曹小华.化学通报,2015,78(12):1113-1117. |
Dawson结构磷钨酸镧催化绿色合成己二酸 |
Green Synthesis of Adipic Acid Catalyzed by Dawson type lanthanum phosphotungstate |
投稿时间:2015-04-02 修订日期:2015-04-28 |
DOI: |
中文关键词: 磷钨酸镧 Dawson结构 30%H2O2 己二酸 绿色合成 |
英文关键词:Lanthanum phosphotungstate Dawson type 30%H2O2 Adipic acid Green synthesis |
基金项目:国家自然科学基金项目(21161009)、江西省自然科学(20132BAB203004,20122BAB213001)、江西省教育厅科技项目(GJJ12616,GJJ13723)及九江学院科技项目(2013KJ005)资助 |
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中文摘要: |
通过复分解法制备出Dawson结构磷钨酸镧(LaH3P2W18O62.nH2O)催化剂,采用FT-IR、SEM对催化剂进行了表征,并将其用于催化30%H2O2氧化环己酮合成己二酸。考察了催化剂用量、30%H2O2用量、反应时间、反应温度及催化剂重复套用次数对己二酸收率的影响。结果表明:自制磷钨酸镧具有Dawson结构,呈椭球状。优化合成工艺为:n(环己酮)/n(30%H2O2)=100/500,w(催化剂)=6.4%(基于环己酮的质量),反应温度100℃,反应时间5.5 h。优化反应条件下,己二酸的收率最高可达86.5%。催化剂重复套用5次,己二酸收率仍可保持为74.1%。 |
英文摘要: |
Dawson type lanthanum phosphotungstate(LaH3P2W18O62.nH2O) was prepared and employed as the catalyst for the synthesis of adipic acid from cyclohexanone with 30% hydrogen peroxide as oxidant. The catalyst was characterized by FT-IR and SEM. TheSeffectsSofSsuchSfactorsSasScatalyst dosage, hydrogen peroxide dosage, reaction temperature, reaction time and reusability of the catalyst were investigated. Experimental results showed that self-prepared lanthanum phosphotungstate catalyst kept primary dawson structure andSappeared in the shape of spherulite. The optimal reaction conditions were as follows: w(LaH3P2W18O62.nH2O)=6.4%( relative to the dosage of cyclohexanon),n(C6H10O)/n(H2O2) = 100/500,reaction temperature 100℃,reaction time 5.5h. UnderStheseSconditions, the isolated yield of adipic acid could reach 86.5%, and it was still over 74.1% whenSthe catalyst wasSreusedSforSfiveStimes. |
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