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丙烯樹脂之研究-六、丙烯脂之製備

Allyl Resins. VI. Preparation of Allyl Esters

摘要


丙烯醇與有機酸或酸酐在普通情況下可生反應,製成丙烯酯。本實驗爲提高丙烯酯之產率,分別探求酜酐,己二酸,檸檬酸等與丙烯醇反應之適當操作條件,以期獲得最高產率。酜酸二丙烯酯之製備-(1)丙烯醇之用量,以比理論量多10%卽可,(2)觸媒,對甲苯磺酸之用量,以2.7% (對酜酐重量計,卽用1/2克分子有機酸或酸酐時,加2公克觸媒)爲宜,(3)不用銅粉比用銅粉時爲佳,(4)反應時間愈長,作用愈完全。反應24小時酜酸二丙烯酯之最高產率可達97.7%。檸檬酸及己二酸等之丙烯酯均可依下述標準條件製備,(1)10%過剩之丙烯醇,(2)用1/2克分子酸時,加6公撮粗甲苯磺酸爲觸媒,250公撮甲苯爲溶劑及脫水劑,(3)不用銅粉爲阻聚劑。如是反應8小時,己二酸丙烯酯最高產率爲97.3%;反應12小時,檸檬酸三丙烯酯最高產率爲85.5%。

關鍵字

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並列摘要


The optimum conditions for preparing allyl esters, such as diallyl phthalate, diallyl adipate and triallyl citrate, had been studied. Allyl alcohol was preferably used in 10% excess of the theoretical guantity. Using 250 ml. toluene as the solvent and azeotroping agent and 2 grams of refined p-toluene sulfonic acid as catalyst, the yield of diallyl phthalate was 97.6% of theorectical, while the time of reaction was 20 hours When 6 ml. of crude toluene sulfonic acid solution containing half gram of p-toluene sulfonic acid per ml. was used as catalyst, diallyl adipate was obtained in 95% yield in 8 bours, and triallyl citrate, 85% yield in 12 hours. It was also found that the use of copper as inhibitor is not necessary and that crude toluene (about 60% toluene) may be used in place of pure toluene without de- creasing the yield appreciably.

並列關鍵字

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