Mechanochemical synthesis of (poly)oxalatomolybdates: In situ reaction monitoring by PXRD

被引：3

作者：

Cindric, Marina ^{[1
]}

Hrenar, Tomica ^{[1
]}

Damjanovic, Vladimir ^{[2
]}

Stilinovic, Vladimir ^{[1
]}

Kuzman, Dino ^{[1
]}

Pisk, Jana ^{[1
]}

Primozic, Ines ^{[1
]}

Vrdoljak, Visnja ^{[1
]}

机构：

[1] Univ Zagreb, Fac Sci, Dept Chem, Horvatovac 102a, Zagreb, Croatia

[2] Univ Zagreb, Sch Med, Dept Chem & Biochem, Salata 3, Zagreb, Croatia

来源：

INORGANICA CHIMICA ACTA | 2019年 / 488卷

关键词：

(Poly)oxalatomolybdates; Mechanochemical synthesis; Vapour- assisted aging; Powder X-ray diffraction method; Characterization; Reaction profiles; REAL-TIME; CHEMOMETRIC ANALYSIS; CRYSTAL-STRUCTURES; MILLING REACTIONS; COMPLEXES; MOFS;

D O I：

10.1016/j.ica.2019.01.006

中图分类号：

O61 [无机化学];

学科分类号：

070301 ; 081704 ;

摘要：

Mechanochemically accelerated vapour-assisted aging and transformation from the amorphous precipitate by aging to the crystalline products were demonstrated to be the efficient methods to synthesize crystalline hydrate and non-hydrate (poly)oxalatomolybdates, [Co(NO2)(NH3)(5)][MoO3(ox)H2O]center dot H2O, [Co(NH3)(6)](2) [Mo4O11(ox)(4)(H2O)]center dot 6H(2)O, [Co(NH3)(6)](4)[Mo4O8(mu-O)(4)(ox)(4)] [MoO3(ox)(H2O)](2)center dot 10H(2)O, [Co(en)(3)](4)[MoO2(mu-O)(ox)](2) [MoO3(ox)(H2O)](2).7H(2)O and [Co(ox)(en)(2)](2)[Mo2O5(ox)(2)(H2O)(2)]center dot 4H(2)O, respectively. We have also studied the transformation kinetics of the amorphous intermediates into the final crystalline oxalatomolybdates in an aqueous slurry at room temperature by in situ powder X-ray diffraction (PXRD) method coupled with numerical methods. Using the principal component analysis, PXRD data tensors were reduced to only one principal component. Reaction profiles were built and total times for completion were determined.

引用

页码：80 / 85

页数：6

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