CN100347090C - Synthesis of TiO2 nanometer particles and bars - Google Patents

Synthesis of TiO2 nanometer particles and bars Download PDF

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CN100347090C
CN100347090C CNB2006100021465A CN200610002146A CN100347090C CN 100347090 C CN100347090 C CN 100347090C CN B2006100021465 A CNB2006100021465 A CN B2006100021465A CN 200610002146 A CN200610002146 A CN 200610002146A CN 100347090 C CN100347090 C CN 100347090C
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nano particle
titanate
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CN1817799A (en
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李亚栋
李晓林
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Tsinghua University
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Abstract

The present invention provides a method for synthesizing TiO2 nanometer particles and nanometer rods, which relates to technology for preparing nanometer material. The method is characterized in that organic titanate and long-chain organic carboxylic acid or NH4HCO3 are used as raw materials in hot solvent, organic amine is used as a mineralizing agent, and organic substances with a low boiling point are used as solvent; the materials are put into a closed reactor to react at 100 to 200 DEG C to synthesize TiO2 nanometer particles and nanometer rods with the advantages of high crystal degree, uniform dimension and redispersion capacity of organic solvent. Other metallic ions can also be doped in a reaction system to form metal doped nanometer TiO2 nanometer particles or nanometer rods. The method has the advantages of easy acquirement and low cost of raw materials, simple device, easy control, favorable technological repetitiveness, stable product quantity and safe and reliable operation. The method provides a necessary structural unit for functional materials of battery electrodes, catalysts, diluted magnetic semiconductors, etc. and can be used in the fields of photocatalysis, optical hydrolysis, solar batteries, spinning electronics, etc.

Description

A kind of TiO 2The synthetic method of nano particle and nanometer rod
Technical field
The present invention relates to a kind of high-crystallinity, size is even, organic solvent is redispersible TiO 2Synthetic and the inner processing method of mixing (comprising iron, cobalt, nickel, manganese, tin) of nano particle and nanometer rod belongs to the inorganic material preparation process technical field.
Background technology
TiO 2Be a kind of important semiconductor material, have special physicochemical character, be with a wide range of applications in fields such as battery, photochemical catalysis, photodissociation water, organism photodegradation and electrochromic windows.With TiO 2For the technology on basis may provide a kind of method for the solution of some most critical issues in the human development (as environmental purification, sun power utilization and life science etc.).Up to the present, the method for traditional synthetic method and bibliographical information all be difficult to obtain high-crystallinity, size all even in organic solvent redispersible TiO 2Nano particle and nanometer rod, thus can't further be assembled into high-quality TiO 2Film makes TiO 2Further industrial application is restricted to a certain extent.Such as, 2003 15 volumes of Germany " advanced material " (Advanccd Materials) have been reported with template for 1205 pages and have been prepared TiO 2Colloidal spheres; 12384 pages of U.S.'s " JACS " (Journal of theAmerican Chemical Society) 2003 125 volumes have been reported Hydrothermal Preparation TiO 2Nanotube; 2003 15 volumes of Germany " advanced material " (Advanced Materials) have reported that the collosol and gel electrophoretic deposition has prepared TiO for 427 pages 2Nanometer rod, this method complex operation, equipment complexity.Other method also has flame oxidation method and solution reaction legal system to be equipped with TiO 2Particle utilizes electrochemical deposition to prepare TiO 2Film.
Summary of the invention
The object of the present invention is to provide a kind of TiO 2Synthetic and the adulterated processing method of internal metal ion of nano particle and nanometer rod.This method is simple to operate, can utilize identical or essentially identical technology under lower temperature and pressure condition, adopts raw material cheap and easy to get, synthetic high-crystallinity, the TiO that size is even, organic solvent is redispersible 2Nano particle and nanometer rod and the adulterated TiO of multiple internal metal ion 2Nano particle and nanometer rod, thus required series structure unit provided for the assembling of functional materialss such as battery electrode, catalyzer and dilute magnetic semiconductor.
Technical scheme of the present invention is as follows:
A kind of TiO 2The synthetic method of nano particle is characterized in that this method carries out as follows:
1) with the NH of 0.5～2g 4HCO 3, the organic amine mineralizer of long-chain organic carboxyl acid, 1～5mL of 1～25mL and 5～15mL low boiling point organic solvent at room temperature mixed, and stir;
2) organic titanate with 1～5mL is added drop-wise in the reaction system of step 1) slowly, the formation mixing solutions that stirs is transferred to mixing solutions in the water heating kettle then, in the reaction 12～48 hours down of 100～200 ℃ of temperature condition, cool to room temperature promptly synthesizes described TiO then 2Nano particle.
In above-mentioned steps 1) in reaction system in add one or more metal soluble salt account for mixing solutions quality 1%～5%, described metal soluble salt is the soluble salt of iron, cobalt, nickel, manganese or tin, promptly synthetic metal-doped TiO 2Nano particle.
Organic titanate of the present invention is any of tetrabutyl titanate, titanium isopropylate or tetraethyl titanate; Described long-chain organic carboxyl acid is any of linolic acid, laurostearic acid or capric acid; Described organic amine mineralizer is any in triethylamine, tripropyl amine or the amino dodecane; Described low boiling point organic solvent is any in hexanaphthene, hexane or the chloroform.
The present invention also provides a kind of TiO 2The synthetic method of nanometer rod is characterized in that this method carries out as follows:
1) the long-chain organic carboxyl acid of 1～25mL, the organic amine mineralizer of 1～5mL and the low boiling point organic solvent of 5～15mL are at room temperature mixed, and stir;
2) organic titanate with 1～5mL is added drop-wise in the reaction system of step 1) slowly, the formation mixing solutions that stirs is transferred to mixing solutions in the water heating kettle then, in the reaction 12～48 hours down of 100～200 ℃ of temperature condition, cool to room temperature promptly synthesizes described TiO then 2Nanometer rod.
At TiO of the present invention 2In the synthetic method of nanometer rod, in the reaction system of described step 1), add one or more metal soluble salt that account for mixing solutions quality 1%～5%, described metal soluble salt is the soluble salt of iron, cobalt, nickel, manganese or tin, promptly synthetic metal-doped TiO 2Nanometer rod.Described organic titanate is any of tetrabutyl titanate, titanium isopropylate or tetraethyl titanate; Described long-chain organic carboxyl acid is any of linolic acid, laurostearic acid or capric acid; Described organic amine mineralizer is any in triethylamine, tripropyl amine or the amino dodecane; Described low boiling point organic solvent is any in hexanaphthene, hexane or the chloroform.
The present invention compared with prior art has the following advantages and beneficial effect: the invention provides a kind of simple and effective preparation high-crystallinity, size is even, organic solvent is redispersible TiO 2The synthetic method of nano particle and nanometer rod has overcome the synthetic TiO of existing method 2Semiconductor material needs high temperature, and product degree of crystallinity is poor, and particle size is inhomogeneous, and is dispersed bad, problems such as complex process; This synthetic method temperature of reaction is lower, and equipment is simple, and raw material is cheap and easy to get, is easy to realize control, good process repeatability, and constant product quality, operational safety is reliable; By the interior metal doping treatment, can synthesize multiple metal-doped TiO in a large number 2Nano particle and nanometer rod.Thereby for the assembling of functional materialss such as battery electrode, catalyzer and dilute magnetic semiconductor provides required series structure unit.
Description of drawings
Fig. 1 is the TiO that makes under 150 ℃ of temperature of reaction 2The x-ray diffractogram of powder of nano particle and nanometer rod.
Fig. 2 a, 2b, 2c are the TiO that makes under 150 ℃ of the temperature 2The different amplification transmission electron microscope photo of nano particle.
Fig. 3 a, 3b, 3c are the TiO that makes under 150 ℃ of the temperature 2The different amplification transmission electron microscope photo of nanometer rod.
Fig. 4 a, 4b are the 2%Sn that makes under 150 ℃ of the temperature 4+Adulterated TiO 2The different amplification transmission electron microscope photo of nanometer rod; Fig. 4 c is the 2%Sn that makes under 150 ℃ 4+Adulterated TiO 2The x ray energy spectrum of nanometer rod.
Embodiment
The present invention is under the solvent thermal condition, with organic titanate and long-chain organic carboxyl acid or NH 4HCO 3Being raw material, is mineralizer with the organic amine, makees solvent in closed reactor with low-boiling-point organic compound, in 100～200 ℃ of temperature condition down synthetic high-crystallinity of reaction, size is even, organic solvent is redispersible TiO 2Nano particle and nanometer rod, the processing by before reacting can realize TiO 2The metal ion mixing of nano particle and nanometer rod further describes reaction mechanism of the present invention and embodiment below.
(1) TiO 2The synthetic method of nano particle and nanometer rod is under the solvent thermal condition, with organic titanate and long-chain organic carboxyl acid or NH 4HCO 3Being raw material, is mineralizer with the organic amine, makees solvent with low-boiling-point organic compound and react synthetic high-crystallinity, size is even, organic solvent is redispersible TiO in closed reactor 2Nano particle and nanometer rod.
This reaction can be expressed as: Ti (OR) 4+ R ' COOH+ organic amine → TiO 2Or
Ti (OR) 4+ NH 4HCO 3+ R ' COOH+ organic amine → TiO 2
(2) TiO of metal ion mixing 2The synthetic method of nano particle and nanometer rod is under the solvent thermal condition, with organic titanate and long-chain organic carboxyl acid or NH 4HCO 3Being raw material, is mineralizer with the organic amine, makees solvent with low-boiling-point organic compound, adds the soluble salt of the metal (comprising iron, cobalt, nickel, manganese, tin) of other kind before reaction, by reacting the TiO of synthetic metal ion mixing 2Nano particle and nanometer rod.
This reaction table is shown: Ti (OR) 4+ NH 4HCO 3+ R ' COOH+ organic amine+Sn 4+→ TiO 2-Sn 4+(dopant material)
Ti (OR) 4+ NH 4HCO 3+ R ' COOH+ organic amine+Fe 3+→ TiO 2-Fe 3+(dopant material)
Ti (OR) 4+ NH 4HCO 3+ R ' COOH+ organic amine+Co 2+→ TiO 2-Co 2+(dopant material)
Ti (OR) 4+ NH 4HCO 3+ R ' COOH+ organic amine+Ni 2+→ TiO 2-Ni 2+(dopant material)
More than various in Ti (OR) 4Represent organic titanate (as tetrabutyl titanate, titanium isopropylate), R ' COOH represents the long-chain organic carboxyl acid, and organic amine refers to triethylamine etc.
Will be further understood that the present invention by the following examples.
Embodiment 1:
At typical TiO 2In the building-up process of nano particle, with NH 4HCO 3(1g), linolic acid (LA, about 25mL), triethylamine (5mL) and hexanaphthene (5mL) are at room temperature evenly mixed with induction stirring, then with Ti (OBu) 4(1mL) be added drop-wise in the solution slowly.At room temperature further stir and make system evenly mixed, then solution is transferred in the stainless steel hydro-thermal still of Teflon (Te Fulong) inner bag, obtain high-crystallinity, size is even, organic solvent is redispersible TiO at 150 ℃ of stoichiometric numbers hour 2Nano particle.
At typical TiO 2In the building-up process of nanometer rod, with linolic acid (LA, about 7mL), triethylamine (5mL) and hexanaphthene (15mL) are at room temperature evenly mixed with induction stirring, with Ti (OBu) 4(1mL) be added drop-wise in the solution slowly.At room temperature electromagnetism further stirs and makes system evenly mixed, then solution is transferred in the stainless steel hydro-thermal still of Teflon (Te Fulong) inner bag 150 ℃ of reactions 2 days, obtains high-crystallinity, size is even, organic solvent is redispersible TiO 2Nanometer rod.
Under same condition, tetrabutyl titanate is changed into organic titanates such as titanium isopropylate, change linolic acid into laurostearic acid, long chain organic acids such as capric acid, triethylamine is changed into organic amines such as amino dodecane, hexanaphthene is changed into low boiling point organic solvents such as hexane, temperature of reaction is controlled at 100,150,200 ℃ respectively, linoleic amount is controlled between 5mL～25mL, to the reaction times be adjusted into 48,32,16,12 hours, with NH 4HCO 3Amount be controlled between 0.5～2g, all can obtain TiO 2Nano particle and nanometer rod.
Embodiment 2:
At typical TiO 2In the building-up process of nano particle, with NH 4HCO 3(0.5g), linolic acid (LA, about 10mL), triethylamine (1mL) and hexanaphthene (10mL) are at room temperature evenly mixed with induction stirring.SnCl with 2% 45H 2O joins in the reaction system.Then with Ti (OBu) 4(2mL) be added drop-wise in the solution slowly.At room temperature further stir and make system evenly mixed, then solution is transferred in the stainless steel hydro-thermal still of Teflon (Te Fulong) inner bag at 180 ℃ of stoichiometric numbers hour.
Under same condition, tetrabutyl titanate is changed into organic titanates such as titanium isopropylate, change linolic acid into laurostearic acid, long chain organic acids such as capric acid, triethylamine is changed into organic amines such as amino dodecane, hexanaphthene is changed into low boiling point organic solvents such as hexane, temperature of reaction is controlled at 100,150,200 ℃ respectively, linoleic amount is controlled between 5mL～25mL, to the reaction times be adjusted into 48,32,16,12 hours, with NH 4HCO 3Amount be controlled at and all can obtain the adulterated high-crystallinity of Sn, size is even, organic solvent is redispersible TiO between 0.5～2g 2Nano particle.
Embodiment 3:
At typical TiO 2In the building-up process of nano particle, with NH 4HCO 3(2g), linolic acid (LA, about 5mL), triethylamine (3mL) and hexanaphthene (5mL) are at room temperature evenly mixed with induction stirring.FeCl with 1% 3Join in the reaction system.Then with Ti (OBu) 4(5mL) be added drop-wise in the solution slowly.At room temperature further stir and make system evenly mixed, then solution is transferred in the stainless steel hydro-thermal still of Teflon inner bag at 100 ℃ of stoichiometric numbers hour.
Under same condition, tetrabutyl titanate is changed into organic titanates such as titanium isopropylate, change linolic acid into laurostearic acid, long chain organic acids such as capric acid, triethylamine is changed into organic amines such as amino dodecane, hexanaphthene is changed into low boiling point organic solvents such as hexane, temperature of reaction is controlled at 100,150,200 ℃ respectively, linoleic amount is controlled between 5mL～25mL, to the reaction times be adjusted into 48,32,16,12 hours, with NH 4HCO 3Amount be controlled at and all can obtain the adulterated high-crystallinity of Fe, size is even, organic solvent is redispersible TiO between 0.5～2g 2Nano particle.
Embodiment 4:
At typical TiO 2In the building-up process of nano particle, with NH 4HCO 3(0.5g), linolic acid (LA, about 20mL), triethylamine (4mL) and hexanaphthene (10mL) are at room temperature evenly mixed with induction stirring.CoCl with 2% 26H 2O joins in the reaction system.Then with Ti (OBu) 4(4mL) be added drop-wise in the solution slowly.At room temperature further stir and make system evenly mixed, then solution is transferred in the stainless steel hydro-thermal still of Teflon inner bag 120 ℃ of reactions five hours.
Under same condition, tetrabutyl titanate is changed into organic titanates such as titanium isopropylate, change linolic acid into laurostearic acid, long chain organic acids such as capric acid, triethylamine is changed into organic amines such as amino dodecane, hexanaphthene is changed into low boiling point organic solvents such as hexane, temperature of reaction is controlled at 100,150,200 ℃ respectively, linoleic amount is controlled between 5mL～25mL, to the reaction times be adjusted into 48,32,16,12 hours, with NH 4HCO 3Amount be controlled at and all can obtain the adulterated high-crystallinity of Co, size is even, organic solvent is redispersible TiO between 0.5～2g 2Nano particle.
Embodiment 5:
At typical TiO 2In the building-up process of nano particle, with NH 4HCO 3(1.5g), linolic acid (LA, about 8mL), triethylamine (8mL) and hexanaphthene (15mL) are at room temperature evenly mixed with induction stirring.NiCl with 3% 26H 2O joins in the reaction system.Then with Ti (OBu) 4(1mL) be added drop-wise in the solution slowly.At room temperature further stir and make system evenly mixed, then solution is transferred in the stainless steel hydro-thermal still of Teflon inner bag at 180 ℃ of stoichiometric numbers hour.
Under same condition, tetrabutyl titanate is changed into organic titanates such as titanium isopropylate, change linolic acid into laurostearic acid, long chain organic acids such as capric acid, triethylamine is changed into organic amines such as amino dodecane, hexanaphthene is changed into low boiling point organic solvents such as hexane, temperature of reaction is controlled at 100,150,200 ℃ respectively, linoleic amount is controlled between 5mL～25mL, to the reaction times be adjusted into 48,32,16,12 hours, with NH 4HCO 3Amount be controlled at and all can obtain the adulterated high-crystallinity of Ni, size is even, organic solvent is redispersible TiO between 0.5～2g 2Nano particle.
Embodiment 6:
At typical TiO 2In the building-up process of nano particle, with NH 4HCO 3(0.5g), linolic acid (LA, about 5mL), triethylamine (1mL) and hexanaphthene (5mL) are at room temperature evenly mixed with induction stirring.MnCl with 5% 24H 2O joins in the reaction system.Then with Ti (OBu) 4(1mL) be added drop-wise in the solution slowly.At room temperature further stir and make system evenly mixed, then solution is transferred in the stainless steel hydro-thermal still of Teflon inner bag at 150 ℃ of stoichiometric numbers hour.
Under same condition, tetrabutyl titanate is changed into organic titanates such as titanium isopropylate, change linolic acid into laurostearic acid, long chain organic acids such as capric acid, triethylamine is changed into organic amines such as amino dodecane, hexanaphthene is changed into low boiling point organic solvents such as hexane, temperature of reaction is controlled at 100,150,200 ℃ respectively, linoleic amount is controlled between 5mL～25mL, to the reaction times be adjusted into 48,32,16,12 hours, with NH 4HCO 3Amount be controlled at and all can obtain the adulterated high-crystallinity of Mn, size is even, organic solvent is redispersible TiO between 0.5～2g 2Nano particle.
Embodiment 7:
At typical TiO 2In the building-up process of nanometer rod, with linolic acid (LA, about 25mL), triethylamine (5mL) and hexanaphthene (15mL) are at room temperature evenly mixed with induction stirring.FeCl with 5% 3Join in the reaction system.Then with Ti (OBu) 4(5mL) be added drop-wise in the solution slowly.At room temperature further stir and make system evenly mixed, then solution is transferred in the stainless steel hydro-thermal still of Teflon inner bag at 200 ℃ of stoichiometric numbers hour.
Under same condition, tetrabutyl titanate is changed into organic titanates such as titanium isopropylate, change linolic acid into laurostearic acid, long chain organic acids such as capric acid, triethylamine is changed into organic amines such as amino dodecane, hexanaphthene is changed into low boiling point organic solvents such as hexane, temperature of reaction is controlled at 100,150,200 ℃ respectively, linoleic amount is controlled between 5mL～25mL, to the reaction times be adjusted into 48,32,16,12 hours, with NH 4HCO 3Amount be controlled at and all can obtain the adulterated high-crystallinity of Fe, size is even, organic solvent is redispersible TiO between 0.5～2g 2Nanometer rod.
Embodiment 8:
At typical TiO 2In the building-up process of nanometer rod, with linolic acid (LA, about 1mL), triethylamine (1mL) and hexanaphthene (5mL) are at room temperature evenly mixed with induction stirring.CoCl with 2% 26H 2O joins in the reaction system.Then with Ti (OBu) 4(1mL) be added drop-wise in the solution slowly.At room temperature further stir and make system evenly mixed, then solution is transferred in the stainless steel hydro-thermal still of Teflon inner bag at 100 ℃ of stoichiometric numbers hour.
Under same condition, tetrabutyl titanate is changed into organic titanates such as titanium isopropylate, change linolic acid into laurostearic acid, long chain organic acids such as capric acid, triethylamine is changed into organic amines such as amino dodecane, hexanaphthene is changed into low boiling point organic solvents such as hexane, temperature of reaction is controlled at 100,150,200 ℃ respectively, linoleic amount is controlled between 5mL～25mL, to the reaction times be adjusted into 48,32,16,12 hours, with NH 4HCO 3Amount be controlled at and all can obtain the adulterated high-crystallinity of Co, size is even, organic solvent is redispersible TiO between 0.5～2g 2Nanometer rod.
Embodiment 9:
At typical TiO 2In the building-up process of nanometer rod, with linolic acid (LA, about 20mL), triethylamine (4mL) and hexanaphthene (10mL) are at room temperature evenly mixed with induction stirring.NiCl with 5% 26H 2O joins in the reaction system.Then with Ti (OBu) 4(4mL) be added drop-wise in the solution slowly.At room temperature further stir and make system evenly mixed, then solution is transferred in the stainless steel hydro-thermal still of Teflon inner bag at 180 ℃ of stoichiometric numbers hour.
Under same condition, tetrabutyl titanate is changed into organic titanates such as titanium isopropylate, change linolic acid into laurostearic acid, long chain organic acids such as capric acid, triethylamine is changed into organic amines such as amino dodecane, hexanaphthene is changed into low boiling point organic solvents such as hexane, temperature of reaction is controlled at 100,150,200 ℃ respectively, linoleic amount is controlled between 5mL～25mL, to the reaction times be adjusted into 48,32,16,12 hours, with NH 4HCO 3Amount be controlled at and all can obtain the adulterated high-crystallinity of Ni, size is even, organic solvent is redispersible TiO between 0.5～2g 2Nanometer rod.
Embodiment 10:
At typical TiO 2In the building-up process of nanometer rod, with linolic acid (LA, about 25mL), triethylamine (15mL) and hexanaphthene (15mL) are at room temperature evenly mixed with induction stirring.MnCl with 3% 24H 2O joins in the reaction system.Then with Ti (OBu) 4(4mL) be added drop-wise in the solution slowly.At room temperature further stir and make system evenly mixed, then solution is transferred in the stainless steel hydro-thermal still of Teflon inner bag at 180 ℃ of stoichiometric numbers hour.
Under same condition, tetrabutyl titanate is changed into organic titanates such as titanium isopropylate, change linolic acid into laurostearic acid, long chain organic acids such as capric acid, triethylamine is changed into organic amines such as amino dodecane, hexanaphthene is changed into low boiling point organic solvents such as hexane, temperature of reaction is controlled at 100,150,200 ℃ respectively, linoleic amount is controlled between 5mL～25mL, to the reaction times be adjusted into 48,32,16,12 hours, with NH 4HCO 3Amount be controlled at and all can obtain the adulterated high-crystallinity of Mn, size is even, organic solvent is redispersible TiO between 0.5～2g 2Nanometer rod.

Claims (6)

1. TiO 2The synthetic method of nano particle is characterized in that this method carries out as follows:
1) with the NH of 0.5～2g 4HCO 3, the organic amine mineralizer of long-chain organic carboxyl acid, 1～5mL of 1～25mL and 5～15mL low boiling point organic solvent at room temperature mixed, and stir; Described long-chain organic carboxyl acid is any of linolic acid, laurostearic acid or capric acid; Described organic amine mineralizer is any in triethylamine, tripropyl amine or the amino dodecane; Described low boiling point organic solvent is any in hexanaphthene, hexane or the chloroform;
2) organic titanate with 1～5mL is added drop-wise in the reaction system of step 1) slowly, the formation mixing solutions that stirs is transferred to mixing solutions in the water heating kettle then, in the reaction 12～48 hours down of 100～200 ℃ of temperature condition, cool to room temperature promptly synthesizes described TiO then 2Nano particle.
2. according to the described TiO of claim 1 2Nano particle synthesizing process, it is characterized in that: add one or more metal soluble salt that account for mixing solutions quality 1%～5% in the reaction system in described step 1), described metal soluble salt is the soluble salt of iron, cobalt, nickel, manganese or tin, promptly synthetic metal-doped TiO 2Nano particle.
3. according to claim 1 or 2 described TiO 2Nano particle synthesizing process is characterized in that: described organic titanate is any of tetrabutyl titanate, titanium isopropylate or tetraethyl titanate.
4. TiO 2The synthetic method of nanometer rod is characterized in that this method carries out as follows:
1) the long-chain organic carboxyl acid of 1～25mL, the organic amine mineralizer of 1～5mL and the low boiling point organic solvent of 5～15mL are at room temperature mixed, and stir; Described long-chain organic carboxyl acid is any of linolic acid, laurostearic acid or capric acid; Described organic amine mineralizer is any in triethylamine, tripropyl amine or the amino dodecane; Described low boiling point organic solvent is any in hexanaphthene, hexane or the chloroform;
2) organic titanate with 1～5mL is added drop-wise in the reaction system of step 1) slowly, the formation mixing solutions that stirs is transferred to mixing solutions in the water heating kettle then, in the reaction 12～48 hours down of 100～200 ℃ of temperature condition, cool to room temperature promptly synthesizes described TiO then 2Nanometer rod.
5. according to the described TiO of claim 4 2The nanometer rod synthetic method, it is characterized in that: in the reaction system of described step 1), add one or more metal soluble salt that account for mixing solutions quality 1%～5%, described metal soluble salt is the soluble salt of iron, cobalt, nickel, manganese or tin, promptly synthetic metal-doped TiO 2Nanometer rod.
6. according to claim 4 or 5 described TiO 2The nanometer rod synthetic method is characterized in that: described organic titanate is any of tetrabutyl titanate, titanium isopropylate or tetraethyl titanate.
CNB2006100021465A 2006-01-19 2006-01-19 Synthesis of TiO2 nanometer particles and bars Expired - Fee Related CN100347090C (en)

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CN106281283A (en) * 2016-08-16 2017-01-04 梅庆波 A kind of long-acting preparation method stablizing microcapsule oil displacement agent
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CN109180048B (en) * 2018-10-30 2021-12-17 江苏苏博特新材料股份有限公司 Nano precursor medium transmission inhibitor and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1524793A (en) * 2003-09-17 2004-09-01 上海工程技术大学 Process for preparing nanometer titanium dioxide
JP2005075662A (en) * 2003-08-29 2005-03-24 Kyoto Univ Titania nanocrystallite aggregate, manufacture method therefor, and photocatalyst
CN1636880A (en) * 2004-12-09 2005-07-13 江苏大学 Prepn process of anatase nanometer TiO2 powder

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005075662A (en) * 2003-08-29 2005-03-24 Kyoto Univ Titania nanocrystallite aggregate, manufacture method therefor, and photocatalyst
CN1524793A (en) * 2003-09-17 2004-09-01 上海工程技术大学 Process for preparing nanometer titanium dioxide
CN1636880A (en) * 2004-12-09 2005-07-13 江苏大学 Prepn process of anatase nanometer TiO2 powder

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