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Metal coordination compound, intermediate, preparation method and application thereof

A technology of metal complexes and coordination bonds, applied in the preparation of imino compounds, nickel organic compounds, chemical instruments and methods, etc.

Active Publication Date: 2021-02-23
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, catalysts that can simultaneously achieve high activity and high insertion rate to catalyze the copolymerization of ethylene and bulk commercialized polar monomers to obtain high molecular weight copolymers have not been reported yet.

Method used

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  • Metal coordination compound, intermediate, preparation method and application thereof
  • Metal coordination compound, intermediate, preparation method and application thereof
  • Metal coordination compound, intermediate, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0314] The synthesis of embodiment 1 compound II

[0315] The preparation method of compound II-1 is as follows:

[0316] Under the action of 12.5g (125mmol) acetylacetone and 44.3g (250mmol) 2,6-diisopropylaniline under the action of 10.6mL (125mmol) concentrated hydrochloric acid, 44.2g of compound IV-1 can be successfully obtained with a yield of 81%. The compound is oxidized by oxygen under the action of 1 equivalent of copper acetate to obtain compound III-1, followed by AlMe 3 The addition gave product II-1 with a total yield of 65% in three steps and a total of 36 g.

[0317]

[0318] The preparation method of compound II-11 is as follows:

[0319] Dissolve 19.4g (193.8mmol) of acetylacetone and 33.8g (190.87mmol) of 2,6-diisopropylaniline in 100mL of toluene, add about 1.0g (2%) of p-toluenesulfonic acid monohydrate, and heat up to reflux Divide water until no water comes out. Then the solvent was removed under reduced pressure, and the residue was distilled und...

Embodiment 2

[0378] The synthesis of embodiment 2 complex I-1

[0379] Compound II-1 (0.67 g, 1.5 mmol) in tetrahydrofuran was slowly added dropwise to KH (0.12 g, 3.0 mmol) in tetrahydrofuran at room temperature, and a large number of bubbles were generated during the dropwise addition. The dropwise addition was completed within ten minutes, and after 12 hours of reaction, it was filtered through diatomaceous earth. The filtrate was slowly added dropwise to NiBr at room temperature 2 (DME) (0.92g, 3.0mmol) in tetrahydrofuran solution, reacted overnight. The solvent was removed under reduced pressure, toluene was added, KBr was removed by filtration, the filtrate was concentrated and recrystallized by adding a small amount of hexane to obtain 1.02 g of red solid I-1 with a yield of 83%.

[0380]

[0381] Elemental analysis: measured (calculated value): C: 48.25 (48.09); H: 6.16 (6.27); N: 3.11 (2.95).

[0382] The coordinating solvent tetrahydrofuran can be removed by conventional dr...

Embodiment 3

[0383] The synthesis of embodiment 3 complex I-2~I-54

[0384] Obtain other compound I-2 (productive rate 65%) with the experimental method identical with embodiment 2; I-3 (productive rate 71%); I-4 (productive rate 59%); I-5 (productive rate 63% ); I-6 (yield 74%); I-7 (yield 76%); I-8 (yield 64%); I-9 (yield 67%); I-10 (yield 55% ); I-11 (55% yield); I-12 (75% yield); I-13 (72% yield); I-14 (58% yield); I-15 (66% yield ); I-16 (61% yield); I-17 (72% yield); I-18 (54% yield); I-19 (67% yield); I-20 (77% yield ); I-21 (yield 68%); I-22 (yield 71%); I-23 (yield 12%); I-24 (yield 38%); I-25 (yield 40% ); I-26 (45% yield); I-27 (50% yield); I-28 (48% yield); I-29 (47% yield); I-30 (36% yield ); I-31 (60% yield); I-32 (3% yield); I-33 (23% yield); I-34 (59% yield); I-35 (16% yield ); I-36 (yield 30%); I-37 (yield 56%); I-38 (yield 54%); I-39 (yield 12%); I-40 (yield 18% ); I-41 (45% yield); I-42 (43% yield); I-43 (25% yield); I-44 (15% yield); I-45 (19% yield ); I-46 (23% y...

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Abstract

The invention discloses a metal coordination compound, an intermediate, a preparation method and application thereof, and provides a metal coordination compound I, which can be independently used forcatalyzing ethylene homopolymerization or used for catalyzing ethylene homopolymerization under the action of a cocatalyst, wherein the catalytic activity can reach up to 10<6> g / (mol Metal) h, the prepared polyethylene has the characteristics that the molecular weight is high, the Mn can reach 10<5>-10<6> g / mol, and the molecular weight distribution is narrow, the prepared polyethylene contains alkane branched chains of 5-40 branched chains / 1000 carbon, in the alkane branched chain, the proportion of a methyl branched chain is 0.60-0.95, the proportion of an ethyl branched chain is 0.01-0.05,the proportion of a propyl branched chain is 0.01-0.05, the proportion of a sec-butyl branched chain is 0.01-0.05, and the proportion of a branched chain greater than C4 is 0.01-0.10, and the meltingtemperature of the polymer is 70-130 DEG C.

Description

technical field [0001] The invention relates to a metal complex, an intermediate, its preparation method and application. Background technique [0002] Since the discovery of the Ziegler-Natta catalyst in the 1950s, highly active MgCl 2 Supported titanium catalysts show good catalytic performance (K.Ziegler et al., Angew.Chem.1995,67,424; K.Ziegler et al., Angew.Chem.1995,67,541; N.Kashiwa et al., USP-3642746,1968) , At present, this catalyst has been used in the industry for the production of high-density polyethylene (HDPE), linear low-density polyethylene (LLDPE), and syndiotactic polypropylene (i-pp). However, this multi-active-site solid catalyst is currently unable to control the polymer structure and performance by adjusting the catalyst structure; the discovery of the fourth group of metallocene catalysts has solved this problem better, because it has a single , so that people can obtain polymers of expected structure (W.Kaminsky et al., Adv.Organomet.Chem.1980,18,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/04C07F15/00C07C251/08C07C251/06C07C251/12C07C251/16C07C249/02C08F110/02C08F210/02C08F4/70
CPCC07F15/045C07F15/0066C07C251/08C07C251/06C07C251/12C07C251/16C07C249/02C08F110/02C08F210/02C07C2601/08C07C2601/14C08F4/7098C08F4/70
Inventor 唐勇季刚宁小山孙秀丽彭爱青
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI