CN110526224A - A kind of mechanical ball mill synthetic method of phosphorus pentasulfide powder - Google Patents
A kind of mechanical ball mill synthetic method of phosphorus pentasulfide powder Download PDFInfo
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- CN110526224A CN110526224A CN201910791155.4A CN201910791155A CN110526224A CN 110526224 A CN110526224 A CN 110526224A CN 201910791155 A CN201910791155 A CN 201910791155A CN 110526224 A CN110526224 A CN 110526224A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/14—Sulfur, selenium, or tellurium compounds of phosphorus
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Abstract
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.
Description
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%).
Embodiment 1
Under argon atmosphere protection, 0.75g vulcanization lithium powder and 1.32g phosphorus pentachloride 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, react ball grinder for 24 hours in the revolving speed continuous ball milling of 500r/min.It after reaction, under an argon atmosphere, will be in ball grinder
Solid product takes out and is added in toluene, is separated by solid-liquid separation, and the solution after separation is distilled to recover liquid toluene and is consolidated at 150 DEG C
Body phosphorus pentachloride.It by remaining solid adding into acetone, is separated by solid-liquid separation, solid is dried at 80 DEG C obtains phosphorus pentasulfide powder
Body.Fig. 1 is the diffraction pattern of the X-ray of its product, can only symbolize the X-ray map of lithium chloride, according to element conservation law, is produced
Centainly there is phosphorus pentasulfide in object.
Embodiment 2
Under argon atmosphere protection, 1.78g vulcanization lithium powder and 4.9g phosphorus pentachloride 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 60:1.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, by ball grinder
Middle solid product takes out and is added in toluene, is separated by solid-liquid separation, and the solution after separation is distilled to recover liquid toluene and is consolidated at 110 DEG C
Body phosphorus pentachloride.It by remaining solid adding into acetone, is separated by solid-liquid separation, solid is dried at 80 DEG C obtains phosphorus pentasulfide powder
Embodiment 3
Under argon atmosphere protection, 0.37g vulcanization lithium powder and 1.3g phosphorus pentachloride 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 20:1.In room temperature condition
Under, so that ball grinder is reacted 100h in the revolving speed continuous ball milling of 300r/min.After reaction, under an argon atmosphere, by ball grinder
Middle solid product takes out and is added in toluene, is separated by solid-liquid separation, and the solution after separation is distilled to recover liquid toluene and is consolidated at 120 DEG C
Body phosphorus pentachloride.It by remaining solid adding into acetone, is separated by solid-liquid separation, solid is dried at 80 DEG C obtains phosphorus pentasulfide powder
Body.
Embodiment 4
Under argon atmosphere protection, 0.71g vulcanization lithium powder and 1.29g phosphorus pentachloride 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 1h in the revolving speed continuous ball milling of 450r/min.It after reaction, under an argon atmosphere, will be in ball grinder
Solid product takes out and is added in toluene, is separated by solid-liquid separation, and the solution after separation is distilled to recover liquid toluene and solid at 140 DEG C
Phosphorus pentachloride.It by remaining solid adding into acetone, is separated by solid-liquid separation, solid is dried at 80 DEG C obtains phosphorus pentasulfide powder.
Claims (9)
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.
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| CN109888378A (en) * | 2019-04-17 | 2019-06-14 | 宁波容百新能源科技股份有限公司 | A kind of high ionic conductivity sulfide solid electrolyte and preparation method thereof based on liquid phase method |
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| US8067108B1 (en) * | 2007-02-14 | 2011-11-29 | Electrochem Solutions, Inc. | Hybrid battery for use over extended temperature range |
| CN101402451A (en) * | 2008-10-27 | 2009-04-08 | 昆明理工大学 | Process for producing power shaped phosphorus pentasulfide |
| CN101863461A (en) * | 2009-10-22 | 2010-10-20 | 辽宁瑞兴化工集团有限公司 | Improvement for feeding mode in preparation method for phosphorus pentasulfide |
| CN103500853A (en) * | 2013-10-08 | 2014-01-08 | 中国科学院宁波材料技术与工程研究所 | Sulfide electrolyte material and preparation method thereof |
| JP2016216307A (en) * | 2015-05-21 | 2016-12-22 | 出光興産株式会社 | Method for producing sulfide solid electrolyte |
| CN106329002A (en) * | 2016-09-30 | 2017-01-11 | 上海空间电源研究所 | Method for efficiently preparing and collecting chalcogenide solid electrolyte |
| CN107195955A (en) * | 2017-04-17 | 2017-09-22 | 哈尔滨工业大学无锡新材料研究院 | A kind of inorganic sulphide electrolyte preparation method |
| CN109786845A (en) * | 2019-01-23 | 2019-05-21 | 蜂巢能源科技有限公司 | Sulfide electrolyte slurry and its preparation method and application |
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