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Method for preparing nanometer titanium dioxide/attapulgite composite material

A technology of nano-titanium dioxide and attapulgite, applied in chemical instruments and methods, fibrous fillers, inorganic pigment treatment, etc., can solve the problems of high price, unfavorable industrial production, and hidden safety hazards of n-butyl titanate, and achieve the goal of preparing The method is simple and easy to implement, with low cost and high safety effect

Inactive Publication Date: 2011-07-27
JIANGSU POLYTECHNIC UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The patent application with publication number CN101121124A discloses a synthesis method of attapulgite composite photocatalyst, using n-butyl titanate as raw material, preparing a sol through its hydrolysis, and then obtaining attapulgite composite material, its disadvantages are: n-butyl titanate is expensive, consumes a lot of energy, and has potential safety hazards, which is not conducive to industrial production
The patent application with the publication number CN101117780A discloses a preparation method of modified attapulgite powder used for papermaking fillers. The raw material used is inorganic titanium salt, and the raw material cost is relatively low, but its disadvantages are: a large amount of oxalic acid, Tartaric acid or citric acid are used as compounding agents, resulting in higher product costs and pollution to the environment

Method used

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  • Method for preparing nanometer titanium dioxide/attapulgite composite material
  • Method for preparing nanometer titanium dioxide/attapulgite composite material
  • Method for preparing nanometer titanium dioxide/attapulgite composite material

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Experimental program
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Effect test

Embodiment 1

[0026] 160 g of attapulgite was added to 640 g of deionized water to prepare a slurry with a mass ratio of m (attapulgite):m (water)=1:4. Measure 300mL of 1mol / L NaOH solution into a 2000mL three-necked flask, and slowly add 1mol / L TiCl dropwise while stirring 4 200 mL of aqueous solution, and control the reaction temperature at 5°C. TiCl 4 After the aqueous solution was added dropwise, the prepared attapulgite slurry was added into a three-necked flask, the temperature was raised to 100° C., and the crystallization reaction was stirred at 100° C. for 0.5 h. The pH value of the system was adjusted to pH=8 with 1 mol / L NaOH solution, filtered, and washed repeatedly until the conductivity of the filtrate was 300 μS / cm, and the washing was completed. Gained filter cake is redispersed in deionized water, is formulated with solid content and is 15% (mass fraction) nano-titanium dioxide / attapulgite composite material slurry, wherein the crystal form of nano-titanium dioxide is the...

Embodiment 2

[0028] 96g of attapulgite was added to 960g of deionized water to prepare a slurry with a mass ratio of m(attapulgite):m(water)=1:10. Measure 400mL of 3mol / L NaOH solution into a 2000mL three-necked flask, and slowly add 4mol / L TiCl dropwise while stirring 4 150 mL of aqueous solution, and control the reaction temperature at 100°C. TiCl 4 After the aqueous solution was added dropwise, the prepared attapulgite slurry was added into a three-necked flask, and the temperature of the system was maintained at 100° C., and the crystallization reaction was stirred for 4 hours. The pH of the system was adjusted to pH=7.5 with 3 mol / L KOH solution, filtered, and washed repeatedly until the conductivity of the filtrate was 180 μS / cm, and the washing was completed. The obtained filter cake is dried to prepare nano titanium dioxide / attapulgite composite material powder, wherein the crystal form of nano titanium dioxide is rutile.

Embodiment 3

[0030] 48 g of attapulgite was added to 480 g of deionized water to prepare a slurry with a mass ratio of m (attapulgite):m (water)=1:10. Measure 400mL of 1.5mol / L NaOH solution into a 2000mL three-necked flask, slowly add 2mol / L TiCl dropwise while stirring 4 150 mL of aqueous solution, and control the reaction temperature at 10°C. TiCl 4 After the aqueous solution was added dropwise, the prepared attapulgite slurry was added into a three-necked flask, the temperature was raised to 85° C., and the crystallization reaction was stirred at 85° C. for 1 h. Adjust the pH of the system to pH=7.6 with 1 mol / L ammonia solution, filter, and wash repeatedly until the conductivity of the filtrate is 150 μS / cm, and the washing is complete. The obtained filter cake is dried to prepare nano titanium dioxide / attapulgite composite material powder, wherein the crystal form of nano titanium dioxide is a mixed crystal form of anatase and rutile.

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Abstract

The invention discloses a nanometer titanium dioxide / attapulgite composite; firstly, adding attapulgite into deionized water to prepare attapulgite slurry; then adding attapulgite slurry into nanometer titanium dioxide precursor to form tinwhite liquid cement of nanometer titanium dioxide / attapulgite composite particles; adjusting the pH value of the liquid cement through alkaline solution, filtering and washing repeatedly so as to remove the impurities in the filter mass; drying the filter mass and making into nanometer titanium dioxide / attapulgite composite powder. The filter mass can be re-dispersed in deionized water to be prepared into nanometer titanium dioxide / attapulgite composite slurry with different solid content. The composite prepared through the method described by the invention combines the excellent properties of nanometer titanium dioxide and attapulgite. The preparation method is simple and easy to realize and requires no high temperature heat treatment and is low inenergy consumption, high in safety and little in pollution, and can conveniently prepare different polymorphs nanometer titanium dioxide / attapulgite composites.

Description

technical field [0001] The invention relates to a composite material prepared by nano titanium dioxide and attapulgite, in particular to a preparation method of the composite material. Background technique [0002] Nano-titanium dioxide is an important inorganic functional material, which is widely used in the fields of ultraviolet shielding, photocatalysis and photoelectric conversion. Attapulgite is a layer chain structure of water-containing magnesium-aluminosilicate clay mineral. It is a natural one-dimensional nanomaterial with excellent adsorption and colloidal properties and low price. It is widely used in printing and dyeing, paint, rubber and plastic, Adhesives, adsorbents, desiccants and oil drilling have been widely used. [0003] The patent application with publication number CN101121124A discloses a synthesis method of attapulgite composite photocatalyst, using n-butyl titanate as raw material, preparing a sol through its hydrolysis, and then obtaining attapulg...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09C1/28C09C1/36C09C3/00
Inventor 姚超方志成陈志刚吴凤芹丁永红李为民王茂华
Owner JIANGSU POLYTECHNIC UNIVERSITY