阅读说明：本技术 一种硫化锂粉体的合成方法 (A kind of synthetic method vulcanizing powder for lithium ) 是由 梁初 王俊豪 孙鑫 张俊 黄辉 张文魁 甘永平 夏阳 于 2019-08-26 设计创作，主要内容包括：本发明公开了一种硫化锂粉体的合成方法,该合成方法包括如下步骤：(1)在惰性气氛保护下,将硫化硅与氧化锂均匀混合,转移至反应器并密封；(2)将反应器内的混合物加热保温反应一定时间；(3)待反应结束后降至室温,将固体产物从反应器中取出,溶剂法回收过量的硫化硅；(4)溶剂法分离剩余固体产物即得到硫化锂粉体。本发明所述的硫化锂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 synthetic method for vulcanizing powder for lithium, which includes the following steps: (1) under inert atmosphere protection, silicon sulfide is uniformly mixed with lithia, reactor is transferred to and seals；(2) the mixture heating and thermal insulation in reactor is reacted into certain time；(3) to be down to room temperature after reaction, solid product is taken out from reactor, solvent method recycles excessive silicon sulfide；(4) solvent method separation remaining solid product obtains lithium sulfide powder.It is of the present invention vulcanization powder for lithium synthetic method have simple process, it is at low cost, be easy to industrialized productive prospecting.)

1. a kind of synthetic method for vulcanizing powder for lithium, which comprises the steps of:

(1) under inert atmosphere protection, silicon sulfide is uniformly mixed with lithia, reactor is transferred to and seals；

(2) mixture in reactor is heated to certain temperature and insulation reaction certain time；

(3) it is down to room temperature after reaction, takes out the product in reactor, solvent method recycles excessive silicon sulfide；

(4) vulcanization powder for lithium can be obtained in solvent method separation remaining solid product.

2. claim 1 as described in it is a kind of vulcanize powder for lithium synthetic method, which is characterized in that the silicon sulfide and lithia Purity be not less than 90%.

3. a kind of synthetic method for vulcanizing powder for lithium as described in claim 1, which is characterized in that silicon sulfide in the step (1) Molar ratio with lithia is (1-3): 2.

4. a kind of synthetic method for vulcanizing powder for lithium as described in claim 1, which is characterized in that in the step (2), heating Heating rate is 0.5-20 DEG C/min, and insulation reaction temperature is 100-500 DEG C, soaking time 1-100h.

5. a kind of synthetic method for vulcanizing powder for lithium as described in claim 1, which is characterized in that in the step (3), solvent method Recycling excessive silicon sulfide is solid product to be added in a certain amount of benzene, and the additive amount of benzene, which is subject to, sufficiently dissolves silicon sulfide, solid-liquid Separation, obtains the benzole soln of silicon sulfide, liquid benzene is distilled to recover at 85-120 DEG C, remaining is silicon sulfide.

6. a kind of synthetic method for vulcanizing powder for lithium as described in claim 1, which is characterized in that in the step (4), solvent method Separation is remaining solid to be added in a certain amount of ethyl alcohol, and the additive amount of ethyl alcohol, which is subject to, sufficiently dissolves lithium sulfide, is separated by solid-liquid separation, obtains It to the ethanol solution of lithium sulfide, is distilled at 80-100 DEG C, recycles ethyl alcohol, and dried solid at 90-100 DEG C and vulcanized Powder for lithium.

7. a kind of synthetic method for vulcanizing powder for lithium as claimed in claim 6, which is characterized in that inertia described in step (1) Atmosphere is the gas not reacted with reactant and product or their mixture, including argon gas and nitrogen.

Technical field

The invention belongs to field of material synthesis technology, and in particular to a kind of synthetic method for vulcanizing powder for lithium.

Background technique

Lithium sulfide is a kind of inorganic compound, chemical formula Li₂S belongs to cubic system, anti-fluorite structure, in sky It is easily deliquesced in gas.Currently, the synthetic method in relation to lithium sulfide is less, Chinese invention patent (publication number CN106784754A) is public It has opened and sulphur powder has been put into the tetrahydrofuran solution containing lithium triethylborohydride, after sufficiently reacting, by solid powder and liquid Body separation obtains lithium sulfide；Chinese invention patent (publication number CN108190845A) discloses, and sulphur powder and metallic lithium powder are added In liquefied ammonia, after sufficiently reacting, solid powder is separated with liquid and obtains lithium sulfide.Above-mentioned two classes method requires to have used The harmful solvent of poison, efficiency is lower, higher cost, expensive, it is difficult to realize industrialized production.In addition, using lithium sulfate and Coke is raw material, also can get lithium sulfide by 800-900 DEG C of high-temperature calcination method.But there are purity for lithium sulfide made from this method It is not high, the disadvantages of batch difference, energy consumption, it is also not susceptible to industrialized production.Thus, develop a kind of novel, efficient, environmental-friendly Lithium sulfide synthetic method is 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 powder for lithium of industrialized production.

It is as follows that the technical scheme adopted by the invention to solve the technical problem:

Lithium sulfide synthesis method of the present invention, is realized using heating, synthetic method the following steps are included:

(1) under inert atmosphere protection, silicon sulfide is uniformly mixed with lithia, reactor is transferred to and seals；

(2) mixture in reactor is heated to certain temperature and insulation reaction certain time；

(3) it is down to room temperature after reaction, takes out the product in reactor, solvent method recycles excessive silicon sulfide；

(4) vulcanization powder for lithium can be obtained in solvent method separation remaining solid product.

In the present invention, the purity of silicon sulfide and lithia is not less than 90% in the step (1).

In the present invention, the molar ratio of silicon sulfide and lithia is (1-3) in the step (1): 2.

In the present invention, in the step (2), the heating rate of heating is 0.5-20 DEG C/min, and insulation reaction temperature is 100-500 DEG C, soaking time 1-100h.

In the present invention, in the step (3), it is that solid product is added to a certain amount of benzene that solvent method, which recycles excessive silicon sulfide, In, the additive amount of benzene, which is subject to, sufficiently dissolves silicon sulfide, is separated by solid-liquid separation, obtains the benzole soln of silicon sulfide, steam at 85-120 DEG C Withdrawal liquid benzene is evaporated, remaining is silicon sulfide.

In the present invention, in the step (4), solvent method separation is remaining solid to be added in a certain amount of ethyl alcohol, ethyl alcohol Additive amount, which is subject to, sufficiently dissolves lithium sulfide, is separated by solid-liquid separation, obtains the ethanol solution of lithium sulfide, distill at 80-100 DEG C, returns Ethyl alcohol is received, and dries solid at 90-100 DEG C and obtains vulcanization powder for lithium.

In the present invention, inert atmosphere described in step (1) be the gas not reacted with reactant and product or Their mixture, including argon gas and nitrogen.

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

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

Lithium sulfide is synthesized under heating using silicon sulfide and lithia in the present invention, is a kind of green of resource rational utilization Synthetic method.This method is environmental-friendly, is easy to industrializing implementation, and no exhaust gas and waste generate.

Detailed description of the invention

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

Specific implementation method

With reference to the accompanying drawing, technical solution of the present invention is described further with specific embodiment, but guarantor of the invention It is without being limited thereto to protect range.

The purity of silicon sulfide and lithia that the embodiment of the present invention uses is not less than chemical pure (> 90%).