通过复分解法制备出Dawson结构磷钨酸镧(La H3P2W18O62·n H2O),采用FT IR、SEM对其进行了表征,并将其用于催化30%H2O2氧化环己酮合成己二酸。考察了其用量、30%H2O2用量、反应时间、反应温度及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。优化合成工艺条件为:n(环己酮)/n(30%H2O2)=100/500,w(磷钨酸镧)=6.4%(基于环己酮的质量),反应温度100℃,反应时间5.5h。优化反应条件下,己二酸的收率最高可达86.5%。磷钨酸镧重复套用5次,己二酸收率仍可保持为74.1%。
Dawson type lanthanum phosphotungstate( La H3P2W18O62·n H2 O,La HPW) was prepared and characterized by FT IR and SEM,and employed as the catalyst for the synthesis of adipic acid( AA) from cyclohexanone with 30% hydrogen peroxide as oxidant. The effects of dosages of La HPW and hydrogen peroxide,reaction temperature and time,and reusability of La HPW on the yield of AA were investigated. The results showed that self-prepared La HPW kept primary Dawson structure and appeared in the shape of spherulite. The optimal reaction conditions for the synthesis of AA were w( La HPW) = 6. 4%( relative to the dosage of cyclohexanon),n( C6H10O) / n( H2O2) = 100 /500,reaction temperature 100℃,reaction time 5. 5h. Under these conditions,the isolated yield of AA could reach 86. 5%,and it was still over 74. 1% when La HPW was reused for five times.