化学反应工程与工艺2024,Vol.40Issue(4) :289-297.DOI:10.11730/j.issn.1001-7631.2024.04.0289.09

氧化物负载磷钨酸催化甘露醇脱水反应的研究

Dehydration of Mannitol Catalyzed by Oxide Supported Phosphotungstic Acid

陈涵铭 莫学坤 郑燕春 徐冰冰 侯铭轩 葛峻逍 朱明乔
化学反应工程与工艺2024,Vol.40Issue(4) :289-297.DOI:10.11730/j.issn.1001-7631.2024.04.0289.09

氧化物负载磷钨酸催化甘露醇脱水反应的研究

Dehydration of Mannitol Catalyzed by Oxide Supported Phosphotungstic Acid

陈涵铭 1莫学坤 2郑燕春 3徐冰冰 2侯铭轩 4葛峻逍 4朱明乔1
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作者信息

  • 1. 浙江大学化学工程与生物工程学院,浙江 杭州 310058;浙江大学衢州研究院,浙江 衢州 324000
  • 2. 浙江江正和流体科技股份有限公司,浙江 杭州 310014
  • 3. 衢州巨化锦纶有限责任公司,浙江 衢州 324000
  • 4. 浙江大学化学工程与生物工程学院,浙江 杭州 310058
  • 折叠

摘要

分别以SiO2,TiO2,ZrO2和Al2O3为载体,采用浸渍法负载Keggin型磷钨酸,制备了一系列不同负载量的催化剂.通过红外光谱(FT-IR)、X射线衍射(XRD)、扫描电镜(SEM)和程序升温脱附(NH3-TPD)等表征手段分析催化剂.在无溶剂、减压条件下,使用制得的催化剂,研究了催化剂催化甘露醇脱水反应的性能,考察了催化剂载体种类、磷钨酸负载量、反应时间、反应温度和催化剂用量对甘露醇转化率和脱水产物的影响.结果表明,以 30%PW/SiO2为催化剂,催化反应性能较好,较佳的工艺条件是催化剂与甘露醇质量比为0.03,反应温度为170℃,反应时间为2 h,反应体系真空度为 0.09 MPa,在此条件下甘露醇的转化率为 100.0%,2,5-脱水山梨醇收率为 55.7%,1,4-脱水甘露醇收率为 9.7%,异甘露醇收率为 25.9%,副产物收率为8.5%.

Abstract

A series of supported catalysts with different loading amounts were prepared by impregnating Keggin-type phosphotungstic acid onto SiO2,TiO2,ZrO2,and Al2O3 carriers.Characterization methods such as infrared spectroscopy(FT-IR),X-ray diffraction(XRD),scanning electron microscopy(SEM),and temperature programmed desorption(NH3-TPD)were used to analyze the catalyst.The performance of the prepared catalysts in the dehydration of mannitol was studied under solvent-free and depressurized conditions.The effects of catalyst carrier type,phosphotungstic acid loading,reaction time,reaction temperature,and catalyst dosage on the conversion of mannitol and dehydration products were investigated.The results showed that the 30%PW/SiO2 catalyst exhibited superior catalytic performance.The optimal process conditions were a catalyst to mannitol mass ratio of 0.03,a reaction temperature of 170℃,a reaction time of 2 h,and a vacuum degree of 0.09 MPa.Under these conditions,the conversion of mannitol was 100.0%,the yield of 2,5-sorbitan was 55.7%,the yield of 1,4-mannitan was 9.7%,the yield of isomannide was 25.9%,and the yield of other components was 8.5%.

关键词

甘露醇脱水/催化剂/负载型磷钨酸/反应条件/金属氧化物

Key words

dehydration of mannitol/catalyst/supported phosphotungstic acid/reaction conditions/metal oxides

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基金项目

浙江大学衢州研究院科技计划项目(IZQ2022KJ3011)

衢州市科技计划项目(2022K05)

衢州市科技计划项目(2021F012)

浙江省生产制造方式转型示范项目(2207-330851-04-02-952183)

出版年

2024
化学反应工程与工艺
联合化学反应工程研究所 ,中石化上海石油化工研究院

化学反应工程与工艺

CSTPCD
影响因子:0.392
ISSN:1001-7631
参考文献量4
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