CN110452321A - A kind of preparation method of graphene/benzene composite material - Google Patents
A kind of preparation method of graphene/benzene composite material Download PDFInfo
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- CN110452321A CN110452321A CN201910696856.XA CN201910696856A CN110452321A CN 110452321 A CN110452321 A CN 110452321A CN 201910696856 A CN201910696856 A CN 201910696856A CN 110452321 A CN110452321 A CN 110452321A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F112/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F112/02—Monomers containing only one unsaturated aliphatic radical
- C08F112/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F112/06—Hydrocarbons
- C08F112/08—Styrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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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
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- Medicinal Chemistry (AREA)
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- Carbon And Carbon Compounds (AREA)
Abstract
A kind of preparation method of graphene/benzene composite material, styrene, dispersing agent and water are placed in test bottle, carry out ultrasonic disperse；After the completion of styrene dispersion, graphene solution is slowly added dropwise into system, needs to continue to carry out ultrasound during being added dropwise, continues ultrasonic disperse after completion of dropwise addition；After dispersion, stirring is opened, reaction is warming up to 70-90 DEG C；After temperature is stablized, initiator is added into reaction flask, maintains the temperature at 70-90 DEG C, sustained response 3-5 hours；After polymerization, reaction temperature is reduced to 40-60 DEG C, reducing agent is added；It is warming up to 80-90 DEG C, sustained response 2-3 hours, is then reduced to room temperature, experiment terminates.The preparation method of graphene/poly styrene composite material provided by the present invention, obtained composite material are detected under digital microscope, and the phenomenon that bulky grain reunion does not occur in favorable dispersibility.The present invention has been prepared each phase and has been uniformly dispersed, containing the few high-quality composite material of impurity by simple and effective synthetic method.
Description
Technical field
The invention belongs to field of polymer composite material, are related to a kind of preparation side of graphene/poly styrene composite material
Method.
Background technique
Polystyrene is by styrene monomer polymer free radical addition polymerization as general thermoplastic resin
One of, it is cheap with its, mobility is strong, chemical property is stable, high thermal resistance the advantages that, packaging, building materials, insulation, biology and
The fields such as aircraft industry are widely used in the production and life of the people.But polystyrene matter is crisp, not impact resistance, poor heat resistance, heat
Deformation temperature is low (generally at 78-98 DEG C), is easy burning and smoke is big, belongs to combustible material, therefore application is restricted.
It can satisfy heat management, electronics industry middle-high density, high integration group by the high thermal conductivity plastics of filler of graphene
The requirement of development is filled, development prospect is boundless.Currently, preparing graphene/polymer composites preparation method is all
Using graphene as raw material, prepared using solution mixing method, melt-blending process and emulsion polymerization.But solution mixing method needs make
With organic solvent, post-processing causes adverse effect to environment.Melt-blending process graphene gathers in the polymer and is not easy to disperse,
And it is poor with the interface interaction of polymer.There are partial emulsifier and other auxiliary agents in emulsion polymerization product, purity is not high.
Situ aggregation method can guarantee graphene in the composite evenly dispersed, and key is that starting monomer can be evenly dispersed
Graphene nanometer sheet and it is inserted into graphene nanometer sheet interlayer.
Summary of the invention
It is an object of the invention to solve above-mentioned technical problem, propose a kind of graphene dispersion into inside polystyrene material
Method, the present invention has many advantages, such as that graphene dispersion effect is good, experimental implementation is simple and impurity content is few.
A kind of preparation method of graphene/benzene composite material of the present invention, which is characterized in that the composite wood
Material includes following components and its weight fraction (following material is calculated with dry weight):
Graphene oxide (being based on 100 by styrene dosage): 5-20；
Styrene: 100；
Dispersing agent (being based on 1 by graphene oxide dosage): 4-8；
Initiator (being based on 100 by styrene dosage): 3-8；
Reducing agent (being based on 1 by graphene oxide dosage): 1-10；
Ethyl alcohol (being based on 100 by styrene dosage): 50-100；
Water (being based on 100 by styrene dosage): 100.
A kind of preparation method of graphene/benzene composite material, which is characterized in that the preparation method includes following step
It is rapid:
S1: styrene, dispersing agent and water are placed in test bottle, progress ultrasonic disperse, and ultrasonic time 1-3 hours；
S2: after the completion of styrene dispersion, graphene solution is slowly added dropwise into S1 system, time for adding 10-30 minutes, is added dropwise
It needs to continue to carry out ultrasound in the process, continue ultrasonic disperse 30-60 minutes after completion of dropwise addition；
S3: after dispersion, stirring is opened, reaction is warming up to 70-90 DEG C；
S4: after temperature is stablized, initiator is added into reaction flask, maintains the temperature at 70-90 DEG C, sustained response 3-5 hours；
S5: after polymerization, reaction temperature is reduced to 40-60 DEG C, reducing agent is added；
S6: it is warming up to 80-90 DEG C, sustained response 2-3 hours, is then reduced to room temperature, experiment terminates.
Preferably, the dispersing agent is selected from one of polyvinyl alcohol, tricalcium phosphate.
Preferably, the initiator is selected from one of ammonium persulfate, sodium peroxydisulfate, potassium peroxydisulfate.
Preferably, the reducing agent is selected from one of L-AA, hydrazine hydrate, sodium borohydride.
It is well known that contain a large amount of hydroxyl, carboxyl, epoxy group and carbonyl on graphene oxide molecular structure, this
The polarity of a little oxygen-containing groups is larger, and dispersibility in water is relatively good.The present invention by dispersing agent it is existing by styrene monomer water/
It carries out fully dispersed in ethanol solution, then graphene oxide is being distributed in styrene droplet.Then, it is being uniformly dispersed
As initiator causes the polymerization of styrene in system afterwards.Since graphene oxide itself has extremely strong adsorption capacity,
Styrene monomer can start polymerization reaction in a manner of in-situ polymerization on graphene oxide.Finally, passing through reducing agent again for oxygen
The reduction of graphite alkene, can obtain the uniform graphene/poly styrene composite material of graphene dispersion.
The preparation method of graphene/poly styrene composite material provided by the present invention, obtained composite material is in number
It is detected under word microscope, favorable dispersibility, the phenomenon that bulky grain reunion is not occurred.The present invention passes through simple and effective conjunction
At method, each phase is prepared and has been uniformly dispersed, containing the few high-quality composite material of impurity.
Detailed description of the invention
Fig. 1: the digital microscope photo that graphene disperses in styrene
Specific embodiment:
In order to which further the present invention will be described, presently preferred embodiments of the present invention is now given.But the present invention can be with
Many different forms are realized, however it is not limited to embodiment described herein.On the contrary, purpose of providing these embodiments is
It makes the disclosure of the present invention more thorough and comprehensive.
Embodiment 1
First water 100g, ethyl alcohol 50g are added in reaction flask, stirred evenly, styrene monomer 100g, polyvinyl alcohol is then added
Reaction flask is put into ultrasonic disperse instrument by 20g, and ultrasonic disperse 2 hours.Then, under conditions of ultrasonic disperse, oxygen is slowly added dropwise
Graphite alkene solution 5g(dry weight), after completion of dropwise addition, ultrasonic disperse 30 minutes.Reaction temperature is increased to 70 DEG C, persulfuric acid is added
Ammonium 3g sustained response 5 hours, then reduces reaction temperature to 40 DEG C, L-AA 5g is added, it is small to be warming up to 80 DEG C of reactions 3
When, reaction temperature is finally reduced to room temperature.
Embodiment 2
First water 100g, ethyl alcohol 80g are added in reaction flask, stirred evenly, styrene monomer 100g, polyvinyl alcohol is then added
Reaction flask is put into ultrasonic disperse instrument by 90g, and ultrasonic disperse 1 hour.Then, under conditions of ultrasonic disperse, oxygen is slowly added dropwise
Graphite alkene solution 15g(dry weight), after completion of dropwise addition, ultrasonic disperse 40 minutes.Reaction temperature is increased to 80 DEG C, persulfuric acid is added
Sodium 5g sustained response 4 hours, then reduces reaction temperature to 50 DEG C, hydrazine hydrate 75g is added, it is small to be warming up to 85 DEG C of reactions 2.5
When, reaction temperature is finally reduced to room temperature.
Embodiment 3
First water 100g, ethyl alcohol 100g are added in reaction flask, stirred evenly, styrene monomer 100g, tricresyl phosphate is then added
Reaction flask is put into ultrasonic disperse instrument by calcium 160g, and ultrasonic disperse 3 hours.Then, it under conditions of ultrasonic disperse, slowly drips
Add graphene oxide solution 20g(dry weight), after completion of dropwise addition, ultrasonic disperse 60 minutes.Reaction temperature is increased to 90 DEG C, was added
Potassium sulfate 8g sustained response 3 hours, then reduces reaction temperature to 60 DEG C, sodium borohydride 200g is added, is warming up to 90 DEG C of reactions
3 hours, reaction temperature was finally reduced to room temperature.
The above, is only presently preferred embodiments of the present invention, is not that the invention has other forms of limitations, any ripe
Know the equivalent reality that professional and technical personnel was changed or be modified as equivalent variations possibly also with the technology contents of the disclosure above
Example is applied applied to other fields, but without departing from the technical solutions of the present invention, according to the technical essence of the invention to
Any simple modification, equivalent variations and remodeling, still fall within the protection of technical solution of the present invention made by upper embodiment.
Claims (5)
1. a kind of preparation method of graphene/benzene composite material, which is characterized in that the composite material includes following components
And its weight fraction (following material is calculated with dry weight):
Graphene oxide (being based on 100 by styrene dosage): 5-20；
Styrene: 100；
Dispersing agent (being based on 1 by graphene oxide dosage): 4-8；
Initiator (being based on 100 by styrene dosage): 3-8；
Reducing agent (being based on 1 by graphene oxide dosage): 1-10；
Ethyl alcohol (being based on 100 by styrene dosage): 50-100；
Water (being based on 100 by styrene dosage): 100.
2. a kind of preparation method of graphene/benzene composite material, which is characterized in that the preparation method includes following step
It is rapid:
S1: styrene, dispersing agent and water are placed in test bottle, progress ultrasonic disperse, and ultrasonic time 1-3 hours；
S2: after the completion of styrene dispersion, graphene solution is slowly added dropwise into S1 system, time for adding 10-30 minutes, is added dropwise
It needs to continue to carry out ultrasound in the process, continue ultrasonic disperse 30-60 minutes after completion of dropwise addition；
S3: after dispersion, stirring is opened, reaction is warming up to 70-90 DEG C；
S4: after temperature is stablized, initiator is added into reaction flask, maintains the temperature at 70-90 DEG C, sustained response 3-5 hours；
S5: after polymerization, reaction temperature is reduced to 40-60 DEG C, reducing agent is added；
S6: it is warming up to 80-90 DEG C, sustained response 2-3 hours, is then reduced to room temperature, experiment terminates.
3. a kind of according to claim 1, preparation method of graphene/benzene composite material, which is characterized in that described point
Powder is selected from one of polyvinyl alcohol, tricalcium phosphate.
4. a kind of according to claim 1, preparation method of graphene/benzene composite material, which is characterized in that described to draw
It sends out agent and is selected from one of ammonium persulfate, sodium peroxydisulfate, potassium peroxydisulfate.
5. a kind of according to claim 1, preparation method of graphene/benzene composite material, which is characterized in that described to go back
Former agent is selected from one of L-AA, hydrazine hydrate, sodium borohydride.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113387700A (en) * | 2021-07-06 | 2021-09-14 | 山东利特纳米技术有限公司 | Preparation method of compact and flexible graphene/PS composite heat-conducting film |
Citations (4)
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|---|---|---|---|---|
| CN102827315A (en) * | 2012-08-30 | 2012-12-19 | 合肥工业大学 | Graphene oxide/polystyrene nano composite and preparation method thereof |
| CN106188608A (en) * | 2016-07-25 | 2016-12-07 | 江苏利士德化工有限公司 | A kind of method of the expandable polystyrene particles of preparation of industrialization graphene-containing |
| CN106220774A (en) * | 2016-08-31 | 2016-12-14 | 齐齐哈尔大学 | A kind of preparation method of polystyrene/graphene nano composite material |
| CN106519300A (en) * | 2016-10-31 | 2017-03-22 | 无锡云亭石墨烯技术有限公司 | Preparation and application method for water-based modified graphene slurry |
-
2019
- 2019-07-30 CN CN201910696856.XA patent/CN110452321A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827315A (en) * | 2012-08-30 | 2012-12-19 | 合肥工业大学 | Graphene oxide/polystyrene nano composite and preparation method thereof |
| CN106188608A (en) * | 2016-07-25 | 2016-12-07 | 江苏利士德化工有限公司 | A kind of method of the expandable polystyrene particles of preparation of industrialization graphene-containing |
| CN106220774A (en) * | 2016-08-31 | 2016-12-14 | 齐齐哈尔大学 | A kind of preparation method of polystyrene/graphene nano composite material |
| CN106519300A (en) * | 2016-10-31 | 2017-03-22 | 无锡云亭石墨烯技术有限公司 | Preparation and application method for water-based modified graphene slurry |
Non-Patent Citations (1)
| Title |
|---|
| 严海晨 等: ""分散聚合原位制备聚苯乙烯/氧化石墨烯复合微球"", 《南京工业大学学报（自然科学版）》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113387700A (en) * | 2021-07-06 | 2021-09-14 | 山东利特纳米技术有限公司 | Preparation method of compact and flexible graphene/PS composite heat-conducting film |
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Application publication date: 20191115 |