Method for preparation of pillared zirconium phosphate material by self-assembly technology

A self-assembly technology and zirconium phosphate column technology are applied in the field of preparing zirconium phosphate column support materials to achieve the effect of good pore structure and large specific surface area

Active Publication Date: 2013-01-30
CHANGZHOU XIAOGUO INFORMATION SERVICES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the limitation of the volume of polyhydroxymetallic cations, it is used as a propping agent to synthesize microporous or mesoporous materials of laminated zirconium phosphate. The pore diameter of the obtained laminated materials generally does not exceed 2.5 nm. There are still many difficulties in the synthesis of the range
Due to the limitation of its ion volume, it is used as a propping agent to synthesize microporous or mesoporous materials of laminated zirconium phosphate. The pore diameter of the obtained laminated materials generally does not exceed 2.5nm, and the synthesis of larger mesoporous sizes still face more difficulties
Moreover, the use of polyhydroxy metal cations as propping agents has disadvantages such as difficult control of the column structure and wide pore size distribution.

Method used

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  • Method for preparation of pillared zirconium phosphate material by self-assembly technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1: In a dry 100 mL beaker, 0.3 g of α-ZrP powder was dispersed in 28.5 mL of deionized water, and 1.5 mL of 0.2 mol.L -1 Methylamine aqueous solution, wherein the solid-to-liquid ratio is 1:100 g / mL, the molar ratio of methylamine:α-zirconium phosphate is 0.3:1, and magnetically stirred at room temperature for 2 hours. Add 20mL dropwise to the above solution with a concentration of 0.1 mol.L -1 Cetyltrimethylammonium bromide aqueous solution, wherein the molar ratio of cetyltrimethylammonium bromide: α-zirconium phosphate is 2:1, was magnetically stirred at room temperature for 4 hours. Continue to add 4.5 mL of tetraethyl orthosilicate to the above solution, wherein the molar ratio range of tetraethyl orthosilicate: α-zirconium phosphate is 20:1, and adjust the above-mentioned concentration with 25% concentrated ammonia water after magnetic stirring at room temperature for 1 hour. The pH of the solution was adjusted to 9, and the solid phase was separated by...

Embodiment 2

[0019] Example 2: In a dry 100 mL beaker, 0.3 g of α-ZrP powder was dispersed in 28.5 mL of deionized water, and 1.5 mL of 0.2 mol.L -1 Methylamine aqueous solution, wherein the solid-to-liquid ratio is 1:100 g / mL, the molar ratio of methylamine:α-zirconium phosphate is 0.3:1, and magnetically stirred at room temperature for 2 hours. Add 20mL dropwise to the above solution with a concentration of 0.1 mol.L -1 Cetyltrimethylammonium bromide aqueous solution, wherein the molar ratio of cetyltrimethylammonium bromide: α-zirconium phosphate is 2:1, was magnetically stirred at room temperature for 4 hours. Continue to add 6.7 mL of tetraethyl orthosilicate to the above solution, wherein the molar ratio range of tetraethyl orthosilicate: α-zirconium phosphate is 30:1, and then adjust the above with 25% concentrated ammonia water after magnetic stirring at room temperature for 1 hour. The pH of the solution was adjusted to 9, and the solid phase was separated by suction filtration...

Embodiment 3

[0020] Example 3: In a dry 100 mL beaker, 0.3 g of α-ZrP powder was dispersed in 28.5 mL of deionized water, and then 1.5 mL of 0.2 mol.L -1 Methylamine aqueous solution, wherein the solid-to-liquid ratio is 1:100 g / mL, the molar ratio of methylamine:α-zirconium phosphate is 0.3:1, and magnetically stirred at room temperature for 2 hours. Add 20 mL of 0.1 mol.L to the above solution drop by drop -1 Tetradecyltrimethylammonium bromide aqueous solution, wherein the molar ratio of tetradecyltrimethylammonium bromide: α-zirconium phosphate is 2:1, was magnetically stirred at room temperature for 4 hours. Continue to add 4.5 mL of tetraethyl orthosilicate to the above solution, wherein the molar ratio range of tetraethyl orthosilicate: α-zirconium phosphate is 20:1, and adjust the above-mentioned concentration with 25% concentrated ammonia water after magnetic stirring at room temperature for 1 hour. The pH of the solution was adjusted to 9, and the solid phase was separated by ...

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Abstract

Belonging to the technical field of material preparation, the invention discloses a method for preparation of a pillared zirconium phosphate material by a self-assembly technology. The method consists of: taking layered zirconium phosphate as a raw material, utilizing methylamine to strip the layered zirconium phosphate into single sheets, anchoring cetyl trimethyl ammonium bromide and other long-chain quaternary ammonium salts on single zirconium phosphate sheets, adopting ethyl silicate as a silicon source, making use of cetyl trimethyl ammonium bromide as a template agent to form micelles, employing the self-assembly technology to form intercalated zirconium phosphate with ethyl silicate micelles between layers, and then carrying out calcination to remove the template agent, thus obtaining the silicon oxide pillared zirconium phosphate material. The silicon oxide pillared zirconium phosphate material in the invention has a larger specific surface area and a better pore structure, and the P-OH acid site on a zirconium phosphate laminate surface is well preserved.

Description

technical field [0001] The invention relates to a method for preparing a zirconium phosphate pillar material by using a self-assembly technology, and belongs to the technical field of material preparation. Background technique [0002] Zirconium phosphate compounds are a new class of multifunctional mesoporous materials developed in recent years, and they are one of the most studied materials in the famous family of layered solid acid materials. Layered zirconium phosphate (α-ZrP) is bonded by strong covalent bonds between atoms on the same plane, and atoms between adjacent layers are bonded by van der Waals force. This special form of interlayer force allows Different numbers and types of guests are inserted into the host molecules. When some large-volume ions, ion clusters or molecules are introduced between the host molecules, the formed pillars will stably stretch the laminates, exposing the acidic active sites on the laminates. , forming a class of pillared materials ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
Inventor 陈若愚刘文晋花益香王红宁钟璟刘小华
Owner CHANGZHOU XIAOGUO INFORMATION SERVICES
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