反应详情

A copolymer prepolymer of diphenylbutadiyne and p-diethynylbenzene was prepared in refluxing benzene solvent. The polymerization vessel was charged with 63 parts of diphenylbutadiyne, 2 parts of diethynylbenzene, 600 parts of benzene, and 2 parts of chlorobenzene. After heating to reflux, 2 parts of a catalyst mixture prepared by mixing 2 parts of nickelacetylacetonate and 4 parts of triphenylphosphine in 20 parts of benzene were added. After 1 hour, an additional 10 parts of diethynylbenzene was added. After 2 hours, 10 parts of diethynylbenzene and 2 parts of catalystsolution were added. After 3 hours, 20 parts of diethynylbenzene and 4 parts of catalyst solution were added. After a total reaction period of 7 hours, gas-liquid chromatographic analysis of the reaction mixture showed that 10% of each of the monomeric components remained. The solution was added to 5 times its volume of methanol, and 77 parts of the copolymer wasprecipitated. It had an acetylene content of 8.4% and an aromatic to olefin hydrogen ratio of 8:1.

1. temperatureAfter heating
2. temperatureto reflux
3. custom2 parts of a catalyst mixture prepared
4. additionwere added
5. waitAfter 2 hours
6. waitAfter 3 hours
7. customAfter a total reaction period of 7 hours, gas-liquid chromatographic analysis of the reaction mixture