Method of preparing layered alpha-titanium phosphate

A titanium phosphate and layered technology, which is applied in the field of preparation of layered α-titanium phosphate, can solve the problems of potential safety hazards for operators, high requirements for corrosion resistance of equipment, and low crystallinity of products, and achieve low production costs and high equipment efficiency. The effect of low requirements and broad application prospects

Inactive Publication Date: 2007-09-12
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the methods for preparing layered titanium phosphate mainly include reflux method and hydrofluoric acid method, but these two methods have disadvantages such as long reaction time, low product crystallinity, high requirements on corrosion resistance of equipment, and potential safety hazards for operators.

Method used

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  • Method of preparing layered alpha-titanium phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1, the preparation of layered α-titanium phosphate

[0016] Slowly add 8.5g of tetrabutyl titanate dropwise into 50mL of deionized water to make it fully hydrolyzed, filter and wash the hydrolyzed precipitate 3 times, then add 9.8g of 85% H 3 PO 4 solution and 10mL deionized water, at this time the H in the mixture 3 PO 4 The concentration of the mixture was 5.5mol / L, and then the mixture was transferred to a polytetrafluoroethylene-lined stainless steel autoclave, placed in an incubator, reacted at 180°C for 16 hours, cooled to room temperature, and centrifuged with deionized water Wash until the pH value is 3.8, and finally dry the product at 50°C to obtain layered α-titanium phosphate.

[0017] Sampling, scanning electron microscope (SEM) and X-ray diffraction (XRD) analysis are carried out to the layered α-titanium phosphate prepared by the above-mentioned method, scanning electron microscope observation result is as shown in Figure 1 (figure A is the ...

Embodiment 2

[0018] Embodiment 2, preparation of layered α-titanium phosphate

[0019] Slowly add 7.11 g of tetraisopropyl titanate dropwise into 40 mL of deionized water to make it fully hydrolyzed, filter and wash the hydrolyzed precipitate 5 times, then add 31.16 g of 85% H 3 PO 4 solution and 10mL deionized water, at this time the H in the mixture 3 PO 4 The molar concentration is 10mol / L. Transfer the mixture to a polytetrafluoroethylene-lined stainless steel autoclave, put it in a thermostat, react at 150°C for 24 hours, cool to room temperature, and wash with deionized water until the pH value is 7, and finally the product is dried at 60° C. to obtain layered α-titanium phosphate.

[0020] Sampling was carried out to the layered α-titanium phosphate prepared by the above method for scanning electron microscopy and X-ray diffraction analysis. The test results showed that the above method had obtained a product with good crystallinity, regular and uniform shape, uniform and fine pa...

Embodiment 3

[0021] Embodiment 3, preparation of layered α-titanium phosphate

[0022] Slowly add 5.70 g of ethyl titanate dropwise into 30 mL of deionized water to fully hydrolyze it, filter and wash the hydrolyzed precipitate 4 times, then add 14.3 g of 85% H 3 PO 4 solution and 10mL deionized water, at this time the H in the mixture 3 PO 4 The molar concentration is 7mol / L. Transfer the mixture to a polytetrafluoroethylene-lined stainless steel autoclave, put it in a constant temperature box, react at 200°C for 4 hours, cool to room temperature, and wash with deionized water until the pH value is 6, and finally the product is dried at 70° C. to obtain layered α-titanium phosphate.

[0023] Sampling was carried out to the layered α-titanium phosphate prepared by the above method for scanning electron microscopy and X-ray diffraction analysis. The test results showed that the above method had obtained a product with good crystallinity, regular and uniform shape, uniform and fine partic...

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Abstract

This invention discloses a method for preparing laminated alpha-Ti3(PO4)2, which mixes Ti salt with deionized water in the proportion of 1 :4-10 to get deposit after being hydrolyzed fully to be cleaned and mixed in the proportion of 1 : 20-30 : 3-15, then the concentration of H3PO4 in the mixed solution is 4-12mol/L, then transfers the mixed solution into a high pressure kettle and reacts for 4-24 h under 150-200deg.C to be cooled to room temperature t obe cleaned to 3-7 pH value to be dried to get laminated alpha-Ti3(PO4)2.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to a preparation method of layered alpha-titanium phosphate. Background technique [0002] Layered α-titanium phosphate (α-Ti(HPO 4 ) 2 ·H 2 O) is a cationic compound, which has the characteristics of high temperature resistance, radiation resistance, strong acid resistance, insoluble in water and organic solvents, etc. In addition, the compound has the same ion exchange performance as ion exchange resin, such as can be used for recycling Separating cesium and strontium isotopes, extracting potassium and cesium from seawater, and having the same selective adsorption and catalytic properties as zeolite, at the same time, its phosphate layer is also the substrate for preparing intercalation compounds and layered column catalytic materials. Compared with layered α-zirconium phosphate, layered α-titanium phosphate is easier to delaminate and colloid, which is more conducive to th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/26C01G23/00
Inventor 程萍邓长生戴遐明李冰
Owner TSINGHUA UNIV
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