CN106220774B - A kind of preparation method of polystyrene/graphene nanocomposite - Google Patents
A kind of preparation method of polystyrene/graphene nanocomposite Download PDFInfo
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- CN106220774B CN106220774B CN201610793500.4A CN201610793500A CN106220774B CN 106220774 B CN106220774 B CN 106220774B CN 201610793500 A CN201610793500 A CN 201610793500A CN 106220774 B CN106220774 B CN 106220774B
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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
- C08F212/00—Copolymers 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
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—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
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
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Abstract
A kind of preparation method of polystyrene/graphene nanocomposite, the invention belongs to the modified fields of graphene,, in order to solve to be easy residual solvent in the existing method for preparing polymer/graphene nano composite material, graphene nanometer sheet disperses uneven problem in starting monomer for it.Preparation method: one, graphene nanometer sheet powder, St and dispersing aid are mixed, ultrasonic disperse is uniform, obtains graphene nanometer sheet dispersion liquid；Two, graphene nanometer sheet dispersion liquid is transferred in reaction flask, then adds initiator initiation St generation in-situ polymerization and prepares reaction solution；Three, discharge bubble in reaction solution implantation glass reactor, will be stood, PS/ graphene nanocomposite material is obtained after hardening.The present invention realizes uniform and stable dispersion of the graphene nanometer sheet in PS matrix, and residual solvent is not present by dispersing aid of DMA, improves the glass transition temperature and conductivity of PS/ graphene nanocomposite material.
Description
Technical field
The invention belongs to the modified fields of graphene, and in particular to the preparation method of polymer/graphene nano composite material.
Background technique
Graphene nanocomposite material typically refers to high-molecular organic material or inorganic non-metallic material and graphene nano
A kind of new material that piece is obtained by combination process, due to it in one aspect or certain several respect have more excellent spy
Property, it has broad application prospects in many fields.Graphene nanocomposite material preparation method includes direct blending, original position
Polymerization, sol-gal process and hydro-thermal method etc., direct blending are directly uniformly to mix graphene nanometer sheet with other materials,
Be prepare graphene nanocomposite material application earliest, most easily realize industrialized method, mechanical blending method, solution can be passed through
The specific implementation such as blending method, melt-blending process.Since graphene nanometer sheet and other materials interface bond strength are relatively low, remain
The problems such as solvent is not easy to remove and graphene nanometer sheet is easy the reunion in other materials matrix is direct blending preparation
The main problem that graphene nano material faces at present.
In-situ polymerization prepares polymer/graphene nano composite material, is to evenly spread to graphene nanometer sheet first
In starting monomer, and monomer molecule is made to be inserted into the interlayer of graphene nanometer sheet as far as possible, then adds initiator and cause raw material
Polymerization reaction occurs for monomer, obtains polymer/graphene nano composite material.In-situ polymerization can guarantee graphene nano
Piece in the composite evenly dispersed, key are that starting monomer evenly dispersed graphene nanometer sheet and can be inserted into
Graphene nanometer sheet interlayer.But since graphene nanometer sheet and nonpolarity or low pole starting monomer compatibility are poor, graphite
Alkene nanometer sheet is possible to be dispersed in starting monomer after having to pass through surface treatment.
Summary of the invention
It is residual the purpose of the present invention is to solve being easy in the existing method for preparing polymer/graphene nano composite material
Solvent is stayed, graphene nanometer sheet disperses uneven problem in starting monomer, and provides a kind of PS/ graphene nanocomposite material
Preparation method.
The preparation method of PS/ graphene nanocomposite material of the present invention is realized according to the following steps:
One, graphene nanometer sheet powder, St (styrene) and dispersing aid are placed in reactor, it is equal through ultrasonic disperse
It is even, obtain graphene nanometer sheet dispersion liquid；
Two, graphene nanometer sheet dispersion liquid is transferred in the reaction flask equipped with condenser pipe, blender and nitrogen inlet, is added
Enter azodiisobutyronitrile, be warming up to 70~90 DEG C under stirring conditions, is cooled to 50 DEG C after reacting 0.8~1.2h, adds
Dibenzoyl peroxide is stirred for 1.0~1.5h, obtains reaction solution；
Three, reaction solution is fed into glass reactor, is stood up to bubble-free in reaction solution, in 40~50 DEG C of water-bath items
Until reaction solution hardens under part, PS/ graphene nanocomposite material is obtained；
Wherein dispersing aid described in step 1 is dimethylaminoethyl acrylate methyl ammonia ethyl ester (DMA), vinyl trimethoxy silicon
Alkane coupling agent or monoalkoxy class titanate coupling agent.
The present invention is modified graphene by the method for in-situ polymerization, and improves its dispersion performance.The present invention is first
Graphene nanometer sheet dispersion liquid is prepared with graphene nanometer sheet powder, styrene (St), dispersing aid, then adds initiator
Cause styrene (St) generation in-situ polymerization and obtains PS/ graphene nanocomposite material.Under conditions of dispersing aid, St can
Evenly dispersed graphene nanometer sheet and it is inserted into graphene nanometer sheet interlayer.Wherein with second comonomer dimethylaminoethyl acrylate methyl ammonia
Ethyl ester (DMA) is that dispersing aid itself can participate in home position polymerization reaction, so there is no residual for PS/ graphene nanocomposite material
Stay Solvent.
The PS/ graphene nanocomposite material that the present invention is prepared realizes graphene nanometer sheet in PS matrix
Uniform and stable dispersion improves heat resistance and antistatic property of PS etc., makes the glass of PS/ graphene nanocomposite material
Change transition temperature and improve 10 DEG C or more, the conductivity of PS/ graphene nanocomposite material can reach 7 × 10-5S/m or so.
Detailed description of the invention
Fig. 1 is DMA in embodiment one to graphene/St dispersion liquid peptizaiton petrographic microscope figure；
Fig. 2 is KH-171 in embodiment two to graphene/St dispersion liquid peptizaiton petrographic microscope figure；
Fig. 3 is JTW-101 in embodiment three to graphene/St dispersion liquid peptizaiton petrographic microscope figure；
Fig. 4 is JTW-105 in example IV to graphene/St dispersion liquid peptizaiton petrographic microscope figure；
Fig. 5 is the DSC curve figure for the PS/ graphene nanocomposite material that embodiment one obtains, wherein 1 represents PS, 2 are represented
P (St-DMA), 3 represent PS/ graphene nanocomposite material；
Fig. 6 is the DSC curve figure for the PS/ graphene nanocomposite material that embodiment two obtains, wherein 1 represents PS, 2 are represented
PS (0.5wt%) containing a small amount of KH-171,3 represent PS/ graphene nanocomposite material；
Fig. 7 is the DSC curve figure for the PS/ graphene nanocomposite material that embodiment three obtains, wherein 1 represents PS, 2 are represented
PS (0.5wt%) containing a small amount of JTW-101,3 represent PS/ graphene nanocomposite material；
Fig. 8 is the DSC curve figure for the PS/ graphene nanocomposite material that example IV obtains, wherein 1 represents PS, 2 are represented
PS (0.5wt%) containing a small amount of JTW-105,3 represent PS/ graphene nanocomposite material.
Specific embodiment
Specific embodiment 1: the preparation method of present embodiment PS/ graphene nanocomposite material is real according to the following steps
It applies:
One, graphene nanometer sheet powder, St (styrene) and dispersing aid are placed in reactor, it is equal through ultrasonic disperse
It is even, obtain graphene nanometer sheet dispersion liquid；
Two, graphene nanometer sheet dispersion liquid is transferred in the reaction flask equipped with condenser pipe, blender and nitrogen inlet, is added
Enter azodiisobutyronitrile, be warming up to 70~90 DEG C under stirring conditions, is cooled to 50 DEG C after reacting 0.8~1.2h, adds
Dibenzoyl peroxide is stirred for 1.0~1.5h, obtains reaction solution；
Three, reaction solution is fed into glass reactor, is stood up to bubble-free in reaction solution, in 40~50 DEG C of water-bath items
Until reaction solution hardens under part, PS/ graphene nanocomposite material is obtained；
Wherein dispersing aid described in step 1 is dimethylaminoethyl acrylate methyl ammonia ethyl ester (DMA), vinyl trimethoxy silicon
Alkane coupling agent or monoalkoxy class titanate coupling agent.
Present embodiment step 2 is reacted under the protection of nitrogen.
Specific embodiment 2: the present embodiment is different from the first embodiment in that the vinyl trimethoxy
The model KH-171 of silane coupling agent.Other steps and parameter are same as the specific embodiment one.
Coupling agent-vinyltrimethoxysilane molecule one end methoxy hydrolysis that present embodiment uses becomes Si-
OH can occur chemical reaction with the remaining-OH of graphene surface and form ehter bond, realize the close connection of coupling agent and graphene；
The vinyl and styrene-compatible of the coupling agent other end, and realize chemistry even during next radical copolymerization
It connects, makes graphene uniform is stable to be dispersed in St and its PS polymeric matrix.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that the monoalkoxy class
The model JTW-101 or JTW-105 of titanate coupling agent.Other steps and parameter are the same as one or two specific embodiments.
Coupling agent-monoalkoxy class metatitanic acid ester molecule one end monoalkoxy hydrolyzable that present embodiment uses becomes
Ti-OH can occur chemical reaction with the remaining-OH of graphene surface and form ehter bond, realize that coupling agent and the close of graphene connect
It connects；The titanate-based and styrene-compatible of the coupling agent other end, make graphene uniform it is stable be dispersed in St and its PS polymer
In matrix.
Specific embodiment 4: in advance to step 1 unlike one of present embodiment and specific embodiment one to three
In St and dimethylaminoethyl acrylate methyl ammonia ethyl ester using vacuum distillation method purified.Other steps and parameter and specific reality
It is identical to apply one of mode one to three.
Present embodiment is by purifying to remove polymerization inhibitor.
Specific embodiment 5: described in step 1 unlike one of present embodiment and specific embodiment one to four
The mass ratio of graphene nanometer sheet powder, St and dispersing aid is (0.05~0.1): (10~20): (0.02~0.1).It is other
Step and parameter are identical as one of specific embodiment one to four.
Specific embodiment 6: described in step 2 unlike one of present embodiment and specific embodiment one to five
Azodiisobutyronitrile accounts for the 0.3%~0.8% of graphene nanometer sheet dispersion liquid mass percentage.Other steps and parameter and tool
One of body embodiment one to five is identical.
Specific embodiment 7: step 2 unlike one of present embodiment and specific embodiment one to six is stirring
Under conditions of be warming up to 75~85 DEG C, be cooled to 50 DEG C after reacting 1h, add dibenzoyl peroxide.Other steps and parameter
It is identical as one of specific embodiment one to six.
Specific embodiment 8: present embodiment and step 2 unlike specific embodiment seven are under stirring conditions
80 DEG C are warming up to, 50 DEG C is cooled to after reacting 1h, adds dibenzoyl peroxide.Other steps and parameter and specific embodiment party
Formula seven is identical.
Specific embodiment 9: peroxide in step 2 unlike one of present embodiment and specific embodiment one to eight
Change dibenzoyl and accounts for the 0.03%~0.08% of reaction solution mass percentage.Other steps and parameter and specific embodiment one
It is identical to one of eight.
Specific embodiment 10: stone described in step 1 unlike one of present embodiment and specific embodiment one to nine
The partial size of black alkene nanometer sheet powder is 10~60 μm.Other steps and parameter are identical as one of specific embodiment one to nine.
Embodiment one: the preparation method of the present embodiment PS/ graphene nanocomposite material is realized according to the following steps:
One, by 0.05g graphene nanometer sheet powder, 10g St (styrene) and 0.05g dispersing aid methacrylic acid two
First ammonia ethyl ester (DMA) is placed in reactor, through ultrasonic disperse 2h, obtains graphene nanometer sheet dispersion liquid；
Two, graphene nanometer sheet dispersion liquid is transferred to the 100mL three-necked bottle equipped with condenser pipe, blender and nitrogen inlet
In, 0.05g azodiisobutyronitrile is added, is warming up to 80 DEG C under stirring conditions, is cooled to 50 DEG C after reacting 1h, adds
0.006g dibenzoyl peroxide, is stirred for 1.5h, obtains reaction solution；
Three, reaction solution is fed into teat glass, influx height 6cm, is stood up to bubble-free, glass in reaction solution
Test tube is under 50 DEG C of water bath conditions until reaction solution hardening, obtains PS/ graphene nanocomposite material.
PS/ graphene nanocomposite material is prepared in the present embodiment, realizes graphene nanometer sheet in PS matrix
Uniform and stable dispersion, P (St-DMA) of the glass transition temperature of PS/ graphene nanocomposite material relative to not containing graphene
Material improves 10 DEG C or more, and the introducing of graphene improves the heat resistance of PS；The conductivity of PS/ graphene nanocomposite material
It is 7.42 × 10-5S/m has reached the standard of anti-static material.
Embodiment two: the present embodiment is 0.05g dispersing aid vinyl trimethoxy from step 1 unlike embodiment one
Base silane coupling agent (KH-171).
PS/ graphene nanocomposite material is prepared in the present embodiment, realizes graphene nanometer sheet in PS matrix
Uniform and stable dispersion, the glass transition temperature of PS/ graphene nanocomposite material is relative to (0.5wt%) containing a small amount of KH-171
PS material improve 10 DEG C or more, the introducing of graphene improves the heat resistance of PS；The electricity of PS/ graphene nanocomposite material
Conductance is 7.38 × 10-5S/m has reached the standard of anti-static material.
Embodiment three: the present embodiment is 0.05g dispersing aid monoalkoxy class titanium from step 1 unlike embodiment one
Acid esters coupling agent JTW-101.
Example IV: the present embodiment is 0.05g dispersing aid monoalkoxy class titanium from step 1 unlike embodiment one
Acid esters coupling agent JTW-105.
PS/ graphene nanocomposite material is prepared in embodiment three and four, realizes graphene nanometer sheet in PS matrix
In uniform and stable dispersion, the glass transition temperature of PS/ graphene nanocomposite material is relative to containing a small amount of JTW-101
The PS material of (0.5wt%) or JTW-105 (0.5wt%) improve 10 DEG C or more, and the introducing of graphene improves the heat-resisting of PS
Performance；The conductivity for the PS/ graphene nanocomposite material that dispersing aid uses JTW-101 or JTW-105 to obtain for 7.35 ×
10-5S/m has reached the standard of anti-static material.
Dimethylaminoethyl acrylate methyl ammonia ethyl ester (DMA) as described in the examples, which is commercially available from Shanghai Aladdin biochemical technology share, to be had
Limit company.Vinyltrimethoxysilane coupling agent (KH-171) or monoalkoxy class titanate coupling agent (JTW-101, JTW-
105) Nanjing is commercially available from through Tian Wei Chemical Co., Ltd..
Claims (7)
1. the preparation method of polystyrene/graphene nanocomposite, it is characterised in that be to follow these steps to realize:
One, graphene nanometer sheet powder, St and dispersing aid are placed in reactor, it is uniform through ultrasonic disperse, obtain graphene
Nanometer sheet dispersion liquid；
Two, graphene nanometer sheet dispersion liquid is transferred in the reaction flask equipped with condenser pipe, blender and nitrogen inlet, is added even
Nitrogen bis-isobutyronitrile is warming up to 70~90 DEG C under stirring conditions, is cooled to 50 DEG C after reacting 0.8~1.2 h, adds peroxide
Change dibenzoyl, is stirred for 1.0 ~ 1.5h, obtains reaction solution；
Three, reaction solution is fed into glass reactor, is stood up to bubble-free in reaction solution, under 40 ~ 50 DEG C of water bath conditions
Until reaction solution hardens, PS/ graphene nanocomposite material is obtained；
Wherein dispersing aid described in step 1 is the model KH-171 or single alcoxyl of vinyltrimethoxysilane coupling agent
The model JTW-101 or JTW-105 of base class titanate coupling agent.
2. the preparation method of polystyrene/graphene nanocomposite according to claim 1, it is characterised in that step
The mass ratio of graphene nanometer sheet powder, St and dispersing aid described in one is (0.05~0.1): (10~20): (0.02~
0.1).
3. the preparation method of polystyrene/graphene nanocomposite according to claim 1, it is characterised in that step
Azodiisobutyronitrile described in two accounts for the 0.3%~0.8% of graphene nanometer sheet dispersion liquid mass percentage.
4. the preparation method of polystyrene/graphene nanocomposite according to claim 1, it is characterised in that step
Two are warming up to 75~85 DEG C under stirring conditions, are cooled to 50 DEG C after reacting 1 h, add dibenzoyl peroxide.
5. the preparation method of polystyrene/graphene nanocomposite according to claim 4, it is characterised in that step
Two are warming up to 80 DEG C under stirring conditions, are cooled to 50 DEG C after reacting 1 h, add dibenzoyl peroxide.
6. the preparation method of polystyrene/graphene nanocomposite according to claim 1, it is characterised in that step
Dibenzoyl peroxide accounts for the 0.03%~0.08% of reaction solution mass percentage in two.
7. the preparation method of polystyrene/graphene nanocomposite according to claim 1, it is characterised in that step
The partial size of the one graphene nanometer sheet powder is 10~60 μm.
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| CN107522961B (en) * | 2017-03-30 | 2019-10-11 | 上海大学 | Polystyrene-based high-heat-conductive composite material and preparation method thereof |
| CN107955260A (en) * | 2017-11-14 | 2018-04-24 | 闽南师范大学 | A kind of graphene dispersion method and application |
| CN108084344B (en) * | 2017-12-20 | 2020-02-21 | 中国石油大学(华东) | Preparation method of graphene aqueous dispersion liquid |
| CN109627402B (en) * | 2018-12-14 | 2021-02-26 | 江南大学 | Preparation method of polystyrene-based high-refractive-index nano composite material |
| US10850304B2 (en) | 2019-01-21 | 2020-12-01 | Guangdong University Of Technology | Method and device for processing microstructure arrays of polystyrene-graphene nanocomposites |
| CN110452321A (en) * | 2019-07-30 | 2019-11-15 | 山东鲁泰控股集团有限公司 | A kind of preparation method of graphene/benzene composite material |
| CN111635471B (en) * | 2020-06-18 | 2021-05-25 | 北京理工大学 | Flame-retardant polystyrene resin and preparation method and application thereof |
| CN113150488B (en) * | 2021-04-20 | 2022-12-13 | 白坤玉 | Clothes hanger with mosquito repelling effect and preparation method thereof |
| CN114130286B (en) * | 2021-12-08 | 2024-03-26 | 安徽威能电源科技有限公司 | Lead powder production stirring device of lead-acid storage battery |
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