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O-methoxy phenylhydrazone dicaryon metal complex and preparation method and application thereof

A technology of o-methoxyphenylhydrazone and o-methoxy, which is applied in the application field of preparing high molecular weight polyethylene catalysts, and achieves the effects of high yield, cheap and easy-to-obtain raw materials, and simple and easy preparation methods

Inactive Publication Date: 2016-04-20
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Relatively speaking, binuclear non-metallocene catalysts are still in their infancy. Although many articles have been published in recent years, most of them remain on compound synthesis and molecular structure identification. The catalytic mechanism, the structure-activity relationship between catalyst structure and catalytic activity are still to be investigated. Further research [Nie Yujing et al., Industrial Catalysis, 2010,18(1), 1008-1143; Nie Yujing et al., Industrial Catalysis, 2010,18(2), 7-11]

Method used

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  • O-methoxy phenylhydrazone dicaryon metal complex and preparation method and application thereof
  • O-methoxy phenylhydrazone dicaryon metal complex and preparation method and application thereof
  • O-methoxy phenylhydrazone dicaryon metal complex and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0025] The preparation of embodiment 1 binuclear titanium metal complex

[0026] (1) Preparation of ligand o-methoxyphenylhydrazone:

[0027] Method 1: Add 2.72g (20mmol) of phenylhydrazine to the Schlenk reaction flask, and add o-methoxybenzaldehyde (2.16g, 20mmol) in an equimolar amount at room temperature, the reaction is exothermic, and the resulting molten reaction solution Stirring was continued until it was solidified, and then the light yellow crystalline solid obtained by recrystallization with hot n-hexane was the target ligand o-methoxybenzaldehyde phenylhydrazone (4.02 g), and the yield was 89%.

[0028] Method 2: Add o-methoxybenzaldehyde (2.16g, 20mmol) and 20mL of ethanol in a Schlenk reaction flask, add an equimolar amount of phenylhydrazine (2.72g, 20mmol) dropwise at 0°C, and the reaction solution gradually rises to room temperature , continue to stir and react overnight, concentrate under reduced pressure to generate a solid, filter, and recrystallize the o...

Embodiment 2

[0031] The application of embodiment 2 complex as catalyst in catalytic ethylene polymerization (MAO is as cocatalyst)

[0032] Aggregation condition selection:

[0033] At 10atm, when the molar ratio of MAO:catalyst is 1000:1, the temperature is changed, and the activity at 20°C, 30°C, 40°C, and 50°C is tested respectively, and the activity is 1.2×10 5 , 1.5×10 5 , 1.2×10 5 , 1.0×10 5 gPE / mol(Cat.) h. When the temperature was 30°C, the molar ratios of MAO:catalyst were tested at 1500:1, 2000:1, and 2500:1 respectively, and the activity was 1.7×10 5 , 2.9×10 5 , 2.6×10 5 gPE / mol(Cat.) h.

[0034] (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 steel cylinder, which can continuously replenish ethylene through a spiral steel pipe, so as to maintain a constant pressure (under 10atm pressure) during the polymerization reaction. ). After the polymerizati...

Embodiment 3

[0041] The application of embodiment 3 complex as catalyst in catalytic ethylene polymerization (MMAO is as cocatalyst)

[0042] Aggregation condition selection:

[0043] At 10atm, at a temperature of 30°C, the MMAO:catalyst molar ratios of 1000:1, 1500:1, 2000:1, and 2500:1 were respectively tested for their activities, which were 2.4×10 4 , 5.4×10 4 , 4.4×10 4 , 3.0×10 4 gPE / mol(Cat.) h. When the molar ratio of MMAO:catalyst is 1500:1, the temperature is changed, and the activity at 20°C, 40°C, and 50°C is tested respectively, which are 5.2×10 4 , 4.8×10 4 , 4.4×10 4 gPE / mol(Cat.) h.

[0044] (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 steel cylinder, which can continuously replenish ethylene through a spiral steel pipe, so as to maintain a constant pressure (under 10atm pressure) during the polymerization reaction. ). After the polymerization...

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Abstract

The invention provides an o-methoxy phenylhydrazone dicaryon metal complex, a preparation method thereof. The complex is used as a catalyst for preparing high-molecular-weight polyethylene. The complex is obtained through the method including the steps that o-methoxy phenylhydrazone reacts with a tetrahydrofuran solution with a half of molar weight of TiX4(THF)2 after being subjected to the hydrogen abstraction together with lithium diisopropylamide (LDA). The prepared dual-core dicaryon complex serving as the catalyst is easy to prepare, applied raw materials are low in price and easy to obtain, and the activation of methylaluminoxane (MAO) or modified methylaluminoxane (MMAO) can be used for catalyzing vinyl polymerization. It is shown through experiment results that the catalyst system can be used for preparing high-molecular-weight linear polyethylene, and most of obtained polyethylene has the weight-average molecular weight above one million, the high melting point between 133.4 DEG C and 134.8 DEG C, the molecular weight between 1.90 and 3.33 and intermediate catalysis activity.

Description

technical field [0001] The invention relates to a dinuclear titanium metal complex, in particular to a dinuclear titanium metal complex of o-methoxyphenylhydrazone, a preparation method thereof, and an application thereof as a catalyst for preparing high molecular weight polyethylene. Background technique [0002] Due to the fact that the molecule contains two central metal atoms at the same time, the binuclear metal catalyst has a special effect (that is, a synergistic effect) on each other, which can affect the activity of the olefin polymerization catalyst and the performance of the polymer. The melting point and crystallinity of the obtained polymer , molecular weight and molecular weight distribution have changed to a certain extent (Massimiliano, et al, Chem. Rev., 2011, 111, 2450-2485). For example, the metallocene olefin polymerization catalyst is a kind of olefin polymerization catalyst that has been industrialized very early. It has the characteristics of high cata...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/28C08F4/642C08F10/02
CPCC07F7/28C08F4/6401C08F4/6428C08F10/02
Inventor 段新娥白生弟魏学红刘滇生孙文华
Owner SHANXI UNIV
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