Method for preparing zirconium phosphate

A technology of zirconium phosphate and zirconium salt, applied in the field of preparing zirconium phosphate α-Zr2·H2O, can solve the problems of long reaction time, high reaction temperature and harsh conditions, and achieve the effect of saving raw materials, quick effect and low consumption of raw materials

Inactive Publication Date: 2006-10-25
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these methods avoid the use of highly corrosive HF, the reaction temperature is high, the reaction time is long, and the conditions are harsh.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 22g ZrOCl in 300ml pure water 2 ·8H 2 After O is dissolved, add 5ml 40wt% HF, then put in 15ml85wt% H 3 PO 4 , heat up to 80°C while stirring and keep for 2 hours, after cooling, filter and wash with pure water until the liquid pH ≈ 6, dry at 75°C, then conduct lens observation, particle size analysis and X-ray diffraction analysis, the result is the average particle size In 1.3μm hexagonal flake α-Zr(HPO 4 ) 2 ·H 2 O.

Embodiment 2

[0027] at 3m 3 Reactor, add 2.75m 3 Deionized water, put in 225Kg ZrOCl 2 ·8H 2 O, add 75Kg 40wt% HF after dissolving, then put 245Kg 85wt% H 3 PO 4 , under stirring at 60r / min, the temperature was raised at a rate of 20°C / h, and kept at 80°C for 3 hours, then unloaded from the reactor and cooled to room temperature, filtered and washed, and then sampled for lens observation, particle size analysis and X-ray diffraction analysis , the result is hexagonal flake α-Zr(HPO 4 ) 2 ·H 2 O.

Embodiment 3

[0029] Dissolve 1mol of zirconium carbonate in 4000ml of water, add 1mol of 40wt% HF aqueous solution and 2mol of 85wt% H 3 PO 4; Stir the mixture at 60°C for 4 hours; filter after cooling, wash with water until the pH of the washing liquid is ≈ 6, and dry to obtain zirconium phosphate α-Zr (HPO 2 ) 2 ·H 2 O crystals. Then carry out lens observation, particle size analysis and X-ray diffraction analysis. 4 ) 2 ·H 2 O.

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Abstract

The invention relates to a method for preparing zirconium phosphate α-Zr (HPO 4 ) 2 ・H 2 O's method. In this method, 1mol of soluble zirconium salt is dissolved in 4000-5000ml of water, and 1-2mol of 40wt% HF aqueous solution and 2-3mol of 85wt% H 3 PO 4 ; Then stir the mixture at 60-90°C for 2-4 hours; filter after cooling, wash with water until the pH of the washing liquid is ≈ 6, and dry to obtain zirconium phosphate α-Zr (HPO 4 ) 2 ・H 2 O crystals. This method uses the complexation catalysis of a small amount of hydrofluoric acid, and uses the minimum ZrOCl at a low temperature (60-90°C). 2 ・8H 2 O / H 3 PO 4 Raw material ratio, manufacture sub-micron to several micron α-Zr(HPO 4 ) 2 ・H 2 O crystal powder, compared with the prior art, has the advantage of only using a small amount of hydrofluoric acid and concentrated phosphoric acid, which not only saves raw materials but also reduces environmental pollution, while also maximizing production safety; the reaction The reaction temperature is low, the reaction time is short, the energy consumption is low, and the cost is low.

Description

technical field [0001] The invention relates to a method for preparing zirconium phosphate α-Zr (HPO 4 ) 2 ·H 2 O's method. Background technique [0002] Zirconium phosphate α-Zr(HPO 4 ) 2 ·H 2 O crystal is an excellent cation exchanger, widely used in atomic energy industry (collection of radioactive elements), chemical industry (catalyst carrier), medicine and health (medicine intermediate carrier, antibacterial agent, raw material for hemodialysis machine) and other fields. [0003] Currently, the preparation of zirconium phosphate α-Zr (HPO 4 ) 2 ·H 2 The HF method is often used for O crystals. The soluble zirconium salt (zirconium oxychloride or zirconium nitrate) is dissolved in hydrofluoric acid ((HF), and after adding phosphoric acid, the product is obtained under heating and stirring. For example, document 1 (.J .Inorg.Nucl.Chem.30,317,1968), 5.5g ZrOCl 2 ·8H 2 O was dissolved in 80ml of water, and 4ml of 40% hydrofluoric acid and 46ml of 85% concentrated...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/00C01B25/26
Inventor 陈运法李自强吴镇江叶树峰谢裕生
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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