Large-particle zirconium phosphate and preparation method thereof
A technology of zirconium phosphate and large particles, which is applied in the direction of chemical instruments and methods, phosphorus compounds, and active ingredients of phosphorus compounds, etc. It can solve problems such as poor ion exchange capacity, and achieve the effects of easy industrialization, large particles, and simple methods
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[0030] The present invention provides a method for preparing large particles of zirconium phosphate, comprising:
[0031] a. Carbonate and zirconium oxychloride are mixed, heated and reacted to generate zirconium carbonate precipitate, and filtration to obtain zirconium carbonate;
[0032] b, the zirconia carbonate is mixed with the alkali solution to generate a zirconium hydroxide precipitate, filtered to obtain zirconia;
[0033] c, the zirconia hydroxide and phosphoric acid mixed, heating reaction, the formation of zirconium phosphate precipitation, after filtration, washing, drying, to give large particles of zirconium phosphate, the average diameter of 10-50 microns.
[0034] In the above preparation of zirconium carbonate precipitation, the amount ratio of carbonate (preferably sodium carbonate) to the substance of zirconium oxychloride is 2-5 (preferably 3-4). Under stirring, the zirconium oxychloride solution is slowly added to the sodium carbonate solution to form a zirco...
Embodiment 1
[0052]The 64.4g zirconium oxychloride octahydrate was dissolved in 200g pure water, 70.0g sodium carbonate was dissolved in 200g pure water, and the zirconium oxychloride solution was slowly added to the above sodium carbonate solution, stirred, and soon formed a white precipitate of zirconium carbonate gel. Heating and stirring at 90 °C for 2h, controlling the stirring speed of 400r / min, zirconium carbonate is often crystallized completely. Then it is cooled to room temperature, the crystallization is filtered, converted to zirconia with sodium hydroxide solution (containing 16.0g NaOH), and then slowly added to zirconium hydroxide at 70-80 °C and stirred with dilute phosphoric acid (containing 85% phosphoric acid 50 g), and then heated at 80 °C for 1h. Neutralize the excess phosphoric acid with sodium hydroxide, filter and clean the inorganic salts in zirconium phosphate, and then dry in varnish at 60 °C to give a layer of zirconium phosphate 57.8g, a moisture content of 22.9%, ...
Embodiment 2
[0056] 64.4g of zirconium chloride octahydrate was dissolved in 200g of pure water, 64.0g of sodium carbonate was dissolved in 200g of pure water, and the zirconium oxychloride solution was slowly added to the above sodium carbonate solution, stirred, and soon formed a white precipitate of zirconium carbonate gel. Heating and stirring at 90 °C for 2h, controlling the stirring speed of 300r / min, zirconium carbonate is often crystallized completely. Then it is cooled to room temperature, the crystallization is filtered, converted to zirconium hydroxide with sodium hydroxide solution (containing 16.0g NaOH), and then slowly added to zirconium hydroxide at 70-80 °C and stirred with dilute phosphoric acid (containing 85% phosphoric acid), and then heated at 80 °C for 1h. Neutralize the excess phosphoric acid with sodium hydroxide, filter and wash the inorganic salts in zirconium phosphate, and then dry in vacuo at 60 °C to give a layer of zirconium phosphate 56.6g, a moisture content o...
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