Zirconium metal complex of furan aldehyde (ketone) hydrazone as well as preparation method and application of zirconium metal complex

A technology of metal complexes and furan aldehydes, which is applied in the field of zirconium metal complexes, can solve problems such as unsuitable solution polymerization processes, and achieve the effects of simple and easy preparation methods, high yields, and cheap and easy-to-obtain raw materials

Inactive Publication Date: 2013-11-20
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Metallocene catalysts have high catalytic activity, but they only show high activity at room temperature, which is not suitable for the solution polymerization process at high temperature commonly used in industry today.

Method used

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  • Zirconium metal complex of furan aldehyde (ketone) hydrazone as well as preparation method and application of zirconium metal complex
  • Zirconium metal complex of furan aldehyde (ketone) hydrazone as well as preparation method and application of zirconium metal complex
  • Zirconium metal complex of furan aldehyde (ketone) hydrazone as well as preparation method and application of zirconium metal complex

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The preparation of embodiment 1 zirconium metal complex

[0024] Preparation of Ligand 2-furylcarbaldehyde phenylhydrazone:

[0025] Dissolve 2-furylcarbaldehyde (1.92g, 20mmol) in 20ml of ethanol, add an equimolar amount of phenylhydrazine (2.16g, 20mmol) dropwise at 0°C, the reaction solution gradually rises to room temperature, and more Pale yellow solid, continue to stir the reaction overnight. The ethanol was removed by suction filtration, and the yellow solid was washed with ether to obtain a light yellow solid, which was the ligand 2-furaldehyde phenylhydrazone (2.87 g), with a yield of 77%.

[0026] Preparation of zirconium metal complexes of tetrahydrofuran-coordinated 2-furylaldehyde phenylhydrazone trichloride:

[0027] At 0°C, add an equimolar amount of LDA (0.27g, 2.52mmol) to a solution of the ligand compound 2-furylaldehyde phenylhydrazone (0.47g, 2.52mmol) in about 25ml of ether to obtain a yellow suspension Gradually warm to room temperature and stir...

Embodiment 2

[0028] The application of embodiment 2 complex as catalyst in catalytic ethylene polymerization

[0029] Aggregation condition selection:

[0030] At 10atm, when the molar ratio of MAO:catalyst is 1000:1, the temperature is changed, and the activity at 30°C, 50°C, 70°C, and 90°C is tested respectively, which are 0.96×10 5 , 1.52×10 5 , 1.96×10 5 , 0.44×10 5 gPE / mol(Zr) h. When the temperature is 70°C, test the MAO respectively: the molar ratio of the catalyst is 500:1, 1500:1, and the activity when 2000:1 is respectively 0.52×10 5 , 1.64×10 5 , 1.52×10 5 gPE / mol(Zr) h.

[0031] 1: The polymerization of ethylene is carried out in a stainless steel pressure kettle with a volume of 250ml. The pressure kettle is connected with a buffered ethylene cylinder, which can continuously replenish ethylene through a spiral steel pipe, so as to maintain a constant pressure during the polymerization reaction (under 10atm pressure) . After the polymerization kettle is fully dried, it i...

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Abstract

The invention provides a zirconium metal complex of furan aldehyde (ketone) hydrazone, a preparation method of the zirconium metal complex and an application of the complex as a catalyst to the preparation of ultra-high molecular weight polyethylene. The preparation method of the complex comprises the following steps of: subjecting the furan aldehyde (ketone) hydrazone and lithium diisopropylamide (LDA) to dehydrogenation reaction, then, subjecting the furan aldehyde (ketone) hydrazone and a tetrahydrofuran solution of ZrX4 to reaction to obtain the complex, wherein the tetrahydrofuran solution of ZrX4 is same as the furan aldehyde (ketone) hydrazone in molar weight. The complex and alkylaluminoxane are formed into a catalytic system for catalyzing vinyl polymerization. Experimental results show that the catalytic system adopted by the invention can be used for preparing ultra-high molecular weight polyethylene with the weight-average molecular weight ranging from 2.3*106g / mol to 7.3*106g / mol, and has moderate catalytic activity. The complex provided by the invention is simple and easy to prepare, easy for obtaining raw materials, high in yield, easy for purification and the like.

Description

technical field [0001] The invention relates to a zirconium metal complex, specifically a zirconium metal complex of furan aldehyde (ketone) hydrazone, a preparation method thereof, and its application as a catalyst for preparing ultra-high molecular weight polyethylene. Background technique [0002] Ultra-high molecular weight polyethylene (UHMWPE) is a thermoplastic with a molecular weight greater than one million. Long molecular chain means higher molecular weight, and the main advantages given to UHMWPE are high hardness, toughness, wear resistance and stress crack resistance. In addition, UHMWPE also has good lubricity, chemical resistance and excellent electrical properties. Due to the excellent physical properties of ultra-high molecular weight polyethylene, it is widely used in the fields of machinery, transportation, textile, papermaking, mining, agriculture, chemical industry and sports equipment, such as mechanical parts, running parts of looms, bearings, Gears,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/00C08F10/02C08F4/642
CPCY02P20/52
Inventor 段新娥童红波钞建宾魏学红刘滇生
Owner SHANXI UNIV
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