CN100425338C - Method for preparing photocatalyst of Nano titanium dichloride through acidolysis of dinbutyl phthalate titanic acid by chloroactic acid - Google Patents

Abstract

A process for preparing nano-TiO2 photocatalyst by acidifying the butyl titanate by chloroacetic acid includes such steps as installing stirrer, condenser and thermometer to a three-mouth bottle, sequentially adding butyl titanate and chloroacetic acid while stirring, heating to 80-120 deg.C, reacting for 2-8 hr, drying, grinding, and calcining at 300-600 deg.C for 2 hr. Said photocatalyst can be used for catalytic degradation of methylene blue under UV irradiation for improving its decoloring efficiency.

Description

Monoxone acidolysis tetrabutyl titanate prepares the method for nano titanium dioxide photocatalyst

Technical field

The present invention relates to a kind of preparation method of nano titanium dioxide photocatalyst, particularly relate to a kind of method of utilizing monoxone acidolysis tetrabutyl titanate to prepare nano titanium dioxide photocatalyst.

Background technology

Nano-TiO ₂Be a kind of novel inorganic functional material, have particular performances such as specific area is big, surface-active is high, absorbing properties is good, be widely used in fields such as fine ceramics raw material, catalyst, sensor, semiconductor, high-grade automobile finish and cosmetics; Simultaneously, nano-TiO ₂Have suitable energy gap, bigger surface area, stronger oxidation-reduction quality and nontoxic, low cost and other advantages are widely used as the catalyst of light-catalyzed reaction.Therefore, nano-TiO ₂Become a synthetic research focus of ultrafine inorganic powder in recent years.

At present, preparation nano-TiO ₂Method kinds more than ten such as sol-gal process, sluggish precipitation, micro emulsion method and hydro-thermal method are arranged.In the preparation method of various titanium dioxide nanocrystalline photochemical catalysts, sol-gel process is widely adopted.This method has the equipment less investment, synthesis temperature is low and multiple advantage such as easy controlled doping.Adopt this method to prepare TiO ₂Nano particle is normally with Ti (OR) ₄Be raw material, by control Ti (OR) ₄Hydrolysis speed obtain suitable presoma, and then roasting obtains nano-TiO at a certain temperature ₂Because Ti (OR) ₄At normal temperatures hydrolysis can take place rapidly, in order to make Ti (OR) ₄Hydrolysis carry out with suitable speed, common way is at first with Ti (OR) ₄Mix the solution that obtains debita spissitudo and pH value with absolute ethyl alcohol equal solvent and appropriate amount of acid, then water is mixed the alcohol solution that obtains suitable acidity with absolute ethyl alcohol equal solvent and appropriate amount of acid, again the latter is added drop-wise among the former with proper speed, obtain making it be transformed into gel again behind the colloidal sol, again with gel drying, roasting gets TiO at last ₂Nano-powder.Make and prepare nano-TiO in this way ₂Exist cycle long (generally at least 4～5 days), alcohols equal solvent to be difficult to shortcomings such as recovery, contaminated environment, production cost height.

Summary of the invention

The object of the present invention is to provide a kind of method of utilizing monoxone acidolysis tetrabutyl titanate to prepare nano titanium dioxide photocatalyst, this method is to add tetrabutyl titanate, monoxone successively by certain raw material proportioning in there-necked flask, heating, react 3～8h at a certain temperature, then with the reactant mixture drying; Behind the porphyrize under different temperatures roasting 2h promptly get nano-TiO ₂Powder.

The objective of the invention is to be achieved through the following technical solutions:

Monoxone acidolysis tetrabutyl titanate prepares the method for nano titanium dioxide photocatalyst, at there-necked flask agitating device, condenser and thermometer are installed earlier, under agitation add tetrabutyl titanate, monoxone successively, be heated to 80～120 ℃, isothermal reaction 2～8h, with the reactant mixture drying, in 300～600 ℃ of following roasting 2h, gained is nano-TiO behind the porphyrize then ₂Powder.

Aforesaid monoxone acidolysis tetrabutyl titanate prepares the method for nano titanium dioxide photocatalyst, and the tetrabutyl titanate of its adding is that 20.0g, monoxone are 22.2～33.3g.

Advantage of the present invention and effect are:

1. the present invention is a raw material with tetrabutyl titanate and monoxone, does not need to use the alcohols equal solvent, and its production process is simple, and the cycle is short, can reduce nano-TiO ₂Production cost.

2. the titanium dioxide optical catalyst that makes of the present invention can be used for catalytic degradation methylene blue under the UV-irradiation, after the 2h irradiation, can improve the decolorizing efficiency of methylene blue solution, there is no " three wastes " and pollutes.

The specific embodiment

Method for preparing catalyst

In having the reaction unit that stirs that refluxes, in there-necked flask, add tetrabutyl titanate, monoxone successively by certain raw material proportioning, heating is reacted 2～8h, at a certain temperature then with the reactant mixture drying; Behind the porphyrize under different temperatures roasting 2h promptly get nano-TiO ₂Powder.

The photocatalysis performance test

Certain density methylene blue solution 1000mL is loaded in the homemade photo catalysis reactor, starts stirring, sampling with its absorbance at maximum absorption wavelength 680nm place of spectrophotometric instrumentation, is designated as A ₀Add the 0.30g catalyst then in reactor, open uviol lamp after fully mixing, take a sample behind the 120min, centrifugation 10min gets supernatant liquor, surveys its absorbance at the 680nm place, is designated as A _tCalculate its decolorizing efficiency η by formula 1-1.

$\mathrm{\η}=\frac{A_0-A_t}{A_0}\×100\%---1-1$

In the formula: A ₀-initial absorbance; A _t-t absorbance constantly.

Embodiment and properties of product

After there-necked flask is installed agitating device, condenser and thermometer, stir and add tetrabutyl titanate 20.0g (0.06mol), monoxone 22.2～33.3g (0.24～0.36mol) down successively, be heated to 80～120 ℃, isothermal reaction 2～8h is then with the reactant mixture drying; Behind the porphyrize in 300～600 ℃ of following roasting 2h, gained nano-TiO ₂Powder is tested the performance that it is used for degraded methylene blue solution under the UV-irradiation by (2) described method.

(1) control acidolysis reaction temperature is 90 ℃, the tetrabutyl titanate consumption is 20.0g (0.06mol), the monoxone consumption is 22.2g (0.24mol), sintering temperature is 500 ℃, gained nano TiO 2 powder is with after methylene blue solution mixes, through UV-irradiation 2h, the decolorizing efficiency of methylene blue solution is 91.49%.Adopt sol-gel process gained nano-TiO ₂The decolorizing efficiency that is used for the photocatalytic degradation methylene blue solution under identical reaction condition is 94.12%.

(2) control acidolysis reaction temperature is 90 ℃, and the tetrabutyl titanate consumption is 20.0g (0.06mol), and the monoxone consumption is 14.4g (0.24mol), and sintering temperature is 400 ℃, the gained nano-TiO ₂Powder is with after methylene blue solution mixes, and through UV-irradiation 2h, the decolorizing efficiency of methylene blue solution is 91.72%.

The contrast experiment

Adopt the obtained nano-TiO of this method in order further to investigate ₂The photocatalysis performance of powder, this paper also adopt sol-gel process and hydrothermal synthesis method to prepare nano-TiO respectively ₂Powder is with these three kinds of prepared nano-TiOs of method ₂Powder is respectively applied for catalytic degradation methylene blue solution under the UV-irradiation, and the gained result is as follows:

0 20 40 60 80 100 120

Sol-gel process 0.00 28.00 54.10 73.80 85.09 92.30 94.12

Hydrothermal synthesis method 0.00 24.00 50.61 68.90 80.54 86.52 91.74

Method 0 30.25 56.86 76.05 89.92 97.62 99.86 of the present invention

Therefrom as can be seen, the preparation method has certain influence to the performance that the gained photochemical catalyst is used for catalytic degradation methylenum careuleum under the UV-irradiation.Adopt the prepared nano-TiO of this method ₂Photocatalysis performance the best of powder.As seen, utilize the direct prepared in reaction nano-TiO of acetate and tetrabutyl titanate ₂It is simple that photochemical catalyst has technology really, and excellent product performance does not have the advantage that " three wastes " pollute.

Claims (2)

1. monoxone acidolysis tetrabutyl titanate prepares the method for nano titanium dioxide photocatalyst, it is characterized in that, at there-necked flask agitating device, condenser and thermometer are installed earlier, under agitation add tetrabutyl titanate, monoxone successively, be heated to 80～120 ℃, isothermal reaction 2～8h is then with the reactant mixture drying, in 300～600 ℃ of following roasting 2h, gained is nano-TiO behind the porphyrize ₂Powder.

2. monoxone acidolysis tetrabutyl titanate according to claim 1 prepares the method for nano titanium dioxide photocatalyst, it is characterized in that, the tetrabutyl titanate of adding is that 20.0g, monoxone are 22.2～33.3g.