CN101214977B - Preparation method of lithium zirconate material for absorbing carbon dioxide at high temperature - Google Patents
Preparation method of lithium zirconate material for absorbing carbon dioxide at high temperature Download PDFInfo
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- CN101214977B CN101214977B CN200710063282XA CN200710063282A CN101214977B CN 101214977 B CN101214977 B CN 101214977B CN 200710063282X A CN200710063282X A CN 200710063282XA CN 200710063282 A CN200710063282 A CN 200710063282A CN 101214977 B CN101214977 B CN 101214977B
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- lithium zirconate
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2
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Abstract
The invention relates to a novel process for preparing a lithium zirconate material capable of absorbing CO2 at high temperature, which needs not complex doping of multiple elements, but only needs nano ZrO2 and nano Li2CO3 as raw materials to obtain the lithium zirconate material via wet-mixing, microwave treatment and high-temperature calcining. Compared with the prior art, the invention has the advantages of low synthesis temperature, energy consumption reduction, simple process of preparation and easy industrial production.
Description
Technical field
The present invention relates to a kind ofly at high temperature can directly absorb CO
2Lithium zirconate (Li
2ZrO
3) preparation methods.
Background technology
In a lot of industrial production such as generation current factory, petroleum chemical enterprise still main with fossil oils such as oil, coal, Sweet natural gases as the main energy, because combustion of fossil fuels can discharge a large amount of CO
2Gas causes the Greenhouse effect aggravation.Usually therefore the expellant gas temperature, syntheticly at high temperature can absorb CO efficiently, rapidly than higher from the High Temperature Furnaces Heating Apparatus of power station, petroleum chemical enterprise etc.
2Material, thereby reduce CO
2Gas purging has become one of important channel of alleviating Greenhouse effect.And the lithium zirconate material can directly absorb CO between 450～700 ℃ of high temperature
2, so it is expected to become high temperature CO
2The absorbing material of gas.
People such as the K.Nakagawa of Toshiba Corp have just carried out since 1997 at high temperature can directly absorbing CO
2The research of lithium zirconate material (JP 999214 (1997), and JP 10085553 (1998), and JP 11253746 (1999), JP 11253738 (1999), JP2000-262837 (2000), JP2000-262890 (2000), JP2000-176406 (2000), JP2000-176403 (2000).The at present existing high temperature that is used for absorbs CO
2The lithium zirconate material, preparation technology's more complicated, and long reaction time, power consumption is big.The inventor has carried out certain improvement to the preparation technology of this material.
Summary of the invention
The object of the present invention is to provide the easy lithium zirconate preparation methods of a kind of preparation manipulation.Lithium zirconate preparation methods provided by the present invention is to be the ZrO of 20～200nm with particle diameter
2The Li of (weight ratio is 48～75%) and particle diameter 0.3um
2CO
3(weight ratio is 25～52%) mixes in solvent, through microwave treatment, prepares lithium zirconate through high-temperature calcination then in High Temperature Furnaces Heating Apparatus in microwave oven.
The microwave power that is applied among the present invention is 500～2500W, and the treatment time is 10～120min.
The calcining temperature of material is 550～700 ℃ among the present invention, insulation 3～6h.
Solvent used in the present invention is methyl alcohol, ethanol, formic acid, acetate, acetone, the mixing solutions of perhaps wherein any two kinds or two or more arbitrary proportions.
The present invention at first adopts microwave treatment, calcines the preparation that realizes the lithium zirconate material through certain temperature again.The material preparation temperature is lower, has reduced energy consumption.Preparation process technology is simple, is easy to suitability for industrialized production.The CO of material
2Absorptive character are good, and the material with optimal absorption performance is CO first
2Absorptive capacity reaches 25.61wt% approximately, and after 25 absorption circulations, the absorptive capacity rate of fall-off is 0.47 ‰.
Description of drawings
Fig. 1 is the CO of lithium zirconate material of the present invention
2Circulation absorptive character curve, X-coordinate is a cycle index among the figure, and ordinate zou is the percentage ratio that weight increases, and unit is wt%.
Embodiment
Embodiment 1
Take by weighing the ZrO that particle diameter is 20nm
223.81g and particle diameter is the Li of 0.3 μ m
2CO
325.79g put into beaker jointly, in beaker, add ethanolic soln, make jelly under stirring.In the microwave oven of 500W power, handle 120min, calcine 6h down, through the lithium zirconate material that grinds, screening obtains median size 2.4 μ m at 700 ℃.With synthetic lithium zirconate material in 500 ℃, 20%CO
2(80% air) constant temperature down keeps for some time, reaches absorption equilibrium post-absorption capacity and reaches 19.28wt%.
Embodiment 2
Take by weighing the ZrO that particle diameter is 120nm
225.41g and particle diameter is the Li of 0.3um
2CO
322.53g put into beaker jointly, in beaker, add methyl alcohol, alcohol mixed solution, make jelly under stirring.In the microwave oven of 2500W power, handle 10min, calcine 6h down, through the lithium zirconate material that grinds, screening obtains median size 4.1 μ m at 550 ℃.With synthetic lithium zirconate material in 500 ℃, 20%CO
2(80% air) constant temperature down keeps for some time, reaches absorption equilibrium post-absorption capacity and reaches 20.67wt%.
Embodiment 3
Take by weighing the ZrO that particle diameter is 100nm
227.21g and particle diameter is the Li of 0.3um
2CO
316.68g put into beaker jointly, in beaker, add the mixing solutions of ethanol and formic acid, and add a spot of acetate and acetone, make jelly under stirring.In the microwave oven of 1800W power, handled 30 minutes, calcine 2h down, through the lithium zirconate material that grinds, screening obtains median size 3.3 μ m at 700 ℃.With synthetic lithium zirconate material in 500 ℃, 20%CO
2(80% air) constant temperature down keeps for some time, reaches absorption equilibrium post-absorption capacity and reaches 25.61wt%.At 500 ℃, 20%CO
2(80% air) be constant temperature 3h down, and constant temperature keeps carrying out under the such test procedure of 1h lithium zirconate absorption CO under 700 ℃ of air atmospheres
2Circulation absorptive character tests, absorb circulation through 25 times after, the absorptive capacity rate of fall-off is 0.47 ‰, the results are shown in Figure 1.
Embodiment 4
Take by weighing the ZrO that particle diameter is 150nm
228.41g and particle diameter is the Li of 0.3um
2CO
319.74g put into beaker jointly, in beaker, add the mixing solutions of methyl alcohol and formic acid, and add a spot of acetone, make jelly under stirring.In the microwave oven of 800W power, handle 60min, calcine 3h down, through the lithium zirconate material that grinds, screening obtains median size 3.7 μ m at 700 ℃.With synthetic lithium zirconate material in 500 ℃, 20%CO
2(80% air) constant temperature down keeps for some time, reaches absorption equilibrium post-absorption capacity and reaches 22.65wt%.
Take by weighing the ZrO that particle diameter is 200nm
229.12g and particle diameter is the Li of 0.3um
2CO
39.71g put into beaker jointly, in beaker, add the mixing solutions of methyl alcohol and acetate, and add a spot of formic acid, ethanol and acetone, make jelly under stirring.In the microwave oven of 1000W power, handle 50min, calcine 4h down, through the lithium zirconate material that grinds, screening obtains median size 5.6 μ m at 700 ℃.With synthetic lithium zirconate material in 500 ℃, 20%CO
2(80% air) constant temperature down keeps for some time, reaches absorption equilibrium post-absorption capacity and reaches 21.28wt%.
Claims (4)
1. one kind at high temperature can directly absorb CO
2The lithium zirconate preparation methods, it is characterized in that:
With weight percent be 48～75%, particle diameter is the ZrO of 20～200nm
2Be 25～52% with weight percent, the Li of particle diameter 0.3 μ m
2CO
3In solvent, mix, in microwave oven,, in High Temperature Furnaces Heating Apparatus, prepare lithium zirconate then through high-temperature calcination through microwave treatment.
2. preparation method according to claim 1 is characterized in that the microwave power that is applied is 500～2500W, and the treatment time is 10～120min.
3. preparation method according to claim 1 is characterized in that calcining temperature is 550～700 ℃, insulation 3～6h.
4. preparation method according to claim 1 is characterized in that employed solvent is methyl alcohol, ethanol, formic acid, acetate, acetone, the mixing solutions of perhaps wherein any two kinds or two or more arbitrary proportions.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710063282XA CN101214977B (en) | 2007-01-05 | 2007-01-05 | Preparation method of lithium zirconate material for absorbing carbon dioxide at high temperature |
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|---|---|---|---|
| CN200710063282XA CN101214977B (en) | 2007-01-05 | 2007-01-05 | Preparation method of lithium zirconate material for absorbing carbon dioxide at high temperature |
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| CN101214977A CN101214977A (en) | 2008-07-09 |
| CN101214977B true CN101214977B (en) | 2011-07-20 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731076A (en) * | 2012-07-07 | 2012-10-17 | 蚌埠玻璃工业设计研究院 | Lithium silicate ceramic material absorbing high-temperature carbon dioxide and preparation method thereof |
| CN103183509A (en) * | 2013-04-17 | 2013-07-03 | 清华大学 | Lithium titanate ceramic ball tritium propagation material and preparation method thereof |
| CN103172372B (en) * | 2013-04-17 | 2014-11-26 | 清华大学 | Lithium zirconate ceramic ball tritium breeding material and preparation method thereof |
| CN103265071B (en) * | 2013-04-24 | 2014-11-26 | 河北师范大学 | Method for preparation of Li2ZrO3 cell material |
| CN109261116A (en) * | 2017-07-17 | 2019-01-25 | 天津工业大学 | A kind of preparation method of the zirconic acid lithium material of absorbing carbon dioxide at high temperature |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1140703A (en) * | 1996-04-22 | 1997-01-22 | 中国核动力研究设计院 | Process for producing high-purity monoclinic-phase lithium meta-zirconate ceramic material |
| US6737364B2 (en) * | 2002-10-07 | 2004-05-18 | International Business Machines Corporation | Method for fabricating crystalline-dielectric thin films and devices formed using same |
| CN1865154A (en) * | 2006-04-21 | 2006-11-22 | 山西大学 | Method for preparing cubic phase babrium titanate using microwave method |
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2007
- 2007-01-05 CN CN200710063282XA patent/CN101214977B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1140703A (en) * | 1996-04-22 | 1997-01-22 | 中国核动力研究设计院 | Process for producing high-purity monoclinic-phase lithium meta-zirconate ceramic material |
| US6737364B2 (en) * | 2002-10-07 | 2004-05-18 | International Business Machines Corporation | Method for fabricating crystalline-dielectric thin films and devices formed using same |
| CN1865154A (en) * | 2006-04-21 | 2006-11-22 | 山西大学 | Method for preparing cubic phase babrium titanate using microwave method |
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