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Simple method for preparing sphere analogous alpha-zirconium phosphate

A zirconium phosphate, spherical-like technology, which is applied in the field of simple preparation of spherical-like zirconium phosphate materials, can solve the problems of long process steps, time-consuming, pollution, etc., and achieve easy operation, good repeatability, and simple molding equipment Effect

Inactive Publication Date: 2009-02-25
BEIJING UNIV OF CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the operation, it is necessary to use organic amine solutions harmful to the environment such as methylamine, ethylamine, ethylenediamine, diethylamine, etc. to perform peeling treatment on the layered α-zirconium phosphate powder. The process causes pollution to the environment, and labor protection needs to be strengthened in actual operation, and the process operation steps are long, relatively complicated, and time-consuming

Method used

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  • Simple method for preparing sphere analogous alpha-zirconium phosphate
  • Simple method for preparing sphere analogous alpha-zirconium phosphate
  • Simple method for preparing sphere analogous alpha-zirconium phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A: 4.5g ZrOCl 2 ·8H 2O is dissolved in concentration and is made into 125ml solution in the hydrochloric acid solution of 2mol / L, and the phosphoric acid that molar concentration is 4mol / L and the hydrochloric acid that molar concentration is 2mol / L are mixed according to volume ratio and prepare 125ml mixed acid solution in the ratio of 3 to 5; ZrOCl 2 The salt solution and the mixed acid solution are added to the total back-mixed liquid film reactor at the same time, the slit width between the rotor and the stator of the reactor is adjusted to 0.02mm, the working voltage is 100V, and the rotor speed is 4000rpm, and the obtained mixed slurry is added to the crystallization Stir in the kettle, keep the temperature of the mixed slurry in the kettle at 95-105°C for reflux crystallization for 6 hours, and obtain zirconium phosphate gel;

[0028] Add it into 80ml of 85% phosphoric acid solution by mass, mix evenly, stir and reflux for 16 hours at 90°C, separate and wash t...

Embodiment 2

[0033] A: 5.5g ZrOCl 2 ·8H 2 O is dissolved in concentration and is made into 125ml solution in 2mol / L hydrochloric acid solution, and the phosphoric acid that molar concentration is 4mol / L and the hydrochloric acid that molar concentration is 2mol / L are mixed according to the ratio of 1 to 1 according to volume ratio and prepare 125ml mixed acid solution; ZrOCl 2 The salt solution and the mixed acid solution were added to the total back-mixed liquid film reactor at the same time, the slit width between the rotor and the stator of the reactor was adjusted to 0.03mm, the working voltage was 90V, and the rotor speed was 4000rpm, and the obtained mixed slurry was added to the crystallization Stir in the kettle, keep the temperature of the mixed slurry in the kettle at 95-105°C for reflux crystallization for 6 hours, and obtain zirconium phosphate gel;

[0034] Add it into 50ml of 85% phosphoric acid solution by mass and mix evenly, stir and reflux for 3 days at 80°C, centrifuge...

Embodiment 3

[0038] A: 7gZrOCl 2 ·8H 2 O is dissolved in a hydrochloric acid solution with a concentration of 2mol / L to prepare a 125ml solution, and phosphoric acid with a molar concentration of 4mol / L and hydrochloric acid with a molar concentration of 2mol / L are mixed according to the volume ratio of 7 to 5 to prepare 125ml of mixed acid solution ; ZrOCl 2 The salt solution and the mixed acid solution were placed in a fully back-mixed liquid film reactor, the slit width between the reactor rotor and the stator was adjusted to 0.02mm, the working voltage was 100V, and the rotor speed was 4000rpm, and the obtained mixed slurry was added to the crystallization Stir in the kettle, keep the temperature of the mixed slurry in the kettle at 95-105°C for reflux crystallization for 7 hours, and obtain zirconium phosphate gel;

[0039] Add it into 100ml of 85% phosphoric acid solution by mass, mix evenly, and stir and reflux for 4 days at 70°C to obtain α-zirconium phosphate raw powder.

[004...

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Abstract

The invention discloses a simple making method of sphere-like zirconium phosphate, which comprises the following steps: beating hydrochloric solution of ZrOCl2 and the composite solution of phosphoric acid and alcaine with bulk rate at 1: 1 into full-returned liquid-mixing film reactor to mix; crystallizing through programmed temperature-controlled dynamic crystallizing method; synthesizing nanometer-grade or sub-micron grade layered alpha-zirconium phosphate particle; obtaining the alpha-zirconium phosphate particle to add into certain solid content of alpha-zirconium phosphate colloid slurry to fit for moulding without stripping disposal; moulding and drying through rotary patterned spray drier; obtaining the sphere-like alpha-zirconium phosphate with grain size between 10 and 100um through controlling the spray drying condition to adjust the grain size of the moulding particle.

Description

technical field [0001] The invention relates to a convenient preparation method for preparing spherical zirconium phosphate materials. Background technique [0002] Zirconium phosphate compounds are a large class of multifunctional layered materials developed in recent years, in which α-zirconium phosphate (α-Zr(HPO 4 ) 2 .H 2 O, abbreviated as α-ZrP) is the most representative. The layers of α-zirconium phosphate are stacked together in the way of ABAB. Each layer consists of Zr atoms that are approximately in the same plane, and the upper and lower layers of O that sandwich the Zr atoms 3 P-OH composition. O pointing to the space in the layer 3 The P-OH group shares 3 oxygen atoms with the Zr atom, and its hydrogen proton (P-OH) is acidic and can be exchanged. It has the same ion exchange performance as ion exchange resin. Compared with ion exchange resin, its advantages It has better thermal stability. The water molecules in the layer form hydrogen bonds with the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/26C01G25/00
Inventor 张法智王晓颖段雪徐庆红义建军
Owner BEIJING UNIV OF CHEM TECH
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