CN108314031A - The preparation method of vinyl functionalization graphene - Google Patents
The preparation method of vinyl functionalization graphene Download PDFInfo
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- CN108314031A CN108314031A CN201810304123.2A CN201810304123A CN108314031A CN 108314031 A CN108314031 A CN 108314031A CN 201810304123 A CN201810304123 A CN 201810304123A CN 108314031 A CN108314031 A CN 108314031A
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Abstract
The preparation method of vinyl functionalization graphene, is related to a kind of preparation method of graphite alkene, and this method first step obtains graphene oxide by improving Hummers methods by graphite oxidation, stripping after freeze-drying；Second step, graphene oxide obtained by the first step is dispersed in appropriate solvent, at a certain temperature, silane coupling agent hydrolysis containing vinyl generates Si OH groups and generates Si O C keys with graphite oxide alkene reaction certain time, to obtain vinyl functionalization graphene, ultrasonic disperse, obtains functionalization graphene in a suitable solvent, for product through processing such as filtering, centrifugation, washing, dryings, it is vinyl functionalization graphene to obtain black solid powder.Vinyl functionalization graphene prepared by the present invention has good enhancing, toughening effect, preparation method simple, and condition is easy to control, convenient post-treatment, can have potential using value in resin tooth, toughening or other field.
Description
Technical field
The present invention relates to a kind of preparation methods of graphene, more particularly to a kind of preparation of vinyl functionalization graphene
Method.
Background technology
Graphene is sp2The mono-layer graphite piece for the honeycomb structure that hydridization is constituted, first paper publishing about graphene
In 2004, the two-dimensional material being stabilized at room temperature has been prepared for the first time, and having broken two-dimensional material cannot stablize at room temperature
Therefore existing saying, finder obtain Nobel Prize in physics in 2010.Since graphene has excellent power
It learns, electric property, while there is higher light transmittance, be concerned as the newcomer of carbon family, greatly studied
Person prepares large area in research and prepares single layer or few layer graphene；It is same to prepare graphene powder material in research there are many researcher
Material, wherein oxidation-reduction method are to prepare the most common method of graphene powder at present, and realize that graphene powder is made on a large scale
A standby most potential method.At the same time, Many researchers are in research Graphene derivative, the hybrid material of graphene
Deng the modification of graphene can make it be more applicable for the requirement in a certain field.
The research direction of graphene increasingly tends to two aspects, is on the one hand the system of large area single layer or few layer graphene
It is standby, on the other hand it is the preparation of graphene powder, including the preparation of modified graphene powder.In order to improve or improve graphite
The property and application aspect of alkene, other atoms or functional group are introduced by chemical doping into graphene, can preferably be expanded
Its physics and chemical property, the graphene of vinyl modified have an excellent mechanical performance, electric conductivity, mechanical property and fire-retardant
Performance.
Invention content
The purpose of the present invention is to provide a kind of preparation method of vinyl functionalization graphene, this method passes through improvement
Graphite oxidation, stripping are obtained graphene oxide by Hummers methods after freeze-drying；Silane coupling agent hydrolysis containing vinyl generates Si-
OH groups generate Si-O-C keys with graphite oxide alkene reaction certain time, to obtain vinyl functionalization graphene, the present invention
The vinyl functionalization graphene of preparation has good enhancing, toughening effect, makes it in resin tooth, toughening or other field
In have potential using value.
The purpose of the present invention is what is be achieved through the following technical solutions：
The preparation method of vinyl functionalization graphene, the method includes following preparation process：
The preparation method of the vinyl functionalization graphene is that two steps carry out, the first step, and graphite is passed through modified Hummers
Method prepares graphene oxide；Second step in a suitable solvent by graphene oxide dispersion is reacted with the compound containing vinyl
Several hours, product obtain black solid powder through centrifugation, washing, drying process；
In the first step synthesizes graphene oxide, persulfate used is sodium peroxydisulfate, potassium peroxydisulfate, over cure in preoxidation process
Any one or a few mixture in sour ammonium；Reaction temperature is controlled at 80 DEG C；Reaction time is 3-6h；Prepare graphite oxide
Cold stage need to control system temperature at 15 DEG C hereinafter, control temperature is needed to be less than 30 DEG C in dilution during alkene；
In second step, solvent for use is water or any one of methanol, ethyl alcohol, THF, DMF or several and water mixture；
In second step, reaction temperature controls between 40-60 DEG C, reaction time 6-8h；KH-570 silane coupling agents, A-151 silicon
The ratio of the reagents containing vinyl and graphene oxide such as alkane coupling agent, A-171 silane coupling agents and A-172 silane coupling agents
5:1-10:1；Cleaning solvent is water and uses freeze-drying.
The preparation method of the vinyl functionalization graphene, the vinyl functionalization prepared according to the method described above
Graphene-structured is as follows：
。
Advantages of the present invention is with effect：
1, the preparation method of vinyl functionalization graphene provided by the invention is simple, and equipment requirement is low, and raw material is easy to get, and can be used for
In terms of material modification.
2, preparation method provided by the invention is simple, and condition is easy to control, convenient post-treatment.
3, vinyl functionalization graphene prepared by the present invention has better later use to be worth, and can be used for obtaining and contains stone
The high polymer of black alkene.
4, vinyl functionalization graphene prepared by the present invention is black solid powder, has good enhancing, toughening effect
Fruit, preparation method are simple, and condition is easy to control, convenient post-treatment.The present invention is directed to synthesis of vinyl functionalization graphenes, make it
There can be potential using value in resin tooth, toughening or other field.
Specific implementation mode
The following describes the present invention in detail with reference to examples.
Embodiment 1：
The first step：The 30ml concentrated sulfuric acids are added into the 250ml there-necked flasks equipped with reflux condensing tube, thermometer and magneton, are added
10g graphite is added in 8.5g ammonium persulfates, 8.5g phosphorus pentoxides after being heated to 80 DEG C, insulation reaction 3.5h is diluted with water to 1L
Afterwards, it filters, wash to PH ≈ 7, be dried overnight to obtain pre-oxidation graphite for 80 DEG C in baking oven；By the 375ml concentrated sulfuric acids, gained and oxygen
Graphite uniformly mixes under condition of ice bath, slowly by 40gKMnO4It is added in mixed liquor, during which ensures that temperature is less than 15 DEG C,
By warming-in-water to 35 DEG C, insulation reaction 2h after finishing, gained mixed liquor is diluted with water to 3L under condition of ice bath, ensures temperature
Less than 30 DEG C, H is added2O260ml, system are orange solution, remove supernatant after standing overnight, and are washed 3 times with 5% dilute hydrochloric acid,
After being washed with distilled water 3 times, water adds system mixed liquor to be 2L, is ultrasonically treated 5h, the graphene oxide after freeze-drying.
Second step：0.5g graphene oxides are weighed, the graphene oxide water of 10mg/ml is obtained after distilled water 50ml, ultrasonic 1h
Solution is transferred into 250ml three-necked flasks, addition 1gKH-570 silane coupling agents, and insulation reaction 6h at 40 DEG C is down to room
Centrifuge washing is carried out after temperature, is about washed with distilled water 3-5 times, black powder is obtained after freeze-drying, is vinyl functionalization
Graphene.
Embodiment 2：
The first step：With embodiment 1.
Second step：Weigh 0.5g graphene oxides, distilled water 25ml, after ethyl alcohol 75ml, ultrasonic 1h 5mg/ml oxidation
Graphene ethanol water is transferred into 250ml three-necked flasks, and 1gKH-570 silane coupling agents are added, are kept the temperature at 40 DEG C
6h is reacted, carry out centrifuge washing is cooled to room temperature, is about washed with distilled water 3-5 times, black powder is obtained after freeze-drying, be
Vinyl functionalization graphene.
Embodiment 3：
The first step：With embodiment 1.
Second step：0.5g graphene oxides are weighed, the graphene oxide water of 10mg/ml is obtained after distilled water 50ml, ultrasonic 1h
Solution is transferred into 250ml three-necked flasks, addition 1g A-172 silane coupling agents, and insulation reaction 6h at 40 DEG C is down to room
Centrifuge washing is carried out after temperature, is about washed with distilled water 3-5 times, black powder is obtained after freeze-drying, is vinyl functionalization
Graphene.
Embodiment 4：
The first step：With embodiment 1.
Second step：0.5g graphene oxides are weighed, the graphene oxide water of 10mg/ml is obtained after distilled water 50ml, ultrasonic 1h
Solution is transferred into 250ml three-necked flasks, addition 1g A-151 silane coupling agents, and insulation reaction 6h at 40 DEG C is down to room
Centrifuge washing is carried out after temperature, is about washed with distilled water 3-5 times, black powder is obtained after freeze-drying, is vinyl functionalization
Graphene.
Embodiment 5：
The first step：With embodiment 1.
Second step：0.5g graphene oxides are weighed, the graphene oxide water of 10mg/ml is obtained after distilled water 50ml, ultrasonic 1h
Solution is transferred into 250ml three-necked flasks, addition 1g A-171 silane coupling agents, and insulation reaction 6h at 40 DEG C is down to room
Centrifuge washing is carried out after temperature, is about washed with distilled water 3-5 times, black powder is obtained after freeze-drying, is vinyl functionalization
Graphene.
Claims (2)
1. the preparation method of vinyl functionalization graphene, which is characterized in that the method includes following preparation process：
The preparation method of the vinyl functionalization graphene is that two steps carry out, the first step, and graphite is passed through modified Hummers
Method prepares graphene oxide；Second step in a suitable solvent by graphene oxide dispersion is reacted with the compound containing vinyl
Several hours, product obtain black solid powder through centrifugation, washing, drying process；
In the first step synthesizes graphene oxide, persulfate used is sodium peroxydisulfate, potassium peroxydisulfate, over cure in preoxidation process
Any one or a few mixture in sour ammonium；Reaction temperature is controlled at 80 DEG C；Reaction time is 3-6h；Prepare graphite oxide
Cold stage need to control system temperature at 15 DEG C hereinafter, control temperature is needed to be less than 30 DEG C in dilution during alkene；
In second step, solvent for use is water or any one of methanol, ethyl alcohol, THF, DMF or several and water mixture；
In second step, reaction temperature controls between 40-60 DEG C, reaction time 6-8h；KH-570 silane coupling agents, A-151 silicon
The ratio of the reagents containing vinyl and graphene oxide such as alkane coupling agent, A-171 silane coupling agents and A-172 silane coupling agents
5:1-10:1；Cleaning solvent is water and uses freeze-drying.
2. the preparation method of vinyl functionalization graphene according to claim 1, which is characterized in that described according to above-mentioned
Vinyl functionalization graphene structure prepared by method is as follows：
。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109930381A (en) * | 2019-03-14 | 2019-06-25 | 福建省银河服饰有限公司 | A kind of preparation method of the hydrophilic washable fabric finishing agent of antibacterial |
| CN110218284A (en) * | 2019-05-16 | 2019-09-10 | 国家纳米科学中心 | A kind of preparation method and quartz crystal oscillator piece preparation method of graphene-based polymer |
| US20230026484A1 (en) * | 2021-07-22 | 2023-01-26 | Zhejiang Normal University | Vinyl-modified nanofillers as interfacial compatibilizers and method for producing compatibilized polymer blends |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109930381A (en) * | 2019-03-14 | 2019-06-25 | 福建省银河服饰有限公司 | A kind of preparation method of the hydrophilic washable fabric finishing agent of antibacterial |
| CN109930381B (en) * | 2019-03-14 | 2021-04-13 | 福建省银河服饰有限公司 | Preparation method of antibacterial hydrophilic washable fabric finishing agent |
| CN110218284A (en) * | 2019-05-16 | 2019-09-10 | 国家纳米科学中心 | A kind of preparation method and quartz crystal oscillator piece preparation method of graphene-based polymer |
| CN110218284B (en) * | 2019-05-16 | 2022-09-23 | 国家纳米科学中心 | Preparation method of graphene-based polymer and preparation method of quartz crystal oscillator plate |
| US20230026484A1 (en) * | 2021-07-22 | 2023-01-26 | Zhejiang Normal University | Vinyl-modified nanofillers as interfacial compatibilizers and method for producing compatibilized polymer blends |
| US12012502B2 (en) * | 2021-07-22 | 2024-06-18 | Zhejiang Normal University | Vinyl-modified nanofillers as interfacial compatibilizers and method for producing compatibilized polymer blends |
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