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Binuclear rare earth olefin polymerization catalyst and application thereof

A technology of olefin polymerization and catalyst, which is applied in the field of catalysts for binuclear rare earth olefin polymerization, and achieves the effect of high stereoregularity and high catalytic activity

Active Publication Date: 2020-09-04
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some previously reported dinuclear or polynuclear rare earth metal complexes are usually bridged by H or alkyl σ bond coordination (Macromolecules 2004, 37, 5860; Macromolecules 2006, 39, 1359-1363; ChemComm, 2015, 51, 5063 -5065), or through the connection of two monovalent ligands by phenyl, ferrocene and other groups (CN201210117207, CN201711172220), and the bifunctional rare earth metal complex is bridged by adding a bifunctional Lewis base Not yet reported

Method used

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  • Binuclear rare earth olefin polymerization catalyst and application thereof
  • Binuclear rare earth olefin polymerization catalyst and application thereof
  • Binuclear rare earth olefin polymerization catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Preparation of mononuclear rare earth complex 1

[0040]

[0041] At 0°C, n-butyllithium was slowly added dropwise to the hexane solution of Cp*, then naturally warmed to room temperature and stirred overnight, resulting in a large amount of pale yellow precipitate. Subsequently, suction filtration was carried out in an inert gas glove box, the obtained solid was washed twice with hexane, and dried under vacuum to obtain a light yellow powder solid which was the Cp*Li compound. At room temperature, the THF solution of Cp*Li was slowly added dropwise to YCl 3 .nTHF in THF suspension, then heated to reflux overnight. After the reaction, the THF solution was drained, and toluene was added for extraction. Concentrate the toluene extract and recrystallize at -30°C to obtain a white solid that is the rare earth chloride Cp* 2 YCl 2 Li(THF) 2 .

[0042] At -30°C, a toluene solution of o-dimethylaminobenzyllithium (AbzLi) was slowly added dropwise to Cp* 2 YCl 2 Li(T...

Embodiment 2

[0045] Preparation of mononuclear rare earth complex 2

[0046]

[0047] At -30°C, alkyllithium (TMSCH 2 The toluene solution of Li) is slowly added dropwise to Cp* 2 YCl 2 Li(THF) 2 In the toluene solution, the reaction was continued for 4 h after naturally rising to room temperature. After the reaction is completed, filter with a sand core funnel, and the filtrate is dried under vacuum to obtain a yellow oil, which is washed with a small amount of n-hexane to obtain a light yellow powder, which is Cp* 2 YACH 2 TMS product (compound 2).

[0048] NMR data: 1 H-NMR (600MHz, C6D6): 0.00 (s, 2H, CH2TMS), 0.44 (s, 9H, SiMe3), 1.98 (s, 30H, Cp-Me).

Embodiment 3

[0050] Preparation of mononuclear rare earth complex 3

[0051]

[0052] The synthesis of compound 3 refers to the synthesis of compound 1, YCl in the starting material 3 .nTHF replaced with GdCl 3 .nTHF, the experimental procedure is the same, the product obtained is light yellow powder solid. Due to the paramagnetic characteristics of the +3-valent Gd compound, NMR characterization cannot be performed, only for Cp* 2 GdCl 2 Li(THF) 2 X-ray single crystal diffraction characterization was carried out.

[0053]

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Abstract

The invention relates to a binuclear rare earth olefin polymerization catalyst and an application thereof. The binuclear rare earth olefin polymerization catalyst is composed of a main catalyst, a cocatalyst and a chain transfer reagent, the main catalyst is a binuclear rare earth complex stabilized by Lewis base and is represented by a chemical formula [I] and a chemical formula [II], and Ln is atransition metal element of the IIIB group in the periodic table of elements. The binuclear rare earth olefin polymerization catalyst is suitable for solution polymerization and can catalyze polymerization of 1,3-butadiene with high activity, and polybutadiene rubber prepared through the polymerization reaction has high cis-1, 4-content and narrow molecular weight distribution; compared with a corresponding mononuclear rare earth complex, the complex has the advantages of activity and stereoselectivity.

Description

technical field [0001] The technical field of the present invention relates to a catalyst for dinuclear rare earth olefin polymerization, in particular to a Lewis base-stabilized dinuclear dicene rare earth olefin polymerization catalyst and its application. Background technique [0002] The catalyst system for olefin rubber is the key to the production technology of olefin rubber. The catalyst systems currently used mainly include nickel (Ni) series, titanium (Ti) series, cobalt (Co) series, rare earth neodymium (Nd) series and lithium (Li) series. Department, etc. (Jiang Liansheng et al., Rare Earth Butadiene Rubber. Metallurgical Industry Press, 2016, 39). Among them, the rare earth catalyst is the most distinctive variety with excellent comprehensive performance. The olefin rubber produced by it has a high cis-structure content, a high linear structure regularity, a high molecular weight and a narrow distribution. [0003] In 1970, Changchun Institute of Applied Chemist...

Claims

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Application Information

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IPC IPC(8): C08F136/06C08F4/52C08F4/54C08F4/58
CPCC08F136/06C08F2410/03C08F2420/01C08F4/545C08F4/58
Inventor 胡泓梵周生远李新乐孙鑫张雪芹辛世煊
Owner PETROCHINA CO LTD
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