CN107381628B - One kind platy particles of layered potassium titanate containing zinc and its hydrothermal preparing process - Google Patents
One kind platy particles of layered potassium titanate containing zinc and its hydrothermal preparing process Download PDFInfo
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- CN107381628B CN107381628B CN201710744719.XA CN201710744719A CN107381628B CN 107381628 B CN107381628 B CN 107381628B CN 201710744719 A CN201710744719 A CN 201710744719A CN 107381628 B CN107381628 B CN 107381628B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
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- C01G23/005—Alkali titanates
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- 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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- 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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- 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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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/51—Particles with a specific particle size distribution
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- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
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Abstract
The invention discloses a kind of platy particles of layered potassium titanate containing zinc and preparation method thereof, belong to field of material preparation.By TiO2With Zn (NO3)2·6H2O is added in KOH aqueous solution, and stirring is uniformly mixed raw material, is carried out hydro-thermal reaction and is filtered, washed, is dried after reaction, obtains the platy particles of layered potassium titanate containing zinc.The composition expression formula of the platy particles is K0.8Zn0.4Ti1.6O4, the length is 1~2 μm, with a thickness of 100~200nm.Compared to conventional solid-state method and molten-salt growth method, the stratiform K of the technology of the present invention preparation0.8Zn0.4Ti1.6O4Platy particles partial size is small, with high purity, pattern and microstructure are controllable, and its preparation process is simple, and low energy consumption, and repeatability is high, is conducive to industrialized production.
Description
Technical field
The invention belongs to field of material preparation, and in particular to one kind platy particles of layered potassium titanate containing zinc and its hydro-thermal preparation
Method.
Background technique
Layered titanate is a kind of typical lamellar compound, and there is good photocatalytic, electrochemistry and ion to hand over
It is transsexual can be equal, and can by the way that doping, interlayer be pillared etc. that modifications means carry out the design of molecular level to it, cuts out and assembles,
The photocatalytic activity and chemical property of material are improved, there is important potential using value.
Layered titanate is as battery active material and catalysis material, and performance is largely by its microcosmic shape
Looks, partial size and specific surface area are determined.Currently, (the K of layered potassium titanate containing zinc0.8Zn0.4Ti1.6O4) preparation method be mainly
Solid phase method and molten-salt growth method.Fujimoto K et al. [Journal of Ion Exchange, 2014,25 (1): 12-15] passes through solid
Phase reaction method, by K2CO3, TiO2It is uniformly mixed with ZnO with certain molar ratio, reacts 16h under 1000 DEG C~1050 DEG C high temperature
Prepare the K of stratiform0.8Zn0.4Ti1.6O4；The K for the stratiform that this method is prepared0.8Zn0.4Ti1.6O4The big, partial size point with partial size
Cloth wide (length is about 5~50 μm, with a thickness of 2~5 μm) and purity is low.In addition, all there is complex process, energy consumption in these methods
High, the disadvantages of reaction time is long, it is unfavorable for industrialized production.
Summary of the invention
In order to overcome the problems of the above-mentioned prior art, the purpose of the present invention is to provide a kind of layered potassium titanates containing zinc
Platy particles and its hydrothermal preparing process, this method reaction condition is mild, easy to operate, and repeatability is high, by containing for party's legal system
The partial size of zinc layered potassium titanate particle is small, with high purity, pattern and microstructure are controllable.
To achieve the goals above, the present invention uses following technical scheme.
The invention discloses a kind of hydrothermal preparing process of platy particles of layered potassium titanate containing zinc, by TiO2And Zn
(NO3)2·6H2O is added to KOH
In aqueous solution, stirring is uniformly mixed raw material, carries out hydro-thermal reaction and is filtered, washed, is dried after reaction,
Obtain the platy particles of layered potassium titanate containing zinc.
Preferably, the TiO2、Zn(NO3)2·6H2The amount ratio of O and KOH aqueous solution is 5g:5.35g:(15~100)
mL。
Preferably, the concentration of the KOH aqueous solution is 3~10mol/L.
Preferably, the hydrothermal temperature is 150~300 DEG C.
Preferably, the hydro-thermal reaction time be 4~for 24 hours.
Preferably, to be washed with water, drying is carried out at 50~80 DEG C for the washing.
The invention also discloses using the platy particles of layered potassium titanate containing zinc made from above-mentioned hydrothermal preparing process, this contains
The composition expression formula of zinc layered potassium titanate platy particles is K0.8Zn0.4Ti1.6O4。
Preferably, which is 1~2 μm, with a thickness of 100~200nm.
Compared with prior art, the invention has the characteristics that:
The hydrothermal preparing process of the platy particles of layered potassium titanate containing zinc disclosed by the invention, with TiO2As titanium source, Zn
(NO3)2·6H2O is sufficiently mixed as zinc source, and with certain density KOH aqueous solution, then carries out hydrothermal crystallization reaction, is made and is contained
The K of zinc layer structure0.8Zn0.4Ti1.6O4Platy particles compare conventional solid-state method and molten-salt growth method, and preparation process of the present invention is simple,
Low energy consumption, and repeatability is high, is conducive to industrialized production.
Further, hydro-thermal reaction of the invention is carried out at 150~300 DEG C, and treatment temperature is very low, compared to existing
Technology needs react 16h under 1000 DEG C~1050 DEG C high temperature, hence it is evident that have low energy consumption, low for equipment requirements, safety is good, ring
The advantage of border close friend.
Through the platy particles of layered potassium titanate containing zinc produced by the present invention, partial size is small and narrowly distributing (length is about 1~2 μm, thick
Degree is 100~200nm), purity is high, pattern and microstructure are controllable.
Detailed description of the invention
Fig. 1 is the XRD spectrum of the particle of layered potassium titanate containing zinc prepared by the present invention；
Fig. 2 is the SEM photograph of the particle of layered potassium titanate containing zinc prepared by the present invention.
Specific embodiment
With reference to the accompanying drawing and specific embodiment the invention will be described in further detail:
Embodiment 1
By 5g TiO2With 5.35g Zn (NO3)2·6H2O is added in the KOH aqueous solution that 15mL concentration is 3mol/L, is stirred
Mixing is uniformly mixed raw material, in 150 DEG C of progress hydro-thermal reaction 4h, after reaction, is filtered, is washed with water, is dry at 50 DEG C,
Obtain the K of layered potassium titanate containing zinc0.8Zn0.4Ti1.6O4Platy particles, length is about 1~2 μm, with a thickness of 100~200nm.
Embodiment 2
By 5g TiO2With 5.35g Zn (NO3)2·6H2O is added in the KOH aqueous solution that 20mL concentration is 6mol/L, is stirred
Mixing is uniformly mixed raw material, in 180 DEG C of progress hydro-thermal reaction 8h, after reaction, is filtered, is washed with water, is dry at 60 DEG C,
Obtain the K of layered potassium titanate containing zinc0.8Zn0.4Ti1.6O4Platy particles, length is about 1~2 μm, with a thickness of 100~200nm.
Embodiment 3
By 5g TiO2With 5.35g Zn (NO3)2·6H2O is added in the KOH aqueous solution that 15mL concentration is 10mol/L, is stirred
Mixing is uniformly mixed raw material, in 250 DEG C of progress hydro-thermal reaction 12h, after reaction, is filtered, is washed with water, done at 55 DEG C
It is dry, obtain the K of layered potassium titanate containing zinc0.8Zn0.4Ti1.6O4Platy particles, length is about 1~2 μm, with a thickness of 100~200nm.
Embodiment 4
By 5g TiO2With 5.35g Zn (NO3)2·6H2O is added in the KOH aqueous solution that 50mL concentration is 10mol/L, is stirred
Mixing is uniformly mixed raw material, in 280 DEG C of progress hydro-thermal reaction 12h, after reaction, is filtered, is washed with water, done at 80 DEG C
It is dry, obtain the K of layered potassium titanate containing zinc0.8Zn0.4Ti1.6O4Platy particles, length is about 1~2 μm, with a thickness of 100~200nm.
Embodiment 5
By 5g TiO2With 5.35g Zn (NO3)2·6H2O is added in the KOH aqueous solution that 50mL concentration is 10mol/L, is stirred
Mixing is uniformly mixed raw material, 300 DEG C of progresss hydro-thermal reactions for 24 hours, after reaction, filtered, be washed with water, is dry at 70 DEG C
It is dry, obtain the K of layered potassium titanate containing zinc0.8Zn0.4Ti1.6O4Platy particles, length is about 1~2 μm, with a thickness of 100~200nm.
Embodiment 6
By 5g TiO2With 5.35g Zn (NO3)2·6H2O is added in the KOH aqueous solution that 70mL concentration is 6mol/L, is stirred
Mixing is uniformly mixed raw material, in 300 DEG C of progress hydro-thermal reaction 4h, after reaction, is filtered, is washed with water, is dry at 65 DEG C,
Obtain the K of layered potassium titanate containing zinc0.8Zn0.4Ti1.6O4Platy particles, length is about 1~2 μm, with a thickness of 100~200nm.
Embodiment 7
By 5g TiO2With 5.35g Zn (NO3)2·6H2O is added in the KOH aqueous solution that 25mL concentration is 3mol/L, is stirred
Mixing is uniformly mixed raw material, 150 DEG C of progresss hydro-thermal reactions for 24 hours, after reaction, filtered, be washed with water, is dry at 70 DEG C
It is dry, obtain the K of layered potassium titanate containing zinc0.8Zn0.4Ti1.6O4Platy particles, length is about 1~2 μm, with a thickness of 100~200nm.
Embodiment 8
By 5g TiO2With 5.35g Zn (NO3)2·6H2O is added in the KOH aqueous solution that 60mL concentration is 5mol/L, is stirred
Mixing is uniformly mixed raw material, in 200 DEG C of progress hydro-thermal reaction 12h, after reaction, is filtered, is washed with water, done at 80 DEG C
It is dry, obtain the K of layered potassium titanate containing zinc0.8Zn0.4Ti1.6O4Platy particles, length is about 1~2 μm, with a thickness of 100~200nm.
Table 1 is the chemical group for analyzing to obtain present invention preparation cobalt containing layer shape potassium titanate platy particles by X-ray fluorescence spectra
At, it can be seen that the chemical composition that the present invention prepares cobalt containing layer shape potassium titanate platy particles is K0.8Zn0.4Ti1.6O4。
Table 1 is that the element of the particle of layered potassium titanate containing zinc prepared by the present invention forms
| Composition | K2O | ZnO | TiO2 |
| Molar percentage (%) | 17.24 | 16.12 | 66.64 |
It is by the K of layered potassium titanate containing zinc prepared by the present invention referring to Fig. 10.8Zn0.4Ti1.6O4The XRD spectrum of platy particles.
As seen from the figure, the K of layered potassium titanate containing zinc obtained by the present invention0.8Zn0.4Ti1.6O4Platy particles are 10 degree attached in 2theta
Closely show layered titanate characteristic diffraction peak.It referring to fig. 2, is by layered potassium titanate containing zinc prepared by the present invention
K0.8Zn0.4Ti1.6O4The SEM photograph of platy particles.It can be clearly seen that from figure: the layered titanic acid containing zinc that the present invention obtains
Potassium K0.8Zn0.4Ti1.6O4Platy particles pattern be plate, length be about 1~2 μm, with a thickness of 100~200nm.
Claims (3)
1. a kind of hydrothermal preparing process of the platy particles of layered potassium titanate containing zinc, which is characterized in that by TiO2With Zn (NO3)2·
6H2O is added in KOH aqueous solution, and stirring is uniformly mixed raw material, carries out hydro-thermal reaction, after reaction, be filtered, washed,
It is dry, obtain the platy particles of layered potassium titanate containing zinc；
The length of the platy particles of layered potassium titanate containing zinc is 1~2 μm, with a thickness of 100~200nm；
The TiO2、Zn(NO3)2·6H2The amount ratio of O and KOH aqueous solution is 5g:5.35g:(15~100) mL；The KOH
The concentration of aqueous solution is 3~10mol/L；
The hydrothermal temperature be 150~300 DEG C, the hydro-thermal reaction time be 4~for 24 hours.
2. the hydrothermal preparing process of the platy particles of layered potassium titanate containing zinc according to claim 1, it is characterised in that: described
To be washed with water, drying is carried out at 50~80 DEG C for washing.
3. being existed using the platy particles of layered potassium titanate containing zinc, feature made from hydrothermal preparing process of any of claims 1 or 2
In: the composition expression formula for containing zinc layered potassium titanate platy particles is K0.8Zn0.4Ti1.6O4。
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6677041B1 (en) * | 1999-03-16 | 2004-01-13 | Otsuka Chemical Co., Ltd. | Platy potassium titanate, process for producing the same, and friction material |
| CN1910239A (en) * | 2004-01-16 | 2007-02-07 | 大塚化学株式会社 | Flame-retardant and flame-retardant resin composition |
| CN101248008A (en) * | 2005-08-25 | 2008-08-20 | 大塚化学株式会社 | Flaky titanic acid having polymerizable functional groups, suspension of the same, and coating films made therefrom |
| CN101619494A (en) * | 2009-08-03 | 2010-01-06 | 浙江大学 | Method for preparing perovskite structure lead titanate monocrystal nano rod |
| CN101962808A (en) * | 2010-06-17 | 2011-02-02 | 马玉馨 | High-efficiency and energy-saving potassium titanate whisker preparation method |
| CN103073054A (en) * | 2013-02-04 | 2013-05-01 | 河北工业大学 | Preparing method of nano band potassium titanate (K2Ti6O13) |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3062497B1 (en) * | 1999-06-04 | 2000-07-10 | 大塚化学株式会社 | Method for producing flaky titanate |
| JP4091337B2 (en) * | 2002-05-16 | 2008-05-28 | 大塚化学ホールディングス株式会社 | Method for producing magnesium potassium titanate and lithium potassium titanate |
-
2017
- 2017-08-25 CN CN201710744719.XA patent/CN107381628B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6677041B1 (en) * | 1999-03-16 | 2004-01-13 | Otsuka Chemical Co., Ltd. | Platy potassium titanate, process for producing the same, and friction material |
| CN1910239A (en) * | 2004-01-16 | 2007-02-07 | 大塚化学株式会社 | Flame-retardant and flame-retardant resin composition |
| CN101248008A (en) * | 2005-08-25 | 2008-08-20 | 大塚化学株式会社 | Flaky titanic acid having polymerizable functional groups, suspension of the same, and coating films made therefrom |
| CN101619494A (en) * | 2009-08-03 | 2010-01-06 | 浙江大学 | Method for preparing perovskite structure lead titanate monocrystal nano rod |
| CN101962808A (en) * | 2010-06-17 | 2011-02-02 | 马玉馨 | High-efficiency and energy-saving potassium titanate whisker preparation method |
| CN103073054A (en) * | 2013-02-04 | 2013-05-01 | 河北工业大学 | Preparing method of nano band potassium titanate (K2Ti6O13) |
Non-Patent Citations (3)
| Title |
|---|
| Ion-exchange property of lepidocrocite-type K0.8Zn0.4Ti1.6O4 using NH4NO3 molten salt;Kenjiro FUJIMOTO et al.;《J.Ion.Exch》;20141231;第25卷(第1期);第12-15页 |
| 水热合成钛酸钾一维纳米材料的微结构表征及其催化性能研究;刘慧;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20120515(第05期);摘要，第11页 |
| 钛酸钾材料的制备及其性能;刘玉民等;《化工进展》;20081231;第27卷(第12期);第1982-1985页 |
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