CN106435225A

CN106435225A - Method of dissolving basic zinc carbonate from solid mixture of samaric carbonate and basic zinc carbonate

Info

Publication number: CN106435225A
Application number: CN201610233792.6A
Authority: CN
Inventors: 郝先库; 张瑞祥; 马显东; 赵永志; 刘海旺; 王士智; 刘莎莎; 斯琴毕力格; 许宗泽; 贾红梅
Original assignee: JINGRUI NEW MATERIAL CO Ltd BAOTOU; Baotou Rare Earth Research Institute
Current assignee: JINGRUI NEW MATERIAL CO Ltd BAOTOU; Baotou Rare Earth Research Institute; Santoku Corp
Priority date: 2016-04-15
Filing date: 2016-04-15
Publication date: 2017-02-22

Abstract

The invention relates to a method of dissolving basic zinc carbonate from a solid mixture of samaric carbonate and basic zinc carbonate and belongs to the field of rare earth hydrometallurgy. The method comprises the following steps of: adding a samarium-europium separating rare earth saponification residual liquid containing NH4Cl and a solid mixture of samaric carbonate and basic zinc carbonate into a reaction tank; then adding a solid NH4Cl; adjusting the pH value of the solution to 7 with ammonia water; performing a reaction at a certain time at a reaction temperature of 60 DEG C, wherein the basic zinc carbonate is dissolved into the solution from the solid mixture while samaric carbonate is insoluble; and performing filtration, washing and firing to obtain a samarium oxide product, the ZnO content of which is 0.005%. The method can lower the production cost and simplify the production step, so that industrialization is conveniently realized.

Description

The method dissolving basic zinc carbonate from samaric carbonate and basic zinc carbonate solid mixture

Technical field

The present invention relates to a kind of method dissolving basic zinc carbonate from samaric carbonate and basic zinc carbonate solid mixture, belong to In field of rare earth hydrometallurgy.

Background technology

Current enterprise uses Eu in zinc powder reduction europium-enriched solution³⁺Prepare europium oxide technique, in europium-enriched solution, add zinc powder By Eu³⁺It is reduced into Eu²⁺, and zinc powder is changed into Zn²⁺Enter in earth solution, containing Zn²⁺Earth solution as reduction extraction Feed liquid, at reduction extraction segregation section Zn²⁺As easy extraction component with Sm³⁺、Gd³⁺Return after back extraction Deng trivalent rare earth ions To samarium europium segregation section, Zn²⁺With Sm³⁺Flow out from samarium europium segregation section raffinate together, with ammonium hydrogen carbonate as the precipitating reagent of samarium, obtain To samaric carbonate precipitation, in order to control the content of impure zinc in samaric carbonate precipitation, industrialized production may often be such that samarium incomplete Precipitation, in mother liquor of precipitation of ammonium, reserved concentration is the Sm of 0.01-0.02 mol/L³⁺, after centrifugal solid-liquid separates, filtrate is contained Sm³⁺And Zn²⁺Again with ammonium hydrogen carbonate by Sm³⁺Precipitation is complete, the mixture being precipitated as samaric carbonate and basic zinc carbonate obtaining, In order to reclaim samarium in mixture, use hydrochloric acid to dissolve the mixture of samaric carbonate and basic zinc carbonate, then use N₂₃₅Or P₅₀₇Extraction Separate, obtain without Zn²⁺SmCl₃Solution, this technological operation operation is loaded down with trivial details, relatively costly.

Content of the invention

Present invention aim at providing a kind of side dissolving basic zinc carbonate from samaric carbonate and basic zinc carbonate solid mixture Method, the method is by basic zinc carbonate dissolution from samaric carbonate and basic zinc carbonate solid mixture, prepares ZnO content and is less than The Sm of 0.005%₂O₃Product.

Technical solution：

The present invention adds in retort and contains NH₄More than the samarium europium rare-earth separating saponification of Cl, liquid, samaric carbonate and basic zinc carbonate consolidates Body mixture, NH in liquid more than rare-earth sodium saponification₄Cl concentration is 2.24 mol/L, and more than rare-earth sodium saponification, liquid and solid mixture weight ratio are 10:1, in solid mixture, samaric carbonate and basic zinc carbonate percentage by weight are 90-50%:10-50%, after stirring, adds Solid NH₄Cl, liquid and NH more than rare-earth sodium saponification₄Cl weight ratio is 10:0.41-0.94, NH₄After Cl dissolves, with ammoniacal liquor by solution ph Being formulated to 7, when reaction temperature 60 DEG C, in 4 hours reaction time, basic zinc carbonate is dissolved into solution from solid mixture, carbon Acid samarium does not dissolves, and through filtration, washing, calcination, obtains the samarium oxide product less than 0.005% for the ZnO content.

Invention effect

The present invention adds NH₄Cl and with ammoniacal liquor allotment solution ph be key problem in technology；If the NH adding₄Cl measures deficiency, only Part basic zinc carbonate is dissolved into solution from solid mixture, the NH of addition₄Cl amount too much, can improve basic zinc carbonate Solubility, but basic zinc carbonate can not be completely dissolved, also can increase production cost；If allocating solution ph without ammoniacal liquor, only Small part basic zinc carbonate is had to be dissolved into solution from solid mixture, too high by ammoniacal liquor allotment solution ph, can not be by admittedly In body mixture, basic zinc carbonate is dissolved in solution；So control NH₄Cl addition and with ammoniacal liquor allocate solution ph size, Can be dissolved out basic zinc carbonate from solid mixture, samaric carbonate does not dissolves, it is simple to realize industrialization.

Detailed description of the invention

Embodiment 1

3000 L are added to contain NH in retort₄Cl concentration be 2.24 mol/L samarium europium rare-earth separating saponification more than liquid, add 300 Kg contains 90% samaric carbonate and 10% basic zinc carbonate solid mixture, after stirring, adds 123 kg solid NH₄Cl, NH₄Cl is molten Xie Hou, adds ammoniacal liquor allotment solution ph to be 7, and when reaction temperature 60 DEG C, in 4 hours reaction time, basic zinc carbonate is from solid Mixture is dissolved in solution, and samaric carbonate does not dissolves, and through filtration, washing, calcination, obtains the samarium oxide that ZnO content is 0.002% Product.

Embodiment 2

3000 L are added to contain NH in retort₄Cl concentration be 2.24 mol/L samarium europium rare-earth separating saponification more than liquid, add 300 Kg contains 70% samaric carbonate and 30% basic zinc carbonate solid mixture, after stirring, adds 203 kg solid NH₄Cl, NH₄Cl is molten Xie Hou, adds ammoniacal liquor allotment solution ph to be 7, and when reaction temperature 60 DEG C, in 4 hours reaction time, basic zinc carbonate is from solid Mixture is dissolved in solution, and samaric carbonate does not dissolves, and through filtration, washing, calcination, obtains the samarium oxide that ZnO content is 0.003% Product.

Embodiment 3

3000 L are added to contain NH in retort₄Cl concentration be 2.24 mol/L samarium europium rare-earth separating saponification more than liquid, add 300 Kg contains 50% samaric carbonate and 50% basic zinc carbonate solid mixture, after stirring, adds 282 kg solid NH₄Cl, NH₄Cl is molten Xie Hou, adds ammoniacal liquor allotment solution ph to be 7, and when reaction temperature 60 DEG C, in 4 hours reaction time, basic zinc carbonate is from solid Mixture is dissolved in solution, and samaric carbonate does not dissolves, and through filtration, washing, calcination, obtains the samarium oxide that ZnO content is 0.0035% Product.

Claims

1. the method dissolving basic zinc carbonate from samaric carbonate and basic zinc carbonate solid mixture, it is characterised in that in reaction Tank adds and contains NH₄The solid mixture of liquid, samaric carbonate and basic zinc carbonate, rare-earth sodium saponification more than the samarium europium rare-earth separating saponification of Cl NH in remaining liquid₄Cl concentration is 2.24 mol/L, and more than rare-earth sodium saponification, liquid and solid mixture weight ratio are 10:1, in solid mixture Samaric carbonate and basic zinc carbonate percentage by weight are 90-50%:10-50%, after stirring, adds solid NH₄Cl, rare-earth sodium saponification Remaining liquid and NH₄Cl weight ratio is 10:0.41-0.94, NH₄After Cl dissolves, with ammoniacal liquor, solution ph is formulated to 7, in reaction temperature When 60 DEG C, in 4 hours reaction time, basic zinc carbonate is dissolved into solution from solid mixture, and samaric carbonate does not dissolves, through filtering, Washing, calcination, obtain the samarium oxide product less than 0.005% for the ZnO content.