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Sphere analogous alpha-zirconium phosphate and preparing method thereof

A technology of zirconium phosphate and spherical shape, which is applied in the field of preparation of spherical zirconium phosphate materials, can solve the problem of less α-zirconium phosphate, and achieve the effects of easy operation, mild synthesis conditions and simple operation

Active Publication Date: 2009-08-26
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are very few studies on the formation of α-zirconium phosphate
At present, there is only one report (Florent Carn, Alain Derre', Wilfrid Neri, Odile Babot, Herve'Deleuzeb, Re'nal Backov, New J.Chem., 2005, 29) about the preparation of α-zirconium phosphate foam in the domestic and foreign literature. 1346-1350)

Method used

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  • Sphere analogous alpha-zirconium phosphate and preparing method thereof
  • Sphere analogous alpha-zirconium phosphate and preparing method thereof
  • Sphere analogous alpha-zirconium phosphate and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 4.5gZrOCl 2 ·8H 2 O is dissolved in 125ml concentration of 2mol / L hydrochloric acid solution, and the molar concentration is 4mol / L phosphoric acid 15ml and the molar concentration is 2mol / L hydrochloric acid 25ml is mixed to prepare mixed acid solution; ZrOCl 2 The salt solution was slowly added dropwise into the mixed acid solution to obtain a zirconium phosphate gel; it was added into 80ml of 85% phosphoric acid solution by mass and mixed uniformly, stirred and refluxed for 16 hours at a temperature of 90°C, separated and dried. That is, the original powder of α-zirconium phosphate is obtained.

[0029] Dissolve 3.6 g of the dried α-zirconium phosphate raw powder sample in 200 ml of deionized water, add 2 ml of methylamine solution with a concentration of 6 g / L dropwise, then ultrasonicate the formed gel for 0.5 hour, and place it at room temperature for 4 One day, the exfoliated α-zirconium phosphate colloid was obtained.

[0030] The obtained exfoliated zirconiu...

Embodiment 2

[0033] 5.5gZrOCl 2 ·8H 2 O is dissolved in 125ml concentration and is 2mol / L hydrochloric acid solution, the phosphoric acid 25ml that molar concentration is 4mol / L is mixed with the hydrochloric acid 25ml that molar concentration is 2mol / L to prepare mixed acid solution; ZrOCl 2 The salt solution is slowly added dropwise into the mixed acid solution to obtain zirconium phosphate gel; it is added to 50ml of phosphoric acid solution with a mass percentage of 85% and mixed evenly, and stirred and refluxed for 3 days at a temperature of 80°C to obtain α - Raw powder of zirconium phosphate.

[0034] Dissolve 2 g of the dried α-zirconium phosphate raw powder sample in 200 ml of deionized water, add 1 ml of ethylamine solution with a concentration of 5 g / L dropwise, then ultrasonicate the formed gel for 1 hour, and finally place it at room temperature for 4 One day, the exfoliated α-zirconium phosphate colloid was obtained.

[0035] The obtained exfoliated zirconium phosphate col...

Embodiment 3

[0037] 7gZrOCl 2 ·8H 2 O is dissolved in 125ml of hydrochloric acid solution with a concentration of 2.3mol / L, 35ml of phosphoric acid with a molar concentration of 4mol / L and 25ml of hydrochloric acid with a molar concentration of 2mol / L are mixed to prepare a mixed acid solution; ZrOCl 2 Slowly add the salt solution into the mixed acid solution to obtain a zirconium phosphate gel; add it to 100ml of 85% phosphoric acid solution by mass and mix evenly, and stir and reflux for 4 days at a temperature of 70°C to obtain α- Zirconium phosphate raw powder.

[0038] Dissolve 5 g of the dried α-zirconium phosphate raw powder sample in 300 ml of deionized water, add 3 ml of methylamine solution with a concentration of 5.5 g / L dropwise, then ultrasonicate the formed colloid for 1.5 hours, and finally place it at room temperature for 4 One day, the exfoliated α-zirconium phosphate colloid was obtained.

[0039] The obtained exfoliated zirconium phosphate colloid was formulated into ...

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Abstract

The invention relates to a method for preparing a quasi-spherical zirconium phosphate material. In particular, it relates to a quasi-spherical zirconium phosphate whose particle size can be adjusted between 10 and 100 μm and a preparation method thereof. First, the lamellar zirconium phosphate raw powder is synthesized by the reflux method, and then the layered zirconium phosphate powder sample is peeled off by the method of organic amine peeling to obtain a single-layer zirconium phosphate colloid, and finally the powder is processed by a rotary spray dryer. Shaped to obtain a quasi-spherical zirconium phosphate sample. The method has unique technological conditions, simple operation and mild synthesis conditions. Shaped zirconium phosphate materials can be used as catalysts, catalyst supports, adsorbents, ion exchangers, and the like.

Description

technical field [0001] The invention relates to a method for preparing a quasi-spherical zirconium phosphate material. In particular, it relates to a quasi-spherical zirconium phosphate whose particle size can be adjusted between 10 and 100 μm and a preparation method thereof. The zirconium phosphate material can be used as a catalyst, a catalyst carrier, an adsorbent, an ion exchanger, and the like. Background technique [0002] In recent years, the application of nanomaterials has become more and more extensive. Among various nanomaterials, layered compounds with nanoscale interlayer spacing present a wide range of fields due to their unique intercalation reaction characteristics and rich and excellent physical and chemical properties. The development prospects of layered compounds have become research hotspots at home and abroad in the fields of science and technology and industry. Zirconium phosphate compounds are a large class of multifunctional layered materials deve...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/26B01J27/18B01J32/00B01J20/02
Inventor 张法智王晓颖徐庆红段雪义建军
Owner PETROCHINA CO LTD
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