相转移催化剂用于异戊基黄原酸盐合成工艺的研究
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摘要
以异戊醇、二硫化碳、氢氧化钠为原料,加入相转移催化剂EP,采用溶剂法合成了异戊基黄原酸盐。考察了有无催化剂存在、催化剂加量、溶剂用量、反应时间对反应的影响,确定了最佳合成条件为:催化剂EP用量为异戊醇质量的2.5%,反应时间5.5 h,异戊醇与二硫化碳摩尔比为1∶5,温度为30℃。在该反应条件下,反应的转化率可达到96%,合成的异戊基黄原酸盐纯度可达到82%。试验结果表明:相转移催化剂的加入有效的加快了反应速率,极大地缩短了异戊基黄原酸盐的合成时间,同时催化剂的加入对异戊基黄原酸盐的选矿效果无明显影响。
Isoamyl xanthate is synthesized by solvent method with isoamyl alcohol, carbon disulfide and sodium hydroxide as raw materials and EP as phase transfer catalyst. The effects of catalyst existence, catalyst dosage, solvent dosage and reaction time on the reaction are investigated. The optimum synthesis conditions are determined as follows: the catalyst EP dosage is 2.5% of the mass of isopentanol, the reaction time is 5.5 h, the molar ratio of isopentanol to carbon disulfide is 1∶5,and the reaction temperature is 30 ℃.Under this reaction condition,the conversion can reach 96%, the purity of the synthesized isoamyl xanthate can reach 82%. The results show that the addition of phase transfer catalyst effectively accelerates the reaction rate and greatly shortens the synthesis time of isoamyl xanthate, while the addition of catalyst has no obvious effect on the beneficiation efficiency of isoamyl xanthate.
Isoamyl xanthate is synthesized by solvent method with isoamyl alcohol, carbon disulfide and sodium hydroxide as raw materials and EP as phase transfer catalyst. The effects of catalyst existence, catalyst dosage, solvent dosage and reaction time on the reaction are investigated. The optimum synthesis conditions are determined as follows: the catalyst EP dosage is 2.5% of the mass of isopentanol, the reaction time is 5.5 h, the molar ratio of isopentanol to carbon disulfide is 1∶5,and the reaction temperature is 30 ℃.Under this reaction condition,the conversion can reach 96%, the purity of the synthesized isoamyl xanthate can reach 82%. The results show that the addition of phase transfer catalyst effectively accelerates the reaction rate and greatly shortens the synthesis time of isoamyl xanthate, while the addition of catalyst has no obvious effect on the beneficiation efficiency of isoamyl xanthate.
引文
[1] 马鑫.烷基黄原酸盐捕收剂的绿色合成工艺研究[D]:长沙:中南大学,2013.
[2] 吴鲲魁,张志强,赵桂利.相转移助催化剂在有机合成中的应用[J].鞍山科技大学学报,2005,28(2):99-101.
[3] 李杰.提高黄药质量方法的探讨[J].铜业工程,2002,2:58-60.
[4] 周继亮.烷基黄原酸酯系列药剂的合成与应用[D]:长沙:中南大学,2003.
[5] 张铸勇.精细有机合成单元反应[M].上海:华东理工大学出版社,2003.
[2] 吴鲲魁,张志强,赵桂利.相转移助催化剂在有机合成中的应用[J].鞍山科技大学学报,2005,28(2):99-101.
[3] 李杰.提高黄药质量方法的探讨[J].铜业工程,2002,2:58-60.
[4] 周继亮.烷基黄原酸酯系列药剂的合成与应用[D]:长沙:中南大学,2003.
[5] 张铸勇.精细有机合成单元反应[M].上海:华东理工大学出版社,2003.