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Ni-Pd metal complex as well as preparation method, application and product thereof and application of product

A technology of metal complexes and nickel-palladium, applied in the field of nickel-palladium metal complexes and their preparation, can solve the problems of uncontrollable regioselectivity and stereoregularity of polar monomers, nitrogen-heterocyclic carbene decomposition, and low activity , to achieve high catalytic activity and thermal stability

Active Publication Date: 2019-02-12
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The researchers introduced the above structure into ligands to synthesize transition metal olefin polymerization catalysts with various structures. These catalysts have many excellent properties, even comparable to classic metallocene catalysts, and can make α-olefins and vinyl polar monomers Direct copolymerization, but low activity, uncontrollable regioselectivity and stereoregularity of polar monomers, nitrogen heterocyclic carbene is easy to decompose due to self-reduction elimination, and it can catalyze olefin monomers such as norbornene at high temperature less active

Method used

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  • Ni-Pd metal complex as well as preparation method, application and product thereof and application of product
  • Ni-Pd metal complex as well as preparation method, application and product thereof and application of product
  • Ni-Pd metal complex as well as preparation method, application and product thereof and application of product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0084] The preparation method of metal complex, concrete steps are as follows:

[0085] (1) React urea compounds and oxalyl chloride in acetonitrile at 66°C for 12 hours to obtain imidazolidine chloride salt. After the reaction, the product is purified by recrystallization from toluene, wherein the chlorine atom in oxalyl chloride and urea The molar ratio of the compound is 5:1, and the urea compound is a compound with the structure of formula (a) and a compound with the structure of formula (c), in the formula, R 1 , R 4 , R 9 and R 12 is methyl, R 2 , R 3 , R 10 and R 11 is hydrogen, L is oxygen;

[0086] (2) react imidazolidine chloride salt, diamine compound and triethylamine in n-heptane at 60°C for 24h to obtain phenylenediamine imidazolidine ligand, wherein, imidazolidine chloride salt, diamine compound and The molar ratio of triethylamine is 2:1:4, and the structural formula of diamine compounds is as formula (e), wherein R 5 , R 6 , R 7 and R 8 is hydrogen...

Embodiment 2

[0091] The preparation method of metal complex, concrete steps are as follows:

[0092] (1) React urea compounds and phosgene in n-heptane at 60°C for 15 hours to obtain imidazolidine chloride salt. After the reaction, the product is purified by extraction with dichloromethane, wherein the chlorine atom in phosgene The molar ratio with urea compound is 4:1, and urea compound is the compound with formula (a) structure and the compound with formula (c) structure, in the formula, R 1 , R 4 , R 9 and R 12 is phenyl, R 2 , R 3 , R 10 and R 11 is hydrogen, L is oxygen;

[0093] (2) React imidazolidine chloride salts, diamine compounds and triethylamine in methylene chloride at 100°C for 10 h to obtain phenylenediamine imidazolidine ligands, wherein imidazolidine chloride salts, diamine compounds and The molar ratio of triethylamine is 2.3:1:2.2, and the structural formula of diamine compounds is as formula (e), wherein R 5 , R 6 , R 7 and R 8 is hydrogen;

[0094] (3) R...

Embodiment 3

[0098] The preparation method of metal complex, concrete steps are as follows:

[0099] (1) React urea compounds and triphosgene in toluene at 90° C. for 6 h to prepare imidazolidine chloride salts, wherein the molar ratio of chlorine atoms in triphosgene to urea compounds is 7:1, and urea compounds have The compound of formula (a) structure and the compound with formula (c) structure, in the formula, R 1 , R 4 , R 9 and R 12 is methyl, R 2 , R 3 , R 10 and R 11 is hydrogen, L is sulfur;

[0100] (2) React imidazolidine chloride salts, diamine compounds and triethylamine in acetonitrile at 90°C for 18 hours to obtain phenylenediamine imidazolidine ligands. After the reaction, the product is purified by extraction with chloroform , wherein, the molar ratio of imidazolidine chloride salt, diamine compound and triethylamine is 2:1:4, and the structural formula of diamine compound is as formula (e), wherein R 5 and R 8 for hydrogen, R 6 and R 7 is fluorine;

[0101] (...

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Abstract

The invention relates to a Ni-Pd metal complex as well as a preparation method, application and a product thereof and application of the product. The Ni-Pd complex is prepared through reaction of a phenylenediamine imidazolidine ligand and a metal precursor, and the structural formula of the prepared Ni-Pd metal complex is shown as follows: (the formula is shown in the description), wherein in theformula, R1-R12 are independently selected from hydrogen, alkyl, substituendum of alkyl, alkoxy, alkyl sulphanyl, halogen, nitryl, aryl and substituendum of aryl, M is Ni<2+> or Pd<2+>, and X and Y are independently selected from halogen and alkyl. The product of the Ni-Pd metal complex is mainly obtained by compounding the Ni-Pd metal complex and a promoter, and the Ni-Pd metal complex and the product thereof can both be used for catalyzing polymerization of olefine monomer. The method is easy to operate, the prepared Ni-Pd metal complex and the product thereof have high activity and good thermal stability, the number-average molecular weight and the insertion rate of the olefine polymer obtained through catalysis are high when the Ni-Pd metal complex is used for catalyzing the olefine monomer, and the Ni-Pd metal complex has very good popularization value.

Description

technical field [0001] The invention belongs to the field of olefin catalysis, and relates to a nickel-palladium metal complex and its preparation method, application, product and application of the product. Background technique [0002] Polyolefin has become the polymer material with the largest production volume, the fastest development speed and the most widely used. Its output accounts for more than one-third of the total polymer materials in the world. Among them, coordination polymerization catalysts are the core of the development of the polyolefin industry. . [0003] Polyolefin catalysts include Ziegler-Natta type heterogeneous catalysts (DE Pat 889229 (1953)), metallocene catalysts (Kaminsky.W., Berlin: Springer, 1999.), non-procene transition metal catalysts (Yasunori Y, Organometallics, 2001,20(23):4793-4799), late transition metal catalysts (Brookhart M., J.Am.Chem.Soc, 1995,117(23):6414-6415). Among them, late-transition metal catalysts have attracted extensi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/04C07F15/00C08F132/08C08F120/14C08F118/12C08F116/18C08F116/20C08F210/02C08F4/70
CPCC07F15/0066C07F15/045C08F116/18C08F116/20C08F118/12C08F120/14C08F132/08C08F210/02C08F4/7006
Inventor 蔡正国舒鑫李明远李彦青
Owner DONGHUA UNIV
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