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Polyethylene/montmorillonite nanometer composite material and method for preparing same by in-situ polymerization

A nano-composite material and in-situ polymerization technology, applied in the field of polymer materials, to achieve mild reaction conditions, simple operation, and improved efficiency

Inactive Publication Date: 2011-10-19
SHENZHEN KEJU NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the active groups of MMT, that is, hydroxyl groups, are exposed at the edge of MMT, so how to increase the loading capacity of the catalyst becomes a big challenge.

Method used

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  • Polyethylene/montmorillonite nanometer composite material and method for preparing same by in-situ polymerization
  • Polyethylene/montmorillonite nanometer composite material and method for preparing same by in-situ polymerization
  • Polyethylene/montmorillonite nanometer composite material and method for preparing same by in-situ polymerization

Examples

Experimental program
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Effect test

Embodiment 1

[0056] The method for preparing exfoliated polyethylene / montmorillonite nanocomposites by in-situ polymerization, the specific steps are as follows:

[0057] (1) Add 100ml benzene, 2g compound 1, 1ml Et(OH) in dry 250ml two-necked bottle 2 and 0.02g TsOH. Connect a water trap to the reaction flask, reflux at 80°C for one day under magnetic stirring, and then evaporate the solvent to dryness on a rotary evaporator. The crude product was recrystallized from benzene;

[0058] (II) In a dry 250ml two-necked flask, add 0.6g undecylamine and dissolve in 100ml CH 3 CN, then add 2.0g K 2 CO 3 powder, and fitted with a condenser tube, another 3.8g of the synthetic product prepared in step (I) was dissolved in 50ml of CH 3 CN was installed in a dropping funnel, and the reaction device was placed in an ice bath, and added dropwise under magnetic stirring. After 0.5 hour, the temperature was raised to 35°C and the reaction was continued for 1 day. After the reaction, the mixed solu...

Embodiment 2

[0066] The method for preparing exfoliated polyethylene / montmorillonite nanocomposites by in-situ polymerization, the specific steps are as follows:

[0067] (1) as step (I) in embodiment 1;

[0068] (II) as step (II) in embodiment 1;

[0069] (III) get the product prepared in 3g step (II), 0.12g TsOH, 0.13g H 2 O was added to 50ml CH 3 COCH 3 , pass into N 2 To evacuate the air, react at room temperature for 3 days; evaporate the solvent to dryness after the reaction, and use Et 2 O and H 2 O for liquid separation operation, keep the organic phase, and then evaporate the solvent to obtain the crude product. The crude product was purified by column chromatography, and the eluent was purified with Et 2 O and n-C 6 h 14 Mixed solvent (1 / 3, v / v); Obtain loaded modifier;

[0070] (IV) Dissolve 4 g of load modifier compound in C 2 h 5 OH / H 2 O (3 / 7, v / v) reacts with an equivalent amount of HCl to protonate it in a mixed solvent, heats to 60° C. and conducts an ion exch...

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Abstract

The invention discloses a polyethylene / montmorillonite nanometer composite material and a method for preparing the same by in-situ polymerization. The method for preparing the polyethylene / montmorillonite nanometer composite material by in-situ polymerization includes the following steps of: obtaining a supported organic modifier, a metallocene catalyst and montmorillonite; displacing the supported organic modifier into interlayers of the montmorillonite through ion exchange reaction to obtain organically modified montmorillonite; loading the metallocene catalyst into interlayers of the montmorillonite to obtain a supported catalyst; and carrying out in-situ polymerization on the supported catalyst with ethylene gases under the water-free and oxygen-free condition to obtain the polyethylene / montmorillonite nanometer composite material. The method for preparing the polyethylene / montmorillonite nanometer composite material by in-situ polymerization effectively reduces the catalyst amount and production cost, improves the production efficiency, and has moderate reaction condition, low requirements for equipment and simple operation, and is suitable for industrialization production.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a polyethylene / montmorillonite nanocomposite material and a method for preparing the polyethylene / montmorillonite nanocomposite material by in-situ polymerization. Background technique [0002] In situ intercalation polymerization is an effective method to prepare polyolefin / montmorillonite (PE / MMT) nanocomposites. It is characterized in that the catalyst is loaded between the montmorillonite layers so that the olefin polymerization reaction can be carried out between the layers. This method is considered to be a better method for obtaining filler dispersion than solution blending and melt blending. However, this approach still has two challenges that remain to be resolved. First, because the driving force for MMT stripping in the in-situ intercalation polymerization method is that the polymer molecular chains gradually grow between the layers to stretch t...

Claims

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Application Information

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IPC IPC(8): C08F110/02C08F2/44C08K9/04C08K3/34C08F4/02C08F4/642C08F4/6592
Inventor 徐东徐永任昌义
Owner SHENZHEN KEJU NEW MATERIAL
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