CN103539194A - Method for preparing flake cerium carbonate - Google Patents
Method for preparing flake cerium carbonate Download PDFInfo
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- CN103539194A CN103539194A CN201310440636.3A CN201310440636A CN103539194A CN 103539194 A CN103539194 A CN 103539194A CN 201310440636 A CN201310440636 A CN 201310440636A CN 103539194 A CN103539194 A CN 103539194A
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- ammonium bicarbonate
- trivalent cerium
- cerium ion
- cerous carbonate
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Abstract
The invention discloses a method for preparing flake cerium carbonate, which comprises the following steps: preparing a trivalent cerium ion solution A with a concentration of 0.58-0.87 mol/L and an ammonium bicarbonate solution B with a concentration of 1.27-1.9 mol/L firstly, so that the molar ratio of trivalent cerium ions to ammonium bicarbonate in the solutions is 2:7; and adding 1% volume of the ammonium bicarbonate solution B into a reaction container firstly, then respectively simultaneously adding the trivalent cerium ion solution A and the ammonium bicarbonate solution B at a slow speed into the reaction container, washing generated precipitations by using deionized water C, and finally, carrying out suction filtration on cerium carbonate precipitations subjected to suitable washing, and drying the obtained product. The method is small in energy consumption and low in material consumption, and has the advantages of low material impurity level requirements, simple post-processing, high application value, and the like.
Description
Technical field
The present invention relates to a kind of preparation method of cerous carbonate, specially refer to a kind of preparation method of sheet cerous carbonate.
Background technology
Cerous carbonate is mainly used in the aspects such as advanced liquid crystal polishing powder, purifying air, vehicle exhaust absorption.Cerous carbonate generally adopts bicarbonate of ammonia directly to join in muriate, nitrate or the sulfate liquor of cerium and goes, and generates the carbonate of cerium, owing to being subject to the restriction of condition, often can only obtain the amorphous precipitated or crystal of cerium; The preparation of cerous carbonate is generally carried out under low concentration or comparatively high temps.What the former had just started to form is amorphous precipitated, and digestion time that need to be longer just may form crystalline precipitate, and output is extremely low and production stability is poor, produces a large amount of lower concentration ammonium salt waste water simultaneously and is difficult to process; And the latter can form crystalline precipitate, but supplies consumption is larger, and energy consumption is high, and cerous carbonate is easily at high temperature oxidized.
Cerous carbonate easily forms amorphous precipitated or colloid in the process of precipitation, the precipitation generating is owing to there is no fixed sturcture, surface tissue is complicated, in precipitation, be difficult for afterwards separated with water, be difficult for washing, easily absorption, occlusion or parcel impurity, exist impurity high, large difficulty, the unfavorable suitability for industrialized production that realizes of waiting of post-processed difficulty.Cerous carbonate at high temperature can generate a kind of crystalline precipitation, but exists energy consumption high, and loss of material is serious, and product impurity is high, and has the phenomenon of high temperature oxidation, product colour jaundice.
Summary of the invention
The present invention is according to above-mentioned technical problem, a kind of preparation method of sheet cerous carbonate is provided, object be in order to solve at present yielding poorly of existing aspect preparing at cerous carbonate, energy consumption is high, the cerous carbonate complex structure that obtains is not single and the problems such as impurity height that cause due to structure.The method is prepared a kind of pure white crystalline form sheet cerous carbonate under lower temperature, to raw material and auxiliary material require level lower, product purity is high, is easy to suitability for industrialized production.
The technical solution used in the present invention is: a kind of preparation method of sheet cerous carbonate, and wherein the reaction principle of cerous carbonate is:
The preparation method of a kind of sheet cerous carbonate provided by the invention, its concrete steps are as follows:
The first step, the ammonium bicarbonate soln B that the trivalent cerium ion solution A that outfit concentration is 0.58mol/L ~ 0.87mol/L and concentration are 1.27mol/L ~ 1.9mol/L;
Second step, is equipped with trivalent cerium ion solution A and the ammonium bicarbonate soln B of proper volume, changes and in proportioning, makes bicarbonate of ammonia excessive 10% ~ 16%, and making trivalent cerium ion in solution and the mol ratio of bicarbonate of ammonia is 2:7;
The 3rd step, first add the ammonium bicarbonate soln B of 1% volume to reaction vessel, with speed slowly, trivalent cerium ion solution A and ammonium bicarbonate soln B are joined in reaction vessel simultaneously respectively afterwards, react after about 5min, the flow of trivalent cerium ion solution A and ammonium bicarbonate soln B is opened greatly by its volume ratio, guaranteed that trivalent cerium ion solution A and ammonium bicarbonate soln B have flowed simultaneously;
The 4th step, by the precipitate with deionized water C washing generating, in surveying wash water, specific conductivity is less than 10 μ s/cm and stops washing;
The 5th step, the cerous carbonate that washing is suitable precipitates suction filtration post-drying 3 hours, makes ceria content be greater than 50%.
The temperature of reaction of described trivalent cerium ion solution A and ammonium bicarbonate soln B is 55 ℃.
Temperature for the deionized water C of washing precipitation in described step 4 is 35 ℃ ~ 45 ℃.
Bake out temperature in described step 5 after washing is 55 ℃ ~ 65 ℃.
Described trivalent cerium ion solution A adopts solution of cerium chloride by oxidation or cerous nitrate solution.
Described trivalent cerium ion solution A can also adopt CeO2, and its concentration is 100g/L ~ 150g/L, and corresponding bicarbonate of ammonia B concentration is 100g/L ~ 150g/L.
Beneficial effect of the present invention is: energy consumption is little, supplies consumption is lower; Do not exist Ce3+ by the possibility of high temperature oxidation simultaneously; Because this invention is precipitated as moment, separate out, do not need ageing, with short production cycle; Have that the requirement of material impurity level is lower, post-processed is simple, using value advantages of higher.
Accompanying drawing explanation
Fig. 1 is reaction principle figure of the present invention;
Wherein A is trivalent cerium solution, and B is ammonium bicarbonate soln, and C is deionized water.
Fig. 2 is the Electronic Speculum figure of embodiment 1;
Fig. 3 is the Electronic Speculum figure of embodiment 2;
Fig. 4 is the Electronic Speculum figure of embodiment 3.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
A preparation method for sheet cerous carbonate, this sheet cerous carbonate reaction principle is as follows:
As shown in Figure 1, trivalent cerium solution A is that to roll over CeO2 be 100g/L ~ 150g/L to concentration 0.58mol/L ~ 0.87mol/L() Ce3+ solution, regulator solution acidity to 0.1 ± 0.01mol/L, 55 ± 5 ℃ of temperature; B is concentration 1.27mol/L ~ 1.9mol/L(100g/L ~ 150g/L) ammonium bicarbonate soln, 55 ± 5 ℃ of temperature; C is deionized water, 55 ± 5 ℃ of temperature;
When reaction starts, open stirring, first add a small amount of ammonium bicarbonate soln B to deionized water C, after a while trivalent cerium solution A is also joined in deionized water C, trivalent cerium solution A joins in deionized water C simultaneously and completes and react with ammonium bicarbonate soln B.
Concrete implementation step prepared by this sheet cerous carbonate is:
The first step, the trivalent cerium ion solution A that outfit concentration is 0.58mol/L ~ 0.87mol/L; The ammonium bicarbonate soln B that outfit concentration is 1.27mol/L ~ 1.9mol/L;
Second step, according to the amount of plan preparing product, be equipped with trivalent cerium ion solution A and the molten B of bicarbonate of ammonia of proper volume, in assurance trivalent cerium ion solution A and ammonium bicarbonate soln B, the mol ratio of trivalent cerium ion and bicarbonate of ammonia is 2:7 (bicarbonate of ammonia excessive 10% ~ 16% is advisable);
The 3rd step, first add the ammonium bicarbonate soln B of 1% volume to deionized water C, with speed slowly, trivalent cerium ion solution A and ammonium bicarbonate soln B are joined in deionized water C simultaneously respectively afterwards, react after about 5min, the flow of trivalent cerium ion solution A and ammonium bicarbonate soln B is opened greatly by its volume ratio, guaranteed that trivalent cerium ion solution A and ammonium bicarbonate soln B have flowed simultaneously.
The 4th step, wash the precipitation generating with 40 ℃ of left and right deionized water C, in survey wash water, specific conductivity is less than 10 μ s/cm and stops washing;
The 5th step is dried 3 hours at 60 ℃ after washing suitable cerous carbonate precipitation suction filtration, guarantees that its folding ceria content is greater than 50% and is advisable, and bake out temperature is unsuitable too high, and the time should not be oversize, otherwise can cause the oxidative phenomena of cerous carbonate, affects product quality.
Specific embodiment of the present invention is as follows:
Example one:
1. being equipped with concentration is 0.58mol/L solution of cerium chloride by oxidation 1L, is equipped with the bicarbonate of ammonia 1.6L of 1.27mol/L, controls their temperature 55 ℃ of left and right;
2. 0.5L deionized water C is added in 3L beaker, and puts into water-bath insulation to 55 ℃;
3. open and stir, rotating speed 250r/min, first the bicarbonate of ammonia being equipped with is added to 16ml to deionized water C, after bicarbonate of ammonia and solution of cerium chloride by oxidation are slowly dropped in beaker simultaneously, bicarbonate of ammonia and Cerium II Chloride flow are about 16ml/min, react and bicarbonate of ammonia flow is opened after about 5min greatly to 50ml/min, Cerium II Chloride flow is opened greatly to 33ml/min, till having flowed.
4. by 40 ℃ of deionized water C repeated washing cerous carbonate precipitations, make its wash water specific conductivity be less than 10 μ s/cm;
5. the 60 ℃ of oven dry 3h in baking oven of the cerous carbonate after washing completely had both been obtained to finished product pure white sheet cerous carbonate.
Electronic Speculum figure as shown in Figure 2.
Example two
Cerium II Chloride in example one is changed to cerous nitrate, repeats example one experimental procedure and obtain equally pure white sheet cerous carbonate.
Electronic Speculum figure as shown in Figure 3.
Example three
1. being equipped with concentration is the solution of cerium chloride by oxidation 100L of 0.87mol/l, the ammonium bicarbonate soln 160L that outfit concentration is 1.9mol/L;
2. in 500L weighing apparatus warm water bath reaction vessel, first add about 50L deionized water C, be incubated 55 ℃;
3. open and stir, first add bicarbonate of ammonia cumulative volume 1% to deionization C, after bicarbonate of ammonia and solution of cerium chloride by oxidation are slowly added dropwise in deionized water C simultaneously, after crystalline precipitate to be formed, bicarbonate of ammonia flow is opened into 5L/min, solution of cerium chloride by oxidation concentration is opened into 3L/min, and the reaction times is controlled at 30min left and right.
4. by 40 ℃ of deionized water C repeated washing cerous carbonate precipitations, make its wash water specific conductivity be less than 10 μ s/cm;
5. the 60 ℃ of oven dry 3h in baking oven of the cerous carbonate after washing completely had both been obtained to finished product pure white sheet cerous carbonate.
Electronic Speculum figure as shown in Figure 4.
Claims (6)
1. a preparation method for sheet cerous carbonate, is characterized in that, preparation method's concrete steps of this sheet cerous carbonate are as follows:
The first step, the ammonium bicarbonate soln B that the trivalent cerium ion solution A that outfit concentration is 0.58mol/L ~ 0.87mol/L and concentration are 1.27mol/L ~ 1.9mol/L;
Second step, is equipped with trivalent cerium ion solution A and the ammonium bicarbonate soln B of proper volume, changes and in proportioning, makes bicarbonate of ammonia excessive 10% ~ 16%, and making trivalent cerium ion in solution and the mol ratio of bicarbonate of ammonia is 2:7;
The 3rd step, first add the ammonium bicarbonate soln B of 1% volume to reaction vessel, with speed slowly, trivalent cerium ion solution A and ammonium bicarbonate soln B are joined in reaction vessel simultaneously respectively afterwards, react after about 5min, the flow of trivalent cerium ion solution A and ammonium bicarbonate soln B is opened greatly by its volume ratio, guaranteed that trivalent cerium ion solution A and ammonium bicarbonate soln B have flowed simultaneously;
The 4th step, by the precipitate with deionized water C washing generating, in surveying wash water, specific conductivity is less than 10 μ s/cm and stops washing;
The 5th step, the cerous carbonate that washing is suitable precipitates suction filtration post-drying 3 hours, makes ceria content be greater than 50%.
2. the preparation method of a kind of sheet cerous carbonate according to claim 1, is characterized in that: the temperature of reaction of described trivalent cerium ion solution A and ammonium bicarbonate soln B is 55 ℃.
3. the preparation method of a kind of sheet cerous carbonate according to claim 1, is characterized in that: the temperature of the described deionized water C for washing precipitation is 35 ℃ ~ 45 ℃.
4. the preparation method of a kind of sheet cerous carbonate according to claim 1, is characterized in that: the bake out temperature after described washing is 55 ℃ ~ 65 ℃.
5. the preparation method of a kind of sheet cerous carbonate according to claim 1, is characterized in that: described trivalent cerium ion solution A adopts Cerium II Chloride or cerous nitrate solution.
6. the preparation method of a kind of sheet cerous carbonate according to claim 1, is characterized in that: described trivalent cerium ion can also adopt CeO2, and its concentration is 100g/L ~ 150g/L, and corresponding bicarbonate of ammonia concentration is 100g/L ~ 150g/L.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104310456A (en) * | 2014-10-14 | 2015-01-28 | 瑞科稀土冶金及功能材料国家工程研究中心有限公司 | Production method and device of fine-grained low-chloride rare earth carbonate |
| CN112126977A (en) * | 2020-08-11 | 2020-12-25 | 南昌大学 | Method for preparing high-purity flaky single crystal and flaky crystal dense aggregated cerium carbonate |
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Cited By (2)
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| CN112126977A (en) * | 2020-08-11 | 2020-12-25 | 南昌大学 | Method for preparing high-purity flaky single crystal and flaky crystal dense aggregated cerium carbonate |
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