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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 improving adsorption performance, environmental protection, and high hydrothermal stability

Inactive Publication Date: 2010-01-27
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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  • Organic phosphonium transition metal salt graded hole material preparing method and the application
  • Organic phosphonium transition metal salt graded hole material preparing method and the application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Under stirring at room temperature, add 1.03g of organic phosphonic acid HEDP into 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 at a slow speed for 24h, and crystallize at 80°C for 24h . After the product is filtered, washed with water and dried, an organic / inorganic hybrid porous material is obtained. The samples were tested by XRD, N 2 Adsorption / desorption, SEM, TEM, XPS, NMR characterization confirmed that organic phosphonate titanium with macroporous / mesoporous structure. The BET specific surface area of ​​the material is 257m 2 / g; the pore volume is 0.052cm 3 / g; the macropore diameter is 50-200nm; the mesopore diameter is 2.44nm. Among them, 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 h, and crystallized at 80° C. for 24 h. The resulting material has a BET specific surface area of ​​15m 2 / g; the pore volume is 0.074cm 3 / g; macropore diameter is 50-1000nm; mesopore diameter is 2.48nm. Among them, the P content is 5.38%.

Embodiment 3

[0025] Adopt the preparation process of embodiment 2, add the BET specific surface area of ​​the material that 0.37g concentrated HCl obtains is 86m 2 / g; the pore volume is 0.074cm 3 / g; the macropore diameter is 50-2000nm; the mesopore diameter is 3.22nm and 8.22nm.

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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 hierarchical porous material, in particular to a preparation method and application of an organic phosphonic acid transition metal salt porous material. Novel organic-inorganic hybrid metal oxide and phosphonate (titanium, aluminum, zirconium, etc. salts) materials are used for the adsorption of heavy metal ions. Background technique [0002] Porous materials, such as molecular sieves, have been widely concerned due to their large specific surface area and ordered pore structure, and have been tried to be applied in research fields such as catalysis, adsorption, separation and sensors. CN1387942A discloses a kind of preparation method of high adsorption titanium silicate, adopts ethyl orthosilicate as silicon source, polyethylene glycol (PEG-600) is additive, synthesizes a kind of silicic acid with nanoporous structure step by step titanium. This method must strictly control the hydrolysis conditions, the...

Claims

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Application Information

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