CN106243463B - A kind of preparation method of Polymer/nano graphite flake/silicon dioxide composite material - Google Patents
A kind of preparation method of Polymer/nano graphite flake/silicon dioxide composite material Download PDFInfo
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- CN106243463B CN106243463B CN201610763251.4A CN201610763251A CN106243463B CN 106243463 B CN106243463 B CN 106243463B CN 201610763251 A CN201610763251 A CN 201610763251A CN 106243463 B CN106243463 B CN 106243463B
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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
- C08K7/00—Use of ingredients characterised by shape
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/17—Component parts, details or accessories; Auxiliary operations
- B29C45/76—Measuring, controlling or regulating
- B29C45/77—Measuring, controlling or regulating of velocity or pressure of moulding material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/17—Component parts, details or accessories; Auxiliary operations
- B29C45/76—Measuring, controlling or regulating
- B29C45/78—Measuring, controlling or regulating of temperature
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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
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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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The present invention relates to polymer composites field, the preparation method of specifically a kind of Polymer/nano graphite flake/silicon dioxide composite material.The grain size of graphite is thermally expanded in the raw material that the composite material uses as 0.2 ~ 0.6 mm, Nano-meter SiO_22Grain size be 9-15nm；It is 3 that the preparation method, which is by mass ratio,:10~20：20 ~ 50 thermal expansion graphite, Nano-meter SiO_22With polymer by mechanical agitation melt blending, graphite and Nano-meter SiO_2 are thermally expanded2Interaction Force so that thermally expanding the stripping of graphite original position forms nano graphite flakes, is made Polymer/nano graphite flake/silicon dioxide composite material.The present invention is using different dimensions filler to the difference of Shearing Flow response mode in mechanical agitation, it establishes between filler and interacts, making thermal expansion graphite, stripping forms nano graphite flakes in situ, and the stripping in situ and the Nano-meter SiO_2 that thermally expand graphite may be implemented by such configuration control method2Fine dispersion, while make polymer mechanical property and hot property effectively improve.
Description
Technical field
The present invention relates to polymer composites field, specifically a kind of Polymer/nano graphite flake/silica is compound
The preparation method of material.
Background technology
Polyethylene as a kind of common high molecular material, it is excellent, cheap due to processing performance the advantages that, in reality
It is used widely in life.But polyethylene there are mechanical strengths low, non-refractory itself, it is yielding the shortcomings of, in certain journey
Its application in engineering field is limited on degree.Currently, have numerous studies be related to by different fillers and polyethylene it is compound with
Realize the high performance of polyethylene, Li[Dagang Li,et al.Materials and Design 85(2015)54-59]Deng
People is prepared for polyethylene/charcoal powder composite material, discusses three kinds of different types of charcoal powder (pine charcoal, fruit tree charcoal, bamboo and woods
Charcoal) influence to composite materials property and electric conductivity, when charcoal powder additive amount is 70%, the stretching of composite material
Intensity is carried respectively to 102MPa, 86.8MPa, 72.9MPa, conductivity can reach 3.0 × 10-1S/cm, 3.7 × 10-1S/cm,
3.9×10-1S/cm；Park[Soo-Jin Park,et al.Journal of Industrial and Engineering
Chemistry 21(2015)155-157]Et al. using multi wall carbon pipe improve high density polyethylene (HDPE) capability of electromagnetic shielding, work as carbon
When pipe content is 18wt%, the capability of electromagnetic shielding of prepared composite material can reach 58dB when frequency is 1.4GHZ；Qaiss
[Abou el kacem Qaiss,et al.Mechanics of Materials 98(2016)36-43]Et al. pass through melting
Blend method is prepared for monkey grass/montmorillonite/composite polyethylene material, when the additive amount of two kinds of fillers is 12.5wt%
When, the tensile strength and Young's modulus of composite material can promote 11% and 49%, and the thermal stability of material is also with montmorillonite content
Raising and increase.
The advantages that graphene nanometer sheet is due to its higher Young's modulus, mechanical strength, thermal conductivity, becomes polymerization
The important Na meter Tian Liao [ that object is modified;Zhixiong Huang,et al.Composites:Part A 87(2016)10-22].Mesh
The preceding research that high-performance polymer nanocomposite is prepared using graphene nanometer sheet has many reports.Taheri et al.
[F.Taheri,et al.Materials and Design 66(2015)142-149]It is filled using modified graphene nanometer sheet
It is prepared for epoxy resin/graphite alkene nanocomposite, it is compound when modified graphene nanometer sheet additive amount is 0.5%
15% and 82% has been respectively increased when unmodified graphene is added in stretch modulus and the fracture toughness ratio of material.Yu et al.
[Jaesang Yu,et al.Composites:Part A 69(2015)219-225]Graphene is received by the method for molding
Rice piece is blended with mutual-phenenyl two acid bromide two alcohol ester is prepared for composite material, and is studied its thermal coefficient, and research is found
The graphene nanometer sheet of addition 20wt% can make the thermal coefficient of composite material reach 1.98W/mK.However, graphene price compared with
Height, and easily reuniting in a polymer matrix, thus in actual production using graphene to polymer be modified there are still
It is difficult.
Graphite is thermally expanded to be obtained through high-temperature process by expansible graphite.Expansible graphite intercalator when heated, which decomposes, to be generated
A large amount of expansiveness gases, push graphite layers to open, and make interlayer that physical expansion occur, and are formed internal thin by a large amount of nano-graphites
" graphite worm " structure of piece composition.In ultrasound, shearing etc. under outer field actions, thermally expands and more loose inside graphite pile up piece
Layer structure can be partially stripped, and be formed by several nano graphite flakes formed to tens monolithic layer graphite.
Therefore, graphite is thermally expanded as filler using low cost, is made by introducing shear action during composite processing
Stripping generates nano graphite flakes, it can be achieved that the effective of nano graphite flakes disperses and its to polymer high performance to expanded graphite in situ
Modified purpose.High-performance polyethylene nanocomposite is prepared by above method, operating method is simple, of low cost,
And it is easily achieved large-scale production, the application range to widening polyethylene is of great significance.
Invention content
The present invention provides a kind of Polymer/nano graphite flake/titanium dioxide to prepare composite material with high performance
The preparation method of silicon composite.
The present invention is achieved by the following technical solutions：A kind of Polymer/nano graphite flake/silicon dioxide composite material
Preparation method, the grain size of graphite is thermally expanded in the raw material that the composite material uses as 0.2~0.6mm, Nano-meter SiO_22Grain
Diameter is 9-15nm；It is 3 that the preparation method, which is by mass ratio,:10~20：20~50 thermal expansion graphite, Nano-meter SiO_22With polymer
By mechanical agitation melt blending, graphite and Nano-meter SiO_2 are thermally expanded2Interaction Force to thermally expand graphite stripping shape in situ
At nano graphite flakes, Polymer/nano graphite flake/silicon dioxide composite material (masterbatch) is made.
It is 10~20 that composite material (masterbatch) of the present invention, which introduces in preparation process and thermally expands graphite quality ratio,：3
Nano-meter SiO_22, (graphite, Nano-meter SiO_2 are thermally expanded using different dimensions filler2) to Shearing Flow response mode in mechanical agitation
Difference is established between filler and is interacted, and making thermal expansion graphite, stripping forms nano graphite flakes in situ, while making Nano-meter SiO_22Point
Property is dissipated to improve；Stripping in situ and the Nano-meter SiO_2 of thermal expansion graphite may be implemented by such configuration control method2Good point
It dissipates, while the mechanical property of polymer and hot property is effectively improved.Composite material (masterbatch) of the present invention relative to
Directly use nano graphite flakes, Nano-meter SiO_22With polymer be blended composite material, have it is of low cost, easy to operate, be easy to
Realize large-scale production and the advantages such as nano-particle favorable dispersibility.
Experiments have shown that only in the range of the grain size of raw material of the present invention and mass ratio, thermally expanding graphite just can be former
Position stripping forms nano graphite flakes, while Nano-meter SiO_22Aggregate dispersibility improves；It is according to other grain sizes or mass ratio, then difficult
With realize graphite flake layer be effectively peeled off and Nano-meter SiO_22The fine dispersion of particle.
In order to further dilute masterbatch, reduce filer content, the present invention on the basis of above-mentioned composite material (masterbatch) into
Nano-meter SiO_2 is added in one step2With polymer by melt blending after, be granulated, vacuum drying, obtain polymer content be 88.5~
89.5wt%, nano graphite flakes content are 0.5~1.5wt% and Nano-meter SiO_22Content is the high performance composite of 10wt%
Material.
When it is implemented, it is real in torque rheometer to prepare the mechanical agitation melt blending used in composite material (masterbatch)
It applies, Nano-meter SiO_2 is further added2Implement in double screw extruder with the melt blending after polymer.
Further, the polymer is polyethylene.Certainly, when implementing technical solution of the present invention, it is not limited to
Other thermoplastic macromolecule materials also can be used in polythene material, when specific implementation.
When used polymer is polyethylene, the mechanical agitation melt blending of material is 135 in torque rheometer
~140 DEG C realization.The melt blending of material is realized at 165~190 DEG C in double screw extruder.
Preferably, after granulation vacuum drying temperature be 40~60 DEG C, drying time be 12~for 24 hours.
In order to which the performance to high-performance composite materials measures, be granulated, be dried in vacuo after by injection molding machine 170~
200 DEG C, injection molding under pressure 35-40MPa.
Description of the drawings
Fig. 1 is PE/SiO2And PE/GNPs/SiO2The stereoscan photograph of composite material.As seen from the figure, PE/SiO2It is compound
SiO in material2Dispersibility it is poor, average grain diameter is about 450nm, and thermally expand graphite be added after PE/GNPs/SiO2Composite wood
SiO in material2Size be substantially reduced, average grain diameter is reduced to 300nm or so, illustrates that this preparation method can be realized effectively
SiO2Fine dispersion.
Fig. 2 is PE/GNPs/SiO2The transmission electron microscope photo of composite material.As seen from the figure, nano graphite flakes are dispersed in
In PE matrixes, grain size is 40nm or so, it was demonstrated that this preparation method can make thermal expansion graphite, and stripping generates nano-graphite in situ
Piece.
Fig. 3,4,5 are respectively the stretching, bending, heat resistance curve graph of high-performance composite materials.It can be seen from the figure that
Compared with pure polyethylene, PE/GNPs/nano-SiO2The stretching of composite material, bending, heat resistance obtain different degrees of
It improves.
Specific implementation mode
Embodiment one：
A kind of preparation method of high-performance composite materials includes the following steps：
(1) it is taken out immediately after expansible graphite being thermally expanded 40s in 900 DEG C of Muffle furnace, room temperature cooling；
(2) step (1) obtained product is scattered in absolute ethyl alcohol, 1h is handled in Ultrasonic Cell Disruptor, room temperature is waved
Hair falls absolute ethyl alcohol, and drying is placed into 80 DEG C of vacuum drying ovens for 24 hours after ethyl alcohol volatilization completely；
(3) by the thermal expansion graphite that step (2) obtained grain size is 0.2~0.6mm, with the nanometer that grain size is 9-15nm
SiO2With polyethylene in mass ratio 3:10:30 prepare composite material in torque rheometer, at 190 DEG C, the condition of rotating speed 40rpm
It is lower to carry out masterbatch dilution using parallel dual-screw extruding machine so that nano graphite flakes and nano silicon dioxide and polyethylene in system
Percent content is respectively 0.5wt%, 10wt%, 89.5wt%, dries 12h after granulation in 50 DEG C of vacuum drying ovens, passes through note
High performance PE/GNPs/SiO is made in molding machine injection molding under 200 DEG C, pressure 40MPa2Composite material batten.
Embodiment two：
A kind of preparation method of high-performance composite materials includes the following steps：
(1) it is taken out immediately after expansible graphite being thermally expanded 40s in 900 DEG C of Muffle furnace, room temperature cooling；
(2) step (1) obtained product is scattered in absolute ethyl alcohol, 1h is handled in Ultrasonic Cell Disruptor, room temperature is waved
Hair falls absolute ethyl alcohol, and drying is placed into 80 DEG C of vacuum drying ovens for 24 hours after ethyl alcohol volatilization completely；
(3) by the thermal expansion graphite that step (2) obtained grain size is 0.2~0.6mm, with the nanometer that grain size is 9-15nm
SiO2With polyethylene in mass ratio 3:10:30 prepare composite material in torque rheometer, at 190 DEG C, the condition of rotating speed 40rpm
It is lower to carry out masterbatch dilution using parallel dual-screw extruding machine so that nano graphite flakes and nano silicon dioxide and polyethylene in system
Percent content is respectively 1wt%, 10wt%, 89wt%, dries 12h after granulation in 50 DEG C of vacuum drying ovens, passes through injection molding machine
High performance PE/GNPs/SiO is made in injection molding under 200 DEG C, pressure 40MPa2Composite material batten.
Embodiment three：
A kind of preparation method of high-performance composite materials includes the following steps：
(1) it is taken out immediately after expansible graphite being thermally expanded 40s in 900 DEG C of Muffle furnace, room temperature cooling；
(2) step (1) obtained product is scattered in absolute ethyl alcohol, 1h is handled in Ultrasonic Cell Disruptor, room temperature is waved
Hair falls absolute ethyl alcohol, and drying is placed into 80 DEG C of vacuum drying ovens for 24 hours after ethyl alcohol volatilization completely；
(3) by the thermal expansion graphite that step (2) obtained grain size is 0.2~0.6mm, with the nanometer that grain size is 9-15nm
SiO2With polyethylene in mass ratio 3:10:30 prepare composite material in torque rheometer, at 190 DEG C, the condition of rotating speed 40rpm
It is lower to carry out masterbatch dilution using parallel dual-screw extruding machine so that nano graphite flakes and nano silicon dioxide and polyethylene in system
Percent content is respectively 1.5wt%, 10wt%, 88.5wt%, dries 12h after granulation in 50 DEG C of vacuum drying ovens, passes through note
High performance PE/GNPs/SiO is made in molding machine injection molding under 200 DEG C, pressure 40MPa2Composite material batten.
Example IV：
A kind of preparation method of high-performance composite materials includes the following steps：
(1) it is taken out immediately after expansible graphite being thermally expanded 40s in 900 DEG C of Muffle furnace, room temperature cooling；
(2) step (1) obtained product is scattered in absolute ethyl alcohol, 1h is handled in Ultrasonic Cell Disruptor, room temperature is waved
Hair falls absolute ethyl alcohol, and drying is placed into 80 DEG C of vacuum drying ovens for 24 hours after ethyl alcohol volatilization completely；
(3) by the thermal expansion graphite that step (2) obtained grain size is 0.2~0.6mm, with the nanometer that grain size is 9-15nm
SiO2With polyethylene in mass ratio 3:15:20 prepare composite material in torque rheometer, at 190 DEG C, the condition of rotating speed 40rpm
It is lower to carry out masterbatch dilution using parallel dual-screw extruding machine so that nano graphite flakes and nano silicon dioxide and polyethylene in system
Percent content is respectively 1.5wt%, 10wt%, 88.5wt%, dries 12h after granulation in 50 DEG C of vacuum drying ovens, passes through note
High performance PE/GNPs/SiO is made in molding machine injection molding under 200 DEG C, pressure 40MPa2Composite material batten.
Embodiment five：
A kind of preparation method of high-performance composite materials includes the following steps：
(1) it is taken out immediately after expansible graphite being thermally expanded 40s in 900 DEG C of Muffle furnace, room temperature cooling；
(2) step (1) obtained product is scattered in absolute ethyl alcohol, 1h is handled in Ultrasonic Cell Disruptor, room temperature is waved
Hair falls absolute ethyl alcohol, and drying is placed into 80 DEG C of vacuum drying ovens for 24 hours after ethyl alcohol volatilization completely；
(3) by the thermal expansion graphite that step (2) obtained grain size is 0.2~0.6mm, with the nanometer that grain size is 9-15nm
SiO2With polyethylene in mass ratio 3:20:50 prepare composite material in torque rheometer, at 190 DEG C, the condition of rotating speed 40rpm
It is lower to carry out masterbatch dilution using parallel dual-screw extruding machine so that nano graphite flakes and nano silicon dioxide and polyethylene in system
Percent content is respectively 1.0wt%, 10wt%, 89wt%, dries 12h after granulation in 50 DEG C of vacuum drying ovens, passes through injection molding
High performance PE/GNPs/SiO is made in machine injection molding under 200 DEG C, pressure 40MPa2Composite material batten.
Following table is the composite material stretching obtained by embodiment one to embodiment three, heat resistance contrast table
Claims (1)
1. a kind of preparation method of Polymer/nano graphite flake/silicon dioxide composite material, which is characterized in that the composite wood
The grain size of thermal expansion graphite is 0.2~0.6mm in the raw material that material uses, Nano-meter SiO_22Grain size be 9-15nm；The preparation method
Be by mass ratio be 3:10~20：20~50 thermal expansion graphite, Nano-meter SiO_22With polyethylene by mechanical agitation melt blending,
Thermally expand graphite and Nano-meter SiO_22Interaction Force so that thermally expanding the stripping of graphite original position forms nano graphite flakes, is made poly- second
Alkene/nano graphite flakes/silicon dioxide composite material；
Nano-meter SiO_2 is further added in the polyethylene/nano graphite flakes/silicon dioxide composite material2With polyethylene by melting altogether
It after mixed, is granulated, 40~60 DEG C of vacuum drying 12~for 24 hours, acquisitions polymerized ethylene content is 88.5~89.5wt%, and nano graphite flakes contain
Amount is 0.5~1.5wt% and Nano-meter SiO_22Content is the high-performance composite materials of 10wt%；
The mechanical agitation melt blending is implemented in 135~140 DEG C of torque rheometer, and Nano-meter SiO_2 is further added2
With the melt blending after polyethylene implemented in 165~190 DEG C of double screw extruder.
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| CN107815114A (en) * | 2017-10-11 | 2018-03-20 | 上海阿莱德实业股份有限公司 | A kind of flexible compound graphite-based material for possessing high thermal conductivity energy and preparation method thereof |
| CN111320868B (en) * | 2018-12-17 | 2023-02-28 | 杜邦聚合物有限公司 | Polymer composition with high dielectric constant and low dielectric loss |
| CN112142041A (en) * | 2020-09-30 | 2020-12-29 | 南通大学 | Quartz fiber solid waste SiO2Transformation and utilization method of |
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| CN104292631A (en) * | 2014-09-29 | 2015-01-21 | 苏州博利迈新材料科技有限公司 | Heat-conducting wear-resisting polypropylene resin and preparation method thereof |
| CN105062073A (en) * | 2015-08-11 | 2015-11-18 | 燕山大学 | Preparation method of expanded graphite, glass fiber and polyether sulfone sealing composite material |
| CN105037766A (en) * | 2015-09-18 | 2015-11-11 | 哈尔滨理工大学 | SiO2Preparation method of hollow sphere/graphene oxide/polyimide composite film |
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