CN102336942B - Polyester/polyethylene/carbon nanotube ternary composite material and preparation method thereof - Google Patents
Polyester/polyethylene/carbon nanotube ternary composite material and preparation method thereof Download PDFInfo
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- CN102336942B CN102336942B CN201010233309.7A CN201010233309A CN102336942B CN 102336942 B CN102336942 B CN 102336942B CN 201010233309 A CN201010233309 A CN 201010233309A CN 102336942 B CN102336942 B CN 102336942B
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Abstract
The invention relates to a polyester/polyethylene/carbon nanotube ternary composite material and its preparation method. The ternary composite material takes an annular polyester oligomer, polyethylene and carbon nanotube as main raw materials, the preparation is performed through reactive blending, the unique performance of the carbon nanotube is used for promoting the compatibility of polyester and polyethylene incompatibility system, the enhancement of the compatibility of polyester and polyethylene can be observed by the obtained ternary composite material through a field-emission scanning electron microscope, thereby the compatible effect of the carbon nanometer is realized. Compared with the prior art, the method of the invention has the advantages of simple operation, easy industrialization production and the like.
Description
Technical field
The invention belongs to polymer composite preparation field, especially relate to a kind of polyester/polyethylene/carbon nanometer pipe ternary matrix material and preparation method thereof.
Background technology
In recent years, owing to adding inorganic nano-particle as compatilizer in incompatible polymer alloy, can obtain is the trielement composite material of increase-volume, thereby is developed greatly.In this type of trielement composite material, inorganic nano-particle is different from traditional compatilizer as grafts, due to the feature of its larger specific surface area and rigidity own, polymkeric substance is easily adsorbed on the surface of nanoparticle, so add the nanoparticle phase structure of stabilization of polymer preferably, thereby play the effect of increase-volume.
As a kind of nano material with unique texture, carbon nanotube starts to be made an addition to widely prepares trielement composite material in incompatible polymer blend.(the Wu D.F. such as Wu, Zhang Y.S., Zhang M., Yu W., Biomacromolecules, 2009,10,417-424.) prepared polycaprolactone/poly(lactic acid)/multi-walled carbon nano-tubes (PCL/PLA/MWNTs) ternary nano composite material by the method for melt blending, research finds to add the carbon nanotube (f-MWNTs) of functionalization in PCL/PLA system, and f-MWNTs is optionally distributed in PCL external phase and PCL and PLA two-phase interface place; And the f-MWNTs of these selective distributions has produced very large impact to the interfacial energy of whole system, result is along with the increase of f-MWNTs content, and the size of disperse phase PLA also reduces gradually, and has also had the combination of better interface between PCL and PLA.Janke etc. [
p., Bhattacharyya A.R., Janke A., Polymer, 2003,44,8061-8069.] first prepare polycarbonate/multi-walled carbon nano-tubes (PC/MWNTs) master batch by melt blending, and then carry out melt blending with this master batch and polyethylene (PE), prepare the PE/PC/MWNTs ternary nano composite material with PE and PC co-continuous phase.Because the consistency of MWNTs and PE is better, in Blending Processes, MWNTs moves mutually to PE, result MWNTs part is distributed on PE and PC interface, these MWNTs have improved the interface compatibility between PE and PC effectively, has improved two alternate interface binding powers.But preparation method's complexity of these matrix materials, can not carry out industrialization production.
Summary of the invention
Object of the present invention be exactly provide in order to overcome the defect that above-mentioned prior art exists that a kind of method is simple, polyester/polyethylene/carbon nanometer pipe ternary matrix material of being easy to suitability for industrialized production and preparation method thereof.
Object of the present invention can be achieved through the following technical solutions: a kind of polyester/polyethylene/carbon nanometer pipe ternary matrix material, it is characterized in that, and this trielement composite material comprises following component and weight part content:
Polyethylene 10～90;
Polyester 90～10;
Carbon nanotube 1～5;
Polyester catalyst 0.18～0.02.
Described polyethylene is Low Density Polyethylene or high density polyethylene(HDPE), and its melt index is 0.2～10g/10min (190 DEG C, 2.16kg).
Described polyester is oligopolymer polyester, is selected from one or more in polyethylene terephthalate cyclic oligomer, Poly(Trimethylene Terephthalate) cyclic oligomer, polybutylene terephthalate cyclic oligomer.
Described carbon nanotube is Single Walled Carbon Nanotube or multi-walled carbon nano-tubes, and length is 10～30 microns, and its diameter is 10～20nm, has larger specific surface area.
Described polyester catalyst is selected from one or more in tributyl oxyethyl group tin, n-butyl tin chloride dihydroxide, positive metatitanic acid four (2-ethylhexyl) ester.
The preferred n-butyl tin chloride dihydroxide of described polyester catalyst.
A preparation method for polyester/polyethylene/carbon nanometer pipe ternary matrix material, is characterized in that, the method comprises the following steps:
(1) prepare raw material according to following component and weight part content:
Polyethylene 10～90;
Polyester 90～10;
Carbon nanotube 1～5;
Polyester catalyst 0.18～0.02;
(2) above-mentioned raw materials is added in Banbury mixer, make the good polyester/polyethylene/carbon nanometer pipe ternary matrix material of consistency in 230～260 DEG C of blend 5～10min of temperature.
The rotating speed of described Banbury mixer is 50～100rpm.
Compared with prior art, the present invention is directed to the inconsistent feature of polyester and polyethylene blend material, in conjunction with the feature of carbon nanotube, a kind of polyester/polyethylene/carbon nanometer pipe ternary matrix material and preparation method thereof is provided, realize the increase-volume of two-phase incompatibility system, adopt the method for banburying to prepare trielement composite material, this method is simple, is easy to suitability for industrialized production.
Figure of description
Fig. 1 is scanning electron microscope (FESEM) figure of PBT/HDPE of the present invention (30/70) different amplification;
Fig. 2 is scanning electron microscope (FESEM) figure of the trielement composite material different amplification of the present invention's carbon nanotube of having added 3phr;
Fig. 3 is scanning electron microscope (FESEM) figure of PBT/HDPE of the present invention (30/70) different amplification;
Fig. 4 is scanning electron microscope (FESEM) figure of the trielement composite material different amplification of the present invention's carbon nanotube of having added 3phr.
Embodiment
Embodiment further illustrates of the present invention below, but not limits the scope of the invention.
Embodiment 1
The present invention relates to a kind of polyester/polyethylene/carbon nanometer pipe ternary matrix material and preparation method thereof, realize as follows:
Take dry carbon nanotube 1.8g, high density polyethylene(HDPE) 42g (melt index is 7g/10min), polybutylene terephthalate cyclic oligomer 18g, polyester catalyst 0.036g, add in Banbury mixer, in 235 DEG C of blend 10min of temperature, rotating speed is 70rpm, makes consistency good polybutylene terephthalate/high density polyethylene(HDPE)/carbon nanometer pipe ternary matrix material.
The trielement composite material of preparation characterizes by field emission scanning electron microscope (FESEM), and because carbon nanotube plays the effect of expanding material in the incompatible system of polyester/polyethylene, thereby two-phase consistency increases.See accompanying drawing 1, as can be seen, the interface of two-phase is because add the fuzzy of carbon nanotube change, and consistency improves.
Embodiment 2～5:
| Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Low Density Polyethylene (g) | 10 | 20 | ||
| High density polyethylene(HDPE) (g) | 90 | 70 | ||
| Polyethylene terephthalate cyclic oligomer (g) | 90 | 20 |
| Polybutylene terephthalate cyclic oligomer (g) | 10 | 70 | ||
| Single Walled Carbon Nanotube (g) | 1 | 4 | ||
| Multi-walled carbon nano-tubes (g) | 3 | 5 | ||
| Tributyl oxyethyl group tin (g) | 0.18 | 0.15 | ||
| Positive metatitanic acid four (2-ethylhexyl) ester (g) | 0.1 | 0.02 | ||
| Banbury mixer temperature (DEG C) | 230 | 260 | 240 | 250 |
| The blend time (min) | 5 | 6 | 8 | 9 |
| Rotating speed (rpm) | 50 | 60 | 80 | 100 |
According to the method for embodiment 1, make polyester/polyethylene/carbon nanometer pipe ternary matrix material of embodiment 2-5, the trielement composite material of preparation characterizes by field emission scanning electron microscope (FESEM), because carbon nanotube plays the effect of expanding material in the incompatible system of polyester/polyethylene, two-phase consistency increases.
Embodiment 6
A preparation method for polyester/polyethylene/carbon nanometer pipe ternary matrix material, the method comprises the following steps:
(1) prepare raw material according to following component and weight part content:
Melt index is the polyethylene 10 of 0.2g/10min;
Poly(Trimethylene Terephthalate) cyclic oligomer 90;
Length is the carbon nanotube 5 that 10 microns, diameter are 10nm;
N-butyl tin chloride dihydroxide 0.18;
(2) above-mentioned raw materials is added in Banbury mixer, in 230 DEG C of blend 10min of temperature, rotating speed is that 100rpm makes the good polyester/polyethylene/carbon nanometer pipe ternary matrix material of consistency.
Embodiment 7
A preparation method for polyester/polyethylene/carbon nanometer pipe ternary matrix material, the method comprises the following steps:
(1) prepare raw material according to following component and weight part content:
Melt index is the polyethylene 90 of 10g/10min;
Poly(Trimethylene Terephthalate) cyclic oligomer 10;
Length is the carbon nanotube 1 that 30 microns, diameter are 20nm;
N-butyl tin chloride dihydroxide 0.02;
(2) above-mentioned raw materials is added in Banbury mixer, in 260 DEG C of blend 5min of temperature, rotating speed is that 50rpm makes the good polyester/polyethylene/carbon nanometer pipe ternary matrix material of consistency.
Claims (8)
1. polyester/polyethylene/carbon nanometer pipe ternary matrix material, is characterized in that, this trielement composite material comprises following component and weight part content:
Described polyester is oligopolymer polyester.
2. polyester/polyethylene/carbon nanometer pipe ternary matrix material according to claim 1, is characterized in that, described polyethylene is Low Density Polyethylene or high density polyethylene(HDPE), and its melt index is 0.2～10g/10min, and test condition is 190 DEG C, 2.16kg.
3. polyester/polyethylene/carbon nanometer pipe ternary matrix material according to claim 1, it is characterized in that, described oligopolymer polyester is selected from one or more in polyethylene terephthalate cyclic oligomer, Poly(Trimethylene Terephthalate) cyclic oligomer, polybutylene terephthalate cyclic oligomer.
4. polyester/polyethylene/carbon nanometer pipe ternary matrix material according to claim 1, is characterized in that, described carbon nanotube is Single Walled Carbon Nanotube or multi-walled carbon nano-tubes, and length is 10～30 microns, and its diameter is 10～20nm.
5. polyester/polyethylene/carbon nanometer pipe ternary matrix material according to claim 1, is characterized in that, described polyester catalyst is selected from one or more in tributyl oxyethyl group tin, n-butyl tin chloride dihydroxide, positive metatitanic acid four (2-ethylhexyl) ester.
6. polyester/polyethylene/carbon nanometer pipe ternary matrix material according to claim 5, is characterized in that, the preferred n-butyl tin chloride dihydroxide of described polyester catalyst.
7. a preparation method for polyester/polyethylene/carbon nanometer pipe ternary matrix material as claimed in claim 1, is characterized in that, the method comprises the following steps:
(1) prepare raw material according to following component and weight part content:
Described polyester is oligopolymer polyester;
(2) above-mentioned raw materials is added in Banbury mixer, make the good polyester/polyethylene/carbon nanometer pipe ternary matrix material of consistency in temperature 230～260oC blend 5～10min.
8. the preparation method of polyester/polyethylene/carbon nanometer pipe ternary matrix material according to claim 7, is characterized in that, the rotating speed of described Banbury mixer is 50～100rpm.
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Non-Patent Citations (2)
| Title |
|---|
| Effect of Microfiber Reinforcement on the Morphology,Electrical, and Mechanical Properties of the Polyethylene/Poly(ethylene terephthalate)/Carbon Nanotube Composites;Sertan Yesil et al;《POLYMER ENGINEERING AND SCIENCE》;20100625;第50卷(第11期);2093-2105 * |
| Sertan Yesil et al.Effect of Microfiber Reinforcement on the Morphology,Electrical, and Mechanical Properties of the Polyethylene/Poly(ethylene terephthalate)/Carbon Nanotube Composites.《POLYMER ENGINEERING AND SCIENCE》.2010,第50卷(第11期), |
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