CN106220774A - A kind of preparation method of polystyrene/graphene nano composite material - Google Patents
A kind of preparation method of polystyrene/graphene nano composite material Download PDFInfo
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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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- 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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- 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
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Abstract
A kind of preparation method of polystyrene/graphene nano composite material, the invention belongs to Graphene modification field, it is in order to solve easy residual solvent in the existing method preparing polymer/graphene nano composite material, the problem that graphene nanometer sheet disperses inequality in starting monomer.Preparation method: one, graphene nanometer sheet powder body, 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 bulb, then adds initiator and cause St to occur in-situ polymerization to prepare reactant liquor;Three, by reactant liquor implantation glass reactor, stand and discharge bubble, after hardening, obtain PS/ graphene nanocomposite material.Present invention achieves the graphene nanometer sheet uniform and stable dispersion in PS matrix, there is not residual solvent with DMA for dispersing aid, improve glass transition temperature and the electrical conductivity of PS/ graphene nanocomposite material.
Description
Technical field
The invention belongs to Graphene modification field, be specifically related to the preparation method of polymer/graphene nano composite material.
Background technology
Graphene nanocomposite material typically refers to high-molecular organic material or Inorganic Non-metallic Materials and graphene nano
The class new material that sheet is obtained by combination process, due to it, in one aspect or certain several respect has more excellent spy
Property, have broad application prospects in a lot of fields.Graphene nanocomposite material preparation method includes direct blending, in situ
Polymerization, sol-gal process and hydro-thermal method etc., direct blending is directly uniformly to be mixed with other material by graphene nanometer sheet,
It is to prepare graphene nanocomposite material application the earliest, the most easily to realize industrialized method, mechanical blending method, solution can be passed through
Blending method, melt-blending process etc. are embodied as.Owing to graphene nanometer sheet and other material interface bond strength are than relatively low, residual
Solvent be not easy to remove and graphene nanometer sheet easily in other material matrix the problem such as reunion be prepared by direct blending
The subject matter that graphene nano material faces at present.
In-situ polymerization prepares polymer/graphene nano composite material, is first to be evenly spread to by graphene nanometer sheet
In starting monomer, and make monomer molecule be inserted into the interlayer of graphene nanometer sheet as far as possible, then add initiator and cause raw material
Monomer generation polyreaction, obtains polymer/graphene nano composite material.In-situ polymerization ensure that graphene nano
Sheet in the composite dispersed, it it is critical only that starting monomer can dispersed graphene nanometer sheet and being inserted into
Graphene nanometer sheet interlayer.But owing to graphene nanometer sheet is with nonpolar or the low pole starting monomer compatibility is poor, graphite
Alkene nanometer sheet has to pass through after surface processes and its is possible to be dispersed in starting monomer.
Summary of the invention
The invention aims to solve in the existing method preparing polymer/graphene nano composite material the most residual
Staying solvent, graphene nanometer sheet disperses the problem of inequality 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 realizes according to the following steps:
One, graphene nanometer sheet powder body, St (styrene) and dispersing aid are placed in reactor, equal through ultrasonic disperse
Even, obtain graphene nanometer sheet dispersion liquid;
Two, it is transferred to graphene nanometer sheet dispersion liquid to be furnished with in the reaction bulb of condensing tube, agitator and nitrogen inlet, adds
Enter azodiisobutyronitrile, under conditions of stirring, be warming up to 70~90 DEG C, be cooled to 50 DEG C after reaction 0.8~1.2h, add
Dibenzoyl peroxide, is stirred for 1.0~1.5h, obtains reactant liquor;
Three, reactant liquor is fed in glass reactor, stands until bubble-free in reactant liquor, at 40~50 DEG C of water-bath bars
Until reactant liquor hardening under part, obtain PS/ graphene nanocomposite material;
Wherein the dispersing aid described in step one is dimethylaminoethyl acrylate methyl ammonia ethyl ester (DMA), vinyl trimethoxy silicon
Alkane coupling agent or monoalkoxy class titanate coupling agent.
Graphene is modified by the present invention by the method for in-situ polymerization, and improves its dispersive property.The present invention is first
Prepare graphene nanometer sheet dispersion liquid with graphene nanometer sheet powder body, styrene (St), dispersing aid, then add initiator
Styrene (St) is caused to occur in-situ polymerization to obtain PS/ graphene nanocomposite material.Under conditions of dispersing aid, St can
Dispersed graphene nanometer sheet and be 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 PS/ graphene nanocomposite material does not exist residual
Stay Solvent.
The PS/ graphene nanocomposite material that the present invention prepares, it is achieved that graphene nanometer sheet is in PS matrix
Uniform and stable dispersion, improves heat resistance and the antistatic property etc. of PS, makes the glass of PS/ graphene nanocomposite material
Changing transition temperature and improve more than 10 DEG C, the electrical conductivity of PS/ graphene nanocomposite material can reach 7 × 10-5About S/m.
Accompanying drawing explanation
Fig. 1 is the DMA polarizing microscope figure to Graphene/St dispersion liquid peptizaiton in embodiment one;
Fig. 2 is the KH-171 polarizing microscope figure to Graphene/St dispersion liquid peptizaiton in embodiment two;
Fig. 3 is the JTW-101 polarizing microscope figure to Graphene/St dispersion liquid peptizaiton in embodiment three;
Fig. 4 is the JTW-105 polarizing microscope figure to Graphene/St dispersion liquid peptizaiton in embodiment four;
Fig. 5 is the DSC curve figure of the PS/ graphene nanocomposite material that embodiment one obtains, and wherein 1 represents PS, and 2 represent
P (St-DMA), 3 represent PS/ graphene nanocomposite material;
Fig. 6 is the DSC curve figure of the PS/ graphene nanocomposite material that embodiment two obtains, and wherein 1 represents PS, and 2 represent
PS (0.5wt%) Han a small amount of KH-171,3 represent PS/ graphene nanocomposite material;
Fig. 7 is the DSC curve figure of the PS/ graphene nanocomposite material that embodiment three obtains, and wherein 1 represents PS, and 2 represent
PS (0.5wt%) Han a small amount of JTW-101,3 represent PS/ graphene nanocomposite material;
Fig. 8 is the DSC curve figure of the PS/ graphene nanocomposite material that embodiment four obtains, and wherein 1 represents PS, and 2 represent
PS (0.5wt%) Han a small amount of JTW-105,3 represent PS/ graphene nanocomposite material.
Detailed description of the invention
Detailed description of the invention one: the preparation method of present embodiment PS/ graphene nanocomposite material is real according to the following steps
Execute:
One, graphene nanometer sheet powder body, St (styrene) and dispersing aid are placed in reactor, equal through ultrasonic disperse
Even, obtain graphene nanometer sheet dispersion liquid;
Two, it is transferred to graphene nanometer sheet dispersion liquid to be furnished with in the reaction bulb of condensing tube, agitator and nitrogen inlet, adds
Enter azodiisobutyronitrile, under conditions of stirring, be warming up to 70~90 DEG C, be cooled to 50 DEG C after reaction 0.8~1.2h, add
Dibenzoyl peroxide, is stirred for 1.0~1.5h, obtains reactant liquor;
Three, reactant liquor is fed in glass reactor, stands until bubble-free in reactant liquor, at 40~50 DEG C of water-bath bars
Until reactant liquor hardening under part, obtain PS/ graphene nanocomposite material;
Wherein the dispersing aid described in step one 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.
Detailed description of the invention two: the vinyl trimethoxy that present embodiment is described unlike detailed description of the invention one
The model of silane coupler is KH-171.Other step and parameter are identical with detailed description of the invention one.
The methoxy hydrolysis of coupling agent vinyltrimethoxy silane molecule one end that present embodiment uses becomes Si-
OH, can occur chemical reaction to form ehter bond with the-OH of graphenic surface residual, it is achieved coupling agent and the compact siro spinning technology of Graphene;
The vinyl of the coupling agent other end and styrene-compatible, and during ensuing radical copolymerization, realize chemistry even
Connect, make stable being dispersed in St and PS polymeric matrix of graphene uniform.
Detailed description of the invention three: the monoalkoxy class that present embodiment is described unlike detailed description of the invention one or two
The model of titanate coupling agent is JTW-101 or JTW-105.Other step and parameter are identical with detailed description of the invention one or two.
The monoalkoxy hydrolyzable of coupling agent monoalkoxy class titanate esters molecule one end that present embodiment uses becomes
Ti-OH, can occur chemical reaction to form ehter bond with the-OH of graphenic surface residual, it is achieved coupling agent closely connects with Graphene
Connect;The titanate-based of the coupling agent other end and styrene-compatible, make graphene uniform stable be dispersed in St and PS polymer
In matrix.
Detailed description of the invention four: present embodiment unlike one of detailed description of the invention one to three in advance to step one
In St and dimethylaminoethyl acrylate methyl ammonia ethyl ester use decompression distillation method be purified.Other step and parameter are real with concrete
Execute one of mode one to three identical.
Present embodiment is by being purified to remove polymerization inhibitor.
Detailed description of the invention five: described in present embodiment step one unlike one of detailed description of the invention one to four
The mass ratio of graphene nanometer sheet powder body, St and dispersing aid is (0.05~0.1): (10~20): (0.02~0.1).Other
Step and parameter are identical with one of detailed description of the invention one to four.
Detailed description of the invention six: described in present embodiment step 2 unlike one of detailed description of the invention one to five
Azodiisobutyronitrile accounts for the 0.3%~0.8% of graphene nanometer sheet dispersion liquid weight/mass percentage composition.Other step and parameter and tool
One of body embodiment one to five is identical.
Detailed description of the invention seven: present embodiment step 2 unlike one of detailed description of the invention one to six is stirring
Under conditions of be warming up to 75~85 DEG C, reaction 1h after be cooled to 50 DEG C, add dibenzoyl peroxide.Other step and parameter
Identical with one of detailed description of the invention one to six.
Detailed description of the invention eight: present embodiment unlike detailed description of the invention seven step 2 stirring under conditions of
It is warming up to 80 DEG C, is cooled to 50 DEG C after reaction 1h, adds dibenzoyl peroxide.Other step and parameter and specific embodiment party
Formula seven is identical.
Detailed description of the invention nine: peroxide in present embodiment step 2 unlike one of detailed description of the invention one to eight
Change dibenzoyl and account for the 0.03%~0.08% of reactant liquor weight/mass percentage composition.Other step and parameter and detailed description of the invention one
Identical to one of eight.
Detailed description of the invention ten: stone described in present embodiment step one unlike one of detailed description of the invention one to nine
The particle diameter of ink alkene nanometer sheet powder body is 10~60 μm.Other step and parameter are identical with one of detailed description of the invention one to nine.
Embodiment one: the preparation method of the present embodiment PS/ graphene nanocomposite material realizes according to the following steps:
One, by 0.05g graphene nanometer sheet powder body, 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 being furnished with condensing tube, agitator and nitrogen inlet
In, add 0.05g azodiisobutyronitrile, under conditions of stirring, be warming up to 80 DEG C, be cooled to 50 DEG C after reaction 1h, add
0.006g dibenzoyl peroxide, is stirred for 1.5h, obtains reactant liquor;
Three, being fed in teat glass by reactant liquor, influx height is 6cm, stands until bubble-free, glass in reactant liquor
Test tube until reactant liquor hardening, obtains PS/ graphene nanocomposite material under 50 DEG C of water bath condition.
The present embodiment prepares PS/ graphene nanocomposite material, it is achieved that graphene nanometer sheet is in PS matrix
Uniform and stable dispersion, the glass transition temperature of PS/ graphene nanocomposite material is relative to the P (St-DMA) of not graphene-containing
Material improves more than 10 DEG C, and the introducing of Graphene improves the heat resistance of PS;The electrical 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 step one unlike embodiment one is 0.05g dispersing aid vinyl trimethoxy
Base silane coupling agent (KH-171).
The present embodiment prepares PS/ graphene nanocomposite material, it is achieved that graphene nanometer sheet is in PS matrix
Uniform and stable dispersion, the glass transition temperature of PS/ graphene nanocomposite material is relative to containing a small amount of KH-171 (0.5wt%)
PS material improve more than 10 DEG C, 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 step one unlike embodiment one is 0.05g dispersing aid monoalkoxy class titanium
Acid esters coupling agent JTW-101.
Embodiment four: the present embodiment step one unlike embodiment one is 0.05g dispersing aid monoalkoxy class titanium
Acid esters coupling agent JTW-105.
Embodiment three and four prepares PS/ graphene nanocomposite material, it is achieved that graphene nanometer sheet is at 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
(0.5wt%) or JTW-105 (0.5wt%) PS material improve more than 10 DEG C, the introducing of Graphene improves the heat-resisting of PS
Performance;The electrical conductivity of PS/ graphene nanocomposite material that dispersing aid uses JTW-101 or JTW-105 to obtain is 7.35 ×
10-5S/m, has reached the standard of anti-static material.
Dimethylaminoethyl acrylate methyl ammonia ethyl ester (DMA) described in embodiment has commercially available from Shanghai Aladdin biochemical technology share
Limit company.Vinyltrimethoxy silane coupling agent (KH-171) or monoalkoxy class titanate coupling agent (JTW-101, JTW-
105) commercially available from Nanjing through Tian Wei Chemical Co., Ltd..
Claims (10)
1. the preparation method of polystyrene/graphene nano composite material, it is characterised in that be to follow these steps to realize:
One, graphene nanometer sheet powder body, St and dispersing aid are placed in reactor, uniform through ultrasonic disperse, obtain Graphene
Nanometer sheet dispersion liquid;
Two, it is transferred to be furnished with in the reaction bulb of condensing tube, agitator and nitrogen inlet by graphene nanometer sheet dispersion liquid, adds even
Nitrogen bis-isobutyronitrile, is warming up to 70~90 DEG C under conditions of stirring, is cooled to 50 DEG C, adds peroxide after reaction 0.8~1.2h
Change dibenzoyl, be stirred for 1.0~1.5h, obtain reactant liquor;
Three, reactant liquor is fed in glass reactor, stands until bubble-free in reactant liquor, under 40~50 DEG C of water bath condition
Until reactant liquor hardening, obtain PS/ graphene nanocomposite material;
Wherein the dispersing aid described in step one be dimethylaminoethyl acrylate methyl ammonia ethyl ester, vinyltrimethoxy silane coupling agent or
Monoalkoxy class titanate coupling agent.
The preparation method of polystyrene/graphene nano composite material the most according to claim 1, it is characterised in that described
The model of vinyltrimethoxy silane coupling agent be KH-171.
The preparation method of polystyrene/graphene nano composite material the most according to claim 1, it is characterised in that described
The model of monoalkoxy class titanate coupling agent be JTW-101 or JTW-105.
The preparation method of polystyrene/graphene nano composite material the most according to claim 1, it is characterised in that in advance
The method that St in step one and dimethylaminoethyl acrylate methyl ammonia ethyl ester use decompression distillation is purified.
The preparation method of polystyrene/graphene nano composite material the most according to claim 1, it is characterised in that step
The mass ratio of graphene nanometer sheet powder body, St and dispersing aid described in one is (0.05~0.1): (10~20): (0.02~
0.1)。
The preparation method of polystyrene/graphene nano composite material the most 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 weight/mass percentage composition.
The preparation method of polystyrene/graphene nano composite material the most according to claim 1, it is characterised in that step
Two are warming up to 75~85 DEG C under conditions of stirring, be cooled to 50 DEG C, add dibenzoyl peroxide after reaction 1h.
The preparation method of polystyrene/graphene nano composite material the most according to claim 7, it is characterised in that step
Two are warming up to 80 DEG C under conditions of stirring, be cooled to 50 DEG C, add dibenzoyl peroxide after reaction 1h.
The preparation method of polystyrene/graphene nano composite material the most according to claim 1, it is characterised in that step
In two, dibenzoyl peroxide accounts for the 0.03%~0.08% of reactant liquor weight/mass percentage composition.
The preparation method of polystyrene/graphene nano composite material the most according to claim 1, it is characterised in that step
The particle diameter of graphene nanometer sheet powder body described in rapid one is 10~60 μm.
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CN107522961A (en) * | 2017-03-30 | 2017-12-29 | 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 |
CN108084344A (en) * | 2017-12-20 | 2018-05-29 | 中国石油大学(华东) | A kind of preparation method of graphene aqueous liquid dispersion |
CN109627402A (en) * | 2018-12-14 | 2019-04-16 | 江南大学 | A kind of preparation method of polystyrene-based high refractive index nano composite material |
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 |
CN111635471A (en) * | 2020-06-18 | 2020-09-08 | 北京理工大学 | Flame-retardant polystyrene resin and preparation method and application thereof |
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CN113150488A (en) * | 2021-04-20 | 2021-07-23 | 白坤玉 | Clothes hanger with mosquito repelling effect and preparation method thereof |
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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 |
CN108084344A (en) * | 2017-12-20 | 2018-05-29 | 中国石油大学(华东) | A kind of preparation method of graphene aqueous liquid dispersion |
CN109627402A (en) * | 2018-12-14 | 2019-04-16 | 江南大学 | A kind of preparation method of polystyrene-based high refractive index nano composite material |
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 |
CN111635471A (en) * | 2020-06-18 | 2020-09-08 | 北京理工大学 | Flame-retardant polystyrene resin and preparation method and application thereof |
CN113150488A (en) * | 2021-04-20 | 2021-07-23 | 白坤玉 | Clothes hanger with mosquito repelling effect and preparation method thereof |
CN113150488B (en) * | 2021-04-20 | 2022-12-13 | 白坤玉 | Clothes hanger with mosquito repelling effect and preparation method thereof |
CN114130286A (en) * | 2021-12-08 | 2022-03-04 | 安徽威能电源科技有限公司 | Lead powder production stirring device of lead-acid storage battery |
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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