化工学报
化工學報
화공학보
JOURNAL OF CHEMICAL INDUSY AND ENGINEERING (CHINA)
2015年
8期
3072-3077
,共6页
磺化竹炭%竹材%催化剂%乙酸丁酯%酯化反应%对甲苯磺酸
磺化竹炭%竹材%催化劑%乙痠丁酯%酯化反應%對甲苯磺痠
광화죽탄%죽재%최화제%을산정지%지화반응%대갑분광산
sulfonated carbon%bamboo%catalyst%butyl acetate%esterification%p-toluenesulfonic acid
以竹粉为原料、对甲苯磺酸为磺化剂,一锅法制备合成了新型磺化竹炭材料(SBC)。利用元素分析、酸碱反滴定、热重分析(TGA)、X射线光电子能谱(XPS)、X射线衍射(XRD)和傅里叶红外(FTIR)等对所制备的SBC进行了表征。以乙酸和正丁醇的酯化反应为探针反应,评价了SBC的催化作用,考察了催化剂用量、反应温度、酸醇摩尔比等的影响。结果表明,在反应温度为80℃、反应时间4 h、SBC用量为正丁醇质量的10%、酸醇摩尔比为3.5:1的适宜条件下,正丁醇转化率达到91.8%,选择性99.5%。SBC重复使用5次,正丁醇转化率仍可达80%以上。此外,SBC催化其他酯化反应体系的实验结果表明,SBC催化活性接近或优于商品离子交换树脂Amberlyst-15。
以竹粉為原料、對甲苯磺痠為磺化劑,一鍋法製備閤成瞭新型磺化竹炭材料(SBC)。利用元素分析、痠堿反滴定、熱重分析(TGA)、X射線光電子能譜(XPS)、X射線衍射(XRD)和傅裏葉紅外(FTIR)等對所製備的SBC進行瞭錶徵。以乙痠和正丁醇的酯化反應為探針反應,評價瞭SBC的催化作用,攷察瞭催化劑用量、反應溫度、痠醇摩爾比等的影響。結果錶明,在反應溫度為80℃、反應時間4 h、SBC用量為正丁醇質量的10%、痠醇摩爾比為3.5:1的適宜條件下,正丁醇轉化率達到91.8%,選擇性99.5%。SBC重複使用5次,正丁醇轉化率仍可達80%以上。此外,SBC催化其他酯化反應體繫的實驗結果錶明,SBC催化活性接近或優于商品離子交換樹脂Amberlyst-15。
이죽분위원료、대갑분광산위광화제,일과법제비합성료신형광화죽탄재료(SBC)。이용원소분석、산감반적정、열중분석(TGA)、X사선광전자능보(XPS)、X사선연사(XRD)화부리협홍외(FTIR)등대소제비적SBC진행료표정。이을산화정정순적지화반응위탐침반응,평개료SBC적최화작용,고찰료최화제용량、반응온도、산순마이비등적영향。결과표명,재반응온도위80℃、반응시간4 h、SBC용량위정정순질량적10%、산순마이비위3.5:1적괄의조건하,정정순전화솔체도91.8%,선택성99.5%。SBC중복사용5차,정정순전화솔잉가체80%이상。차외,SBC최화기타지화반응체계적실험결과표명,SBC최화활성접근혹우우상품리자교환수지Amberlyst-15。
A novel sulfonated carbon from bamboo (SBC) was prepared by one-pot method using p-toluenesulfonic acid as sulfonating agent. The structure and property of SBC were characterized using elemental analysis, acid-base inverse titration, thermo-gravimetric analysis (TGA), X-ray photon spectroscopy (XPS), XRD and FTIR. Esterification ofn-butanol with acetic acid was used as a standard reaction to evaluate the catalytic performance of SBC. The influences of catalyst amount, temperature and molar ratio of acid to alcohol were fully investigated.91.8% conversion ofn-butanol with 99.5% selectivity was achieved under the following conditions: reaction temperature 80℃, reaction time 4 h, catalyst amount 10% (mass) ofn-butanol, molar ratio of acetic acid ton-butanol 3.5:1. Above 80% conversion ofn-butanol could still be reached after SBC was used for 5 times. Additionally, SBC showed comparable or superior catalytic activity in other esterification reactions in comparison with the commercial ion exchange resin Amberslyst-15, which demonstrated that SBC has a good prospect in industrial applications.