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),

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

Example Embodiment

[0038] Example 1

[0039] Preparation of mononuclear rare earth complex 1

[0040]

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

[0042] At -30℃, slowly drop the toluene solution of o-dimethylaminobenzyl lithium (AbzLi) to Cp* 2 YCl 2 Li(THF) 2 In t...

Example Embodiment

[0044] Example 2

[0045] Preparation of mononuclear rare earth complex 2

[0046]

[0047] -30℃, the alkyl lithium (TMSCH 2 Li) toluene solution is slowly added dropwise to Cp* 2 YCl 2 Li(THF) 2 In the toluene solution, the reaction was continued for 4h after naturally warming to room temperature. After the reaction is completed, filter with a sand core funnel, and the filtrate is drained under vacuum to obtain a yellow oil, and 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).

Example Embodiment

[0049] Example 3

[0050] Preparation of mononuclear rare earth complex 3

[0051]

[0052] The synthesis of compound 3 refers to the synthesis of compound 1, and the YCl in the starting material 3 .nTHF changed to GdCl 3 .nTHF, the experimental procedures are the same, and the resulting product is a pale yellow powder solid. Due to the paramagnetic characteristics of +3-valent Gd compounds, NMR characterization is not possible, only Cp* 2 GdCl 2 Li(THF) 2 X-ray single crystal diffraction characterization was performed.

[0053]

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PUM

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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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