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A kind of preparation method of low impurity entrained lanthanum carbonate or lanthanum cerium carbonate

A technology of lanthanum cerium carbonate and lanthanum carbonate, which is applied in rare earth metal carbonate, chemical instruments and methods, rare earth metal compounds, etc., can solve the problems of increasing process links, cerium oxidation loss, and large human injury, and improve product quality. Effect

Active Publication Date: 2017-08-04
NAT ENG RES CENT OF RARE EARTH METALLURGY & FUNCTION MATERIALS +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is also possible to use this technology to cause cerium oxidation loss
In addition, copper impurities in the rare earth chloride solution are often removed by sulfide precipitation technology. During the production process of this technology, highly toxic gas hydrogen sulfide with the smell of rotten eggs will be released, which is harmful to the human body.
At the same time, these methods have increased the process links, thereby increasing the processing cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Using 282.5g / L lanthanum chloride solution as the raw material solution, the manganese dioxide content in the raw material solution is 0.23g / L, and the copper oxide content is 18mg / L. Use 2.5mol / L ammonium bicarbonate as the precipitant solution. Leave fresh water at the bottom of the precipitation reactor, and add lanthanum carbonate seeds with a manganese dioxide content < 0.0010 wt % and a copper oxide content < 0.0010 wt % according to the seed crystal REO: the raw material liquid REO is 5 wt %. At 20°C, add rare earth chloride and ammonium bicarbonate solution into the reaction kettle at the same time, the ratio of the addition rate is 2:1, the pH value of the precipitation reaction is ≤6.0, and the pH value of the precipitation end point is 6.6~6.8. The ammonium bicarbonate solution was added for 2 hours, and the reaction was completed by aging for 1 hour. Solid-liquid separation and washing with a small amount of water to obtain a lanthanum carbonate product wit...

Embodiment 2

[0018] Using 282.5g / L lanthanum chloride solution as the raw material solution, the manganese dioxide content in the raw material solution is 0.23g / L, and the copper oxide content is 18mg / L. Use 3.0mol / L ammonium bicarbonate as the precipitant solution. Leave the carbon supernatant at the bottom of the precipitation reactor, and add lanthanum carbonate seeds with manganese dioxide content < 0.0010 wt % and copper oxide content < 0.0010 wt % according to the amount of seed crystal REO: raw material liquid REO is 1 wt %. At 40°C, add rare earth chloride and ammonium bicarbonate solution into the reaction kettle at the same time, the ratio of the addition rate is 1:1, the pH value of the precipitation reaction is ≤ 6.0, the addition time of the ammonium bicarbonate solution is 5 hours, and the pH value at the end of the precipitation is 6.2~6.4. Solid-liquid separation and washing with a small amount of water yielded a lanthanum carbonate product with a total REO content of 45.7...

Embodiment 3

[0020] Using 267.5g / L lanthanum cerium chloride solution as the raw material solution, the manganese dioxide content in the raw material solution is 0.44g / L, and the copper oxide content is 22mg / L. Use 2.5mol / L ammonium bicarbonate as the precipitant solution. Keep tap water at the bottom of the precipitation reactor as the bottom liquid, and add lanthanum cerium carbonate seed crystals with a manganese dioxide content of 0.0017 wt % and a copper oxide content of ≤0.0020 wt % according to the amount of seed crystal REO: raw material liquid REO is 10 wt %. At 30°C, add the rare earth chloride and ammonium bicarbonate solution into the reaction kettle at the same time, the ratio of the addition rate is 3:1, and the pH value of the precipitation reaction is ≤6.0. The ammonium bicarbonate solution was added for 4 hours, and the pH at the end of the precipitation was 6.2-6.4. After the reaction was completed, solid-liquid separation and washing with a small amount of water resulte...

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Abstract

The invention relates to a preparation method of low-impurity-entrainment lanthanum carbonate or cerium lanthanum carbonate. The preparation method is characterized in that a lanthanum carbonate or cerium lanthanum carbonate solution is taken as a feed solution, an ammonium bicarbonate solution is taken as an ammonium bicarbonate, and new water or carbon precipitation supernatant is left at the bottom of a precipitation reaction kettle to serve as a base solution. The preparation method comprises the following steps: adding lanthanum carbonate or cerium lanthanum carbonate seed crystal in which seed crystal REO (Rare Earth Oxide) to feed solution REO is 1 percent by weight to 10 percent by weight; adding rare earth chloride and the ammonium bicarbonate solution into a reaction kettle at the same time at 20-50 DEG C to carry out a precipitation reaction, wherein the adding rate ratio is 1:1-3:1; at the end of the reaction, performing solid-liquid separation and water washing to obtain a carbonate lanthanum or cerium lanthanum carbonate product. The preparation method has the advantages that the process parameters of feeding way, relative feeding rate, precipitation pH value and final pH value of a ammonium bicarbonate precipitation lanthanum carbonate or cerium lanthanum carbonate solution are adjusted, so that manganese, copper and the like do not undergo the precipitation reaction, and the formed carbonate lanthanum or cerium lanthanum carbonate product has the characteristics of less soft agglomeration, small crystalline grain size and less entrainment of manganese and copper impurities.

Description

technical field [0001] The invention relates to a method for preparing low-impurity entrained lanthanum carbonate or lanthanum-cerium carbonate, which belongs to the field of hydrometallurgy. Background technique [0002] In the high-temperature roasting and decomposition process of concentrated sulfuric acid for rare earth concentrate, during the removal of impurities in sulfuric acid and the conversion to rare earth chloride extraction, industrial magnesium oxide is used as a neutralizer and saponification agent, resulting in impurities such as manganese and copper in the mixed rare earth chloride feed solution The content is high. After the mixed rare earth chloride is separated into a single rare earth, the manganese dioxide content in the lanthanum chloride or lanthanum cerium chloride solution reaches 0.2~0.7g / L, and the copper oxide content is 5~30mg / L, resulting in carbonic acid after ammonium bicarbonate precipitation. Impurities such as manganese and copper in lan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00
CPCC01F17/247C01P2006/80
Inventor 崔建国马志鸿田皓许涛侯睿恩乔军张旭霞
Owner NAT ENG RES CENT OF RARE EARTH METALLURGY & FUNCTION MATERIALS