CN108529667A - Based on Ti2The method that AlC prepares different-shape titanate - Google Patents
Based on Ti2The method that AlC prepares different-shape titanate Download PDFInfo
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- CN108529667A CN108529667A CN201810427853.1A CN201810427853A CN108529667A CN 108529667 A CN108529667 A CN 108529667A CN 201810427853 A CN201810427853 A CN 201810427853A CN 108529667 A CN108529667 A CN 108529667A
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- Prior art keywords
- titanate
- alc
- shape
- lye
- different
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 17
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 13
- 239000003513 alkali Substances 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 43
- 238000001914 filtration Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims 4
- 239000010936 titanium Substances 0.000 abstract description 24
- 239000002131 composite material Substances 0.000 abstract description 4
- 229910052719 titanium Inorganic materials 0.000 abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 238000007634 remodeling Methods 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract 1
- 229910009819 Ti3C2 Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical group N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910009818 Ti3AlC2 Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000002127 nanobelt Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 229910009817 Ti3SiC2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- -1 kalium ion Chemical class 0.000 description 1
- 229910052757 nitrogen Chemical group 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Based on Ti2The method that AlC prepares different-shape titanate, by Ti2AlC powder is mixed with a certain concentration and the lye of quality, carry out hydro-thermal reaction for a period of time in a certain temperature conditions, products therefrom filters, washing, it is dry, obtain the titanate of different-shape, one side alkali can react to form titanate with titanium layer, alkali can be with Al layers of reaction conducive to the removal of Al simultaneously, to realize the remodeling of structure, ultimately form the composite material of titanate and carbon, the titanate of different-shape can be prepared, prepared titanate morphology controllable, size uniform, it is dispersed preferable, it is simple with method, morphology controllable, the characteristics of being easy to repeat.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, more particularly to a kind of to be based on Ti2AlC prepares different-shape metatitanic acid
The method of salt.
Background technology
MAX phases are a kind of three-layer laminated crystal, are typically expressed as Mn+1AXn(n=1,2,3), wherein M represents transition metal
Element, A are mainly third or the 4th major element, and X is carbon or nitrogen.Common MAX phases have Ti3AlC2、Ti2AlC。
To Ti3AlC2、Ti2AlC, which carries out Al layers of selective etch, can correspond to obtain stratiform Ti3C2、Ti2C, the stratified material of this titanium-based by
In suitable interlamellar spacing, low operating voltage and chemical stability are as the research hotspot in terms of electrochemistry, microstructure
Determine chemical property performance.Common alkalization method prepares titanate using butyl titanate, titanium tetrachloride as titanium source, in addition document 1
[Acs Nano, 2017,11 (5)] Dong etc. is based on Ti3C2By the way that H is added2O2, NaOH or KOH hydrothermal oxidizations prepare metatitanic acid
The preparation of titanate has been expanded in salt nanobelt, progress, be applied to novel sodium-ion battery and kalium ion battery show it is excellent
Different performance.Document 2 [Advanced Energy Materials, 2017,7 (18)] Zou etc. is directly by Ti3SiC2As preceding
It drives body and a kind of nucleocapsid is obtained by KOH hydro-thermal process, its chemical property is further promoted by subsequent reduction treatment.
Document 3 [Nano Energy, 2018,46:20-28.] Huang etc. be stirred at room temperature by Ti3C2-MXene convert it is anti-
It answers, is prepared for being grown in two-dimentional Ti3C2One-dimensional amorphous state Na in nanometer sheet0.23TiO2The sandwich shape Na of nanobelt0.23TiO2/
Ti3C2Composite material.The sandwich shape being made of one-dimensional ultrathin nanometer band, two-dimentional electrical-conductive nanometer piece and three-dimensional sandwich structure
Na0.23TiO2/Ti3C2Composite material exhibits go out excellent chemical property.The above technology is mostly two-step method, compared to one-step method,
Technological process is complex.
Invention content
In order to overcome the disadvantages of the above prior art, the purpose of the present invention is to provide one kind being based on Ti2AlC prepares different
The method of pattern titanate can prepare the titanate of different-shape, have simple method, morphology controllable, be easy to the spy repeated
Point.
In order to achieve the above object, the technical solution that the present invention takes is：
Based on Ti2The method that AlC prepares different-shape titanate, steps are as follows：
Grain size is less than to 48 μm of Ti2AlC powder and the lye of a concentration of 0.5~50mol/L are mixed, Ti2AlC powder
The mass ratio of end and lye is 1：(150~570) carry out hydro-thermal reaction 4~for 24 hours, gained under 120~200 DEG C of temperature conditions
Product filters, and washs, dry, obtains the titanate of different-shape.
Prepared titanate pattern is column, rodlike and sheet.
The concentration of the lye is in 42~50molL-1, Ti2The mass ratio of AlC powder and lye is 1：(504~570),
Hydro-thermal reaction 4h~for 24 hours is carried out under 120~200 DEG C of temperature conditions, products therefrom filtering is washed, dry, available column
Titanate.
The concentration of the lye is in 2~42molL-1, Ti2The mass ratio of AlC powder and lye is 1：(167~504),
Hydro-thermal reaction 4h~for 24 hours is carried out under 120~200 DEG C of temperature conditions, products therefrom filtering is washed, dry, available rodlike
Titanate.
The concentration of the lye is in 0.5~2molL-1, Ti2The mass ratio of AlC powder and lye is 1：(150~167),
Hydro-thermal reaction 4h~for 24 hours is carried out under 120~200 DEG C of temperature conditions, products therefrom filtering is washed, dry, available sheet
Titanate.
The lye is KOH or NaOH.
The present invention having the beneficial effect that compared with prior art：
The present invention uses one-step method, one side alkali that can react to form titanate with titanium layer, while alkali can be with Al layers instead
Conducive to the removal of Al the composite material of titanate and carbon should be ultimately formed to realize the remodeling of structure.The technology is based on
Ti2The ternary layered materials of AlC can prepare the titanate of different-shape, and prepared titanate morphology controllable, divides size uniform
It is preferable to dissipate property, has the characteristics that simple method, morphology controllable, be easy to repeat.
Description of the drawings
Fig. 1 (a) is that embodiment one obtains the XRD diagram of column titanate；(b) it is that embodiment one obtains column titanate
SEM schemes.
Fig. 2 (a) is that embodiment two obtains the XRD diagram of rodlike titanate；(b) it is that embodiment two obtains rodlike titanate
SEM schemes.
Fig. 3 (a) is that embodiment three obtains the XRD diagram of sheet titanate；(b) it is that embodiment three obtains sheet titanate
SEM schemes.
Specific implementation mode
The present invention is described in further details with reference to embodiment.
Embodiment one：
Grain size is less than to 48 μm of Ti2AlC powder and the KOH solution of a concentration of 40mol/L are mixed, Ti2AlC powder
Mass ratio with lye is 1：150, hydro-thermal reaction 10h is carried out under 180 DEG C of temperature conditions, products therefrom filtering is washed, done
It is dry, obtain column titanate, referring to Fig. 1 (a), illustrate to form titanate, referring to Fig. 1 (b), it is seen that column titanate it is complete
Pattern.
Embodiment two：
Grain size is less than to 48 μm of Ti2AlC powder and the KOH solution of a concentration of 16mol/L are mixed, Ti2AlC powder
Mass ratio with lye is 1：300, hydro-thermal reaction 5h is carried out under 180 DEG C of temperature conditions, products therefrom filtering is washed, dry,
Rodlike titanate is obtained, referring to Fig. 2 (a), illustrates to form titanate, referring to Fig. 2 (b), it is seen that the completeness of rodlike titanate
Looks.
Embodiment three：
Grain size is less than to 48 μm of Ti2AlC powder and the KOH solution of a concentration of 0.5mol/L are mixed, Ti2AlC powder
Mass ratio with lye is 1：500, hydro-thermal reaction 5h is carried out under 180 DEG C of temperature conditions, products therefrom filtering is washed, dry,
Sheet titanate is obtained, referring to Fig. 3 (a), illustrates to form titanate, referring to Fig. 3 (b), it is seen that the completeness of sheet titanate
Looks.
Claims (6)
1. being based on Ti2The method that AlC prepares different-shape titanate, which is characterized in that include the following steps：
Grain size is less than to 48 μm of Ti2AlC powder and the lye of a concentration of 0.5~50mol/L are mixed, Ti2AlC powder with
The mass ratio of lye is 1：(150~570) carry out hydro-thermal reaction 4~for 24 hours, products therefrom under 120~200 DEG C of temperature conditions
Filtering is washed, dry, obtains the titanate of different-shape.
2. according to claim 1 be based on Ti2The method that AlC prepares different-shape titanate, which is characterized in that prepared
Titanate pattern be column, rodlike and sheet.
3. according to claim 1 be based on Ti2The method that AlC prepares different-shape titanate, which is characterized in that the alkali
The concentration of liquid is in 42~50molL-1, Ti2The mass ratio of AlC powder and lye is 1：(504~570), in 120~200 DEG C of temperature
Hydro-thermal reaction 4h~for 24 hours is carried out under the conditions of degree, products therefrom filtering is washed, dry, available column titanate.
4. according to claim 1 be based on Ti2The method that AlC prepares different-shape titanate, which is characterized in that the alkali
The concentration of liquid is in 2~42molL-1, Ti2The mass ratio of AlC powder and lye is 1：(167~504), in 120~200 DEG C of temperature
Hydro-thermal reaction 4h~for 24 hours is carried out under the conditions of degree, products therefrom filtering is washed, dry, available rodlike titanate.
5. according to claim 1 be based on Ti2The method that AlC prepares different-shape titanate, which is characterized in that the alkali
The concentration of liquid is in 0.5~2molL-1, Ti2The mass ratio of AlC powder and lye is 1：(150~167), in 120~200 DEG C of temperature
Hydro-thermal reaction 4h~for 24 hours is carried out under the conditions of degree, products therefrom filtering is washed, dry, available sheet titanate.
6. according to claim 1 be based on Ti2The method that AlC prepares different-shape titanate, which is characterized in that the alkali
Liquid is KOH or NaOH.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810427853.1A CN108529667B (en) | 2018-05-07 | 2018-05-07 | Based on Ti2Method for preparing titanates with different shapes from AlC |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810427853.1A CN108529667B (en) | 2018-05-07 | 2018-05-07 | Based on Ti2Method for preparing titanates with different shapes from AlC |
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| CN108529667A true CN108529667A (en) | 2018-09-14 |
| CN108529667B CN108529667B (en) | 2020-04-28 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0522894A1 (en) * | 1991-07-03 | 1993-01-13 | Rhone-Poulenc Chimie | Alkaline-earth and/or rare earth titanates based composition and preparation thereof |
| CN102390864A (en) * | 2011-08-18 | 2012-03-28 | 中南大学 | Preparation method of flaky potassium hexatitanate |
| CN103296267A (en) * | 2013-06-06 | 2013-09-11 | 吉林大学 | Preparation method of flake lithium titanate |
-
2018
- 2018-05-07 CN CN201810427853.1A patent/CN108529667B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0522894A1 (en) * | 1991-07-03 | 1993-01-13 | Rhone-Poulenc Chimie | Alkaline-earth and/or rare earth titanates based composition and preparation thereof |
| CN102390864A (en) * | 2011-08-18 | 2012-03-28 | 中南大学 | Preparation method of flaky potassium hexatitanate |
| CN103296267A (en) * | 2013-06-06 | 2013-09-11 | 吉林大学 | Preparation method of flake lithium titanate |
Non-Patent Citations (1)
| Title |
|---|
| GUODONG ZOU ET AL.: ""Hydrogenated Core–Shell MAX@K2Ti8O17 Pseudocapacitance with Ultrafast Sodium Storage and Long-Term Cycling"", 《ADV. ENERGY MATER.》 * |
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| CN108529667B (en) | 2020-04-28 |
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Effective date of registration: 20231127 Address after: Room B32, 6th Floor, Commercial Complex Building, Yinhu Entrepreneurship Street, Wanli Street, Jiujiang District, Wuhu City, Anhui Province, 241000 Patentee after: Wuhu Huirui Information Technology Co.,Ltd. Address before: 710021 Shaanxi province Xi'an Weiyang university campus of Shaanxi University of Science and Technology Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY |