CN109337120A - A kind of graphene oxide composite material and preparation method thereof and purposes - Google Patents

A kind of graphene oxide composite material and preparation method thereof and purposes Download PDF

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Publication number
CN109337120A
CN109337120A CN201811146814.0A CN201811146814A CN109337120A CN 109337120 A CN109337120 A CN 109337120A CN 201811146814 A CN201811146814 A CN 201811146814A CN 109337120 A CN109337120 A CN 109337120A
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graphene oxide
composite material
oxide composite
preparation
hydro
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CN109337120B (en
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王雨霏
陈寿
彭晓华
唐武飞
张胜
谷晓昱
王旋
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Shenzhen TONGCHAN Lixing Technology Group Co.,Ltd.
Beijing University of Chemical Technology
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Beijing University of Chemical Technology
Shenzhen Beauty Star Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/10Encapsulated ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • C08K3/042Graphene or derivatives, e.g. graphene oxides

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
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  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Fireproofing Substances (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a kind of graphene oxide composite material and preparation method thereof and purposes.The preparation method of graphene oxide composite material of the invention, comprising the following steps: isopropanol, aluminium isopropoxide and graphene oxide are added in deionized water;Then hydro-thermal reaction is carried out, graphene oxide composite material is obtained.The preparation method of graphene oxide composite material of the present invention can quickly and easily prepare graphene oxide composite material, prepared graphene oxide composite material has the characteristics that flame retarding efficiency is high, it can be used as the fire retardant of polymer material, the damage to polymer material mechanical property can be reduced, and improves the dispersibility of graphene oxide in the polymeric material.

Description

A kind of graphene oxide composite material and preparation method thereof and purposes
Technical field
The present invention relates to field of graphene more particularly to a kind of graphene oxide composite material and preparation method thereof with On the way.
Background technique
The unique Two-dimensional Carbon atom lamellar structure of graphite alkenes material makes it have excellent thermal conductivity, electric conductivity and good Good barrier property can be used as a kind of fire retardant to improve the flame retardant property of polymer material.Aluminium hydroxide, magnesium hydroxide etc. Inorganic compound is used in polymer formulators the work that can also play that fire-retardant, synergistic is fire-retardant, presses down cigarette as common inorganic fire retardants With, and it is non-toxic, non-corrosive, but a large amount of additions are needed, and can damage to polymer material mechanical property larger.
Therefore, the existing technology needs to be improved and developed.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of graphene oxide composite material and its Preparation method and purposes, it is intended to solve inorganic fire retardants in the prior art and need a large amount of additions, and can be to polymer material mechanics The larger problem of performance compromise.
A kind of preparation method of graphene oxide composite material, wherein the following steps are included:
Isopropanol, aluminium isopropoxide and graphene oxide are added in deionized water;
Then hydro-thermal reaction is carried out, graphene oxide composite material is obtained.
The preparation method of the graphene oxide composite material, wherein after the hydro-thermal reaction further include:
The product that hydro-thermal reaction obtains is washed and dried, graphene oxide composite material is obtained.
The preparation method of the graphene oxide composite material, wherein the isopropanol, the aluminium isopropoxide with it is described The mass ratio of graphene oxide is 100-20:80-5:5-0.1.
The preparation method of the graphene oxide composite material, wherein the isopropanol, the aluminium isopropoxide with it is described The mass ratio of graphene oxide is 70-30:25-15:1.
The preparation method of the graphene oxide composite material, wherein the temperature of the hydro-thermal reaction is 100-300 ℃。
The preparation method of the graphene oxide composite material, wherein the time of the hydro-thermal reaction is 6-48h.
The preparation method of the graphene oxide composite material, wherein the temperature of the hydro-thermal reaction is 150-220 ℃。
The preparation method of the graphene oxide composite material, wherein the time of the hydro-thermal reaction is 20-25h.
A kind of graphene oxide composite material, wherein the graphene oxide composite material includes graphene oxide and packet Overlay on the boehmite of the surface of graphene oxide.
A kind of purposes of graphene oxide composite material as described above, wherein use the graphene oxide composite material Make the fire retardant of polymer material.
The utility model has the advantages that the preparation method of graphene oxide composite material of the present invention can be prepared quickly and easily Graphene oxide composite material.Graphene oxide composite material prepared by the present invention has the characteristics that flame retarding efficiency is high, can use Make the fire retardant of polymer material, the damage to polymer material mechanical property can be reduced, and improves graphene oxide poly- Close the dispersibility in object material.
Detailed description of the invention
Fig. 1 is the infrared spectrogram of graphene oxide composite material prepared by the present invention and graphene oxide.
Fig. 2 is the XRD diagram of graphene oxide composite material prepared by the present invention.
Fig. 3 is the scanning electron microscope (SEM) photograph of graphene oxide.
Fig. 4 is the scanning electron microscope (SEM) photograph of graphene oxide composite material prepared by the present invention.
Fig. 5 is another scanning electron microscope (SEM) photograph of graphene oxide composite material prepared by the present invention.
Fig. 6 is another scanning electron microscope (SEM) photograph of graphene oxide composite material prepared by the present invention.
Specific embodiment
The present invention provides a kind of graphene oxide composite material and preparation method thereof and purposes, for make the purpose of the present invention, Technical solution and effect are clearer, clear, and the present invention is described in more detail below.It should be appreciated that described herein Specific embodiment is only used to explain the present invention, is not intended to limit the present invention.
A kind of preparation method of graphene oxide composite material, wherein the following steps are included:
Isopropanol, aluminium isopropoxide and graphene oxide are added in deionized water;
Then hydro-thermal reaction is carried out, graphene oxide composite material is obtained.
The preparation method of graphene oxide composite material of the present invention is that one kind passes through hydro-thermal reaction in graphene oxide The method that surface in situ synthesizes boehmite, obtained graphene oxide composite material are a kind of boehmite claddings Graphene oxide.The present invention can simply and rapidly prepare the graphene oxide (oxygen of boehmite cladding by hydro-thermal method Graphite alkene composite material).The preparation method simple process of graphene oxide composite material of the present invention, is suitble to extensive work Industry production.
Preferably, after the hydro-thermal reaction further include:
The product that hydro-thermal reaction obtains is washed and dried, graphene oxide composite material is obtained.
The present invention passes through the product obtained after hydro-thermal reaction and washs and dry, and can remove the impurity in product, mention The purity of high product.
Preferably, the mass ratio of the isopropanol, the aluminium isopropoxide and the graphene oxide is 100-20:80-5: 5-0.1.The above-mentioned preferred mass ratio of the present invention is conducive to improve yield, and promotes boehmite cladding graphene oxide Covered effect.It is highly preferred that the mass ratio of the isopropanol, the aluminium isopropoxide and the graphene oxide is 70-30:25- 15:1。
Preferably, the temperature of the hydro-thermal reaction is 100-300 DEG C.Hydrothermal temperature preferred for this invention, favorably In the yield and reaction rate that improve product, and then reduce production cost.It is highly preferred that the temperature of the hydro-thermal reaction is 150-220℃。
Preferably, the time of the hydro-thermal reaction is 6-48h.Comparatively, the present invention preferred hydro-thermal reaction when Between be that product formation rate is very fast, and a period of time with higher yields.It is highly preferred that the time of the hydro-thermal reaction is 20-25h。
The present invention provides a kind of graphene oxide composite material, wherein the graphene oxide composite material includes oxidation Graphene and the boehmite for being coated on the surface of graphene oxide.Boehmite has peptization performance good, caking property By force, have the characteristics that specific surface height, Kong Rong great.Graphene has continuous, intensive lamellar structure, when poly- added with graphene When conjunction object material encounters high temperature or open fire, the lamellar structure that graphene is continuous, intensive can prevent oxygen from entering material It is internal.The excessively high heat in part can be transmitted to rapidly the rest part of material by the excellent thermal conductivity of graphene, so that heat Dispersion is rapidly to delay the intensity of a fire to propagate.And the surface area of grapheme material is big, it is easier to which absorption generates in combustion Organic volatile.Graphene oxide is graphene after oxidation processes, and graphite oxide still keeps the layer structure of graphite, but Many oxygroup functional groups are introduced on each layer of graphene monolithic.Graphene oxide composite material of the present invention is a kind of Boehmite and the integrated fire retardant of graphene oxide, can play boehmite and graphene oxide respectively advantage, from And cooperate with the flame retarding efficiency for improving product.
The present invention also provides a kind of purposes of graphene oxide composite material as described above, wherein by the graphite oxide Alkene composite material is used as the fire retardant of polymer material.Graphene oxide composite material of the present invention is a kind of boehmite Graphene oxide is coated, the damage to polymer material mechanical property can be reduced, and improve graphene oxide in polymeric material Dispersibility in material.
Technical solution of the present invention is further described below by specific embodiment.
Embodiment 1
100g isopropanol and 5g aluminium isopropoxide and 5g graphene oxide are added in deionized water;
Then, hydro-thermal reaction 48h under the conditions of 100 DEG C will obtain product washing drying, finally obtain oxidation stone after hydro-thermal reaction Black alkene composite material.
Embodiment 2
100g isopropanol and 80g aluminium isopropoxide and 5g graphene oxide are added in deionized water;
Then, hydro-thermal reaction for 24 hours, will obtain product washing drying, finally obtain oxidation stone under the conditions of 200 DEG C after hydro-thermal reaction Black alkene composite material.
Embodiment 3
20g isopropanol and 5g aluminium isopropoxide and 0.1g graphene oxide are added in deionized water;
Then, hydro-thermal reaction 48h under the conditions of 200 DEG C will obtain product washing drying, finally obtain oxidation stone after hydro-thermal reaction Black alkene composite material.
Embodiment 4
20g isopropanol and 80g aluminium isopropoxide and 4g graphene oxide are added in deionized water;
Then, hydro-thermal reaction 6h under the conditions of 300 DEG C will obtain product washing drying, finally obtain oxidation stone after hydro-thermal reaction Black alkene composite material.
Embodiment 5
60g isopropanol and 5g aluminium isopropoxide and 5g graphene oxide are added in deionized water;
Then, hydro-thermal reaction 6h under the conditions of 300 DEG C will obtain product washing drying, finally obtain oxidation stone after hydro-thermal reaction Black alkene composite material.
Embodiment 6
40g isopropanol and 5g aluminium isopropoxide and 0.1g graphene oxide are added in deionized water;
Then, hydro-thermal reaction 48h under the conditions of 100 DEG C will obtain product washing drying, finally obtain oxidation stone after hydro-thermal reaction Black alkene composite material.
The graphene oxide composite material being prepared is detected.
Fig. 1 be the present invention prepared by graphene oxide composite material (GO-AlOOH) and graphene oxide (GO) it is infrared Spectrogram.As shown in figure 1 shown in the infrared spectroscopy of graphene oxide composite material, in 3281cm-1The sharp absorption peak at place is Al-O- The asymmetric stretching vibration of H group, 3089cm-1The sharp absorption peak at place is Al-O-H group symmetrical stretching vibration;In 1063cm-1 The sharp absorption peak and 1155cm nearby occurred-1The acromion nearby occurred be Al-O-H group symmetric curvature vibration and it is asymmetric Bending vibration, in 729cm-1Nearby occur be Al-O group distortion vibration 1620cm-1With 1464 cm-1Place is respectively to aoxidize The absorption peak of C=C and CO-H in graphene, shows there is boehmite generation on graphene oxide.Furthermore graphite oxide is compared The infrared spectrogram of alkene, in 1720cm-1C=O absorption peak at place disappears substantially, infers in reaction process and reduction reaction, oxygen has occurred The part carbonyl on graphite alkene surface is restored by aluminium isopropoxide.
Fig. 2 is the XRD diagram of graphene oxide composite material prepared by the present invention.From fig. 2 it can be seen that being in 2 θ 13.933,28.332,38.477,49.214 equal positions have the characteristic diffraction peak of boehmite to occur, and baseline is more flat Whole, peak intensity is high, and peak type is sharp, shows the boehmite advantages of good crystallization generated.
Fig. 3 is the scanning electron microscope (SEM) photograph (amplification factor 1k) of graphene oxide, and Fig. 4, Fig. 5, Fig. 6 are respectively that amplification factor is The scanning electron microscope (SEM) photograph of graphene oxide composite material prepared by the present invention under 5k, 30k, 30k.It can by above-mentioned scanning electron microscope (SEM) photograph To find out, compared with untreated graphene oxide, it can clearly be seen that in graphene oxide composite material of the present invention Boehmite is completely coated on surface of graphene oxide.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention Protect range.

Claims (10)

1. a kind of preparation method of graphene oxide composite material, which comprises the following steps:
Isopropanol, aluminium isopropoxide and graphene oxide are added in deionized water;
Then hydro-thermal reaction is carried out, graphene oxide composite material is obtained.
2. the preparation method of graphene oxide composite material according to claim 1, which is characterized in that the hydro-thermal reaction Later further include:
The product that hydro-thermal reaction obtains is washed and dried, graphene oxide composite material is obtained.
3. the preparation method of graphene oxide composite material according to claim 1, which is characterized in that the isopropanol, The mass ratio of the aluminium isopropoxide and the graphene oxide is 100-20:80-5:5-0.1.
4. the preparation method of graphene oxide composite material according to claim 3, which is characterized in that the isopropanol, The mass ratio of the aluminium isopropoxide and the graphene oxide is 70-30:25-15:1.
5. the preparation method of graphene oxide composite material according to claim 1, which is characterized in that the hydro-thermal reaction Temperature be 100-300 DEG C.
6. the preparation method of graphene oxide composite material according to claim 1, which is characterized in that the hydro-thermal reaction Time be 6-48h.
7. the preparation method of graphene oxide composite material according to claim 5, which is characterized in that the hydro-thermal reaction Temperature be 150-220 DEG C.
8. the preparation method of graphene oxide composite material according to claim 6, which is characterized in that the hydro-thermal reaction Time be 20-25h.
9. a kind of graphene oxide composite material, which is characterized in that the graphene oxide composite material includes graphene oxide With the boehmite for being coated on the surface of graphene oxide.
10. a kind of purposes of graphene oxide composite material as claimed in claim 9, which is characterized in that by the graphite oxide Alkene composite material is used as the fire retardant of polymer material.
CN201811146814.0A 2018-09-29 2018-09-29 Graphene oxide composite material and preparation method and application thereof Active CN109337120B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112645373A (en) * 2020-12-17 2021-04-13 安徽理工大学 Gamma-AlOOH/RGO composite wave-absorbing material and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112645373A (en) * 2020-12-17 2021-04-13 安徽理工大学 Gamma-AlOOH/RGO composite wave-absorbing material and preparation method thereof
CN112645373B (en) * 2020-12-17 2023-05-02 安徽理工大学 Gamma-AlOOH/RGO composite wave-absorbing material and preparation method thereof

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