CN101851010A

CN101851010A - Synthesizing method for transition metal sulfide

Info

Publication number: CN101851010A
Application number: CN 201010193829
Authority: CN
Inventors: 焦丽芳; 袁华堂; 王一菁; 王庆红; 宋大卫; 杜红梅; 彭文修; 韩燕�
Original assignee: Nankai University
Current assignee: Nankai University
Priority date: 2010-06-08
Filing date: 2010-06-08
Publication date: 2010-10-06
Anticipated expiration: 2030-06-08
Also published as: CN101851010B

Abstract

The invention relates to a synthesizing method for a transition metal sulfide, which comprises the following steps: 1) dissolving cobalt salt or copper salt which can be dissolved in ethanol in ethanol, then adding CS2; 2) transferring the obtain solution to an autoclave for conducting heated and constant-temperature reaction to produce transition metal sulfide powder; and 3) sequentially filtering, washing and vacuum-drying the produced transition metal sulfide powder to obtain the finished product, wherein the cobalt salt or copper salt which can be dissolved in ethanol is sulfate, chlorate, nitrate or acetate. The invention has the advantages that the cost of raw materials is low, the production technology is simple, the reaction conditions can be easily controlled, the template agent and the surfactant are not required, the uniformity of the obtained product is good, the environment-friendliness is high and the mass production of the transition metal sulfide is facilitated.

Description

A kind of synthetic method of transient metal sulfide

[technical field]

The present invention relates to field of material synthesis technology, particularly a kind of synthetic method of transient metal sulfide.

[background technology]

In recent years, transient metal sulfide is because performances such as its excellent light, electricity, magnetic, lubricated and catalysis, and caused extensive studies interest, now be successfully applied to every field, as the negative material of commercial catalysts, lithium ion battery and alkaline secondary cell, semiconductor material, photoelectron material etc.Transient metal sulfide also is applied to the environmental protection field, is bringing into play important effect aspect the heavy metal removal.

Traditional synthetic technology of transient metal sulfide relates to high energy and noble gas protection heterogeneous reaction down more, adopts usually that high temperature gas phase or high temperature solid-state are synthetic, ion exchange reaction is synthetic, methods such as organism pyrolysis and electrochemical synthesis.But these methods have the raw materials cost height, the working condition harshness, and complex process, controllable factor is few, can't form shortcomings such as batch process, is unfavorable for the widespread production and the application of transient metal sulfide.

[summary of the invention]

The objective of the invention is at above-mentioned existing problems, a kind of synthetic method of transient metal sulfide is provided, this method raw materials cost is low, production technique simple, reaction conditions is easy to control, need not to add template and tensio-active agent, the products obtained therefrom high conformity, non-environmental-pollution helps the mass production of transient metal sulfide.

Technical scheme of the present invention:

A kind of synthetic method of transient metal sulfide may further comprise the steps:

1) will dissolve in alcoholic acid cobalt salt or mantoquita and be dissolved in ethanol, add CS then ₂2) above-mentioned solution is transferred in the autoclave, carries out the heated constant temperature reaction, generate the transient metal sulfide powder; 3) the transient metal sulfide powder that generates is filtered successively, washing and vacuum drying treatment, can make finished product.

Describedly dissolve in the alcoholic acid cobalt salt or mantoquita is vitriol, chlorate, nitrate or acetate.

Described cobalt salt or mantoquita and CS ₂Mol ratio be 1: 50～150, cobalt salt or mantoquita and consumption of ethanol are than being 0.25mol/L.

The temperature of described heated constant temperature reaction is (180～240) ℃, reaction times 24h.

Described washing methods is respectively given a baby a bath on the third day after its birth inferior with deionized water and dehydrated alcohol, vacuum drying vacuum tightness is-0.1MPa that the time is 12h.

Advantage of the present invention is: raw materials cost is cheap, and production technique is simple, and reaction conditions is easy to control, does not need template and tensio-active agent, the products obtained therefrom high conformity, and eco-friendly advantage helps the mass production of transient metal sulfide.

[description of drawings]

Fig. 1 is X-ray diffraction (XRD) figure of transient metal sulfide, wherein, and the X-ray diffractogram of the CoS that Figure 1A is generated for embodiment 1, the CoS that Figure 1B is generated for embodiment 2 ₂X-ray diffractogram, the X-ray diffractogram of the CuS that Fig. 1 C is generated for embodiment 3.

Fig. 2 is scanning electron microscope (SEM) figure of transient metal sulfide, wherein, and the sem photograph of the CoS that Fig. 2 A is generated for embodiment 1, the CoS that Fig. 2 B is generated for embodiment 2 ₂Sem photograph, the sem photograph of the CuS that Fig. 2 C is generated for embodiment 3.

[embodiment]

Embodiment 1:

The 2.5mmol cobalt chloride is dissolved in 10ml ethanol, adds 10mlCS ₂, be transferred to then in the autoclave, heat 24h down at 220 ℃, behind the naturally cooling, use deionized water and absolute ethanol washing three times respectively, dry 12h can obtain transient metal sulfide under 60 ℃.

Present embodiment 1 transient metal sulfide that generates consist of CoS.Its X-ray diffractogram (XRD) is shown in accompanying drawing 1A, and its sem photograph (SEM) is shown in accompanying drawing 2A.

Embodiment 2:

2.5mmol cobaltous sulfide cobalt is dissolved in 10ml ethanol, adds 20mlCS ₂, be transferred to then in the autoclave, heat 24h down at 220 ℃, behind the naturally cooling, use deionized water and absolute ethanol washing three times respectively, dry 12h can obtain transient metal sulfide under 60 ℃.

Present embodiment 2 transient metal sulfide that generates consist of CoS ₂Its X-ray diffractogram (XRD) is shown in accompanying drawing 1B, and its sem photograph (SEM) is shown in accompanying drawing 2B.

Embodiment 3:

The 2.5mmol cupric chloride is dissolved in 10ml ethanol, adds 15mlCS ₂, be transferred to after the stirring in the autoclave, heat 24h down at 220 ℃, behind the naturally cooling, use deionized water and absolute ethanol washing three times respectively, dry 12h can obtain transient metal sulfide under 60 ℃.

Present embodiment 3 transient metal sulfide that generates consist of CuS.Its X-ray diffractogram (XRD) is shown in accompanying drawing 1C, and its sem photograph (SEM) is shown in accompanying drawing 2C.

Claims

1. the synthetic method of a transient metal sulfide is characterized in that may further comprise the steps: 1) will dissolve in alcoholic acid cobalt salt or mantoquita and be dissolved in ethanol, and add CS then ₂2) above-mentioned solution is transferred in the autoclave, carries out the heated constant temperature reaction, generate the transient metal sulfide powder; 3) the transient metal sulfide powder that generates is filtered successively, washing and vacuum drying treatment, can make finished product.

2. according to the synthetic method of the described transient metal sulfide of claim 1, it is characterized in that: describedly dissolve in the alcoholic acid cobalt salt or mantoquita is vitriol, chlorate, nitrate or acetate.

3. according to the synthetic method of the described transient metal sulfide of claim 1, it is characterized in that: described cobalt salt or mantoquita and CS ₂Mol ratio be 1: 50～150, cobalt salt or mantoquita and consumption of ethanol are than being 0.25mol/L.

4. according to the synthetic method of the described transient metal sulfide of claim 1, it is characterized in that: the temperature of described heated constant temperature reaction is (180～240) ℃, reaction times 24h.

5. according to the synthetic method of the described transient metal sulfide of claim 1, it is characterized in that: described washing methods is respectively given a baby a bath on the third day after its birth inferior with deionized water and dehydrated alcohol, vacuum drying vacuum tightness is-0.1MPa that the time is 12h.