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A catalyst for regulating side arm effect, its preparation method and its application

A catalyst and reaction technology, applied in the field of catalysts regulated by the sidearm effect, can solve problems such as low activity, low copolymer molecular weight, low insertion ratio, etc.

Active Publication Date: 2020-01-03
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there have been extensive studies on such catalysts, many catalysts exhibit low activity, low copolymer molecular weight, low insertion ratio

Method used

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  • A catalyst for regulating side arm effect, its preparation method and its application
  • A catalyst for regulating side arm effect, its preparation method and its application
  • A catalyst for regulating side arm effect, its preparation method and its application

Examples

Experimental program
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preparation example Construction

[0064] The present invention provides a kind of preparation method of the catalyst described in above-mentioned technical scheme, comprises the following steps:

[0065] reacting a compound having a structure shown in formula (II) with a precursor compound in an organic solvent to obtain a catalyst having a structure shown in formula (I);

[0066]

[0067] The precursor compound is selected from trans-[(Y) 2 Ni(Cl)R 7 ] nickel precursor compound and / or (tmeda)Pd(R 6 ) 2 The palladium precursor compound, tmeda is tetramethylethylenediamine.

[0068] In the present invention, the organic solvent is preferably selected from tetrahydrofuran, petroleum ether, toluene, benzene, methylene chloride, tetrachloromethane, ether, 1,4-dioxane and 1,2-dichloroethane One or more; more preferably selected from 1,4-dioxane.

[0069] In the present invention, the trans-[(Y) 2 Ni(Cl)R 7 ] The nickel precursor compound is preferably trans-[(PPh 3 ) 2 Ni(Cl)Ph], Ph is an aryl group.

...

Embodiment 1

[0098] Embodiment 1: the preparation of 2-((2-methoxyphenyl) (phenyl) phosphino) benzenesulfonic acid

[0099]

[0100]At 0°C, n-butyllithium (concentration of 2.5 moles per liter, 8 milliliters, 20 millimoles) was slowly added dropwise to a mixture of benzenesulfonic acid (1.58 grams, 10 millimoles) dissolved in 25 milliliters of tetrahydrofuran, reaction 1 Hour. Then, a mixed solution of phenylphosphine dichloride (1.35 ml, 10 mmol) dissolved in 25 ml of tetrahydrofuran was added thereto, and reacted at room temperature for 2 hours to obtain a mixed solution A. 2-Bromoanisole (1.86 g, 10 mmol) was dissolved in 20 ml of tetrahydrofuran under nitrogen protection and cooled to minus 78°C. n-Butyllithium (concentration: 2.5 moles per liter, 4 milliliters, 10 millimoles) was added slowly, and reacted at minus 78° C. for 1 hour. The obtained lithium salt was added to the mixed solution A at minus 78°C, and reacted at room temperature for 24 hours. The solvent was spin-dried,...

Embodiment 2

[0101] Embodiment 2: the preparation of 2-((2-phenoxyphenyl) (phenyl) phosphino) benzenesulfonic acid

[0102]

[0103] The synthesis procedure is the same as in Example 1, except that 1-bromo-2-phenoxybenzene (2.49 grams, 10 mmol) was added to obtain a white solid (2.8 g, 65% yield), i.e. 2-( (2-phenoxyphenyl)(phenyl)phosphino)benzenesulfonic acid. 1 H NMR (400MHz, CDCl3) δ8.39 (dd, J = 7.2, 5.1Hz, 1H), 7.84-7.71 (m, 2H), 7.70-7.57 (m, 5H), 7.49 (m, 1H), 7.41- 7.26(m,4H),7.26-7.14(m,2H),6.96-6.82(m,3H).13C NMR(100MHz,CDCl3)δ160.27(d,J=1.8Hz),153.93(s),152.79 (d, J=9.0Hz), 136.71(d, J=2.0Hz), 135.25(s), 135.17(s), 134.75(d, J=12.1Hz), 134.37(d, J=2.9Hz), 133.15 (d, J=11.3Hz), 130.21(s), 130.04(d, J=13.3Hz), 129.84(d, J=13.2Hz), 129.31(d, J=9.3Hz), 125.72(s), 123.92 (d, J=13.4Hz), 120.27(s), 119.01(d, J=88.5Hz), 116.67(d, J=6.2Hz), 112.38(d, J=97.3Hz), 108.48(d, J= 97.5Hz).31P NMR (162MHz, CDCl3) δ-1.14. ESI-MS (m / z): [M-H] - Calculated: C24H18O4PS, 433.0658; Found: 433...

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Abstract

The invention provides a catalyst regulated by the side arm effect, a preparation method and application thereof. The catalyst has the structure shown in the formula (I). The catalyst can catalyze lowcarbon olefin polymerization or copolymerization of C2-C6, has the very high heat stability and activity on low carbon olefin polymerization of C2-C6, and produces poly-low carbon olefin with the linearity and high molecular weight. The catalyst has the catalytic effect on copolymerization of low carbon olefin of C2-C6 and methyl acrylate to produce a copolymer of a polar monomer with the high molecular weight, and the catalyst has the high insertion ratio. The test result shows that the catalyst catalyzes homopolymerization of ethylene, the activity can be as high as 8.7; the number-averagemolecular weight is as high as 105100g / mol; the number-average molecular weight of the copolymer product of ethylene and methyl acrylate is as high as 82500g / mol; and the highest insertion ratio of methyl acrylate is 21.4%. The formula I is shown in the description.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a catalyst regulated by the side arm effect, its preparation method and its application. Background technique [0002] Polyolefins have low prices and excellent physical properties, making them indispensable materials in today's society. In olefin polymerization, catalysts determine olefin polymerization behavior, polymer structure and properties, and polymer particle morphology. The development of olefin polymerization catalysts makes polyolefin products rich in variety and excellent in performance, and promotes the development of the whole polyolefin. [0003] Among them, late transition metal catalysts occupy an important position in the field of olefin polymerization. The development of new catalysts is the key to realize high-performance polyolefin materials. For example, diimide palladium and nickel catalysts can synthesize polyolefin materials with different topologie...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/80C07F15/00C07F15/04C08F110/02C08F210/02C08F220/14
CPCC07F15/006C07F15/04C08F4/80C08F110/02C08F210/02C08F220/14
Inventor 陈昶乐梁涛
Owner UNIV OF SCI & TECH OF CHINA