曲阜师范大学学报(自然科学版)
麯阜師範大學學報(自然科學版)
곡부사범대학학보(자연과학판)
JOURNAL OF QUFU NORMAL UNIVERSITY (NATURAL SCIENCE EDITION)
2009年
3期
61-63
,共3页
闫涛%张在庆%孙学军%尤进茂
閆濤%張在慶%孫學軍%尤進茂
염도%장재경%손학군%우진무
草酸%苯甲醇%对甲基苯磺酸%草酸二苄酯
草痠%苯甲醇%對甲基苯磺痠%草痠二芐酯
초산%분갑순%대갑기분광산%초산이변지
oxalic acid:benzyl alcohol: p-toluene sulphonic acid: dibenzyl oxalate
以草酸和苯甲醇为原料,采用三种不同的催化剂对甲苯磺酸、硫酸氢钾、强酸性阳离子交换树脂,三种不同的带水剂甲苯、苯、环己烷,合成了草酸二苄酯.并通过熔点、红外图谱,质谱对产物的结构进行表征.研究了反应物的配比、催化剂的种类和用量、带水剂的种类和用量对产物收率的影响.试验结果表明,当n(草酸)∶ n(苯甲醇)=1∶ 2.2(摩尔比);催化剂为对甲苯磺酸,用量为草酸质量的0.5%(0.13 g);苯为带水剂,用量40 mL,反应时间40 min;反应产率高达96.2%.
以草痠和苯甲醇為原料,採用三種不同的催化劑對甲苯磺痠、硫痠氫鉀、彊痠性暘離子交換樹脂,三種不同的帶水劑甲苯、苯、環己烷,閤成瞭草痠二芐酯.併通過鎔點、紅外圖譜,質譜對產物的結構進行錶徵.研究瞭反應物的配比、催化劑的種類和用量、帶水劑的種類和用量對產物收率的影響.試驗結果錶明,噹n(草痠)∶ n(苯甲醇)=1∶ 2.2(摩爾比);催化劑為對甲苯磺痠,用量為草痠質量的0.5%(0.13 g);苯為帶水劑,用量40 mL,反應時間40 min;反應產率高達96.2%.
이초산화분갑순위원료,채용삼충불동적최화제대갑분광산、류산경갑、강산성양리자교환수지,삼충불동적대수제갑분、분、배기완,합성료초산이변지.병통과용점、홍외도보,질보대산물적결구진행표정.연구료반응물적배비、최화제적충류화용량、대수제적충류화용량대산물수솔적영향.시험결과표명,당n(초산)∶ n(분갑순)=1∶ 2.2(마이비);최화제위대갑분광산,용량위초산질량적0.5%(0.13 g);분위대수제,용량40 mL,반응시간40 min;반응산솔고체96.2%.
Taking oxalic acid and benzyl alcohol as raw materials, dibenzyl oxalate was synthesized by using p-toluene sulphonic acid,potassium bisultfute,strong acid ionic exchange resin as catalysts and Toluene,benzene,cyclohexane as water-carrying agents. Structure of the product was identified by means of melting point measurement,IR and LC-MS. By a single factor test, effects of the reactant ratio, variety and quantity of the catalysts and water-carrying agents on the reaction were studied.Results showed the optimal reaction conditions: were n(oxalic acid)∶ n(benzyl alcohol)=1∶ 2.2(mole ratio), p-toluene sulphonic acid 0.15 g, benzene 40 mL, reaction time 40 min, the yield of dibenzyl oxalate reached up to 96.2%.