CN104891550A - Method of preparing ceria by mixed precipitant - Google Patents
Method of preparing ceria by mixed precipitant Download PDFInfo
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Abstract
A method of preparing ceria by a mixed precipitant mainly comprises the steps of enabling a mixed solution of ammonium bicarbonate and ammonia as the precipitant to perform combined action with inoculating crystals, precipitating rare earth ions in a rare earth chloride solution to obtain a mixture with primary alkali type cerous carbonate and subsidiary cerous carbonate and cerium hydroxide, and further firing to prepare a rare earth ceria product. The prepared ceria accords with industry standards; reaction conditions of the method are mild; energy consumption during preparing process is obviously reduced, and the cost is low; meanwhile, the carbon dioxide emission is greatly reduced, and obvious social benefit and environmental benefit are achieved.
Description
Technical field
The present invention relates to a kind of separation method of rare earth element, particularly rare-earth wet method metallurgy separation method.
Background technology
Rare earth element is called as " VITAMIN " of modern industry and magical novel material " treasure-house ", and the rare earth of commercially concluding the business 90% is rare earth oxide.Present stage is mainly that rare earth oxide is prepared in intermediate calcination with rare earth carbonate, only calculates from the conversion process of material, prepares 1 ton of cerium dioxide and will discharge carbonic acid gas 767.44 kilograms.Because the whole world is to the attention of carbon dioxide discharge-reduction problem, searching manufacturing cost is lower, CO2 emissions less, the better preparation method of rare earth oxide dispersing property, is more and more subject to the attention of rare earth circle.
Cerium dioxide is mainly used in the stablizer of glass industry, discoloring agent, radiation shielding glass, luminescent material and the various alloy materials of manufacture etc.Prepare in the process of cerous carbonate at use bicarbonate of ammonia, because bicarbonate of ammonia is acid salt, produce corresponding hydrochloric acid in reaction process, its bicarbonate of ammonia added has 50% to play neutralization of acid with base, this not only consumes a large amount of chemical materialss, but also can release a large amount of carbonic acid gas.In the method preparing basic carbonate cerium, usually adopt the synthesis of High Temperature High Pressure hydro-thermal method, application is extremely restricted.Liu Lingyun etc. (rare earth, the 34th volume fourth phase, 95 ~ 97 pages) at high temperature add solid ammonium bicarbonate and prepare basic carbonate cerium, and reaction process foam is large, are temperature requiredly greater than 95 DEG C, and easily bring impurity and foreign material into.The people such as Guo Zhiyan (functional materials, supplementary issue (38 volume) in 2007,2096 ~ 2098 pages) are that carbon source prepares basic carbonate cerium under hydrothermal conditions with urea; preparation process time is long; tooling cost is high, temperature required height, not easily large-scale production.
Summary of the invention
The object of this invention is to provide one and can reduce energy consumption and cost, CO2 emissions can be reduced again and can the method that cerium dioxide be prepared by mixed precipitant of suitability for industrialized production simultaneously.The method is mainly using the mixing solutions of bicarbonate of ammonia and ammoniacal liquor as precipitation agent, itself and crystal seed acting in conjunction, by the rare earth ion precipitation in re chloride, to obtain basic carbonate cerium be main, cerous carbonate and cerous hydroxide is auxiliary mixture, prepares RE CeO 2 product further by calcination.
Main contents of the present invention are as follows:
(1) make raw material with the bicarbonate of ammonia of technical grade and the ammoniacal liquor of technical grade, become the mixed precipitation agent solution of 2.00 ~ 5.50mol/L according to bicarbonate of ammonia integral molar quantity with the proportions of ammoniacal liquor integral molar quantity 55 ~ 25:45 ~ 75;
(2) be 0.60 ~ 1.20mol/L by certain volume concentration, the solution of cerium chloride by oxidation of pH=4 ~ 5 imports in reactive tank, adding using basic carbonate cerium, cerous carbonate and cerous hydroxide is that auxiliary mixture is as crystal seed, the mass percent of each component of this crystal seed is respectively: basic carbonate cerium 90 ~ 95%, cerous carbonate 0 ~ 5% and cerous hydroxide 0 ~ 10%, and its consumption is 10% ~ 20% of required precipitation Cerium II Chloride quality;
(3) solution of cerium chloride by oxidation to 50 ~ 70 DEG C that obtain of heating steps 2, under agitation evenly add the mixed precipitation agent solution that step 1 is prepared, and its consumption is to need on the basis of 3mol mixed precipitant excessive 5 ~ 10% at precipitation 1mol Cerium II Chloride;
(4) control added the time of mixed precipitation agent solution at 4 ~ 10 hours, and reinforced complete continuation stirring 10 minutes controls the pH value of solution terminal 6.6 ~ 8.2;
(5) the basic carbonate cerium obtained by vacuum filtration step 4 is master, cerous carbonate and cerous hydroxide is auxiliary mixed sediment, and carries out drip washing once to throw out, and washing water consumption is at least 4 times of throw out quality;
(6) throw out that step 5 obtains is put into retort furnace calcination, control calcination temperature 400 ~ 650 DEG C, calcination time is 2 ~ 8 hours, obtains cerium dioxide product.
The present invention compared with prior art tool has the following advantages:
1, the basic carbonate cerium that prepared by the method is master, cerous carbonate and cerous hydroxide is auxiliary mixed sediment, and content of rare earth is between 60% ~ 68%.This product has the advantages that size-grade distribution interval is narrow, particle supernatant is filtered soon, easily, content of rare earth is high.Be main, cerous carbonate and cerous hydroxide by basic carbonate cerium be cerium dioxide prepared by auxiliary mixed sediment, pure color, Granular composite evenly, good fluidity, under lower calcination temperature, just can reach the product requirement that content of rare earth is greater than 99.0%.
2, when using mixed precipitant, the addition of ammoniacal liquor is 45 ~ 75%, means the carbonic acid gas 45 ~ 75% by directly reducing precipitation process generation.1 ton of cerium dioxide is prepared in calcination link, common cerous carbonate produces the carbonic acid gas of 383.72kg, and basic carbonate cerium be main, cerous carbonate and cerous hydroxide is that auxiliary mixed sediment produces the carbonic acid gas of 255.81kg and the water vapor of 52.33kg, oxide compound per ton directly reduces by the CO2 emissions of 33%, has obvious social benefit and environmental benefit.
3, basic carbonate cerium to be main, cerous carbonate and cerous hydroxide be auxiliary mixed sediment calcination temperature is lower than the calcination temperature of cerous carbonate, and the energy consumption of calcination process is by reduction by more than 40%.
4, the present invention significantly can reduce the tooling cost of cerium dioxide.One is the raw material preparing bicarbonate of ammonia due to ammoniacal liquor itself, can save bicarbonate of ammonia usage quantity 45 ~ 75%, reduces the traffic capacity of bicarbonate of ammonia, the volume of goods loaded and unloaded and meltage simultaneously; It two is promoted to 60 ~ 68% due to the intermediate product grade preparing cerium dioxide, and make product package material reduce 30%, the transportation cost of unit oxide compound significantly reduces; Its three calcinations energy consumption reduces nature and can cut down finished cost.
5, method reaction conditions of the present invention is gentleer, simple to operate.
Embodiment
Embodiment 1:
The technical grade bicarbonate of ammonia 150Kg of nitrogen content >17% is dissolved in pure water, is mixed with the ammonium bicarbonate soln that volumetric molar concentration is 3.50mol/L.With mass percent concentration be 19.35% technical grade ammoniacal liquor preparation volumetric molar concentration be the ammonia soln of 10.50mol/L.Get above-mentioned ammonium bicarbonate soln and ammonia soln respectively, according to bicarbonate of ammonia integral molar quantity: the proportions of ammoniacal liquor integral molar quantity=45:55 becomes total mol concentration to be the mixed precipitation agent solution 720L of 5.50mol/L.Be 0.60mol/L, pH=4.0 by concentration, volume is that the solution of cerium chloride by oxidation of 2000L imports in reactive tank, be heated to 65 DEG C, add 30Kg crystal seed, this crystal seed contains the basic carbonate cerium of massfraction 94%, the cerous carbonate of 4% and the cerous hydroxide of 2%, under agitation evenly adds above-mentioned compounding conjunction precipitant solution 720L.Controlling feed time is 5 hours, mother liquor terminal pH=7.4, continues stirring 10 minutes.By vacuum filtration, to obtain basic carbonate cerium (94%) be main, cerous carbonate (4%) and cerous hydroxide (2%) is auxiliary mixed sediment, and to throw out drip washing once, washing water consumption is the deionized water of 1350L.Analyzing throw out content of rare earth is 62.43%, throw out is put into retort furnace calcination, and controlling calcination temperature is 650 DEG C, and calcination time 2 hours, obtains cerium dioxide product, and detecting total amount of rare earth is 99.01%.
Embodiment 2:
The technical grade bicarbonate of ammonia 182Kg of nitrogen content >17% is dissolved in pure water, is mixed with the ammonium bicarbonate soln that volumetric molar concentration is 2.98mol/L.With mass percent concentration be 18.56% technical grade ammoniacal liquor preparation volumetric molar concentration be the ammonia soln of 10.10mol/L.Get above-mentioned ammonium bicarbonate soln and ammonia soln respectively, according to bicarbonate of ammonia integral molar quantity: ammoniacal liquor integral molar quantity is that the proportions of 50:50 becomes total mol concentration to be the mixed precipitation agent solution 950L of 4.61mol/L.Be 0.90mol/L, pH=4.5 by concentration, volume is that the solution of cerium chloride by oxidation of 1500L imports in reactive tank, be heated to 65 DEG C, add 25Kg crystal seed, this crystal seed contains the basic carbonate cerium of massfraction 94%, the cerous carbonate of 5% and the cerous hydroxide of 1%, under agitation evenly adds above-mentioned compounding conjunction precipitant solution 950L.Controlling feed time is 4 hours, mother liquor terminal pH=6.8, continues stirring 10 minutes.By vacuum filtration, to obtain basic carbonate cerium (94%) be main, cerous carbonate (5%) and cerous hydroxide (1%) is auxiliary mixed sediment, and to throw out drip washing once, washing water consumption is the deionized water of 1450L.Analyzing throw out content of rare earth is 64.85%, throw out is put into retort furnace calcination, and controlling calcination temperature is 500 DEG C, and calcination time 3 hours, obtains cerium dioxide product, and detecting total amount of rare earth is 99.23%.
Embodiment 3:
The technical grade bicarbonate of ammonia 245Kg of nitrogen content >17% is dissolved in pure water, is mixed with the ammonium bicarbonate soln that volumetric molar concentration is 1.10mol/L.With mass percent concentration be 18.56% technical grade ammoniacal liquor preparation volumetric molar concentration be the ammonia soln of 10.10mol/L.Get above-mentioned ammonium bicarbonate soln and ammonia soln respectively, according to bicarbonate of ammonia integral molar quantity: the proportions of ammoniacal liquor integral molar quantity=50:50 becomes total mol concentration to be the mixed precipitation agent solution 2930L of 2.00mol/L.Be 1.20mol/L, pH=4.5 by concentration, volume is that the solution of cerium chloride by oxidation of 1500L imports in reactive tank, be heated to 60 DEG C, add 31Kg crystal seed, this crystal seed contains the basic carbonate cerium of massfraction 94%, the cerous carbonate of 5% and the cerous hydroxide of 1%, under agitation evenly adds above-mentioned compounding conjunction precipitant solution 2930L.Controlling feed time is 8 hours, mother liquor terminal pH=7.0, continues stirring 10 minutes.By vacuum filtration, to obtain basic carbonate cerium (94%) be main, cerous carbonate (5%) and cerous hydroxide (1%) is auxiliary mixed sediment, and to throw out drip washing once, washing water consumption is the deionized water of 2050L.Analyzing throw out content of rare earth is 60.67%, throw out is put into retort furnace calcination, and controlling calcination temperature is 650 DEG C, and calcination time 2 hours, obtains cerium dioxide product, and detecting total amount of rare earth is 99.26%.
Embodiment 4:
The technical grade bicarbonate of ammonia 157Kg of nitrogen content >17% is dissolved in pure water, is mixed with the ammonium bicarbonate soln that volumetric molar concentration is 2.04mol/L.With mass percent concentration be 18.56% technical grade ammoniacal liquor preparation volumetric molar concentration be the ammonia soln of 10.10mol/L.Get above-mentioned ammonium bicarbonate soln and ammonia soln respectively, according to bicarbonate of ammonia integral molar quantity: the proportions of ammoniacal liquor integral molar quantity=50:50 becomes total mol concentration to be the mixed precipitation agent solution 1120L of 3.38mol/L.Be 0.60mol/L, pH=5.0 by concentration, volume is that the solution of cerium chloride by oxidation of 2000L imports in reactive tank, be heated to 55 DEG C, add 25Kg crystal seed, this crystal seed contains the basic carbonate cerium of massfraction 94%, the cerous carbonate of 5% and the cerous hydroxide of 1%, under agitation evenly adds above-mentioned compounding conjunction precipitant solution 1120L.Controlling feed time is 10 hours, mother liquor terminal pH=7.0, continues stirring 10 minutes.By vacuum filtration, to obtain basic carbonate cerium (94%) be main, cerous carbonate (5%) and cerous hydroxide (1%) is auxiliary mixed sediment, and to throw out drip washing once, washing water consumption is the deionized water of 1260L.Analyzing throw out content of rare earth is 65.95%, throw out is put into retort furnace calcination, and controlling calcination temperature is 425 DEG C, and calcination time 4 hours, obtains cerium dioxide product, and detecting total amount of rare earth is 99.38%.
Embodiment 5:
The technical grade bicarbonate of ammonia 185Kg of nitrogen content >17% is dissolved in pure water, is mixed with the ammonium bicarbonate soln that volumetric molar concentration is 2.70mol/L.With mass percent concentration be 19.35% technical grade ammoniacal liquor preparation volumetric molar concentration be the ammonia soln of 10.50mol/L.Get above-mentioned ammonium bicarbonate soln and ammonia soln respectively, according to bicarbonate of ammonia integral molar quantity: the proportions of ammoniacal liquor integral molar quantity=55:45 becomes total mol concentration to be the mixed precipitation agent solution 950L of 4.05mol/L.Be 0.60mol/L, pH=4.5 by concentration, volume is that the solution of cerium chloride by oxidation of 2000L imports in reactive tank, be heated to 70 DEG C, add 32Kg crystal seed, this crystal seed contains the basic carbonate cerium of massfraction 95% and the cerous carbonate of 5%, under agitation evenly adds above-mentioned compounding conjunction precipitant solution 950L.Controlling feed time is 6 hours, mother liquor terminal pH=6.6, continues stirring 10 minutes.By vacuum filtration, to obtain basic carbonate cerium (95%) be main, cerous carbonate (5%) and cerous hydroxide (0) is auxiliary mixed sediment, and to throw out drip washing once, washing water consumption is the deionized water of 1400L.Analyzing throw out content of rare earth is 60.00%, throw out is put into retort furnace calcination, and controlling calcination temperature is 450 DEG C, and calcination time 3.5 hours, obtains cerium dioxide product, and detecting total amount of rare earth is 99.65%.
Embodiment 6:
Be dissolved in pure water by the technical grade bicarbonate of ammonia 115Kg of nitrogen content >17%, preparation volumetric molar concentration is the ammonium bicarbonate soln of 1.20mol/L.With mass percent concentration be 18.56% technical grade ammoniacal liquor preparation volumetric molar concentration be the ammonia soln of 10.10mol/L.Get above-mentioned ammonium bicarbonate soln and ammonia soln respectively, according to bicarbonate of ammonia integral molar quantity: the proportions of ammoniacal liquor integral molar quantity=34:66 becomes total mol concentration to be the mixed precipitation agent solution 1380L of 2.86mol/L.Be 0.60mol/L, pH=4.5 by concentration, volume is that the solution of cerium chloride by oxidation of 2000L imports in reactive tank, be heated to 60 DEG C, add 41Kg crystal seed, this crystal seed contains the basic carbonate cerium of massfraction 94%, the cerous carbonate of 1% and the cerous hydroxide of 5%, under agitation evenly adds above-mentioned compounding conjunction precipitant solution 1380L.Controlling feed time is 9 hours, mother liquor terminal pH=7.8, continues stirring 10 minutes.By vacuum filtration, to obtain basic carbonate cerium (94%) be main, cerous carbonate (1%) and cerous hydroxide (5%) is auxiliary mixed sediment, and to throw out drip washing once, washing water consumption is the deionized water of 1250L.Analyzing throw out content of rare earth is 68.00%, throw out is put into retort furnace calcination, and controlling calcination temperature is 400 DEG C, and calcination time 8 hours, obtains cerium dioxide product, and detecting total amount of rare earth is 99.16%.
Embodiment 7
83 kilograms, the technical grade bicarbonate of ammonia of nitrogen content >17% is dissolved in pure water, is mixed with the ammonium bicarbonate soln that volumetric molar concentration is 1.20mol/L.With mass percent concentration be 5.70% technical grade ammoniacal liquor preparation volumetric molar concentration be the ammonia soln of 3.26mol/L.Get above-mentioned ammonium bicarbonate soln and ammonia soln respectively, according to bicarbonate of ammonia integral molar quantity: the proportions of ammoniacal liquor integral molar quantity=25:75 becomes total mol concentration to be the mixed precipitation agent solution 1740L of 2.28mol/L.Be 0.60mol/L, pH=4.5 by concentration, volume is that the solution of cerium chloride by oxidation of 2000L imports in reactive tank, be heated to 50 DEG C, add 41Kg crystal seed, this crystal seed contains the basic carbonate cerium of massfraction 90% and the cerous hydroxide of 10%, under agitation evenly adds above-mentioned compounding conjunction precipitant solution 1740L.Controlling feed time is 10 hours, mother liquor terminal pH=8.2, continues stirring 10 minutes.By vacuum filtration, to obtain basic carbonate cerium (90%) be main, cerous carbonate (0) and cerous hydroxide (10%) is auxiliary mixed sediment, and to throw out drip washing once, washing water consumption is the deionized water of 1250L.Analyzing throw out content of rare earth is 66.60%, throw out is put into retort furnace calcination, and controlling calcination temperature is 450 DEG C, and calcination time 3 hours, obtains cerium dioxide product, and detecting total amount of rare earth is 99.54%.
Claims (1)
1. prepared a method for cerium dioxide by mixed precipitant, it is characterized in that:
(1) make raw material with the bicarbonate of ammonia of technical grade and the ammoniacal liquor of technical grade, become the mixed precipitation agent solution of 2.00 ~ 5.50mol/L according to bicarbonate of ammonia integral molar quantity with the proportions of ammoniacal liquor integral molar quantity 55 ~ 25:45 ~ 75;
(2) be 0.60 ~ 1.20mol/L by certain volume concentration, the solution of cerium chloride by oxidation of pH=4 ~ 5 imports in reactive tank, adding using basic carbonate cerium, cerous carbonate and cerous hydroxide is that auxiliary mixture is as crystal seed, the mass percent of each component of this crystal seed is respectively: basic carbonate cerium 90 ~ 95%, cerous carbonate 0 ~ 5% and cerous hydroxide 0 ~ 10%, and its consumption is 10% ~ 20% of required precipitation Cerium II Chloride quality;
(3) solution of cerium chloride by oxidation to 50 ~ 70 DEG C that obtain of heating steps 2, under agitation evenly add the mixed precipitation agent solution that step 1 is prepared, and its consumption is to need on the basis of 3mol mixed precipitant excessive 5 ~ 10% at precipitation 1mol Cerium II Chloride;
(4) control added the time of mixed precipitation agent solution at 4 ~ 10 hours, and reinforced complete continuation stirring 10 minutes controls the pH value of solution terminal 6.6 ~ 8.2;
(5) the basic carbonate cerium obtained by vacuum filtration step 4 is master, cerous carbonate and cerous hydroxide is auxiliary mixed sediment, and carries out drip washing once to throw out, and washing water consumption is at least 4 times of throw out quality;
(6) throw out that step 5 obtains is put into retort furnace calcination, control calcination temperature 400 ~ 650 DEG C, calcination time is 2 ~ 8 hours, obtains cerium dioxide product.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105967218A (en) * | 2016-05-06 | 2016-09-28 | 益阳鸿源稀土有限责任公司 | Preparation method of cerous carbonate with low content of chloride ions by hydrochloric acid system |
| CN106673046A (en) * | 2017-01-10 | 2017-05-17 | 益阳鸿源稀土有限责任公司 | Setting conversion method for preparing alkali type cerium carbonate precursor and superfine cerium dioxide |
| CN107502762A (en) * | 2017-08-29 | 2017-12-22 | 江西理工大学 | The method that ion type rareearth leaches mother liquor one-step method removing impurity by means of precipitation Extraction of rare earth |
| CN107601545A (en) * | 2017-10-23 | 2018-01-19 | 常州市卓群纳米新材料有限公司 | A kind of preparation method of bulky grain cerous carbonate |
| CN107760867A (en) * | 2017-09-14 | 2018-03-06 | 中国北方稀土（集团）高科技股份有限公司 | The method for preparing mixed rare earth carbonate with mixed precipitant under sulfuric acid system |
| CN107973332A (en) * | 2018-01-23 | 2018-05-01 | 包头科日稀土材料有限公司 | A kind of method for preparing high rare-earth content basic carbonate cerium |
| CN108178178A (en) * | 2018-01-23 | 2018-06-19 | 包头科日稀土材料有限公司 | A kind of method for preparing small particle basic carbonate cerium |
| CN108275710A (en) * | 2018-01-15 | 2018-07-13 | 赣州湛海工贸有限公司 | A method of preparing large particle rare-earth oxide |
| CN108439792A (en) * | 2018-04-28 | 2018-08-24 | 郭舒洋 | A kind of glass fining agent |
| CN110104671A (en) * | 2019-05-14 | 2019-08-09 | 华南理工大学 | A kind of induction method for crystallising of flake cerium carbonate |
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| CN105967218A (en) * | 2016-05-06 | 2016-09-28 | 益阳鸿源稀土有限责任公司 | Preparation method of cerous carbonate with low content of chloride ions by hydrochloric acid system |
| CN106673046A (en) * | 2017-01-10 | 2017-05-17 | 益阳鸿源稀土有限责任公司 | Setting conversion method for preparing alkali type cerium carbonate precursor and superfine cerium dioxide |
| CN106673046B (en) * | 2017-01-10 | 2017-12-05 | 益阳鸿源稀土有限责任公司 | Setting conversion method prepares basic carbonate cerium precursor and fine cerium oxide |
| CN107502762A (en) * | 2017-08-29 | 2017-12-22 | 江西理工大学 | The method that ion type rareearth leaches mother liquor one-step method removing impurity by means of precipitation Extraction of rare earth |
| CN107502762B (en) * | 2017-08-29 | 2022-01-07 | 江西理工大学 | Method for extracting rare earth by one-step precipitation and impurity removal of ionic rare earth leaching mother liquor |
| CN107760867A (en) * | 2017-09-14 | 2018-03-06 | 中国北方稀土（集团）高科技股份有限公司 | The method for preparing mixed rare earth carbonate with mixed precipitant under sulfuric acid system |
| CN107601545A (en) * | 2017-10-23 | 2018-01-19 | 常州市卓群纳米新材料有限公司 | A kind of preparation method of bulky grain cerous carbonate |
| CN108275710A (en) * | 2018-01-15 | 2018-07-13 | 赣州湛海工贸有限公司 | A method of preparing large particle rare-earth oxide |
| CN107973332A (en) * | 2018-01-23 | 2018-05-01 | 包头科日稀土材料有限公司 | A kind of method for preparing high rare-earth content basic carbonate cerium |
| CN108178178A (en) * | 2018-01-23 | 2018-06-19 | 包头科日稀土材料有限公司 | A kind of method for preparing small particle basic carbonate cerium |
| CN108439792A (en) * | 2018-04-28 | 2018-08-24 | 郭舒洋 | A kind of glass fining agent |
| CN110104671A (en) * | 2019-05-14 | 2019-08-09 | 华南理工大学 | A kind of induction method for crystallising of flake cerium carbonate |
| CN110104671B (en) * | 2019-05-14 | 2021-06-08 | 华南理工大学 | Induced crystallization method of flaky cerium carbonate |
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