/ml is then prepared into, takes above-mentioned oxidation stone
Black alkene solution 45ml adds in 0.36g and is modified gallic acid, adjusts PH to 9, then ultrasound 30 minutes stirs under the conditions of 80 DEG C
Dispersion 2 hours.Then 0.3g boron nitride, ultrasonic disperse 30 minutes are added in.It finally pours into mold, volatilizees at ambient temperature molten
Agent, drying and forming-film.
Embodiment 3：
Graphene oxide is prepared by modified Hummers, the aqueous dispersions of 10mg/ml is then prepared into, takes above-mentioned oxidation
Graphene solution 36ml adds in 0.36g Dopamine hydrochlorides, adds in Tris buffer solutions and adjusts PH to 8.5,30 minutes ultrasonic, so
It is dispersed with stirring under the conditions of 80 DEG C afterwards 2 hours.Then 0.3g nano-celluloses, ultrasonic disperse 30 minutes are added in.Finally pour into mould
In tool, solvent flashing at ambient temperature, drying and forming-film.
Embodiment 4：
Graphene oxide is prepared by modified Hummers, the aqueous dispersions of 4mg/ml is then prepared into, takes above-mentioned oxidation stone
Black alkene solution 90ml adds in 0.36g Dopamine hydrochlorides, adds in Tris buffer solutions and adjusts PH to 9, ultrasound 30 minutes, Ran Hou
It is dispersed with stirring under the conditions of 80 DEG C 2 hours.Then 0.3g carbon nanotubes, ultrasonic disperse 30 minutes are added in.Finally pour into mold,
Solvent flashing under room temperature, drying and forming-film.
Embodiment 5：
Graphene oxide is prepared by modified Hummers, the aqueous dispersions of 5mg/ml is then prepared into, takes above-mentioned oxidation stone
Black alkene solution 70ml adds in 0.35g aluminium, adjusts PH to 9, then ultrasound 30 minutes is dispersed with stirring 2 hours under the conditions of 80 DEG C.
Then 0.3g silicon carbide, ultrasonic disperse 30 minutes are added in.It finally pours into mold, at ambient temperature solvent flashing, is dried to
Film.
Embodiment 6：
Graphene oxide is prepared by modified Hummers, the aqueous dispersions of 8mg/ml is then prepared into, takes above-mentioned oxidation stone
Black alkene solution 45ml adds in 0.36g montmorillonites, adjusts PH to 9, then it is small to be dispersed with stirring 2 under the conditions of 80 DEG C for ultrasound 30 minutes
When.Then 0.3g hydroxyapatites, ultrasonic disperse 30 minutes are added in.It finally pours into mold, at ambient temperature solvent flashing,
Drying and forming-film.
The membrane material that said program is prepared can reach 15W m in the thermal conductivity factor of in-plane-1K-1, vertical plane
Thermal conductivity factor can reach 0.8W m-1·K-1, tensile strength reach 35Mpa；In addition its flame retardant property is good, does not have below 500 DEG C
There is hot release, in 540 DEG C of most high fever release temperature, peak heat release 37Wg‐1Below.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (7)
1. a kind of fire-retardant graphene flexible membrane of high heat conduction, which is characterized in that will have resistance by way of functionalization or grafting
The reducing agent of combustion property is introduced to graphene oxide layer surface and graphene oxide is restored, and then adds filler and is assembled into
Film obtains；The mass ratio of the reducing agent and graphene oxide with anti-flammability is 1：1~10, the going back with anti-flammability
The mass ratio of former agent and filler is 1~1.2：1.
2. the preparation method of the fire-retardant graphene flexible membrane of high heat conduction described in claim 1, which is characterized in that include the following steps：
(1) reducing agent with anti-flammability is added in graphene oxide aqueous dispersions, adjusts PH to 8~10,30~90 points of ultrasound
Then clock is dispersed with stirring completely under the conditions of 50~90 DEG C；The quality of the reducing agent and graphene oxide with anti-flammability
Than being 1：1~10；
(2) then add in filler, ultrasonic disperse 30~90 minutes；The mass ratio of the reducing agent and filler with anti-flammability is
1~1.2：1；
(3) last solvent flashing obtains the fire-retardant graphene flexible membrane of the high heat conduction after dry.
3. the preparation method of the fire-retardant graphene flexible membrane of high heat conduction according to claim 2, which is characterized in that the stirring point
It is 60~150 minutes to dissipate the time.
4. the preparation method of the fire-retardant graphene flexible membrane of high heat conduction according to claim 2, which is characterized in that described that there is resistance
The reducing agent of combustion property is Modified Citric Acid sodium, aluminium, modified gallic acid, dopamine, DOPA amine derivative, modification of chitosan,
Any one of POSS, layered metal oxide；The modification refers to have compound by chemistry or physical method
Anti-flammability.
5. the preparation method of the fire-retardant graphene flexible membrane of high heat conduction according to claim 2, which is characterized in that the filler is
It is one or more in nano-cellulose, carbon nanotube, nanometer silicon carbide, boron nitride, nanometer hydroxyapatite.
6. the preparation method of the fire-retardant graphene flexible membrane of high heat conduction according to claim 2, which is characterized in that in step (3)
The solvent flashing at 20~70 DEG C.
7. application of the fire-retardant graphene flexible membrane of high heat conduction described in claim 1 as dissipation from electronic devices material.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108689400A (en) * | 2018-06-28 | 2018-10-23 | 合肥艾飞新材料有限公司 | A kind of fire-retardant graphene film and preparation method thereof |
| CN109054151A (en) * | 2018-07-11 | 2018-12-21 | 河南科技大学 | A kind of polyolefin flame-retardant composite material and preparation method |
| CN109824971A (en) * | 2019-03-07 | 2019-05-31 | 华东理工大学 | By the elastomer and preparation method of the fire-retardant enhancing of biomimetic modification graphene |
| CN109880178A (en) * | 2019-03-21 | 2019-06-14 | 东北林业大学 | A kind of nano-cellulose enhancing graphene oxide/poly-dopamine layered bionic material and preparation method thereof |
| CN110144063A (en) * | 2019-05-13 | 2019-08-20 | 浙江工业大学 | A kind of heat conductive insulating cellulose membrane and preparation method thereof |
| CN110303731A (en) * | 2019-07-04 | 2019-10-08 | 中科广化（重庆）新材料研究院有限公司 | A kind of epoxy composite material and its preparation method and application that high thermal conductivity is fire-retardant |
| CN110540198A (en) * | 2019-09-25 | 2019-12-06 | 广东工业大学 | Graphene oxide-based self-repairing flame-retardant composite film, preparation thereof and fire alarm |
| CN110619982A (en) * | 2019-09-25 | 2019-12-27 | 广东工业大学 | Graphene oxide-based composite material and preparation method and application thereof |
| CN111518317A (en) * | 2020-05-13 | 2020-08-11 | 上海交通大学 | High-thermal-conductivity and water-transmission composite film material and preparation method and application thereof |
| CN112382829A (en) * | 2020-10-14 | 2021-02-19 | 江西银汇新能源有限公司 | Functionalized flexible membrane and preparation method and application thereof |
| CN112552556A (en) * | 2020-12-09 | 2021-03-26 | 四川华造宏材科技有限公司 | Degradable high-thermal-conductivity composite material and preparation method thereof |
| CN114889175A (en) * | 2022-05-25 | 2022-08-12 | 福州大学 | Preparation and application of modified graphene oxide/hydroxyapatite nanowire composite paper |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108689400A (en) * | 2018-06-28 | 2018-10-23 | 合肥艾飞新材料有限公司 | A kind of fire-retardant graphene film and preparation method thereof |
| CN109054151B (en) * | 2018-07-11 | 2021-04-02 | 河南科技大学 | Polyolefin flame-retardant composite material and preparation method thereof |
| CN109054151A (en) * | 2018-07-11 | 2018-12-21 | 河南科技大学 | A kind of polyolefin flame-retardant composite material and preparation method |
| CN109824971A (en) * | 2019-03-07 | 2019-05-31 | 华东理工大学 | By the elastomer and preparation method of the fire-retardant enhancing of biomimetic modification graphene |
| CN109824971B (en) * | 2019-03-07 | 2021-09-07 | 华东理工大学 | Bionic modified graphene flame-retardant reinforced elastomer and preparation method thereof |
| CN109880178A (en) * | 2019-03-21 | 2019-06-14 | 东北林业大学 | A kind of nano-cellulose enhancing graphene oxide/poly-dopamine layered bionic material and preparation method thereof |
| CN110144063A (en) * | 2019-05-13 | 2019-08-20 | 浙江工业大学 | A kind of heat conductive insulating cellulose membrane and preparation method thereof |
| CN110303731A (en) * | 2019-07-04 | 2019-10-08 | 中科广化（重庆）新材料研究院有限公司 | A kind of epoxy composite material and its preparation method and application that high thermal conductivity is fire-retardant |
| CN110303731B (en) * | 2019-07-04 | 2022-01-28 | 中科广化（重庆）新材料研究院有限公司 | High-thermal-conductivity flame-retardant epoxy composite material and preparation method and application thereof |
| CN110619982B (en) * | 2019-09-25 | 2021-07-06 | 广东工业大学 | Graphene oxide-based composite material and preparation method and application thereof |
| CN110619982A (en) * | 2019-09-25 | 2019-12-27 | 广东工业大学 | Graphene oxide-based composite material and preparation method and application thereof |
| CN110540198A (en) * | 2019-09-25 | 2019-12-06 | 广东工业大学 | Graphene oxide-based self-repairing flame-retardant composite film, preparation thereof and fire alarm |
| CN111518317A (en) * | 2020-05-13 | 2020-08-11 | 上海交通大学 | High-thermal-conductivity and water-transmission composite film material and preparation method and application thereof |
| CN111518317B (en) * | 2020-05-13 | 2021-12-28 | 上海交通大学 | High-thermal-conductivity and water-transmission composite film material and preparation method and application thereof |
| CN112382829A (en) * | 2020-10-14 | 2021-02-19 | 江西银汇新能源有限公司 | Functionalized flexible membrane and preparation method and application thereof |
| CN112552556A (en) * | 2020-12-09 | 2021-03-26 | 四川华造宏材科技有限公司 | Degradable high-thermal-conductivity composite material and preparation method thereof |
| CN112552556B (en) * | 2020-12-09 | 2022-07-01 | 四川华造宏材科技有限公司 | Degradable high-thermal-conductivity composite material and preparation method thereof |
| CN114889175A (en) * | 2022-05-25 | 2022-08-12 | 福州大学 | Preparation and application of modified graphene oxide/hydroxyapatite nanowire composite paper |
| CN114889175B (en) * | 2022-05-25 | 2023-07-18 | 福州大学 | Preparation and application of modified graphene oxide/hydroxyapatite nanowire composite paper |
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Application publication date: 20180622 |