CN114573019A - Method for preparing sodium titanate - Google Patents
Method for preparing sodium titanate Download PDFInfo
- Publication number
- CN114573019A CN114573019A CN202210237513.9A CN202210237513A CN114573019A CN 114573019 A CN114573019 A CN 114573019A CN 202210237513 A CN202210237513 A CN 202210237513A CN 114573019 A CN114573019 A CN 114573019A
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- CN
- China
- Prior art keywords
- sodium titanate
- sodium
- titanium dioxide
- sodium fluoride
- certain
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- GROMGGTZECPEKN-UHFFFAOYSA-N sodium metatitanate Chemical compound [Na+].[Na+].[O-][Ti](=O)O[Ti](=O)O[Ti]([O-])=O GROMGGTZECPEKN-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims abstract description 36
- 239000011775 sodium fluoride Substances 0.000 claims abstract description 18
- 235000013024 sodium fluoride Nutrition 0.000 claims abstract description 18
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000011812 mixed powder Substances 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000012312 sodium hydride Substances 0.000 description 1
- 229910000104 sodium hydride Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
Images
Classifications
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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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a method for preparing sodium titanate. Titanium dioxide and sodium fluoride are taken as raw materials; adding a certain amount of sodium fluoride to titanium dioxide; heating the mixed powder to a proper temperature for a period of time in a certain atmosphere to obtain the sodium titanate. The invention has simple raw materials, simple process and low cost.
Description
Technical Field
The invention provides a method for preparing sodium titanate, belonging to the field of material synthesis.
Background
The sodium titanate has the characteristic of zero tension in the process of embedding or removing sodium ions, so that the charge-discharge cycle of the sodium ion battery can reach thousands of times, and the service life of the battery is greatly prolonged.
Sodium sources currently used for the preparation of sodium titanate from titanium dioxide as a titanium source are mainly sodium carbonate (CN 108516580A, CN107903054, DOI: 10.3969/j. issn.1674-3644.2020.03.003), sodium hydroxide (CN 109148876A, CN111370662A, CN 103232063A) and sodium hydride (CN 106315668A). However, the process using sodium fluoride as a sodium source is not reported.
Therefore, the process for preparing the sodium titanate by directly reacting the titanium dioxide with the sodium fluoride has the novelty of the reaction principle and has important significance for preparing the sodium titanate product.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for preparing sodium titanate. The invention is realized by the following technical scheme.
A method for preparing sodium titanate comprises the following specific steps:
titanium dioxide and sodium fluoride are taken as raw materials; adding a certain proportion of sodium fluoride into titanium dioxide; heating the mixed powder to a proper temperature for a period of time in a certain atmosphere to obtain the sodium titanate.
The titanium dioxide is powder or block with purity of more than 10% and particle size of more than 1 nm.
The sodium fluoride is powder or block with purity of more than 10%.
The certain proportion refers to the mass ratio of the sodium fluoride to the titanium dioxide, and the range is 0.1: 10-3: 1.
The certain atmosphere is an atmosphere containing oxygen or hydrogen or nitrogen or argon or ethanol or methanol.
The proper temperature is 600-1300 ℃.
The certain time is 1-300 min.
The invention has the beneficial effects that: simple raw materials, simple process and low cost.
Drawings
FIG. 1 is an XRD pattern of sodium titanate obtained in example 1.
FIG. 2 is an SEM photograph of sodium titanate obtained in example 1.
Detailed Description
The present invention will be further described with reference to the following embodiments.
Example 1
The method for preparing the sodium titanate comprises the following steps:
titanium dioxide powder with the purity of 99.9 percent and the diameter of about 20 nm and sodium fluoride with the purity of 99.9 percent are taken as raw materials; adding 0.03 time of sodium fluoride into titanium dioxide powder; heating the mixed powder to 700 ℃ in the air, and preserving the heat for 60 min to obtain the sodium titanate. XRD and SEM of the obtained sodium titanate are shown in figure 1 and figure 2 respectively.
Example 2
The method for preparing the sodium titanate comprises the following steps:
titanium dioxide powder with the purity of 80 percent and the diameter of about 2 mu m and sodium fluoride with the purity of 50 percent are taken as raw materials; adding 0.2 times of sodium fluoride by mass into titanium dioxide powder; heating the mixed powder to 800 ℃ in nitrogen, and preserving the heat for 150 min to prepare the sodium titanate.
Example 3
The method for preparing the sodium titanate comprises the following steps:
titanium dioxide powder with the purity of 30 percent and the diameter of about 50 mu m and sodium fluoride with the purity of 10 percent are taken as raw materials; adding 2.0 times of sodium fluoride into titanium dioxide powder; heating the mixed powder to 1000 ℃ in the atmosphere containing ethanol, and preserving the temperature for 10 min to prepare the sodium titanate.
Claims (7)
1. A method for preparing sodium titanate, characterized in that:
the preparation method takes titanium dioxide and sodium fluoride as raw materials; adding a certain proportion of sodium fluoride into titanium dioxide; and heating the mixed powder to a proper temperature for a period of time in a certain atmosphere to obtain the sodium titanate.
2. The method for producing sodium titanate according to claim 1, characterized in that: the titanium dioxide is powder or block with purity of more than 10% and particle size of more than 1 nm.
3. The method for producing sodium titanate according to claim 1, characterized in that: the sodium fluoride is powder or block with purity of more than 10%.
4. The method for producing sodium titanate according to claim 1, characterized in that: the certain proportion refers to the mass ratio of the sodium fluoride to the titanium dioxide, and the range is 0.1: 10-3: 1.
5. The method for producing sodium titanate according to claim 1, characterized in that: the certain atmosphere is an atmosphere containing oxygen or hydrogen or nitrogen or argon or ethanol or methanol.
6. The method for producing sodium titanate according to claim 1, characterized in that: the proper temperature is 600-1300 ℃.
7. The method for producing sodium titanate according to claim 1, characterized in that: the certain time is 1-300 min.
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CN202210237513.9A CN114573019A (en) | 2022-03-11 | 2022-03-11 | Method for preparing sodium titanate |
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CN202210237513.9A CN114573019A (en) | 2022-03-11 | 2022-03-11 | Method for preparing sodium titanate |
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CN202210237513.9A Pending CN114573019A (en) | 2022-03-11 | 2022-03-11 | Method for preparing sodium titanate |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4609694A (en) * | 1983-11-21 | 1986-09-02 | Otsuka Chemical Co., Ltd. | Process for preparing metamorphosed alkaline titanates |
CN101275276A (en) * | 2007-12-25 | 2008-10-01 | 山东大学 | Preparation for sodium titanate crystal whisker |
CN105870437A (en) * | 2016-05-10 | 2016-08-17 | 北京泰和九思科技有限公司 | Shape-controllable nano lithium titanate composite and preparation method thereof and lithium ion battery |
CN106374085A (en) * | 2015-07-20 | 2017-02-01 | 马鞍山首拓新能源科技有限公司 | Lithium ion battery material preparation method |
-
2022
- 2022-03-11 CN CN202210237513.9A patent/CN114573019A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4609694A (en) * | 1983-11-21 | 1986-09-02 | Otsuka Chemical Co., Ltd. | Process for preparing metamorphosed alkaline titanates |
CN101275276A (en) * | 2007-12-25 | 2008-10-01 | 山东大学 | Preparation for sodium titanate crystal whisker |
CN106374085A (en) * | 2015-07-20 | 2017-02-01 | 马鞍山首拓新能源科技有限公司 | Lithium ion battery material preparation method |
CN105870437A (en) * | 2016-05-10 | 2016-08-17 | 北京泰和九思科技有限公司 | Shape-controllable nano lithium titanate composite and preparation method thereof and lithium ion battery |
Non-Patent Citations (1)
Title |
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杨全红等: "《石墨烯电化学储能技术》", vol. 1, 华东理工大学出版社, pages: 171 * |
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Inventor after: Ye Qianxu Inventor after: Jing Yuhan Inventor after: Cai Jinming Inventor after: Zhang Mingqian Inventor after: Li Ting Inventor before: Jing Yuhan Inventor before: Ye Qianxu Inventor before: Cai Jinming Inventor before: Zhang Mingqian Inventor before: Li Ting |