CN100436327C - Prepn process transition metal sulfide intercalated lithium - Google Patents

Abstract

The invention discloses a preparation method for transition metal sulfide intercalation lithium, which utilizes the medium-temperature and high-pressure characteristics of solvothermal, puts solvent, transition metal sulfide and reducing agent in a high-pressure reaction kettle, and solvothermally reaction, wherein the molar ratio of the reducing agent to the transition metal sulfide is 1:1 to 12:1, and the lithium intercalation compound Li _x MS ₂ with x (lithium insertion amount) in the range of 0.75 to 1.90 can be obtained, which can not only make The transition metal sulfides are fully exfoliated or most of them are exfoliated, and the yield of transition metal sulfide intercalation materials can reach more than 85%.

Description

A kind of preparation method of transition metal sulfide intercalation lithium

technical field

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

Currently, the exfoliation-restacking preparation method is used to manufacture transition metal sulfide intercalation materials. That is, lithium is inserted into the transition metal sulfide interlayer domain at room temperature first to form a lithium intercalation compound Li _x MS ₂ (M is Mo, W, Nb, etc.), and then Li _x MS ₂ is reacted with water to achieve The MS ₂ sheets are peeled off, and finally the host and guest are re-accumulated 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 materials is low.

Contents of the invention

The purpose of the present invention is to provide a preparation method for transition metal sulfide intercalation lithium which can obtain high lithium intercalation amount and improve the yield and quality of intercalation materials.

The technical scheme of the present invention is as follows: a preparation method for lithium intercalation of transition metal sulfide is realized by the following scheme: put solvent, transition metal sulfide and reducing agent Thermal reaction, wherein the molar ratio of the reducing agent to the transition metal sulfide is 1:1 to 12:1, the molar ratio of the reducing agent to the solvent is 0.03:1 to 0.42:1, and the pressure of the reactor is 0.3 Mpa～100Mpa, the lithium intercalation compound Li _x MS ₂ with an x range of 0.75～1.90 can be obtained; the above solvent is cyclohexane or n-hexane or their mixture, and the above reducing agent is n-butyl lithium or lithium borohydride.

The molar ratio of the reducing agent to the transition metal sulfide is 2:1˜8:1.

The reaction temperature of the thermal reaction of the above-mentioned cyclohexane or n-hexane or their mixture is 85-120°C.

A high lithium intercalation amount x can achieve sufficient or most of the transition metal sulfide exfoliation, thereby improving the yield and quality of intercalation materials and meeting the technical and economic requirements. After adopting the above scheme, the method of the present invention utilizes the medium-temperature and high-pressure characteristics of solvothermal to obtain the lithium intercalation compound Li _x MS ₂ with x (lithium insertion amount) ranging from 0.75 to 1.90, which can not only fully strip transition metal sulfides or maximize Partial exfoliation, and the yield of the transition metal sulfide intercalation material can reach more than 85%.

Detailed ways

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

(1) According to the concentration requirement of 0.5mol·dm ^-3 , prepare 12 cubic decimeters of n-hexane solution of n-butyllithium;

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

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

(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);

(5) stop reaction, cool down naturally;

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

(7) Vacuum drying to obtain lithium intercalation compound Li _x WS ₂ .

Claims (3)

1, a kind of preparation method of transition metal sulfide intercalated lithium, it is characterized in that: be achieved by the following scheme: solvent, transient metal sulfide and reductive agent are put into autoclave solvent thermal reaction under 75～150 ℃ of temperature, wherein, reductive agent is 1: 1～12: 1 with the ratio of the mole number of transient metal sulfide, reductive agent is 0.03: 1～0.42: 1 with the ratio of the mole number of solvent, the pressure of reactor is 0.3MPa～100MPa, just can get the x scope and be 0.75～1.90 slotting lithium compound LixMS2; Above-mentioned solvent is hexanaphthene or normal hexane or their mixture, and above-mentioned reductive agent is n-Butyl Lithium or lithium borohydride.

2, the preparation method of a kind of transition metal sulfide intercalated lithium according to claim 1 is characterized in that: above-mentioned reductive agent is 2: 1～8: 1 with the ratio of the mole number of transient metal sulfide.

3, the preparation method of a kind of transition metal sulfide intercalated lithium according to claim 1 is characterized in that: the temperature of reaction of above-mentioned hexanaphthene or normal hexane or their mixture thermal response is 85～120 ℃.