CN102992274B - Method for preparing dysprosium carbonate peroxide - Google Patents
Method for preparing dysprosium carbonate peroxide Download PDFInfo
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- CN102992274B CN102992274B CN201210383494.7A CN201210383494A CN102992274B CN 102992274 B CN102992274 B CN 102992274B CN 201210383494 A CN201210383494 A CN 201210383494A CN 102992274 B CN102992274 B CN 102992274B
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Abstract
The invention relates to a method for preparing dysprosium carbonate peroxide, belonging to material preparation processes. The method comprises the following steps: preparing an ammonium bicarbonate solution by using ammonium bicarbonate, ammonia water and deionized water, adding a dysprosium nitrate solution into the ammonium bicarbonate solution to obtain a mixed solution consisting of the ammonium bicarbonate, the ammonia water and the dysprosium nitrate, adding hydrogen peroxide into the mixed solution to generate dysprosium carbonate peroxide precipitates, ageing, and filtering and washing the precipitates to obtain dysprosium carbonate peroxide products, which are uniform in particle and good in flowability and have a granular appearance formed by lamella stacking.
Description
Technical field
The present invention relates to a kind of method preparing dysprosium carbonate peroxide, belong to a kind of material preparation process.
Background technology
Reactive oxygen compounds sends visible ray in chemical reaction process, and peroxycarbonate compares one of active area in Chemiluminescence Study field.Dysprosium carbonate peroxide be a kind of not soluble in water, be less than the 100 DEG C solids not decomposing, easily preserve in temperature, dysprosium ion has unique electronic structure, as the additive of glass, Nd-Fe-B permanent magnet, also in metal halid lamp, magneto-optical memory material, yttrium iron or yttrium aluminum garnet, nuclear industry, the transmitting of dysprosium ion forms primarily of two emission bands: one is yellow emission band, another is blue emissive band, when suitable Huang/blue light strength than, Dy
3+by transmitting white, mix the luminescent material of dysprosium likely as two primary colours inorganic fluorescent powders, dysprosium ion plays auxiliary catalysis enhancement in chemiluminescent process progresses.Dysprosium carbonate peroxide is a kind of reactive oxygen compounds, have high-energy, active oxygen is high due to the energy state than ground state oxygen molecule, therefore shows the reactive behavior far above ground state oxygen molecule, its chemiluminescence activity is higher than sodium carbonate peroxide, is the oxygenant of a kind of " green " relatively.Dysprosium carbonate peroxide has highly sensitive, that selectivity is good chemical luminous system, likely becomes Chemiluminescence Study, application focus.Preparation and the research of the sodium carbonate peroxide of reported in literature are relatively many, and dysprosium carbonate peroxide preparation method and sodium carbonate peroxide preparation method completely different, because dysprosium carbonate is not soluble in water, as by dysprosium carbonate and water furnishing pulpous state, add hydrogen peroxide, after stirring certain hour, filter, wash, detect by analysis, precipitation is still dysprosium carbonate; Ammonium bicarbonate soln is added again as joined in Dysprosium trinitrate solution by hydrogen peroxide, or hydrogen peroxide joined in ammonium bicarbonate soln join in Dysprosium trinitrate solution again, two kinds of methods are after fully reacting, and what obtain is precipitated as dysprosium carbonate, and it is infeasible for utilizing traditional method to prepare dysprosium carbonate peroxide.
Summary of the invention
The object of the present invention is to provide a kind of uniform particles, good fluidity, pattern is superimposed as the preparation method of granular dysprosium carbonate peroxide by sheet.
Technical solution:
Technical solution: the present invention adds bicarbonate of ammonia in the reactor and concentration is the ammoniacal liquor of 28%, bicarbonate of ammonia and ammoniacal liquor mol ratio are 1: 0.67-1.17, add deionized water again, bicarbonate of ammonia and deionized water mol ratio are 1: 6-9.1, obtaining concentration is 3.7-4.5mol/L ammonium bicarbonate soln, at room temperature, the Dysprosium trinitrate solution that concentration is 0.98-1.56mol/L is added in ammonium bicarbonate soln, bicarbonate of ammonia and Dysprosium trinitrate mol ratio are 1: 0.046-0.056, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Dysprosium trinitrate; The hydrogen peroxide that concentration is 30% is added in mixing solutions, Dysprosium trinitrate and hydrogen peroxide mol ratio are 1: 2.3-4.1, reaction 1-4 hour, generation dysprosium carbonate peroxide precipitates, static ageing 24-48 hour, by sedimentation and filtration, washing, obtain uniform particles, good fluidity, pattern is superimposed as granular dysprosium carbonate peroxide product by sheet.
Invention effect: in the present invention, ammonium bicarbonate concentration and digestion time are crucial, add ammoniacal liquor and can improve ammonium bicarbonate concentration in solution, when ammonium bicarbonate concentration is lower than 3.7mol/L, the a small amount of flocks adding the generation of Dysprosium trinitrate solution is not easily dissolved, the concentration of Dysprosium trinitrate in ammonium bicarbonate soln is less, product yield is low, along with ammonium bicarbonate concentration in solution raises, Dysprosium trinitrate concentration also raises, it is high that the dysprosium carbonate peroxide generated precipitates a yield, only has formation bicarbonate of ammonia, the mixing solutions of ammoniacal liquor and Dysprosium trinitrate, dysprosium carbonate peroxide precipitation could be generated when adding hydrogen peroxide.Digestion time is the key factor determining dysprosium carbonate peroxide granularity, and digestion time is less than 4 hours, and dysprosium carbonate peroxide deposit seeds is very thin, sad filter, static ageing more than 24 hours, is precipitated uniform particles, good fluidity, and pattern is superimposed as granular dysprosium carbonate peroxide by sheet.The present invention is convenient to realize suitability for industrialized production, utilizes factory's tradition oxalic acid dysprosium precipitation operation, just can prepare dysprosium carbonate peroxide product.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of dysprosium carbonate peroxide of the present invention;
Fig. 2 is the infrared spectrogram of dysprosium carbonate peroxide of the present invention;
Fig. 3 is the SEM figure of dysprosium carbonate peroxide of the present invention.
Embodiment
Embodiment 1
Add 350g bicarbonate of ammonia and 28% ammoniacal liquor 300ml in the reactor, add deionized water 520ml, obtaining concentration is 4.43mol/L ammonium bicarbonate soln, at room temperature, in ammonium bicarbonate soln, add the Dysprosium trinitrate solution that 180ml concentration is 1.18mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Dysprosium trinitrate; In mixing solutions, add the hydrogen peroxide that 70ml concentration is 30%, react 3.5 hours, produce dysprosium carbonate peroxide precipitation, static ageing 40 hours, by sedimentation and filtration, washing, obtains the dysprosium carbonate peroxide product of uniform particles, good fluidity.
Embodiment 2
Add 350g bicarbonate of ammonia and 28% ammoniacal liquor 200ml in the reactor, add deionized water 620ml, obtaining concentration is 4.43mol/L ammonium bicarbonate soln, at room temperature, in ammonium bicarbonate soln, add the Dysprosium trinitrate solution that 208ml concentration is 0.98mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Dysprosium trinitrate; In mixing solutions, add the hydrogen peroxide that 85ml concentration is 30%, react 4 hours, produce dysprosium carbonate peroxide precipitation, static ageing 28 hours, by sedimentation and filtration, washing, obtains the dysprosium carbonate peroxide product of uniform particles, good fluidity.
Embodiment 3
Add 300g bicarbonate of ammonia and 28% ammoniacal liquor 300ml in the reactor, add deionized water 550ml, obtaining concentration is 3.8mol/L ammonium bicarbonate soln, at room temperature, in ammonium bicarbonate soln, add the Dysprosium trinitrate solution that 131ml concentration is 1.56mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Dysprosium trinitrate; In mixing solutions, add the hydrogen peroxide that 52ml concentration is 30%, react 2.5 hours, produce dysprosium carbonate peroxide precipitation, static ageing 30 hours, by sedimentation and filtration, washing, obtains the dysprosium carbonate peroxide product of uniform particles, good fluidity.
Claims (1)
1. prepare the method for dysprosium carbonate peroxide, it is characterized in that, bicarbonate of ammonia is added and concentration is the ammoniacal liquor of 28% in reactor, bicarbonate of ammonia and ammoniacal liquor mol ratio are 1: 0.67-1.17, add deionized water again, bicarbonate of ammonia and deionized water mol ratio are 1: 6-9.1, obtaining concentration is 3.7-4.5mol/L ammonium bicarbonate soln, at room temperature, the Dysprosium trinitrate solution that concentration is 0.98-1.56mol/L is added in ammonium bicarbonate soln, bicarbonate of ammonia and Dysprosium trinitrate mol ratio are 1: 0.046-0.056, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Dysprosium trinitrate; The hydrogen peroxide that concentration is 30% is added in mixing solutions, Dysprosium trinitrate and hydrogen peroxide mol ratio are 1: 2.3-4.1, reaction 1-4 hour, generation dysprosium carbonate peroxide precipitates, static ageing 24-48 hour, by sedimentation and filtration, washing, obtain uniform particles, good fluidity, pattern is superimposed as granular dysprosium carbonate peroxide product by sheet.
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| CN201210383494.7A CN102992274B (en) | 2012-09-22 | 2012-09-22 | Method for preparing dysprosium carbonate peroxide |
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| CN201210383494.7A CN102992274B (en) | 2012-09-22 | 2012-09-22 | Method for preparing dysprosium carbonate peroxide |
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| CN102992274A CN102992274A (en) | 2013-03-27 |
| CN102992274B true CN102992274B (en) | 2015-01-28 |
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| RU2182164C2 (en) * | 1996-03-27 | 2002-05-10 | Солвей Интерокс (Сосьете Аноним) | Sodium percarbonate, method of selection of sodium percarbonate, composition of detergent |
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