CN104098132A - Preparation method for {100} crystal plane anatase TiO2 nano-particles - Google Patents

Preparation method for {100} crystal plane anatase TiO2 nano-particles Download PDF

Info

Publication number
CN104098132A
CN104098132A CN201410367311.1A CN201410367311A CN104098132A CN 104098132 A CN104098132 A CN 104098132A CN 201410367311 A CN201410367311 A CN 201410367311A CN 104098132 A CN104098132 A CN 104098132A
Authority
CN
China
Prior art keywords
tio
hydrogen peroxide
crystal face
nano particle
titanium
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.)
Granted
Application number
CN201410367311.1A
Other languages
Chinese (zh)
Other versions
CN104098132B (en
Inventor
李建明
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ningbo micro nano New Material Technology Co., Ltd
Original Assignee
李建明
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by 李建明 filed Critical 李建明
Priority to CN201410367311.1A priority Critical patent/CN104098132B/en
Publication of CN104098132A publication Critical patent/CN104098132A/en
Application granted granted Critical
Publication of CN104098132B publication Critical patent/CN104098132B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The application of the invention discloses a preparation method for {100} crystal plane anatase TiO2 nano-particles. The preparation method comprises the following steps: performing hydration reaction on a titanium source to obtain hydrated TiO2 precipitation, and dispersing the hydrated TiO2 precipitation into an alkaline hydrogen peroxide solution for realizing a hydrothermal reaction so as to obtain the exposed active {100} crystal plane anatase TiO2 nano-particles, wherein the pH value of the alkaline hydrogen peroxide solution is 8-13. By the adoption of the preparation method for the {100} crystal plane anatase TiO2 nano-particles, the exposed active {100} crystal plane anatase TiO2 nano-particles of which particle sizes are less than 15 nanometers can be prepared.

Description

One is prepared { 100} crystal face Anatase TiO 2the method of nano particle
Technical field
The present invention relates to functional photocatalyst material preparation field, relate in particular to one and prepare { 100} crystal face Anatase TiO 2the method of nano particle.
Background technology
Titanium dioxide (TiO 2) owing to thering is the features such as abundant, nontoxic, the good stability in source, be subject to the extensive concern of industrial and scientific research circle.In the recent period, Anatase TiO 2be considered to one of optimal photocatalyst material, be widely used in photocatalysis air-cleaning and photochemical catalysis water treatment.
Anatase TiO 2photocatalysis efficiency and its size, pattern, exposure crystal face, degree of scatter, crystallinity etc. closely bound up, as a rule, little particle size has large specific surface area, can adsorb more organism, shows higher photocatalysis efficiency; Equally, the degree of scatter of particle is larger, is more conducive to the lifting of photocatalysis efficiency; In addition TiO, 2pattern directly determined that it,, to the absorbing and scattering of light of light, has determined the separation efficiency in light induced electron-hole, in general, there is the TiO of accurate one-dimentional structure pattern (as wire, tubulose, bar-shaped and spindle body shape etc.) 2conventionally show higher photocatalysis efficiency.
It is worthy of note, expose high reactivity crystal face (as 100} or 001} crystal face) Anatase TiO 2can show better photocatalysis effect.The TiO of a thermodynamically stable Anatase 2tendency forms the octahedra particle of a small amount of rescinded angle, and particle is by 8 SA { 101} and 2 highly active { 001} crystal face formations.Wherein, { the shared ratio of 101} crystal face, up to 94%,, very easily disappears due to features such as its activity is high, poor stabilities mainly due to high reactivity crystal face in the process of growth of material.Therefore, Anatase TiO 2process of growth very easily expose low activity crystal face { 101} crystal face forms octahedra particle.In the recent period, adopt fluorion as stablizer, prepare and expose a large amount of high reactivities { Anatase TiO of 001} crystal face 2micron particle, and confirm that it has higher photocatalytic activity.Subsequently, a series of research work all carry out to prepare a large amount of exposures { Anatase TiO of 001} crystal face how 2.These work comprise how increasing oarse-grained rescinded angle degree, subtract improvement of short grained particle diameter and synthetic method etc.
Have theoretical reckoner bright, { 100} crystal face is than { 101} crystal face has higher crystal face energy, and has some scholars to think that its crystal face can be also higher than { 001} crystal face.But, about exposing a large amount of high reactivities { Anatase TiO of 100} crystal face 2the synthetic report of nano particle seldom.Preparation at present exposes a large amount of high reactivities { Anatase TiO of 100} crystal face 2the method of nano particle is presoma for adopting sodium titanate nanotubes, directly to its hydrothermal conversion, exposes a large amount of { cubic column Anatase TiO of 100} crystal face to prepare to have 2nanometer rod.Aforesaid method can be prepared to have and expose a large amount of { cubic column Anatase TiO of 100} crystal face 2nanometer rod mainly due to sodium titanate nanotubes relatively stable and it decompose process in can discharge gradually hydroxide ion, play the stable { effect of 100} crystal face.The above-mentioned Anatase TiO preparing 2particle is cubic column pattern, and the particle diameter of particle is all greater than 50 nanometers.Therefore, synthetic size is less than exposure activity { the 100} crystal face Anatase TiO of 50 nanometers 2nano particle is still a technical barrier.
Summary of the invention
In view of the deficiencies in the prior art, the invention provides one and prepare { 100} crystal face Anatase TiO 2the method of nano particle, can prepare exposure activity { the Anatase TiO of 100} crystal face that grain size is less than 15 nanometers 2nano particle.
One provided by the present invention is prepared { 100} crystal face Anatase TiO 2the method of nano particle, comprising:
Titanium source is obtained to hydration TiO by hydrolysis reaction 2precipitation;
By described hydration TiO 2precipitation is dispersed in alkaline hydrogen peroxide solution carries out hydro-thermal reaction, obtains exposing active { the Anatase TiO of 100} crystal face 2nano particle; The pH value of described alkaline hydrogen peroxide solution is 8 to 13.
Preferably, in hydrogen peroxide solution, add alkali or in alkaline solution, add hydrogen peroxide and obtain described alkaline hydrogen peroxide solution.
Preferably, the pH value of described alkaline hydrogen peroxide solution is 8.5 to 10.5.
Preferably, described titanium source is selected from one or several the combination in titanium ethanolate, titanium propanolate, tetrabutyl titanate, titanium ethylene glycolate, glycerol titanium, titanium sulfate, titanyl sulfate, titanium tetrachloride, titanium tetrafluoride, ammonium titanium fluoride.
Preferably, described hydrolysis reaction generates hydration TiO for described titanium source being dispersed in to direct hydrolysis in deionized water 2precipitation, or, described hydrolysis reaction is one or more the mixing solutions in the aqueous solution of the aqueous solution by slowly add tetramethylammonium hydroxide aqueous solution, the tetraethyl ammonium hydroxide aqueous solution, the TPAOH aqueous solution, the TBAH aqueous solution, ammoniacal liquor, aqueous sodium hydroxide solution, potassium hydroxide aqueous solution, from amine to described titanium source, urea, makes the hydrolysis of titanium source generate hydration TiO 2precipitation.
Preferably, purify and obtain described hydration TiO in described titanium source after hydrolysis reaction 2precipitation; Described purification is used for removing ion, obtains the hydration TiO of purity more than 97% 2precipitation, described purification mode adopts the combination of one or several modes in washing-centrifugation, washing-membrane sepn, washing-filtration and dialysis.
Preferably, described alkali is one or more the mixture in Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH, TBAH, ammoniacal liquor, amine substance, urea, and alkali concn is 0 to 0.1 mole every liter.
Preferably, in described alkaline hydrogen peroxide solution, the volume fraction of hydrogen peroxide is 0.5% to 8%.
Preferably, described hydration TiO 2the massfraction that precipitation is dispersed in described alkaline hydrogen peroxide solution is 0.001% to 5%.
Preferably, the temperature of described hydro-thermal reaction is 60 to 160 degrees Celsius, and the time is 1 to 48 hour.
TiO prepared by the present invention 2nano particle has high reactivity, and { 100} crystal face, spindle body shape, single-size, grain diameter can be less than that 15 nanometers, photocatalytic activity are high, good dispersity, the feature such as be difficult for reuniting, pollution-free, have good application prospect in fields such as photocatalysis air-cleaning and photochemical catalysis water treatments.
The present invention has the following advantages:
1, the TiO that the method obtains 2nano particle is spindle body shape, and grain diameter can be less than 15 nanometers, monodispersity is good;
2, the TiO that the method obtains 2nano particle exposes a large amount of high reactivities { 100} crystal face;
3, the TiO that the method obtains 2it is good that nano particle has suspension property, is difficult for the feature of reuniting;
4, the TiO that the method obtains 2photocatalysis efficiency is high, can be applicable to the field such as photocatalysis air-cleaning and photochemical catalysis water treatment.
Brief description of the drawings
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, to the accompanying drawing of required use in embodiment or description of the Prior Art be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those skilled in the art, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is that the present invention prepares { 100} crystal face Anatase TiO 2the method flow diagram of nano particle.
Fig. 2 is that the present invention prepares { 100} crystal face Anatase TiO 2the spindle shape TiO that the method for nano particle prepares 2the scanning electron microscope (SEM) photograph of nano particle; In Fig. 2, the product that figure (a) and figure (b) obtain for embodiment 1, particle size were is 10 to 15 nanometers, length is 20 to 30 nanometers; The product that figure (c) and figure (d) obtain for embodiment 2, particle size were is 8 to 10 nanometers, length is 12 to 15 nanometers.
Fig. 3 is the spindle shape TiO that embodiment 1 prepares 2the high-resolution-ration transmission electric-lens figure of nano particle, can find out TiO by lattice fringe in figure and Fourier's electronics Transformation Graphs 2the direction of growth of particle is <001> direction, and particle side exposes a large amount of high reactivities { 100} crystal face.
Fig. 4 is the spindle shape TiO that embodiment 1 prepares 2the optical picture of nano particle, not free settling.
Embodiment
In order to make those skilled in the art person understand better the technical scheme in the application, below in conjunction with the accompanying drawing in the embodiment of the present application, technical scheme in the embodiment of the present application is clearly and completely described, obviously, described embodiment is only some embodiments of the present application, instead of whole embodiment.Based on the embodiment in the application, the every other embodiment that those of ordinary skill in the art obtain under the prerequisite of not making creative work, should belong to the scope of protection of the invention.
Please refer to Fig. 1, the one that one embodiment of the present invention provide is prepared { 100} crystal face Anatase TiO 2the method of nano particle, comprises the following steps:
Titanium source is obtained to hydration TiO by hydrolysis reaction 2precipitation;
By described hydration TiO 2precipitation is dispersed in alkaline hydrogen peroxide solution carries out hydro-thermal reaction, obtains exposing active { the Anatase TiO of 100} crystal face 2nano particle; The pH value of described alkaline hydrogen peroxide solution is 8 to 13.
Further, described alkaline hydrogen peroxide solution obtains by adding alkali in hydrogen peroxide solution or add hydrogen peroxide in alkaline solution.Described alkali can be one or more the mixture in Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH, TBAH, ammoniacal liquor, amine substance, urea, and the concentration of described alkali can be 0 to 0.1 mole every liter.The pH value of described alkaline hydrogen peroxide solution can be 8.5 to 10.5, and in described alkaline hydrogen peroxide solution, the volume fraction of hydrogen peroxide can be 0.5% to 8%.
Further, described titanium source is selected from one or several the combination in titanium ethanolate, titanium propanolate, tetrabutyl titanate, titanium ethylene glycolate, glycerol titanium, titanium sulfate, titanyl sulfate, titanium tetrachloride, titanium tetrafluoride, ammonium titanium fluoride.
Further, described hydrolysis reaction generates hydration TiO for described titanium source being dispersed in to direct hydrolysis in deionized water 2precipitation, or, described hydrolysis reaction is one or more the mixing solutions in the aqueous solution of the aqueous solution by slowly add tetramethylammonium hydroxide aqueous solution, the tetraethyl ammonium hydroxide aqueous solution, the TPAOH aqueous solution, the TBAH aqueous solution, ammoniacal liquor, aqueous sodium hydroxide solution, potassium hydroxide aqueous solution, from amine to described titanium source, urea, makes the hydrolysis of titanium source generate hydration TiO 2precipitation.
Further, purify and obtain described hydration TiO in described titanium source after hydrolysis reaction 2precipitation; Described purification is used for removing ion, obtains the hydration TiO of purity more than 97% 2precipitation, described purification mode adopts the combination of one or several modes in washing-centrifugation, washing-membrane sepn, washing-filtration and dialysis.
Further, described hydration TiO 2the massfraction that precipitation is dispersed in described alkaline hydrogen peroxide solution is 0.001% to 5%.The temperature of described hydro-thermal reaction is 60 to 160 degrees Celsius, and the time is 1 to 48 hour.
The TiO preparing by above-mentioned present embodiment 2nano particle has high reactivity, and { 100} crystal face, spindle body shape, single-size, grain diameter can be less than that 15 nanometers, photocatalytic activity are high, good dispersity, the feature such as be difficult for reuniting, pollution-free, have good application prospect in fields such as photocatalysis air-cleaning and photochemical catalysis water treatments.
Above-mentioned present embodiment has the following advantages:
1, can find out with reference to figure 2 TiO that present embodiment obtains 2nano particle is spindle body shape, and grain diameter is less than 15 nanometers, monodispersity is good;
2, can find out with reference to figure 3 TiO that present embodiment obtains 2nano particle exposes a large amount of high reactivities { 100} crystal face;
3, can find out with reference to figure 4 TiO that present embodiment obtains 2it is good that nano particle has suspension property, is difficult for the feature of reuniting;
4, the TiO that the method obtains 2photocatalysis efficiency is high, can be applicable to the field such as photocatalysis air-cleaning and photochemical catalysis water treatment.
Embodiment 1
Under agitation condition, by 2.5 grams of titanium sulfate dispersing and dissolvings in 100 ml deionized water.Slowly drip concentration and be the Tetramethylammonium hydroxide of 0.1 mole every liter in above-mentioned solution, until solution is neutral (pH value is about 7), make titanium sulfate be hydrolyzed gradually generation hydration TiO 2precipitation.By hydration TiO 2precipitate ultrasonic dispersion, with deionized water wash repeatedly, centrifugation obtains the hydration TiO of high purity (purity is more than 97%) 2precipitation.Secondly, prepare 200 milliliters of hydrogen peroxide solutions that hydrogen peroxide volume fraction is 2%, add weak ammonia to regulate it to form the alkaline hydrogen peroxide solution that pH value is 10.5.Subsequently, by the high purity hydrous TiO after above-mentioned washing 2precipitate ultrasonic be scattered in above-mentioned pH value be 10.5 and the hydrogen peroxide volume fraction alkaline hydrogen peroxide solution that is 2% in and stir after 1 hour, in 120 degrees Celsius of lower hydro-thermal reactions 6 hours, obtain figure a and shown a large amount of active { the spindle body shape Anatase TiO of 100} crystal face of exposure of figure b in Fig. 2 2nano particle, described spindle body shape Anatase TiO 2the particle size were of nano particle is 10 to 15 nanometers, and length is about 20 to 30 nanometers.The spindle shape TiO that Fig. 3 the present embodiment prepares 2the high-resolution-ration transmission electric-lens figure of nano particle, can find out TiO by lattice fringe in figure and Fourier's electronics Transformation Graphs 2the direction of growth of particle is <001> direction, and particle side exposes a large amount of high reactivities { 100} crystal face.Fig. 4 is the spindle shape TiO that the present embodiment prepares 2the optical picture of nano particle, can find out obtained spindle shape TiO 2nano particle is free settling not.
Embodiment 2
Under agitation condition, by 2.5 grams of titanium sulfate dispersing and dissolvings in 100 ml deionized water.Slowly drip concentration and be the Tetramethylammonium hydroxide of 0.1 mole every liter in above-mentioned solution, until solution is neutral (pH value is about 7), make titanium sulfate be hydrolyzed gradually generation hydration TiO 2precipitation.By hydration TiO 2precipitate ultrasonic dispersion, with deionized water wash repeatedly, obtain highly purified hydration TiO 2precipitation, centrifugation obtains highly purified hydration TiO 2precipitation.Secondly, prepare 200 milliliters of hydrogen peroxide solutions that hydrogen peroxide volume fraction is 2%, add weak ammonia to regulate it to form the alkaline hydrogen peroxide solution that pH value is 8.5.Subsequently, by the purity after above-mentioned washing at 97% above hydration TiO 2precipitate ultrasonic be scattered in above-mentioned pH value be 8.5 and the hydrogen peroxide volume fraction alkaline hydrogen peroxide solution that is 2% in and stir 1 hour, then in 120 degrees Celsius of lower hydro-thermal reactions 6 hours, obtain a small amount of active { the spindle body shape Anatase TiO of 100} crystal face of exposure as shown in the figure c in Fig. 2 and figure d 2nano particle, can find out described Anatase TiO 2the particle diameter of nano particle is 8 to 10 nanometers, and length is about 12 to 15 nanometers.
Embodiment 3
Under agitation condition, by 5 grams of titanium sulfate dispersing and dissolvings in 100 ml deionized water.Slowly drip concentration and be the ammoniacal liquor of 0.2 mole every liter in above-mentioned solution, until solution is neutral (pH value is about 7), make titanium sulfate be hydrolyzed gradually generation hydration TiO 2precipitation.By hydration TiO 2precipitate ultrasonic dispersion, with deionized water wash repeatedly, obtain the hydration TiO of purity more than 97% 2precipitation, centrifugation.Secondly, prepare 200 milliliters of hydrogen peroxide solutions that hydrogen peroxide volume fraction is 5%, adding rare Tetramethylammonium hydroxide to regulate it to become pH value is 9 alkaline hydrogen peroxide solution.Subsequently, by washing after purity at 97% above hydration TiO 2precipitation dispersed with stirring in above-mentioned pH value be 9 and the hydrogen peroxide volume fraction alkaline hydrogen peroxide solution that is 5% in and stir after 2 hours, in 100 degrees Celsius of lower hydro-thermal reactions 8 hours, obtain exposing activity { the spindle body shape Anatase TiO of 100} crystal face 2nano particle.
Embodiment 4
Under agitation condition, by 3 grams of titanyl sulfate dispersing and dissolvings in 100 ml deionized water.Slowly drip concentration and be the ammoniacal liquor of 0.2 mole every liter in above-mentioned solution, until solution is neutral (pH value is about 7), make titanyl sulfate be hydrolyzed gradually generation hydration TiO 2precipitation.By hydration TiO 2precipitate ultrasonic dispersion, with deionized water wash repeatedly, obtain highly purified hydration TiO 2precipitation, centrifugation.Secondly, prepare 200 milliliters of hydrogen peroxide solutions that hydrogen peroxide volume fraction is 5%, adding weak ammonia to regulate its pH value is 11 formation alkaline hydrogen peroxide solution.Subsequently, by washing after purity at 97% above hydration TiO 2precipitate ultrasonic be scattered in above-mentioned pH value be 11 and the hydrogen peroxide volume fraction alkaline hydrogen peroxide solution that is 5% in and stir after 1 hour, in 80 degrees Celsius of lower hydro-thermal reactions 24 hours, obtain exposing active { the spindle body shape Anatase TiO of 100} crystal face 2nano particle.
Embodiment 5
Under agitation condition, by 3 milliliters of ultrasonic being scattered in 100 ml deionized water of titanium tetrachloride.Slowly drip concentration and be the ammoniacal liquor of 0.1 mole every liter in above-mentioned solution, until solution is neutral (pH value is about 7), make titanium tetrachloride be hydrolyzed gradually generation hydration TiO 2precipitation.By hydration TiO 2precipitate ultrasonic dispersion, with deionized water wash repeatedly, obtain highly purified hydration TiO 2precipitation, centrifugation.Secondly, prepare 200 milliliters of aqueous hydrogen peroxide solutions that hydrogen peroxide volume fraction is 3%, add weak ammonia to regulate it to form the alkaline hydrogen peroxide solution that pH value is 12.Subsequently, by the high purity hydrous TiO after washing 2precipitate ultrasonic be scattered in above-mentioned pH value be 12 and the hydrogen peroxide volume fraction alkaline hydrogen peroxide solution that is 5% in and stir after 1 hour, in 140 degrees Celsius of lower hydro-thermal reactions 4 hours, obtain exposing a large amount of activity { spindle body shape Anatase TiO of 100} crystal face 2nano particle.
Embodiment 6
Under agitation condition, 2 milliliters of ultrasonic being scattered in 100 ml deionized water of titanium isopropylate are hydrolyzed and generate hydration TiO 2precipitation, and centrifugation.Secondly, prepare 100 milliliters of hydrogen peroxide solutions that hydrogen peroxide volume fraction is 2%, add weak ammonia to regulate it to form the alkaline hydrogen peroxide solution that pH is 9.Subsequently, by above-mentioned hydration TiO 2precipitate ultrasonic be scattered in above-mentioned pH value be 9 and the hydrogen peroxide volume fraction alkaline hydrogen peroxide solution that is 2% in and stir after 1 hour, in 105 degrees Celsius of lower hydro-thermal reactions 6 hours, obtain exposing active { the spindle body shape Anatase TiO of 100} crystal face 2nano particle.
Embodiment 7
Under agitation condition, 2 milliliters of ultrasonic being scattered in 100 ml deionized water of tetrabutyl titanate are hydrolyzed and generate hydration TiO 2precipitation, and centrifugation.Secondly, prepare 100 milliliters of hydrogen peroxide solutions that hydrogen peroxide volume fraction is 0.5%, add weak ammonia to regulate it to form the alkaline hydrogen peroxide solution that pH value is 13.Subsequently, by above-mentioned hydration TiO 2precipitate ultrasonic be scattered in above-mentioned pH value be 13 and the hydrogen peroxide volume fraction alkaline hydrogen peroxide solution that is 0.5% in and stir after 1 hour, in 100 degrees Celsius of lower hydro-thermal reactions 8 hours, obtain exposing active { the spindle body shape Anatase TiO of 100} crystal face 2nano particle.
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the scope of protection of present invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.

Claims (10)

1. prepare { 100} crystal face Anatase TiO for one kind 2the method of nano particle, is characterized in that, comprising:
Titanium source is obtained to hydration TiO by hydrolysis reaction 2precipitation;
By described hydration TiO 2precipitation is dispersed in alkaline hydrogen peroxide solution carries out hydro-thermal reaction, obtains exposing active { the Anatase TiO of 100} crystal face 2nano particle; The pH value of described alkaline hydrogen peroxide solution is 8 to 13.
2. prepare as claimed in claim 1 { 100} crystal face Anatase TiO 2the method of nano particle, is characterized in that: in hydrogen peroxide solution, add alkali or in alkaline solution, add hydrogen peroxide obtaining described alkaline hydrogen peroxide solution.
3. prepare as claimed in claim 1 { 100} crystal face Anatase TiO 2the method of nano particle, is characterized in that: the pH value of described alkaline hydrogen peroxide solution is 8.5 to 10.5.
4. prepare as claimed in claim 1 { 100} crystal face Anatase TiO 2the method of nano particle, is characterized in that: described titanium source is selected from one or several the combination in titanium ethanolate, titanium propanolate, tetrabutyl titanate, titanium ethylene glycolate, glycerol titanium, titanium sulfate, titanyl sulfate, titanium tetrachloride, titanium tetrafluoride, ammonium titanium fluoride.
5. prepare as claimed in claim 1 { 100} crystal face Anatase TiO 2the method of nano particle, is characterized in that: described hydrolysis reaction generates hydration TiO for described titanium source being dispersed in to direct hydrolysis in deionized water 2precipitation, or, described hydrolysis reaction is one or more the mixing solutions in the aqueous solution of the aqueous solution by slowly add tetramethylammonium hydroxide aqueous solution, the tetraethyl ammonium hydroxide aqueous solution, the TPAOH aqueous solution, the TBAH aqueous solution, ammoniacal liquor, aqueous sodium hydroxide solution, potassium hydroxide aqueous solution, from amine to described titanium source, urea, makes the hydrolysis of titanium source generate hydration TiO 2precipitation.
6. prepare as claimed in claim 1 { 100} crystal face Anatase TiO 2the method of nano particle, is characterized in that: purify and obtain described hydration TiO in described titanium source after hydrolysis reaction 2precipitation; Described purification is used for removing ion, obtains the hydration TiO of purity more than 97% 2precipitation, described purification mode adopts the combination of one or several modes in washing-centrifugation, washing-membrane sepn, washing-filtration and dialysis.
7. prepare as claimed in claim 2 { 100} crystal face Anatase TiO 2the method of nano particle, it is characterized in that: described alkali is one or more the mixture in Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, TPAOH, TBAH, ammoniacal liquor, amine substance, urea, and alkali concn is 0 to 0.1 mole every liter.
8. prepare as claimed in claim 1 { 100} crystal face Anatase TiO 2the method of nano particle, is characterized in that: in described alkaline hydrogen peroxide solution, the volume fraction of hydrogen peroxide is 0.5% to 8%.
9. prepare as claimed in claim 1 { 100} crystal face Anatase TiO 2the method of nano particle, is characterized in that: described hydration TiO 2the massfraction that precipitation is dispersed in described alkaline hydrogen peroxide solution is 0.001% to 5%.
10. prepare as claimed in claim 1 { 100} crystal face Anatase TiO 2the method of nano particle, is characterized in that: the temperature of described hydro-thermal reaction is 60 to 160 DEG C, and the time is 1 to 48 hour.
CN201410367311.1A 2014-07-30 2014-07-30 One kind prepares { 100 } crystal face Anatase TiO2The method of nano particle Active CN104098132B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410367311.1A CN104098132B (en) 2014-07-30 2014-07-30 One kind prepares { 100 } crystal face Anatase TiO2The method of nano particle

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410367311.1A CN104098132B (en) 2014-07-30 2014-07-30 One kind prepares { 100 } crystal face Anatase TiO2The method of nano particle

Publications (2)

Publication Number Publication Date
CN104098132A true CN104098132A (en) 2014-10-15
CN104098132B CN104098132B (en) 2017-04-05

Family

ID=51666730

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410367311.1A Active CN104098132B (en) 2014-07-30 2014-07-30 One kind prepares { 100 } crystal face Anatase TiO2The method of nano particle

Country Status (1)

Country Link
CN (1) CN104098132B (en)

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104261465A (en) * 2014-10-27 2015-01-07 李建明 Method for preparing titanate, titanic acid and titanium dioxide
CN105664839A (en) * 2016-03-30 2016-06-15 中国科学院生态环境研究中心 Lanthanum-loaded titanium dioxide adsorption material for commonly removing arsenic and fluorine and preparation method of lanthanum-loaded titanium dioxide adsorption material
RU2602536C1 (en) * 2015-09-25 2016-11-20 Федеральное государственное бюджетное учреждение науки Институт органического синтеза им. И.Я. Постовского Уральского отделения Российской академии наук (ИОС УрО РАН) Method of producing titanium dioxide/carbon composite
CN106186053A (en) * 2015-05-04 2016-12-07 中国石油化工股份有限公司 A kind of synthetic method of self-assembled nanometer titanium dioxide
CN106698507A (en) * 2017-02-21 2017-05-24 京东方科技集团股份有限公司 Method for preparing anatase titanium dioxide
CN106914230A (en) * 2017-02-08 2017-07-04 武汉理工大学 A kind of flower-shaped titania photocatalyst of helicoid and preparation method thereof
CN107010657A (en) * 2017-04-10 2017-08-04 江西师范大学 The anatase TiO that a kind of high energy { 001 } crystal face-selective corrodes2It is classified microballoon and its preparation method and application
CN107210379A (en) * 2015-01-21 2017-09-26 康宁精密素材株式会社 For the light extraction substrate of organic luminescent device and the organic luminescent device including it
CN108128803A (en) * 2018-03-09 2018-06-08 陕西科技大学 A kind of method that water-soluble titanium dioxide nano-particle is prepared using titanium valve as presoma
CN108975390A (en) * 2018-09-06 2018-12-11 中国石油天然气股份有限公司 A kind of threadiness hierarchical structure lithium titanate and its preparation method and application
CN109603550A (en) * 2018-12-14 2019-04-12 佛山市铁人环保科技有限公司 A kind of water solubility photocatalyst titanium oxide sol spray and preparation method thereof
CN110422878A (en) * 2019-09-11 2019-11-08 中南大学 One kind preparing anatase titanium dioxide TiO by ammonium titanium fluoride2The method of powder
CN110482600A (en) * 2019-09-11 2019-11-22 中南大学 A method of rutile titanium dioxide powder is prepared by tetrafluoro oxygen titanium acid ammonium
CN110697770A (en) * 2019-11-18 2020-01-17 江苏师范大学 Anatase TiO2Method for preparing decahedron
CN109319829B (en) * 2018-09-03 2021-01-29 中国石油天然气股份有限公司 Porous structure lithium titanate and preparation method and application thereof
CN114797692A (en) * 2022-04-07 2022-07-29 福建商学院 Preparation method of chitosan-based composite aerogel material capable of removing formaldehyde at room temperature

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101559979A (en) * 2009-05-22 2009-10-21 东华大学 Method for preparing extrafine anatase titanium dioxide nano rods

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101559979A (en) * 2009-05-22 2009-10-21 东华大学 Method for preparing extrafine anatase titanium dioxide nano rods

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
JIANMING LI ET AL.: "Tetragonal faceted-nanorods of anatase TiO2 single crystals with a large percentage of active {100} facets", 《CHEM. COMMUN.》 *

Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104261465B (en) * 2014-10-27 2016-07-06 李建明 A kind of preparation method of titanate, metatitanic acid and titanium dioxide
CN104261465A (en) * 2014-10-27 2015-01-07 李建明 Method for preparing titanate, titanic acid and titanium dioxide
CN107210379A (en) * 2015-01-21 2017-09-26 康宁精密素材株式会社 For the light extraction substrate of organic luminescent device and the organic luminescent device including it
CN106186053A (en) * 2015-05-04 2016-12-07 中国石油化工股份有限公司 A kind of synthetic method of self-assembled nanometer titanium dioxide
RU2602536C1 (en) * 2015-09-25 2016-11-20 Федеральное государственное бюджетное учреждение науки Институт органического синтеза им. И.Я. Постовского Уральского отделения Российской академии наук (ИОС УрО РАН) Method of producing titanium dioxide/carbon composite
CN105664839A (en) * 2016-03-30 2016-06-15 中国科学院生态环境研究中心 Lanthanum-loaded titanium dioxide adsorption material for commonly removing arsenic and fluorine and preparation method of lanthanum-loaded titanium dioxide adsorption material
CN105664839B (en) * 2016-03-30 2018-04-06 中国科学院生态环境研究中心 One kind carries lanthanum titanium dioxide arsenic fluorine altogether except sorbing material and preparation method thereof
CN106914230B (en) * 2017-02-08 2019-09-10 武汉理工大学 A kind of flower-shaped titania photocatalyst of helicoid and preparation method thereof
CN106914230A (en) * 2017-02-08 2017-07-04 武汉理工大学 A kind of flower-shaped titania photocatalyst of helicoid and preparation method thereof
CN106698507A (en) * 2017-02-21 2017-05-24 京东方科技集团股份有限公司 Method for preparing anatase titanium dioxide
CN107010657A (en) * 2017-04-10 2017-08-04 江西师范大学 The anatase TiO that a kind of high energy { 001 } crystal face-selective corrodes2It is classified microballoon and its preparation method and application
CN108128803A (en) * 2018-03-09 2018-06-08 陕西科技大学 A kind of method that water-soluble titanium dioxide nano-particle is prepared using titanium valve as presoma
CN109319829B (en) * 2018-09-03 2021-01-29 中国石油天然气股份有限公司 Porous structure lithium titanate and preparation method and application thereof
CN108975390A (en) * 2018-09-06 2018-12-11 中国石油天然气股份有限公司 A kind of threadiness hierarchical structure lithium titanate and its preparation method and application
CN108975390B (en) * 2018-09-06 2021-01-29 中国石油天然气股份有限公司 Linear hierarchical structure lithium titanate and preparation method and application thereof
CN109603550A (en) * 2018-12-14 2019-04-12 佛山市铁人环保科技有限公司 A kind of water solubility photocatalyst titanium oxide sol spray and preparation method thereof
CN110422878A (en) * 2019-09-11 2019-11-08 中南大学 One kind preparing anatase titanium dioxide TiO by ammonium titanium fluoride2The method of powder
CN110482600A (en) * 2019-09-11 2019-11-22 中南大学 A method of rutile titanium dioxide powder is prepared by tetrafluoro oxygen titanium acid ammonium
CN110697770A (en) * 2019-11-18 2020-01-17 江苏师范大学 Anatase TiO2Method for preparing decahedron
CN110697770B (en) * 2019-11-18 2022-03-25 江苏师范大学 Anatase TiO2Method for preparing decahedron
CN114797692A (en) * 2022-04-07 2022-07-29 福建商学院 Preparation method of chitosan-based composite aerogel material capable of removing formaldehyde at room temperature

Also Published As

Publication number Publication date
CN104098132B (en) 2017-04-05

Similar Documents

Publication Publication Date Title
CN104098132A (en) Preparation method for {100} crystal plane anatase TiO2 nano-particles
CN104190416A (en) Method for preparing metal doped TiO2 nanocrystal particles
CN101376112B (en) Method for preparing anatase titanic oxide sol
Li et al. Morphological control and photodegradation behavior of rutile TiO2 prepared by a low-temperature process
CN101559979B (en) Method for preparing extrafine anatase titanium dioxide nano rods
CN1295977A (en) Simple method for preparing titanium dioxide collosol
CN101525152B (en) Mumm-shaped 3D TiO nanometer material and preparation method thereof
CN101508464B (en) Process for preparing anatase type nano-titanium dioxide
CN103771485B (en) A kind of controllable method for preparing of cupric oxide three-dimensional manometer self-assembly
CN104201364A (en) Method for preparing spinel lithium titanate
CN104192899A (en) Method for preparing TiO2 nanocrystal particles
CN102976403B (en) A kind of controlled difference exposes the TiO of crystal face 2nanocrystalline preparation method
Jongprateep et al. Nanoparticulate titanium dioxide synthesized by sol–gel and solution combustion techniques
Wang et al. Hydrothermal synthesis and photocatalytic properties of pyrochlore Sm2Zr2O7 nanoparticles
CN102826597B (en) Method for preparing nanometer titanium dioxide
CN100445209C (en) Preparation method of new type nano-titanium dioxide powder
CN110201655B (en) One-step method for preparing hollow TiO2Method and application of nano-microspheres
CN101955222A (en) Method for preparing anatase-phase titanium dioxide sol
CN1785503A (en) Preparation method of soluble titanium dioxide nano-crystal
CN1762828A (en) Mesoporous nanopowder titanium dioxide bionic synthesis method
CN105523583B (en) A kind of synthetic method of nano-titanium dioxide powder
Gu et al. Preparation and characterization of highly photocatalytic active hierarchical BiOX (X= Cl, Br, I) microflowers for rhodamine B degradation with kinetic modelling studies
CN109772373A (en) A kind of preparation method with visible light-responded rGO/ black bismuth oxychloride-bismuth-bismuth oxide heterojunction photocatalyst
CN103803633A (en) Preparation method of zinc oxide/titanium dioxide nanometer composite material
CN100337740C (en) Crystal titanium dioxide light catalyst and synthesis thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
TR01 Transfer of patent right

Effective date of registration: 20200304

Address after: 315311 No. 999, Haifeng North Road, Cixi Binhai Economic Development Zone, Zhejiang Province

Patentee after: Ningbo micro nano New Material Technology Co., Ltd

Address before: 100083 Beijing city Haidian District No. 6 Xueyuan Road Furun 1 building A block 1706

Patentee before: Li Jianming

TR01 Transfer of patent right