CN110526247A - A kind of mechanical ball mill synthetic method vulcanizing silicon powder - Google Patents
A kind of mechanical ball mill synthetic method vulcanizing silicon powder Download PDFInfo
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- CN110526247A CN110526247A CN201910792182.3A CN201910792182A CN110526247A CN 110526247 A CN110526247 A CN 110526247A CN 201910792182 A CN201910792182 A CN 201910792182A CN 110526247 A CN110526247 A CN 110526247A
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- ball mill
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- silicon powder
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
Abstract
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.
Description
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%).
Embodiment 1
Under argon atmosphere protection, 0.72g vulcanization lithium powder and 1.28g silicon tetrachloride are added to ball milling after evenly mixing
In tank.Then it is sealed after abrading-ball being put into ball grinder.Wherein abrading-ball gross mass and material total mass ratio are 40:1.In room temperature condition
Under, so that ball grinder is reacted 12h in the revolving speed continuous ball milling of 500r/min.After reaction, under an argon atmosphere, pass through 100 DEG C
It is distilled to recover excessive silicon tetrachloride.Solid product in ball grinder is taken out and is added in benzene, after separation of solid and liquid, is vulcanized
The benzole soln of silicon, 120 DEG C of retort solutions obtain solid, and 100 DEG C of drying solids can be obtained vulcanization silicon powder.Fig. 1 produces for it
The diffraction pattern of the x-ray of object can only symbolize the X-ray map of lithium chloride, according to mass conservation law, centainly have sulphur in product
SiClx.
Embodiment 2
Under argon atmosphere protection, 1.0g vulcanization lithium powder and 3.6g silicon tetrachloride are added to ball grinder after evenly mixing
In.Then it is sealed after abrading-ball being put into ball grinder.Wherein abrading-ball gross mass and material total mass ratio are 60:1.In room temperature condition
Under, so that ball grinder is reacted 20h in the revolving speed continuous ball milling of 350r/min.After reaction, under an argon atmosphere, it is steamed by 60 DEG C
Evaporate the excessive silicon tetrachloride of recycling.Solid product in ball grinder is taken out and is added in benzene, after separation of solid and liquid, obtains Containing Sulfur
The benzole soln of silicon, 82 DEG C of retort solutions obtain solid, and 100 DEG C of drying solids can be obtained vulcanization silicon powder.
Embodiment 3
Under argon atmosphere protection, 0.53g vulcanization lithium powder and 2.76g silicon tetrachloride are added to ball milling after evenly mixing
In tank.Then it is sealed after abrading-ball being put into ball grinder.Wherein abrading-ball gross mass and material total mass ratio are 10:1.In room temperature condition
Under, so that ball grinder is reacted 2h in the revolving speed continuous ball milling of 500r/min.After reaction, under an argon atmosphere, it is steamed by 80 DEG C
Evaporate the excessive silicon tetrachloride of recycling.Solid product in ball grinder is taken out and is added in benzene, after separation of solid and liquid, obtains Containing Sulfur
The benzole soln of silicon, 90 DEG C of retort solutions obtain solid, and 100 DEG C of drying solids can be obtained vulcanization silicon powder.
Embodiment 4
Under argon atmosphere protection, 2.53g vulcanization lithium powder and 4.79g silicon tetrachloride are added to ball milling after evenly mixing
In tank.Then it is sealed after abrading-ball being put into ball grinder.Wherein abrading-ball gross mass and material total mass ratio are 80:1.In room temperature condition
Under, so that ball grinder is reacted 100h in the revolving speed continuous ball milling of 100r/min.After reaction, under an argon atmosphere, pass through 90 DEG C
It is distilled to recover excessive silicon tetrachloride.Solid product in ball grinder is taken out and is added in benzene, after separation of solid and liquid, obtains sulfur-bearing
The benzole soln of SiClx, 100 DEG C of retort solutions obtain solid, and 100 DEG C of drying solids can be obtained vulcanization silicon powder.
Claims (10)
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.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112777571A (en) * | 2021-02-10 | 2021-05-11 | 山东瑞福锂业有限公司 | Method for synthesizing battery-grade lithium sulfide |
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| US20130029227A1 (en) * | 2011-07-26 | 2013-01-31 | Toyota Motor Engineering & Manufacturing North America, Inc. | Polyanion active materials and method of forming the same |
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| US20190036157A1 (en) * | 2017-07-25 | 2019-01-31 | Institute of Nuclear Energy Research, Atomic Energy Council, Executive Yuan, R.O.C. | All-solid-state battery, hybrid-structured solid electrolyte membrane and manufacturing methods thereof |
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2019
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| CN1807431A (en) * | 2005-10-31 | 2006-07-26 | 杭州师范学院 | Multiple functional radical silicide preparation method |
| CN104659411A (en) * | 2009-02-27 | 2015-05-27 | 丰田自动车株式会社 | Sulfide solid electrolyte material |
| US20130029227A1 (en) * | 2011-07-26 | 2013-01-31 | Toyota Motor Engineering & Manufacturing North America, Inc. | Polyanion active materials and method of forming the same |
| CN105502410A (en) * | 2015-12-23 | 2016-04-20 | 中国船舶重工集团公司第七一八研究所 | Preparation and purification methods of silicon tetrafluoride |
| US20190036157A1 (en) * | 2017-07-25 | 2019-01-31 | Institute of Nuclear Energy Research, Atomic Energy Council, Executive Yuan, R.O.C. | All-solid-state battery, hybrid-structured solid electrolyte membrane and manufacturing methods thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112777571A (en) * | 2021-02-10 | 2021-05-11 | 山东瑞福锂业有限公司 | Method for synthesizing battery-grade lithium sulfide |
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Application publication date: 20191203 |