CN103058724B - Preparation method of large-particle gadolinium oxide - Google Patents
Preparation method of large-particle gadolinium oxide Download PDFInfo
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- CN103058724B CN103058724B CN201210386973.4A CN201210386973A CN103058724B CN 103058724 B CN103058724 B CN 103058724B CN 201210386973 A CN201210386973 A CN 201210386973A CN 103058724 B CN103058724 B CN 103058724B
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Abstract
The invention relates to a preparation method of large-particle gadolinium oxide, and belongs to a preparation technology of materials. The method comprises the following steps of: preparing an ammonium bicarbonate solution with ammonium bicarbonate, ammonia water and deionized water, adding gadolinium chloride solution to the ammonium bicarbonate solution to obtain a mixed solution of ammonium bicarbonate, ammonia water and gadolinium chloride, adding hydrogen peroxide to the mixed solution to generate an oxygen gadolinium carbonate precipitation, aging for 24-48 hours, filtering and washing the precipitation, and keeping the firing temperature at 900-1200 DEG C for thermal insulation for 4 hours to obtain the large-particle gadolinium oxide product, which has the characteristics of uniform particle, favorable liquidity, and the morphology of which appears to be a petal piled by sheet and the central grain size D50 of which is 120-240 micrometers.
Description
Technical field
The present invention relates to a kind of method of preparing macrobead gadolinium sesquioxide, belong to a kind of material preparation process.
Background technology
Gadolinium sesquioxide is in field widespread uses such as catalysis, pottery, Solid Oxide Fuel Cell, luminescent material, polishing materials.For example gadolinium sesquioxide adulterated TiOx is made catalyzer can efficient degradation tropeolin-D, and gadolinium sesquioxide also can be used as the main component in solid fuel cell.Along with scientific and technological development, different technologies field has also proposed many requirements to gadolinium sesquioxide particle size.At present more to the research of nano level gadolinium sesquioxide, the research to macrobead gadolinium sesquioxide and preparation technology are relatively less.Granularity control and mensuration thereof when the gadolinium sesquioxide that document Deng Han celery is shown synthesizes, the tenth national rare earth elementary analytical chemistry symposium collection of thesis, 2003, provides gadolinium sesquioxide preparation method, prepare gadolinium oxalate precipitation with oxalic acid and Gadolinium trichloride, after gadolinium oxalate calcination, obtain 2-6 μ m gadolinium sesquioxide product; In rare-earth industry is produced, adopt oxalic acid, bicarbonate of ammonia, sodium carbonate as precipitation agent, Gadolinium trichloride is as feed liquid, and the gadolinium oxalate, the calcination of gadolinium carbonate precipitation process that obtain, obtain medium particle diameter D
50for the gadolinium sesquioxide product of 1-15 μ m.
Summary of the invention
The object of the present invention is to provide a kind of uniform particles, good fluidity, pattern is petal-shaped, the medium particle diameter D that thin slice builds up
50be the preparation method of the macrobead gadolinium sesquioxide of 120 μ m-240 μ m.
Technical solution: the present invention adds respectively ammoniacal liquor and the deionized water that bicarbonate of ammonia, concentration are 28% in reactor, the mol ratio of bicarbonate of ammonia, ammoniacal liquor and deionized water is 1: 1: 6.27, adding concentration is the Gadolinium trichloride solution of 1.09mol/L, bicarbonate of ammonia and Gadolinium trichloride mol ratio are 1: 0.031, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Gadolinium trichloride; Be 30% hydrogen peroxide to adding concentration in mixing solutions, Gadolinium trichloride and hydrogen peroxide mol ratio are 1: 2.6, react 2.5 hours, ageing 24-48 hour, obtain peroxide gadolinium carbonate precipitation, by sedimentation and filtration, washing, calcination temperature is 900-1200 DEG C, be incubated 4 hours, obtaining uniform particles, good fluidity, pattern is petal-shaped, the medium particle diameter D that thin slice builds up
50it is the macrobead gadolinium sesquioxide of 120 μ m-240 μ m.
Invention effect
In the present invention, peroxide gadolinium carbonate precipitation digestion time and calcination temperature are to prepare macrobead gadolinium sesquioxide key, in peroxide gadolinium carbonate preparation method, digestion time is the key factor that determines peroxide gadolinium carbonate granularity, digestion time is less than 4 hours, and peroxide gadolinium carbonate deposit seeds is very thin, sad filter, static ageing is more than 24 hours, obtain macrobead peroxide gadolinium carbonate, peroxide gadolinium carbonate is at 900-1200 DEG C at calcination temperature, obtains medium particle diameter D
50for the gadolinium sesquioxide product of 120-240 μ m, control peroxide gadolinium carbonate precipitation digestion time and calcination temperature, can prepare varying particle size, uniform particles, good fluidity, pattern is that thin slice builds up petal-like gadolinium sesquioxide product, and this technique is convenient to realize suitability for industrialized production.
Brief description of the drawings
Fig. 1 is the XRD figure of macrobead gadolinium sesquioxide of the present invention;
Fig. 2 is the particle size distribution figure of macrobead gadolinium sesquioxide of the present invention;
Fig. 3 is the SEM figure of macrobead gadolinium sesquioxide of the present invention.
Embodiment
Embodiment 1
In reactor, add ammoniacal liquor and deionized water 520ml that 350g bicarbonate of ammonia, 300ml concentration are 28%, then to add 125ml concentration be the Gadolinium trichloride solution of 1.09mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Gadolinium trichloride; Be 30% hydrogen peroxide to adding 36ml concentration in mixing solutions, react 2.5 hours, ageing 24 hours, obtains peroxide gadolinium carbonate precipitation, and by sedimentation and filtration, washing, calcination temperature is 900 DEG C, insulation 4h, and obtaining medium particle diameter is the macrobead gadolinium sesquioxide of 124.0 μ m.
Embodiment 2
In reactor, add ammoniacal liquor and deionized water 520ml that 350g bicarbonate of ammonia, 300ml concentration are 28%, then to add 125ml concentration be the Gadolinium trichloride solution of 1.09mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Gadolinium trichloride; Be 30% hydrogen peroxide to adding 36ml concentration in mixing solutions, react ageing 32 hours 2.5 hours, obtain peroxide gadolinium carbonate precipitation, by sedimentation and filtration, washing, calcination temperature is 1000 DEG C, insulation 4h, obtaining medium particle diameter is the macrobead gadolinium sesquioxide of 158.4 μ m.
Embodiment 3
In reactor, add ammoniacal liquor and deionized water 520ml that 350g bicarbonate of ammonia, 300ml concentration are 28%, then to add 125ml concentration be the Gadolinium trichloride solution of 1.09mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Gadolinium trichloride; Be 30% hydrogen peroxide to adding 36ml concentration in mixing solutions, react ageing 44 hours 2.5 hours, obtain peroxide gadolinium carbonate precipitation, by sedimentation and filtration, washing, calcination temperature is 1100 DEG C, insulation 4h, obtaining medium particle diameter is the macrobead gadolinium sesquioxide of 191.4 μ m.
Embodiment 4
In reactor, add ammoniacal liquor and deionized water 520ml that 350g bicarbonate of ammonia, 300m1 concentration are 28%, then to add 125ml concentration be the Gadolinium trichloride solution of 1.09mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Gadolinium trichloride; Be 30% hydrogen peroxide to adding 36ml concentration in mixing solutions, react ageing 48 hours 2.5 hours, obtain peroxide gadolinium carbonate precipitation, by sedimentation and filtration, washing, calcination temperature is 1200 DEG C, insulation 4h, obtaining medium particle diameter is the macrobead gadolinium sesquioxide of 240.7 μ m.
Claims (4)
1. prepare the method for macrobead gadolinium sesquioxide, it is characterized in that, in reactor, add ammoniacal liquor and deionized water 520ml that 350g bicarbonate of ammonia, 300ml concentration are 28%, then to add 125ml concentration be the Gadolinium trichloride solution of 1.09mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Gadolinium trichloride; Be 30% hydrogen peroxide to adding 36ml concentration in mixing solutions, react 2.5 hours, ageing 24 hours, obtains peroxide gadolinium carbonate precipitation, and by sedimentation and filtration, washing, calcination temperature is 900 DEG C, insulation 4h, and obtaining medium particle diameter is the macrobead gadolinium sesquioxide of 124.0 μ m.
2. prepare the method for macrobead gadolinium sesquioxide, it is characterized in that, in reactor, add ammoniacal liquor and deionized water 520ml that 350g bicarbonate of ammonia, 300ml concentration are 28%, then to add 125ml concentration be the Gadolinium trichloride solution of 1.09mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Gadolinium trichloride; Be 30% hydrogen peroxide to adding 36ml concentration in mixing solutions, react ageing 32 hours 2.5 hours, obtain peroxide gadolinium carbonate precipitation, by sedimentation and filtration, washing, calcination temperature is 1000 DEG C, insulation 4h, obtaining medium particle diameter is the macrobead gadolinium sesquioxide of 158.4 μ m.
3. prepare the method for macrobead gadolinium sesquioxide, it is characterized in that, in reactor, add ammoniacal liquor and deionized water 520ml that 350g bicarbonate of ammonia, 300ml concentration are 28%, then to add 125ml concentration be the Gadolinium trichloride solution of 1.09mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Gadolinium trichloride; Be 30% hydrogen peroxide to adding 36ml concentration in mixing solutions, react ageing 44 hours 2.5 hours, obtain peroxide gadolinium carbonate precipitation, by sedimentation and filtration, washing, calcination temperature is 1100 DEG C, insulation 4h, obtaining medium particle diameter is the macrobead gadolinium sesquioxide of 191.4 μ m.
4. prepare the method for macrobead gadolinium sesquioxide, it is characterized in that, in reactor, add ammoniacal liquor and deionized water 520ml that 350g bicarbonate of ammonia, 300ml concentration are 28%, then to add 125ml concentration be the Gadolinium trichloride solution of 1.09mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Gadolinium trichloride; Be 30% hydrogen peroxide to adding 36ml concentration in mixing solutions, react ageing 48 hours 2.5 hours, obtain peroxide gadolinium carbonate precipitation, by sedimentation and filtration, washing, calcination temperature is 1200 DEG C, insulation 4h, obtaining medium particle diameter is the macrobead gadolinium sesquioxide of 240.7 μ m.
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| CN108483480A (en) * | 2018-04-11 | 2018-09-04 | 内蒙古科技大学 | The method for preparing gadolinium oxide with plant precipitating reagent |
| CN109052450B (en) * | 2018-09-17 | 2020-10-16 | 江苏国盛新材料有限公司 | Preparation method of high-purity gadolinium oxide |
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