CN102205985A - Preparation method for yttrium oxide with different specific surface area - Google Patents
Preparation method for yttrium oxide with different specific surface area Download PDFInfo
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- CN102205985A CN102205985A CN 201110083449 CN201110083449A CN102205985A CN 102205985 A CN102205985 A CN 102205985A CN 201110083449 CN201110083449 CN 201110083449 CN 201110083449 A CN201110083449 A CN 201110083449A CN 102205985 A CN102205985 A CN 102205985A
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Abstract
Disclosed is a preparation method for yttrium oxide with different specific surface areas, which is characterized by, at a temperature of 30 to 90 DEG C, adding 4 to 6 M of ammoniacal liquor into 0.4 to 0.6 M of a yttrium chloride solution until the solution reaches a pH value of 7 to 8, stirring the solution for 5 to 10 min, adding an oxalic acid solution with a mass concentration of 15 to 25% until a complete deposition is obtained, stirring the mixture for 15 to 20 min, filtering and carrying out calcination at a temperature of 800 DEG C. The invention has the advantages of a simple process, a short preparation time, low cost and capacity of preparing yttrium oxide with different specific surface areas at various reaction temperatures.
Description
Technical field
The invention belongs to the hydrometallurgy field, relate to the preparation method of different specific surface area yttrium oxide.
Background technology
The preparation method of yttrium oxide has a lot, and the Zhang Yawen of Peking University etc. have further investigation to the preparation of oxalic acid solution precipitation yttrium oxide, but the specific surface area of the yttrium oxide of preparation is less, has only 1-10m
2/ g.At present, the preparation method of bigger serface yttrium oxide is a lot, but otherwise with regard to the cost height, add tensio-active agent hydrazine etc., the production cycle is long.Still the not convenient cheaply at present simple and easy method for preparing the bigger serface yttrium oxide.
Summary of the invention
The objective of the invention is to propose a kind of preparation method of different specific surface area yttrium oxide at existing industrial bigger serface yttrium oxide preparation method deficiency.
The present invention is achieved by the following technical solutions.
Under 30-90 ℃ of temperature condition, in the 0.4-0.6M yttrium chloride solution, the ammoniacal liquor that adds 4-6M is to pH7-8, stir 5-10min, the adding mass percent concentration is that the oxalic acid solution precipitation of 15-25% is complete, stirs 15-20min, filters, drain and can get the yttrium oxalate product, this product gets the yttrium oxide product 800 ℃ of following calcinations.
Following table is under the different temperature of reaction section condition, the product specific surface area scope that obtains.
| Temperature of reaction (℃) | 30-40 | 40-60 | 60-80 | 80-90 |
| Specific surface area (m 2/g） | 10-20 | 20-25 | 25-30 | 30-40 |
Technology of the present invention is simple, preparation time is short, cost is low, can prepare different specific surface area yttrium oxide under different temperature of reaction.
Embodiment
The present invention will be further described by following examples.
Embodiment 1.
In the 2000ml beaker, prepare 0.5M yttrium chloride solution 800ml, to pH7, stir 5min, add then that to prepare mass percent concentration in advance be 20% oxalic acid solution 500ml at 35-40 ℃ of ammoniacal liquor that adds down 5M.Restir 15min filters, and drains and can get the yttrium oxalate product, and this product gets the yttrium oxide product 800 ℃ of following calcinations.This product specific surface area is 12m
2/ g.
Embodiment 2.
In the 1500L reactor, carry out, prepare 0.5M yttrium chloride solution 800L, to pH8, stir 8min, add then that to prepare mass percent concentration in advance be 20% oxalic acid solution 500L at 30-35 ℃ of ammoniacal liquor that adds down 5M.Restir 15min filters, and drains and can get the yttrium oxalate product, and this product gets the yttrium oxide product 800 ℃ of following calcinations.This product specific surface area is 17m
2/ g.
Embodiment 3.
In the 2000ml beaker, prepare 0.5M yttrium chloride solution 800ml, to pH7.5, stir 10min, add then that to prepare mass percent concentration in advance be 20% oxalic acid solution 500ml at 85-90 ℃ of ammoniacal liquor that adds down 5M.Restir 15min filters, and drains and can get the yttrium oxalate product, and this product gets the yttrium oxide product 800 ℃ of following calcinations.This product specific surface area is 39m
2/ g.
Embodiment 4.
In the 1500L reactor, carry out, prepare 0.5M yttrium chloride solution 800L, to pH8, stir 10min, add then that to prepare mass percent concentration in advance be 20% oxalic acid solution 500L at 80-90 ℃ of ammoniacal liquor that adds down 5M.Restir 15min filters, and drains and can get the yttrium oxalate product, and this product gets the yttrium oxide product 800 ℃ of following calcinations.This product specific surface area is 37m
2/ g.
Embodiment 5.
In the 1500L reactor, carry out, prepare 0.5M yttrium chloride solution 800L, to pH8, stir 10min, add then that to prepare mass percent concentration in advance be 20% oxalic acid solution 500L at 40-50 ℃ of ammoniacal liquor that adds down 5M.Restir 15min filters, and drains and can get the yttrium oxalate product, and this product gets the yttrium oxide product 800 ℃ of following calcinations.This product specific surface area is 22m
2/ g.
Embodiment 6.
In the 1500L reactor, carry out, prepare 0.5M yttrium chloride solution 800L, to pH8, stir 10min, add then that to prepare mass percent concentration in advance be 20% oxalic acid solution 500L at 50-60 ℃ of ammoniacal liquor that adds down 5M.Restir 18min filters, and drains and can get the yttrium oxalate product, and this product gets the yttrium oxide product 800 ℃ of following calcinations.This product specific surface area is 24m
2/ g.
Embodiment 7.
In the 1500L reactor, carry out, prepare 0.5M yttrium chloride solution 800L, to pH8, stir 10min, add then that to prepare mass percent concentration in advance be 20% oxalic acid solution 500L at 60-70 ℃ of ammoniacal liquor that adds down 5M.Restir 17min filters, and drains and can get the yttrium oxalate product, and this product gets the yttrium oxide product 800 ℃ of following calcinations.This product specific surface area is 27m
2/ g.
Embodiment 8.
In the 1500L reactor, carry out, prepare 0.5M yttrium chloride solution 800L, to pH8, stir 10min, add then that to prepare mass percent concentration in advance be 20% oxalic acid solution 500L at 70-80 ℃ of ammoniacal liquor that adds down 5M.Restir 19min filters, and drains and can get the yttrium oxalate product, and this product gets the yttrium oxide product 800 ℃ of following calcinations.This product specific surface area is 28m
2/ g.
Claims (1)
1. the preparation method of different specific surface area yttrium oxide, it is characterized in that under 30-90 ℃ of temperature condition, in the 0.4-0.6M yttrium chloride solution, the ammoniacal liquor that adds 4-6M is to pH7-8, stir 5-10min, the adding mass percent concentration is that the oxalic acid solution precipitation of 15-25% is complete, stirs 15-20min, filter 800 ℃ of following calcinations.
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| CN 201110083449 CN102205985A (en) | 2011-04-02 | 2011-04-02 | Preparation method for yttrium oxide with different specific surface area |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583491A (en) * | 2012-02-15 | 2012-07-18 | 淄博市周村磊宝耐火材料有限公司 | Method for preparing high-purity yttrium oxide from gemstone waste and/or ceramic waste |
| CN103803630A (en) * | 2014-01-27 | 2014-05-21 | 福建省长汀金龙稀土有限公司 | Method for preparing yttria of different sizes and different appearances |
| CN105858706A (en) * | 2015-01-22 | 2016-08-17 | 湖南稀土金属材料研究院 | Method for preparing yttrium oxide powder |
| CN106044832A (en) * | 2016-06-07 | 2016-10-26 | 福建省长汀金龙稀土有限公司 | Preparation method of yttrium oxide with central grain size being 20-50 microns |
| CN108751247A (en) * | 2018-08-17 | 2018-11-06 | 常州市卓群纳米新材料有限公司 | A kind of preparation method with the nano yttrium oxide for stablizing BET |
| CN111634935A (en) * | 2020-04-24 | 2020-09-08 | 广西科学院 | Microwave preparation method of nano rare earth oxide |
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| CN1064472A (en) * | 1991-02-26 | 1992-09-16 | 通用电气公司 | Adopt hydroxide coprecipitation step to prepare the method for yttrium oxide-gadolinium sesquioxide ceramic scintillator |
| JPH07109118A (en) * | 1993-10-13 | 1995-04-25 | Shin Etsu Chem Co Ltd | Production of rare earth element oxide |
| CN1410353A (en) * | 2001-09-30 | 2003-04-16 | 暨南大学 | Manufacturing method of nano yttrium oxide powder |
| CN1986423A (en) * | 2006-12-19 | 2007-06-27 | 王必庆 | Process of preparing zirconia and yttria with Y-doped cubic zirconia powder |
| CN101113019A (en) * | 2007-07-03 | 2008-01-30 | 李树昌 | Method for reclaiming zirconium oxide and yttrium oxide from zirconium-containing solid waste |
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2011
- 2011-04-02 CN CN 201110083449 patent/CN102205985A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1064472A (en) * | 1991-02-26 | 1992-09-16 | 通用电气公司 | Adopt hydroxide coprecipitation step to prepare the method for yttrium oxide-gadolinium sesquioxide ceramic scintillator |
| JPH07109118A (en) * | 1993-10-13 | 1995-04-25 | Shin Etsu Chem Co Ltd | Production of rare earth element oxide |
| CN1410353A (en) * | 2001-09-30 | 2003-04-16 | 暨南大学 | Manufacturing method of nano yttrium oxide powder |
| CN1986423A (en) * | 2006-12-19 | 2007-06-27 | 王必庆 | Process of preparing zirconia and yttria with Y-doped cubic zirconia powder |
| CN101113019A (en) * | 2007-07-03 | 2008-01-30 | 李树昌 | Method for reclaiming zirconium oxide and yttrium oxide from zirconium-containing solid waste |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583491A (en) * | 2012-02-15 | 2012-07-18 | 淄博市周村磊宝耐火材料有限公司 | Method for preparing high-purity yttrium oxide from gemstone waste and/or ceramic waste |
| CN103803630A (en) * | 2014-01-27 | 2014-05-21 | 福建省长汀金龙稀土有限公司 | Method for preparing yttria of different sizes and different appearances |
| CN105858706A (en) * | 2015-01-22 | 2016-08-17 | 湖南稀土金属材料研究院 | Method for preparing yttrium oxide powder |
| CN106044832A (en) * | 2016-06-07 | 2016-10-26 | 福建省长汀金龙稀土有限公司 | Preparation method of yttrium oxide with central grain size being 20-50 microns |
| CN108751247A (en) * | 2018-08-17 | 2018-11-06 | 常州市卓群纳米新材料有限公司 | A kind of preparation method with the nano yttrium oxide for stablizing BET |
| CN111634935A (en) * | 2020-04-24 | 2020-09-08 | 广西科学院 | Microwave preparation method of nano rare earth oxide |
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Application publication date: 20111005 |