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Method of preparing nano-polyethylene fiber using TiCl4/MCM-41 catalytic system extrusion polymerization

A technology of polyethylene fiber and MCM-41 is applied in the field of preparing nanometer polyethylene fiber by extrusion polymerization of TiCl4/MCM-41 catalytic system, which can solve the problems of high polymerization pressure, high price, increase production cost and the like, and achieve low cost , the preparation process is simple, the effect of the process is simple

Inactive Publication Date: 2007-05-16
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Both of these methods require high polymerization pressure during the polymerization process, and relatively expensive metallocene catalysts are used, thus increasing production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Under nitrogen protection, 1 gram of MCM-41 (pore size: 2.9 nm) treated at 400°C was added to 40 ml of n-hexane, and 8 ml of triethylaluminum with a concentration of 0.955 mol / l was stirred at room temperature for 1 hour. Wash three times with n-hexane; add 5ml of TiCl 4 The n-hexane solution (0.91mol / l) was reacted at room temperature for 2 hours, then washed three times with n-hexane, and the n-hexane solvent was removed in vacuum to obtain a powdery solid catalyst with a titanium loading of 1.34mmolTi / g.

[0022] Under normal pressure at 50°C, 4.6mg β-cyclodextrin and 16.5mg TiCl 4 / MCM-41 catalyst was added to 50ml of n-hexane, stirred and reacted for 2 minutes, then ethylene gas was introduced to make it saturated, then 0.5ml of diluted triethylaluminum ([Al] / [Ti]=20) was added and reacted for 30 minutes Afterwards, it is terminated with acidified ethanol, and the product is filtered, washed and dried to obtain nano-polyethylene fibers with a diameter of 30-80 nm....

Embodiment 2

[0024] Using the supported catalyst prepared in Example 1, carry out ethylene polymerization under normal pressure at 50°C, 3.8mg β-cyclodextrin and 23.9mg TiCl 4 / MCM-41 catalyst, [Al] / [Ti]=20, the reaction time is 30 minutes, the product is filtered, washed and dried to obtain nano polyethylene fibers with a diameter of 30-80nm.

Embodiment 3

[0026] Using the supported catalyst prepared in Example 1, carry out ethylene polymerization under normal pressure at 30°C, 4.3mgβ-cyclodextrin and 18.8mg TiCl 4 / MCM-41 catalyst, [Al] / [Ti]=20, the reaction time is 30 minutes, the product is filtered, washed and dried to obtain nano polyethylene fibers with a diameter of 30-80nm.

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Abstract

A process for preparing polyethene nanofibres by extrusion polymerizing with TiCl4 / MCM-41 catalyst system includes such steps as adding carrier to n-hexane, treating by triethyl aluminium, washing with n-hexane to obtain suspension, diluting TiCl4 by n-hexane, adding it to said suspension, reacting while stirring, vacuum removal of n-hexane to obtain carried catalyst, mixing it with triethyl aluminium as cocatalyst, beta-cyclodextrin and ethane, and extrusion polymerizing. Said steps are performed in high-purity N2.

Description

technical field [0001] The present invention relates to a kind of adopting TiCl 4 / MCM-41 catalytic system extrusion polymerization method for preparing nano polyethylene fibers. technical background [0002] With the development of nanotechnology, nanomaterials are more and more widely used in practice. Nanofibers have become a research hotspot because of their large specific surface area and high strength. At present, the common preparation methods of nanofibers include gel spinning method, drawing method, electrospinning method, etc., but these preparation methods all require a series of specific processing equipment and complicated processing procedures. [0003] Aida et al. reported a method of loading titanocene dichloride on mesoporous silica fibers, using MAO as a co-catalyst, and catalyzing ethylene polymerization at a high pressure of 1Mpa to prepare nano-polyethylene fibers, because the PE chains are stretched. Chain, so this fiber has higher strength, the disc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F110/02C08F4/642B29C47/00
Inventor 董晓臣王立孙天旭俞豪杰周峻峰
Owner ZHEJIANG UNIV