超高交联树脂的氯代烷烃后交联法制备及对咖啡因的吸附研究  

PREPARATION OF HYPERCROSSLINKED POLYSTYRENE via POST-CROSSLINKING BY CHLOROALKANES AND ADSORPTION OF CAFFEINE

作　　者：李发达 徐媛媛 于均超 徐满才[1] LI Fada;XU Yuanyuan;YU Junchao;XU Mancai(College of Chemistry and Chemical Engineering,Hunan Normal University Changsha 410081,China;College of Medicine and Chemical Engineering,Lianyungang Technical College Lianyungang 222006,China)

机构地区：[1]湖南师范大学化学化工学院,长沙410081 [2]连云港职业技术学院医药与化学工程学院,江苏连云港222006

出　　处：《离子交换与吸附》2022年第1期48-59,共12页Ion Exchange and Adsorption

基　　金：连云港职业技术学院新医药开发与生物技术应用创新团队资助项目

摘　　要：以三氯甲烷为外交联剂,以AlCl_(3)为催化剂,经Friedel-Crafts后交联反应将大孔低交联聚苯乙烯(PS)后交联,制备得到超高交联聚苯乙烯树脂HCPS-C_(1),树脂的BET比表面积从PS的19.5m^(2)/g提高到HCPS-C_(1)的522m^(2)/g;再以1,2-二氯乙烷为外交联剂,以FeCl_(3)为催化剂,将HCPS-C_(1)后交联,制备得到了比表面积高达791m^(2)/g的超高交联聚苯乙烯树脂HCPS-C_(1)-C_(2)。测定了HCPS-C_(1)和HCPS-C_(1)-C_(2)对咖啡因的吸附性能,并与商用树脂XAD4及氯甲基化聚苯乙烯后交联树脂HCPS-CM进行对比,结果表明,HCPS-C_(1)有着接近于XAD4对咖啡因的吸附量,而HCPS-C_(1)-C_(2)对咖啡因的吸附量远高于XAD4,且略高于HCPS-CM。平衡浓度为100mg/L时,HCPS-C_(1)-C_(2)对咖啡因的吸附量可达148.2mg/g,优于文献报道的大多数吸附材料。本文以简单易得的氯代烷代替剧毒致癌的氯甲醚进行后交联反应制备吸附性能优良的超高交联吸附树脂,极具工业应用前景。The hypercrosslinked polystyrene resin HCPS-C_(1)was prepared from macroporous slightly cross-linked polystyrene(PS)via the Friedel-Crafts post-crosslinking reaction by using trichloromethane as the external cross-linker and AlCl_(3) as the catalyst,and the BrunauerEmmett-Teller(BET)surface area(S_(BET))of HCPS-C_(1)rose to 522m^(2)/g from 19.5m^(2)/g of PS.Then the hyper-cross-linked polystyrene resin HCPS-C_(1)-C_(2)with S_(BET)of 791m^(2)/g was prepared via post-crosslinking of HCPS-C_(1)by using 1,2-dichloroethane as the external cross-linker and FeCl_(3)as the catalyst.Adsorption performance of HCPS-C_(1)and HCPS-C_(1)-C_(2)for caffeine in aqueous solution was tested,and was compared with that of commercial adsorbent resin of XAD4 and HCPS-MC,the hypercrosslinked polystyrene prepared by post-crosslinking of chloromethylated polystyrene(CMPS).The results showed that HCPS-C_(1)had the adsorption capacity of caffeine near XAD4,while HCPS-C_(1)-C_(2)displayed much higher adsorption capacity of caffeine than XAD4,and slightly higher than HCPS-MC.The adsorption capacity of caffeine on HCPS-C_(1)-C_(2)amounted to 148.2 mg/g at the equilibrium concentration of 100 mg/L,which was higher than that on some other adsorbents reported in the literature.A hypercrosslinked polystyrene adsorbent resin with excellent adsorption performance was prepared by using inexpensive commercial chloroalkanes instead of the highly toxic and carcinogenic agent chloromethyl methyl ether as external crosslinkers in this paper,which is of value in industrial production of hypercrosslinked adsorbents.

关 键 词：超高交联聚苯乙烯 Friedel-Crafts后交联 三氯甲烷 二氯乙烷 吸附 咖啡因 

分 类 号：TQ324.8[化学工程—合成树脂塑料工业] O647.3[理学—物理化学]