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Catalyst for preparation of polyketone by copolymerization of carbon monoxide and phenylethene

A carbon monoxide and styrene technology, applied in the field of catalysts, can solve the problems of low catalytic activity, achieve the effects of reducing costs, improving catalytic activity, and reducing dosage

Inactive Publication Date: 2010-05-19
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 carbon monoxide and styrene into polyketones, and its catalytic activity is not high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Mix the distilled 4-picoline and palladium-carbon catalyst in a certain ratio, heat and reflux in an oil bath for a certain period of time, filter, and evaporate the filtrate under reduced pressure with a rotary evaporator to obtain a white solid, and then use ethyl acetate to process the product After recrystallization, 4,4'-dimethyl-2,2'-bipyridyl crystals can be obtained.

[0010] In a 100mL stainless steel autoclave with electromagnetic stirring, add methanol 4mL, add the catalyst, the catalyst composition is: palladium acetate 0.0125mmol, holmium phosphate 0.0125mmol, 4,4'-dimethyl 2,2'-bipyridine 0.05mmol , p-toluenesulfonic acid 0.025mmol, p-benzoquinone 2.5mmol, styrene 8mL, then keep the pressure of carbon monoxide at 2.0MPa, react at 80°C for 2 hours, terminate the reaction by releasing the pressure, precipitate with industrial ethanol, filter, The product was washed and vacuum-dried at 60° C. to obtain 5.25 g of a copolymer product with a catalytic activity o...

Embodiment 2

[0011] Embodiment two (for comparison)

[0012] Under the same conditions as in Example 1, a copolymer of carbon monoxide and styrene was prepared. The difference is that the palladium acetate in the catalyst is changed from 0.0125mmol to 0.025mmol, the bidentate ligand is changed from 4,4'-dimethyl 2,2'-bipyridine to 2,2'-bipyridine, and no rare earth is added. Salt phosphate holmium, obtains 3.89 grams of copolymerization product, catalytic activity 751gSTCO / gPd·h.

Embodiment 3

[0014] Under the same conditions as in Example 1, a copolymer of carbon monoxide and styrene was prepared. The difference is that the palladium acetate in the catalyst was changed from 0.0125mmol to 0.025mmol, and the rare earth salt holmium phosphate was not added to obtain 6.83g of copolymerized product, and the catalytic activity at this time was 1284gSTCO / gPd·h.

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PUM

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Abstract

The invention discloses a catalyst for preparing polyketone via copolymerization of carbon monoxide and styrene, belonging to the preparation technique of polyketone; wherein, the catalyst comprises palladium acetate, benzoquinone and p-toluene sulfonic acid, sulfamic acid, fluoboric acid or the mixture with Pka less than three; and 4, 4'-dimethyl-2, 2'-bipyridine and rare earth salt of praseodymium phosphate, neodymium phosphate, europium phosphate, dysprosium phosphate, holmium phosphate or the mixture with different proportions are adopted as the ligand of the catalyst. The catalyst for preparing polyketone via copolymerization of carbon monoxide and styrene has the advantages that catalytic activity of the catalyst is improved by one to three times when the 4, 4'-dimethyl-2, 2'-bipyridine and a certain amount of rare earth phosphate salts are added under the condition of the same amount of palladium acetate as the main catalyst; and catalyst cost is effectively reduced.

Description

technical field [0001] The invention relates to a catalyst for preparing polyketone by copolymerization of carbon monoxide and styrene, which belongs to the preparation technology of polyketone. Background technique [0002] The aliphatic polyketone synthesized by the copolymerization of carbon monoxide and olefin is a new type of polymer material, which has many excellent properties and is widely used in a wide range of fields. Polyketone has good gas barrier properties and excellent heat resistance. It can be stretched and processed, and can also be made into biodegradable and photodegradable resins. This makes polyketone the first choice for environmentally friendly packaging in the 21st century; polyketone is also a An excellent functional material intermediate. Due to the presence of carbonyl groups in the main chain of polyketone, it can be chemically modified: more than 20 kinds of functional polymers such as polyalcohol, polythiol, polyurethane, polyamide and polyes...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G67/02
Inventor 郭锦棠赵海洋张雪梅陈志坤叶雅琴
Owner TIANJIN UNIV
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