摘要
用PEG400-CuCl_2-NiCl_2复合催化剂,由氯代特戊烷和甲醛合成频那酮,研究了PEG400-CuCl_2-NiCl_2复合催化剂对氯代特戊烷转化率的影响,以及PEG400-CuCl_2-NiCl_2催化剂的用量、CuCl_2/NiCl_2不同摩尔比、反应温度、甲醛滴加时间和盐酸浓度对频那酮收率的影响。用GC、GC-MS等分析仪器测试了体系中物质的含量及结构,提出了当PEG400-CuCl_2-NiCl_2催化剂存在的条件下合成频那酮的最佳工艺条件是:反应时间7 h、反应温度90℃、n(CuCl_2/NiCl_2)∶n(氯代特戊烷)为3∶100、n(CuCl_2/NiCl_2)∶n(PEG400)为1∶1、n(CuCl_2)∶n(NiCl_2)为1∶1、盐酸的质量浓度为28%。频那酮的收率为77%。
Using PEG400-CuCl2-NiCl2 as composite catalyst, pinacolone is synthesized by 2-chloro-2-methylbutane with formaldehyde .Effecting of PEG400-CuCl2-NiCl2 catalyst on the percent conversion of 2-chloro-2-methylbutane and the various factors such as usage of PEG 400-CuCl2-NiCl2 composite cata-lyst,different moral ratio of CuCl2 and NiCl2,reaction temperature,titration time of formaldehyde and con-centration of hydrochloric acid solution have been studied ,testing the substance content and structure in the reaction system by GC ,GC-MS.The optimal process conditions are：reaction time is 7 h,reaction tem-perature is 90℃,the moral ratio of CuCl 2/NiCl2 and 2-chloro-2-methylbutane is 3∶100,the moral ratio of CuCl2/NiCl2 and PEG400 is 1∶1,the moral ratio of CuCl2 and NiCl2 is 1∶1,the concentration of hydro-chloric acid solution is 28%.The yield of pinacolone is 77%.
出处
《应用化工》
CAS
CSCD
北大核心
2016年第11期2076-2079,共4页
Applied Chemical Industry
基金
江苏高校品牌专业建设工程资助项目(PPZY2015A044)
