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Preparation method of alkali metal intercalated transition metal disulfide

A technology of disulfides and transition metals is applied in the field of preparation of alkali metal intercalated transition metal disulfides, which can solve the problems of high price of experimental reagents, high equipment requirements, dangerous reactions, etc., and achieves easy operation, safe synthesis process, The effect of expanding the layer spacing

Inactive Publication Date: 2011-01-19
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] (2) SnS2 reacts with n-butyllithium under nitrogen and anhydrous conditions, the conditions are harsh, the price of experimental reagents is high, and there is a certain danger in the reaction
[0007] (3) The ultra-high vacuum method requires high equipment, and all operations need to be carried out in a nitrogen-filled glove box

Method used

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  • Preparation method of alkali metal intercalated transition metal disulfide
  • Preparation method of alkali metal intercalated transition metal disulfide

Examples

Experimental program
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Effect test

Embodiment 1

[0018] a, take chemically pure tin disulfide 2.0050g, join in the dehydrated alcohol of 150ml, stir 30 minutes under the condition of ice bath;

[0019] b. When the temperature of the above solution drops to 0°C, add 0.1660 g of analytically pure sodium borohydride, then keep stirring, and add 0.2203 g, 0.2067 g, 0.3012 g and 0.3029 g of sodium borohydride in four times every 8 hours, After stirring and reacting for 72 hours, centrifuge to obtain a brown solid product, then filter and wash the product with absolute ethanol, and dry naturally to obtain a compound intercalated with sodium tin disulfide.

Embodiment 2

[0021] a, take chemically pure tin disulfide 1.0150g, join in the anhydrous methanol of 100ml, stir 20 minutes under the condition of ice bath;

[0022] b. Add 0.2005g of analytically pure potassium borohydride when the temperature of the above solution drops to 0°C, and then keep stirring, and add 0.2267g, 0.2379g, 0.2013g and 0.2777g of potassium borohydride in four times every 10 hours, After stirring and reacting for 96 hours, centrifuge to obtain a brown solid product, then filter and wash the product with anhydrous methanol, and dry naturally to obtain a compound intercalated with potassium tin disulfide.

[0023] See attached figure 1 , for the product potassium tin disulfide intercalation compound (KSnS 2 ) for XRD spectrum detection, it can be seen from the spectrum that the product has a strong peak at about 10 degrees, which can confirm that the alkali metal ions have been well inserted between the sheets of the transition metal dichalcogenide inorganic material. ...

Embodiment 3

[0025] a, take chemically pure tin disulfide 1.0375g, join in the anhydrous methanol of 80ml, stir 30 minutes under the condition of ice bath;

[0026] b. When the temperature of the above solution drops to 0°C, add 0.1037g of analytically pure potassium borohydride, then keep stirring, and add 0.0637g, 0.3587g and 0.1900g of potassium borohydride three times every 10 hours, and stir for 96 hours After centrifugation, a brown solid product was obtained, and then the product was filtered and washed with anhydrous methanol, and the compound intercalated with potassium tin disulfide was obtained after natural drying.

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Abstract

The invention discloses a preparation method of alkali metal intercalated transition metal disulfide, which is characterized by taking the disulfide as the intercalated subject and borohydride as the intercalated object and intercalating the alkali metal ions among the lamellae of the transition metal disulfide inorganic materials through hybridization reaction to prepare the compound of the alkali metal ion intercalated disulfide. Compared with the prior art, the method has safe and simple synthesis process, is convenient to operate, expands the interlamellar spacing of the disulfide, provides cheap and easily-obtained raw materials for synthesis of functional intercalated composite materials and has broad application prospect.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis materials, in particular to a preparation method of alkali metal intercalated transition metal disulfides. Background technique [0002] Intercalation compound is a new type of multifunctional material. It combines layered host compounds with different functional intercalation guests to obtain layered materials with special properties. Compared with conventional composite materials, intercalation materials have Significant changes have been made in thermal, mechanical, optical, electrical and magnetic properties. Therefore, the research on intercalated layered compounds not only has very important basic theoretical academic value, but also has broad practical prospects. As the research on intercalation compounds in the fields of electrochemical energy storage, sensors, catalyst supports and sealing materials continues to deepen, such as catalyst precursors, photosensitizers and organic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/20C01G19/00C01G39/06
Inventor 吕晴李强
Owner EAST CHINA NORMAL UNIV
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