CN102992273A - Method for preparing erbium carbonate peroxide - Google Patents
Method for preparing erbium carbonate peroxide Download PDFInfo
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- CN102992273A CN102992273A CN2012103834928A CN201210383492A CN102992273A CN 102992273 A CN102992273 A CN 102992273A CN 2012103834928 A CN2012103834928 A CN 2012103834928A CN 201210383492 A CN201210383492 A CN 201210383492A CN 102992273 A CN102992273 A CN 102992273A
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- erbium
- bicarbonate
- ammonia
- peroxide
- carbonic acid
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Abstract
The invention relates to a method for preparing erbium 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 an erbium chloride solution into the ammonium bicarbonate solution to obtain a mixed solution consisting of the ammonium bicarbonate, the ammonia water and the erbium chloride, adding hydrogen peroxide into the mixed solution, standing and ageing for 12 hours till erbium carbonate peroxide precipitates begin to generate, ageing for 24-48 hours, and filtering and washing the precipitates to obtain erbium carbonate peroxide products, which are uniform in particle and good in flowability and take the shape of flower-like particles formed by lamellas.
Description
Technical field
The present invention relates to a kind of method for preparing peroxide carbonic acid erbium, belong to a kind of material preparation process.
Background technology
Reactive oxygen compounds sends visible light in chemical reaction process, peroxycarbonate is one of the field of relatively enlivening in the Chemiluminescence Study field.Peroxide carbonic acid erbium is a kind of not soluble in water, be not decompose below 100 ℃ in temperature, the solid of easily preserving, because the special electron structure of erbium ion, acceptant energy also sends the light of characteristic wavelength, erbium belongs to active ions in the rare earth element, have excellent luminescent properties and energy transformation function, in the chemoluminescence process, play the auxiliary catalysis enhancement, peroxide carbonic acid erbium is a kind of reactive oxygen compounds, has high-energy, active oxygen is because higher than the energy state of ground state oxygen molecule, therefore shown the reactive behavior far above the ground state oxygen molecule, high at chemoluminescence specific activity sodium carbonate peroxide, be a kind of relatively oxygenant of " green ".Peroxide carbonic acid erbium has chemical luminous system highly sensitive, that selectivity is good, will become the focus of Chemiluminescence Study and application.
Summary of the invention
The object of the present invention is to provide a kind of uniform particles, good fluidity, pattern is made of the peroxide carbonic acid erbium preparation method of flower-shaped particle thin slice.
Technical solution: the present invention adds bicarbonate of ammonia and concentration in reactor be 28% ammoniacal liquor, bicarbonate of ammonia and ammoniacal liquor mol ratio are 1: 0.67-1.17, add again deionized water, bicarbonate of ammonia and deionized water mol ratio are 1: 6-9.1, obtaining concentration is the 3.7-4.5mol/L ammonium bicarbonate soln, at room temperature, adding concentration in the ammonium bicarbonate soln is the Erbium trichloride solution of 1.21-1.71mol/L, bicarbonate of ammonia and Erbium trichloride mol ratio are 1: 0.036-0.058 obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Erbium trichloride; Add concentration in the mixing solutions and be 30% hydrogen peroxide, Erbium trichloride and hydrogen peroxide mol ratio are 1: 2.95-7, reacted 1-4 hour, static ageing began to produce peroxide carbonic acid erbium precipitation in 12 hours, ageing 24-48 hour, with sedimentation and filtration, washing, obtain uniform particles, good fluidity, pattern is made of the peroxide carbonic acid erbium product of flower-shaped particle thin slice.
The invention effect
Bicarbonate of ammonia concentration and static digestion time are crucial among the present invention, add ammoniacal liquor and can improve bicarbonate of ammonia concentration in the solution, when bicarbonate of ammonia concentration is lower than 3.7mol/L, it is dissolved that adding Erbium trichloride solution has a small amount of flocks to be difficult for, the concentration of Erbium trichloride in ammonium bicarbonate soln is less, product yield is low, is unfavorable for suitability for industrialized production; When bringing up to 4.5mol/L along with bicarbonate of ammonia concentration from 3.7mol/L in the solution, Erbium trichloride concentration raises, and yield of peroxide carbonic acid erbium precipitation of generation also improves, and meets commercial production conditions; Only have the mixing solutions that forms bicarbonate of ammonia, ammoniacal liquor and Erbium trichloride, could generate peroxide carbonic acid erbium precipitation when adding hydrogen peroxide.Static digestion time reaches 12 hours, begins to produce peroxide carbonic acid erbium precipitation, and digestion time reached more than 24 hours, obtains the peroxide carbonic acid erbium precipitation of uniform particles, good fluidity.The present invention is convenient to realize suitability for industrialized production, utilizes factory's tradition erbium oxalate precipitation operation, just can prepare peroxide carbonic acid erbium product.
Description of drawings
Fig. 1 is the XRD figure spectrum of peroxide carbonic acid erbium of the present invention;
Fig. 2 is the infrared spectrogram of peroxide carbonic acid erbium of the present invention;
Fig. 3 is the SEM figure of peroxide carbonic acid erbium of the present invention.
Embodiment
Embodiment 1
In reactor, add 350g bicarbonate of ammonia and 28% ammoniacal liquor 300ml, add deionized water 520ml, obtaining concentration is the 4.43mol/L ammonium bicarbonate soln, at room temperature, adding 130ml concentration in the ammonium bicarbonate soln is the Erbium trichloride solution of 1.71mol/L, obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Erbium trichloride; Add 110ml concentration in the mixing solutions and be 30% hydrogen peroxide, reacted 1.5 hours, static ageing began to produce peroxide carbonic acid erbium precipitation in 12 hours, static ageing is after 24 hours, with sedimentation and filtration, washing, obtain uniform particles, good fluidity, pattern is made of the peroxide carbonic acid erbium product of flower-shaped particle thin slice.
Embodiment 2
In reactor, add 455g bicarbonate of ammonia and 28% ammoniacal liquor 260ml, add deionized water 806ml, obtaining concentration is the 4.43mol/L ammonium bicarbonate soln, at room temperature, adding 208ml concentration in the ammonium bicarbonate soln is the Erbium trichloride solution of 1.32mol/L, obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Erbium trichloride; Add 150ml concentration in the mixing solutions and be 30% hydrogen peroxide, reacted 4 hours, static ageing began to produce peroxide carbonic acid erbium precipitation in 12 hours, static ageing is after 26 hours, with sedimentation and filtration, washing, obtain uniform particles, good fluidity, pattern is made of the peroxide carbonic acid erbium product of flower-shaped particle thin slice.
Embodiment 3
In reactor, add 390g bicarbonate of ammonia and 28% ammoniacal liquor 390ml, add deionized water 715ml, obtaining concentration is the 3.8mol/L ammonium bicarbonate soln, at room temperature, adding 178ml concentration in the ammonium bicarbonate soln is the Erbium trichloride solution of 1.21mol/L, obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Erbium trichloride; Add 87ml concentration in the mixing solutions and be 30% hydrogen peroxide, reacted 2.5 hours, static ageing began to produce peroxide carbonic acid erbium precipitation in 12 hours, static ageing is after 30 hours, with sedimentation and filtration, washing, obtain uniform particles, good fluidity, pattern is made of the peroxide carbonic acid erbium product of flower-shaped particle thin slice.
Claims (1)
1. the method for preparing peroxide carbonic acid erbium, it is characterized in that, add bicarbonate of ammonia and concentration in the reactor and be 28% ammoniacal liquor, bicarbonate of ammonia and ammoniacal liquor mol ratio are 1: 0.67-1.17, add again deionized water, bicarbonate of ammonia and deionized water mol ratio are 1: 6-9.1, obtaining concentration is the 3.7-4.5mol/L ammonium bicarbonate soln, at room temperature, adding concentration in the ammonium bicarbonate soln is the Erbium trichloride solution of 1.21-1.71mol/L, bicarbonate of ammonia and Erbium trichloride mol ratio are 1: 0.036-0.058 obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Erbium trichloride; Add concentration in the mixing solutions and be 30% hydrogen peroxide, Erbium trichloride and hydrogen peroxide mol ratio are 1: 2.95-7, reacted 1-4 hour, static ageing began to produce peroxide carbonic acid erbium precipitation in 12 hours, ageing 24-48 hour, with sedimentation and filtration, washing, obtain uniform particles, good fluidity, pattern is made of the peroxide carbonic acid erbium product of flower-shaped particle thin slice.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210383492.8A CN102992273B (en) | 2012-09-22 | 2012-09-22 | Method for preparing erbium carbonate peroxide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210383492.8A CN102992273B (en) | 2012-09-22 | 2012-09-22 | Method for preparing erbium carbonate peroxide |
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| CN102992273A true CN102992273A (en) | 2013-03-27 |
| CN102992273B CN102992273B (en) | 2015-03-11 |
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| CN201210383492.8A Active CN102992273B (en) | 2012-09-22 | 2012-09-22 | Method for preparing erbium carbonate peroxide |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1415544A (en) * | 2002-10-31 | 2003-05-07 | 施越群 | Method for producing holmium oxide and erbium oxide |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1415544A (en) * | 2002-10-31 | 2003-05-07 | 施越群 | Method for producing holmium oxide and erbium oxide |
Non-Patent Citations (1)
| Title |
|---|
| MARI E. DE VASCONCELLOS等: "Solubility behavior of rare earths with ammonium carbonate and ammonium carbonate plus ammonium hydroxide:Precipitation of their peroxicarbonates", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
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