CN103101968A - Potassium titanate nanowire and preparation method thereof - Google Patents
Potassium titanate nanowire and preparation method thereof Download PDFInfo
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- CN103101968A CN103101968A CN2011103520945A CN201110352094A CN103101968A CN 103101968 A CN103101968 A CN 103101968A CN 2011103520945 A CN2011103520945 A CN 2011103520945A CN 201110352094 A CN201110352094 A CN 201110352094A CN 103101968 A CN103101968 A CN 103101968A
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Abstract
The invention relates to a potassium titanate nanowire and a preparation method thereof. The potassium titanate nanowire has a potassium octatitanate (K2Ti8O17) crystal form, diameter between 4 and 9 nm, length between 100 and 1000 nm, and uniform morphology. The preparation method of the potassium titanate nanowire is characterized by comprising the following steps: (1) adding a solid or liquid titanium source into an alcohol-water solution of potassium hydroxide, and rapidly stirring to form a homogeneous suspension; (2) placing the suspension obtained in the step (1) into stainless steel autoclave with a polytetrafluoroethylene lining, and subjecting the suspension to a hydrothermal treatment for 24-72 h at temperature of 373-473K; and (3) after the reaction, washing the precipitate product with deionized water and dilute hydrochloric acid until a washing fluid reaches a neutral state, and drying to obtain the potassium titanate nanowire. The preparation method has simple process and flow, wide parameter adjustable range, strong repeatability and low cost, and shows a commercial prospect.
Description
Technical field
The present invention relates to a kind of Nano lines of potassium titanate and preparation method thereof, particularly a kind of diameter less than the high length-diameter ratio Nano lines of potassium titanate of 10 nanometers, belongs to inorganic nano material and synthesis technical field.
Background technology
Nano lines of potassium titanate is the very excellent matrix material enhancement nanofiber of a kind of performance, has good mechanical property and physicals, also has very high electrical insulating property and heat-resisting heat-proof quality (1200 oC in air).The coefficient of expansion and plastics are suitable, and the composite reinforced plastics consistency is good, show good wear resistance and oilness.Be widely used in fields such as engineering plastics, friction materials, heat insulation, insulating material.
The preparation method of the bibliographical information Nano lines of potassium titanate of at present existing some amount.But all more than 100 nanometers, specific surface area is less for prepared nanowire diameter, the comparatively small amt of nano wire under unit mass.And some adopts high temperature solid-state scorification, and energy consumption is higher, and due to easy sintering between nano wire under high temperature, nano wire is not independently to exist with single form.Constantly there is alkali (K2O) to melt out in sintering process, reaction vessel is had serious corrodibility.Therefore, need to seek a kind of less energy-consumption, the preparation method, prepare the Nano lines of potassium titanate with minor diameter, bigger serface, high length-diameter ratio and polymolecularity cheaply.
Eight potassium titanates (K2Ti8O17) are shared by the octahedra limit of TiO6 or summit, form case type tunnel-like structures, have more excellent wear-resisting, heat insulation and shock resistance.Although the report such as Sun Xiaoming, Li Yadong synthesized eight Nano lines of potassium titanate of diameter below 100 nanometers (Inorg. Chem. 2002,41,4996-4998).But, show only to have the diameter of individual nanowires less according to the transmission electron microscope photo in above-mentioned document, in 15 nanometers left and right, still, the nanowire diameter of the overwhelming majority all between 20～30, pattern and heterogeneity.At present, diameter has no report less than polymolecularity eight potassium titanates (K2Ti8O17) nano wire of 10 nanometers, pattern homogeneous.
Summary of the invention
The invention provides a kind of Nano lines of potassium titanate, it is characterized in that, is eight potassium titanates (K2Ti8O17) crystal formations, diameter between 4～9 nanometers, length between 100～1000 nanometers, the pattern homogeneous.
The present invention also provides a kind of preparation method of Nano lines of potassium titanate, it is characterized in that comprising the steps:
(1) solid phase or liquid phase titanium source are joined in the alcohol solution of potassium hydroxide, rapid stirring makes it form uniform suspension;
(2) will be put into the stainless steel autoclave of teflon lined by the suspension of step (1) gained, carry out hydrothermal treatment consists 24～72 hours at the temperature of 373～473K;
(3) after reaction finishes, precipitated product is washed with deionized water and dilute hydrochloric acid, until washings approaches neutrality, drying obtains Nano lines of potassium titanate after processing.
Solid phase titanium source described in step (1) is a kind of or its combination in rutile titanium dioxide powder, anatase titanium dioxide powder, brookite type titanium dioxide powder; Described liquid phase titanium source is a kind of or its combination in positive four butyl esters of metatitanic acid, isopropyl titanate, titanium sulfate.
In alcohol solution described in step (1), the amount concentration of potassium hydroxide is 0.5 mol/L～15 mol/L; Described alcohol is ethanol, and shared volume percent is 0%～90%.
It is 0.5 gram/100 milliliter～5 grams/100 milliliter that solid phase titanium source described in step (1) adds the alcohol solution volume ratio of quality and potassium hydroxide; It is 5 milliliters/100 milliliters～20 milliliters/100 milliliters that described liquid phase titanium source adds the alcohol solution volume ratio of volume and potassium hydroxide.
The amount concentration of the dilute hydrochloric acid described in step (3) is between 0.01 mol/L～0.2 mol/L.
In a preferred technical scheme of the present invention, described solid phase titanium source can be rutile titanium dioxide powder, anatase titanium dioxide powder or brookite type titanium dioxide powder, can be also the mixture of above-mentioned crystal formation titanium dioxide powder;
In another preferred technical scheme of the present invention, described liquid phase titanium source can be positive four butyl esters of metatitanic acid, isopropyl titanate, titanium sulfate etc., can be also the mixture in above-mentioned two or more liquid phase titanium source;
In another another preferred technical scheme of the present invention, the alcohol that adds in described alcohol solution is ethanol, and shared volume percent is between 0%～90%.
The potassium titanate that obtains by above-mentioned preparation method is the K2Ti8O17 crystal formation, and its crystal formation and standard powdery diffractometry card (JCPDS:41-1100) match.Pattern is the linear of one dimension, diameter between 4～9 nanometers, length between 100～1000 nanometers, the pattern homogeneous, purity is high, stability is strong, can synthesize in enormous quantities, can be widely used in engineering plastics, abrasive rubber, the fields such as heat insulation and insulating material.This preparation method's technique and simple flow, the parameter variable range is wide, and repeatable strong, cost is low, is a kind of preparation method who possesses commercial promise.
Description of drawings
Fig. 1: the X-ray powder diffraction collection of illustrative plates of the Nano lines of potassium titanate that is made by embodiment 2.
Fig. 2: the transmission electron microscope photo of the Nano lines of potassium titanate that is made by embodiment 2.
Fig. 3: the high-resolution-ration transmission electric-lens photo of the Nano lines of potassium titanate that is made by embodiment 2.
Embodiment
The present invention is further elaborated below by embodiment, and its purpose only is better to understand content of the present invention.Therefore, the cited case does not limit protection scope of the present invention.
Embodiment 1:
15 milliliters of titanium sulfates join (volume percent of ethanol is 20%) in the potassium hydroxide alcohol solution that 130 ml concns are 3 mol/L, and vigorous stirring mixes it in the titanium sulfate fast hydrolyzing.Then suspension is put into the stainless steel autoclave that volume is 200 milliliters of teflon lined, reaction is 60 hours under 393K.After reaction finishes, precipitated product is washed with deionized water and dilute hydrochloric acid, until washings approaches neutrality, obtain Nano lines of potassium titanate after drying treatment.
The crystal formation of obtained Nano lines of potassium titanate and standard powdery diffractometry card (JCPDS:41-1100) match, and nanowire diameter is about 6 nanometers, and length is between 100～800 nanometers, and purity is more than 99%.
Embodiment 2:
8 milliliters of positive four butyl esters of metatitanic acid join (volume percent of ethanol is 10%) in the potassium hydroxide alcohol solution that 65 ml concns are 5 mol/L, and vigorous stirring mixes it in the positive four butyl ester fast hydrolyzings of metatitanic acid.Then suspension is put into the stainless steel autoclave that volume is 100 milliliters of teflon lined, reaction is 48 hours under 423K.After reaction finishes, precipitated product is washed with deionized water and dilute hydrochloric acid, until washings approaches neutrality, obtain Nano lines of potassium titanate after drying treatment.
The crystal formation of obtained Nano lines of potassium titanate and standard powdery diffractometry card (JCPDS:41-1100) match, and nanowire diameter is about 7 nanometers, and length is between 100～1000 nanometers, and purity is more than 99%.
Embodiment 3:
4 milliliters of isopropyl titanates join (volume percent of ethanol is 15%) in the potassium hydroxide alcohol solution that 35 ml concns are 2 mol/L, and vigorous stirring mixes it in the isopropyl titanate fast hydrolyzing.Then suspension is put into the stainless steel autoclave that volume is 50 milliliters of teflon lined, reaction is 48 hours under 413K.After reaction finishes, precipitated product is washed with deionized water and dilute hydrochloric acid, until washings approaches neutrality, obtain Nano lines of potassium titanate after drying treatment.
The crystal formation of obtained Nano lines of potassium titanate and standard powdery diffractometry card (JCPDS:41-1100) match, and nanowire diameter is about 5 nanometers, and length is between 200～800 nanometers, and purity is more than 99%.
Embodiment 4:
The commercial P25 type of 3 grams titanium dioxide powder (goldschmidt chemical corporation P25 type titanium dioxide, rutile is 3:7 with the ratio of anatase octahedrite, median size 30 nanometers) join (volume percent of ethanol is 30%) in the potassium hydroxide alcohol solution that 140 ml concns are 10 mol/L, rapid stirring mixes it simultaneously.Then suspension is put into the stainless steel autoclave that volume is 200 milliliters of teflon lined, reaction is 36 hours under 403K.After reaction finishes, precipitated product is washed with deionized water and dilute hydrochloric acid, until washings approaches neutrality, obtain Nano lines of potassium titanate after drying treatment.
The crystal formation of obtained Nano lines of potassium titanate and standard powdery diffractometry card (JCPDS:41-1100) match, and nanowire diameter is about 8 nanometers, and length is between 100～500 nanometers, and purity is more than 99%.
Embodiment 5:
1.5 gram rutile titanium dioxide powder joins (volume percent of ethanol is 50%) in the potassium hydroxide alcohol solution that 65 ml concns are 12 mol/L, rapid stirring mixes it simultaneously.Then suspension is put into the stainless steel autoclave that volume is 100 milliliters of teflon lined, reaction is 48 hours under 453K.After reaction finishes, precipitated product is washed with deionized water and dilute hydrochloric acid, until washings approaches neutrality, obtain Nano lines of potassium titanate after drying treatment.
The crystal formation of obtained Nano lines of potassium titanate and standard powdery diffractometry card (JCPDS:41-1100) match, and nanowire diameter is about 9 nanometers, and length is between 100～1000 nanometers, and purity is more than 99%.
Embodiment 6:
0.8 gram anatase titanium dioxide powder joins (volume percent of ethanol is 0%) in the potassium hydroxide alcohol solution that 30 ml concns are 8 mol/L, rapid stirring mixes it simultaneously.Then suspension is put into the stainless steel autoclave that volume is 50 milliliters of teflon lined, reaction is 72 hours under 433K.After reaction finishes, precipitated product is washed with deionized water and dilute hydrochloric acid, until washings approaches neutrality, obtain Nano lines of potassium titanate after drying treatment.
The crystal formation of obtained Nano lines of potassium titanate and standard powdery diffractometry card (JCPDS:41-1100) match, and nanowire diameter is about 6 nanometers, and length is between 100～600 nanometers, and purity is more than 99%.
Claims (6)
1. a Nano lines of potassium titanate, is characterized in that, is eight potassium titanate (K
2Ti
8O
17) crystal formation, diameter between 4～9 nanometers, length between 100～1000 nanometers, the pattern homogeneous.
2. according to the preparation method of claims 1 described a kind of Nano lines of potassium titanate, it is characterized in that comprising the steps:
(1) solid phase or liquid phase titanium source are joined in the alcohol solution of potassium hydroxide, rapid stirring makes it form uniform suspension;
(2) will be put into the stainless steel autoclave of teflon lined by the suspension of step (1) gained, carry out hydrothermal treatment consists 24～72 hours at the temperature of 373～473K;
(3) after reaction finishes, precipitated product is washed with deionized water and dilute hydrochloric acid, until washings approaches neutrality, drying obtains Nano lines of potassium titanate after processing.
3. a kind of preparation method of Nano lines of potassium titanate according to claim 2, it is characterized in that, the solid phase titanium source described in step (1) is a kind of or its combination in rutile titanium dioxide powder, anatase titanium dioxide powder, brookite type titanium dioxide powder; Described liquid phase titanium source is a kind of or its combination in positive four butyl esters of metatitanic acid, isopropyl titanate, titanium sulfate.
4. a kind of preparation method of Nano lines of potassium titanate according to claim 2, is characterized in that, in the alcohol solution described in step (1), the amount concentration of potassium hydroxide is 0.5 mol/L～15 mol/L; Described alcohol is ethanol, and shared volume percent is 0%～90%.
5. a kind of preparation method of Nano lines of potassium titanate according to claim 2, is characterized in that, it is 0.5 gram/100 milliliter～5 grams/100 milliliter that the solid phase titanium source described in step (1) adds the alcohol solution volume ratio of quality and potassium hydroxide; It is 5 milliliters/100 milliliters～20 milliliters/100 milliliters that described liquid phase titanium source adds the alcohol solution volume ratio of volume and potassium hydroxide.
6. a kind of preparation method of Nano lines of potassium titanate according to claim 2, is characterized in that, the amount concentration of the dilute hydrochloric acid described in step (3) is between 0.01 mol/L～0.2 mol/L.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106099093A (en) * | 2016-06-16 | 2016-11-09 | 西南大学 | Titanium-based oxide K containing potassium2ti8o17preparation method and products thereof and application |
| CN106629827A (en) * | 2016-11-18 | 2017-05-10 | 中国科学院合肥物质科学研究院 | Potassium titanate nano-ribbon and preparation method and application thereof |
| CN106629840A (en) * | 2016-11-17 | 2017-05-10 | 广东工业大学 | Preparation method of truncated cylinder-shaped octahedral anatase type TiO2 |
| 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 |
| CN106800308A (en) * | 2016-12-24 | 2017-06-06 | 张家港大塚化学有限公司 | The preparation method and applications of potassium titanate nanofiber |
| CN107381627A (en) * | 2017-08-25 | 2017-11-24 | 陕西科技大学 | A kind of cupric layered potassium titanate platy particles and its hydrothermal preparing process |
| CN107381626A (en) * | 2017-08-25 | 2017-11-24 | 陕西科技大学 | A kind of iron content layered potassium titanate platy particles and its hydrothermal preparing process |
| CN107555488A (en) * | 2017-08-25 | 2018-01-09 | 陕西科技大学 | A kind of cobalt containing layer shape potassium titanate platy particles and its hydrothermal preparing process |
| CN110735135A (en) * | 2018-07-18 | 2020-01-31 | 南京理工大学 | Synthesis method of potassium titanate arrays with different nanostructures |
| CN113327775A (en) * | 2021-05-28 | 2021-08-31 | 河北工业大学 | Preparation method of potassium ion micro hybrid capacitor and electrode material |
| CN116712973A (en) * | 2023-06-29 | 2023-09-08 | 昆明理工大学 | Carbon-doped potassium titanate composite material and preparation method and application thereof |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106099093A (en) * | 2016-06-16 | 2016-11-09 | 西南大学 | Titanium-based oxide K containing potassium2ti8o17preparation method and products thereof and application |
| CN106629840A (en) * | 2016-11-17 | 2017-05-10 | 广东工业大学 | Preparation method of truncated cylinder-shaped octahedral anatase type TiO2 |
| CN106629840B (en) * | 2016-11-17 | 2017-11-17 | 广东工业大学 | A kind of truncated cylinder shape octahedron Detitanium-ore-type TiO2Preparation method |
| CN106629827A (en) * | 2016-11-18 | 2017-05-10 | 中国科学院合肥物质科学研究院 | Potassium titanate nano-ribbon and preparation method and application thereof |
| 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 |
| CN106800308A (en) * | 2016-12-24 | 2017-06-06 | 张家港大塚化学有限公司 | The preparation method and applications of potassium titanate nanofiber |
| CN107555488A (en) * | 2017-08-25 | 2018-01-09 | 陕西科技大学 | A kind of cobalt containing layer shape potassium titanate platy particles and its hydrothermal preparing process |
| CN107381626A (en) * | 2017-08-25 | 2017-11-24 | 陕西科技大学 | A kind of iron content layered potassium titanate platy particles and its hydrothermal preparing process |
| CN107381627A (en) * | 2017-08-25 | 2017-11-24 | 陕西科技大学 | A kind of cupric layered potassium titanate platy particles and its hydrothermal preparing process |
| CN107381626B (en) * | 2017-08-25 | 2019-06-14 | 陕西科技大学 | A kind of iron content layered potassium titanate platy particles and its hydrothermal preparing process |
| CN107555488B (en) * | 2017-08-25 | 2019-06-14 | 陕西科技大学 | A kind of cobalt containing layer shape potassium titanate platy particles and its hydrothermal preparing process |
| CN110735135A (en) * | 2018-07-18 | 2020-01-31 | 南京理工大学 | Synthesis method of potassium titanate arrays with different nanostructures |
| CN113327775A (en) * | 2021-05-28 | 2021-08-31 | 河北工业大学 | Preparation method of potassium ion micro hybrid capacitor and electrode material |
| CN113327775B (en) * | 2021-05-28 | 2022-04-29 | 河北工业大学 | Preparation method of potassium ion micro hybrid capacitor and electrode material |
| CN116712973A (en) * | 2023-06-29 | 2023-09-08 | 昆明理工大学 | Carbon-doped potassium titanate composite material and preparation method and application thereof |
| CN116712973B (en) * | 2023-06-29 | 2024-01-23 | 昆明理工大学 | Carbon-doped potassium titanate composite material and preparation method and application thereof |
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Application publication date: 20130515 |