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
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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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