CN110980801A - Preparation of potassium titanate (K)2Ti4O9) Method (2) - Google Patents
Preparation of potassium titanate (K)2Ti4O9) Method (2) Download PDFInfo
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- CN110980801A CN110980801A CN201911230469.3A CN201911230469A CN110980801A CN 110980801 A CN110980801 A CN 110980801A CN 201911230469 A CN201911230469 A CN 201911230469A CN 110980801 A CN110980801 A CN 110980801A
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- potassium titanate
- potassium hydroxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/005—Alkali titanates
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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Abstract
The invention discloses a method for preparing potassium titanate (K)2Ti4O9) The method comprises the following steps: s1, preparing a potassium hydroxide solution: dissolving potassium hydroxide in diethylene glycol to prepare a potassium hydroxide solution with the concentration of 2-5 mol/L; s2 preparation of potassium titanate: mixing Ti2AlN (or Ti)3AlC2) Placing the mixture into a potassium hydroxide solution, stirring the mixture at a constant speed by a stirrer, and introducing argon gas for heating to prepare potassium titanate; s3: separating and purifying potassium titanate: centrifugally washing the mixture for a period of time at a certain rotating speed by deionized water, and then taking the precipitate as a lower layer to obtain potassium titanate; the method has the advantages of low energy consumption, safety, environmental protection, simple and time-saving operation, low cost and the like, and aims to provide the method for applying the potassium titanate to the cathode material of the sodium-ion battery.
Description
Technical Field
The invention relates to a method for producingPreparation of potassium titanate (K)2Ti4O9) The method of (1).
Background
Potassium titanate is a novel inorganic material, has the characteristics of high strength, heat resistance, strong acid and alkali resistance, high infrared reflectance and the like, and can be widely used as an insulating material, a heat insulating material, a friction material, a reinforcing material, a catalyst carrier, an ion exchange material and the like. The traditional potassium titanate preparation method has the defects of high equipment requirement, complex operation, high preparation energy consumption and the like due to the fact that the traditional potassium titanate preparation method is carried out under the conditions of high temperature and high pressure, such as a solvent method, a melting method, a sintering method, a slow cooling sintering method and the like.
Disclosure of Invention
The invention aims to solve the problems and provide a method for preparing potassium titanate (K)2Ti4O9) The method has the advantages of low energy consumption, safety, environmental protection, simple and time-saving operation, low cost and the like, and aims to provide the method for applying the potassium titanate to the sodium ion negative electrode material.
In order to realize the purpose, the invention adopts the technical scheme that:
preparation of potassium titanate (K)2Ti4O9) The method comprises the following steps:
s1, preparing a potassium hydroxide solution: dissolving potassium hydroxide in diethylene glycol to prepare a potassium hydroxide solution with the concentration of 2-5 mol/L;
s2 preparation of potassium titanate: mixing Ti2AlN (or Ti)3AlC2) Placing the mixture into a potassium hydroxide solution, stirring the mixture at a constant speed by a stirrer, and introducing argon gas for heating to prepare potassium titanate;
s3: separating and purifying potassium titanate: and centrifugally washing the mixture for a period of time at a certain rotating speed by deionized water, and then taking the precipitate as a lower layer to obtain the potassium titanate.
Further, in step S2, the argon gas is introduced at a rate of 1-4L/min.
Further, in step S2, the stirring speed of the stirrer is 200-500 rpm.
Further, in step S2, the heating reaction temperature is controlled to be 200-230 ℃.
Further, in step S2, the heating reaction time is 2.5-5 h.
Further, in step S3, the speed was controlled at 3500rpm and the washing time was 5min during the centrifugation with deionized water.
The invention has the beneficial effects that:
the method selects potassium hydroxide to MAX material Ti2AlN、Ti3AlC2Etching to prepare potassium titanate (K) under normal pressure and low temperature2Ti4O9) The appearance is in a petal-sheet shape, and the layers are clear; has the advantages of low energy consumption, safety, environmental protection, simple operation, time saving, low cost and the like. Simultaneously, the method is utilized to provide potassium titanate (K)2Ti4O9) A method for applying the negative electrode material of a sodium-ion battery.
Drawings
FIG. 1 shows the invention K2Ti4O9XRD pattern of (a).
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, specific embodiments thereof are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed as broadly as the present invention is capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Referring to fig. 1, the present invention is exemplified by the following three embodiments.
Example 1.
50ml of diethylene glycol and 5.6g of potassium hydroxide are added into a three-neck flask, and the mixture is heated and stirred for 20min at 40 ℃ until the potassium hydroxide solid is completely dissolved, so that 2mol/L of the potassium hydroxide solution of diethylene glycol is obtained. Mixing 1g of Ti2AlN was added to the potassium hydroxide solution, and the reaction was stirred at 210 ℃ for 4 hours under the protection of a 2L/min argon stream, with the stirring speed controlled at 200rpm, and the liquid was prevented from excessively volatilizing by using a condenser tube. Reaction junctionAnd finally, repeatedly centrifuging and cleaning the sample solution to be neutral by using deionized water, and performing suction filtration to obtain clean powder.
Example 2.
50ml of diethylene glycol and 11.2g of potassium hydroxide are added into a three-neck flask, and the mixture is heated and stirred for 20min at 40 ℃ until the potassium hydroxide solid is completely dissolved, so that 4mol/L of the potassium hydroxide solution of diethylene glycol is obtained. Mixing 1g of Ti3AlC2Adding into potassium hydroxide solution, stirring and reacting at 200 deg.C for 5h under the protection of 4L/min argon gas flow, controlling the stirring speed at 400rpm, and preventing the liquid from excessively volatilizing by using a condenser tube. And after the reaction is finished, repeatedly centrifuging and cleaning the sample solution to be neutral by using deionized water, and performing suction filtration to obtain cleaned powder.
Example 3.
50ml of diethylene glycol and 11.2g of potassium hydroxide are added into a three-neck flask, and the mixture is heated and stirred for 20min at 40 ℃ until the potassium hydroxide solid is completely dissolved, so that 4mol/L of the potassium hydroxide solution of diethylene glycol is obtained. Mixing 1g of Ti3AlC2Adding into potassium hydroxide solution, stirring and reacting at 220 deg.C for 3h under the protection of 3L/min argon gas flow, controlling the stirring speed at 400rpm, and preventing the liquid from excessively volatilizing by using a condenser tube. And after the reaction is finished, repeatedly centrifuging and cleaning the sample solution to be neutral by using deionized water, and performing suction filtration to obtain cleaned powder.
Example 4.
50ml of diethylene glycol and 5.6g of potassium hydroxide are added into a three-neck flask, and the mixture is heated and stirred for 20min at 40 ℃ until the potassium hydroxide solid is completely dissolved, so that 2mol/L of the potassium hydroxide solution of diethylene glycol is obtained. Mixing 1g of Ti3AlC2Adding into potassium hydroxide solution, stirring at 230 deg.C under the protection of 2L/min argon gas flow for 5h, controlling stirring speed at 300rpm, and preventing liquid from excessively volatilizing by using a condenser tube. And after the reaction is finished, repeatedly centrifuging and cleaning the sample solution to be neutral by using deionized water, and performing suction filtration to obtain cleaned powder.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
The principles and embodiments of the present invention are explained herein using specific examples, which are presented only to assist in understanding the method and its core concepts of the present invention. The foregoing is only a preferred embodiment of the present invention, and it should be noted that there are objectively infinite specific structures due to the limited character expressions, and it will be apparent to those skilled in the art that a plurality of modifications, decorations or changes may be made without departing from the principle of the present invention, and the technical features described above may be combined in a suitable manner; such modifications, variations, combinations, or adaptations of the invention using its spirit and scope, as defined by the claims, may be directed to other uses and embodiments.
Claims (6)
1. Preparation of potassium titanate (K)2Ti4O9) The method is characterized by comprising the following steps:
s1, preparing a potassium hydroxide solution: dissolving potassium hydroxide in diethylene glycol to prepare a potassium hydroxide solution with the concentration of 2-5 mol/L;
s2 preparation of potassium titanate: mixing Ti2AlN (or Ti)3AlC2) Placing the mixture into a potassium hydroxide solution, stirring the mixture at a constant speed by a stirrer, and introducing argon gas for heating to prepare potassium titanate;
s3: separating and purifying potassium titanate: and centrifugally washing the mixture for a period of time at a certain rotating speed by deionized water, and then taking the precipitate as a lower layer to obtain the potassium titanate.
2. The method for preparing potassium titanate (K) according to claim 12Ti4O9) The method of (2), characterized by: in step S2, the argon gas is introduced at a rate of 1-4L/min.
3. A process for producing titanic acid according to claim 1Potassium (K)2Ti4O9) The method of (2), characterized by: in step S2, the stirring speed of the stirrer is 200-500 rpm.
4. The method for preparing potassium titanate (K) according to claim 12Ti4O9) The method of (2), characterized by: in step S2, the heating reaction temperature is controlled to be 200-230 ℃.
5. The method for preparing potassium titanate (K) according to claim 12Ti4O9) The method of (2), characterized by: in step S2, the heating reaction time is 2.5-5 h.
6. The method for preparing potassium titanate (K) according to claim 12Ti4O9) The method of (2), characterized by: in step S3, the speed was controlled at 3500rpm and the washing time was 5min during centrifugation with deionized water.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112018358A (en) * | 2020-08-17 | 2020-12-01 | 五邑大学 | Nitrogen-doped/carbon-coated potassium titanate material and preparation method thereof |
| CN112018355A (en) * | 2020-08-14 | 2020-12-01 | 五邑大学 | Preparation method of three-dimensional rod-shaped potassium titanate material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106745209A (en) * | 2016-12-24 | 2017-05-31 | 句容亿格纳米材料厂 | A kind of preparation method of potassium titanate |
| CN108658122A (en) * | 2017-03-30 | 2018-10-16 | 中国科学院大连化学物理研究所 | A kind of two-dimensional metallic carbonitride derives nano material and preparation method thereof |
-
2019
- 2019-12-05 CN CN201911230469.3A patent/CN110980801A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106745209A (en) * | 2016-12-24 | 2017-05-31 | 句容亿格纳米材料厂 | A kind of preparation method of potassium titanate |
| CN108658122A (en) * | 2017-03-30 | 2018-10-16 | 中国科学院大连化学物理研究所 | A kind of two-dimensional metallic carbonitride derives nano material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| YI LIU ET AL.: ""Conversion of Ti2AlC to C-K2Ti4O9 via a KOH assisted hydrothermal treatment and its application in lithium-ion battery anodes"", 《ELECTROCHIMICA ACTA》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112018355A (en) * | 2020-08-14 | 2020-12-01 | 五邑大学 | Preparation method of three-dimensional rod-shaped potassium titanate material |
| WO2022032749A1 (en) * | 2020-08-14 | 2022-02-17 | 五邑大学 | Method for preparing three-dimensional rod-like potassium titanate material |
| CN112018358A (en) * | 2020-08-17 | 2020-12-01 | 五邑大学 | Nitrogen-doped/carbon-coated potassium titanate material and preparation method thereof |
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