By-product butene mixture, B-B raffinate from the butadiene production in naphtha cracking plant was directly polymerized under various reaction conditions in search for the possible application of otherwise wasted product.
The composition of the butene mixture was analysed by gas chromatography. The analysis indicated that unsaturated components were added up to 90%.
The polymerization was carried out in glass-made pressure bottles at the temperature range from -78℃ to 0℃. At the lower temperatures the polymers of higher molecular weight were obtained.
Sulfuric acid, aluminum chloride and borontrifluoride etherate were used as catalysts. Aluminum chloride was dissolved in 2-nitropropane before use. While sulfuric acid system yielded only oligomers of very low molecular weight, aluminum chloride system gave the higher molecular weight product.
As the amount of catalyst increases, the yield of polymer increased but low molecular weight product was obtained.
Difficulty was encountered in removing the catalyst after the reaction. Alkali washing often gave rather stable emulsion which did not separate readily on standing. Addition of inorganic salts helped somewhat. However certain effective system had to be found.
After washing, the resinous product was subjected to vacuum to strip the volatile contaminant. The final products were clear syrupy resins.
산 처리한 고령토에 비닐기를 가진 모노마를 넣으면 중합반응이 일어나서 고령표면이 유기물질로 덮혀있음을 I R로 확인하였다.
중합반응은 액상과 기상으로 모두 시켜 보았다. 스티렌이 50%의 이소부텐을 함유하고 있는 부텐혼합물보다 중합반응이 더 잘 일어났다. 모노마의 농도를 증가시켰더니 중합체의 수득율이 증가했다.
수분의 함유량이 고령토의 산성도에 결정적인 역할을 해서 약간의 수분을 함유해도 중합반응은 일어나지 않았다.
생성된 중합체는 고령토 표면에 화학결합을 이루고 있는 것이 아니고 용매에 녹이면 중합체만을 분리할 수 있었다.
고령토 표면에 접착되어 있는 중합체의 분석은 하기 어려웠다.
