CN108178178A - A kind of method for preparing small particle basic carbonate cerium - Google Patents

A kind of method for preparing small particle basic carbonate cerium Download PDF

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Publication number
CN108178178A
CN108178178A CN201810061560.6A CN201810061560A CN108178178A CN 108178178 A CN108178178 A CN 108178178A CN 201810061560 A CN201810061560 A CN 201810061560A CN 108178178 A CN108178178 A CN 108178178A
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CN
China
Prior art keywords
cerium
basic carbonate
small particle
preparing small
carbonate cerium
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CN201810061560.6A
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Chinese (zh)
Inventor
卢国贞
鲁强
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Baotou Cohi Rare Earth Material Co Ltd
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Baotou Cohi Rare Earth Material Co Ltd
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Application filed by Baotou Cohi Rare Earth Material Co Ltd filed Critical Baotou Cohi Rare Earth Material Co Ltd
Priority to CN201810061560.6A priority Critical patent/CN108178178A/en
Publication of CN108178178A publication Critical patent/CN108178178A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/20Compounds containing only rare earth metals as the metal element
    • C01F17/247Carbonates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer

Abstract

The invention discloses a kind of methods for preparing small particle basic carbonate cerium, using mixed precipitant as cerium ion precipitating reagent, parallel-flow precipitation mode is taken with cerous nitrate solution, using the washing water of pure water or basic carbonate cerium as reactive tank bottom liquid, control the pH value of mother liquor terminal, make cerium ion precipitation complete, basic carbonate cerium is obtained through plate-frame filtering, washing, drying.Using the mixed solution of ammonium hydroxide and ammonium hydrogen carbonate, as cerium ion precipitating reagent, large-scale production can be realized, low energy consumption, and product quality stability is good, is polluted without impurity, and without repeatedly rinsing, waste water yield is few, safe and environmentally friendly in the present invention at normal temperatures.

Description

A kind of method for preparing small particle basic carbonate cerium
Technical field:
The present invention relates to a kind of methods for preparing basic carbonate cerium, and small particle basic carbonate cerium is prepared more particularly to a kind of Method.
Background technology:
With the development of Rare Earth Industry in China, market is more and more to the rare-earth products demand of special physical property.Basic carbonate Cerium is since with special property, prospect is widely used general.It is mainly used for glass industry, polishing material, luminescent material, red Pigment etc..
At present, the basic carbonate cerium of small grain size is prepared mainly using hydro-thermal method, using cerous nitrate as cerium source, using urea as carbon source In 120 DEG C or more high―temperature nucleis.Hydro-thermal method prepares basic carbonate cerium, and there are the deficiencies of high energy consumption, complex process, low production efficiency. In addition, somebody proposes to prepare basic carbonate cerium using sodium carbonate and sodium hydroxide, this method is needed there are the pollution of sodium ion Repeated multiple times washing causes the waste of water resource.
Invention content:
The purpose of the present invention is to provide a kind of production efficiency height, low energy consumption, technical process is easy to control, and pollution-free, The method for saving the preparation small particle basic carbonate cerium of water resource.
The purpose of the present invention is implemented by following technical solution:A kind of method for preparing small particle basic carbonate cerium, with mixing Precipitating reagent takes parallel-flow precipitation mode, using the leaching of pure water or basic carbonate cerium as cerium ion precipitating reagent with cerous nitrate solution Wash water controls the pH value of mother liquor terminal, makes cerium ion precipitation complete, through plate-frame filtering, washing, dry as reactive tank bottom liquid To basic carbonate cerium.
Preferably, the total alkalinity of the mixed precipitant is 3~6mol/L.
Preferably, the mixed precipitant is ammonium hydroxide and the mixed solution of ammonium hydrogen carbonate.
Preferably, the molar ratio of ammonium hydroxide and ammonium hydrogen carbonate is 1.38~1.42 in the mixed precipitant:1.
Preferably, the temperature of the mixed precipitant is 20~30 DEG C, and addition flow velocity is 3.7~16.5L/min, during addition Between for 40~90min, the addition time is related with reacting tankage, while is influenced by pretreatment amount.Mixed precipitant dosage is reason By the 100~105% of dosage, theoretical amount is calculated by chemical equation.
Preferably, a concentration of 0.5~1.0mol/L of the cerous nitrate solution, temperature are 20~30 DEG C, and pH is 5.0~6.0, Addition flow velocity is 10.0~21.3L/min, and the addition time is 40~90min, and the addition time is related with reaction tankage, while by Pretreatment amount influences.
Preferably, the pH value of the mother liquor terminal is 6.6~7.4.
Preferably, the reactive tank bottom liquid temperature is 20~30 DEG C.
Preferably, continue to stir 5min after stopping charging, then obtain alkali formula carbon through the plate-frame filtering, washing, drying Sour cerium.
Advantages of the present invention:The present invention uses the mixed solution of ammonium hydroxide and ammonium hydrogen carbonate as cerium ion precipitating reagent, normal Large-scale production can be realized under temperature, low energy consumption, and product quality stability is good, is polluted without impurity, without repeatedly rinsing, waste water Yield is few, safe and environmentally friendly.The total amount of rare earth of the basic carbonate cerium prepared using the method for the present invention 68.25~73.14%, D50Between 1.5~3.0 μm, the quality requirement of the small particle basic carbonate cerium of the market demand is complied fully with.D50 refers in powder It is worth grain size, represents that the size distribution percentage by volume of sample reaches grain size corresponding when 50%.The method of the present invention reaction condition Mildly, it is simple to operate and friendly to environment, is easily docked with prior art, being processed into for small particle basic carbonate cerium can be greatly lowered This.
Specific embodiment:
Embodiment 1:The molar ratio of ammonium hydroxide and ammonium hydrogen carbonate is 1.38:1, temperature is 30 DEG C, and total alkalinity is 3.0mol/L's Mixed precipitant 654L.Using 2500LPP reactive tanks, add in 20 DEG C of pure water 300L and do not had paddle.A concentration of 1.0mol/L, pH It is 6.0, temperature is 30 DEG C of cerous nitrate solution 640L.Reactive tank stirring is opened, it is molten to add in cerous nitrate according to flow velocity 10.7L/min Liquid, synchronous cocurrent add in mixed precipitant according to flow velocity 10.9L/min, and feed time is 60min, and wherein mixed precipitant is used 102% for theoretical amount is measured, mother liquor terminal pH=7.0 continues stirring 5 minutes, then directly slurry is detached by sheet frame, And sediment is eluted with the pure water of 30 DEG C of temperature, volume 770L, filter cake obtains basic carbonate cerium through 70 DEG C, drying in 8 hours.Alkali Formula cerous carbonate sampling analysis, total amount of rare earth 70.62%, D50=2.1 μm.
Embodiment 2:The molar ratio of ammonium hydroxide and ammonium hydrogen carbonate is 1.40:1, temperature is 20 DEG C, and total alkalinity is 4.0mol/L's Mixed precipitant 504L.Using 2500LPP reactive tanks, add in 20 DEG C of pure water 300L and do not had paddle.A concentration of 1.0mol/L, pH =6.0, temperature is 20 DEG C of cerous nitrate solution 640L.Reactive tank stirring is opened, it is molten to add in cerous nitrate according to flow velocity 10.0L/min Liquid, synchronous cocurrent add in mixed precipitation agent solution according to flow velocity 7.9L/min, and feed time is 64min, wherein mixed precipitation Agent dosage is theoretical 105%, mother liquor terminal pH=7.4, continues stirring 5 minutes, then directly slurry is detached by sheet frame, And sediment is eluted with the pure water of 30 DEG C of temperature, volume 770L, filter cake obtains basic carbonate cerium through 90 DEG C, drying in 6 hours.Alkali Formula cerous carbonate sampling analysis, total amount of rare earth 71.38%, D50=1.5 μm.
Embodiment 3:The molar ratio of ammonium hydroxide and ammonium hydrogen carbonate is 1.42:1, temperature is 25 DEG C, and total alkalinity is 6.0mol/L's Mixed precipitant 333L.Using 2500LPP reactive tanks, add in 25 DEG C of washing water 300L and do not had paddle.A concentration of 0.5mol/L, PH=6.0, the cerous nitrate solution 1280L that temperature is 25 DEG C.Reactive tank stirring is opened, nitric acid is added according to flow velocity 14.2L/min Cerium solution, synchronous cocurrent add in mixed precipitation agent solution according to flow velocity 3.7L/min, and feed time is 90min, wherein mixing Precipitating reagent dosage is theoretical 104%, mother liquor terminal pH=7.2, continues stirring 5 minutes, slurry is directly then passed through sheet frame Separation, and sediment is eluted with the pure water of 30 DEG C of temperature, volume 770L, filter cake obtains alkali formula carbon through 50 DEG C, drying in 12 hours Sour cerium.Basic carbonate cerium sampling analysis, total amount of rare earth 72.38%, D50=2.3 μm.
Embodiment 4:The molar ratio of ammonium hydroxide and ammonium hydrogen carbonate is 1.40:1, temperature is 30 DEG C, and total alkalinity is 4.0mol/L's Mixed precipitant 480L.Using 2500LPP reactive tanks, add in 30 DEG C of washing water 300L and do not had paddle.A concentration of 0.75mol/ L, pH=6.0, the cerous nitrate solution 853L that temperature is 30 DEG C.Reactive tank stirring is opened, nitric acid is added according to flow velocity 17.4L/min Cerium solution, synchronous cocurrent add in mixed precipitation agent solution according to flow velocity 9.8L/min, and feed time is 49min, wherein mixing Just, mother liquor terminal pH=6.6 continues stirring 5 minutes, then directly slurry by sheet frame is detached, is used in combination precipitating reagent dosage 30 DEG C of temperature, volume 770L pure water to sediment elute, filter cake through 60 DEG C, 10 hours drying obtain basic carbonate cerium.Alkali formula Cerous carbonate sampling analysis, total amount of rare earth 68.25%, D50=2.0 μm.
Embodiment 5:The molar ratio of ammonium hydroxide and ammonium hydrogen carbonate is 1.40:1, temperature is 25 DEG C, and total alkalinity is 3.0mol/L's Mixed precipitant 660L.Using 2500LPP reactive tanks, add in 25 DEG C of pure water 300L and do not had paddle.A concentration of 0.75mol/L, PH=6.0, the cerous nitrate solution 853L that temperature is 25 DEG C.Reactive tank stirring is opened, cerous nitrate is added according to flow velocity 21.3L/min Solution, synchronous cocurrent add in mixed precipitation agent solution according to flow velocity 16.5L/min, and feed time is 40min, wherein mixing is heavy Agent dosage in shallow lake is theoretical 103%, mother liquor terminal pH=7.2, continues stirring 5 minutes, and slurry is directly then passed through sheet frame point From, and sediment is eluted with the pure water of 30 DEG C of temperature, volume 770L, filter cake obtains basic carbonate through 100 DEG C, drying in 5 hours Cerium.Basic carbonate cerium sampling analysis, total amount of rare earth 73.14%, D50=3.0 μm.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.

Claims (9)

  1. A kind of 1. method for preparing small particle basic carbonate cerium, it is characterised in that:Using mixed precipitant as cerium ion precipitating reagent, Parallel-flow precipitation mode is taken with cerous nitrate solution, using the washing water of pure water or basic carbonate cerium as reactive tank bottom liquid, control The pH value of mother liquor terminal makes cerium ion precipitation complete, basic carbonate cerium is obtained through plate-frame filtering, washing, drying.
  2. 2. a kind of method for preparing small particle basic carbonate cerium according to claim 1, it is characterised in that:The mixing is heavy The total alkalinity of shallow lake agent is 3~6mol/L.
  3. 3. a kind of method for preparing small particle basic carbonate cerium according to claim 1 or 2, it is characterised in that:It is described mixed Precipitating reagent is closed as ammonium hydroxide and the mixed solution of ammonium hydrogen carbonate.
  4. 4. a kind of method for preparing small particle basic carbonate cerium according to claim 3, it is characterised in that:The mixing is heavy The molar ratio of ammonium hydroxide and ammonium hydrogen carbonate is 1.38~1.42 in the agent of shallow lake:1.
  5. 5. a kind of method for preparing small particle basic carbonate cerium according to claim 4, it is characterised in that:The mixing is heavy The temperature of shallow lake agent is 20~30 DEG C, and addition flow velocity is 3.7~16.5L/min.
  6. 6. a kind of method for preparing small particle basic carbonate cerium according to claim 5, it is characterised in that:The cerous nitrate Solution concentration is 0.5~1.0mol/L, and temperature is 20~30 DEG C, and pH is 5.0~6.0, and addition flow velocity is 10.0~21.3L/ min。
  7. 7. a kind of method for preparing small particle basic carbonate cerium according to claim 1, it is characterised in that:The mother liquor is whole The pH value of point is 6.6~7.4.
  8. 8. a kind of method for preparing small particle basic carbonate cerium according to claim 1, it is characterised in that:The reactive tank Bottom liquid temperature is 20~30 DEG C.
  9. 9. a kind of method for preparing small particle basic carbonate cerium according to claim 1, it is characterised in that:After stopping charging Continue to stir 5min, then obtain basic carbonate cerium through the plate-frame filtering, washing, drying.
CN201810061560.6A 2018-01-23 2018-01-23 A kind of method for preparing small particle basic carbonate cerium Pending CN108178178A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108423703A (en) * 2018-06-20 2018-08-21 乐山沃耐稀电子材料有限公司 A kind of production method of fine grain shape cerous carbonate

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103172101A (en) * 2012-12-13 2013-06-26 浙江海洋学院 Preparation method of alkali-type cerous carbonate
CN104891550A (en) * 2015-07-03 2015-09-09 燕山大学 Method of preparing ceria by mixed precipitant

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103172101A (en) * 2012-12-13 2013-06-26 浙江海洋学院 Preparation method of alkali-type cerous carbonate
CN104891550A (en) * 2015-07-03 2015-09-09 燕山大学 Method of preparing ceria by mixed precipitant

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
李凤生: "《特种超细粉体制备技术及应用》", 31 January 2002 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108423703A (en) * 2018-06-20 2018-08-21 乐山沃耐稀电子材料有限公司 A kind of production method of fine grain shape cerous carbonate

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Application publication date: 20180619

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