CN106582591A - Preparation method of quadrangular anatase type TiO2 - Google Patents

Preparation method of quadrangular anatase type TiO2 Download PDF

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Publication number
CN106582591A
CN106582591A CN201611013596.4A CN201611013596A CN106582591A CN 106582591 A CN106582591 A CN 106582591A CN 201611013596 A CN201611013596 A CN 201611013596A CN 106582591 A CN106582591 A CN 106582591A
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preparation
time
period
certain
reaction
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Inventor
方杨飞
魏志钢
颜家鸿
刘月
梁凯
潘湛昌
胡光辉
黄嘉丽
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Guangdong University of Technology
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Guangdong University of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063Titanium; Oxides or hydroxides thereof
    • B01J35/39
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08Heat treatment
    • B01J37/10Heat treatment in the presence of water, e.g. steam
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/04Oxides; Hydroxides
    • C01G23/047Titanium dioxide
    • C01G23/053Producing by wet processes, e.g. hydrolysing titanium salts
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/04Oxides; Hydroxides
    • C01G23/047Titanium dioxide
    • C01G23/08Drying; Calcining ; After treatment of titanium oxide
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM

Abstract

The invention discloses a preparation method of quadrangular anatase type TiO2. The method comprises the following steps that sodium hydroxide, P25 and deionized water are used for performing a hydrothermal reaction to obtain sodium titanate, then, sodium titanate is evenly dispersed into the deionized water, the mixture is transferred into an autoclave with a polytetrafluoroethylene liner for a hydrothermal reaction, after the reaction is completed, an obtained product is filtered and dried, and the quadrangular anatase type TiO2 is obtained. The method is simple in synthetic technology, low in cost and high in purity, meets the large-scale industrial production condition and has the wide application prospect.

Description

A kind of quadrangular shape Detitanium-ore-type TiO2Preparation method
Technical field
The invention belongs to new inorganic material synthesis technical field, and in particular to a kind of quadrangular shape Detitanium-ore-type TiO2's Preparation method.
Background technology
With science and technology development and people's living standard generally improve, environmental problem it is increasingly serious, water process is into for people One of the key content paid close attention to, catalysis material is pursued because of its environmental protection by scientific circles, wherein TiO2As earliest The material for using has become the representative in the field.TiO2As a kind of semi-conducting material, with low cost, chemical stability it is good, Nontoxic the advantages of, at the aspect such as the energy and environmental improvement good application prospect is shown.
Common titanium dioxide has anatase, three kinds of crystalline structures of rutile and brockite.Wherein, anatase nano-TiO2 Powder body has optimal photocatalysis performance, is widely used in photocell/solar energy, battery, photic electrochromics, photocatalyst, intelligence Can the aspect such as face coat and sensor.It is found that by light activated TiO from Fujishima and Houda in 19722Can on electrode So that water decomposition, as hydrogen and after oxygen, TiO2 catalysis materials are always the focus of lot of domestic and foreign scholar's research.TiO2 Low cost, nontoxic and good stability.Extensive research simultaneously is also indicated that compared with the method for being usually used in curbing environmental pollution at present such as Chemical oxidation, biodegradation, high temperature incineration, physical absorption etc., nano-TiO2Semi-conducting material generates surface photoproduction-hole because of it And there is extremely strong photochemical catalytic oxidation ability, its catabolite is the small-molecule substance of the non-secondary pollution such as water and carbon dioxide, Many fields are had been supplied at present.
Nearest several years, expose not coplanar TiO2Article in terms of nanocrystalline nanostructured in other words is very more, Hui Ming Cheng et al. are prepared for the TiO of the different crystal faces of micron-sized exposure2, then test their photocatalytic activity.He Result show, TiO2{ 100 } compared to { 101 } and { 001 } with higher activity.They are attributed to difference reason Crystal face there is different level structures, and the co-ordination state of surface atom.But it is clear that such explanation can not allow people It is satisfied, the TiO that they use2Sample is all that micron is brilliant, and actually used TiO2Photocatalyst also has very big difference.
It was found that most of method can only prepare the TiO of hundreds of nanometer of exposure particular crystal plane to several micron-scales2Receive Meter Jing, and for the TiO of tens nano-scales2It is nanocrystalline then helpless.Therefore, it is necessary to developing one kind prepares TiO2Nanometer Brilliant method, can regulate and control TiO2Nanocrystalline exposure crystal face, this will be research TiO2Catalytic property the catalysis of one model is provided Agent, while being also beneficial to develop highly active TiO2Catalysis material.
The content of the invention
It is an object of the invention to provide a kind of process is simple, easy to operate quadrangular shape Detitanium-ore-type TiO2Preparation Method.
Technical scheme, comprises the following steps:
(1) solid NaOH is weighed, in being dissolved in beaker, constant volume shakes up in volumetric flask, is configured to certain density NaOH molten Liquid.
(2) NaOH solution of certain volume is measured, the P25 of certain mass is weighed, is added and is carried teflon-lined In autoclave, ultrasound a period of time, stirring a period of time, reaction a period of time under certain reaction temperature.
(3) room temperature is cooled to, obtains white precipitate, adjust pH value, be then centrifuged for separating, washing is dried, and obtains metatitanic acid Sodium.
(4) sodium titanate of certain mass is weighed, the deionized water of certain volume is measured, is added and is carried polytetrafluoroethyllining lining Autoclave in, ultrasound a period of time, stirring a period of time, under certain reaction temperature reaction a period of time.
(5) after the completion of question response, room temperature is cooled to, obtains white precipitate, be then centrifuged for separating, be dried, obtain quadrangular Shape Detitanium-ore-type TiO2
Certain density NaOH solution is 8-12mol/L in the step (1).
The NaOH solution of certain volume is measured in the step (2), the P25 for weighing certain mass adds for 1mL NaOH solutions Enter 0.0025-0.0035g P25.
Certain reaction temperature is 110-140 DEG C in the step (2), and reaction a period of time is 22-26h.
Ultrasound a period of time is 10-15min in the step (2), (4), and stirring a period of time is more than 1h.
Solution ph is adjusted in the step (3) and is about 9-11.
Dry run temperature is 60-70 DEG C in the step (3), (5), and drying time is 10-14h.
In the step (4), the sodium titanate of the certain mass, when back-pressure kettle product is 60mL, its quality is 0.0625-0.085g。
Certain reaction temperature is 180-220 DEG C in the step (4), and reaction a period of time is 22-26h.
Advantages of the present invention:
1st, the present invention can obtain a kind of quadrangular shape Detitanium-ore-type TiO2Powder body material, with high specific surface
Product catalysis activity.
2nd, cost of material used in the present invention is cheap, needs instrument and equipment and course of reaction simple.
3rd, can be by controlling efficiency factor so as to control reaction and crystal growth.
4th, the technical process of hydrothermal synthesis method is relatively simple, it is easy to accomplish, it is easy to control, whole preparation process
Nonhazardouss material is produced.
Description of the drawings
Fig. 1 is quadrangular shape Detitanium-ore-type TiO2SEM spectrograms
Specific embodiment
Embodiment 1
Sodium hydroxide 40g is weighed, is dissolved in water in beaker, stirred at once, after cooling, in proceeding to 100mL volumetric flasks Constant volume shakes up.40mL NaOH solutions are measured, 1g P25, ultrasonic 10min is added thereto to, 1h is stirred, is then proceeded to poly- four In the autoclave of fluorothene liner, under 120 DEG C of reaction temperature 24h is reacted.After the cooling of question response kettle, outwell inside liner Supernatant, is left white solid, adjusts its pH value and is about 10, is then centrifuged for separating, and washing is positioned in 60 DEG C of baking oven and is dried 12h, obtains sodium titanate.
Sodium titanate 0.0725g of gained is weighed, 40mL deionized waters are measured, ultrasonic 10min stirs 30min, proceeds to and carry In teflon-lined autoclave, under 200 DEG C of reaction temperature 24h is reacted.After the cooling of question response kettle, inside liner is outwelled The supernatant in face, is left white solid, is then centrifuged for separating, and washing is positioned in 60 DEG C of baking oven and is dried 12h, obtains four ribs Column Detitanium-ore-type TiO2
Embodiment 2
Sodium hydroxide 35g is weighed, is dissolved in water in beaker, stirred at once, after cooling, in proceeding to 100mL volumetric flasks Constant volume shakes up.40mL NaOH solutions are measured, 1g P25, ultrasonic 10min is added thereto to, 1h is stirred, is then proceeded to poly- four In the autoclave of fluorothene liner, under 120 DEG C of reaction temperature 24h is reacted.After the cooling of question response kettle, outwell inside liner Supernatant, is left white solid, adjusts its pH value and is about 10, is then centrifuged for separating, and washing is positioned in 60 DEG C of baking oven and is dried 12h, obtains sodium titanate.
Sodium titanate 0.065g of gained is weighed, 40mL deionized waters are measured, ultrasonic 10min stirs 30min, proceeds to and carry In teflon-lined autoclave, under 200 DEG C of reaction temperature 24h is reacted.After the cooling of question response kettle, inside liner is outwelled The supernatant in face, is left white solid, is then centrifuged for separating, and washing is positioned in 60 DEG C of baking oven and is dried 12h, obtains four ribs Column Detitanium-ore-type TiO2
Embodiment 3
Sodium hydroxide 40g is weighed, is dissolved in water in beaker, stirred at once, after cooling, in proceeding to 100mL volumetric flasks Constant volume shakes up.40mL NaOH solutions are measured, 1g P25, ultrasonic 10min is added thereto to, 1h is stirred, is then proceeded to poly- four In the autoclave of fluorothene liner, under 130 DEG C of reaction temperature 24h is reacted.After the cooling of question response kettle, outwell inside liner Supernatant, is left white solid, adjusts its pH value and is about 10, is then centrifuged for separating, and washing is positioned in 60 DEG C of baking oven and is dried 12h, obtains sodium titanate.
Sodium titanate 0.0725g of gained is weighed, 40mL deionized waters are measured, ultrasonic 10min stirs 30min, proceeds to and carry In teflon-lined autoclave, under 180 DEG C of reaction temperature 24h is reacted.After the cooling of question response kettle, inside liner is outwelled The supernatant in face, is left white solid, is then centrifuged for separating, and washing is positioned in 60 DEG C of baking oven and is dried 12h, obtains four ribs Column Detitanium-ore-type TiO2
Embodiment 4
Sodium hydroxide 38g is weighed, is dissolved in water in beaker, stirred at once, after cooling, in proceeding to 100mL volumetric flasks Constant volume shakes up.40mL NaOH solutions are measured, 1g P25, ultrasonic 10min is added thereto to, 1h is stirred, is then proceeded to poly- four In the autoclave of fluorothene liner, under 120 DEG C of reaction temperature 24h is reacted.After the cooling of question response kettle, outwell inside liner Supernatant, is left white solid, adjusts its pH value and is about 10, is then centrifuged for separating, and washing is positioned in 60 DEG C of baking oven and is dried 12h, obtains sodium titanate.
Sodium titanate 0.07g of gained is weighed, 40mL deionized waters are measured, ultrasonic 10min stirs 30min, proceeds to poly- In the autoclave of tetrafluoroethene liner, under 200 DEG C of reaction temperature 24h is reacted.After the cooling of question response kettle, liner the inside is outwelled Supernatant, be left white solid, be then centrifuged for separate, washing, be positioned in 60 DEG C of baking oven and be dried 12h, obtain quadrangular Shape Detitanium-ore-type TiO2
Embodiment 5
Sodium hydroxide 40g is weighed, is dissolved in water in beaker, stirred at once, after cooling, in proceeding to 100mL volumetric flasks Constant volume shakes up.40mL NaOH solutions are measured, 1g P25, ultrasonic 10min is added thereto to, 1h is stirred, is then proceeded to poly- four In the autoclave of fluorothene liner, under 120 DEG C of reaction temperature 24h is reacted.After the cooling of question response kettle, outwell inside liner Supernatant, is left white solid, adjusts its pH value and is about 10, is then centrifuged for separating, and washing is positioned in 60 DEG C of baking oven and is dried 12h, obtains sodium titanate.
Sodium titanate 0.075g of gained is weighed, 40mL deionized waters are measured, ultrasonic 10min stirs 30min, proceeds to and carry In teflon-lined autoclave, under 210 DEG C of reaction temperature 24h is reacted.After the cooling of question response kettle, inside liner is outwelled The supernatant in face, is left white solid, is then centrifuged for separating, and washing is positioned in 60 DEG C of baking oven and is dried 12h, obtains four ribs Column Detitanium-ore-type TiO2
Embodiment 6
Sodium hydroxide 44g is weighed, is dissolved in water in beaker, stirred at once, after cooling, in proceeding to 100mL volumetric flasks Constant volume shakes up.40mL NaOH solutions are measured, 1g P25, ultrasonic 10min is added thereto to, 1h is stirred, is then proceeded to poly- four In the autoclave of fluorothene liner, under 120 DEG C of reaction temperature 24h is reacted.After the cooling of question response kettle, outwell inside liner Supernatant, is left white solid, adjusts its pH value and is about 10, is then centrifuged for separating, and washing is positioned in 60 DEG C of baking oven and is dried 12h, obtains sodium titanate.
Sodium titanate 0.08g of gained is weighed, 40mL deionized waters are measured, ultrasonic 10min stirs 30min, proceeds to poly- In the autoclave of tetrafluoroethene liner, under 200 DEG C of reaction temperature 24h is reacted.After the cooling of question response kettle, liner the inside is outwelled Supernatant, be left white solid, be then centrifuged for separate, washing, be positioned in 60 DEG C of baking oven and be dried 12h, obtain quadrangular Shape Detitanium-ore-type TiO2

Claims (9)

1. a kind of preparation method of quadrangular shape anatase type tio2, it is characterised in that comprise the steps:
(1) solid NaOH is weighed, in being dissolved in deionized water, constant volume shakes up in volumetric flask, is configured to certain density NaOH molten Liquid.
(2) NaOH solution of certain volume is measured, the P25 of certain mass is weighed, is added and is carried teflon-lined high pressure In kettle, ultrasound a period of time, stirring a period of time, reaction a period of time under certain reaction temperature.
(3) room temperature is cooled to, obtains white precipitate, adjust pH value, be then centrifuged for separating, be dried, obtain sodium titanate.
(4) sodium titanate of certain mass is weighed, the deionized water of certain volume is measured, is added high with teflon-lined In pressure kettle, ultrasound a period of time, stirring a period of time, reaction a period of time under certain reaction temperature.
(5) after the completion of question response, room temperature is cooled to, obtains white precipitate, be then centrifuged for separating, be dried, obtain quadrangular shape sharp Titanium ore TiO2.
2. preparation method according to claim 1, it is characterised in that:In the step (1), the certain density NaOH Solution, its concentration is 8~12mol/L.
3. preparation method according to claim 1, it is characterised in that:In the step (2), the certain volume that measures NaOH solution, the P25 for weighing certain mass is that 1mL NaOH solutions add 0.0025~0.0035g P25.
4. preparation method according to claim 1, it is characterised in that:In the step (2), described hydrothermal temperature For 110~140 DEG C, the hydro-thermal reaction time is 22~26h.
5. preparation method according to claim 1, it is characterised in that:In the step (3), described regulation solution ph For 9~11.
6. preparation method according to claim 1, it is characterised in that:In the step (3), (5), described dry run Temperature is 60~70 DEG C, and drying time is 10~14h.
7. preparation method according to claim 1, it is characterised in that:It is described in the step (4) in the step (4) The sodium titanate of certain mass, when back-pressure kettle product is 60mL, its quality is 0.0625~0.085g.
8. preparation method according to claim 1, it is characterised in that:In the step (2), (4), one section of described ultrasound Time is 10~15min, and described stirring is for a period of time more than 1h.
9. preparation method according to claim 1, it is characterised in that:In the step (4), described hydrothermal temperature For 180~220 DEG C, the hydro-thermal reaction time is 22~26h.
CN201611013596.4A 2016-11-17 2016-11-17 Preparation method of quadrangular anatase type TiO2 Withdrawn CN106582591A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101190800A (en) * 2006-11-30 2008-06-04 中国科学院过程工程研究所 Method for preparing rutile-type titanium dioxide by hydrothermal method
CN102701275A (en) * 2012-06-01 2012-10-03 华北电力大学 Method for preparing TiO2 nano laces
CN103833076A (en) * 2012-11-27 2014-06-04 王泰林 Nickel oxide-titanium dioxide nano composite material
CN104192899A (en) * 2014-08-15 2014-12-10 李建明 Method for preparing TiO2 nanocrystal particles
CN104941617A (en) * 2015-06-16 2015-09-30 南昌航空大学 Titanium dioxide nanosheet grafted titanium dioxide nanorod heterojunction composite material

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101190800A (en) * 2006-11-30 2008-06-04 中国科学院过程工程研究所 Method for preparing rutile-type titanium dioxide by hydrothermal method
CN102701275A (en) * 2012-06-01 2012-10-03 华北电力大学 Method for preparing TiO2 nano laces
CN103833076A (en) * 2012-11-27 2014-06-04 王泰林 Nickel oxide-titanium dioxide nano composite material
CN104192899A (en) * 2014-08-15 2014-12-10 李建明 Method for preparing TiO2 nanocrystal particles
CN104941617A (en) * 2015-06-16 2015-09-30 南昌航空大学 Titanium dioxide nanosheet grafted titanium dioxide nanorod heterojunction composite material

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Application publication date: 20170426