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Prepn process transition metal sulfide intercalated lithium

A transition metal and sulfide technology, applied in the field of preparation of transition metal sulfide lithium intercalation, can solve the problems of low yield of transition metal sulfide intercalation materials, low stripping and heavy stacking efficiency, etc.

Inactive Publication Date: 2007-03-21
HUAQIAO UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the lithium insertion amount x between the transition metal sulfide interlayers is small at room temperature, which makes the subsequent stripping and restacking efficiency low, and the yield of transition metal sulfide intercalation materials is low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0010] Using n-butyllithium as a reducing agent and n-hexane as a solvent, a preparation method for transition metal sulfide intercalation lithium of the present invention is realized through the following steps:

[0011] (1) According to 0.5mol·dm -3 Concentration requirements, prepare 12 cubic decimeters of n-hexane solution of n-butyllithium;

[0012] (2) Weigh 0.5kg of tungsten disulfide and pour it into a 20 cubic decimeter autoclave;

[0013] (3) The n-hexane solution of 12 cubic decimeters of n-butyllithium prepared is added in the autoclave, and the reactor is tightly covered;

[0014] (4) Heating the reactor and reacting at a constant temperature of 95°C for 5 hours (the pressure of the reactor was about 2Mpa at this time);

[0015] (5) stop reaction, cool down naturally;

[0016] (6) unloading, with hexanaphthene or normal hexane or their mixture washing product, remove unnecessary n-butyllithium;

[0017] (7) Vacuum drying to obtain lithium intercalation compoun...

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Abstract

The present invention discloses preparation process of transition metal sulfide intercalated lithium compound. By means of solvent heat with medium temperature and high pressure, solvent, transition metal sulfide and reductant are reacted in a high pressure kettle at 75-150 deg.c, with the molar ratio between the reductant and the transition metal sulfide being 1 to 12, to obtain intercalated lithium compound LixMS2 with lithium inserting amount x of 0.75-1.90. The preparation process can peel off transition metal sulfide fully to reach transition metal sulfide intercalated material yield up to 85 %.

Description

technical field [0001] The invention relates to a preparation method for transition metal sulfide intercalation lithium, which can be used to manufacture transition metal sulfide intercalation materials. Background technique [0002] Currently, the exfoliation-restacking preparation method is used to manufacture transition metal sulfide intercalation materials. That is, lithium is first inserted into the transition metal sulfide interlayer domain at room temperature to form the lithium intercalation compound Li x MS 2 (M is Mo, W, Nb, etc.), and then Li x MS 2 Reaction with water to achieve MS 2 The sheets are peeled off, and finally the host and guest are reaccumulated into an intercalation composite under the action of the guest. However, the lithium intercalation amount x between the transition metal sulfide layers is small at room temperature, which makes the subsequent stripping and restacking efficiency low, and the yield of transition metal sulfide intercalation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G1/12C01B17/20
Inventor 林碧洲许百环
Owner HUAQIAO UNIVERSITY