CN100436327C - Prepn process transition metal sulfide intercalated lithium - Google Patents
Prepn process transition metal sulfide intercalated lithium Download PDFInfo
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- CN100436327C CN100436327C CNB2006100962401A CN200610096240A CN100436327C CN 100436327 C CN100436327 C CN 100436327C CN B2006100962401 A CNB2006100962401 A CN B2006100962401A CN 200610096240 A CN200610096240 A CN 200610096240A CN 100436327 C CN100436327 C CN 100436327C
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- metal sulfide
- transition metal
- lithium
- solvent
- reductive agent
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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
The present invention relates to a kind of preparation method of transition metal sulfide intercalated lithium, can be used for making transition metal sulfide intercalated layer material.
Background technology
What at present, make that transition metal sulfide intercalated layer material adopts is to peel off-heavily pile up the preparation method.Just, at ambient temperature lithium is inserted in the transient metal sulfide interlamination region earlier, forms and insert lithium compound Li
xMS
2(M is Mo, W, Nb etc.), after with Li
xMS
2Realize MS with the water reaction
2Peeling off of lamella allows host and guest's body weight be piled into intercalation composite material at last under the object effect.But the lithium insertion amount x of transient metal sulfide interlayer is less under the room temperature condition, make follow-up peel off and heavy deposition efficiency lower, the productive rate of transition metal sulfide intercalated layer material is lower.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method who obtains the transition metal sulfide intercalated lithium of high lithium insertion amount, the productive rate that improves intercalation material and quality.
Technical scheme of the present invention is such: a kind of preparation method of transition metal sulfide intercalated lithium, 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 Li
xMS
2Above-mentioned solvent is hexanaphthene or normal hexane or their mixture, and above-mentioned reductive agent is n-Butyl Lithium or lithium borohydride.
Above-mentioned reductive agent is 2: 1～8: 1 with the ratio of the mole number of transient metal sulfide.
The temperature of reaction of above-mentioned hexanaphthene or normal hexane or their mixture thermal response is 85～120 ℃.
High lithium insertion amount x can realize fully peeling off of transient metal sulfide or the overwhelming majority is peeled off, thereby has improved the productive rate and the quality of intercalation material, satisfies the requirement of Technological Economy.After adopting such scheme, the inventive method is utilized the middle temperature high pressure characteristics of solvent thermal, can get x (lithium insertion amount) scope and be 0.75～1.90 slotting lithium compound Li
xMS
2, transient metal sulfide is fully peeled off or the overwhelming majority is peeled off, and transition metal sulfide intercalated layer material productive rate is reached more than 85%.
Embodiment
With the n-Butyl Lithium is reductive agent, and normal hexane is a solvent, and the preparation method that his thing of a kind of transition metal sulphur of the present invention is inserted lithium realizes as follows:
(1) presses 0.5moldm
-3Concentration requirement, 12 cubic decimeters of the hexane solutions of preparation n-Butyl Lithium;
(2) taking by weighing tungsten disulfide 0.5kg pours in 20 cubic decimeters the autoclave;
The hexane solution of 12 cubic decimeters of n-Butyl Lithiums (3) will preparing joins in the autoclave, covers tight reactor;
(4) reacting by heating still is in 95 ℃ of following isothermal reactions 5 hours (this moment, the pressure of reactor was about 2Mpa);
(5) stopped reaction, naturally cooling;
(6) discharging with hexanaphthene or normal hexane or their mixture washed product, is removed unnecessary n-Butyl Lithium;
(7) vacuum-drying promptly gets and inserts lithium compound Li
xWS
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 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100962401A CN100436327C (en) | 2006-09-29 | 2006-09-29 | Prepn process transition metal sulfide intercalated lithium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100962401A CN100436327C (en) | 2006-09-29 | 2006-09-29 | Prepn process transition metal sulfide intercalated lithium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1931725A CN1931725A (en) | 2007-03-21 |
| CN100436327C true CN100436327C (en) | 2008-11-26 |
Family
ID=37877775
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100962401A Expired - Fee Related CN100436327C (en) | 2006-09-29 | 2006-09-29 | Prepn process transition metal sulfide intercalated lithium |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100436327C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948099B (en) * | 2010-09-15 | 2012-08-08 | 华东师范大学 | Preparation method of alkali metal intercalated transition metal disulfide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1413910A (en) * | 2002-11-27 | 2003-04-30 | 南开大学 | Transition metal sulfied nano-pipe and preparation process and its application |
| US20040105808A1 (en) * | 2000-03-06 | 2004-06-03 | Reshef Tenne | Reactors for producing inoraganic fullerene-like tungsten disulfide hollow nanoparticles and nanotubes |
| CN1613750A (en) * | 2004-09-24 | 2005-05-11 | 武汉大学 | Preparation for metal sulfide |
-
2006
- 2006-09-29 CN CNB2006100962401A patent/CN100436327C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040105808A1 (en) * | 2000-03-06 | 2004-06-03 | Reshef Tenne | Reactors for producing inoraganic fullerene-like tungsten disulfide hollow nanoparticles and nanotubes |
| CN1413910A (en) * | 2002-11-27 | 2003-04-30 | 南开大学 | Transition metal sulfied nano-pipe and preparation process and its application |
| CN1613750A (en) * | 2004-09-24 | 2005-05-11 | 武汉大学 | Preparation for metal sulfide |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1931725A (en) | 2007-03-21 |
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Granted publication date: 20081126 Termination date: 20100929 |