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Preparation and application of organic phosphonate titanium oxide heterozygous mesoporous material

A technology of hybrid materials and mesoporous materials, which is applied in the field of preparation of porous materials, can solve problems such as the limitation of phosphonic acids, and achieve high mechanical stability, good ultraviolet and visible light catalytic performance, and high hydrothermal stability.

Inactive Publication Date: 2008-09-17
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The organic phosphonic acid modified alumina and organophosphonic acid aluminum mesoporous materials have also been reported recently, but the phosphonic acid used is limited to mono- or bis-phosphonic acid

Method used

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  • Preparation and application of organic phosphonate titanium oxide heterozygous mesoporous material
  • Preparation and application of organic phosphonate titanium oxide heterozygous mesoporous material
  • Preparation and application of organic phosphonate titanium oxide heterozygous mesoporous material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Under stirring at room temperature, 1.53 g of organic phosphonic acid sodium salt EDTMPS was added to a mixed solution of 30 ml of ethanol and 15 ml of water, stirred until the solution was clear, and the pH value of the solution was adjusted to 1 with hydrochloric acid. Slowly add 1.702 g of butyl titanate dropwise, continue stirring at a slow speed for 24 hours, and crystallize at 80° C. for 24 hours. After the product is filtered, washed with water and dried, an organic / inorganic hybrid porous material (T-EDTMPS) is obtained. The samples were tested by XRD, TG-DSC, N 2 Adsorption / desorption, SEM, TEM, XPS, FT-IR, UV-vis, 31 P and 13 C MAS NMR characterization confirmed that it is an organic phosphonate titanium oxide hybrid material with mesoporous structure. Among them, TEM shows that the material has irregular worm-like mesopores ( figure 1 ); The XRD spectrum shows that the material is a single anatase crystal form ( figure 2 ); the nitrogen adsorption-desor...

Embodiment 2

[0027] Using the preparation process of Example 1, the organic phosphonic acid DTMPPA sodium salt was added to a mixed solution of 30 ml of ethanol and 15 ml of water, stirred until the solution was clear, and the pH value of the solution was adjusted to 1 with hydrochloric acid. Slowly add 1.702 g of Ti(BuOT) dropwise, continue stirring at a slow speed for 24 hours, and crystallize at 80°C for 24 hours. After the product is filtered, washed with water and dried, an organic / inorganic hybrid mesoporous material (T-DTMPPA) is obtained. Among them, TEM shows that the material has irregular worm-like mesopores ( figure 1 ); The XRD spectrum shows that the material is a single anatase crystal form ( figure 2 ); the nitrogen adsorption-desorption isotherm and the corresponding pore size distribution plots show that the material has a typical mesoporous structure ( image 3 ), the BET specific surface area is 128m 2 / g; the pore volume is 0.19cm 3 / g; the mesopore size is 3.6nm....

Embodiment 3

[0029] Get sample 0.02g in embodiment 1 and 2 and make catalyst, be suspended in the 30mg / L rhodamine B aqueous solution of 100ml, be that 125W high pressure mercury lamp and household incandescent lamp of 365nm are used as light source respectively with cut-off wavelength, Figure 4 (a) and 4(b) are comparisons of the degradation effects of samples on Rhodamine B under ultraviolet light and visible light irradiation, respectively. The second figure shows the as-synthesized hybrid material relative to the pure mesoporous TiO 2 It has high photocatalytic activity.

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Abstract

The invention relates to a preparation method of porous materials, in particular to a preparation method and application of an organic-inorganic hybrid material with mesoporous structure. The porous material with mesoporous structure is titanium dioxide material of bisphosphonates hybrid of various organic phosphoric acid groups in framework; wherein, the weight percentage of the organic phosphoric P is 7-10.5wt%. The material is synthesized directly through the method of hydrothermal synthesis and can be used in the photocatalytic degradation of organic dye molecules under ultraviolet and visible light and heavy metal ion adsorption, having excellent effect; the product has strong preferential absorption capacity, especially for Cd (II) ion. The preparation method has the advantages of simple equipment, mild synthesis conditions and easily available raw materials; therefore, the preparation method is suitable for industrial mass production.

Description

technical field [0001] The invention relates to the preparation of porous materials, in particular to the preparation method and application of an organic phosphonate titanium oxide hybrid mesoporous material. Novel organic-inorganic hybrid materials for photocatalytic degradation of organic dye molecules and adsorption of heavy metal ions. Background technique [0002] Organic-inorganic hybrid materials have increasingly attracted great interest due to their multifunctionality derived from both organic groups and inorganic components. They have great application prospects in research fields such as catalysis, adsorption, separation and sensors. Paper Chem.Mater.12 (2000) 1268-1272 prepared titanium oxide / phenyl phosphonate hybrid material in non-aqueous system by two-step sol-gel process, but the synthetic product is non-porous and has no effect on its applied research. The paper Chem.Eur.J.12 (2006) 3507-3514 reported a titanium phosphonate and titanium oxide phosphonat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/38B01J31/24B01J20/22
Inventor 袁忠勇马天翼张雪军
Owner NANKAI UNIV
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