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Production method for ferrum-free Zr(SO4)2

A production method and SO4 technology, applied in zirconium sulfate and other directions, can solve the problems of serious equipment corrosion, incomplete method, difficult filtration, etc., and achieve the effects of small product loss, complete separation and high product purity.

Active Publication Date: 2016-11-09
LIAONING PETROCCHEM VOCATIONAL & TECH COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This separation of Fe 3+ The method is incomplete, Fe(OH) 3 Filtration is difficult, and some Zr(SO 4 ) 2 Also generates Zr(OH) 4 Sedimentation causes loss
Or use the method of adding hydrochloric acid to remove iron, that is, add a certain amount of hydrochloric acid in a crystallization process to make iron form [FeCl 4 ] - It does not form a eutectic with zirconium sulfate and reduces the adsorption by zirconium sulfate to achieve the effect of iron removal. This method has serious equipment corrosion

Method used

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  • Production method for ferrum-free Zr(SO4)2

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] a. The zirconium sulfate solution containing ferrous ions and ferric ions is placed in a container, continuously stirred and added dropwise with a mass fraction of 15% hydroxylamine hydrochloride solution in the container, when thiocyanate is added dropwise to the zirconium sulfate solution When the potassium acid potassium solution is no longer red, it is considered that ferric ions are no longer detected; then the pH value of the solution is adjusted to 4 with a mass fraction of 26% ammonia solution; during this process, the following chemical reaction equation occurs:

[0022] 2Fe 3+ +2NH 2 OH·HCl=2Fe 2+ +N 2 ↑+4H + +2H 2 O+2Cl -

[0023] b. Stir continuously and add dropwise an o-phenanthroline solution with a mass fraction of 8% to the solution reacted in step a, and add potassium ferricyanide dropwise to the solution. When no blue precipitate is generated, it is deemed unsafe Ferrous ions were detected again. Continuously dripping the sodium chloride solut...

Embodiment 2

[0028] a. The zirconium sulfate solution containing ferrous ions and ferric ions is placed in a container, continuously stirred and added dropwise with a mass fraction of 10% hydroxylamine hydrochloride solution in the container, when adding thiocyanate dropwise to the zirconium sulfate solution When the potassium acid potassium solution is no longer red, it is considered that there is no ferric ion detected; then the pH value of the solution is adjusted to 5 with a mass fraction of 25% ammonia solution;

[0029] b. Stir constantly and add dropwise the o-phenanthroline solution with a mass fraction of 5% in the solution reacted in step a, and add potassium ferricyanide dropwise in the solution. Ferrous ions were detected again. Continuously add the calcium chloride solution that mass fraction is 30% in the container again, until there is no precipitation to generate again, after filtering, the liquid of gained is iron-free Zr(SO 4 ) 2 solution;

[0030] c. Put the solid rea...

Embodiment 3

[0032] a. The zirconium sulfate solution containing ferrous ions and ferric ions is placed in a container, continuously stirred and added dropwise with a mass fraction of 20% hydroxylamine hydrochloride solution in the container, when adding thiocyanate dropwise to the zirconium sulfate solution When the potassium acid potassium solution is no longer red, it is considered that ferric ions are no longer detected; then the pH value of the solution is adjusted to 3 with a mass fraction of 28% ammonia solution;

[0033] b. Stir continuously and add dropwise the o-phenanthroline solution with a mass fraction of 10% in the solution reacted in step a, and add potassium ferricyanide dropwise in the solution. Ferrous ions were detected again. Continuously dripping the potassium chloride solution that the mass fraction is 40% in the container again, until there is no precipitation to generate again, after filtering, the gained liquid is iron-free Zr(SO 4 ) 2 solution;

[0034] c. Put...

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Abstract

A disclosed production method for ferrum-free Zr(SO4)2 comprises the following steps: a, putting a zirconium sulfate solution containing a ferrous ion and a ferric ion in a container, dropwise adding an organic reducing agent solution into the container with continuous stirring until no ferric ion is not detected out, and then adjusting the pH value of the solution to 3-5 by using an ammonia water solution; and b, dropwise adding a phenanthroline solution into the solution reacted after step a with continuous stirring until no ferrous ion is detected out, then continuously dropwise adding a soluble chloride solution or a sodium picrate solution into the container until no precipitate is generated, and performing solid-liquid separation, so as to obtain a liquid, that is the ferrum-free Zr(SO4)2 solution. The beneficial effects comprise that the original production technological process does not need changing; Fe is completely separated; the product purity is high; no waste is generated; the precipitant can be recycled and production cost is low; the precipitant selectivity is high and product loss is small; and no Zr(OH)4 precipitate is generated under an acidic condition.

Description

technical field [0001] The present invention relates to a kind of production method of zirconium sulfate, especially a kind of iron-free Zr(SO 4 ) 2 production method. Background technique [0002] The industrial production of zirconium sulfate mainly includes: one is that zircon is sintered or alkali-fused, washed with water, leached with sulfuric acid, precipitated with ammonia water, washed to remove sodium, dissolved with sulfuric acid, evaporated and crystallized, and recrystallized to obtain zirconium sulfate products. The other is to obtain zirconium sulfate products through alkali fusion, water washing, hydrochloric acid leaching, hydrolysis, sulfuric acid dissolution and crystallization of zircon. The above two production processes all need to be pickled, and the metal impurity iron in the raw material reacts with the acid and enters the zirconium sulfate solution, which affects the quality of the product. In industrial iron removal, oxidants are usually added af...

Claims

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Application Information

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IPC IPC(8): C01G25/06
CPCC01G25/06C01P2006/80
Inventor 邸万山
Owner LIAONING PETROCCHEM VOCATIONAL & TECH COLLEGE
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