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Method for preparing size-controllable easily-peelable layered nanometer zirconium phosphate

A layered nanotechnology, easy-to-peel technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of high crystallinity, complex process, poor effect, etc., to achieve easy process control, simple preparation process, Overcome difficult peeling effects

Active Publication Date: 2018-09-04
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method first synthesizes ordinary zirconium phosphate, which is in a stacked state, contains a large number of hydroxyl groups on the surface, and has a large interlayer force, then uses an intercalation agent for pre-intercalation, and then peels off. The process is relatively complicated. And the effect is not good, the synthesized α-ZrP has high crystallinity, large crystal particle size, uncontrollable sheet size

Method used

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  • Method for preparing size-controllable easily-peelable layered nanometer zirconium phosphate
  • Method for preparing size-controllable easily-peelable layered nanometer zirconium phosphate
  • Method for preparing size-controllable easily-peelable layered nanometer zirconium phosphate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034]Prepare 60 mL of concentrated phosphoric acid with a concentration of 3 mol / L, add 6.00 g of zirconium oxychloride, 6.00 g of methylamine, and 0.20 g of sodium dodecylbenzenesulfonate, and mechanically stir at a speed of 300 r / min for 20 min to fully disperse it. Then the mixed solution was poured into a hydrothermal reaction kettle (100 mL), and reacted at 200° C. for 3 h. After the reaction, the mixed solution was naturally cooled to room temperature. Pour off the supernatant, and centrifuge the milky white precipitate in the lower layer (10000r / min, 10min) to separate the solid from the liquid. The obtained solid product is washed with an appropriate amount of deionized water, and then centrifuged. Repeat the above centrifugation treatment and deionized water washing steps 4 times to make the pH of the centrifuged supernatant ≥ 5. The washed solid product was dried in an oven at 80°C for 12 hours, and then observed by scanning electron microscope, X-ray diffraction a...

Embodiment 2

[0037] Prepare 60 mL of concentrated phosphoric acid with a concentration of 6 mol / L, add 6.00 g of zirconium sulfate, 6.00 g of ethylenediamine, and 0.20 g of sodium dodecylbenzenesulfonate, stir mechanically at a speed of 500 r / min for 20 min to fully disperse it, and then The mixed solution was poured into a hydrothermal reaction kettle (100 mL), and reacted at 150° C. for 12 h. After the reaction, the mixed solution was naturally cooled to room temperature. Pour off the supernatant, and centrifuge the milky white precipitate in the lower layer (10000r / min, 10min) to separate the solid from the liquid. The obtained solid product is washed with an appropriate amount of deionized water, and then centrifuged. Repeat the above centrifugation treatment and deionized water washing steps 3 times to make the pH of the centrifuged supernatant ≥ 5. The washed solid product was dried in an oven at 80°C for 12 hours, and then subjected to scanning electron microscope observation, X-ra...

Embodiment 3

[0040] Prepare 75mL of concentrated phosphoric acid with a concentration of 3mol / L, add 10.00g of zirconium carbonate, 7.50g of ethylenediamine, and 0.75g of octadecyltrimethylammonium bromide, and mechanically stir for 30min at a speed of 300r / min to fully disperse , and then the mixed solution was poured into a hydrothermal reactor (100 mL), and reacted at 250° C. for 36 h. After the reaction, the mixed solution was naturally cooled to room temperature. Pour off the supernatant, and centrifuge the milky white precipitate in the lower layer (10000r / min, 10min) to separate the solid from the liquid. The obtained solid product is washed with an appropriate amount of deionized water, and then centrifuged. Repeat the above centrifugation treatment and deionized water washing steps 4 times to make the pH of the centrifuged supernatant ≥ 5. The washed solid product was dried in an oven at 80°C for 12 hours, and then subjected to scanning electron microscope observation, X-ray diff...

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Abstract

The invention discloses a method for preparing size-controllable easily-peelable layered nanometer zirconium phosphate. The method comprises the following steps: adding phosphoric acid or metal phosphate into deionized water to prepare a solution with a concentration of 3 to 12 mol / L, then adding a water-soluble inorganic zirconium salt, a surfactant and an intercalator, and carrying out mechanical stirring at a rotating speed of 200 to 500 r / min for 20-30 min so as to realize sufficient dispersion; transferring a mixed solution obtained in the previous step mixture to a hydrothermal reactionkettle and carrying out a reaction at 150-250 DEG C for 3-72 h; after the completion of the reaction, naturally cooling the mixed solution to room temperature; and subjecting a white precipitate to centrifugation, washing with water, and drying successively so as to obtain size-controllable easily-peelable layered nanometer zirconium phosphate. Compared with the prior art, the invention has the following advantages: water is used as a reaction medium, and a fluorine-containing compound is not used; the preparation method is simple in process; and the prepared zirconium phosphate has a controllable size in a range of 100 to 3000 nm, high crystallinity, regular structure, easiness in peeling during processing and good compatibility with polymers.

Description

technical field [0001] The invention relates to a nanometer two-dimensional layered metal compound and a preparation method thereof, in particular to a preparation method of a size-controllable and easy-to-peel layered nanometer zirconium phosphate. Background technique [0002] Layered nano-zirconium phosphate is a new type of two-dimensional nanomaterial with excellent ion exchange, adsorption and solid acid catalysis properties, and can be used in the atomic energy industry (collection of radioactive elements), chemical materials (catalyst or catalyst carrier), Medical and health (drug intermediates, antibacterial agents, raw materials for hemodialysis machines) and other fields. In addition, due to the layered nano zirconium phosphate has a large number of Acid point (H + ) and Lewis acid point (Zr 4+ ), which will catalyze the cross-linking of polymers into charcoal during the high temperature process, forming a dense protective layer to block the transfer of oxygen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L23/12C08K3/32C01B25/37B01J27/16
Inventor 赖学军李佳欣曾幸荣李红强谢华理刘韫聪
Owner SOUTH CHINA UNIV OF TECH
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