Preparation method of zirconium sulfate

Abstract

The invention discloses a zirconium sulfate preparation method, which comprises: carrying out a reaction on crushed zircon sand and sulfuric acid for 3-5 h under a pressurization heating condition, sequentially adding water to wash and filter after the reaction is completed, collecting a filtrate, removing impurities from the filtrate, and crystallizing an obtained zirconium sulfate solution to obtain zirconium sulfate. Zirconium sulfate is prepared by directly reacting zircon sand with sulfuric acid under the conditions of heating and pressurizing, alkali fusion is not adopted, sodium hydroxide or sodium carbonate is avoided, the step of removing sodium is omitted, and high-purity zirconium sulfate can be obtained only through one-time crystallization.

Description

technical field [0001] The invention belongs to the field of zirconium sulfate preparation, in particular to a method for preparing zirconium sulfate. Background technique [0002] Zirconium sulfate is an intermediate product used to prepare other zirconium compounds, and can also be sold as a finished product for rubber, papermaking, leather tanning and other industries. There are many ways to produce zirconium sulfate. The methods for producing zirconium sulfate from zircon are: (1) zircon → alkali fusion → water washing → sulfuric acid leaching → ammonia precipitation → washing to remove sodium → sulfuric acid dissolution → evaporation crystallization → recrystallization → Zirconium sulfate products; (2) Zircon → alkali fusion → water washing → hydrochloric acid leaching → hydrolysis → sulfuric acid dissolution → crystallization → zirconium sulfate products. There are following disadvantages from the above two methods: [0003] (1) Both method 1 and method 2 use alkali ...

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Problems solved by technology

[0003] (1) Both method 1 and method 2 use alkali fusion, and the raw material for alkali fusion is generally sodium hydroxide or sodium carbonate, which increases the subsequent sodium removal step and forms Na 2 [ZrO(SO 4 ) 2 ]·3H 2 The double salt of O is more difficult to remove sodium; (2) method 1 and method 2 both have alkali fusion steps, so it is necessary to increase the step of acid solution leaching. In method 1, sulfuric acid leaching is used, and the amount of sulfuric acid needs to be precisely controlled. Insufficient sulfuric acid, the Na in the transition material 2 ZrSiO 5 It is difficult to leaching, the leaching rate is low, and the silicic acid is not well condensed, it is difficult to filter, the sulfuric acid is too much, the acidity of the leachate is too high, it is difficult to evaporate, and it is easy to form silica gel during the evaporation process, and it is difficult to filter; in the second method, hydrochloric acid is used for leaching, which is easy to cause The production equipment is severely corroded; (3) method one requires recrystallization to obtain high-purity zirconium sulfate, while method two uses low-acid leaching and high-acid dissolution, and the product yield is low