CN103058724A - Preparation method of large-particle gadolinium oxide - Google Patents

Preparation method of large-particle gadolinium oxide Download PDF

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Publication number
CN103058724A
CN103058724A CN2012103869734A CN201210386973A CN103058724A CN 103058724 A CN103058724 A CN 103058724A CN 2012103869734 A CN2012103869734 A CN 2012103869734A CN 201210386973 A CN201210386973 A CN 201210386973A CN 103058724 A CN103058724 A CN 103058724A
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gadolinium
ammonia
bicarbonate
hours
concentration
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CN103058724B (en
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郝先库
张瑞祥
赵永志
汪立新
刘海旺
王士智
胡珊珊
马显东
许宗泽
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JINGRUI NEW MATERIAL CO Ltd BAOTOU
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JINGRUI NEW MATERIAL CO Ltd BAOTOU
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/40—Bio-organic fraction processing; Production of fertilisers from the organic fraction of waste or refuse

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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

The method for preparing the macrobead gadolinium sesquioxide
Technical field
The present invention relates to a kind of method for preparing the 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 the gadolinium sesquioxide adulterated TiOx make catalyzer can efficient degradation tropeolin-D, gadolinium sesquioxide also can be used as the main component in the solid fuel cell.Along with the development of science and technology, the different technologies field has also proposed many requirements to the gadolinium sesquioxide particle size.At present more to the research of nano level gadolinium sesquioxide, relatively less to research and the preparation technology of macrobead gadolinium sesquioxide.Granularity control and mensuration thereof when the gadolinium sesquioxide that document Deng Han celery is shown is synthetic, the tenth national rare earth elementary analytical chemistry symposium collection of thesis 2003, provides the gadolinium sesquioxide preparation method, prepare the gadolinium oxalate precipitation with oxalic acid and Gadolinium trichloride, obtain 2-6 μ m gadolinium sesquioxide product after the gadolinium oxalate calcination; Adopt oxalic acid, bicarbonate of ammonia, yellow soda ash as precipitation agent in rare-earth industry is produced, Gadolinium trichloride is as feed liquid, and the gadolinium oxalate that obtains, gadolinium carbonate precipitation obtain medium particle diameter D through calcination 50Gadolinium sesquioxide product for 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: it is 28% ammoniacal liquor and deionized water that the present invention adds respectively bicarbonate of ammonia, concentration in the 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; Add concentration in the mixing solutions and be 30% hydrogen peroxide, Gadolinium trichloride and hydrogen peroxide mol ratio are 1: 2.6, reacted 2.5 hours, ageing 24-48 hour, obtain peroxide gadolinium carbonate precipitation, with sedimentation and filtration, washing, calcination temperature is 900-1200 ℃, 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.
The invention effect
Peroxide gadolinium carbonate precipitation digestion time and calcination temperature are that preparation macrobead gadolinium sesquioxide is crucial among the present invention, among the peroxide gadolinium carbonate preparation method, digestion time is the key factor that determines peroxide gadolinium carbonate granularity, digestion time was 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, the peroxide gadolinium carbonate is under 900-1200 ℃ at calcination temperature, obtains medium particle diameter D 50Gadolinium sesquioxide product for 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.
Description of 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
Adding 350g bicarbonate of ammonia, 300ml concentration are 28% ammoniacal liquor and deionized water 520ml in reactor, and adding 125ml concentration is the Gadolinium trichloride solution of 1.09mol/L again, obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Gadolinium trichloride; Add 36ml concentration in the mixing solutions and be 30% hydrogen peroxide, react 2.5 hours, ageing 24 hours obtains peroxide gadolinium carbonate precipitation, and with sedimentation and filtration, washing, calcination temperature is 900 ℃, is incubated 4h, and obtaining medium particle diameter is the macrobead gadolinium sesquioxide of 124.0 μ m.
Embodiment 2
Adding 350g bicarbonate of ammonia, 300ml concentration are 28% ammoniacal liquor and deionized water 520ml in reactor, and adding 125ml concentration is the Gadolinium trichloride solution of 1.09mol/L again, obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Gadolinium trichloride; Add 36ml concentration in the mixing solutions and be 30% hydrogen peroxide, reacted ageing 32 hours 2.5 hours, obtain peroxide gadolinium carbonate precipitation, with sedimentation and filtration, washing, calcination temperature is 1000 ℃, insulation 4h, obtaining medium particle diameter is the macrobead gadolinium sesquioxide of 158.4 μ m.
Embodiment 3
Adding 350g bicarbonate of ammonia, 300ml concentration are 28% ammoniacal liquor and deionized water 520ml in reactor, and adding 125ml concentration is the Gadolinium trichloride solution of 1.09mol/L again, obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Gadolinium trichloride; Add 36ml concentration in the mixing solutions and be 30% hydrogen peroxide, reacted ageing 44 hours 2.5 hours, obtain peroxide gadolinium carbonate precipitation, with sedimentation and filtration, washing, calcination temperature is 1100 ℃, insulation 4h, obtaining medium particle diameter is the macrobead gadolinium sesquioxide of 191.4 μ m.
Embodiment 4
Adding 350g bicarbonate of ammonia, 300m1 concentration are 28% ammoniacal liquor and deionized water 520ml in reactor, and adding 125ml concentration is the Gadolinium trichloride solution of 1.09mol/L again, obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Gadolinium trichloride; Add 36ml concentration in the mixing solutions and be 30% hydrogen peroxide, reacted ageing 48 hours 2.5 hours, obtain peroxide gadolinium carbonate precipitation, with sedimentation and filtration, washing, calcination temperature is 1200 ℃, insulation 4h, obtaining medium particle diameter is the macrobead gadolinium sesquioxide of 240.7 μ m.

Claims (1)

1. the method for preparing the macrobead gadolinium sesquioxide, it is characterized in that, add respectively bicarbonate of ammonia, concentration in the reactor and be 28% ammoniacal liquor and deionized water, 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; Add concentration in the mixing solutions and be 30% hydrogen peroxide, Gadolinium trichloride and hydrogen peroxide mol ratio are 1: 2.6, reacted 2.5 hours, ageing 24-48 hour, obtain peroxide gadolinium carbonate precipitation, with sedimentation and filtration, washing, calcination temperature is 900-1200 ℃, 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.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN109052450A (en) * 2018-09-17 2018-12-21 江苏国盛新材料有限公司 A kind of preparation method of high-purity mangesium oxide gadolinium

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN109052450A (en) * 2018-09-17 2018-12-21 江苏国盛新材料有限公司 A kind of preparation method of high-purity mangesium oxide gadolinium

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