Bidentate ligand 4,4í»- bis (hydroxymethyl)-2,2í»dipyridine, preparation thereof and application to polyketone synthesis

A technology of bidentate ligand and dimethylol, which is applied in the field of catalysts for the synthesis of polyketones, can solve the problems of low catalytic activity and relative molecular weight, and achieve high relative molecular weight, good catalytic activity and improved relative molecular weight. Effect

Inactive Publication Date: 2008-11-12
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The currently used ligand is 2,2'-bipyridine. This catalytic system is used in the process of copolymerization of

Method used

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  • Bidentate ligand 4,4í»- bis (hydroxymethyl)-2,2í»dipyridine, preparation thereof and application to polyketone synthesis
  • Bidentate ligand 4,4í»- bis (hydroxymethyl)-2,2í»dipyridine, preparation thereof and application to polyketone synthesis
  • Bidentate ligand 4,4í»- bis (hydroxymethyl)-2,2í»dipyridine, preparation thereof and application to polyketone synthesis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 4,4'-dimethylol-2,2'-bipyridine synthesis reaction:

[0027]

[0028] Add the distilled 4-picoline and palladium-carbon catalyst in the ratio of 40:1 (g / g) to a 250mL three-necked flask in turn, stir, and heat in an oil bath after mixing evenly. Reflux at 160°C for 72h, stop the reaction, and filter after cooling. The filtrate was collected, and the resulting filtrate was distilled under reduced pressure until a white solid was precipitated. After collecting the solid, recrystallize it with ethyl acetate to obtain 4,4'-dimethyl-2,2'-bipyridyl crystals with a melting point of 171-172°C.

[0029] Under magnetic stirring, 9.7 mmol of Na 2 Cr 2 o 7 Slowly added to concentrated sulfuric acid, and after stirring for 30 min, 4.3 mmol of 4,4'-dimethyl-2,2'-bipyridine was further added thereto. Orange-yellow flocs were formed immediately in the solution, and the stirring was continued, the flocs gradually turned dark green, and the reaction stopped after 30 minutes. The...

Embodiment 2

[0038] Embodiment 2 (for comparison)

[0039] Under the same conditions as in Example 1, a copolymer of carbon monoxide and styrene was prepared. The difference is that the amount of bidentate ligand was changed from 0.1mmol to 0.125mmol to obtain 7.01g of copolymerized product with a catalytic activity of 1318gSTCO / gPd·h. Relative molecular mass M n =8450, M w =13275, M w / M n = 1.572.

Embodiment 3

[0040] Embodiment 3 (for comparison)

[0041] Under the same conditions as in Example 1, a copolymer of carbon monoxide and styrene was prepared. The difference is that the bidentate ligand was changed from 4,4'-dimethylol-2,2'-bipyridine to 2,2'-bipyridine, and 4.41 g of copolymerized product was obtained with a catalytic activity of 829 gSTCO / gPd h . Relative molecular mass M n =4392, Mw=6261, Mw / Mn=1.426.

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Abstract

The present invention relates to bidentate ligand 4,4'-dihydroxy methyl-2,2-dipyridine and an application for preparing and synthesizing silicone. The catalyzer for synthesizing the silicone comprises: acetic acid palladium, para-benzoquinone, paratoluenesulfonic acid, sulfamic acid, fluoboric acid or a mixture thereof, and the bidentate ligand 4,4'-dihydroxy methyl-2,2-dipyridine. Carbon monoxide and styrene which are raw materials is polymerized with absolute methanol which is a solvent, for 1 to 3 hours and at a condition that the catalyzer is existed, the temperature is 20 to 80 DEG C and the pressure is 1 to 10 MPa. The catalyzer is good in catalytic activity, the yield of the silicone is high, and the synthesized silicone is high in relative molecular weight. At a condition that the dosage of main catalyzer acetic acid palladium is the same, the addition of the 4,4'-dihydroxy methyl-2,2-dipyridine causes that not only the catalytic activity of the catalyzer is improved by 1 to 3 times, but also the relative molecular weight of the produced silicone is improved by 2 times.

Description

technical field [0001] The present invention relates to a catalyst for synthesizing polyketones, in particular to a bidentate ligand 4,4'-dimethylol-2,2'-bipyridine and the preparation and synthesis of polyketones, specifically 4,4'- Dimethylol-2,2'-bipyridine is used as a catalyst for the copolymerization of carbon monoxide and styrene to prepare polyketones. Background technique [0002] Today, as petroleum resources are dwindling, the coal chemical industry, which uses coal as raw material, has received attention again. Copolymerization of olefins with abundant and cheap carbon monoxide is one of the effective ways to manufacture functional polyolefins. Polyketone (STCO) is a linear strictly alternating copolymer prepared by the copolymerization of carbon monoxide (CO) and α-olefin. The raw material CO comes from a wide range of sources, reducing the cost compared to most materials synthesized from petroleum. More importantly, the carbonyl group on the polyketone main c...

Claims

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Application Information

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IPC IPC(8): C07D213/30C08G67/02
Inventor 郭锦棠赵海洋冯亚凯李鹏
Owner TIANJIN UNIV
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