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在镍系催化丁二烯聚合中,助催化剂BF_3·OEt_2在加氢汽油中溶解性差,往往形成非均相体系,因而降低了催化剂体系的稳定性和氟的利用率。我们曾研究了A1(i-Bu)_3分别与丙醇、丁醇、戊醇,己醇、辛醇、壬醇、癸醇和十六醇按等摩尔交换,制得A1(i-Bu)_2OR作助催化剂,观察Al/B与催化活性的关系,发现以十六醇为最好,Al/B在0.25—0.95聚合活性较高,超出此限活性迅速下降。为了进一步提高Al/B,采用了向镍催化体系添加醇的方法。聚合实验证实了该法可提高氟的利用率。测定醇-硼体系的~1HNMR,证实了醇-硼分子间形成了氟-氢氢键。
In the nickel-catalyzed butadiene polymerization, the co-catalyst BF_3 · OEt_2 has poor solubility in hydrogenated gasoline and often forms a heterogeneous system, thus reducing the stability of the catalyst system and the utilization rate of fluorine. We have studied that A1 (i-Bu) _3 is exchanged equimolar with propanol, butanol, pentanol, hexanol, octanol, nonanol, As a co-catalyst, the relationship between Al / B and catalytic activity was observed. It was found that cetyl alcohol was the best, and the polymerization activity of Al / B was higher at 0.25-0.95. The activity beyond this limit decreased rapidly. In order to further improve Al / B, a method of adding alcohol to a nickel catalyst system has been adopted. Polymerization experiments confirmed that the method can improve the utilization of fluorine. The ~ 1H NMR of the alcohol-boron system confirmed the formation of fluorine-hydrogen hydrogen bonds between the alcohol-boron molecules.