Background technology
Utilize photocatalyst decomposing organic matter under rayed to become one of great research topic of polluting control, and obtained a series of progress.But the photocatalyst TiO that is most widely used
2Majority is to exist with form Powdered or the film attitude, but powder catalyst separates and the recovery difficulty, film attitude TiO
2The specific surface area of photocatalyst is low.Therefore, people wish that development structure is controlled, specific surface area is big, easily separated, TiO efficiently
2Photocatalyst.
In recent years, by the regulation and control nanometer material structure, the monodimension nanometer material of novelties such as assembling nanometer line, nanotube, nanometer rod becomes the focus of research.The orderly TiO of one dimension wherein
2Nano-wire array has excellent physical chemistry such as controllable structure, specific surface area are big, carrier mobility efficient height, demonstrates wide application prospect in photocatalysis field.Present TiO
2The preparation method of nano-array has on the high purity titanium sheet and prepares TiO
2The electrochemical oxidation process of nano-tube array utilizes porous anodic aluminium oxide (AAO) as template, in conjunction with sol-gel, electrochemical deposition, hydrolysis method, and the orderly TiO of the one dimension of preparation
2Nano wire or nano-tube array.But these methods need special equipment and instrument, and preparation technology is complicated.This patent has provided a kind of softening orderly rutile phase TiO of-hydrothermal method synthesizing one-dimensional that adopts
2The technology of nano-wire array.
Summary of the invention
In order to overcome the weak point in the existing photocatalyst technology of preparing, purpose provides the new Ti O that a kind of application art is simple, specific surface area is big, catalytic activity is high
2The synthetic method of nano-wire array photocatalyst.
The invention provides a kind of new Ti O
2There is orderly nano-wire array in the nano-wire array photocatalyst in photocatalyst, crystallization TiO
2Crystalline phase be rutile structure, the diameter of nano-wire array is about 100~300nm.
Photocatalyst outward appearance of the present invention is the canescence film, has good photocatalytic activity.
TiO with photocatalytic activity of the present invention
2The softening length of schooling Preparation Method of nano-wire array, concrete step is as follows:
(1) slide glass that will clean with ethanolic soln is put into ultrasonic washing instrument and is cleaned after several minutes, cleans up with deionized water again.
(2) take by weighing a certain amount of tetrabutyl titanate and titanium tetrachloride respectively according to stoichiometric ratio, and it is dissolved in respectively in a certain amount of toluene solution;
(3) slide glass that cleans up is put into stainless steel, in the closed reactor of white polytetrafluoroethylpipe liner, and add a certain amount of hydrochloric acid.
(4), slowly add a certain amount of toluene, tetrabutyl titanate and titanium tetrachloride solution with the glass stick drainage.
(5) reactor is put into loft drier and heat-treat, temperature of reaction is 130~180 ℃, and the reaction times is 6~22h.
(6) at room temperature with the reactor naturally cooling, outwell the TiO that solution can obtain generating on slide glass
2Nano-wire array.
The beneficial effect of the technology of the present invention is new Ti O
2Preparation technology's temperature of reaction of nano-wire array photocatalyst is low, technology is simple to operation, need not high-temperature heat treatment, cost reduces, gained photocatalyst specific surface area is big, photocatalytic activity is high.Characterize the back after tested and find, adopt the TiO of this method preparation
2The nano-wire array photocatalyst, the degree of crystallinity height, specific surface area is big.The photochemical catalysis experimental result shows: the 50ml concentration that contains the 0.15g photocatalyst be the percent of decolourization of tropeolin-D under the 250W high voltage mercury lamp radiation of 20mg/L behind 1h near 100%, the result shows the TiO that adopts softening-Hydrothermal Preparation
2The nano-wire array photocatalyst has good photocatalytic activity.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1:
The slide glass that will clean with ethanolic soln is put into ultrasonic washing instrument and is cleaned after several minutes, cleans up with deionized water again.Putting it into inside is equipped with in the sealed reactor of poly-tetrafluoro hexene liner standby.With toluene is solvent, and configuration concentration is the tetrabutyl titanate solution of 1mol/L and the titanium tetrachloride solution of 1mon/L respectively.With the glass stick drainage, slowly add a certain amount of concentrated hydrochloric acid, toluene, tetrabutyl titanate solution and titanium tetrachloride solution are in reactor, and making its volume ratio is 1: 10: 1: 1.Again reactor is placed on temperature and is in 180 ℃ the baking oven, behind the 22h with its taking-up.Treat after its cooling the slide glass of bottom to be taken out, on slide glass, will obtain TiO
2The nanometer linear array.
Embodiment 2:
The slide glass that will clean with ethanolic soln is put into ultrasonic washing instrument and is cleaned after several minutes, cleans up with deionized water again.Putting it into inside is equipped with in the sealed reactor of poly-tetrafluoro hexene liner standby.With toluene is solvent, and configuration concentration is the tetrabutyl titanate solution of 1mon/L and the titanium tetrachloride solution of 1mon/L respectively.With the glass stick drainage, slowly add a certain amount of concentrated hydrochloric acid, toluene, tetrabutyl titanate solution and titanium tetrachloride solution are in reactor, and making its volume ratio is 1: 10: 1: 1.Again reactor is placed on temperature and is in 180 ℃ the baking oven, behind the 14h with its taking-up.Treat after its cooling the slide glass of bottom to be taken out, on slide glass, will obtain TiO
2The nanometer linear array.
Embodiment 3:
The slide glass that will clean with ethanolic soln is put into ultrasonic washing instrument and is cleaned after several minutes, cleans up with deionized water again.Putting it into inside is equipped with in the sealed reactor of poly-tetrafluoro hexene liner standby.With toluene is solvent, and configuration concentration is the tetrabutyl titanate solution of 1mon/L and the titanium tetrachloride solution of 1mon/L respectively.With the glass stick drainage, slowly add a certain amount of concentrated hydrochloric acid, toluene, tetrabutyl titanate solution and titanium tetrachloride solution are in reactor, and making its volume ratio is 1: 10: 1: 1.Again reactor is placed on temperature and is in 180 ℃ the baking oven, behind the 6h with its taking-up.Treat after its cooling the slide glass of bottom to be taken out, on slide glass, will obtain TiO
2The nanometer linear array.
Example 4:
The slide glass that will clean with ethanolic soln is put into ultrasonic washing instrument and is cleaned after several minutes, cleans up with deionized water again.Putting it into inside is equipped with in the sealed reactor of poly-tetrafluoro hexene liner standby.With toluene is solvent, and configuration concentration is the tetrabutyl titanate solution of 1mon/L and the titanium tetrachloride solution of 1mon/L respectively.With the glass stick drainage, slowly add a certain amount of concentrated hydrochloric acid, toluene, tetrabutyl titanate solution and titanium tetrachloride solution are in reactor, and making its volume ratio is 1: 10: 1: 1.Again reactor is placed on temperature and is in 150 ℃ the baking oven, behind the 22h with its taking-up.Treat after its cooling the slide glass of bottom to be taken out, on slide glass, will obtain TiO
2The nanometer linear array.
Embodiment 5:
The slide glass that will clean with ethanolic soln is put into ultrasonic washing instrument and is cleaned after several minutes, cleans up with deionized water again.Putting it into inside is equipped with in the sealed reactor of poly-tetrafluoro hexene liner standby.With toluene is solvent, and configuration concentration is the tetrabutyl titanate solution of 1mon/L and the titanium tetrachloride solution of 1mon/L respectively.With the glass stick drainage, slowly add a certain amount of concentrated hydrochloric acid, toluene, tetrabutyl titanate solution and titanium tetrachloride solution are in reactor, and making its volume ratio is 1: 10: 1: 1.Again reactor is placed on temperature and is in 150 ℃ the baking oven, behind the 14h with its taking-up.Treat after its cooling the slide glass of bottom to be taken out, on slide glass, will obtain TiO
2The nanometer linear array.
Embodiment 6:
The slide glass that will clean with ethanolic soln is put into ultrasonic washing instrument and is cleaned after several minutes, cleans up with deionized water again.Putting it into inside is equipped with in the sealed reactor of poly-tetrafluoro hexene liner standby.With toluene is solvent, and configuration concentration is the tetrabutyl titanate solution of 1mon/L and the titanium tetrachloride solution of 1mon/L respectively.With the glass stick drainage, slowly add a certain amount of concentrated hydrochloric acid, toluene, tetrabutyl titanate solution and titanium tetrachloride solution in reactor,, making its volume ratio is 1: 10: 1: 1.Again reactor is placed on temperature and is in 150 ℃ the baking oven, behind the 6h with its taking-up.Treat after its cooling the slide glass of bottom to be taken out, on slide glass, will obtain TiO
2The nanometer linear array.
Example 7:
The slide glass that will clean with ethanolic soln is put into ultrasonic washing instrument and is cleaned after several minutes, cleans up with deionized water again.Putting it into inside is equipped with in the sealed reactor of poly-tetrafluoro hexene liner standby.With toluene is solvent, and configuration concentration is the tetrabutyl titanate solution of 1mon/L and the titanium tetrachloride solution of 1mon/L respectively.With the glass stick drainage, slowly add a certain amount of concentrated hydrochloric acid, toluene, tetrabutyl titanate solution and titanium tetrachloride solution are in reactor, and making its volume ratio is 1: 10: 1: 1.Again reactor is placed on temperature and is in 130 ℃ the baking oven, behind the 22h with its taking-up.Treat after its cooling the slide glass of bottom to be taken out, on slide glass, will obtain TiO
2The nanometer linear array.
Embodiment 8:
The slide glass that will clean with ethanolic soln is put into ultrasonic washing instrument and is cleaned after several minutes, cleans up with deionized water again.Putting it into inside is equipped with in the sealed reactor of poly-tetrafluoro hexene liner standby.With toluene is solvent, and configuration concentration is the tetrabutyl titanate solution of 1mon/L and the titanium tetrachloride solution of 1mon/L respectively.With the glass stick drainage, slowly add a certain amount of concentrated hydrochloric acid, toluene, tetrabutyl titanate solution and titanium tetrachloride solution are in reactor, and making its volume ratio is 1: 10: 1: 1.Again reactor is placed on temperature and is in 130 ℃ the baking oven, behind the 14h with its taking-up.Treat after its cooling the slide glass of bottom to be taken out, on slide glass, will obtain TiO
2The nanometer linear array.
Embodiment 9:
The slide glass that will clean with ethanolic soln is put into ultrasonic washing instrument and is cleaned after several minutes, cleans up with deionized water again.Putting it into inside is equipped with in the sealed reactor of poly-tetrafluoro hexene liner standby.With toluene is solvent, and configuration concentration is the tetrabutyl titanate solution of 1mon/L and the titanium tetrachloride solution of 1mon/L respectively.With the glass stick drainage, slowly add a certain amount of concentrated hydrochloric acid, toluene, tetrabutyl titanate solution and titanium tetrachloride solution are in reactor, and making its volume ratio is 1: 10: 1: 1.Again reactor is placed on temperature and is in 130 ℃ the baking oven, behind the 6h with its taking-up.Treat after its cooling the slide glass of bottom to be taken out, on slide glass, will obtain TiO
2The nanometer linear array.
The present invention open with disclose contain rutile new Ti O mutually
2Nano-wire array photocatalyst and softening-hydrothermal preparing process thereof can be by using for reference this paper disclosure, although the present invention is described by preferred embodiment, but those skilled in the art obviously can change content described herein in not breaking away from content of the present invention, spirit and scope, or increase and decrease some condition, in particular, replacement that all are similar and change are conspicuous to those skilled in the art, and they are regarded as being included in spirit of the present invention, scope and the content.