CN1458068A - Trigonal structure potassium titanate and its preparing method - Google Patents
Trigonal structure potassium titanate and its preparing method Download PDFInfo
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- CN1458068A CN1458068A CN 03129114 CN03129114A CN1458068A CN 1458068 A CN1458068 A CN 1458068A CN 03129114 CN03129114 CN 03129114 CN 03129114 A CN03129114 A CN 03129114A CN 1458068 A CN1458068 A CN 1458068A
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- potassium titanate
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Abstract
The present invention provides trigonal structure potassium titanate and its preparation process, and belongs to the field of new type of inorganic functional material. The trigonal structure potassium titanate has the molecule expression of KTiO2(OH), with space group of R-3c. During the preparation, single metal titanium or its compound and potassium hydroxide as material and deionized water are filled in reactor in the filling rate of 50-85 % and made to produce hydrothermal reaction at 100-200 deg.c for 2-48 hr. The solution of single metal titanium or its compound has concentration of 0.4-3 mol/L and KOH solution has concentration of 10-40 mol/L. The produced trigonal structure potassium titanate may be used as functional ceramic crystal see, ferroelectric ceramic, cationic adsorbent, exchange material, catalyst carrier, etc.
Description
Technical field
The present invention relates to a kind of trigonal crystal structure potassium titanate and preparation method thereof, belong to the novel inorganic field of functional materials.
Background technology
Potassium titanate crystal whisker is a kind of inorganic short fiber material, uses K usually
2OnTiO
2(n=1,2,4,6,8) represent its composition.
At TiO
2-K
2In the O system, present ubiquity two potassium titanates, potassium tetratitanate and three kinds of stable crystal states of six potassium titanates, they are monoclinic crystal and spacer identical (C2/m).K
2Ti
2O
5The crystalline structure of whisker can be used TiO
5Triangle two cones represent that the triangle cone has been interconnected to form a kind of laminate structure, potassium ion occupy interlayer, and parallel with fibre axis.K
2Ti
4O
9The crystalline structure of whisker is TiO
6The laminate structure that is connected to form is shared at octahedra rib and angle, and potassium ion occupy interlayer.K
2Ti
6O
13Crystalline structure be TiO
6The tunnel structure of octahedra chain formation, potassium ion is fixed among the tunnel, and fibre axis is parallel with the tunnel axle.
And up to the present, also do not report trigonal crystal structure potassium titanate compound both at home and abroad.
Summary of the invention
The present invention has prepared the potassium titanate compound of this new texture by regulating hydrothermal synthesizing condition and processing parameter with hydrothermal reaction at low temperature.
The molecular formula of this compound is KTiO
2(OH), spacer is R-3c (No.167).The a of this compound and c are respectively 9.8934 and 28.686 .Its crystal characteristics can reduce 3 points: (1) each Ti and six O form TiO
6Octahedron is because wherein two O and H cause TiO in conjunction with making the corresponding Ti-O of institute strong than other length
6The octahedra deformity that produces; (2) adjacent six TiO
6The octahedra tunnel channel architecture that forms hexagonal columnar along the c direction with open architecture; (3) the potassium titanate crystal bar is grown along the c direction.
Described potassium titanate compound is to reach by the following technical solutions:
With single metal titanium compound (titanium dioxide or metatitanic acid four fourth fat etc.) or metal titanium and KOH is starting material, pack into and be with in the teflon-lined reactor, adding deionized water again makes the reaction vessel compactedness be controlled at 50～85% of reactor volume, this moment, the concentration range of single metal titanium compound was 0.4mol/L～3mol/L, the concentration range 10mol/L of KOH～40 mol/L.Reactor is put into baking oven, in 100～200 ℃ temperature range, be incubated 2～48hrs, 2～5 ℃/min of heat-up rate, furnace cooling.Carrying out solid-liquid separation subsequently, with reaction product ultra-sonic dispersion 30min., is 7 with washed with de-ionized water until the pH value, uses the dehydrated alcohol dispersion treatment again, carries out drying treatment 4hrs then under 80～100 ℃ of temperature, obtains KTiO
2(OH) powder.
Potassium titanate (the KTiO that the present invention prepares
2(OH)) the brilliant length of rod is 7～50 μ m, particle diameter 3～10 μ m, and along with the increase of compactedness and soaking time, the diameter chap that rod is brilliant, length increases; Wherein, work as KOH=10mol/L, TiO
2=1mol/L, 200 ℃ of reaction 6hrs can obtain the potassium titanate nanofiber of particle diameter 20～50nm and length-to-diameter ratio 10～120.
By to the researching and analysing of its structure and pattern, this novel potassium titanate is with a wide range of applications.
From microscopic appearance, the hexagonal columnar pattern of rule is one of preferred material as the function ceramics crystal seed, can be used to prepare the texturing pottery of bismuth potassium titanate system;
The OH group causes TiO in the structure
6Octahedra distortion makes that positive and negative charge does not overlap in the crystalline structure, and this may cause the phenomenon of spontaneous polarization, and promptly this novel potassium titanate might have ferroelectric properties:
Consider that from crystalline structure this potassium titanate has and K
2Ti
4O
9And K
0.8Ti
1.73Li
0.27O
4Similar open architecture, the K in the tunnel of this open architecture
+Ion can with other positively charged ion or H
+Ion exchanges, and has high chemically reactive, can be used as cation-adsorption, exchange material and support of the catalyst etc.
Hydrothermal preparing process used in the present invention can reduce the powder synthesis temperature greatly, and technology is simple, has avoided introducing because of powder reuniting and the impurity calcined and ball milling causes, and the size of crystal grain, component and form can obtain regulation and control.
Description of drawings
Fig. 1 is potassium titanate KTiO after the hydro-thermal reaction
2(OH) XRD figure spectrum.
Fig. 2, Fig. 3 are potassium titanate KTiO after the hydro-thermal reaction
2(OH) the brilliant SEM photo of rod.
Fig. 4 is potassium titanate KTiO after the hydro-thermal reaction
2(OH) the TEM photo of nanofiber.Hydrothermal condition is that temperature of reaction is 200 ℃, soaking time 6hrs, and compactedness is that 80% Fig. 5, Fig. 6 are the potassium titanate crystalline structure (spacer is R-3c) that belongs to trigonal system, and Fig. 5 is for being parallel to the c direction of principal axis, and Fig. 6 is perpendicular to the c direction of principal axis.
Embodiment
Further specify substantive distinguishing features of the present invention and marked improvement below in conjunction with embodiment.Be noted that the present invention is not limited to following each embodiment.
Embodiment 1:
1. preparation of raw material: anatase octahedrite TiO
2, KOH and deionized water be analytical pure.With 1.146gTiO
2With the 27.374gKOH uniform mixing, add deionized water simultaneously, making its volume is 29ml; 2. feed: the raw material that mixes is packed into, and band gathers tetrem alkene liner, volume is in the stainless reactor of 50ml, tightens sealing; 3. hydro-thermal reaction: reactor is put into programme controlled baking oven, 160 ℃ of hydro-thermal reaction 12hrs, 3 ℃/min. of heat-up rate, furnace cooling; 4. product is handled: ultra-sonic dispersion 30min., and washed with de-ionized water 10 times, dehydrated alcohol disperses, 80 ℃ of oven dry 24hrs..
The brilliant about 10 μ m of diameter of the above-mentioned potassium titanate rod that obtains, the about 50 μ m of length, length-to-diameter ratio is about 5, and size distribution is even, sees Fig. 2.
Embodiment 2:
1. preparation of raw material: metal Ti powder, KOH and deionized water are analytical pure.With 1.305g Ti powder and 85.428g KOH and the abundant mixing of deionized water, total water content is 33.4% (wt%); 2. feed: the raw material that mixes is packed into, and band gathers tetrem alkene liner, volume is in the stainless reactor of 120ml, tightens sealing; 3. hydro-thermal reaction: reactor is put into programme controlled baking oven, 200 ℃ of hydro-thermal reaction 48hrs, 3 ℃/min of heat-up rate, furnace cooling; 4. product is handled: ultra-sonic dispersion 30min, and washed with de-ionized water is to pH=7, and dehydrated alcohol disperses, 80 ℃ of drying treatment 24hrs in baking oven.
Embodiment 3:
1. preparation of raw material: TiO
2, KOH and deionized water be analytical pure.With 1.837g TiO
2With 12.904g KOH uniform mixing, add proper amount of deionized water simultaneously, making its volume is 23ml; 2. feed: the raw material that mixes is packed into, and band gathers tetrem alkene liner, volume is in the stainless reactor of 30ml, tightens sealing; 3. hydro-thermal reaction: reactor is put into programme controlled baking oven, 200 ℃ of hydro-thermal reaction 6hrs, 3 ℃/min of heat-up rate, furnace cooling; 4. product is handled: ultra-sonic dispersion 30min, and washed with de-ionized water 10 times, dehydrated alcohol disperses, 80 ℃ of oven dry 24hrs.
About 20～the 50nm of mean diameter of the above-mentioned potassium titanate nanofiber that obtains, length-to-diameter ratio 10～120 is seen Fig. 3.
Claims (5)
1, a kind of trigonal crystal structure potassium titanate, its molecular formula is KTiO
2(OH), spacer is R-3c.
2, the method for the synthetic trigonal crystal structure potassium titanate of a kind of hydro-thermal comprises batching, mixing, hydro-thermal reaction, solid-liquid separation, cleaning, oven dry, it is characterized in that:
(1) be raw material with single metal titanium compound or metal titanium and potassium hydroxide, pack in the reaction vessel, adding deionized water makes the reaction vessel compactedness be controlled at its volumetrical 50～85%, the concentration of single metal titanium compound of reaction vessel or metal titanium is 0.4mol/L～3mol/L, the concentration of KOH is 10mol/L～40mol/L
(2) hydrothermal reaction condition is 100～200 ℃, insulation 2～48hrs.
3,, it is characterized in that described single metal titanium compound is a kind of in titanium dioxide and the metatitanic acid four fourth fat by the method for the synthetic trigonal crystal structure potassium titanate of the described a kind of hydro-thermal of claim 2.
4, by the method for claim 2 or the synthetic trigonal crystal structure potassium titanate of 3 described a kind of hydro-thermals, it is characterized in that employed TiO
2Concentration be 1mol/L, the concentration of KOH is 10mol/L, 200 ℃ of hydro-thermal reactions, the insulation 6hrs.
5, be used as function ceramics crystal seed, ferroelectric ceramic(s), cation-adsorption, exchange material or support of the catalyst by the described trigonal crystal structure potassium titanate of claim 1.
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| CNB031291147A CN1304298C (en) | 2003-06-05 | 2003-06-05 | Trigonal structure potassium titanate and its preparing method |
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|---|---|---|---|
| CNB031291147A CN1304298C (en) | 2003-06-05 | 2003-06-05 | Trigonal structure potassium titanate and its preparing method |
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| CN1458068A true CN1458068A (en) | 2003-11-26 |
| CN1304298C CN1304298C (en) | 2007-03-14 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100434366C (en) * | 2005-03-31 | 2008-11-19 | 中国科学院过程工程研究所 | Process for preparing potassium titanate by sub-molten salt method |
| CN102691105A (en) * | 2012-06-12 | 2012-09-26 | 浙江大学 | Method for preparing barium titanate monocrystal nano particles of six-pin structural perovskite |
| CN103101968A (en) * | 2011-11-09 | 2013-05-15 | 上海纳米技术及应用国家工程研究中心有限公司 | Potassium titanate nanowire and preparation method thereof |
| CN106232525A (en) * | 2014-04-28 | 2016-12-14 | 东邦钛株式会社 | The manufacture method of potassium titanate |
| CN106637408A (en) * | 2016-12-23 | 2017-05-10 | 张家港大塚化学有限公司 | Preparation method of acicular short fiber composite potassium hexatitanate crystal whisker |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS516200A (en) * | 1974-07-05 | 1976-01-19 | Central Glass Co Ltd | Kaatsukadatsusuihonyoru chitansankarisenino seizohoho |
| CN1086426C (en) * | 1999-01-07 | 2002-06-19 | 南京化工大学 | Prodn. method of potassium titanate whisker and fiber |
| JP3482461B2 (en) * | 2000-03-28 | 2003-12-22 | 独立行政法人産業技術総合研究所 | Potassium titanate photocatalyst and method for producing the same |
| CN1230381C (en) * | 2001-01-04 | 2005-12-07 | 川铁矿业株式会社 | Potassium titanate powder |
-
2003
- 2003-06-05 CN CNB031291147A patent/CN1304298C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100434366C (en) * | 2005-03-31 | 2008-11-19 | 中国科学院过程工程研究所 | Process for preparing potassium titanate by sub-molten salt method |
| CN103101968A (en) * | 2011-11-09 | 2013-05-15 | 上海纳米技术及应用国家工程研究中心有限公司 | Potassium titanate nanowire and preparation method thereof |
| CN102691105A (en) * | 2012-06-12 | 2012-09-26 | 浙江大学 | Method for preparing barium titanate monocrystal nano particles of six-pin structural perovskite |
| CN106232525A (en) * | 2014-04-28 | 2016-12-14 | 东邦钛株式会社 | The manufacture method of potassium titanate |
| CN106637408A (en) * | 2016-12-23 | 2017-05-10 | 张家港大塚化学有限公司 | Preparation method of acicular short fiber composite potassium hexatitanate crystal whisker |
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| CN1304298C (en) | 2007-03-14 |
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