CN104355616A - High-temperature and high-pressure preparation method of cubic phase lanthanum, manganese and titanium oxide and product thereof - Google Patents
High-temperature and high-pressure preparation method of cubic phase lanthanum, manganese and titanium oxide and product thereof Download PDFInfo
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Abstract
The invention discloses a high-temperature and high-pressure preparation method of cubic phase lanthanum, manganese and titanium oxide and a product thereof, and belongs to the technical field of the preparation of novel functional ceramic material. The method comprises steps that La(NO3)3, MnO and C16H36O4Ti are taken as raw material and prepared into precursor through a sol-gel method, and the precursor is subjected to processes of briquetting, assembly, high-temperature and high-pressure synthesis and cooling depressurization, so as to obtain the cubic phase material with the constituent being La2MnTiO6. The product prepared is small in grain size and high in purity; high-temperature and high-pressure equipment adopted is simple to operate and can rapidly carry out industrialization, and high-quality lanthanum, manganese and titanium oxide cubic phase material can be obtained.
Description
Technical field
The invention belongs to technical field prepared by new function stupalith.Be specifically related to the Emission in Cubic of lanthanum manganese titanium oxide, and with lanthanum nitrate (La (NO
3)
3), manganese oxide (MnO), butyl (tetra) titanate (C
16h
36o
4ti) be raw material, utilize High Temperature High Pressure technology of preparing to synthesize the method for lanthanum manganese titanium oxide Emission in Cubic.
Background technology
Along with development and the progress of society, people are also more deep to the cognition of material, and double negative property becomes in current widespread use the class material occupying critical role already.Double negative property is corresponding to uhligite ABO
3type oxide compound is named, and their general formula can be expressed as A
2b ' B " O
6, " Sauerstoffatom of atom and its nearest neighbour forms B ' O to wherein B ', B
6, B " O
6octahedron, these two kinds of octahedrons form three-dimensional network regularly alternately, and A atom is positioned among 8 adjacent octahedral spaces.Due to B ' and B, " ion has different electronic configurations, different ionic radius and exchange interaction dissimilar each other, thus to replacement, the powerful measure becoming and further investigate its inherent physical essence of adulterating of B position ion.Rare earth double-perovskite compound has stable crystalline structure, unique electromagnetic performance and very high redox, hydrogenolysis, isomerization, electrocatalysis isoreactivity, has very large potentiality to be exploited in the field such as environment protection and Industrial Catalysis.The lanthanum manganese titanium oxide (La (comprising solid phase method, sol-gel method etc.) under current normal condition and prepare
2mnTiO
6) crystalline structure of material is tetragonal.Also do not report at present about the preparation of employing High Temperature High Pressure.The kind adding this type oxide is can be described as mutually by the new texture of research lanthanum manganese titanium oxide, and the different new chemical catalysis function thereupon produced, and the application of Industrial Catalysis aspect can be increased in.
Summary of the invention
The technical problem to be solved in the present invention adopts the new method preparing lanthanum manganese titanium oxide material-HP-HT synthesize method, the method adjusts the formation of the high pressure phase structure of lanthanum manganese titanium oxide mainly through synthesis temperature and pressure, prepare the high pressure phase material of the lanthanum manganese titanium oxide with brand-new structure; And the method is easy to implement.
Lanthanum manganese titanium oxide new texture phase of the present invention, component is La
2mnTiO
6, its structure is cubic structure.
Technical scheme prepared by lanthanum manganese titanium oxide Emission in Cubic of the present invention is as described below.
A preparation method for lanthanum manganese titanium oxide Emission in Cubic, with lanthanum nitrate (La (NO
3)
3), manganese oxide (MnO), butyl (tetra) titanate (C
16h
36o
4ti) be raw material, obtain precursor by sol-gel method, precursor is obtained lanthanum manganese titanium oxide Emission in Cubic material through the technological process of briquetting, assembling, HP-HT synthesize, cooling release; Described precursor, is by 2: 1: 1 mixing in molar ratio of lanthanum nitrate, manganese oxide, butyl (tetra) titanate, prepares gained by sol-gel method; Described briquetting is the precursor that will obtain, and is pressed into sheet by boron nitride (BN) pipe diameter; Said assembling, is sheet-shaped material is loaded boron nitride (BN) pipe, and boron nitride tube is loaded carbon tube heating container, then put into pyrophyllite synthetic cavity; Said HP-HT synthesize carries out in very universal existing high temperature high pressure device, pressure be 5GPa, temperature be 1300 ~ 1600 DEG C at heat-insulation pressure keeping 30 ~ 60 minutes, stop heating, finally cool release.
Above-mentioned technical scheme also can be stated as:
A high temperature and high pressure preparation process for Emission in Cubic lanthanum manganese titanium oxide, the processing step through obtained powdery precursor and HP-HT synthesize obtains Emission in Cubic lanthanum manganese titanium oxide;
Described obtained powdery precursor, be with lanthanum nitrate, manganese oxide, butyl (tetra) titanate in molar ratio 2: 1: 1 for raw material, obtained by sol-gel method;
Described HP-HT synthesize, high temperature high pressure device is carried out; By the compression moulding of powdery precursor, outside parcel boron nitride (BN) layer, loads in pyrophyllite synthetic cavity; Pressure be 5GPa, at temperature is 1300 ~ 1600 DEG C, heat-insulation pressure keeping 30 ~ 60 minutes, cooling release.
Above-mentioned obtained powdery precursor, can obtain by the sol-gel method of prior art, also can obtain according to the following procedure: butyl (tetra) titanate is joined in mass concentration 95% ethanol, produce white precipitate, drip concentrated nitric acid wherein to dissolve completely to precipitation, obtain butyl (tetra) titanate clear solution; By La (NO
3)
3be dissolved in deionized water with MnO, then add glucose or the citric acid of butyl (tetra) titanate clear solution and 4.6 ~ 4.9 times of butyl (tetra) titanate mole numbers, stir and be warming up to 70 DEG C, constant temperature is stirred to solution and becomes thickness formation colloidal sol, and rebake obtains dry bulk colloid; Sinter 3 hours by 500 DEG C, colloid, obtain the presoma of collosol and gel; Presoma is ground to form finely powdered, again obtains powdery precursor after sintering.
Described baking, can at 110 DEG C dry 24 hours.
Described lanthanum nitrate (La (NO
3)
3), manganese oxide (MnO), butyl (tetra) titanate (C
16h
36o
4ti) be raw material, their quality purity>=99.9%.
Described cooling release can be naturally cool to release after room temperature after stopping heating; Can also be stop the rear first pressurize release after 3 ~ 8 minutes of heating, then naturally cool to room temperature.The latter is conducive to reducing dephasign, is conducive to the protection of equipment and reduces the duration of service of press, improves the service efficiency of press.
Compound experiment of the present invention can complete on domestic DS029B type six-plane piercer.The pressure synthesized, temperature and heat-insulation pressure keeping time are the important factors affecting Emission in Cubic lanthanum manganese titanium oxide purity, and optimum synthesis condition of the present invention is synthesis pressure is 5GPa, and synthesis temperature is 1450 DEG C, heat-insulation pressure keeping 30 minutes.
The present invention also asks to protect the product adopting the high temperature and high pressure preparation process of Emission in Cubic lanthanum manganese titanium oxide of the present invention to obtain, and the component of this product is La
2mnTiO
6, its structure is cubic structure.
Beneficial effect of the present invention is, the first, and present method first utilizes sol-gel method to prepare precursor, and reactant is mixed, and products therefrom particle diameter is little, and the final product Emission in Cubic lanthanum manganese titanium oxide purity of gained is high.Second, the high-temperature high-pressure apparatus that the lanthanum manganese titanium oxide that present method is produced adopts is used for producing diamond at present at home in a large number, it is simple to operate, can implement industrialization quickly with its production, and can obtain the lanthanum manganese titanium oxide Emission in Cubic material of high-quality.
Accompanying drawing explanation
Fig. 1 is lanthanum manganese titanium oxide (La prepared by embodiment 1 High Temperature High Pressure
2mnTiO
6) X-ray diffractogram.
Fig. 2 is lanthanum manganese titanium oxide (La prepared by embodiment 2 High Temperature High Pressure
2mnTiO
6) X-ray diffractogram.
Fig. 3 is lanthanum manganese titanium oxide (La prepared by embodiment 3 High Temperature High Pressure
2mnTiO
6) X-ray diffractogram.
Fig. 4 is lanthanum manganese titanium oxide (La prepared by embodiment 4 High Temperature High Pressure
2mnTiO
6) X-ray diffractogram.
Fig. 5 is lanthanum manganese titanium oxide (La prepared by comparative example 1 sol-gel method
2mnTiO
6) X-ray diffractogram.
Embodiment
Embodiment 1:
By butyl (tetra) titanate (C
16h
36o
4ti) join in a small amount of 95% ethanol, produce white precipitate, drip appropriate concentrated nitric acid wherein, until precipitation is dissolved completely, obtain butyl (tetra) titanate clear solution; La (NO in molar ratio
3)
3, MnO and C
16h
36o
4ti takes La (NO at 2: 1: 1
3)
3, MnO, and be dissolved in deionized water, add glucose again, the consumption of glucose is 4.8 times of butyl (tetra) titanate by molar basis, adds wherein by the butyl (tetra) titanate clear solution obtained above, makes its abundant complexing, 70 DEG C of constant temperature water baths stir and form gel, at 110 DEG C, drying must do glue in 24 hours, and dry glue, through 500 DEG C of roastings 3 hours, obtains the presoma of collosol and gel; Presoma is ground to form finely powdered, again obtains precursor after sintering.By precursor abrasive dust, then pressed the flap-type precursor causing into suitably height to load BN pipe, then sample is loaded in pyrophyllite synthetic cavity.Make heating tube with graphite in synthetic cavity, do insulation tube with agalmatolite, synthesis pressure is 5GPa, and temperature is 1450 DEG C, 30 minutes pressure-maintaining and heat-preservation time, and after stopping heating, sample naturally cools to release after room temperature.Emission in Cubic lanthanum manganese titanium oxide (La prepared by this condition
2mnTiO
6) crystallization degree is best, purity is the highest, and concrete X-ray the results are shown in Figure 1.
Glucose in the present embodiment can substitute with the citric acid of identical mole number, and effect is the same.
Embodiment 2:
Adopt the starting material identical with embodiment 1 and assembling, synthesis pressure is 5GPa, and temperature is 1450 DEG C, 60 minutes pressure-maintaining and heat-preservation time, stop heating afterwards sample naturally cool to release after room temperature, cubic structure La prepared by this condition
2mnTiO
6degree of crystallinity is poor.Concrete X-ray the results are shown in Figure 2.
Embodiment 3
Adopt the starting material identical with embodiment 1 and assembling, synthesis pressure is 5GPa, and temperature is 1600 DEG C, 30 minutes pressure-maintaining and heat-preservation time, stop heating afterwards sample naturally cool to release after room temperature, cubic structure La prepared by this condition
2mnTiO
6containing more dephasign.Concrete X-ray the results are shown in Figure 3.
Embodiment 4
Adopt the starting material identical with embodiment 2 and assembling, synthesis pressure is 5GPa, and temperature is 1300 DEG C, 30 minutes pressure-maintaining and heat-preservation time, stop heating afterwards sample naturally cool to release after room temperature, cubic structure La prepared by this condition
2mnTiO
6containing dephasign.Concrete X-ray the results are shown in Figure 4.
Comparative example 1
A certain amount of butyl (tetra) titanate is joined in a small amount of 95% ethanol, produce white precipitate, drip appropriate concentrated nitric acid wherein, until precipitation is dissolved completely, obtain clear solution.La (NO in molar ratio
3)
3, MnO and butyl (tetra) titanate be take La (NO at 2: 1: 1
3)
3, MnO, and be dissolved in deionized water, add the glucose that molar basis is 4.8 times of butyl (tetra) titanate again, then add wherein by the clear solution obtained above, make its abundant complexing, 70 DEG C of constant temperature water baths stir and form gel, at 110 DEG C, drying must do glue in 24 hours, dry glue was through 500 DEG C of presintering 3 hours, and the sample that presintering obtains is again through grinding, compressing tablet, and then at 1400 DEG C of temperature, sintering obtains Tetragonal La in 12 hours
2mnTiO
6.Concrete X-ray the results are shown in Figure 5.
Claims (6)
1. a high temperature and high pressure preparation process for Emission in Cubic lanthanum manganese titanium oxide, the processing step through obtained powdery precursor and HP-HT synthesize obtains Emission in Cubic lanthanum manganese titanium oxide;
Described obtained powdery precursor, be with lanthanum nitrate, manganese oxide, butyl (tetra) titanate in molar ratio 2: 1: 1 for raw material, obtained by sol-gel method;
Described HP-HT synthesize, high temperature high pressure device is carried out; By the compression moulding of powdery precursor, outside parcel boron nitride layer, loads in pyrophyllite synthetic cavity; Pressure be 5GPa, at temperature is 1300 ~ 1600 DEG C, heat-insulation pressure keeping 30 ~ 60 minutes, cooling release.
2. the high temperature and high pressure preparation process of Emission in Cubic lanthanum manganese titanium oxide according to claim 1, it is characterized in that, described obtained powdery precursor, butyl (tetra) titanate is joined in mass concentration 95% ethanol, produce white precipitate, drip concentrated nitric acid wherein to dissolve completely to precipitation, obtain butyl (tetra) titanate clear solution; By La (NO
3)
3be dissolved in deionized water with MnO, then add glucose or the citric acid of butyl (tetra) titanate clear solution and 4.6 ~ 4.9 times of butyl (tetra) titanate mole numbers, stir and be warming up to 70 DEG C, constant temperature is stirred to solution and becomes thickness formation colloidal sol, and rebake obtains dry bulk colloid; Sinter 3 hours by 500 DEG C, colloid, obtain the presoma of collosol and gel; Presoma is ground to form finely powdered, again obtains powdery precursor after sintering.
3. the high temperature and high pressure preparation process of Emission in Cubic lanthanum manganese titanium oxide according to claim 2, is characterized in that, described baking, can be at 110 DEG C dry 24 hours.
4. the high temperature and high pressure preparation process of Emission in Cubic lanthanum manganese titanium oxide according to claim 1 and 2, is characterized in that, described HP-HT synthesize, be synthesis pressure is 5GPa, and synthesis temperature is 1450 DEG C, heat-insulation pressure keeping 30 minutes.
5. the high temperature and high pressure preparation process of Emission in Cubic lanthanum manganese titanium oxide according to claim 1 and 2, it is characterized in that, described lanthanum nitrate, manganese oxide, butyl (tetra) titanate are raw material, their quality purity >=99.9%.
6. the product that the high temperature and high pressure preparation process of the Emission in Cubic lanthanum manganese titanium oxide of claim 1 is obtained, its component is La
2mnTiO
6, structure is cubic structure.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102897845A (en) * | 2012-11-07 | 2013-01-30 | 吉林大学 | High-temperature and high-pressure preparation method for cubic phase barium-iron-antimony oxide |
| CN103198912A (en) * | 2013-04-12 | 2013-07-10 | 吉林大学 | High-temperature and high-pressure preparation method of cubic-phase scandium germanium oxide |
-
2014
- 2014-10-27 CN CN201410591734.1A patent/CN104355616A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102897845A (en) * | 2012-11-07 | 2013-01-30 | 吉林大学 | High-temperature and high-pressure preparation method for cubic phase barium-iron-antimony oxide |
| CN103198912A (en) * | 2013-04-12 | 2013-07-10 | 吉林大学 | High-temperature and high-pressure preparation method of cubic-phase scandium germanium oxide |
Non-Patent Citations (1)
| Title |
|---|
| 孙艳: "稀土双钙钛矿型催化剂对含酚废水光催化净化作用的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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