CN104645957A

CN104645957A - Method for preparing titanium dioxide and sepiolite composite material

Info

Publication number: CN104645957A
Application number: CN201410745156.2A
Authority: CN
Inventors: 张娜
Original assignee: Individual
Current assignee: Individual
Priority date: 2014-12-09
Filing date: 2014-12-09
Publication date: 2015-05-27

Abstract

The invention discloses a method for preparing a titanium dioxide and sepiolite composite material, belonging to the field of preparation of photocatalytic materials. Aiming at the problems that the directly used powdered TiO2 is large in amount, low in optical activity and short in service life and is difficultly recycled, the invention provides the method for preparing the titanium dioxide and sepiolite composite material which is high in photocatalytic performance and easy to recycle. The preparation method comprises the following steps: preparing TiO2 nano-sol by adopting a sol-gel method, loading TiO2 onto the surface of sepiolite by adopting an impregnation method, thereby obtaining the titanium dioxide and sepiolite composite material. The preparation method is simple in process, and the prepared titanium dioxide and sepiolite composite material is high in photocatalytic performance and easy to recycle and has wide application prospects.

Description

A kind of titanium dioxide sepiolite composite material and preparation method thereof

Technical field

The invention belongs to catalysis material preparation field.

Background technology

Photocatalytic-oxidation is turned to a kind of new type water treatment technology, has the potential advantages such as efficient, low consumption.TiO ₂because its spectrochemical property is stablized, high-effect, low cost, is widely used as photochemical catalyst.Directly use powdery TiO ₂carry out photocatalysis oxidation reaction, although can the organic matter of many difficult for biological degradation in the efficient oxidation water, reach except poison, decolour, deodorize until degradable is CO ₂and H ₂the object of the inorganic molecules such as O, but usually suspended phase photocatalytic oxidation exists with water separation difficulty, catalyst amount is large, photolytic activity is low, the life-span is short, the not easily problem such as regeneration.

Summary of the invention

The object of this invention is to provide a kind of photocatalysis performance high, titanium dioxide sepiolite composite material and preparation method thereof easy to be recycled.

The present invention is achieved by the following technical programs: a kind of titanium dioxide sepiolite composite material and preparation method thereof, comprise following two steps: 1, sepiolite carries out modification, sepiolite deionized water is soaked 20 ~ 30min, isolate scum silica frost, filtration, then under 70C constant temperature, leach 10h with the HCl solution that concentration is 1.0mol/L, control liquid-solid ratio is 10:1.Again with distilled water washing, vacuum filtration, removing calcium chlorion, until use AgNO ₃without till white precipitate in solution testing solution, after filtrate being dried, calcine 5 ~ 6h through 500C, take out and naturally cool to room temperature, obtain modified meerschaum, 2, load TiO ₂, under room temperature, 4mL butyl titanate is dissolved in 13.4mL absolute ethyl alcohol, prepare butyl titanate/ethanol solution, be denoted as A liquid O and get 6.6mL absolute ethyl alcohol, 0.6mL deionized water and 1mL1mol/L hydrochloric acid fully mix, make dropping liquid B liquid, under magnetic stirring, B liquid is added drop-wise in A liquid with the speed of 3mL/min, the pH value regulating solution is 4.0, add lg Macrogol 2000 after dripping off to continue to stir 30min, at room temperature peptization l0h, making translucent faint yellow colloidal sol is slowly added drop-wise in the sepiolite of l0g process by obtained colloidal sol when stirring, mix and blend lh, static peptization 20h, centrifugal go out sediment, use deionized water rinsing sediment, dry 6h in vacuum drying chamber, last at 400 ~ 550 DEG C of roasting temperature 4h, obtain catalysis material.

The present invention has following beneficial effect:

The titanium dioxide sepiolite composite photocatalysis performance of preparation is high, and the degradation rate bright red to dyestuff intellectual circle reaches 87%, and easy recovery and reusing and recycling.

Detailed description of the invention

Below in conjunction with specific embodiment, the present invention will be further described.

Specific embodiment: preparation process of the present invention comprises the following steps: 1. sepiolite carries out modification, sepiolite deionized water is soaked 20 ~ 30min, isolate scum silica frost, filtration, then under 70C constant temperature, leach 10h with the HCl solution that concentration is 1.0mol/L, control liquid-solid ratio is 10:1.Wash with distilled water again, vacuum filtration, removing calcium chlorion, until with in AgNO3 solution testing solution without white precipitate till, after filtrate being dried, calcine 5 ~ 6h through 500C, take out and naturally cool to room temperature, obtain modified meerschaum, its preparation technology's flow process is sepiolite-immersion-removing dross-filtration-acid treatment-filtration-drying-500C calcination-cooling-modified meerschaum;

2, load TiO ₂, under room temperature, 4mL butyl titanate is dissolved in 13.4mL absolute ethyl alcohol, prepare butyl titanate/ethanol solution, be denoted as A liquid O and get 6.6mL absolute ethyl alcohol, 0.6mL deionized water and 1mL1mol/L hydrochloric acid fully mix, make dropping liquid B liquid, under magnetic stirring, B liquid is added drop-wise in A liquid with the speed of 3mL/min, the pH value regulating solution is 4.0, add lg Macrogol 2000 after dripping off to continue to stir 30min, at room temperature peptization l0h, making translucent faint yellow colloidal sol is slowly added drop-wise in the sepiolite of l0g process by obtained colloidal sol when stirring, mix and blend lh, static peptization 20h, centrifugal go out sediment, use deionized water rinsing sediment, dry 6h in vacuum drying chamber, last at 400 ~ 550 DEG C of roasting temperature 4h, obtain catalysis material.

Photocatalytic degradation is tested: take the finished product that lg is obtained, add fill l00mL, concentration is that in the 250mL beaker of the bright red solution of 20mg/L intellectual circle, static lh makes it fully adsorb, and using the concentration of now solution as initial concentration; Then be placed on irradiation (distance of liquid level and lamp is 20cm) under 250W high-pressure sodium lamp, take out a small amount of supernatant liquor after certain hour, survey its absorbance 226nm place (record with TUl800 ultraviolet-uisible spectrophotometer intellectual circle is bright red has the last one absworption peak at about 226nm); Then refund in beaker, continue irradiation, so repeatedly, until decolour completely; Under similarity condition, make a blank assay (not adding catalyst), to eliminate the degraded of pure ultraviolet light simultaneously.Experimental configuration shows that the degradation rate bright red to dyestuff intellectual circle reaches 87%.

above content is the further description done the present invention in conjunction with concrete embodiment, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.

Claims

1. a titanium dioxide sepiolite composite material and preparation method thereof, it is characterized in that: comprise following two steps: 1, sepiolite carries out modification, sepiolite deionized water is soaked 20 ~ 30min, isolate scum silica frost, filtration, then under 70C constant temperature, leach 10h with the HCl solution that concentration is 1.0mol/L, control liquid-solid ratio is 10:1, wash with distilled water again, vacuum filtration, removing calcium chlorion, until use AgNO ₃without till white precipitate in solution testing solution, after filtrate being dried, calcine 5 ~ 6h through 500C, take out and naturally cool to room temperature, obtain modified meerschaum, 2, load TiO ₂, under room temperature, 4mL butyl titanate is dissolved in 13.4mL absolute ethyl alcohol, prepare butyl titanate/ethanol solution, be denoted as A liquid O and get 6.6mL absolute ethyl alcohol, 0.6mL deionized water and 1mL1mol/L hydrochloric acid fully mix, make dropping liquid B liquid, under magnetic stirring, B liquid is added drop-wise in A liquid with the speed of 3mL/min, the pH value regulating solution is 4.0, add lg Macrogol 2000 after dripping off to continue to stir 30min, at room temperature peptization l0h, making translucent faint yellow colloidal sol is slowly added drop-wise in the sepiolite of l0g process by obtained colloidal sol when stirring, mix and blend lh, static peptization 20h, centrifugal go out sediment, use deionized water rinsing sediment, dry 6h in vacuum drying chamber, last at 400 ~ 550 DEG C of roasting temperature 4h, obtain catalysis material.