CN112442219A - Very low density polyethylene/carbon nano tube composite material and preparation method thereof - Google Patents
Very low density polyethylene/carbon nano tube composite material and preparation method thereof Download PDFInfo
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- CN112442219A CN112442219A CN201910799147.4A CN201910799147A CN112442219A CN 112442219 A CN112442219 A CN 112442219A CN 201910799147 A CN201910799147 A CN 201910799147A CN 112442219 A CN112442219 A CN 112442219A
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- 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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- C08K3/041—Carbon nanotubes
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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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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- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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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
- C08K2201/006—Additives being defined by their surface area
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a very low density polyethylene/carbon nanotube composite material prepared by a melt blending method, which is prepared from the following raw materials in parts by weight: 0.01-0.05 part of carbon nano tube and 99.95-99.99 parts of very low density polyethylene. The preparation method is that the dried carbon nano tube and the polyethylene with extremely low density are directly melted and blended to prepare the polyethylene nano composite material. The proper amount of carbon nano tubes are added into the ultra-low density polyethylene matrix to play the effects of strengthening and toughening and improving the heat resistance of the ultra-low density polyethylene matrix. The polyethylene with high strength, high toughness and high thermal stability is successfully prepared, and the application range of the polyethylene is widened.
Description
Technical Field
The invention relates to a melt blending ultra-low density polyethylene/carbon nano tube composite material and a preparation method thereof.
Technical Field
Japanese chemist Iijima discovered carbon nanotubes in 1991, which are characterized by a helical tubular structure formed by a graphite sheet wound around a central axis, and the two ends of the tube are sealed by a pentagonal hemispherical mesh. Each carbon atom in the carbon nano tube is connected with three adjacent carbon atoms to form a hexagonal grid structure, but the hexagonal grid structure in the carbon nano tube generally generates certain bending to form a space topological structure, so that the space topological structure is sp2Mainly hybridized, also containing sp3Hybridization is carried out.
The carbon nano tube is used as a one-dimensional nano material, has light weight, perfect connection of a hexagonal structure and a plurality of abnormal mechanical, electrical and chemical properties. In recent years, the extensive application prospect of the carbon nano-tube and the nano-material is continuously shown along with the research of the carbon nano-tube and the nano-material.
Carbon nanotubes, also known as buckytubes, are one-dimensional quantum materials with a special structure (radial dimension is nanometer magnitude, axial dimension is micrometer magnitude, both ends of the tube are basically sealed). Carbon nanotubes are coaxial circular tubes consisting of several to tens of layers of carbon atoms arranged in a hexagonal pattern. The layers are maintained at a fixed distance of about 0.34nm, with a diameter of typically 2-20 nm. And the carbon hexagons can be divided into three types, namely a zigzag type, an armchair type and a spiral type, according to different orientations of the carbon hexagons in the axial direction. Wherein the helical carbon nanotubes have chirality, and the zigzag and armchair carbon nanotubes have no chirality.
Carbon nanotubes are generally classified into single-walled carbon nanotubes and multi-walled carbon nanotubes. The length of the single-wall carbon nano tube can reach dozens of micrometers, the diameter of the single-wall carbon nano tube is between a few tenths of nanometers and a few nanometers, the length of the multi-wall carbon nano tube can reach a few millimeters, the diameter of the multi-wall carbon nano tube is between a few nanometers and a dozen nanometers, and the interlayer spacing of graphite is kept constant and is generally about 0.34 nm. The carbon nanotube is formed by curling a graphite sheet around a central axis, and the properties of the carbon nanotube are different due to different structures obtained by different curling modes. When the carbon nanotube is curled, an included angle, that is, a helical angle (as in formula 1) may occur between the axial direction of the nanotube in the graphite sheet layer and the hexagonal grid which is kept unchanged.
Carbon nanotubes can exhibit both semiconducting and metallic properties with varying diameters and helix angles: when (n-m) is an integral multiple of 3, it exhibits metallic properties, whereas it exhibits semiconducting properties, and thus the carbon nanotube has excellent properties due to its unique structure. The carbon nano tube has ideal elasticity and extremely high mechanical strength, can bear huge axial tension and huge radial deformation, has the tensile strength of 50-200 GPa which is 100 times that of steel, has the bending strength of 14.2GPa and the elastic modulus of 1.8TPa which is equivalent to that of diamond and is about 5 times that of steel, and has the density of only 1/6 times that of steel.
In addition, carbon nanotubes have high thermal and chemical stability, excellent thermal conductivity, superconducting properties, optical properties, and the like, and have attracted great attention, and their applications have been directed to many aspects, such as composite materials, nanoelectronic devices, catalyst carriers, electrode materials, hydrogen storage materials, and the like. The carbon nanotube can exhibit its elasticity through volume change, and thus can bear more than 40% of tensile strain without exhibiting plastic deformation, brittle behavior or bond fracture, so that when applied to a composite material, the carbon nanotube can be utilized to greatly absorb energy, and the excellent mechanics of strength and toughness are enhanced, so that the carbon nanotube becomes the most promising research hotspot in the field of composite materials.
One of five synthetic resins of Polyethylene (PE) is the resin with the largest output and the largest import quantity in the synthetic resins in China, and the polyethylene is mainly divided into four types of Linear Low Density Polyethylene (LLDPE), Low Density Polyethylene (LDPE), Very Low Density Polyethylene (VLDPE) and High Density Polyethylene (HDPE). The material has the advantages of no odor, no toxicity, easy processing, light weight, chemical corrosion resistance, good electrical insulation, low price and the like, thereby being widely applied to the fields of household appliances, buildings, chemical engineering, packaging, light industry and the like and becoming a material which can not be lacked in daily life.
The Very Low Density Polyethylene (VLDPE) is fourth-generation polyethylene, more than the conventional amount of alpha olefin comonomer (such as butene, hexene, octene and the like) is added in the polymerization process, and the density range is widened to 0.880-0.915 g/cm3The ultra-low density polyethylene has the excellent characteristics of high flexibility, wide temperature use range, excellent puncture resistance, tear resistance, environmental stress crack resistance, no toxicity, no odor and the like, and is widely applied to the fields of films, medical hoses, foaming, wires and cables, injection molding and blow molding, medical and food packaging and the like.
Although very low density polyethylene contains many advantages, its poor strength and stiffness, poor heat resistance, and severe creep under stress, limit its entry into some important markets. In order to expand the application range of the very low density polyethylene, the very low density polyethylene must be modified, and because the carbon nano tube has super strong mechanical property and excellent thermal stability, the thermal stability, rigidity and toughness of the polyethylene can be improved by melt blending the very low density polyethylene and the carbon nano tube.
However, how to apply the carbon nano tube to the ultra-low density polyethylene material to fully exert the super strong mechanical property and the excellent thermal stability of the carbon nano tube so as to prepare the ultra-low density polyethylene nano composite material with high thermal stability, high toughness and high rigidity becomes a technical problem to be solved in the field.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the ultra-low density polyethylene/carbon nanotube composite material with obviously improved thermal performance, rigidity and toughness and the preparation method thereof.
Firstly, the invention provides a very low density polyethylene/carbon nanotube composite material, which comprises the following components in percentage by weight:
99.95 to 99.99 weight portions of very low density polyethylene,
0.01-0.05 weight part of carbon nano tube.
Preferably, the very low density polyethylene/carbon nanotube composite material provided by the invention comprises the following components in parts by weight:
99.95 parts by weight of very low density polyethylene,
0.05 part by weight of carbon nanotubes.
Preferably, the very low density polyethylene/carbon nanotube composite material provided by the invention has a melt flow rate of 0.8-1.0g/10min and a density of 0.880-0.915 g/cm3。
Preferably, the very low density polyethylene/carbon nanotube composite material provided by the invention is characterized in that the carbon nanotube has an outer diameter of 20-30nm, a length of 10-30 μm and a density of 2.1g/m3Surface area greater than 110m2/g。
The invention further provides a preparation method of the very-low-density polyethylene/carbon nanotube composite material, which comprises the following steps of:
(1) heat treatment of the carbon nano tube: weighing a proper amount of carbon nano tubes, putting the carbon nano tubes into an oven, and placing the carbon nano tubes at a temperature of between 80 and 100 ℃ for constant weight so as to remove water absorbed in the carbon nano tubes;
(2) mixing the very low density polyethylene and the carbon nano tubes subjected to heat treatment in the step (1) in a high-speed mixer for 3-5min, wherein the mass ratio of the very low density polyethylene to the carbon nano tubes is 99.95-99.99: 0.01-0.05;
(3) and (3) performing extrusion granulation in a double-screw extruder at the rotating speed of 55-550rpm and the temperature of 160-190 ℃ to obtain the very-low-density polyethylene/carbon nano tube composite material.
Preferably, the preparation method of the very low density polyethylene/carbon nanotube composite material provided by the invention is that the mass ratio of the very low density polyethylene to the carbon nanotube is 99.95: 0.05.
preferably, the preparation method of the very low density polyethylene/carbon nanotube composite material provided by the invention is characterized in that the melt flow rate of the very low density polyethylene polymer is 0.8-1.0g/10min, and the density is 0.880-0.915 g/cm3。
Preferably, the preparation method of the very low density polyethylene/carbon nanotube composite material provided by the invention is characterized in that the outer diameter of the carbon nanotube is 20-30nm, the length of the carbon nanotube is 10-30 μm, and the density of the carbon nanotube is 2.1-2.5g/m3Surface area greater than 110m2/g。
The specific operation of the present invention according to an embodiment of the present invention can be described in detail as follows:
the invention adopts the technical scheme that the ultra-low density polyethylene/carbon nano tube composite material is prepared from the following components in parts by weight:
99.95 to 99.99 weight portions of very low density polyethylene,
0.05-0.01 weight part of carbon nano tube.
Preferably, the very low density polyethylene/carbon nanotube composite material provided by the invention is prepared from the following components in parts by weight:
99.95 parts by weight of polyethylene,
0.05 part by weight of carbon nanotubes.
The invention also provides a preparation method of the ultra-low density polyethylene/carbon nano tube composite material, which comprises the following specific steps:
(1) firstly, the carbon nano-tube nano-particles are subjected to heat treatment, namely, a proper amount of carbon nano-tubes are weighed and put into an oven, and the constant weight is placed at the temperature of 80-100 ℃ to remove water absorbed in the carbon nano-tubes;
(2) then mixing the ultra-low density polyethylene and the carbon nano tube after the heat treatment for 3-5min in a high-speed mixer according to the formula proportion;
(3) the ultra-low density polyethylene/carbon nano tube composite material can be obtained under the conditions that the extrusion granulation rotating speed is 55-550rpm and the temperature is 160-190 ℃ in a double-screw extruder.
In conclusion, the invention has the following advantages:
1. the invention firstly adopts the mixing of the carbon nano tube and the ultra-low density polyethylene to improve the heat resistance, the toughness and the rigidity of the polyethylene, the carbon nano tube has super strong mechanical property and excellent thermal stability, after the carbon nano tube is added, the carbon nano tube plays a role of energy storage, the carbon nano tube and the low density polyethylene generate a stronger physical cross-linking point role to limit the decomposition of the ultra-low density polyethylene, the carbon nano tube plays a role of a nucleating agent, and the carbon nano tube can enter the defects of the ultra-low density polyethylene matrix to change the stress concentration phenomenon of the matrix, thereby playing the effects of strengthening, toughening and improving the heat resistance.
2. In addition, the invention adopts a melt blending method to simply and rapidly prepare the ultra-low density polyethylene/carbon nano tube composite material with high thermal stability, high strength and high toughness.
Drawings
FIG. 1 is a flow chart of the preparation of very low density polyethylene/carbon nanotube composite
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
In the present invention, the type of the very low density polyethylene is not particularly limited, but very low density polyethylene to which an alpha-olefin is added is preferably used, and the melt flow rate of the very low density polyethylene polymer is preferably 0.8 to 1.0g/10min, and the density is preferably 0.880 to 0.915g/cm3. The amount of addition is not particularly limited, and it is preferably 99.95 to 99.99 parts by weight.
In the present invention, the kind of the carbon nanotube is not particularly limited, but the carbon nanotube preferably has an outer diameter of 20 to 30nm, a length of 10 to 30 μm and a density of 2.1 to 2.5g/m3Surface area greater than 110m2(ii) in terms of/g. The amount of addition is not particularly limited, and it is preferably 0.01 to 0.05 parts by weight.
Example 1
(1) Firstly, the carbon nano-particle is subjected to heat treatment, namely 0.25g of carbon nano-particle is weighed and put into an oven, and the carbon nano-particle is placed at the temperature of 100 ℃ for constant weight; to remove the water absorbed in the carbon nano tube;
(2) then 99.99 parts by weight of very low density polyethylene and 0.01 part by weight of the carbon nano tube after the heat treatment are mixed for 5min in a high-speed mixer;
(3) the ultra-low density polyethylene/carbon nano tube composite material can be obtained under the conditions that the extrusion granulation rotating speed is 55rpm and the temperature is 190 ℃ in a double-screw extruder.
Example 2
(1) Firstly, the carbon nano-tube nano-particles are subjected to heat treatment, namely 0.5g of carbon nano-tube is weighed and put into an oven, and the carbon nano-tube is placed at the temperature of 100 ℃ for constant weight; to remove the water absorbed in the carbon nano tube;
(2) then 99.98 weight parts of very low density polyethylene and 0.02 weight part of the carbon nano tube after the heat treatment are mixed for 3min in a high-speed mixer;
(3) the ultra-low density polyethylene/carbon nano tube composite material can be obtained under the conditions that the extrusion granulation rotating speed is 550rPm and the temperature is 160 ℃ in a double-screw extruder.
Example 3
(1) Firstly, the carbon nano-tube nano-particles are subjected to heat treatment, namely 0.75g of carbon nano-tube is weighed and put into an oven, and the carbon nano-tube is placed at the temperature of 100 ℃ for constant weight; to remove the water absorbed in the carbon nano tube;
(2) then mixing 99.97 weight parts of very low density polyethylene and 0.03 weight part of the carbon nano tube after the heat treatment in a high-speed mixer for 4 min;
(3) the ultra-low density polyethylene/carbon nano tube composite material can be obtained under the conditions that the extrusion granulation rotating speed is 100rpm and the temperature is 170 ℃ in a double-screw extruder.
Example 4
(1) Firstly, the carbon nano-particle is subjected to heat treatment, namely 1g of carbon nano-particle is weighed and put into an oven and is placed at the temperature of 100 ℃ for constant weight; to remove the water absorbed in the carbon nano tube;
(2) then 99.96 weight parts of very low density polyethylene and 0.01 weight part of the carbon nano tube after the heat treatment are mixed for 5min in a high-speed mixer;
(3) the ultra-low density polyethylene/carbon nano tube composite material can be obtained under the conditions that the extrusion granulation rotating speed is 200rpm and the temperature is 180 ℃ in a double-screw extruder.
Example 5
(1) Firstly, the carbon nano-particle is subjected to heat treatment, namely 1.25g of carbon nano-particle is weighed and put into an oven, and the carbon nano-particle is placed at the temperature of 100 ℃ for constant weight; to remove the water absorbed in the carbon nano tube;
(2) then mixing 99.95 weight parts of very low density polyethylene and 0.05 weight part of the carbon nano tube after the heat treatment in a high-speed mixer for 3-5 min;
(3) the ultra-low density polyethylene/carbon nano tube composite material can be obtained under the conditions that the extrusion granulation rotating speed is 300rpm and the temperature is 160 ℃ in a double-screw extruder.
Comparative example 1
According to the method of example 1, the polyethylene was directly extruded in a twin-screw extruder at a rotation speed of 55rpm and a temperature of 190 ℃ to obtain a test sample without adding carbon nanotubes. The first table shows the mechanical property analysis results of comparative example 1 and the examples.
TABLE-analysis results of mechanical Properties of comparative example 1 and examples
As can be seen from table one, the strength and modulus of the ultra-low density polyethylene/carbon nanotube nanocomposite are significantly improved by adding the carbon nanotubes into the low density polyethylene matrix, and the carbon nanotubes have excellent mechanical properties, and also have physical cross-linking points, thereby achieving the effects of reinforcement and toughening. The second table shows the results of mechanical property analysis of comparative example 1 and examples.
TABLE II analysis results of mechanical properties of comparative example 1 and example
| Sample (I) | Tmax(℃) |
| Example 1 | 401 |
| Example 2 | 412 |
| Example 3 | 414 |
| Example 4 | 426 |
| Example 5 | 435 |
| Comparative example | 394 |
From the second table, it can be seen that the polar density polyethylene material with carbon nanotubes added has higher heat resistance. The carbon nano tube has excellent thermal stability and better compatibility and interaction force with the polymer, so that the decomposition of the polyethylene with extremely low density is limited.
The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application fall within the scope of the claims of the present patent application. The invention has not been described in detail in order to avoid obscuring the invention.
Claims (8)
1. A very low density polyethylene/carbon nanotube composite material, characterized in that: the composition comprises the following components in percentage by weight:
99.95 to 99.99 weight portions of very low density polyethylene,
0.01-0.05 weight part of carbon nano tube.
2. The very low density polyethylene/carbon nanotube composite of claim 1, wherein: the material comprises the following components in parts by weight:
99.95 parts by weight of very low density polyethylene,
0.05 part by weight of carbon nanotubes.
3. The very low density polyethylene/carbon nanotube composite of claim 1 or 2, wherein: the melt flow rate of the very low density polyethylene is 0.8-1.0g/10min, and the density is 0.880-0.915g/cm3。
4. The very low density polyethylene/carbon nanotube composite of claim 1, wherein: the carbon nanotube has an outer diameter of 20-30nm, a length of 10-30 μm, and a density of 2.1-2.5g/m3Surface area greater than 110m2/g。
5. A preparation method of a very low density polyethylene/carbon nanotube composite material, which is the preparation method of the very low density polyethylene/carbon nanotube composite material of claim 1, is characterized by comprising the following steps: (1) heat treatment of the carbon nano tube: weighing a proper amount of carbon nano tubes, putting the carbon nano tubes into an oven, and placing the carbon nano tubes at a temperature of between 80 and 100 ℃ for constant weight so as to remove water absorbed in the carbon nano tubes;
(2) mixing the very low density polyethylene and the carbon nano tubes subjected to heat treatment in the step (1) in a high-speed mixer for 3-5min, wherein the mass ratio of the very low density polyethylene to the carbon nano tubes is 99.95-99.99: 0.01-0.05;
(3) and (3) performing extrusion granulation in a double-screw extruder at the rotating speed of 55-550rpm and the temperature of 160-190 ℃ to obtain the very-low-density polyethylene/carbon nano tube composite material.
6. The method for preparing the very low density polyethylene/carbon nanotube composite material according to claim 5, wherein the mass ratio of the very low density polyethylene to the carbon nanotubes is 99.95: 0.05.
7. the method for preparing very low density polyethylene/carbon nanotube composite material according to claim 5, wherein the very low density polyethylene polymer has a melt flow rate of 0.8-1.0g/10min and a density of 0.880-0.915 g/cm3。
8. The method of claim 5, wherein the carbon nanotubes have an outer diameter of 20-30nm, a length of 10-30 μm, and a density of 2.1-2.5g/m3Surface area greater than 110m2/g。
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| US20080207817A1 (en) * | 2005-03-31 | 2008-08-28 | Arkema France | Polymer Materials Containing Dispersed Carbon Nanotubes |
| CN101283027A (en) * | 2005-08-08 | 2008-10-08 | 卡伯特公司 | Polymeric compositions containing nanotubes |
| CN102952328A (en) * | 2011-08-24 | 2013-03-06 | 中国石油化工股份有限公司 | Carbon nanotube/polyolefin conductive composite material and preparation method |
| CN103408821A (en) * | 2013-05-27 | 2013-11-27 | 浙江大学宁波理工学院 | Polyethylene/fullerene nano-composite material and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080207817A1 (en) * | 2005-03-31 | 2008-08-28 | Arkema France | Polymer Materials Containing Dispersed Carbon Nanotubes |
| CN101283027A (en) * | 2005-08-08 | 2008-10-08 | 卡伯特公司 | Polymeric compositions containing nanotubes |
| CN102952328A (en) * | 2011-08-24 | 2013-03-06 | 中国石油化工股份有限公司 | Carbon nanotube/polyolefin conductive composite material and preparation method |
| CN103408821A (en) * | 2013-05-27 | 2013-11-27 | 浙江大学宁波理工学院 | Polyethylene/fullerene nano-composite material and preparation method thereof |
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Application publication date: 20210305 |