CN112110428A - Method for synthesizing amino lithium potassium by solid-solid reaction - Google Patents
Method for synthesizing amino lithium potassium by solid-solid reaction Download PDFInfo
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- CN112110428A CN112110428A CN202010860413.2A CN202010860413A CN112110428A CN 112110428 A CN112110428 A CN 112110428A CN 202010860413 A CN202010860413 A CN 202010860413A CN 112110428 A CN112110428 A CN 112110428A
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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
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/087—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms
- C01B21/092—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms containing also one or more metal atoms
- C01B21/0923—Metal imides or amides
- C01B21/0926—Metal imides or amides of alkali metals
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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
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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Abstract
The invention relates to the field of material synthesis, in particular to a method for synthesizing lithium amino potassium through solid-solid reaction. Aiming at the problems of less synthesis method, more complex synthesis process and high cost of the existing lithium amino potassium, the invention provides a method for synthesizing the lithium amino potassium by solid-solid reaction. The synthesis method comprises the steps of taking potassium amino lithium fluoride and lithium amide as raw materials, filling the raw materials into a ball milling tank under the protection of inert gas, vacuumizing the ball milling tank, generating potassium amino lithium and lithium fluoride after ball milling, and separating the lithium amino potassium and the lithium amino by liquid ammonia to obtain the potassium amino lithium. The invention provides a method for synthesizing lithium amino potassium, which has simple process and low cost.
Description
Technical Field
The invention belongs to the field of material synthesis, and particularly relates to a method for synthesizing lithium amino potassium through solid-solid reaction.
Background
Lithium potassium amide is one of the good raw materials of light metal hydrogen storage materials. The lithium amino potassium can effectively improve the thermodynamic and kinetic properties of dehydrogenation/hydrogenation reaction of a metal-N-H system, and can be used as a multi-element hydrogen storage material to participate in hydrogen absorption and desorption reaction, so that the hydrogen desorption rate is improved. The methods for preparing potassium lithium amide are few, and specifically, potassium lithium amide is obtained by ball milling lithium amide and potassium hydride in ammonia gas environment and then reheating the ball milled lithium amide and potassium hydride [ Kiyotaka Goshome, Ankur Jain, Hiroki Miyaoka, Hikaru Yamamoto, Yoshitsugu Kojima, and Takayuki Ichikawa2-KH Composite in MH-NH3 Hydrogen Storage System,Molecules，2019]. The above method has the disadvantages of complex reaction, high cost, etc.
The amino lithium potassium is a good hydrogen storage material, but the existing synthesis process is not comprehensive and efficient.
Disclosure of Invention
The invention aims to solve the problems and provides a simple, efficient and safe method for synthesizing the lithium amino potassium.
The invention relates to a method for preparing lithium amide potassium fluoride, which comprises the steps of generating lithium amide potassium and lithium fluoride by mechanical ball milling of lithium amide and lithium fluoride, and then separating with liquid ammonia to obtain the lithium amide potassium. The specific technical scheme is as follows:
a method for synthesizing amino lithium potassium by solid-solid reaction comprises the following steps:
(1) under inert atmosphere, adding lithium amide and potassium lithium amide fluoride into a ball milling tank according to a certain proportion, adding grinding balls according to a certain ball-to-material ratio, and then sealing the ball milling tank;
(2) after the ball milling tank is vacuumized, the ball milling tank is arranged on a ball mill and is milled for a certain time at a certain rotating speed;
(3) and (4) carrying out post-treatment on the ball-milled product to obtain the amino lithium potassium.
The inert atmosphere in the step (1) is argon, nitrogen or argon/nitrogen mixed gas.
The molar ratio of the lithium amide to the lithium amide potassium fluoride in the step (1) is 3: 1.
the ball material ratio in the step (1) is (40-100): the ball material ratio refers to the mass ratio of the grinding ball to the total mass of the lithium amide and the lithium potassium amide fluoride.
The ball milling rotating speed in the step (2) is 300-500 r/min, and the ball milling time is 24-96 h.
The post-treatment in the step (3) is as follows: transferring the ball-milled product to a liquid ammonia separator, performing solid-liquid separation, collecting liquid, converting liquid ammonia in a liquid ammonia solution into ammonia gas, and obtaining the residual solid, namely the amino lithium potassium.
The chemical reaction equation involved in the synthesis method is as follows:
LiKNH2F+3LiNH2→Li3K(NH2)4+LiF
compared with the prior art, the invention has the following beneficial effects:
(1) the method of the invention does not need high temperature and does not use hydrogen or ammonia, and has high operation safety.
(2) The method of the invention utilizes the reaction of lithium amide and potassium lithium fluoride amide to generate the potassium lithium amide, and is a high-efficiency, simple and low-cost synthesis technology.
Drawings
FIG. 1 is a Fourier infrared spectrum of the product of the reaction of example 1.
Detailed Description
The technical solution of the present invention is further described below by using specific examples, but the scope of the present invention is not limited thereto.
Example 1
Under argon atmosphere, 0.69g of lithium amide and 0.81g of potassium lithium amide fluoride are uniformly mixed and added into a ball milling tank, wherein the ratio of the total weight of the milling balls to the total weight of the materials is 60: 1, vacuumizing the ball milling tank by using a vacuum pump, and continuously ball milling the ball milling tank for 48 hours at the rotating speed of 500 r/min. And after the ball milling is finished, filling the obtained mixture of the lithium amino potassium and the lithium fluoride into a separation container, introducing ammonia gas into the container after condensation, and finally filtering out solid lithium fluoride through solid-liquid separation. Transferring to room temperature environment, and obtaining the amino lithium potassium after the liquid ammonia in the obtained product is volatilized. FIG. 1 is a Fourier infrared spectrum corresponding to a product, wherein the obtained product is lithium amino potassium.
Example 2
Under argon atmosphere, 0.92g of lithium amide and 1.08g of potassium lithium amide fluoride are uniformly mixed and added into a ball milling tank, wherein the ratio of the total weight of the milling balls to the total weight of the materials is 40: 1, vacuumizing the ball milling tank by using a vacuum pump, and continuously ball milling the ball milling tank for 60 hours at the rotating speed of 400 r/min. And after the ball milling is finished, filling the obtained mixture of the lithium amino potassium and the lithium fluoride into a separation container, introducing ammonia gas into the container after condensation, and finally filtering out solid lithium fluoride through solid-liquid separation. Transferring to room temperature environment, and obtaining the amino lithium potassium after the liquid ammonia in the obtained product is volatilized.
Example 3
Under the nitrogen atmosphere, 1.15g of lithium amide and 1.35g of potassium lithium amide fluoride are uniformly mixed and added into a ball milling tank, wherein the ratio of the total weight of a milling ball to the total weight of materials is 80: 1, vacuumizing the ball milling tank by using a vacuum pump, and continuously ball milling the ball milling tank for 24 hours at the rotating speed of 500 r/min. And after the ball milling is finished, filling the obtained mixture of the lithium amino potassium and the lithium fluoride into a separation container, introducing ammonia gas into the container after condensation, and finally filtering out solid lithium fluoride through solid-liquid separation. Transferring to room temperature environment, and obtaining the amino lithium potassium after the liquid ammonia in the obtained product is volatilized.
Example 4
Under the mixed atmosphere of argon and nitrogen, 1.38g of lithium amide and 1.62g of potassium lithium amide fluoride are uniformly mixed and added into a ball milling tank, wherein the ratio of the total weight of the milling balls to the total weight of the materials is 100: 1, vacuumizing the ball milling tank by using a vacuum pump, and continuously ball milling the ball milling tank for 96 hours at the rotating speed of 300 r/min. And after the ball milling is finished, filling the obtained mixture of the lithium amino potassium and the lithium fluoride into a separation container, introducing ammonia gas into the container after condensation, and finally filtering out solid lithium fluoride through solid-liquid separation. Transferring to room temperature environment, and obtaining the amino lithium potassium after the liquid ammonia in the obtained product is volatilized.
The above-described embodiments are merely preferred embodiments of the present invention, which is not intended to be limiting in any way, and other variations and modifications are possible without departing from the scope of the invention as set forth in the appended claims.
Claims (7)
1. A method for synthesizing amino lithium potassium by solid-solid reaction is characterized by comprising the following steps:
(1) under inert atmosphere, adding lithium amide and potassium lithium amide fluoride into a ball milling tank according to a certain proportion, adding grinding balls according to a certain ball-to-material ratio, and then sealing the ball milling tank;
(2) after the ball milling tank is vacuumized, the ball milling tank is arranged on a ball mill and is milled for a certain time at a certain rotating speed;
(3) and (4) carrying out post-treatment on the ball-milled product to obtain the amino lithium potassium.
2. The method for synthesizing lithium amino potassium according to claim 1, which comprises the following steps: the inert atmosphere in the step (1) is argon, nitrogen or argon/nitrogen mixed gas.
3. The method for synthesizing lithium amino potassium according to claim 1, which comprises the following steps: the molar ratio of the lithium amide to the lithium amide potassium fluoride in the step (1) is 3: 1.
4. the method for synthesizing lithium amino potassium according to claim 1, which comprises the following steps: the ball material ratio in the step (1) is (40-100): 1.
5. the method for synthesizing lithium amino potassium according to claim 1, which comprises the following steps: the ball milling rotating speed in the step (2) is 300-500 r/min, and the ball milling time is 24-96 h.
6. The method for synthesizing lithium amino potassium according to claim 1, which comprises the following steps: the post-treatment in the step (3) is as follows: transferring the ball-milled product to a liquid ammonia separator, performing solid-liquid separation, collecting liquid, converting liquid ammonia in a liquid ammonia solution into ammonia gas, and obtaining the residual solid, namely the amino lithium potassium.
7. The method for synthesizing lithium amino potassium according to claim 1, which comprises the following steps: the chemical reaction equation involved in the synthesis method is as follows:
LiKNH2F+3LiNH2→Li3K(NH2)4+LiF。
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5486343A (en) * | 1994-04-25 | 1996-01-23 | Fmc Corporation | Lithium amide process |
| JP2007008738A (en) * | 2005-06-28 | 2007-01-18 | Toyota Central Res & Dev Lab Inc | Composite of hydrides, hydrogen storing material, and manufacturing method thereof |
| CN102225741A (en) * | 2011-04-11 | 2011-10-26 | 复旦大学 | Preparation method of ammonia-containing composite ionic hydrogen storage material |
| CN102530871A (en) * | 2010-12-31 | 2012-07-04 | 中国科学院金属研究所 | Modified borane ammoniate hydrogen storage material and preparation method thereof |
| CN105593159A (en) * | 2013-09-30 | 2016-05-18 | 科学技术设备委员会 | A method of producing hydrogen |
| CN107188121A (en) * | 2017-06-16 | 2017-09-22 | 扬州大学 | A kind of improved LiNH2LiH composite hydrogen storage materials and the method for improving hydrogen storage property |
| CN107915203A (en) * | 2016-10-11 | 2018-04-17 | 中国科学院大连化学物理研究所 | The preparation method and complex hydride hydrogen storage material of complex hydride hydrogen storage material |
| CN107934913A (en) * | 2017-11-14 | 2018-04-20 | 桂林电子科技大学 | The preparation and its application in hydrogen storage material of a kind of composite hydrogen storage material of transition metal fluorides doping |
-
2020
- 2020-08-25 CN CN202010860413.2A patent/CN112110428A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5486343A (en) * | 1994-04-25 | 1996-01-23 | Fmc Corporation | Lithium amide process |
| JP2007008738A (en) * | 2005-06-28 | 2007-01-18 | Toyota Central Res & Dev Lab Inc | Composite of hydrides, hydrogen storing material, and manufacturing method thereof |
| CN102530871A (en) * | 2010-12-31 | 2012-07-04 | 中国科学院金属研究所 | Modified borane ammoniate hydrogen storage material and preparation method thereof |
| CN102225741A (en) * | 2011-04-11 | 2011-10-26 | 复旦大学 | Preparation method of ammonia-containing composite ionic hydrogen storage material |
| CN105593159A (en) * | 2013-09-30 | 2016-05-18 | 科学技术设备委员会 | A method of producing hydrogen |
| CN107915203A (en) * | 2016-10-11 | 2018-04-17 | 中国科学院大连化学物理研究所 | The preparation method and complex hydride hydrogen storage material of complex hydride hydrogen storage material |
| CN107188121A (en) * | 2017-06-16 | 2017-09-22 | 扬州大学 | A kind of improved LiNH2LiH composite hydrogen storage materials and the method for improving hydrogen storage property |
| CN107934913A (en) * | 2017-11-14 | 2018-04-20 | 桂林电子科技大学 | The preparation and its application in hydrogen storage material of a kind of composite hydrogen storage material of transition metal fluorides doping |
Non-Patent Citations (1)
| Title |
|---|
| LIU,YF ET AL.: "Metathesis Reaction-Induced Significant Improvement in Hydrogen Storage Properties of the KF-Added Mg(NH2)2-2LiH System", 《JOURNAL OF PHYSICAL CHEMISTRY C》 * |
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