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In situ polymerization preparing method for carbon nano tube and polytene composite material

A technology of carbon nanotubes and composite materials, which is applied in the field of in-situ polymerization preparation of carbon nanotubes and polyethylene composite materials, which can solve the problems of high viscosity of the polymer mixed system, difficulty in dispersing carbon nanotubes and very uniform composite materials, etc. , to achieve good electrical and mechanical properties, simple preparation method

Inactive Publication Date: 2005-07-20
CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the easy self-aggregation and entanglement of carbon nanotubes and the high viscosity of the polymer mixture system, it is difficult to obtain a composite material with very uniform dispersion of carbon nanotubes by this method.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] 1) Functionalization of carbon nanotubes

[0013] In the 200 milliliters of reaction bottles that condensation and stirring device are housed, add 0.5 gram tube length and be 500 nanometers, the multi-walled carbon nanotube of pipe diameter 20 nanometers, then add 50 milliliters volume ratios and be the sulfuric acid and the nitric acid mixed solution of 3 to 1, React at 130°C for 2 hours, filter out the acid solution, wash the remaining carbon nanotubes with deionized water until the pH value of the washing solution is 6, and dry the samples in vacuum at 80°C for 24 hours to obtain functionalized carbon nanotubes; the reaction yield is 60%; the characteristic absorption peaks of hydroxyl, carbonyl and carboxyl can be seen on the infrared absorption spectrum, and the molar total amount of the three groups on the carbon nanotubes measured by X-ray photoelectron spectroscopy is 30%.

[0014] 2) Reaction of methylaluminoxane with functionalized carbon nanotubes

[0015] T...

Embodiment 2

[0021] 1) Reaction of modified methylaluminoxane with functionalized single-walled carbon nanotubes

[0022] Be 200 microns in the same method with embodiment 1 step 1), the single-walled carbon nanotube functionalization of pipe diameter 2 nanometers, measure the molar total amount of three kinds of groups on the carbon nanotube by X-ray photoelectron spectroscopy 2%.

[0023] The same reactor as in step 2) of Example 1 was treated with water and oxygen removal, saturated with an inert gas, added 0.3 g of functionalized single-walled carbon nanotubes, 20 ml of dehydrated toluene, and 5 ml of 1 mole per liter concentration Modified methylalumoxane toluene solution, the weight ratio of carbon nanotubes to modified methylalumoxane is 1:1; after reacting at 80°C for 1 hour, the solvent is filtered off, and washed three times with toluene to obtain modified methylalumoxane aluminoxane-treated single-walled carbon nanotubes.

[0024] 2) Preparation of carbon nanotube supported di...

Embodiment 3

[0029] 1) Preparation of carbon nanotube supported dichlorodicyclopentadienyl zirconium catalyst

[0030] In the same method with embodiment 1 step 1) the tube length is 500 microns, and the multi-walled carbon nanotubes with a diameter of 300 nanometers are oxidized, and the molar total amount of three kinds of groups on the carbon nanotubes is measured by X-ray photoelectron spectroscopy 5%.

[0031] In the same method as in step 2) of Example 1, functionalized carbon nanotubes were added to 10 milliliters of a toluene solution of 1 mole per liter of concentration of methylalumoxane, and the weight ratio of carbon nanotubes to methylalumoxane was 1 ratio 2. React at 50° C. for 12 hours to obtain carbon nanotubes treated with methylaluminoxane.

[0032] Add 20 milliliters of toluene to the carbon nanotubes processed by methylaluminoxane under inert gas in the reactor that will be equipped with stirring and filter, then add 0.05 gram of dichlorodicyclopentadienyl zirconium, c...

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Abstract

The present invention relates to the preparation process of one kind of composite carbon nanotube / polyethylene material. Single or multiple wall carbon nanotube is treated with oxidant to obtain functional carbon nanotube with hydroxyl, carbonyl and carboxyl groups on the surface; and further reacted with alkyl metallizing compound in inert atmosphere to connect metal organic matter component capable of catalyzing ethylene polymerization to obtain carbon nanotube supporting olefin polymerization catalyst. In the presence of alkyl metallizing compound as catalyst assistant, the prepared carbon nanotube supporting olefin polymerization catalyst catalyzes ethylene polymerization to obtain the composite carbon nanotube / polyethylene material. The composite material has two components homogeneously dispersed, electric and mechanical performance higher than other polyethylene material.

Description

field of invention [0001] The invention belongs to the in-situ polymerization preparation method of carbon nanotube and polyethylene composite material. It specifically relates to the preparation of a carbon nanotube-loaded olefin polymerization catalyst and its in-situ catalyzed ethylene polymerization, so that a polyethylene-based composite material with uniformly dispersed carbon nanotubes can be obtained. Background technique [0002] Carbon nanotubes were discovered in the early 1990s, which have good optical, thermal, electromagnetic and mechanical properties. The preparation of polymer-based composites of carbon nanotubes allows the resulting materials to have improved electrical and mechanical properties. The key to the good performance of the composite is to have the carbon nanotubes uniformly dispersed in the polymer matrix. Chinese patent 02113457.X discloses a method for preparing a polymer-based carbon nanotube composite material. The carbon nanotubes are disp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/44C08F4/642C08K3/04C08L23/06
Inventor 唐涛李世云陈辉石丽雅毕务国
Owner CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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