CN103172101B - Preparation method of alkali-type cerous carbonate - Google Patents
Preparation method of alkali-type cerous carbonate Download PDFInfo
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- CN103172101B CN103172101B CN201210537779.1A CN201210537779A CN103172101B CN 103172101 B CN103172101 B CN 103172101B CN 201210537779 A CN201210537779 A CN 201210537779A CN 103172101 B CN103172101 B CN 103172101B
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Abstract
The invention discloses a preparation method of alkali-type cerous carbonate, and aims to solve the problems of high production cost, complex process and low production efficiency of the conventional alkali-type cerous carbonate using a hydrothermal preparation method. The preparation method of alkali-type cerous carbonate comprises the following steps of: dropping a parallel flow of a cerous nitrate solution and an alkali solution into deionized water under the stirring condition, controlling the pH value to be 9-10, stirring under a room temperature for 4-6 hours, standing for above 12 hours, filtering to obtain a sediment, repeatedly washing the sediment by using deionized water until the pH value is less than 7.5 and drying the sediment at 80-120 DEG C for 12-24 hours to obtain alkali-type cerous carbonate. The raw materials of alkali-type cerous carbonate are low in cost and can be easily obtained; alkali-type cerous carbonate can be prepared by reacting at room temperature, and a hydrothermal reaction condition is not required, so that the energy consumption is low, and the preparation process is simple and easy; the production period is greatly shortened in comparison with the hydrothermal reaction condition; and the production efficiency is improved.
Description
Technical field
The present invention relates to basic carbonate cerium preparing technical field, particularly a kind of preparation method of basic carbonate cerium.
Background technology
Basic carbonate cerium is a kind of important compound containing rare-earth element cerium, by large quantifier elimination, and is applied to many fields, as stablizer, decolourizing agent as glassy product, and polishing powder, formation alloy material etc.
The customary preparation methods of basic carbonate cerium adopts Hydrothermal preparation method, and be specially: with six water cerous nitrates for cerium source, being carbon source with urea, take polyvinylpyrrolidone as tensio-active agent, in aqueous environment, under 100 DEG C of conditions, prepares basic carbonate cerium.Prepare basic carbonate cerium with hydrothermal method and there is following problem: 1, energy consumption and the higher production cost that causes of raw materials cost high, 2, preparation technology is more complicated, the production cycle is long, and production efficiency is low.
A kind of control preparation method of basic carbonate cerium dendrite of the disclosure of the invention of CN 102795652 A, getting solubility cerium salt is dissolved in distilled water, and constantly stir, slowly add ammoniacal liquor, finally add precipitation agent, form mixing solutions, then transfer in autoclave by mixing solutions, sealing, is put in thermostat container and heats, temperature control completes hydro-thermal reaction, obtains hydro-thermal reaction product; With washed with de-ionized water hydro-thermal reaction product, under room temperature, after dry 24h, obtain basic carbonate cerium dendrite.The preparation method of this basic carbonate cerium still adopts Hydrothermal preparation method, still there is energy consumption and the higher production cost that causes of raw materials cost is high, and preparation technology is more complicated, and the production cycle is long, the problem that production efficiency is low.
Summary of the invention
The object of the invention is to overcome that the production cost that basic carbonate cerium adopts Hydrothermal preparation method to exist is high, complex process and the low problem of production efficiency, provide a kind of simple for process, production cost is low, the preparation method of the basic carbonate cerium that production efficiency is high.
The technical solution adopted for the present invention to solve the technical problems is:
A preparation method for basic carbonate cerium, described preparation method's step is as follows:
(1), by 100-250ml cerous nitrate solution and 100-250ml alkaline solution and drip is added in the deionized water under 300-600ml agitation condition, the pH of the hierarchy of control is at 9-10;
(2), after stirred at ambient temperature 4-6 hour, leave standstill more than 12 hours, filter and to obtain precipitation, by deionized water repetitive scrubbing precipitation until pH<7.5; Repetitive scrubbing precipitation is until pH<7.5 is to remove residual alkali;
(3), washing after be deposited in 80-120 DEG C at dry 12-24 h, obtain basic carbonate cerium.
The present invention reacts at ambient temperature and can prepare basic carbonate cerium, and without the need to hydrothermal reaction condition, energy consumption is low, and preparation is simple, and raw material NaOH and the Na of alkaline solution used
2cO
3cheap and easy to get, cost is lower; Production cycle comparatively hydrothermal reaction condition greatly shorten, improve production efficiency.
Control the volume proportion of cerous nitrate solution, alkaline solution and deionized water, the pH accurately controlling reaction system preferably can be beneficial to like this.And the pH controlling reaction system is key point, can the pH of the hierarchy of control is related at 9-10 obtain basic carbonate cerium, once pH deviates from 9-10, cannot obtain basic carbonate cerium, and obtain other product.
As preferably, in step (1), the concentration of cerous nitrate solution is 0.1-0.2mol/L.Concentration is excessive, and the pH of reaction system is difficult to control, and concentration is too small, and cerous nitrate solution needs the amount of use excessive, and production consumes comparatively large, is unfavorable for enhancing productivity, reduces costs.
As preferably, in step (1), alkaline solution is NaOH and Na
2cO
3the solution of formation soluble in water altogether, wherein NaOH concentration is 0.1-0.2mol/L, Na
2cO
3concentration is 0.1-0.2mol/L.Concentration is excessive, and the pH of reaction system is difficult to control, and concentration is too small, and alkaline solution needs the amount of use excessive, and production consumes comparatively large, is unfavorable for enhancing productivity, reduces costs.
The invention has the beneficial effects as follows:
1, starting material are cheap and easy to get, and cost is lower;
2, reaction can prepare basic carbonate cerium at ambient temperature, and without the need to hydrothermal reaction condition, energy consumption is low, and preparation is simple;
3, the production cycle comparatively hydrothermal reaction condition greatly shorten, improve production efficiency.
Accompanying drawing explanation
Fig. 1 is a kind of XRD figure of product of the present invention.
Embodiment
Below by specific embodiment, and by reference to the accompanying drawings, technical scheme of the present invention is described in further detail.
In the present invention, if not refer in particular to, the raw material adopted and equipment etc. all can be buied from market or this area is conventional.Method in following embodiment, if no special instructions, is the ordinary method of this area.
Embodiment 1:
Be 0.2mol/L cerous nitrate solution and 100ml alkaline solution (NaOH and Na by 100ml concentration
2cO
3the solution of formation soluble in water altogether, wherein NaOH concentration is 0.2mol/L, Na
2cO
3concentration is 0.2mol/L) and drip is added in the deionized water under 300ml agitation condition, the pH of the hierarchy of control is 9, stirred at ambient temperature is after 4 hours, leave standstill 15 hours, filter to obtain precipitation, with deionized water repetitive scrubbing precipitation until pH<7.5, after washing be deposited in 80 DEG C at dry 24 h, obtain basic carbonate cerium.
Embodiment 2:
Be 0.1mol/L cerous nitrate solution and 250ml alkaline solution (NaOH and Na by 250ml concentration
2cO
3the solution of formation soluble in water altogether, wherein NaOH concentration is 0.1mol/L, Na
2cO
3concentration is 0.1mol/L) and drip is added in the deionized water under 600ml agitation condition, the pH of the hierarchy of control is 10, stirred at ambient temperature is after 6 hours, leave standstill 18 hours, filter to obtain precipitation, with deionized water repetitive scrubbing precipitation until pH<7.5, after washing be deposited in 120 DEG C at dry 12h, obtain basic carbonate cerium.
Embodiment 3:
Be 0.1mol/L cerous nitrate solution and 200ml alkaline solution (NaOH and Na by 200ml concentration
2cO
3the solution of formation soluble in water altogether, wherein NaOH concentration is 0.2mol/L, Na
2cO
3concentration is 0.1mol/L) and drip is added in the deionized water under 400ml agitation condition, the pH of the hierarchy of control is 9, stirred at ambient temperature is after 5 hours, leave standstill 12 hours, filter to obtain precipitation, with deionized water repetitive scrubbing precipitation until pH<7.5, after washing be deposited in 100 DEG C at dry 20 h, obtain basic carbonate cerium.
The XRD figure of product of the present invention is shown in accompanying drawing 1, figure to show in product and is mainly basic carbonate cerium, comprises CeCO
3oH (JCPDS file no. 41-0013) and Ce
2(CO
3)
2(OH)
2h
2o (JCPDS file no. 46-0368).
Starting material of the present invention are cheap and easy to get, and cost is lower; Reaction can prepare basic carbonate cerium at ambient temperature, and without the need to hydrothermal reaction condition, energy consumption is low, and preparation is simple; Production cycle comparatively hydrothermal reaction condition greatly shorten, improve production efficiency.
Above-described embodiment is one of the present invention preferably scheme, not does any pro forma restriction to the present invention, also has other variant and remodeling under the prerequisite not exceeding the technical scheme described in claim.
Claims (1)
1. a preparation method for basic carbonate cerium, is characterized in that: described preparation method's step is as follows:
(1), by 100-250ml cerous nitrate solution and 100-250ml alkaline solution and drip is added in the deionized water under 300-600ml agitation condition, the pH of the hierarchy of control is at 9-10;
(2), after stirred at ambient temperature 4-6 hour, leave standstill more than 12 hours, filter and to obtain precipitation, by deionized water repetitive scrubbing precipitation until pH<7.5;
(3), washing after be deposited in 80-120 DEG C at dry 12-24 h, obtain basic carbonate cerium;
In step (1), the concentration of cerous nitrate solution is 0.1-0.2mol/L, and alkaline solution is NaOH and Na
2cO
3the solution of formation soluble in water altogether, wherein NaOH concentration is 0.1-0.2mol/L, Na
2cO
3concentration is 0.1-0.2mol/L.
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| CN201210537779.1A CN103172101B (en) | 2012-12-13 | 2012-12-13 | Preparation method of alkali-type cerous carbonate |
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| CN201210537779.1A CN103172101B (en) | 2012-12-13 | 2012-12-13 | Preparation method of alkali-type cerous carbonate |
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| CN103172101B true CN103172101B (en) | 2014-12-17 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103708525B (en) * | 2013-11-29 | 2015-07-15 | 南昌大学 | Production method of high-bulk density fine-grain low-chlorine rare earth carbonate and its oxide |
| CN103896322B (en) * | 2014-03-19 | 2016-09-07 | 青岛科技大学 | A kind of preparation method of dendritic basic carbonate cerium |
| CN105800664A (en) * | 2014-12-29 | 2016-07-27 | 安集微电子（上海）有限公司 | Method for preparing ceria abrasive and application thereof in CMP (Chemical Mechanical Polishing) |
| CN106044831B (en) * | 2016-05-27 | 2017-09-22 | 商洛学院 | A kind of sluggish precipitation prepares sheet SmOHCO3Nanocrystalline method |
| 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 |
| 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 |
| CN110526272B (en) * | 2019-08-28 | 2022-04-15 | 贵州大学 | Micro-nano structure CeCO3Preparation process of OH |
| CN113120943A (en) * | 2019-12-30 | 2021-07-16 | 安集微电子科技（上海）股份有限公司 | Synthesis method of basic cerium carbonate |
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| CN100558639C (en) * | 2008-05-22 | 2009-11-11 | 同济大学 | A kind of pair of hydrolysis regulation and control prepare the method for lanthanum subcarbonate nana-/ micro-crystal |
| CN101798627B (en) * | 2009-02-09 | 2013-07-03 | 有研稀土新材料股份有限公司 | Method for precipitating rare earth |
| CN102659163B (en) * | 2012-04-24 | 2014-06-25 | 包头华美稀土高科有限公司 | Technological method for preparing cerium carbonate with high content of rare earth in one step |
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