CN104891550B - A kind of method that ceria is prepared by mixed precipitant - Google Patents
A kind of method that ceria is prepared by mixed precipitant Download PDFInfo
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- CN104891550B CN104891550B CN201510383126.6A CN201510383126A CN104891550B CN 104891550 B CN104891550 B CN 104891550B CN 201510383126 A CN201510383126 A CN 201510383126A CN 104891550 B CN104891550 B CN 104891550B
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Abstract
A kind of method that ceria is prepared by mixed precipitant, the method is mainly using the mixed solution of ammonium hydrogen carbonate and ammonia as precipitant, it is with crystal seed collective effect, by the rare earth ion precipitation in re chloride, obtain based on basic carbonate cerium, the mixture supplemented by cerous carbonate and cerium hydroxide, further RE CeO 2 product is prepared by calcination.The ceria of present invention preparation meets industry standard, and method of the present invention reaction condition is gentle, and preparation process energy resource consumption substantially reduces, low cost.Meanwhile, greatly reduce the discharge capacity of carbon dioxide, there is obvious social benefit and environmental benefit.
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 referred to as " vitamin " of modern industry and magical new material " treasure-house ", and that commercially concludes the business is dilute
Soil 90% is rare earth oxide.Mainly rare earth oxide is prepared for intermediate calcination with rare earth carbonate at this stage, only from material
Conversion process calculate, preparation 1 ton of ceria will discharge 767.44 kilograms of carbon dioxide.Because the whole world subtracts to carbon dioxide
The attention of row's problem, searching manufacturing cost is lower, CO2 emissions are less, rare earth oxide dispersive property is preferably prepared
Method, is increasingly paid attention to by rare earth circle.
Stabilizer, decolorising agent, non-browning glass, luminescent material and manufacture that ceria is mainly used in glass industry are various
Alloy material etc..During preparing cerous carbonate using ammonium hydrogen carbonate, because ammonium hydrogen carbonate is acid salt, during the course of the reaction
Produce corresponding hydrochloric acid, the ammonium hydrogen carbonate that it adds has 50% to play neutralization of acid with base, and this not only consumes substantial amounts ofization
Work material, but also substantial amounts of carbon dioxide can be released.In the method preparing basic carbonate cerium, generally adopt high-temperature high pressure water
Full-boiled process synthesizes, and application is extremely restricted.Liu Lingyun etc. (rare earth, volume 34 fourth phase, page 95～97) add at high temperature admittedly
Body ammonium hydrogen carbonate prepares basic carbonate cerium, and course of reaction foam is big, temperature required be more than 95 DEG C, and easily bring impurity and miscellaneous into
Thing.Guo Zhiyan et al. (functional material, supplementary issue (volume 38) in 2007, page 2096～2098) under hydrothermal conditions with carbamide as carbon source
Prepare basic carbonate cerium, preparation process time is long, high processing costs, temperature required height, it is difficult large-scale production.
Content of the invention
It is an object of the invention to provide one kind can reducing energy consumption and cost, CO2 emissions can be reduced simultaneously again simultaneously
Can industrialized production the method that ceria is prepared by mixed precipitant.The method is mainly with ammonium hydrogen carbonate and ammonia
As precipitant, it by the rare earth ion precipitation in re chloride, obtains alkali formula carbon with crystal seed collective effect to mixed solution
Mixture based on sour cerium, supplemented by cerous carbonate and cerium hydroxide, prepares RE CeO 2 product by calcination further.
Main contents of the present invention are as follows：
(1) make raw material with the ammonium hydrogen carbonate of technical grade and the ammonia of technical grade, according to ammonium hydrogen carbonate integral molar quantity and ammonia
Integral molar quantity 55～25：45～75 proportions become the mixed precipitation agent solution of 2.00～5.50mol/L；
(2) by certain volume concentration be 0.60～1.20mol/L, the solution of cerium chloride by oxidation of pH=4～5 import reactive tank in,
Add mixture using basic carbonate cerium based on, supplemented by cerous carbonate and cerium hydroxide as crystal seed, the quality of each component of this crystal seed
Percentage ratio is respectively：Basic carbonate cerium 90～95%, cerous carbonate 0～5% and cerium hydroxide 0～10%, its consumption is required heavy
The 10%～20% of shallow lake cerium chloride quality；
(3) solution of cerium chloride by oxidation that heating stepses 2 obtain, to 50～70 DEG C, is uniformly added into the mixed of step 1 preparation under agitation
Close precipitant solution, its consumption is excessive 5～10% on the basis of precipitation 1mol cerium chloride needs 3mol mixed precipitant；
(4) control the time adding mixed precipitation agent solution at 4～10 hours, charging finishes continuation stirring 10 minutes, control
The pH value of solution terminal processed is 6.6～8.2；
(5) based on the basic carbonate cerium being obtained by vacuum filtration step 4, the mixing supplemented by cerous carbonate and cerium hydroxide is sunk
Starch, and drip washing is carried out once to precipitate, drip washing water consumption is at least 4 times of precipitate quality；
(6) precipitate that step 5 obtains is put into Muffle furnace calcination, control 400～650 DEG C of calcination temperature, calcination time
For 2～8 hours, obtain ceria product.
The present invention compared with prior art has the advantage that：
1st, based on the basic carbonate cerium of the method preparation, the mixed sediment supplemented by cerous carbonate and cerium hydroxide, rare earth contains
Amount is between 60%～68%.The spy that this product has that particle size distribution interval is narrow, granule supernatant fast, easily filters, content of rare earth is high
Point.By the ceria of the mixed sediment preparation based on basic carbonate cerium, supplemented by cerous carbonate and cerium hydroxide, color is pure
Just, granule be uniformly dispersed, good fluidity, just can reach under relatively low calcination temperature content of rare earth be more than 99.0% product
Require.
2nd, when using mixed precipitant, the addition of ammonia is 45～75% it is meant that precipitation process product will directly be reduced
Raw carbon dioxide 45～75%.In the standby 1 ton of ceria of burning ring restraining, common cerous carbonate produces the titanium dioxide of 383.72kg
Carbon, and the mixed sediment based on basic carbonate cerium, supplemented by cerous carbonate and cerium hydroxide produce 255.81kg carbon dioxide and
The water vapour of 52.33kg, oxide per ton directly reduces by 33% CO2 emissions, has obvious social benefit and ring
Border benefit.
3rd, based on basic carbonate cerium, the mixed sediment calcination temperature supplemented by cerous carbonate and cerium hydroxide is less than cerous carbonate
Calcination temperature, calcination process energy resource consumption will reduce by more than 40%.
4th, the present invention can be greatly lowered the processing cost of ceria.One is to prepare ammonium hydrogen carbonate due to ammonia in itself
Raw material, ammonium hydrogen carbonate usage amount 45～75% can be saved, reduce the freight volume of ammonium hydrogen carbonate, the volume of goods loaded and unloaded and dissolving simultaneously
Amount；It two is promoted to 60～68% due to preparing the intermediate product grade of ceria, makes product package material reduce 30%, unit
The cost of transportation of oxide is greatly lowered；Its three calcinations energy consumption reduces nature and can reduce processing cost.
5th, method of the present invention reaction condition is gentleer, simple to operate.
Specific embodiment
Embodiment 1:
By nitrogen content>17% technical grade ammonium hydrogen carbonate 150Kg is dissolved in pure water, and being configured to molar concentration is
3.50mol/L ammonium bicarbonate soln.It is that 19.35% technical grade ammonia preparation molar concentration is with mass percent concentration
10.50mol/L ammonia spirit.Take above-mentioned ammonium bicarbonate soln and ammonia spirit respectively, according to ammonium hydrogen carbonate integral molar quantity：
Ammonia integral molar quantity=45：55 proportions become the mixed precipitation agent solution 720L that total mol concentration is 5.50mol/L.Will be dense
Spending for 0.60mol/L, pH=4.0, volume is in the solution of cerium chloride by oxidation importing reactive tank of 2000L, is heated to 65 DEG C, adds 30Kg
Crystal seed, this crystal seed contains the cerium hydroxide of the basic carbonate cerium of mass fraction 94%, 4% cerous carbonate and 2%, under agitation all
Even addition is above-mentioned to be compounded conjunction precipitant solution 720L.Feed time is controlled to be 5 hours, mother solution terminal pH=7.4, continues stirring
10 minutes.Obtain based on basic carbonate cerium (94%) by vacuum filtration, supplemented by cerous carbonate (4%) and cerium hydroxide (2%)
Mixed sediment, and to precipitate drip washing once, drip washing water consumption is the deionized water of 1350L.Analysis precipitate content of rare earth
For 62.43%, precipitate is put into Muffle furnace calcination, control calcination temperature to be 650 DEG C, calcination time 2 hours, obtain titanium dioxide
Cerium product, detection total amount of rare earth is 99.01%.
Embodiment 2:
By nitrogen content>17% technical grade ammonium hydrogen carbonate 182Kg is dissolved in pure water, and being configured to molar concentration is
2.98mol/L ammonium bicarbonate soln.It is that 18.56% technical grade ammonia preparation molar concentration is with mass percent concentration
10.10mol/L ammonia spirit.Take above-mentioned ammonium bicarbonate soln and ammonia spirit respectively, according to ammonium hydrogen carbonate integral molar quantity：
Ammonia integral molar quantity is 50：50 proportions become the mixed precipitation agent solution 950L that total mol concentration is 4.61mol/L.Will be dense
Spending for 0.90mol/L, pH=4.5, volume is in the solution of cerium chloride by oxidation importing reactive tank of 1500L, is heated to 65 DEG C, adds 25Kg
Crystal seed, this crystal seed contains the cerium hydroxide of the basic carbonate cerium of mass fraction 94%, 5% cerous carbonate and 1%, under agitation all
Even addition is above-mentioned to be compounded conjunction precipitant solution 950L.Feed time is controlled to be 4 hours, mother solution terminal pH=6.8, continues stirring
10 minutes.Obtain based on basic carbonate cerium (94%) by vacuum filtration, supplemented by cerous carbonate (5%) and cerium hydroxide (1%)
Mixed sediment, and to precipitate drip washing once, drip washing water consumption is the deionized water of 1450L.Analysis precipitate content of rare earth
For 64.85%, precipitate is put into Muffle furnace calcination, control calcination temperature to be 500 DEG C, calcination time 3 hours, obtain titanium dioxide
Cerium product, detection total amount of rare earth is 99.23%.
Embodiment 3:
By nitrogen content>17% technical grade ammonium hydrogen carbonate 245Kg is dissolved in pure water, and being configured to molar concentration is
1.10mol/L ammonium bicarbonate soln.It is that 18.56% technical grade ammonia preparation molar concentration is with mass percent concentration
10.10mol/L ammonia spirit.Take above-mentioned ammonium bicarbonate soln and ammonia spirit respectively, according to ammonium hydrogen carbonate integral molar quantity：
Ammonia integral molar quantity=50：50 proportions become the mixed precipitation agent solution 2930L that total mol concentration is 2.00mol/L.Will
The solution of cerium chloride by oxidation that concentration is 1.20mol/L, pH=4.5, volume are 1500L imports in reactive tank, is heated to 60 DEG C, adds
31Kg crystal seed, this crystal seed contains the cerium hydroxide of the basic carbonate cerium of mass fraction 94%, 5% cerous carbonate and 1%, in stirring
Under be uniformly added into above-mentioned be compounded conjunction precipitant solution 2930L.Feed time is controlled to be 8 hours, mother solution terminal pH=7.0, continues
Continuous stirring 10 minutes.Obtain based on basic carbonate cerium (94%) by vacuum filtration, cerous carbonate (5%) and cerium hydroxide (1%)
Supplemented by mixed sediment, and to precipitate drip washing once, drip washing water consumption is the deionized water of 2050L.Analysis precipitate is dilute
Native content is 60.67%, and precipitate is put into Muffle furnace calcination, controls calcination temperature to be 650 DEG C, and calcination time 2 hours obtains
Ceria product, detection total amount of rare earth is 99.26%.
Embodiment 4:
By nitrogen content>17% technical grade ammonium hydrogen carbonate 157Kg is dissolved in pure water, and being configured to molar concentration is
2.04mol/L ammonium bicarbonate soln.It is that 18.56% technical grade ammonia preparation molar concentration is with mass percent concentration
10.10mol/L ammonia spirit.Take above-mentioned ammonium bicarbonate soln and ammonia spirit respectively, according to ammonium hydrogen carbonate integral molar quantity：
Ammonia integral molar quantity=50：50 proportions become the mixed precipitation agent solution 1120L that total mol concentration is 3.38mol/L.Will
The solution of cerium chloride by oxidation that concentration is 0.60mol/L, pH=5.0, volume are 2000L imports in reactive tank, is heated to 55 DEG C, adds
25Kg crystal seed, this crystal seed contains the cerium hydroxide of the basic carbonate cerium of mass fraction 94%, 5% cerous carbonate and 1%, in stirring
Under be uniformly added into above-mentioned be compounded conjunction precipitant solution 1120L.Feed time is controlled to be 10 hours, mother solution terminal pH=7.0, continues
Continuous stirring 10 minutes.Obtain based on basic carbonate cerium (94%) by vacuum filtration, cerous carbonate (5%) and cerium hydroxide (1%)
Supplemented by mixed sediment, and to precipitate drip washing once, drip washing water consumption is the deionized water of 1260L.Analysis precipitate is dilute
Native content is 65.95%, and precipitate is put into Muffle furnace calcination, controls calcination temperature to be 425 DEG C, and calcination time 4 hours obtains
Ceria product, detection total amount of rare earth is 99.38%.
Embodiment 5:
By nitrogen content>17% technical grade ammonium hydrogen carbonate 185Kg is dissolved in pure water, and being configured to molar concentration is
2.70mol/L ammonium bicarbonate soln.It is that 19.35% technical grade ammonia preparation molar concentration is with mass percent concentration
10.50mol/L ammonia spirit.Take above-mentioned ammonium bicarbonate soln and ammonia spirit respectively, according to ammonium hydrogen carbonate integral molar quantity：
Ammonia integral molar quantity=55：45 proportions become the mixed precipitation agent solution 950L that total mol concentration is 4.05mol/L.Will be dense
Spending for 0.60mol/L, pH=4.5, volume is in the solution of cerium chloride by oxidation importing reactive tank of 2000L, is heated to 70 DEG C, adds 32Kg
Crystal seed, this crystal seed contains the basic carbonate cerium of mass fraction 95% and 5% cerous carbonate, is uniformly added into above-mentioned being joined under agitation
Mixed precipitation agent solution 950L.Feed time is controlled to be 6 hours, mother solution terminal pH=6.6, continues stirring 10 minutes.By true
Empty sucking filtration obtains based on basic carbonate cerium (95%), the mixed sediment supplemented by cerous carbonate (5%) and cerium hydroxide (0), and right
Once, drip washing water consumption is the deionized water of 1400L for precipitate drip washing.Analysis precipitate content of rare earth is 60.00%, will precipitate
Thing puts into Muffle furnace calcination, controls calcination temperature to be 450 DEG C, and calcination time 3.5 hours obtains ceria product, and detection is dilute
Native total amount is 99.65%.
Embodiment 6:
By nitrogen content>17% technical grade ammonium hydrogen carbonate 115Kg is dissolved in pure water, and preparation molar concentration is 1.20mol/
The ammonium bicarbonate soln of L.With mass percent concentration be 18.56% technical grade ammonia prepare molar concentration be 10.10mol/L's
Ammonia spirit.Take above-mentioned ammonium bicarbonate soln and ammonia spirit respectively, according to ammonium hydrogen carbonate integral molar quantity：Ammonia integral molar quantity
=34：66 proportions become the mixed precipitation agent solution 1380L that total mol concentration is 2.86mol/L.Concentration is
0.60mol/L, pH=4.5, volume are that the solution of cerium chloride by oxidation of 2000L imports in reactive tank, are heated to 60 DEG C, add 41Kg brilliant
Kind, this crystal seed contains the cerium hydroxide of the basic carbonate cerium of mass fraction 94%, 1% cerous carbonate and 5%, under agitation uniformly
Above-mentioned compounding is added to close precipitant solution 1380L.Feed time is controlled to be 9 hours, mother solution terminal pH=7.8, continues stirring
10 minutes.Obtain based on basic carbonate cerium (94%) by vacuum filtration, supplemented by cerous carbonate (1%) and cerium hydroxide (5%)
Mixed sediment, and to precipitate drip washing once, drip washing water consumption is the deionized water of 1250L.Analysis precipitate content of rare earth
For 68.00%, precipitate is put into Muffle furnace calcination, control calcination temperature to be 400 DEG C, calcination time 8 hours, obtain titanium dioxide
Cerium product, detection total amount of rare earth is 99.16%.
Embodiment 7
By nitrogen content>83 kilograms of 17% technical grade ammonium hydrogen carbonate is dissolved in pure water, is configured to molar concentration and is
1.20mol/L ammonium bicarbonate soln.It is that 5.70% technical grade ammonia preparation molar concentration is with mass percent concentration
3.26mol/L ammonia spirit.Take above-mentioned ammonium bicarbonate soln and ammonia spirit respectively, according to ammonium hydrogen carbonate integral molar quantity：
Ammonia integral molar quantity=25：75 proportions become the mixed precipitation agent solution 1740L that total mol concentration is 2.28mol/L.Will
The solution of cerium chloride by oxidation that concentration is 0.60mol/L, pH=4.5, volume are 2000L imports in reactive tank, is heated to 50 DEG C, adds
41Kg crystal seed, this crystal seed contains the basic carbonate cerium of mass fraction 90% and 10% cerium hydroxide, is uniformly added under agitation
Above-mentioned compounding closes precipitant solution 1740L.Feed time is controlled to be 10 hours, mother solution terminal pH=8.2, continues 10 points of stirring
Clock.Obtain based on basic carbonate cerium (90%) by vacuum filtration, the mixing supplemented by cerous carbonate (0) and cerium hydroxide (10%) is sunk
Starch, and to precipitate drip washing once, drip washing water consumption is the deionized water of 1250L.Analyzing precipitate content of rare earth is
66.60%, precipitate is put into Muffle furnace calcination, controls calcination temperature to be 450 DEG C, calcination time 3 hours, obtain ceria
Product, detection total amount of rare earth is 99.54%.
Claims (1)
1. a kind of by mixed precipitant prepare ceria method it is characterised in that：
(1) make raw material with the ammonium hydrogen carbonate of technical grade and the ammonia of technical grade, always rub according to ammonium hydrogen carbonate integral molar quantity and ammonia
You measure 55～25：45～75 proportions become the mixed precipitation agent solution of 2.00～5.50mol/L；
(2) by certain volume concentration be 0.60～1.20mol/L, the solution of cerium chloride by oxidation of pH=4～5 import reactive tank in, add
Mixture using basic carbonate cerium based on, supplemented by cerous carbonate and cerium hydroxide is as crystal seed, the percent mass of each component of this crystal seed
Than respectively it is：Basic carbonate cerium 90～95%, cerous carbonate 0～5% and cerium hydroxide 0～10%, its consumption is required precipitation chlorine
Change the 10%～20% of cerium quality；
(3) solution of cerium chloride by oxidation that heating stepses 2 obtain to 50～70 DEG C, sink by the mixing being uniformly added into step 1 preparation under agitation
Shallow lake agent solution, its consumption is excessive 5～10% on the basis of precipitation 1mol cerium chloride needs 3mol mixed precipitant；
(4) control the time adding mixed precipitation agent solution at 4～10 hours, charging finishes continuation stirring 10 minutes, controls molten
The pH value of liquid terminal is 6.6～8.2；
(5) based on the basic carbonate cerium being obtained by the vacuum filtration step 4, mixed precipitation supplemented by cerous carbonate and cerium hydroxide
Thing, and drip washing is carried out once to precipitate, drip washing water consumption is at least 4 times of precipitate quality；
(6) precipitate that step 5 obtains to be put into Muffle furnace calcination, control 400～650 DEG C of calcination temperature, calcination time is 2～
8 hours, obtain ceria product.
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| CN105967218B (en) * | 2016-05-06 | 2017-10-13 | 益阳鸿源稀土有限责任公司 | A kind of preparation method of the low chlorine root cerous carbonate of hydrochloric acid system |
| 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 |
| 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 |
| CN114604886A (en) * | 2018-01-15 | 2022-06-10 | 赣州湛海新材料科技有限公司 | Method for preparing large-particle rare earth oxide |
| 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 |
| 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 |
| CN108439792A (en) * | 2018-04-28 | 2018-08-24 | 郭舒洋 | A kind of glass fining agent |
| 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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