Metallocene complex, preparation method thereof and catalyst composition

一种茂金属配合物、缩酮的技术，应用在茂金属、化学仪器和方法、含周期表第3/13族元素的化合物等方向，能够解决研究未见报道等问题，达到改变电子效应、增加活性、高插入率的效果

Active Publication Date: 2015-04-29
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The transition metal compound with heterocyclic condensed five-membered ring π ligand and the olefin polymerization reaction using the transition metal compound have been studied now. They have the advantages of high activity and high molecular weight, but they all contain side chains, and they have greater The study of open-space monometallocene complexes without side chains has not been reported

Method used

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  • Metallocene complex, preparation method thereof and catalyst composition
  • Metallocene complex, preparation method thereof and catalyst composition
  • Metallocene complex, preparation method thereof and catalyst composition

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preparation example Construction

[0063] The present invention provides a method for preparing the metallocene complex represented by the above formula (I), comprising:

[0064] When the metallocene complex X shown in formula (I) 1 with X 2 When each is independently a C1-C20 alkoxy group, the metallocene complex represented by the formula (I) is prepared according to the following steps: under the condition of inert gas protection, the cyclopentadiene compound represented by the formula (II) The alkenyl ligand is reacted with the rare earth compound in the first organic solvent to obtain the metallocene complex represented by formula (I).

[0065]

[0066] Wherein, Ln is scandium (Sc), yttrium (Y) and one of the lanthanide fourteen elements with atomic number 57-71;

[0067] R 1 , R 2 , R 3 , R 4 with R 5 each independently selected from H, C1-C20 alkyl, C1-C20 alkyl containing acetal, C1-C20 alkyl containing ketal, C1-C20 alkyl containing ether group, C1-C20 Alkenyl group, C1-C20 alkenyl group con...

Embodiment 1

[0105] Under the condition of nitrogen protection, 0.3g (1.56mmol) of thiophene-fused cyclopentadienyl ligand 1 was dissolved in 8ml of n-hexane, and added dropwise to the solution containing 0.7g (1.56mmol) of Sc(CH 2 SiMe 3 ) 3 (thf) 2 In n-hexane solution, react for 12h, concentrate the reaction solution, and recrystallize to obtain 0.57g of pale yellow thiophene-fused scandium-type scandium complex (I-1), molecular formula C 22 h 41 OSScSi 2 , the productive rate is 75%, and the reaction formula is as follows:

[0106]

[0107] The elemental analysis (%) of the scandium alkyl complex (I-1) obtained in Example 1 was analyzed, and the elemental analysis (%) result was: C58.52; H8.85.

Embodiment 2

[0109] Ligand 1 in Example 1 was replaced by ligand 2, and the rest of the steps were the same to obtain a thiophene-fused scandium-type complex (I-2), molecular formula C 24 h 45 OSScSi 2 , the reaction formula is as follows:

[0110]

[0111] The cenecene-type scandium alkyl complex (I-2) obtained in Example 2 is analyzed by nuclear magnetic resonance, and its hydrogen nuclear magnetic resonance spectrum is obtained, as shown in figure 1 shown. The NMR results are:

[0112] 1 H NMR (C 6 D. 6 ,25℃): δ3.59(br s, 2H, THF), 3.50(br s, 2H, THF), 2.41(s,3H), 2.19(s,3H), 2.15(s,6H), 2.09( s,1H),1.19(br s,4H),0.30(s,18H,CH 2 SiMe 3 ),-0.23(br s,2H,CH 2 SiMe 3 ),-0.28(d,J=0.08Hz,1H,CH 2 SiMe 3 ),-0.37(d,J=0.08Hz,1H,CH 2 SiMe 3 )ppm.

[0113] 13 CNMR (C 6 D. 6 ,25℃): δ133.31, 130.43, 126.24, 124.77, 121.80, 110.18, 109.12, 71.54, 24.96, 24.77, 13.87, 13.30, 13.03, 12.68, 12.64, 12.28, 4.34ppm.

[0114] The elemental analysis (%) of the scandium alkyl complex (I-...

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Abstract

Provided are a metallocene complex, a preparation method therefor, and a catalyst composition. The catalyst composition comprises a metallocene complex as represented by formula (I) and an organic boron salt. In contrast to the prior art, the metallocene complex as represented by the catalyst formula (I) used in the present invention contains no side chain, and has a large open degree of coordination space of the central metal, therefore having a higher catalytic activity and a higher insertion rate for strongly sterically hindered monomers. Moreover, the metallocene complex as represented by formula (I) used in the present invention is a fused heterocyclic cyclopentadienyl ligand, wherein the heterocycle has a strong capacity of supplying electrons, which can be used for fusing the cyclopentadienyl and changing the electronic effect in the metal centre so as to increase the activity of the catalyst. Hence, the metallocene complex as represented by formula (I) can be used for the preparation of a copolymer of ethylene and other alkenes with a high activity and a high insertion rate, and can also be used for catalyzing the polymerization of styrene and substituted styrene with high syndiotacticity and high activity.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a metallocene complex, a preparation method thereof, and a catalyst composition. Background technique [0002] Metallocene complexes refer to compounds in which the central metal is coordinated with one or more cyclopentadienyl groups or their derivatives, and play a very important role as catalysts in various polymerization reactions. Among them, a metal complex combined with one cyclopentadienyl group or one derivative becomes a monometallocene complex. Due to the different types of central metals, the metallocene complexes have completely different characteristics, such as catalytic activity for polymerization reactions, especially in the successful preparation and as an efficient activating reagent organoborane B (C 6 f 5 ) 3 and organoboron salts [Ph 3 C][B(C 6 f 5 ) 4 ] and [PhNMe 2 H][B(C 6 f 5 ) 4 ] Afterwards, monocene rare earth metal-organic co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F19/00C08F4/52C08F112/08C08F210/02C08F212/08C08F232/08C08F210/16C08F232/06
CPCC07F19/00C08F2420/06C07F5/00C07F17/00C08F210/02C08F236/20C08F2500/25C08F112/08C08F2500/03C08F212/08C08F210/16C08F210/14C08F232/00C08F4/54C08F10/00C08F4/52C08F36/20C08F12/08C08F4/58
Inventor 崔冬梅吴春姬姚昌广
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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