催化法制备三乙二醇二异辛酸酯及其性能  

Preparation and performance of triethylene glycol diisooctanoate by catalytic method

作　　者：丁炳伟 李红良 刘自力[2] Ding Bingwei;Li Hongliang;Liu Zili(Hebi Lianhao New Material Co.,Ltd.,Hebi 458000,Henan,China;School of Chemistry and Chemical Engineering,Guangzhou University,Guangzhou 510000,Guangdong,China)

机构地区：[1]鹤壁联昊新材料有限公司,河南鹤壁475000 [2]广州大学化学化工学院,广东广州510000

出　　处：《工业催化》2024年第7期37-42,共6页Industrial Catalysis

基　　金：河南省中央引导地方科技发展专项跨区域研发合作项目(Z20221343016);安阳市重大科技专项计划项目(2022A02GX008)。

摘　　要：采用沉淀-浸渍法制备SO_(4)^(2-)/ZrO_(2)-γ-Al_(2)O_(3)固体酸催化剂,以三乙二醇和2-乙基己酸的酯化反应为探针反应催化法制备三乙二醇二异辛酸酯(TGDE),确定SO_(4)^(2-)/ZrO_(2)-γ-Al_(2)O_(3)固体酸催化剂的最佳制备条件。考察焙烧温度、焙烧时间、硫酸浸渍浓度、硫酸浸渍时间、陈化温度对催化活性的影响,并进一步考察催化剂的循环使用性能。结果表明,焙烧温度为600℃、焙烧时间为5 h、硫酸浸渍浓度为0.6 mol·L^(-1),酸浸渍时间为9 h、陈化温度-20℃时,制备的SO_(4)^(2-)/ZrO_(2)-γ-Al_(2)O_(3)固体酸催化剂具有较好的催化活性,三乙二醇的酯化率达到99.06%,催化剂循环使用5次后,酯化率降至90.54%。目的产物TGDE进行气相色谱、FT-IR、^(1)HNMR和^(13)CNMR分析检测,各项性能指标都达到了国家标准。SO_(4)^(2-)/ZrO_(2)-γ-Al_(2)O_(3)solid acid catalyst was prepared by precipitation-impregnation method.Preparation of triethylene glycol diisooctanoate(TGDE)by catalytic method using esterification reaction of triethylene glycol and 2-ethylhexanoic acid as probe reaction.The optimal conditions of preparation were performed to confirm.The results show that the optimum preparation conditions for solid acid catalyst through precipitation-impregnation method are calcination temperature is 600℃,the calcination time is 5 h,the sulfuric acid impregnation concentration is 0.6 mol·L^(-1),the sulfuric acid impregnation time is 9 h,and the aging temperature is-20℃.The conversion of triethylene glycol reachs to 99.06%and still remains 90.54%after recycling 5 times at the optimum conditions.The target product TGDE was anal-yzed and detected by gas chromatography,FT-IR,^(1)HNMR,and^(13)CNMR,and all performance indicators met the requirements of national standards.

关 键 词：催化剂工程 固体酸 SO_(4)^(2-)/ZrO_(2)-γ-Al_(2)O_(3) 酯化 三乙二醇二异辛酸酯 

分 类 号：TQ426.6[化学工程] TQ414