Bridged diamidino titanium metal catalyst, and preparation method and application thereof

A catalyst, titanium metal technology, applied in the direction of titanium organic compounds, etc., can solve the problems of harsh catalyst storage conditions, low catalyst total yield, unsuitable preparation of raw materials, etc., and achieve the effects of low price, high yield and simple preparation method.

Inactive Publication Date: 2012-05-02
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, they all have defects such as harsh synthesis conditions and low total catalyst yield. In addition, the storage conditions of the catalyst are also very harsh, easy to deactivate, and the synthesis method is complicated, and the raw materials are not suitable for preparation. Therefore, new non-metallocene catalysts has become a research hotspot in recent years

Method used

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  • Bridged diamidino titanium metal catalyst, and preparation method and application thereof
  • Bridged diamidino titanium metal catalyst, and preparation method and application thereof
  • Bridged diamidino titanium metal catalyst, and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Preparation and characterization of embodiment 1 catalyst

[0018] (1) Preparation of Lithium Salt of Bridged Diamidino Ligand

[0019] Under the protection of nitrogen and ice-water bath, tert-butylamine (1.01ml, 9.52mmol) was dissolved in diethyl ether (30cm 3 ), under stirring, slowly add butyllithium in n-hexane solution (2.2mol dm -3 , 4.3cm 3 , 9.52mmol), continued to stir for 3 hours, cooled the reaction solution to 0°C in an ice-water bath, and added 1-naphthonitrile (1.31cm 3 , 9.52mmol), continued to stir for 6 hours, then cooled the reaction solution to 0°C, added dichlorodimethylsilane (0.58cm 3 , 4.76mmol), filtered after reacting for 6 hours, the obtained solution was cooled to 0°C, and a n-hexane solution of butyllithium (2.2mol dm -3 , 4.3cm 3 , 9.52mmol), stirred for 3 hours, concentrated and crystallized to obtain a colorless crystal-like bridged bisamidinyl ligand lithium salt;

[0020] (2) Dissolve the bridged bisamidinyl ligand lithium salt (0...

Embodiment 2

[0024] 1. The preparation of catalyst is the same as in Example 1.

[0025] 2. Ethylene polymerization: Vacuumize a 250 ml stainless steel kettle equipped with a mechanical stirrer and a thermocouple, replace it with nitrogen for 3 times, and then replace it with ethylene for 2 times. After heating up to 50°C, add catalyst (4.4mg, 5μmol) in toluene solution and a certain amount of toluene in sequence, then add methylaluminoxane (1.67mol / L, 4.5ml) to make Al / Zr=1500, and finally add a certain amount of Measure the total volume of toluene to 100 mL. The ethylene pressure was immediately raised to 10 atm and stirred vigorously at 50°C for 30 minutes. The reaction solution was poured out, neutralized by adding 5% hydrochloric acid ethanol solution, and a white solid was precipitated. Filter and dry naturally. Obtained product 0.0412 g, polymerization activity: 1.65×10 4 g mol(Zr) -1 h -1 .

Embodiment 3

[0027] 1. The preparation of catalyst is the same as in Example 1.

[0028]2. Ethylene polymerization: Vacuumize a 250 ml stainless steel kettle equipped with a mechanical stirrer and a thermocouple, replace it with nitrogen for 3 times, and then replace it with ethylene for 2 times. After heating up to 50°C, add catalyst (4.0mg, 5μmol) in toluene solution and a certain amount of toluene in sequence, then add methylaluminoxane (1.67mol / L, 6.0ml) to make Al / Zr=2000, and finally add a certain amount of Measure the total volume of toluene to 100 mL. The ethylene pressure was immediately raised to 10 atm and stirred vigorously at 50°C for 30 minutes. The reaction solution was poured out, neutralized by adding 5% hydrochloric acid ethanol solution, and a white solid was precipitated. Filter and dry naturally. Obtained product 0.0740 g, polymerization activity: 2.96×10 4 g mol(Zr) -1 h -1 .

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Abstract

The invention provides a bridged diamidino titanium metal catalyst, which relates to olefin polymerization catalysts and specifically to a catalyst of diamidino ligand titanium complex characteristic of N-C-N-Si-N-C, with titanium atoms as a center. A preparation method for the catalyst comprises the following steps: under the protection of nitrogen, with tert-butylamine as a starting raw material, converting tert-butylamine into a lithium salt by using n-butyllithium; adding 1-naphthonitrile and carrying out an addition reaction; preparing bridged diamidino neutral ligand through bridging of dichlorodimethylsilane; converting the bridged diamidino neutral ligand into diamidino ligand by using n-butyllithium; reacting the diamidino ligand with titanium tetrachloride to prepare the catalyst. According to the invention, reaction conditions are mild, materials used are simple, easily available and cheap, reaction steps are simple, and yield of the catalyst is high; the catalyst has good catalytic activity on ethylene polymerization.

Description

technical field [0001] The invention relates to a transition metal catalyst for ethylene polymerization, in particular to a bridged bis-amidino ligand titanium metal complex catalyst with an N-C-N-Si-N-C-N skeleton, a preparation method and application thereof. Background technique [0002] One of the keys to the development of the polyolefin industry lies in the catalyst, and the development and innovation of the polyolefin industry are often inseparable from the innovation of the catalyst. Ziegler and Natta respectively use TiCl 4 / AlEt 3 and TiCl 3 / AlEt 2 The catalyst system composed of Cl successfully prepared linear high-density polyethylene and isotactic polypropylene under normal pressure conditions, creating a new era for the polyolefin industry. Brintzinger reported that a class of bridged metallocene catalysts not only has high activity, but also can control the stereo configuration of polymers (H. Schnutenhaus, H.H. Brintzinger, Angew. Chem, Int. Ed., 1979, 1...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/76C08F10/02C07F7/28
Inventor 白生弟刘瑞琴关飞刘滇生
Owner SHANXI UNIV
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