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Preparation method of high-purity tellurium diethyl

A diethyl tellurium, high-purity technology, applied in organic chemistry, etc., can solve the problems of drying and water removal, reducing the performance of CdHgTe thin film materials, and having no infrared detection performance, etc., achieving high yield, simple operation and safe method Efficient effect

Inactive Publication Date: 2017-07-21
FIRST RARE MATERIALS CO LTD
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Problems solved by technology

Chinese patent CN105820099A discloses a process of obtaining high-purity diethyl tellurium from industrial-grade tellurium powder, sodium formaldehyde sulfoxylate, and alkyl halide through raw material synthesis, rectification, analysis and detection, but the method uses an aqueous solution, and the product is dried and removed. Water is difficult, and other impurities are easy to introduce at the same time, and water has a great influence on metal organic chemical vapor deposition, and residual moisture will also greatly reduce the performance of CdHgTe thin film materials, which may have no infrared detection performance

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  • Preparation method of high-purity tellurium diethyl

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preparation example Construction

[0021] The present invention proposes a kind of preparation method of high-purity diethyl tellurium, comprising the following steps:

[0022] S1: In a protective gas atmosphere, cool the tellurium tetrachloride solution to -20°C~-70°C, add ethyl magnesium halide dropwise to it, after the dropwise addition, raise the temperature to -60~0°C, and stir the reaction 1~5h, then raise the temperature to 10~30°C, continue to stir for 1~5h, and prepare the diethyl tellurium mixture;

[0023] S2: Under a protective gas atmosphere, the diethyl tellurium mixture is sequentially subjected to primary distillation, secondary distillation, and vacuum rectification to obtain diethyl tellurium with a purity of more than 5N;

[0024] The tellurium tetrachloride solution is an organic solution formed by dissolving tellurium tetrachloride in an organic solvent.

[0025] In the present invention, preferably, the organic solvent is any one or more of diethyl ether, tetrahydrofuran, toluene, and ben...

Embodiment 1

[0031] Reagent preparation: freshly prepared tellurium tetrachloride, stored under nitrogen environment; dry ethyl bromide: take 40g of calcium chloride and add it to 500ml of ethyl bromide, heat to reflux for 3h; dry tetrahydrofuran: use sodium to reflux tetrahydrofuran, as the indicator diphenylmethane When the ketone turns dark purple, distill off tetrahydrofuran and set aside.

[0032] Preparation of ethylmagnesium bromide: Add 22.08g (0.92mol) of magnesium chips and 250ml of tetrahydrofuran to a 1L three-necked flask, under nitrogen protection, heat the three-necked flask to 40°C, add dropwise 30ml of bromoethane containing 4.9g (0.045mol) The tetrahydrofuran solution is used as an initiator to speed up the reaction reflux, turn off the heating, adjust the drop rate slowly, continue to drop 270ml of tetrahydrofuran solution containing 93.2g (0.855mol) bromoethane, and finish adding within 1.5~2h, the dropwise addition is completed After that, turn on the heating, reflux f...

Embodiment 2

[0038] Reagent preparation: freshly prepare tellurium tetrachloride, store under nitrogen environment; dry ethyl iodide: take 40g of calcium chloride and add it to 500ml of ethyl iodide, heat to reflux for 3h.

[0039]Preparation of ethylmagnesium iodide: Add 22.08g (0.92mol) magnesium chips and 250ml ether to a 1L three-necked flask, under nitrogen protection, heat the three-necked flask to 40°C, add dropwise 30ml containing 7.01g (0.045mol) ethyl iodide To speed up the reaction reflux, turn off the heating, slow down the drop rate, continue to drop 270ml of ether solution containing 133.33g (0.855mol) ethyl iodide, and finish adding within 1.5~2h. After the dropwise addition, turn on Heating, reflux for 1h, set aside.

[0040] Preparation of diethyl tellurium: Under the protection of nitrogen, take 450 ml of ether and dissolve 62.65 g (0.23 mol) of tellurium tetrachloride to form a tellurium tetrachloride solution. The tellurium tetrachloride solution was cooled to -50°C, a...

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Abstract

The invention provides a preparation method of high-purity tellurium diethyl, comprising the steps of S1, cooling tellurium tetrachloride to -20 DEG C to -70 DEG C in a protective gas atmosphere, dropwise adding ethyl magnesium halide, then heating to -60 DEG C to 0 DEG C, stirring and reacting for 1-5 h, heating to 10-30 DEG C, and continuing to stir for 1-5 h to obtain tellurium diethyl mixture; S2, in the protective gas atmosphere, distilling the tellurium diethyl mixture firstly, distilling secondly, and rectifying under reduced pressure to obtain tellurium diethyl having a purity of 5N and above; the tellurium tetrachloride solution is an organic solution formed by dissolving tellurium tetrachloride an organic solvent. The preparation method is simple to perform, the yield of crude tellurium diethyl is high, the purified tellurium diethyl has the purity reaching 5N and above, and the preparation method is good in safety and high in efficiency.

Description

technical field [0001] The invention belongs to the technical field of preparation of organic tellurium compounds, and in particular relates to a preparation method of high-purity diethyl tellurium. Background technique [0002] The infrared detection material is the response element in the infrared detector, also known as the heart of the infrared detector. Among them, CdHgTe photoelectric detection material has a wide temperature range and good temperature stability, low intrinsic carrier concentration, high mobility, and short response time. It is a high-performance near-infrared photodetector material. The method of preparing CdHgTe thin film material has crystal Material growth, liquid phase epitaxy, metal organic chemical vapor deposition and molecular beam epitaxy, etc. Metal Organic Chemical Vapor Deposition (MOCVD for short) technology is an advanced method for manufacturing semiconductor ultra-thin film materials. High-purity metal-organic compounds (that is, MO ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C395/00
CPCC07C395/00
Inventor 薄福丽朱刘马永博
Owner FIRST RARE MATERIALS CO LTD
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