CN102659163B - Technological method for preparing cerium carbonate with high content of rare earth in one step - Google Patents
Technological method for preparing cerium carbonate with high content of rare earth in one step Download PDFInfo
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- CN102659163B CN102659163B CN201210139102.2A CN201210139102A CN102659163B CN 102659163 B CN102659163 B CN 102659163B CN 201210139102 A CN201210139102 A CN 201210139102A CN 102659163 B CN102659163 B CN 102659163B
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Abstract
The invention relates to a technological method for preparing cerium carbonate with the high content of rare earth in one step, belonging to the field of rare earth wet-process metallurgy. The technological method comprises the following steps of: preparing the cerium carbonate with the high content of rare earth in one step, i.e. heating a cerium feed solution with the mass concentration of CeO240-90g/L to 95 DEG C to 105 DEG C, and adding ammonium bicarbonate under a continuous stirring condition to precipitate out the cerium carbonate, wherein the optimal addition amount of the ammonium bicarbonate leads the pH value of the feed solution to be adjusted to be 6.3-6.5, and the optimal addition speed of the ammonium bicarbonate leads the feed solution not to overflow from a tank; and carrying out centrifuge dripping on generated precipitates to obtain the cerium carbonate with the high content of rare earth. The technological method has the advantages that the operation is simple, the production period is short, only few water is needed for preparing the feed solution, water consumption is little, the total content of the rare earth of the produced cerium carbonate can be up to 72%-74%, the quality is stable, and the industrial production is easily realized.
Description
Technical field
The present invention relates to a step and prepare the processing method of high total amount of rare earth cerous carbonate,, belong to rare-earth wet method field of metallurgy.
Technical background
In rare-earth industry is produced, cerous carbonate is to prepare multiple cerium product as the intermediate raw material of various cerium salt and cerium oxide, and its purposes is very extensive, is a kind of important light rare earths product.The cerous carbonate that current industrial routine is produced, after drying, total amount of rare earth is only 42~46%, has limited the production efficiency of cerous carbonate.
Chinese patent CN 101481131A discloses a kind of method that two-step approach is prepared high total amount of rare earth cerous carbonate, this invention the first step is that to add concentration be that bicarbonate of ammonia or the sodium carbonate solution of 80~160g/L is settled out cerous carbonate to 40~80g/L Cerium II Chloride feed liquid by concentration, the add-on of bicarbonate of ammonia or sodium carbonate is 1.5~1.8 times of rare-earth oxidation amount, be 1 by solid-liquid mass ratio: (5~15), washing is at least one times; Second step is 1 by cerous carbonate by solid-liquid mass ratio: (2~3) are warmed up to after sizing mixing more than 97 ℃, and constant temperature 2~3.5h is 1 by solid-liquid mass ratio: (5~10), wash at least one times centrifuge dripping.The cerous carbonate total amount of rare earth that the method is produced can reach more than 70%, but the production cycle is longer, and water loss is large.
Summary of the invention
The object of the present invention is to provide a kind of water loss few, steady quality, after the cerous carbonate centrifuge dripping of production, without airing or oven dry, its total amount of rare earth can reach 72%~74%, and the simple step of technique is prepared the processing method of high total amount of rare earth cerous carbonate.
For achieving the above object, the present invention by the following technical solutions:
Processing method is as follows: preparing high total amount of rare earth cerous carbonate by single stage method, is CeO by mass concentration
2the cerium feed liquid of 40~90g/L is heated to 95 ℃-105 ℃, under constantly stirring, add ammonium bicarbonate precipitation to go out cerous carbonate, the amount of the bicarbonate of ammonia adding is so that the pH value of feed liquid is finally adjusted to 6.3~6.5, add speed not emit groove to be advisable with feed liquid, will after the precipitation centrifuge dripping of generation, obtain high total amount of rare earth cerous carbonate.
Described cerium feed liquid is at least one in the Cerium II Chloride aqueous solution, the cerous sulfate aqueous solution or the cerous nitrate aqueous solution.
The bicarbonate of ammonia that the present invention adds is solid or ammonium bicarbonate aqueous solution.
The invention has the advantages that:
Processing method is simple to operate, with short production cycle, only needs a small amount of water preparation feed liquid, and water loss is few, and its total amount of rare earth of the cerous carbonate of production can reach 72%~74%, and steady quality is easy to realize suitability for industrialized production.
Embodiment
Embodiment 1
Be CeO by mass concentration
2the Cerium II Chloride aqueous solution of 70g/L is heated to 95-102 ℃, and then under constantly stirring, adding mass concentration is the ammonium bicarbonate aqueous solution of 160g/L, and input speed does not emit groove to be advisable with cerium feed liquid, until cerium material liquid pH is adjusted to 6.3~6.5.By the precipitation centrifuge dripping generating, products obtained therefrom total amount of rare earth is 72.15%.
Embodiment 2
Be CeO by mass concentration
2the cerous sulfate aqueous solution of 70g/L is heated to 95-102 ℃, and then under constantly stirring, adding mass concentration is the ammonium bicarbonate aqueous solution of 160g/L, and input speed does not emit groove to be advisable with cerium feed liquid, until cerium material liquid pH is adjusted to 6.3~6.5.By the precipitation centrifuge dripping generating, products obtained therefrom total amount of rare earth is 73.38%.
Embodiment 3
Be CeO by mass concentration
2the cerous nitrate aqueous solution of 70g/L is heated to 95-102 ℃, and then under constantly stirring, adding mass concentration is the ammonium bicarbonate aqueous solution of 160g/L, and input speed does not emit groove to be advisable with cerium feed liquid, until cerium material liquid pH is adjusted to 6.3~6.5.By the precipitation centrifuge dripping generating, products obtained therefrom total amount of rare earth is 72.46%.
Embodiment 4
Be CeO by mass concentration
2the cerous nitrate aqueous solution of 70g/L is heated to 95-102 ℃, then under constantly stirring, adds solid ammonium bicarbonate, and input speed does not emit groove to be advisable with cerium feed liquid, until cerium material liquid pH is adjusted to 6.3~6.5.By the precipitation centrifuge dripping generating, products obtained therefrom total amount of rare earth is 74.09%.
Embodiment 5
Be CeO by mass concentration
2the cerous nitrate of 75g/L and the mixed aqueous solution of cerous sulfate (wherein cerous nitrate is 1: 1 with the ratio of the volumetric molar concentration of cerous sulfate) are heated to 95-102 ℃, then under constantly stirring, add solid ammonium bicarbonate, input speed does not emit groove to be advisable with cerium feed liquid, until cerium material liquid pH is adjusted to 6.3~6.5.By the precipitation centrifuge dripping generating, products obtained therefrom total amount of rare earth is 73.51%.
Claims (1)
1. a step is prepared the processing method of high total amount of rare earth cerous carbonate, it is characterized in that: preparing high total amount of rare earth cerous carbonate by single stage method, is CeO by mass concentration
2the cerium feed liquid of 40~90g/L is heated to 95 ℃-105 ℃, under constantly stirring, add ammonium bicarbonate precipitation to go out cerous carbonate, the amount of the bicarbonate of ammonia adding is so that the pH value of feed liquid is finally adjusted to 6.3~6.5, add speed not emit groove to be advisable with feed liquid, reach obtain total amount of rare earth after the precipitation centrifuge dripping of generation at 72%~74% high total amount of rare earth cerous carbonate, wherein cerium feed liquid is at least one in the Cerium II Chloride aqueous solution, the cerous sulfate aqueous solution or the cerous nitrate aqueous solution; The bicarbonate of ammonia adding is solid or ammonium bicarbonate aqueous solution.
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CN103172101B (en) * | 2012-12-13 | 2014-12-17 | 浙江海洋学院 | Preparation method of alkali-type cerous carbonate |
CN105502470B (en) * | 2015-12-31 | 2017-08-04 | 瑞科稀土冶金及功能材料国家工程研究中心有限公司 | A kind of preparation method of low impurity entrainment lanthanum carbonate or lanthanum carbonate cerium |
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CN101898786A (en) * | 2009-05-25 | 2010-12-01 | 甘肃稀土新材料股份有限公司 | Production method of low-Cl-oilless cerium carbonate product with large specific gravity |
CN102019192B (en) * | 2010-10-28 | 2013-07-03 | 内蒙古包钢和发稀土有限公司 | Process method for oil-free cerium carbonate serving as cleaning catalyst for automobile tail gas |
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Effective date of registration: 20200424 Address after: 053500 Hengde Industrial Park, Jingxian County, Hengshui City, Hebei Province Patentee after: North rare earth Huakai hi tech Hebei Co., Ltd Address before: 014010 the Inner Mongolia Autonomous Region Kundulun Baotou Steel Rare Earth Industrial Park Patentee before: BAOTOU HUAMEI RE PRODUCTS Co.,Ltd. |
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