Organic phosphonium transition metal salt graded hole material preparing method and the application

A transition metal salt and organic phosphonic acid technology, applied in chemical instruments and methods, and other chemical processes, can solve limitations and other problems, and achieve the effects of improved adsorption performance, simple operation, and easy regeneration

Inactive Publication Date: 2007-09-19
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the only few papers on organophosphonic acid-modified alumina and vanadium oxide materials are limited to the mesopore range.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Under stirring at room temperature, add 1.03g of organic phosphonic acid HEDP to a mixed solution of 30ml of ethanol and 15ml of water, stir until the solution is clear, slowly add 1.702g of Ti(BuOT) dropwise, continue to stir slowly for 24h, and crystallize at 80℃ for 24h . After the product is filtered, washed with water, and dried, an organic / inorganic hybrid porous material is obtained. The sample is XRD, N 2 Adsorption / desorption, SEM, TEM, XPS, NMR characterization confirmed that it is an organic titanium phosphonate with a macroporous / mesoporous structure. The BET specific surface area of ​​the material is 257m 2 / g; pore volume is 0.052cm 3 / g; Macropore pore size is 50-200nm; Mesopore pore size is 2.44nm. The P content is 16.54%.

Embodiment 2

[0023] Using the preparation process of Example 1, 3.06 g of organic phosphonate EDTMPS and 3.404 g of Ti(BuOT) were added, stirred at room temperature for 24 hours, and crystallized at 80° C. for 24 hours. The BET specific surface area of ​​the obtained material is 15m 2 / g; pore volume is 0.074cm 3 / g; Macropore pore size is 50-1000nm; Mesopore pore size is 2.48nm. The P content is 5.38%.

Embodiment 3

[0025] Using the preparation process of Example 2, the BET specific surface area of ​​the material obtained by adding 0.37g of concentrated HCl is 86m 2 / g; pore volume is 0.074cm 3 / g; The pore size of the macropore is 50-2000nm; the pore size of the mesopore is 3.22nm and 8.22nm.

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PUM

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Abstract

The invention relates to a preparation for multiporous material, especially a process for preparing organic and inorganic hetero-material with multiporous structure and application thereof. The hetero-material is a transition metal phosphonate with different organic phosphonic acid groups combined on the surface and skeleton of mesoporous and macroporous structure, wherein, the weight percent of the organic phosphonic acid P is 1% to 17%, and the transition metals can be selected from Ti salt, Al salt, Zr salt, etc. The hetero-material is directly synthesized by hydrothermal synthesis and can be used for heavy metal ion absorption with good absorption effect, the invention is provided with simple equipments and moderate synthesis conditions, and the raw materials is available, accordingly, the multiporous material preparing process is suitable for large-scale production.

Description

Technical field [0001] The invention relates to the preparation of a multi-stage porous material, in particular to a preparation method and application of an organic phosphonic acid transition metal salt porous material. New organic-inorganic hybrid metal oxide and phosphonate (titanium, aluminum, zirconium and other salts) materials are used for heavy metal ion adsorption. Background technique [0002] Porous materials, such as molecular sieves, have been receiving extensive attention due to their large specific surface area and ordered pore structure, and have been tried to be used in research fields such as catalysis, adsorption, separation, and sensors. CN1387942A discloses a method for preparing high-adsorption titanium silicate, using ethyl orthosilicate as silicon source and polyethylene glycol (PEG-600) as additive to synthesize a silicic acid with nanoporous structure step by step titanium. The method must strictly control the hydrolysis conditions, the synthesis time is...

Claims

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Application Information

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