CN108530954A - A kind of preparation method of graphene coated aluminium hydrate nano composite material - Google Patents
A kind of preparation method of graphene coated aluminium hydrate nano composite material Download PDFInfo
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- CN108530954A CN108530954A CN201810314731.1A CN201810314731A CN108530954A CN 108530954 A CN108530954 A CN 108530954A CN 201810314731 A CN201810314731 A CN 201810314731A CN 108530954 A CN108530954 A CN 108530954A
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- composite material
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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
- C09C1/40—Compounds of aluminium
- C09C1/407—Aluminium oxides or hydroxides
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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
- 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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- C—CHEMISTRY; METALLURGY
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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
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
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- C—CHEMISTRY; METALLURGY
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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
- C09C3/10—Treatment with macromolecular organic 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a kind of preparation methods of graphene coated aluminium hydrate nano composite material, include the following steps：(1) Na is added in graphite oxide4PW11VO40In solution, it is stirred at room temperature；(2) by Al (CH3COO)3It is added in the solution with PS PEG resins, pH, heating, constant temperature stirring is adjusted with NaOH；(3) by laser irradiation and reaction, black emulsion is obtained；(4) emulsion 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 aluminium hydrate nano composite material.The present invention is at low cost, easy, quick, need not use any photochemical catalyst or reducing agent, realize the graphene coated aluminium hydrate nano composite material 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 aluminium hydrate nano composite material.
Background technology
Aluminium hydroxide is a kind of inorganic fire-retarded filler of the good polymer composites materials of application prospect, market dosage ten
Divide huge.But the compatibility of aluminium hydroxide and high molecular material, dispersibility are very poor, and hydroxide is added into high molecular material
Aluminium usually seriously affects the mechanical property and processing performance of material.Therefore, it is necessary to surface modification treatment be carried out to it, to improve it
With the compatibility of high polymer base-material, the mechanical property of packing material is made not decline, or even makes the Some Mechanical Properties of material
It improves.
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 system of graphene coated aluminium hydrate nano composite material
Preparation Method is stablized by graphene coated aluminium hydrate nano composite material performance prepared by this method, is had with high molecular material
There are good compatibility and dispersibility.
Technical scheme is as follows：
A kind of preparation method of graphene coated aluminium hydrate nano composite material, which is characterized in that include the following steps：
(1) by 150 milliliters of Na of (0.1-0.5 grams) addition of graphite oxide GO4PW11VO40In (0.1-0.3M) solution,
10min is stirred at room temperature under 200rpm；
(2) by Al (CH3COO)3(1.0-2.0 grams) and 1 gram of PS-PEG resin are added in step (1) solution, use NaOH
(0.5M) adjusts pH to 9-11, is heated to 60-80 DEG C, and constant temperature stirs 3h at 300 rpm；
(3) step (2) solution is cooled to room temperature, import Photoreactor in, be irradiated by YLS-2000 laser and
Reaction reacts 6h, obtains black emulsion；
(4) it is deionized water step (3) emulsion to be put into 150 milliliters of volume ratios：N-butanol=1：In 1 mixed liquor,
In 80-120W, 30-50KHz ultrasound 2-3h, filters, filter cake is 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 aluminium hydrate nano composite material.
The beneficial effects of the invention are as follows：
It is multiple that the present invention prepares stable graphene coated aluminium hydrate nano by laser radiation method reduction-oxidation graphite
Condensation material, this method is at low cost, easy, quick, need not use any photochemical catalyst or reducing agent, realize large-scale life
Produce the graphene coated aluminium hydrate nano composite material 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 aluminium hydrate nano composite material；
Fig. 3 is the grain size test chart of graphene coated aluminium hydrate nano composite material；
Fig. 4 is the SEM figures of raw material graphite oxide；
Fig. 5 is the TEM figures of graphene coated aluminium hydrate nano composite material.
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 aluminium hydrate nano composite material, includes the following steps：(1) stone will be aoxidized
150 milliliters of Na of (0.1-0.5 grams) addition of black GO4PW11VO40In (0.1-0.3M) solution, 10min is stirred at room temperature at 200 rpm；
(2) by Al (CH3COO)3(1.0-2.0 grams) and 1 gram of PS-PEG resin are added in step (1) solution, use NaOH
(0.5M) adjusts pH to 9-11, is heated to 60-80 DEG C, and constant temperature stirs 3h at 300 rpm；
(3) step (2) solution is cooled to room temperature, import Photoreactor in, be irradiated by YLS-2000 laser and
Reaction reacts 6h, obtains black emulsion；
(4) it is deionized water step (3) emulsion to be put into 150 milliliters of volume ratios：N-butanol=1：In 1 mixed liquor,
In 80-120W, 30-50KHz ultrasound 2-3h, filters, filter cake is 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 aluminium hydrate nano composite material.
Spread out by X-ray to the sample of above-mentioned raw materials graphite oxide GO and graphene coated aluminium hydrate nano composite material
It penetrates instrument (production of Brooker company of D8 types Germany) to be analyzed (see Fig. 1 and Fig. 2), each parameter is as follows when analysis, CuKαRadiation, pipe
Voltage：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 aluminium hydrate nano composite material 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 aluminium hydroxide composite material prepared using graphite oxide as raw material is less than 5nm, by
This can be obtained, and be successfully prepared nano level graphene coated aluminium hydroxide composite material.
The sample of graphite oxide GO and graphene coated aluminium hydrate nano composite material are given birth to by Hitachi, Japan
The S4800 types scanning electron microscope sem (see Fig. 4) and 120 type transmission electron microscope TEM of Hitachi Libra of production are analyzed (see Fig. 5).Fig. 4
Scheme for the SEM of graphite oxide GO, graphite oxide GO assembles in lamellar structure in figure；Fig. 5 is graphene coated aluminium hydrate nano
The TEM of composite material schemes, it can be seen that graphene coated aluminium hydrate nano composite material 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 aluminium hydrate nano composite material, which is characterized in that include the following steps：
(1) by 150 milliliters of Na of (0.1-0.5 grams) addition of graphite oxide GO4PW11VO40In (0.1-0.3M) solution, at 200 rpm
10min is stirred at room temperature；
(2) by Al (CH3COO)3(1.0-2.0 grams) and 1 gram of PS-PEG resin are added in step (1) solution, are adjusted with NaOH (0.5M)
PH to 9-11 is saved, 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 emulsion is obtained；
(4) it is deionized water step (3) emulsion 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 aluminium hydrate nano composite material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109535553A (en) * | 2018-11-09 | 2019-03-29 | 安徽江淮汽车集团股份有限公司 | A kind of flame-proof weather-resisting PP composite material and preparation method |
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|---|---|---|---|---|
| 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 |
| CN103342355A (en) * | 2013-07-09 | 2013-10-09 | 北京化工大学 | Method for preparing graphene and composite material 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 |
| CN103723704A (en) * | 2012-10-15 | 2014-04-16 | 海洋王照明科技股份有限公司 | Graphene/nano-alumina compound and preparation method thereof |
| CN105439129A (en) * | 2015-11-30 | 2016-03-30 | 洛阳绿仁环保设备有限公司 | Method for preparing graphene/white carbon black composite material from potassium feldspar |
| US20160285084A1 (en) * | 2015-03-27 | 2016-09-29 | Qing Fang | Process for mass-producing silicon nanowires and silicon nanowire-graphene hybrid particulates |
-
2018
- 2018-04-10 CN CN201810314731.1A patent/CN108530954A/en not_active Withdrawn
Patent Citations (7)
| 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 |
| CN103723704A (en) * | 2012-10-15 | 2014-04-16 | 海洋王照明科技股份有限公司 | Graphene/nano-alumina compound and preparation method thereof |
| CN103342355A (en) * | 2013-07-09 | 2013-10-09 | 北京化工大学 | Method for preparing graphene and composite material 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 |
| US20160285084A1 (en) * | 2015-03-27 | 2016-09-29 | Qing Fang | Process for mass-producing silicon nanowires and silicon nanowire-graphene hybrid particulates |
| CN105439129A (en) * | 2015-11-30 | 2016-03-30 | 洛阳绿仁环保设备有限公司 | Method for preparing graphene/white carbon black composite material from potassium feldspar |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109535553A (en) * | 2018-11-09 | 2019-03-29 | 安徽江淮汽车集团股份有限公司 | A kind of flame-proof weather-resisting PP composite material and preparation method |
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