无机盐工业 ›› 2023, Vol. 55 ›› Issue (4): 125-132.doi: 10.19964/j.issn.1006-4990.2022-0382
收稿日期:
2022-06-22
出版日期:
2023-04-10
发布日期:
2023-04-13
作者简介:
郭军(1981— ),男,副教授,博士,主要从事催化与工艺研究;E-mail:justin_gjxt@163.com。
基金资助:
GUO Jun1,2(), ZHANG Taiwen2, ZHANG Dan1
Received:
2022-06-22
Published:
2023-04-10
Online:
2023-04-13
摘要:
采用水热法合成了一例新的多酸基有机-无机杂化物非均相催化剂,并通过X-射线单晶衍射、傅里叶变换红外光谱(IR)、热重分析测试(TG)、X-射线衍射分析(XRD)、元素分析对其进行了表征。X-射线单晶衍射分析表明,化合物的结构式为(PMo12O40)(C5H6N)3[简写为(PMo12)(HPy)3,其中PMo12表示PMo12O40,HPy表示C5H6N],属于正交晶系,Cmca空间群,晶胞参数a=1.910 31(8) nm、b=1.538 22(6) nm、c=1.460 63(6) nm、α=β=γ=90°、V=4.292 0(3) nm3、Z=4、R1=0.062 9、wR2=0.132 4。化合物由2-吡啶甲酸在高温高压下原位脱羧后形成的质子化的3个吡啶环、1个经典的Keggin型[PMo12O40]3-构成,每个次级单元之间通过静电等相互作用进一步形成一维(1D)~二维(2D)结构。催化研究表明:(PMo12O40)(C5H6N)3在催化过氧化氢氧化碘离子为碘单质过程中,其化学反应动力学近似准一级反应,反应速率高达1.205×10-5 mol/(L·s),相对于室温下未添加催化剂时提高了1 839.7倍,该非均相催化剂重复使用5次后转化率仍高达99.96%,表现出较好的催化活性与可重复性。
中图分类号:
郭军, 张太文, 张丹. (PMo12)(HPy)3的合成、表征及催化氧化碘离子性能[J]. 无机盐工业, 2023, 55(4): 125-132.
GUO Jun, ZHANG Taiwen, ZHANG Dan. Synthesis,characterization of (PMo12)(HPy)3 and its catalytic oxidation property of iodide ion[J]. Inorganic Chemicals Industry, 2023, 55(4): 125-132.
表2
化合物(PMo12)(HPy)3的部分氢键数据
D-H···A | d(D-H)/ nm | d(H-A)/ nm | d(D···A)/ nm | ∠(D-H ···A)/(°) |
---|---|---|---|---|
C(1)-H(1A)···O(8) | 0.094 8 | 0.307 9 | 0.342 3 | 103.2 |
C(2)-H(2)···O(5) | 0.095 1 | 0.337 2 | 0.353 1 | 91.770 |
C(5)-H(5)···O(4) | 0.094 9 | 0.346 0 | 0.316 5 | 64.257 |
C(7)-H(7)···O(2) | 0.094 9 | 0.225 2 | 0.318 2 | 166.356 |
C(7)-H(7)···O(4) | 0.094 9 | 0.276 3 | 0.342 2 | 127.24 |
N(1)-H(1)···O(4) | 0.088 0 | 0.359 6 | 0.324 6 | 59.955 |
N(2)-H(2)···O(4) | 0.087 1 | 0.289 9 | 0.346 6 | 124.38 |
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