CN108530952A - A kind of preparation method of graphene coated white carbon nanocomposite - Google Patents
A kind of preparation method of graphene coated white carbon nanocomposite Download PDFInfo
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- CN108530952A CN108530952A CN201810314760.8A CN201810314760A CN108530952A CN 108530952 A CN108530952 A CN 108530952A CN 201810314760 A CN201810314760 A CN 201810314760A CN 108530952 A CN108530952 A CN 108530952A
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- white carbon
- graphene coated
- coated white
- carbon nanocomposite
- filter cake
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/309—Combinations of treatments provided for in groups C09C1/3009 - C09C1/3081
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
Abstract
The invention discloses a kind of preparation methods of graphene coated white carbon nanocomposite, include the following steps：(1) graphite oxide, cyclomethicone are added in deionized water, are stirred at room temperature；(2) PS PEG resins are added in the solution, heating, constant temperature stirring；(3) by laser irradiation and reaction, black gel is obtained；(4) gel is put into the mixed liquor of water/n-butanol, ultrasound filters, obtains filter cake；(5) filter cake is dried in vacuo and is ground, obtain product i.e. graphene coated white carbon nanocomposite.The present invention is at low cost, easy, quick, need not use any photochemical catalyst or reducing agent, realize the graphene coated white carbon nanocomposite for producing environmentally protective stabilization on a large scale.
Description
Technical field
The present invention relates to a kind of preparation methods of graphene coated white carbon nanocomposite.
Background technology
White carbon is unformed SiO2High degree of dispersion white powder, be chiefly used in the reinforcing agent of rubber industry, use white carbon
The automobile tire of reinforced rubber manufacture has the remarkable advantage that wet-sliding resistant performance is good and rolling resistance is low, but processes automobile tire
Carbon black used in sizing material or white carbon category nano-powder, surface energy is high, and nano-dispersion is extremely difficult to mechanical Wet smelting method, and often
It is distributed in rubber matrix with the aggregation that grain size is larger, to damage the physical mechanical property of its vulcanizate.
Graphite oxide reduction method is to prepare the most popular method of graphene at present, reducing agent used mainly have hydrazine hydrate,
Sodium borohydride, p-phenylenediamine etc., although these reducing agents can effectively restore graphene oxide, its huge toxicity limit
Promotion and application are made.
Invention content
The present invention is above-mentioned in order to overcome the shortcomings of, provides a kind of preparation of graphene coated white carbon nanocomposite
Method, is stablized by graphene coated white carbon nanocomposite performance prepared by this method, has good phase with rubber
Capacitive and dispersibility.
Technical scheme is as follows：
A kind of preparation method of graphene coated white carbon nanocomposite, which is characterized in that include the following steps：
(1) graphite oxide GO (0.1-0.5 grams), (1-3 grams) of cyclomethicone are added in 100 ml deionized waters,
Graphite oxide：Cyclomethicone：Deionized water=0.1-0.5 grams：1-3 grams：It 100 milliliters, is stirred at room temperature at 200 rpm
10min；
(2) 1 gram of PS-PEG resin is added in step (1) solution, is heated to 60-80 DEG C, constant temperature stirs at 300 rpm
3h；
(3) step (2) solution is cooled to room temperature, import Photoreactor in, be irradiated by YLS-2000 laser and
Reaction reacts 6h, obtains black gel；
(4) it is deionized water step (3) gel to be put into 150 milliliters of volume ratios：N-butanol=1：In 1 mixed liquor,
80-120W, 30-50KHz ultrasound 2-3h filter, filter cake are washed with deionized to mass conservation；
(5) step (4) filter cake is dried in vacuo 8-10h at 50-80 DEG C, the filter cake after drying is ground, is obtained
Product, that is, graphene coated white carbon nanocomposite.
The beneficial effects of the invention are as follows：
It is nano combined that the present invention prepares stable graphene coated white carbon by laser radiation method reduction-oxidation graphite
Material, this method is at low cost, easy, quick, need not use any photochemical catalyst or reducing agent, realize large-scale production
The graphene coated white carbon nanocomposite of environmentally protective stabilization.
Description of the drawings
Examples of the present invention will be described by way of reference to the accompanying drawings, wherein：
Fig. 1 is the XRD diagram of raw material graphite oxide GO；
Fig. 2 is the XRD diagram of graphene coated white carbon nanocomposite；
Fig. 3 is the grain size test chart of graphene coated white carbon nanocomposite；
Fig. 4 is the SEM figures of raw material graphite oxide；
Fig. 5 is the TEM figures of graphene coated white carbon nanocomposite.
Specific implementation mode
Any feature disclosed in this specification unless specifically stated can be equivalent or with similar purpose by other
Alternative features are replaced.That is, unless specifically stated, each feature is an example in a series of equivalent or similar characteristics
.
A kind of preparation method of graphene coated white carbon nanocomposite, includes the following steps：
(1) graphite oxide GO (0.1-0.5 grams), (1-3 grams) of cyclomethicone are added in 100 ml deionized waters,
Graphite oxide：Cyclomethicone：Deionized water=0.1-0.5 grams：1-3 grams：It 100 milliliters, is stirred at room temperature at 200 rpm
10min；
(2) 1 gram of PS-PEG resin is added in step (1) solution, is heated to 60-80 DEG C, constant temperature stirs at 300 rpm
3h；
(3) step (2) solution is cooled to room temperature, import Photoreactor in, be irradiated by YLS-2000 laser and
Reaction reacts 6h, obtains black gel；
(4) it is deionized water step (3) gel to be put into 150 milliliters of volume ratios：N-butanol=1：In 1 mixed liquor,
80-120W, 30-50KHz ultrasound 2-3h filter, filter cake are washed with deionized to mass conservation；
(5) step (4) filter cake is dried in vacuo 8-10h at 50-80 DEG C, the filter cake after drying is ground, is obtained
Product, that is, graphene coated white carbon nanocomposite.
X-ray diffraction is passed through to the sample of above-mentioned raw materials graphite oxide GO and graphene coated white carbon nanocomposite
Instrument (production of Brooker company of D8 types Germany) is analyzed (see Fig. 1 and Fig. 2), and each parameter is as follows when analysis, CuKαRadiation, pipe electricity
Pressure：40kV, tube current：250mA, 2 θ scanning ranges：
10~90 °, sweep speed：4 °/min, scan mode is continuous scanning, temperature：Room temperature (23 DEG C), relative humidity：
30~40%.
It is the characteristic peak of graphite oxide, this spreads out from fig. 1, it can be seen that occurring an apparent diffraction maximum about at 2 θ=11.1 °
It penetrates peak and belongs to the distance between oxidized graphite flake layer, its spacing 0.794nm is much larger than the interlamellar spacing of graphite.It can from Fig. 2
Go out when graphite oxide is reduced into graphene, graphene about nearby disperse peak occurs in 2 θ=19.26 °, this spreads out with graphite
It is close to penetrate peak position, but diffraction maximum broadens, remitted its fury, this illustrates graphite oxide after laser emission restores, graphene
Structure is kept, and does not agglomerate into graphite again.
Graphene coated white carbon nanocomposite sample is passed through into nano-particle size analysis instrument (NANOPHOX
Particle Size Analysis) it is analyzed (see Fig. 3), test scope：1-10000nm, concentration range：ppm-
70vol%, light source：He-Ne Lasers, wavelength 632.8nm, laser power：10mw, temperature：15-40 DEG C, humidity 20-70% is without cold
It is solidifying.As shown in figure 3, the grain size of the graphene coated white carbon black composite material prepared using graphite oxide as raw material is less than 5nm, thus
It can obtain, be successfully prepared nano level graphene coated white carbon black composite material.
The sample of graphite oxide GO and graphene coated white carbon nanocomposite are produced by Hitachi, Japan
S4800 types scanning electron microscope sem (see Fig. 4) and 120 type transmission electron microscope TEM of Hitachi Libra analyzed (see Fig. 5).Fig. 4 is
The SEM of graphite oxide GO schemes, and graphite oxide GO assembles in lamellar structure in figure；Fig. 5 is that graphene coated white carbon is nano combined
The TEM of material schemes, it can be seen that graphene coated white carbon nanocomposite is successfully prepared.
The invention is not limited in specific implementation modes above-mentioned.The present invention, which expands to, any in the present specification to be disclosed
New feature or any new combination, and disclose any new method or process the step of or any new combination.
Claims (1)
1. a kind of preparation method of graphene coated white carbon nanocomposite, which is characterized in that include the following steps：
(1) graphite oxide GO (0.1-0.5 grams), (1-3 grams) of cyclomethicone are added in 100 ml deionized waters, oxidation
Graphite：Cyclomethicone：Deionized water=0.1-0.5 grams：1-3 grams：100 milliliters, 10min is stirred at room temperature at 200 rpm；
(2) 1 gram of PS-PEG resin is added in step (1) solution, is heated to 60-80 DEG C, constant temperature stirs 3h at 300 rpm；
(3) step (2) solution is cooled to room temperature, imports in Photoreactor, is irradiated and reacts by YLS-2000 laser,
6h is reacted, black gel is obtained；
(4) it is deionized water step (3) gel to be put into 150 milliliters of volume ratios：N-butanol=1：In 1 mixed liquor, in 80-
120W, 30-50KHz ultrasound 2-3h filter, filter cake are washed with deionized to mass conservation；
(5) step (4) filter cake is dried in vacuo 8-10h at 50-80 DEG C, the filter cake after drying is ground, product is obtained
That is graphene coated white carbon nanocomposite.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844761A (en) * | 2010-05-28 | 2010-09-29 | 上海师范大学 | Method of adopting laser radiation for preparing reduction-oxidation graphene |
| CN102343239A (en) * | 2011-05-20 | 2012-02-08 | 四川大学 | Oxidized graphene or graphene/inorganic particle core/shell material and preparation method thereof |
| CN102437320A (en) * | 2011-11-21 | 2012-05-02 | 北京师范大学 | Graphene-coated mesoporous metallic oxide, and preparation method and use thereof |
| CN103571156A (en) * | 2013-09-17 | 2014-02-12 | 广东生益科技股份有限公司 | Thermosetting resin composition and application thereof |
| KR101442418B1 (en) * | 2013-06-19 | 2014-09-22 | 건국대학교 산학협력단 | Method for Isolating Nucleic Acid Using Urea for Disorption of Nucleic Acid from Graphene Oxide |
| CN106517215A (en) * | 2016-10-26 | 2017-03-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of graphene-coated silicon dioxide nanoparticles |
-
2018
- 2018-04-10 CN CN201810314760.8A patent/CN108530952A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844761A (en) * | 2010-05-28 | 2010-09-29 | 上海师范大学 | Method of adopting laser radiation for preparing reduction-oxidation graphene |
| CN102343239A (en) * | 2011-05-20 | 2012-02-08 | 四川大学 | Oxidized graphene or graphene/inorganic particle core/shell material and preparation method thereof |
| CN102437320A (en) * | 2011-11-21 | 2012-05-02 | 北京师范大学 | Graphene-coated mesoporous metallic oxide, and preparation method and use thereof |
| KR101442418B1 (en) * | 2013-06-19 | 2014-09-22 | 건국대학교 산학협력단 | Method for Isolating Nucleic Acid Using Urea for Disorption of Nucleic Acid from Graphene Oxide |
| CN103571156A (en) * | 2013-09-17 | 2014-02-12 | 广东生益科技股份有限公司 | Thermosetting resin composition and application thereof |
| CN106517215A (en) * | 2016-10-26 | 2017-03-22 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of graphene-coated silicon dioxide nanoparticles |
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Application publication date: 20180914 |