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Composite catalist of titanium substitued nickle acenaphthene diimine of synthesizing branched polyvinyl and its preparation process

A branched polyethylene and composite catalyst technology is applied in the field of titanium-substituted acenaphthene diimide nickel composite catalyst and its preparation, which can solve the problems of difficulty in promotion and use, irregular product shape, and high cost, and achieves the advantages of being conducive to popularization and use, and achieving remarkable results. The effect of superiority

Inactive Publication Date: 2005-01-05
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this catalyst needs to use expensive MAO or boron compound as a cocatalyst, the cost is high, and the branching degree of the obtained product is not easy to control, and the product shape is irregular. difficulty

Method used

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  • Composite catalist of titanium substitued nickle acenaphthene diimine of synthesizing branched polyvinyl and its preparation process
  • Composite catalist of titanium substitued nickle acenaphthene diimine of synthesizing branched polyvinyl and its preparation process

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Experimental program
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Effect test

Embodiment 1

[0029] 1. Nickel complex NiL 1 Cl 2 Preparation: Under the protection of nitrogen, dissolve 2 grams of anhydrous nickel chloride in 20 ml of absolute ethanol for 2 to 3 hours. 1 30 g CH 2 Cl 2 solution, reflux reaction for 12 to 16 hours, drained to remove the solvent, washed three times with anhydrous ether, and dried in vacuum to obtain the desired substituted acenaphthylenediimide nickel complex NiL 1 Cl 2 .

[0030] 2. Catalyst preparation:

[0031]2-1. Mix 5 g of microspherical SiO 2 Put it in a tube furnace, heat it under nitrogen, raise the temperature to 600°C, calcine and dehydrate at a constant temperature, cool after 6 hours, and discharge under nitrogen protection to obtain 4 grams of SiO 2 , placed in a reaction flask, add 40ml of heptane, under nitrogen protection and constant stirring, add 2.5mol / L AlEt 3 3ml of hexane solution, maintained at 25-30°C for 30 minutes, vacuum-dried to remove heptane, and obtained pretreated SiO 2 .

[0032] 2-2. Add 1.2 g...

Embodiment 2

[0040] In Step 2-4 of Example 1, 1 gram of TiCl 4 Change to 1 g TiCl 4 and 0.5 g Ti(OR 1 ) 4 All the other conditions and operations are the same as in Example One, and the prepared catalyst is polymerized under the same conditions in Example One.

[0041] The density of the obtained branched polyethylene under the above polymerization conditions is 0.901g / cm 3 , is a plastic body with a branching degree of 14.4. The catalytic efficiency of the catalyst is 50 kgLLDPE / mol(Ti+Ni).

Embodiment 3

[0043] In step 1 of Example 1, NiL 1 Cl 2 Change to NiL 2 Cl 2 , L 1 change to L 2 ; In steps 2-5, 1.624g NiL 1 Cl 2 Change to 1.610gNiL 2 Cl 2 , all the other conditions and operations are the same as in Example 1, and the prepared catalyst is polymerized under the same conditions as in Example 1.

[0044] Under the above polymerization conditions, the density of the obtained branched polyethylene is 0.910g / cm 3 , is a plastic body with a branching degree of 11.3. The catalytic efficiency of the catalyst was 53 kg LLDPE / mol(Ti+Ni).

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Abstract

The invention relates to a Ti-substituted acenaphthene diimine nickel compound catalyste for synthesizing branched polyethylene and its preparing method, supporting Ti compound and substituted acenaphthene diimine nickel complex on a SiO2-MgCl2 compound carrier to act as a main catalyst and using alkyl Al and AlEt2Cl as aid-catalyst. The preparing method adopts dip-reaction method, and the obtained compound catalyst has a spherical particle shape and can make highly branched low-density polyethylene plastics.

Description

technical field [0001] The invention relates to a titanium-substituted acenaphthylenediimide nickel composite catalyst for synthesizing branched polyethylene and a preparation method thereof. Background technique [0002] The traditional Ziegler-Natta (Z-N) catalyst has good catalytic activity for the copolymerization of ethylene and α-olefin, and can produce medium and low density polyethylene with different degrees of branching; but it cannot make polyethylene produce Branching, to obtain branched polyethylene, it is necessary to use expensive α-olefins, which undoubtedly increases the cost of polyethylene, and at the same time, it is not easy to obtain polyethylene with a high degree of branching with this type of catalyst. Diimine complexes of late-transition metal nickel and palladium discovered in the mid-1990s can be oligomerized and in-situ copolymerized from a single ethylene in a catalytic system made of methylaluminoxane (MAO) or boron compounds Synthesis of vari...

Claims

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Application Information

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IPC IPC(8): C08F4/642C08F110/02
Inventor 王海华胡扬剑江洪流
Owner SUN YAT SEN UNIV
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