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A kind of metal complex and its preparation method and the preparation method of olefin binary copolymer

A technology of olefin binary copolymers and metal complexes, which is applied in the fields of materials and chemicals, can solve the problems of inability to obtain polymers and insufficient catalytic efficiency, and achieve excellent mechanical and thermal properties

Active Publication Date: 2019-03-12
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalytic efficiency of such complexes is not enough, and some of them cannot even obtain polymers, so they can only be used for the research of catalytic mechanism and have no commercial practical value.

Method used

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  • A kind of metal complex and its preparation method and the preparation method of olefin binary copolymer
  • A kind of metal complex and its preparation method and the preparation method of olefin binary copolymer
  • A kind of metal complex and its preparation method and the preparation method of olefin binary copolymer

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0034] The preparation method provided by the present invention is to use a transition metal complex with a ligand of a specific structure as a catalyst component for α-olefin, acrylate, methacrylate, acrylic acid, unsaturated carboxylate, acrylamide, Acrylonitrile, unsaturated enol / ether, norbornene carboxylate and other monomers are copolymerized to obtain a polymer with a higher molecular weight, and the molecular chain structure is a binary copolymer. The ligand with a specific structure is a ligand that uses an aromatic heterocycle as a skeleton and is combined with two or more heteroatoms such as nitrogen, phosphorus, arsenic or antimony.

[0035] The present invention provides by reacting specific compounds (A) and / or (B) with transition metal complexes (C) including transition metals belonging to Group IVB to Group VIIB or Group VIII in the periodic table of elements such as nickel and palladium. The metal complex (D) is obtained. And it is provided that by making the...

Embodiment

[0128] The present invention is explained in detail in the following Examples and Comparative Examples, however, the present invention is not limited thereto.

[0129] In the following synthesis examples, unless otherwise stated, operations were performed under a purified nitrogen atmosphere, and dehydrated and deoxygenated solvents were used.

[0130] 1. Evaluation method

[0131] (1) Tm and Tc: Determined by the following DSC measurement.

[0132] Using a PYRIS Diamond DSC differential scanning calorimeter (PerkinElmer Inc.), sample 1 (approximately 5 mg) was melted at 210°C for 5 minutes, and then the temperature was decreased to -20°C at a rate of 10°C / min. After 5 minutes at -20°C, the temperature was raised to 210°C at a rate of 10°C / min to obtain a melting curve. The highest temperature of the main exothermic peak in the temperature lowering step was defined as the crystallization temperature Tc. In addition, the peak top temperature of the main endothermic peak in t...

Embodiment 1

[0135] Example 1: Synthesis of Ligand L1

[0136]

[0137] Add 1a (446mg, 2mmol) sequentially to a 50ml Schlenk bottle that was dried and replaced with nitrogen atmosphere, vacuumize and replace with nitrogen three times, add 15mL of freshly distilled diethyl ether into the syringe, and add n-butyllithium dropwise at -5°C Solution (2.4mmol, 2.3M, 1mL), the resulting reaction system rose to room temperature and reacted for 2h. Diphenylphosphine chloride 1c (0.5 g) was added dropwise at 0° C., and the resulting reaction solution was warmed to room temperature. The initially obtained clear solution gradually became cloudy. After 2 hours, the reaction stopped and a white solid precipitated out. Post-processing: It was detected by TLC spotting that the raw materials were basically completely consumed, and the organic phase was spin-dried and purified by column chromatography to obtain 420 mg of the product (52%).

[0138]

[0139] Dissolve 407mg of the above-mentioned raw ma...

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PUM

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Abstract

The invention discloses a metal complex and a preparation method thereof and a preparation method of an olefin binary copolymer. The metal complex is represented by the following general formula (D): wherein, M represents Group IVB to VIIB in the periodic table of elements transition metals of Group VIII or Group VIII; R 3 represents hydrogen or a hydrocarbon group of 1 to 20 carbon atoms and optionally contains heteroatoms; L 1 Indicates the ligand coordinated to M; X 1 Indicates oxygen or sulfur; E 1 and E 2 independently represent nitrogen, phosphorus, arsenic or antimony; R 4 Each independently represents hydrogen or a hydrocarbon group having 1-20 carbon atoms and optionally containing heteroatoms, wherein at least one R 4 It is a hydrocarbon group having more than 2 heteroatom-containing groups; the present invention also provides a preparation method of the above-mentioned metal complex and its application in olefin polymerization, using the complex of the present invention as a catalyst, can obtain high molecular weight, less linear chain polymer.

Description

technical field [0001] The invention belongs to the technical field of materials and chemicals, and in particular relates to a heteroatom-containing metal complex, a preparation method thereof, and a preparation method of an olefin binary copolymer. Background technique [0002] At present, in the industrial field, ethylene and monomers containing polar groups such as acrylate and vinyl acetate can be copolymerized under high temperature and high pressure conditions to obtain copolymers containing certain polar groups. However, due to the characteristics of the free radical reaction, the resulting copolymer has more branched chains, resulting in problems of low crystallinity and low strength. [0003] Using coordination metal compounds as catalysts to catalyze the copolymerization of ethylene and acrylate / methacrylate is a method that researchers have paid more attention to. As far as the current research situation is concerned, most of the late transition metals used are N...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/04C07F15/00C07F9/50C08F4/70C08F210/02C08F220/14C08F220/18C08F220/34C08F218/08C08F210/16
CPCC07F9/505C07F15/006C07F15/0086C07F15/04C08F210/02C08F210/16C08F220/1804C08F220/34
Inventor 辛世煊李勃天郎笑梅冉印李新乐薛山胡泓梵周生远孙鑫张雪芹马树刚
Owner PETROCHINA CO LTD
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