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在超碱性介质中通过还原其二氧化物制备硫族化物。

Chalcogenides by Reduction of their Dioxides in Ultra-Alkaline Media.

作者信息

Albrecht Ralf, Ruck Michael

机构信息

Faculty of Chemistry and Food Chemistry, Technische Universität Dresden, 01069, Dresden, Germany.

Max-Planck Institute for Chemical Physics of Solids, Nöthnitzer Straße 40, 01187, Dresden, Germany.

出版信息

Angew Chem Int Ed Engl. 2021 Oct 4;60(41):22570-22577. doi: 10.1002/anie.202107642. Epub 2021 Sep 6.

DOI:10.1002/anie.202107642
PMID:34375499
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC8518872/
Abstract

The reaction of chalcogen dioxides ChO (Ch=Se, Te) with As O in a 30 molar KOH hydroflux at about 200 °C yielded crystals of potassium trichalcogenides K Ch with dimensions up to 2 cm. Arsenic trioxide acts as electron donor and is oxidized to arsenate(V). The new heterochalcogenide anion (TeSe ) formed when starting from SeO and TeO simultaneously. The compound K TeSe crystallizes isostructural to K S and K Se . The unexpected redox reaction as well as the precipitation of hygroscopic compounds from an aqueous solution are attributed to a strongly reduced activity of water. The reactions were studied by Raman and UV/Vis spectroscopy. Depending on the concentration of As O , colorless monochalcogenide Ch or orange Se and purple Te anions are dominating the solutions.

摘要

在约200°C的30摩尔氢氧化钾水热流中，二氧化硒（ChO，Ch = Se、Te）与三氧化二砷反应生成尺寸达2厘米的三硫属化物钾（K₂Ch）晶体。三氧化二砷作为电子供体被氧化为砷酸盐（V）。当同时以二氧化硒和二氧化碲为起始原料时，会形成新的杂硫属化物阴离子（TeSe₂²⁻）。化合物K₂TeSe₂与K₂S和K₂Se₂同构结晶。这种意外的氧化还原反应以及从水溶液中沉淀出吸湿性化合物归因于水的活性大幅降低。通过拉曼光谱和紫外/可见光谱对这些反应进行了研究。根据三氧化二砷的浓度，无色的单硫属化物阴离子（Ch⁻）、橙色的硒阴离子（Se₂²⁻）和紫色的碲阴离子（Te₂²⁻）在溶液中占主导地位。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9f29/8518872/ae4e0053a1d2/ANIE-60-22570-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9f29/8518872/1ddaeaa4466a/ANIE-60-22570-g005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9f29/8518872/3b1060456fb3/ANIE-60-22570-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9f29/8518872/3593cf0ffedc/ANIE-60-22570-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9f29/8518872/550dc142b48b/ANIE-60-22570-g007.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9f29/8518872/b0caaad7476d/ANIE-60-22570-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9f29/8518872/ae4e0053a1d2/ANIE-60-22570-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9f29/8518872/1ddaeaa4466a/ANIE-60-22570-g005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9f29/8518872/3b1060456fb3/ANIE-60-22570-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9f29/8518872/3593cf0ffedc/ANIE-60-22570-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9f29/8518872/550dc142b48b/ANIE-60-22570-g007.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9f29/8518872/b0caaad7476d/ANIE-60-22570-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/9f29/8518872/ae4e0053a1d2/ANIE-60-22570-g001.jpg

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