阅读说明：本技术 一种五硫化二磷粉体的机械球磨合成方法 (A kind of mechanical ball mill synthetic method of phosphorus pentasulfide powder ) 是由 梁初 潘良斌 王俊豪 黄辉 张文魁 甘永平 夏阳 张俊 于 2019-08-26 设计创作，主要内容包括：本发明公开了一种五硫化二磷粉体的机械球磨合成方法,该制备方法包括如下步骤：(1)在惰性气氛保护下,将五氯化磷与硫化锂粉末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,将固体产物从球磨罐中取出,回收过量的五氯化磷；(4)将剩余固体产物分离后即可获得五硫化二磷粉体。本发明所述的五硫化二磷粉体的制备方法具有工艺简单、成本低、易于工业化生产的特点。(The invention discloses a kind of mechanical ball mill synthetic method of phosphorus pentasulfide powder, which includes the following steps: that (1) under inert atmosphere protection, phosphorus pentachloride and vulcanization lithium powder 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, solid product is taken out from ball grinder under an inert atmosphere, recycles excessive phosphorus pentachloride；(4) phosphorus pentasulfide powder will be can be obtained after the separation of remaining solid product.Phosphorus pentasulfide raw powder's production technology of the present invention has the characteristics that simple process, at low cost, easy to industrialized production.)

1. a kind of mechanical ball mill synthetic method of phosphorus pentasulfide powder, which comprises the steps of:

(1) under inert atmosphere protection, phosphorus pentachloride and vulcanization lithium powder 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, under an inert atmosphere, solid product is taken out to the excessive phosphorus pentachloride of recycling from ball grinder；

(4) remaining solid product is added in a certain amount of solvent, after separation of solid and liquid, drying solid obtains phosphorus pentasulfide powder Body.

2. a kind of mechanical ball mill synthetic method of phosphorus pentasulfide powder as described in claim 1, which is characterized in that the vulcanization The purity of lithium powder and phosphorus pentachloride is not less than 90%.

3. a kind of mechanical ball mill synthetic method of phosphorus pentasulfide powder as described in claim 1, which is characterized in that the step (1) molar ratio of vulcanization lithium powder and phosphorus pentachloride is 5:(2-4 in).

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

5. a kind of mechanical ball mill synthetic method of phosphorus pentasulfide 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 1-100h, mechanical ball mill reaction temperature are room temperature.

6. a kind of mechanical ball mill synthetic method of phosphorus pentasulfide powder as described in claim 1, which is characterized in that the step (3) in, the method for recycling excessive phosphorus pentachloride is that solid product is added in toluene, after separation of solid and liquid, is obtained containing phosphorus pentachloride Toluene solution, liquid toluene and solid phosphorus pentachloride are distilled to recover at 110-150 DEG C.

7. a kind of mechanical ball mill synthetic method of phosphorus pentasulfide powder as described in claim 1, which is characterized in that the step (4) in, solvent is acetone, and the additive amount of acetone is subject to the impurity in abundant dissolved solid product.

8. a kind of mechanical ball mill synthetic method of phosphorus pentasulfide powder as described in claim 1, which is characterized in that the step (4) in, drying temperature is 80 DEG C.

9. a kind of mechanical ball mill synthetic method of phosphorus pentasulfide powder as described in claim 1, which is characterized in that described is lazy Property atmosphere is the gas that will not be reacted with lithium sulfide, phosphorus pentachloride, lithium chloride and phosphorus pentasulfide, including argon gas, nitrogen and The mixed gas of nitrogen and argon gas.

Technical field

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

Background technique

Phosphorus pentasulfide is a kind of inorganic compound, chemical formula P₂S₅, it is yellow and yellow green crystalline material, drying Shi Wending, but water facile hydrolysis is met into phosphoric acid and hydrogen sulfide.With the development of the industries such as automobile, petroleum, medicine, the five of high quality The demand for vulcanizing two phosphorus powder bodies rises year by year.The synthetic method of existing phosphorus pentasulfide is mainly liquid phase method (Li Gang, five sulphur Change the preparation method of two phosphorus), liquid elemental sulphur (Sulfur) and phosphorus (yellow phosphorus) are stoichiometrically passed through in reaction kettle and are reacted, The reaction product of acquisition passes through distilation, then cools and solidifies the liquid phosphorus pentasulfide after purification.Existing five vulcanization The synthesis technology of two phosphorus there are preparation processes it is complicated, products obtained therefrom quality is not high, energy consumption is high the defects of, thus, develop a kind of new Type, the synthetic method of efficient, environmental-friendly phosphorus pentasulfide 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 phosphorus pentasulfide powder of industrialized production.

Technical solution of the present invention is illustrated below.

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

(1) under inert atmosphere protection, phosphorus pentachloride and vulcanization lithium powder 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, solid product is taken out from ball grinder under an inert atmosphere, is recycled excessive phosphoric Phosphorus；

(4) remaining solid product is added in a certain amount of solvent, after separation of solid and liquid, drying solid obtains phosphorus pentasulfide Powder.

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

In the present invention, the molar ratio of vulcanization lithium powder and phosphorus pentachloride is 5:(2-4 in the step (1)).

In the present invention, vulcanization lithium powder and the gross mass of phosphorus pentachloride 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 1-100h, mechanical ball Mill reaction temperature is room temperature.

In the present invention, in the step (3), the method for recycling excessive phosphorus pentachloride is that solid product is added to toluene In, after separation of solid and liquid, the toluene solution containing phosphorus pentachloride is obtained, in 110-150 DEG C of retort solution withdrawal liquid toluene and solid Phosphorus pentachloride.

In the present invention, in the step (4), solvent is acetone, and the additive amount of acetone is in abundant dissolved solid product Subject to impurity.

In the present invention, in the step (4), drying temperature is 80 DEG C.

In the present invention, the inert atmosphere is that will not react with lithium sulfide, phosphorus pentachloride, lithium chloride and phosphorus pentasulfide Gas, such as the mixed gas of argon gas, nitrogen or nitrogen and argon gas.

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

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

Phosphorus pentasulfide is synthesized under mechanical ball mill using lithium sulfide and phosphorus pentachloride in the present invention, is that a kind of resource is reasonable The green synthesis method utilized.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 synthetic 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 phosphorus pentachloride that the embodiment of the present invention uses is not less than chemical pure (> 90%).