阅读说明：本技术 一种硫化硅粉体的机械球磨合成方法 (A kind of mechanical ball mill synthetic method vulcanizing silicon powder ) 是由 梁初 王俊豪 张佰伦 张文魁 甘永平 夏阳 张俊 黄辉 于 2019-08-26 设计创作，主要内容包括：本发明公开了一种硫化硅粉体的机械球磨合成方法,该合成方法包括如下步骤：(1)在惰性气氛保护下,将硫化锂粉末与四氯化硅加入到密封的球磨罐中；(2)在室温下将球磨罐装在球磨机上,并以一定转速球磨反应一定时间；(3)反应结束后,在惰性气氛下,通过蒸馏方法回收过量的四氯化硅；(4)将球磨罐中固体产物取出并加入到苯中,固液分离后,得到含硫化硅的苯溶液,蒸馏溶液并烘干固体即可获得硫化硅粉体。本发明所述的硫化硅粉体的合成方法具有工艺简单、成本低、易于工业化的生产特点。(The invention discloses a kind of mechanical ball mill synthetic method for vulcanizing silicon powder, which includes the following steps: that (1) under inert atmosphere protection, vulcanization lithium powder and silicon tetrachloride are added in the ball grinder of sealing；(2) at room temperature by ball grinder on ball mill, and with certain revolving speed ball-milling reaction certain time；(3) after reaction, excessive silicon tetrachloride under an inert atmosphere, is recycled by distillating method；(4) solid product in ball grinder is taken out and is added in benzene, after separation of solid and liquid, obtain the benzole soln of sulfur-bearing SiClx, retort solution simultaneously dries solid and can be obtained vulcanization silicon powder.It is of the present invention vulcanization silicon powder synthetic method have simple process, it is at low cost, be easy to industrialized productive prospecting.)

1. a kind of mechanical ball mill synthetic method for vulcanizing silicon powder, which comprises the steps of:

(1) under inert atmosphere protection, vulcanization lithium powder and silicon tetrachloride are added in the ball grinder of sealing；

(2) at room temperature by ball grinder on ball mill, with certain revolving speed machinery ball-milling reaction certain time；

(3) after reaction, excessive silicon tetrachloride under an inert atmosphere, is recycled by distillating method；

(4) solid product in ball grinder is taken out and is added in a certain amount of solvent, after separation of solid and liquid, retort solution is consolidated Body obtains vulcanization silicon powder after drying solid.

2. a kind of mechanical ball mill synthetic method for vulcanizing silicon powder as described in claim 1, which is characterized in that the lithium sulfide The purity of powder and silicon tetrachloride is not less than 90%.

3. a kind of mechanical ball mill synthetic method for vulcanizing silicon powder as described in claim 1, which is characterized in that the step (1) The molar ratio of middle vulcanization lithium powder and silicon tetrachloride is 2:(1-3).

4. a kind of mechanical ball mill synthetic method for vulcanizing silicon powder as described in claim 1, which is characterized in that the step (2) The total mass ratio of the gross mass and abrading-ball of middle vulcanization lithium powder and silicon tetrachloride is 1:(10-80).

5. a kind of mechanical ball mill synthetic method for vulcanizing silicon powder as described in claim 1, which is characterized in that the step (2) In, rotational speed of ball-mill 100-500rpm/min, Ball-milling Time 2-100h, mechanical ball mill reaction temperature are room temperature.

6. a kind of mechanical ball mill synthetic method for vulcanizing silicon powder as described in claim 1, which is characterized in that the step (3) In, the temperature for being distilled to recover excessive silicon tetrachloride is 60-100 DEG C.

7. a kind of mechanical ball mill synthetic method for vulcanizing silicon powder as described in claim 1, which is characterized in that the step (4) In, solvent is benzene, and the additive amount of benzene is subject to the silicon sulfide in abundant dissolved solid product.

8. a kind of mechanical ball mill synthetic method for vulcanizing silicon powder as claimed in claim 7, which is characterized in that distillation removal benzene Temperature is 82-120 DEG C.

9. a kind of mechanical ball mill synthetic method for vulcanizing silicon powder as described in claim 1, which is characterized in that the step (4) In, drying temperature is 100 DEG C.

10. a kind of mechanical ball mill synthetic method for vulcanizing silicon powder as described in claim 1, which is characterized in that the inertia Atmosphere is the gas that will not be reacted with lithium sulfide, silicon tetrachloride, silicon sulfide and lithium chloride, including argon gas, nitrogen and argon gas and The mixed gas of nitrogen.

Technical field

The invention belongs to materials synthesis fields, are related to a kind of mechanical ball mill synthetic method for vulcanizing silicon powder.

Background technique

Silicon sulfide is a kind of inorganic compound, chemical formula SiS₂, belong to rectangle or tetragonal system, it is steady under normal temperature and pressure It is fixed, it meets moisture and just resolves into SiO₂And H₂S.Currently, the synthetic method in relation to silicon sulfide is less.Patent (application publication number JPS62252310A the method for the silicon dioxde reaction acquisition silicon sulfide of sulfur vapor or hydrogen sulfide gas and boiling) is disclosed.This Kind method will be by high-temperature heating, and efficiency is lower, higher cost, it is difficult to realize industrialized production.Therefore develop a kind of novel, high Effect, environmental-friendly silicon sulfide synthetic method are of great significance.

Summary of the invention

The invention aims to solve the deficiencies in the prior art, provide it is a kind of it is efficient, inexpensive, environmental-friendly, be easy to The new method of the synthesis vulcanization silicon powder of industrialized production.

Technical solution of the present invention is illustrated below.

The mechanical ball mill synthetic method of vulcanization silicon powder of the present invention, comprising the following steps:

(1) under inert atmosphere protection, vulcanization lithium powder and silicon tetrachloride are added in the ball grinder of sealing；

(2) at room temperature by ball grinder on ball mill, with certain revolving speed machinery ball-milling reaction certain time；

(3) after reaction, excessive silicon tetrachloride under an inert atmosphere, is recycled by distillating method；

(4) solid product in ball grinder is taken out and is added in a certain amount of solvent, after separation of solid and liquid, retort solution is obtained Solid, and vulcanization silicon powder is obtained after drying solid.

In the present invention, the purity of the vulcanization lithium powder and silicon tetrachloride is not less than 90%.

In the present invention, the molar ratio of vulcanization lithium powder and silicon tetrachloride is 2:(1-3 in the step (1)).

In the present invention, vulcanization lithium powder and the gross mass of silicon tetrachloride and the total mass ratio of abrading-ball are in the step (2) 1:(10-80).

In the present invention, in the step (2), rotational speed of ball-mill 100-500rpm/min, Ball-milling Time 2-100h are mechanical Ball-milling reaction temperature is room temperature.

In the present invention, in the step (3), the temperature for being distilled to recover excessive silicon tetrachloride is 60-100 DEG C.

In the present invention, in the step (4), solvent is benzene, and the additive amount of benzene is with the vulcanization in abundant dissolved solid product Subject to silicon, the temperature of distillation removal benzene is 82-120 DEG C.

In the present invention, in the step (4), drying temperature is 100 DEG C.

In the present invention, the inert atmosphere is the gas that will not be reacted with lithium sulfide, silicon tetrachloride, silicon sulfide and lithium chloride Body, such as the mixed gas of argon gas, nitrogen or argon gas and nitrogen.

In the present invention, " room temperature " is 0-40 DEG C.

Compared with prior art, the present invention its advantages are mainly reflected in:

Silicon sulfide is synthesized under mechanical ball mill using lithium sulfide and silicon tetrachloride in the present invention, is a kind of resource rational utilization Green synthesis method.The synthetic method is efficient, at low cost, environmental-friendly, and is easy to industrializing implementation.

Detailed description of the invention

Fig. 1 is the X-ray diffractogram of 1 reaction product of the embodiment of the present invention.

Specific implementation method

With reference to the accompanying drawing, technical solution of the present invention is described further with specific embodiment, but need to pay attention to It is that the scope of protection of the present invention is not limited to this.

The purity of vulcanization lithium powder and silicon tetrachloride that the embodiment of the present invention uses is not less than chemical pure (> 90%).