CN101337181A - Preparation method of purificant in nano titanic oxide photochemical catalyst chamber - Google Patents

Abstract

The invention discloses a method for preparing a nanometer TiO2 photocatalytic indoor purificant as follows: under the combined action of microwave radiation and higher fatty acid and nonionic surfactants in a proper proportion, the purificant can be prepared under common temperature calcination. In a retort, deionized water is firstly added, a complex surfactant is added under stirring, a hydrolysis inhibitor is used for adjusting the pH value of the solution, then a dipolar organic solvent is added, and the mixture is heated to be slightly boiled, and then titanate is added until a white gel is formed; the gel is distilled by microwaves, washed by ammonia water after the temperature is cooled down, then dried by microwaves, and cooled for discharging, thereby obtaining the nanometer TiO2 photocatalytic indoor purificant responded by visible light. The nanometer TiO2 prepared by the invention has obvious absorption in a visible light region, the wavelength of which is 400-650 nm, and has higher bacteriostatic rate to Escherichia coli, staphylococcus aureus and bacillus subtilis under an indoor fluorescent lamp or an energy-saving lamp; the production cost is low; and the production efficiency is high.

Description

The preparation method of purificant in nano titanic oxide photochemical catalyst chamber

Technical field

The present invention relates to a kind of preparation method of purificant in nano titanic oxide photochemical catalyst chamber, be specifically related to a kind of preparation method of visible light-responded nano titanium dioxide photocatalysis indoor air purification agent.

Background technology

At present, countries in the world all in various degree be faced with the puzzlement that environment goes from bad to worse, and the pollution of indoor organic matter and bacterium is with serious pollution two big classes in miscellaneous indoor pollutant.Traditional processing method has physisorphtion and chemical oxidization method etc.; these methods have significant role to the protection and the improvement of indoor air purification; but these technology exist to some extent efficient low, can not pollutant is thoroughly innoxious, easily produce secondary pollution or energy consumption height, be not suitable for the defective of aspects such as large-scale promotion; thereby, develop more efficient, more economical, have deep oxidation ability, green indoor pollutant improvement technology applied widely particularly to seem and press for.Nano titanium oxide is the photochemical catalytic oxidation agent of a kind of little brilliant degree, bigger serface, organic pollution can be become carbon dioxide and water with the bacterium exhaustive oxidation, and self is nontoxic, and this has opened up an important new way in green indoor pollution improvement field.

Photocatalysis means the two the combination of photochemistry and catalyst, light and catalyst are the necessary conditions that causes and promote photocatalysis oxidation reaction, why semi-conducting material can be as photochemical catalyst, be to determine because of himself photoelectric characteristic, as the semiconductor that plays a crucial role in the photocatalytic oxidation, its band structure is to be full of the low energy valence band of electronics and the high energy conduction band of a sky constitutes by one, regional forbidden band therebetween is a discontinuity zone, when semiconductor is subjected to optical excitation greater than its band-gap energy, electronics on the valence band (being light induced electron) will transit to conduction band, and stays corresponding hole in valence band.

As everyone knows, the energy gap of titanium dioxide big (3.2eV), for this reason, nano titanium oxide can only utilize in the sunshine 3～4% ultraviolet light (wavelength is less than 380nm), bring into play its photocatalytic oxidation, and indoor sunlight is more weak, irradiation time is shorter, this has seriously restricted the effective utilization of nano titanium oxide to visible light, so, its absorption is extended to sunshine and abundant visible region such as indoor fluorescent lamp and electricity-saving lamp, promptly preparing visible light-responded optically catalytic TiO 2 oxidant, is a very important part of indoor purifying application study exploitation, also is the key of purification applications in the optically catalytic TiO 2 oxidation inlet chamber.

For improving the response activity and the utilization ratio of nano-titanium dioxide visible light, at present, study on the modification to nano titanium oxide has been obtained many progress, for example, titanium dioxide is carried out metal or nonmetal doping, semiconductor is compound, modified measures such as noble metal loading, can make the titanium dioxide crystal surface produce defective, suppress the compound of titanium dioxide photoproduction electronics-hole, increase the quantity in titanium dioxide surface activated centre, improve the optically catalytic TiO 2 oxidation activity, but existing method needs high-temperature calcination to prepare nano titanium dioxide powder mostly, energy consumption is big and to the requirement height of equipment, a kind of preparation method of visible-light response type photocatalyst of titanium dioxide indoor air purification agent that has been 200410059680.0 patent disclosure as application number, but needed in 700～900 ℃ air calcination in its preparation process 2～3 hours, so it is one of current problem demanding prompt solution that low temperature prepares visible light-responded purificant in nano titanic oxide photochemical catalyst chamber.

Summary of the invention

The objective of the invention is to overcome the deficiencies in the prior art, the preparation method of the visible light-responded nano titanium dioxide photocatalysis indoor air purification agent that a kind of non high temperature is calcined, production cost is low and production efficiency is high is provided.

The present invention is achieved by the following technical solutions:

In retort, add deionized water 100 mass parts, stir down, add complexed surfactant 0.5～10 mass parts; Behind the 10min, transferring the pH value of solution with hydrolysis inhibitor is 1～4; Behind the 15min, add dipole organic solvent 10～100 mass parts; Mixed liquor is heated to little boiling down, adds the titanate esters of 10 mass parts, become the gel of white to reaction; With the microwave distillation of gel with 300～700W, cooling with the ammonia scrubbing of 0.1mol/L, is used the microwave drying of 300～700W again, and cooling discharging gets visible light-responded nano titanium dioxide photocatalysis indoor air purification agent;

Described complexed surfactant is made up of by mass ratio 1: 5～10 blend higher fatty acids and nonionic surface active agent;

It is one of following that described higher fatty acids is selected from: palmitic acid, stearic acid, linoleic acid;

It is one of following that described nonionic surface active agent is selected from: AEO, OPEO, dodecyl phenol polyethenoxy ether, and the wherein polyoxyethylated degree of polymerization is 5～20;

It is one of following that described dipole organic solvent is selected from: methyl alcohol, ethanol, isopropyl alcohol, oxolane;

It is one of following that described hydrolysis inhibitor is selected from: hydrochloric acid, nitric acid, sulfuric acid, p-methyl benzenesulfonic acid;

It is one of following that described titanate esters is selected from: titanium propanolate, isopropyl titanate, butyl titanate.

The visible light-responded purificant in nano titanic oxide photochemical catalyst chamber of present invention, particle diameter are measured its absorption curve through ultraviolet-visible spectrophotometer and are found between 10～80nm, produce obviously to absorb between wavelength 400～650nm; Fluorescent lamp or electricity-saving lamp at indoor use 21W, 24h to the inhibiting rate of Escherichia coli, staphylococcus aureus and bacillus subtilis greater than 95%, the degradation rate of 24h PARA FORMALDEHYDE PRILLS(91,95) is greater than 70%, and the nano titanium oxide of the specific activity high-temperature calcination of degradation of formaldehyde preparation exceeds 3～10 times.

Microwave is and the diverse mode of heating of traditional heating, traditional heating is to produce high outside and low outside thermograde in heat conducting mode, and being electromagnetic wave, heating using microwave acts on polar molecule dielectric and non-polar molecule dielectric, producing dipole or dipole newly arranges, realize " stirring " of molecular level, can effectively reduce the particle diameter of powder particulate.

Surfactant is that a class is adsorbed on the interface, also can significantly reduce the material of interfacial tension when low concentration very, and the character that this has influenced particle surface is one of effective way that effectively reduces diameter of particle.

The visible light-responded nano titanium dioxide photocatalysis indoor air purification agent of the present invention's preparation, be to adopt microwave radiation and the higher fatty acids of proper proportion and the acting in conjunction of nonionic surface active agent, thereby the surface that has influenced between titanium dioxide fine particles can, under the condition of non high temperature calcining, suppressed the reunion of particulate, its absorption of prepared nano titanium oxide has extended to the scope of visible light 400～650nm, improved photo-quantum efficiency, had that technology is easily controlled, production cost is low and advantage of high production efficiency.

The specific embodiment

Below in conjunction with embodiment the present invention is further described, but protection scope of the present invention is not limited to embodiment.

Embodiment 1:

In retort, add deionized water 100 mass parts, stir down, add complexed surfactant 1 mass parts; Behind the 10min, transferring the pH value of solution with hydrochloric acid is 1; Behind the 15min, add methyl alcohol 100 mass parts; Mixed liquor is heated to little boiling down, adds the titanium propanolate of 10 mass parts, become the gel of white to reaction; With the microwave distillation of gel with 300W, cooling with the ammonia scrubbing of 0.1mol/L, is used the microwave drying discharging of 300W again, promptly gets visible light-responded nano titanium dioxide photocatalysis indoor air purification agent;

Described complexed surfactant is made up of by mass ratio blend in 1: 5 palmitic acid and AEO, and the wherein polyoxyethylated degree of polymerization is 6.

Embodiment 2:

In retort, add deionized water 100 mass parts, stir down, add complexed surfactant 3 mass parts; Behind the 10min, transferring the pH value of solution with nitric acid is 2; Behind the 15min, add ethanol 70 mass parts; Mixed liquor is heated to little boiling down, adds the isopropyl titanate of 10 mass parts, become the gel of white to reaction; With the microwave distillation of gel with 400W, cooling with the ammonia scrubbing of 0.1mol/L, is used the microwave drying of 400W again, and cooling discharging gets visible light-responded nano titanium dioxide photocatalysis indoor air purification agent;

Described complexed surfactant is made up of by mass ratio blend in 1: 7 stearic acid and OPEO, and the wherein polyoxyethylated degree of polymerization is 10.

Embodiment 3:

In retort, add deionized water 100 mass parts, stir down, add complexed surfactant 7 mass parts; Behind the 10min, transferring the pH value of solution with p-methyl benzenesulfonic acid is 4; Behind the 15min, add isopropyl alcohol 10 mass parts; Mixed liquor is heated to little boiling down, adds the butyl titanate of 10 mass parts, become the gel of white to reaction; With the microwave distillation of gel with 700W, cooling with the ammonia scrubbing of 0.1mol/L, is used the microwave drying of 500W again, and cooling discharging gets visible light-responded nano titanium dioxide photocatalysis indoor air purification agent;

Described complexed surfactant is made up of by mass ratio blend in 1: 10 linoleic acid and dodecyl phenol polyethenoxy ether, and the wherein polyoxyethylated degree of polymerization is 16.

Embodiment 4:

In retort, add deionized water 100 mass parts, stir down, add complexed surfactant 10 mass parts; Behind the 10min, transferring the pH value of solution with sulfuric acid is 3; Behind the 15min, add oxolane 60 mass parts; Mixed liquor is heated to little boiling down, adds the butyl titanate of 10 mass parts, become the gel of white to reaction; With the microwave distillation of gel with 500W, cooling with the ammonia scrubbing of 0.1mol/L, is used the microwave drying of 700W again, and cooling discharging gets visible light-responded nano titanium dioxide photocatalysis indoor air purification agent;

Described complexed surfactant is made up of by mass ratio blend in 1: 8 linoleic acid and AEO, and the wherein polyoxyethylated degree of polymerization is 20.

Claims (1)

1. the preparation method of purificant in nano titanic oxide photochemical catalyst chamber is characterized in that being undertaken by following step:

In retort, add deionized water 100 mass parts, stir down, add complexed surfactant 0.5～10 mass parts; Behind the 10min, transferring the pH value of solution with hydrolysis inhibitor is 1～4; Behind the 15min, add dipole organic solvent 10～100 mass parts; Mixed liquor is heated to little boiling down, adds the titanate esters of 10 mass parts, become the gel of white to reaction; With the microwave distillation of gel with 300～700W, cooling with the ammonia scrubbing of 0.1mol/L, is used the microwave drying of 300～700W again, and cooling discharging gets visible light-responded nano titanium dioxide photocatalysis indoor air purification agent;

Described complexed surfactant is made up of by mass ratio 1: 5～10 blend higher fatty acids and nonionic surface active agent;

It is one of following that described higher fatty acids is selected from: palmitic acid, stearic acid, linoleic acid;

It is one of following that described nonionic surface active agent is selected from: AEO, OPEO, dodecyl phenol polyethenoxy ether, and the wherein polyoxyethylated degree of polymerization is 5～20;

It is one of following that described dipole organic solvent is selected from: methyl alcohol, ethanol, isopropyl alcohol, oxolane;

It is one of following that described hydrolysis inhibitor is selected from: hydrochloric acid, nitric acid, sulfuric acid, p-methyl benzenesulfonic acid;

It is one of following that described titanate esters is selected from: titanium propanolate, isopropyl titanate, butyl titanate.