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Nickel acenaphthenequinonediimine/ Fe3O4 carried magnetic nano catalyst for ethene in situ polymerization and its preparation method

A technology of nuclear acenaphthodiimide nickel and mononuclear acenaphthodiimide nickel bromide, applied in the field of acenaphthodiimide nickel/Fe3O4 loaded magnetic nano-catalyst and its preparation, can solve the problem that the degree of branching of products is difficult to control and difficult to manufacture Obtaining nano-magnetic branched polyethylene plastics and elastomers, affecting product uniformity and processing and application performance, and achieving significant superiority

Inactive Publication Date: 2006-12-27
SUN YAT SEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It is reported in the literature that the traditional Ziegler-Natta (Z-N) catalyst combined with nano-magnetic particles is used to prepare the supported catalyst through AlEt 2 Cl is activated to polymerize ethylene in situ, and nano-magnetic polyethylene plastics have been prepared (WangL., et al. Studies on the preparation of new magnetic polyolefins using nanometer magneticZiegler-Natta catalyst J.Appl.Polym.Sci., 1999, 71 , 2087-2089); however, it is difficult to prepare nano-magnetic branched polyethylene plastomers and elastomers without using α-olefins as comonomers
Moreover, the degree of branching of the obtained product is not easy to control, which affects the uniformity and processing application performance of the product.

Method used

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  • Nickel acenaphthenequinonediimine/ Fe3O4 carried magnetic nano catalyst for ethene in situ polymerization and its preparation method
  • Nickel acenaphthenequinonediimine/ Fe3O4 carried magnetic nano catalyst for ethene in situ polymerization and its preparation method
  • Nickel acenaphthenequinonediimine/ Fe3O4 carried magnetic nano catalyst for ethene in situ polymerization and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1. Catalyst preparation:

[0023] (1) Add 0.54g (2.97mmol) acenaphthenequinone and 3.01g (8.19mmol) 4,4'-methylene-bis(2,6-diisopropylaniline) to 50mL toluene, add a few drops of sulfuric acid , Reflux reaction for 14h in a reflux device equipped with a water separator, cool to room temperature, and remove the solvent in vacuo to obtain a brownish-red solid. Using a mixed solvent of ethyl acetate and petroleum ether (volume ratio 1:9) as eluent, 1.22 g of yellow powder solid L was obtained by separation through a silica gel column.

[0024] (2) Under anhydrous and anaerobic conditions, with 20mL CH 2 Cl 2 As a solvent, take 0.6g ligand (L) and 0.46g dibromo(1,2-dimethoxyethane) nickel ((DME)NiBr 2 ) reflux at room temperature under nitrogen protection for 14h, remove the solvent in vacuo, wash three times (30ml×3) with anhydrous ether, and dry in vacuo to obtain the desired mononuclear acenaphthylenediimide nickel complex NiLBr 2 .

[0025] (3) Add 288ml of water t...

Embodiment 2

[0033] 1. Catalyst preparation is the same as embodiment one.

[0034] 2. In Example 1-2, "raise the temperature to 50°C and carry out the polymerization reaction for 1.5h," to "raise the temperature to 20°C and carry out the polymerization reaction for 1.5h," and the remaining conditions and operations are the same as in Example 1.

[0035] The branched polyethylene obtained under the above polymerization conditions is a plastic body with a degree of branching of 18.0 (branch number / 1000C). The catalytic efficiency of the catalyst is 1.94×10 6 g LLDPE / mol Ni h. Contains 3.23% magnetic nanoparticles, its saturation magnetic strength M s =1.284emu g -1 . Observation by transmission electron microscope, Fe 3 o 4 It is uniformly dispersed in the branched polyethylene plastic body in the form of nanoparticles, and its size is about 20nm.

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Abstract

The invention relates to a magnetic nanometer catalyst carried by acenaphthenyl imines nickel / Fe3O4 and the method for preparing the same. Said catalyst comprises main catalyst and adjuvant catalyst, loading mononuclear acenaphthenyl imines nickel composite on nanometer Fe3O4 carrier modified by aluminium trialkyl as main catalyst, taking ALEt2Cl as adjuvant catalyst. The method employs immersion reaction process. The invention employs general-used Et2ALCL as adjuvant catalyst to replace dear MAO, and catalyze ethylene polymerization to produce polyethylene nanometer magnetic Fe3O4 plastic body and elastic body. The molecular chain of prepared polymer contains branch chain of different length, which can improve comprehensive performance for magnetic plastic body and elastic body.

Description

technical field [0001] The invention relates to acenaphthylenediimide nickel / Fe for synthesizing high-branched polyethylene magnetic nano-plastomers and elastomers by in-situ polymerization of ethylene 3 o 4 Loaded magnetic nano catalyst and its preparation method. Background technique [0002] Nano-magnetic plastics are a new class of polymer materials with excellent properties developed in recent years. The preparation of new catalysts and nano-magnetic particles is covalently bonded, thus preventing them from falling off the surface of the magnetic particles. 2 Cl is activated to make ethylene polymerize in situ. Under the condition of anhydrous and oxygen-free, the produced polyethylene continuously wraps the nano-magnetic particles, thus forming a uniform, dense and stable protective layer, and generating a new type of nano-polyolefin composite material. It is reported in the literature that the traditional Ziegler-Natta (Z-N) catalyst combined with nano-magnetic pa...

Claims

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Application Information

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IPC IPC(8): C08F10/02C08F4/70C08F4/613
Inventor 王海华江洪流胡扬剑
Owner SUN YAT SEN UNIV