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Polyester/carbon nano tube-nucleating agent composite material and preparation method thereof

A technology of carbon nanotubes and composite materials, which is applied in the field of polyester/carbon nanotube-nucleating agent composite materials and their preparation, can solve the problems of weakening nucleation ability, reducing the ability of carbon nanotubes to induce nucleation, etc. The effect of crystallization rate, enhanced heterogeneous nucleation crystallization ability, and improved mechanical properties

Inactive Publication Date: 2012-07-04
SHANGHAI GENIUS ADVANCED MATERIAL (GRP) CO LTD
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  • Summary
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AI Technical Summary

Problems solved by technology

So far, the research on improving the crystallization rate of PTT has mainly focused on some inorganic fillers, such as montmorillonite (Cho HW, Lee JS, Prabu AA, Kim KJ. Physical properties of poly(trimethylene terephthalate) / organoclay nanocomposites obtained via melt compounding and in situ polymerization. Polym Compos 2008; 29(12); 1328-36.), barium sulfate (Yao CG, Yang GS. Synthesis, thermal, and rheological properties of poly(trimethylene terephthalate) / BaSO 4 nanocomposites.Polym Adv Technol 2009; 20(10):768-74.), silicon dioxide (Yao CG, Yang GS. Poly(trimethylene terephthalate) / silica nanocomposites prepared by dual in situ polymerization: synthesis, morphology, crystallization behavior and mechanical properties.Polym Int 2010; 59(4):492-500.), etc., it is obvious that it is extremely limited to improve the mechanical properties of PTT, especially the impact resistance, simply from the perspective of increasing the crystallization rate and reducing the size of spherulites
[0004] Since carbon nanotubes were accidentally discovered by Japanese expert Iijima in 1991, due to their excellent physical properties, such as extremely high modulus, strength, and good thermal and electrical conductivity, they have been favored by academics since their discovery. The polymer / carbon nanotube composite material has become the most active research field in the past two decades, and the influence of carbon nanotubes on the crystallization properties of semi-crystalline polymer materials constitutes a polymer / carbon nanotube composite material. The most active branch in the field of materials, a large number of studies have shown that carbon nanotubes can also be used as heterogeneous nucleating agents for semi-crystalline polymers due to their high specific surface area, and PTT / carbon nanotube composites have also been reported (Xu Y, Jia HB, Piao JN, Ye SR, Huang J. Crystallization behavior of poly(trimethylene terephthalate) / multi-walled carbon nanotube composites.J Mater Sci 2008;43(1):417-21.), however, it promotes crystallization The nucleation ability weakens with the increase of the interaction between carbon nanotubes and polymers, that is to say, in order to improve the dispersion of carbon nanotubes in the polymer matrix, it is necessary to modify the carbon nanotubes, which improves the carbon nanotubes. The interaction force between tubes and polymers, but also reduces the nucleation-inducing ability of carbon nanotubes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Add 78 parts of dimethyl terephthalate, 76 parts of 1,3-propanediol and 0.015 parts of n-tetrabutyl titanate into a 250ml three-necked flask equipped with mechanical stirring, start stirring, and control the reaction temperature to 190°C carry out transesterification;

[0032] (2) In the mixed solution after the amount of methanol evaporated by transesterification reaches 92% of the theoretical value of transesterification (2 times of the amount of dimethyl terephthalate), add 0.015 parts of polymerization catalyst zinc acetate, add 0.05 One part of carboxylated single-walled carbon nanotubes with a diameter of 2-10nm and 0.02 part of sodium montmorillonite, the temperature is controlled at 255 ° C, the polycondensation reaction is carried out under a pressure of less than 40 Pa for 4 hours, and the product is obtained by vacuum drying at 80 ° C for 24 hours after the polycondensation is completed. . The obtained sample was hot-pressed into a film at 245°C, and the...

Embodiment 2

[0034] (1) Add 78 parts of dimethyl terephthalate, 76 parts of 1,3-propanediol and 0.015 parts of n-tetrabutyl titanate into a 250ml three-necked flask equipped with mechanical stirring, start stirring, and control the reaction temperature to 190°C carry out transesterification;

[0035](2) in the mixed solution after the methyl alcohol amount that the transesterification steams reaches 92% of the theoretical value of transesterification (2 times of the dimethyl terephthalate substance quality), add 0.015 part of polymerization catalyst zinc acetate, add 1 One part of carboxylated single-walled carbon nanotubes with a diameter of 2-10nm and 0.02 part of sodium montmorillonite, the temperature is controlled at 255 ° C, the polycondensation reaction is carried out under a pressure of less than 40 Pa for 4 hours, and the product is obtained by vacuum drying at 80 ° C for 24 hours after the polycondensation is completed. . The obtained sample was hot-pressed into a film at 245°C,...

Embodiment 3

[0037] (1) Add 78 parts of dimethyl terephthalate, 76 parts of 1,3-propanediol and 0.015 parts of n-tetrabutyl titanate into a 250ml three-necked flask equipped with mechanical stirring, start stirring, and control the reaction temperature to 190°C carry out transesterification;

[0038] (2) In the mixed solution after the methyl alcohol amount that the transesterification steams reaches 92% of the theoretical value of transesterification (2 times of the dimethyl terephthalate substance quality), add 0.015 part of polymerization catalyst zinc acetate, add 5 One part of carboxylated single-walled carbon nanotubes with a diameter of 2-10nm and 0.02 part of sodium montmorillonite, the temperature is controlled at 255 ° C, the polycondensation reaction is carried out under a pressure of less than 40 Pa for 4 hours, and the product is obtained by vacuum drying at 80 ° C for 24 hours after the polycondensation is completed. . The obtained sample was hot-pressed into a film at 245°C...

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Abstract

The invention belongs to the technical field of high polymer material preparation, and in particular relates to a polyester / carbon nano tube-nucleating agent composite material and a preparation method thereof. The composite material provided by the invention comprises the following components in parts by weight: 78 parts of dimethyl terephthalate, 61-100 parts of 1,3-propylene glycol, 0.0078-0.78 part of ester exchange catalyst, 0.0078-0.78 part of polymerization catalyst, 0.05-5 parts of carbon nano tube and 0.02-2 parts of nucleating agent. The invention also provides the preparation method of the polyester / carbon nano tube-nucleating agent composite material. The preparation method comprises two steps, namely ester exchange and polymerization. For the composite material provided by the invention, the addition of the nucleating agent enhances the heterogeneous nucleation crystallization capability, improves the crystallization speed, reduces the sphaerocrystal size of dimethyl terephthalate and improves mechanical property; at the moment, the strength-increasing and toughening capabilities are mainly exerted by the addition of the carbon nano tube so that the great improvement of the property of the composite material can be realized only by less filling, thus the application field of the composite material is greatly expanded.

Description

technical field [0001] The invention belongs to the technical field of polymer material preparation, and in particular relates to a polyester / carbon nanotube-nucleating agent composite material and a preparation method thereof. Background technique [0002] PTT (polytrimethylene terephthalate) is a polyester obtained by polymerizing dimethyl terephthalate or terephthalic acid and 1,3-propanediol. PTT is a new promising polyester polymer newly developed after polyethylene terephthalate (PET) in the 1950s and polybutylene terephthalate (PBT) in the 1970s. Materials, in 1998 by the United States as one of the six new petrochemical products. PTT is a semi-crystalline polymer with high melting temperature and glass transition temperature. It has good wear resistance, heat resistance and chemical resistance, and is widely used in synthetic fibers, films and engineering plastics, etc. field. However, due to the slow crystallization rate of PTT due to its rigidity, its applicatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L67/02C08K13/06C08K9/00C08K7/00C08K3/04C08K3/22C08K3/34C08K3/26C08K5/098C08G63/183
Inventor 陈珍明
Owner SHANGHAI GENIUS ADVANCED MATERIAL (GRP) CO LTD
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