CN107010663B - The method that a kind of tartaric acid-nitrate combustion method prepares zirconic acid yttrium - Google Patents
The method that a kind of tartaric acid-nitrate combustion method prepares zirconic acid yttrium Download PDFInfo
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- CN107010663B CN107010663B CN201710234022.8A CN201710234022A CN107010663B CN 107010663 B CN107010663 B CN 107010663B CN 201710234022 A CN201710234022 A CN 201710234022A CN 107010663 B CN107010663 B CN 107010663B
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- C—CHEMISTRY; METALLURGY
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- C01G25/00—Compounds of zirconium
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- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
A kind of method that tartaric acid nitrate combustion method prepares zirconic acid yttrium, will be with ZrO (NO3)2·H2O, grinding, obtains mixed powder；Tartaric acid and ethylenediamine tetra-acetic acid are mixed, pH value is then adjusted to 2~7, after stirring, is added drop-wise to dropwise in the mortar equipped with mixed powder, side edged is ground, and after being added dropwise to complete, continues grinding uniformly, dry to obtain gel piece；Gel piece is heated at high temperature to obtain fluffy block, fluffy block is heat-treated, obtains zirconic acid yttrium.Present invention process is simple, convenient, easy to operate, and manufacturing cost is relatively low；Reaction system is mild, controllable, and combustion product impurity is few, and loss of product rate is few；The CO that tartaric acid generates when burning2It can play the role of pore-creating and improve soild oxide specific surface area, be conducive to the raising of the photocatalytic activity of powder, and the heat of compound complex agent burning short time release, can promote the quickly synthesis in low temperature of material, comparing existing high temperature solid-state method has the advantages that energy conservation and environmental protection.
Description
Technical field
The invention belongs to field of material preparation, and in particular to a kind of tartaric acid-nitrate combustion method prepares the side of zirconic acid yttrium
Method.
Background technology
Rare earth zirconate is due to unique crystal structure, having high ion conductivity and high-melting-point, which has
Good chemical stability, catalytic activity is high, by the extensive concern of researchers.In thermal barrier coating, solid electrolyte, catalysis
Agent, the processing of level radioactive nuclear waste etc. are widely used that [Xu Qiang, Pan Wei wait the burnt green stone-type Ln of2Zr2O7Ceramics
Progress [J] Rare Metals Materials and engineering, 2005, (34)：1100-1104.].
Since yttrium and another elemental cerium are two kinds of rare earth elements that content is larger on the earth, so dilute compared to other kind
Native zirconates, for zirconic acid yttrium (Y2Zr2O7) application study, raw material acquisition on, have certain resources advantage.Zirconic acid yttrium
At normal temperatures in defect fluorite structure, belong to Fm3m space groups, belong to cubic system.Thermal barrier coating, information detection, fluorescent material and
Have in terms of catalysis material extensively using [Hui Li, et al.Pressure-induced structural
transition of Y2Zr2O7[J].Journal of Alloys and Compounds,2016,660:446-449.]。
The zirconic acid yttrium preparation method of existing report is mainly sol-gal process, hydro-thermal method and high-temperature solid-phase sintering method.Such as
[Jovan í Marc, Sanz Ana, the et al.New red-shade environmental-friendly such as Jovan í Marc
multifunctional pigment based on Tb and Fe doped Y2Zr2O7 for ceramic
Applications and cool roof coatings [J] .Dyes and Pigments, 133 (2016) 33-40.],
[Linhui Gao, Yue An, the et al.Hydrothermal synthesis and such as Linhui Gao
photoluminescence properties of Y2Zr2O7:Tb3+phosphors[J].Journal of Materials
Science,46(2011):1337-1340.] and Hui Li et al. [Hui Li, Qiang Tao, et al.Pressure-
induced structural transition of Y2Zr2O7[J].Journal of Alloys and Compounds,
660(2016):446-449.] target product is made using method mentioned above.In above method, high temperature solid-phase sintering
Method shortcoming be synthesis temperature height, generation Product size it is larger, it is impossible to control grain size, due to component is unevenly distributed and there are impure
Phase has stoichiometry loss；The shortcomings that simple sol-gal process, is that the generation temperature of reactant is higher, the reaction time compared with
It is long.The advantages of hydro-thermal method, is that overcoming component is unevenly distributed, there are the shortcomings that stoichiometry loss, however for equipment will
Ask higher, and the reaction time is longer.
Invention content
The method for preparing zirconic acid yttrium it is an object of the invention to propose a kind of tartaric acid-nitrate combustion method.The method energy
Enough prepare the smaller porous block Y of size2Zr2O7Powder.Present invention process is simple, can be in lower temperature Fast back-projection algorithm high fever
Tie the zirconic acid yttrium powder body of activity.
To achieve the above object, technical scheme is as follows：
The method that a kind of tartaric acid-nitrate combustion method prepares zirconic acid yttrium, includes the following steps：
1) by Y (NO3)3·6H2O and ZrO (NO3)2·H2O grinds after mixing, obtains mixed powder；Wherein, Y (NO3)3·
6H2O and ZrO (NO3)2·H2The molar ratio of O is 1:1；
2) tartaric acid and ethylenediamine tetra-acetic acid are mixed, then adjusts pH value to 2~7, obtain compound complex agent solution；
3) it after compound complex agent solution is stirred, is added drop-wise to dropwise in the mortar equipped with mixed powder, the grinding of side edged, drop
After the completion of adding, continue grinding uniformly, obtain the sticky intermediate of paste；Its mesotartaric acid and Y (NO3)3·6H2The molar ratio of O is 2 ︰
1；
4) the sticky intermediate drying of paste is obtained into gel piece；
5) gel piece is heated at high temperature to obtain fluffy block, fluffy block is heat-treated 1~3h at 500 DEG C~700 DEG C,
Obtain zirconic acid yttrium.
Further improve of the invention is, mole of tartaric acid ︰ ethylenediamine tetra-acetic acids=(1~2) ︰ 1 is pressed in step 2)
Than being mixed.
Further improve of the invention is, pH value is adjusted to 2~7 using ammonium hydroxide in step 2).
Of the invention further improve is that the rotating speed stirred in step 3) is 350~500 revs/min, the time for 6~
12h。
Further improve of the invention is that the time that drop is ground after finishing in step 3) is 15~30min.
Further improve of the invention is that dry temperature is 60~80 DEG C in step 4), and the time is 2~3h.
Of the invention further improve be, it is 10 300~400 DEG C of times that the temperature of step 5) high temperature heating, which is ,~
30min。
Further improve of the invention is, is ground before being heat-treated.
Compared with prior art, the present invention has beneficial effect：
The present invention provides a kind of low, the simple for process new synthetic method-tartaric acid-nitrate combustions of synthesis temperature
Method prepares zirconic acid yttrium.By the way that catalytic active component and catalyst carrier etc. are uniformly mixed with tartaric acid, it is put into certain temperature
In high-temperature heater, the heat released by tartaric acid burning quickly forms soild oxide；Compound complex agent can make precursor liquid
It keeps stablizing in wider pH ranges, is more easy to obtain colloidal sol without precipitating when evaporating solvent；It is prepared by method therefor of the present invention
Y2Zr2O7The advantage of powder is：(1) reaction is non-explosive redox exothermic reaction, and system is put during the reaction
Go out a large amount of heat, be substantially reduced synthesis temperature, so as to reduce zirconic acid yttrium powder reuniting, product obtained is in porous block shape
Looks, crystallinity is high, dispersibility；(2) because the hard aggregation generated in high-temperature sintering process can substantially reduce the sintering activity of powder,
And tartaric acid combustion method can promote the low-temperature sintering of powder, be conducive to synthesize the zirconic acid yttrium powder body of high sintering activity；(3) technique
Simply, it is convenient, special equipment is not needed to, easy to operate, manufacturing cost is relatively low；(4) reaction system is mild, controllable, combustion product
Impurity is few, and loss of product rate is few；(5) CO generated when tartaric acid burns2Pore-creating can be played and improve soild oxide and compare table
The effect of area is conducive to the raising of the photocatalytic activity of powder.And the heat of compound complex agent burning short time release, energy
Enough promote the quickly synthesis in low temperature of material, comparing existing high temperature solid-state method has the advantages that energy conservation and environmental protection.
Description of the drawings
Fig. 1, which is that the present invention is obtained under conditions of embodiment 2, hole bulk Y2Zr2O7The X-ray diffraction (XRD) of crystallite
Collection of illustrative plates.
Fig. 2 is the present invention blocky Y prepared under the conditions of embodiment 22Zr2O7Scanning of the crystallite under 10,000 enlargement ratios
Electronic Speculum (SEM) photo.
Fig. 3 is present invention Y prepared under the conditions of embodiment 22Zr2O7Photocatalytic degradation sieve under 500W Hg lamp irradiations
Red bright B performance maps.
Specific embodiment
The present invention will be described in detail below in conjunction with the accompanying drawings.
Embodiment 1
1) the analytically pure Y (NO of 2mmol are weighed respectively3)3·6H2O and ZrO (NO3)2·H2O is placed in agate mortar fully
Grinding obtains mixed powder.
2) by the molar ratio of tartaric acid ︰ EDTA=1 ︰ 1, quantitative analysis pure tartaric acid and ethylenediamine tetra-acetic acid are weighed
(EDTA), the compound complex agent that tartaric acid concentration is 0.2mol/L is prepared, and compound complex agent pH=7 is adjusted with concentrated ammonia liquor, is obtained
To compound complex agent solution；Wherein, tartaric acid and Y (NO3)3·6H2The molar ratio of O is 2 ︰ 1.
3) after magnetic stirring apparatus rotating speed is 350 revs/min of stirring 12h, compound complex agent solution is added drop-wise to dropwise
In mortar equipped with mixed powder, edged grinding in side after being added dropwise to complete, continues to grind 15min, obtains the sticky intermediate of paste.
4) the sticky intermediate of the paste of gained is placed in the baking oven that temperature has been preheated with 60 DEG C, dry 3h evaporates water
Point, obtain gel piece.
5) gel piece of acquisition is placed in Muffle furnace, 10min is handled at a temperature of 300 DEG C, obtain fluffy block, so
5min is ground in agate mortar afterwards, is subsequently placed in the Muffle furnace for being preheating to 500 DEG C of temperature, is heat-treated 3h, you can obtain mesh
Mark product zirconic acid yttrium (Y2Zr2O7)。
Embodiment 2
1) the analytically pure Y (NO of 3mmol are weighed respectively3)3·6H2O and ZrO (NO3)2·H2O is placed in agate mortar fully
Grinding obtains mixed powder.
2) by the molar ratio of tartaric acid ︰ EDTA=1 ︰ 1, quantitative analysis pure tartaric acid and ethylenediamine tetra-acetic acid are weighed
(EDTA), the compound complex agent that tartaric acid concentration is 0.2mol/L is prepared, and compound complex agent pH=6 is adjusted with concentrated ammonia liquor, is obtained
To compound complex agent solution；Wherein, tartaric acid and Y (NO3)3·6H2The molar ratio of O is 2 ︰ 1.
3) after magnetic stirring apparatus rotating speed is 400 revs/min of stirring 8h, compound complex agent solution is added drop-wise to dress dropwise
Have in the mortar of mixed powder, the grinding of side edged, after being added dropwise to complete, continue to grind 20min, obtain the sticky intermediate of paste.
4) the sticky intermediate of the paste of gained is placed in the baking oven that temperature has been preheated with 80 DEG C, dry 2h evaporates water
Point, obtain gel piece.
5) gel piece of acquisition is placed in Muffle furnace, 15min is handled at a temperature of 350 DEG C, obtain fluffy block, so
5min is ground in agate mortar afterwards, is subsequently placed in the Muffle furnace for being preheating to 600 DEG C of temperature, is heat-treated 2h, you can obtain mesh
Mark product zirconic acid yttrium (Y2Zr2O7)。
It will be seen from figure 1 that the present invention successfully prepares Y using tartaric acid-nitrate combustion method2Zr2O7(comparison ICDD
Card number：01-074-9311).
Figure it is seen that the Y prepared using tartaric acid-nitrate combustion method2Zr2O7In there is hole bulk pattern.
From figure 3, it can be seen that under conditions of 500W Hg lamp irradiations, the zirconic acid yttrium prepared by this patent is in 2h to concentration
Rhodamine B degradation rate for 10mg/L can reach 76.8%, subtract product absorption and dyestuff net degradation rate from after degradation
About 54%.
Embodiment 3
1) the analytically pure Y (NO of 5mmol are weighed respectively3)3·6H2O and ZrO (NO3)2·H2O is placed in agate mortar fully
Grinding obtains mixed powder.
2) by the molar ratio of tartaric acid ︰ EDTA=1 ︰ 2, quantitative analysis pure tartaric acid and ethylenediamine tetra-acetic acid are weighed
(EDTA), the compound complex agent that tartaric acid concentration is 0.2mol/L is prepared, and compound complex agent pH=5 is adjusted with concentrated ammonia liquor, is obtained
To compound complex agent solution；Wherein, tartaric acid and Y (NO3)3·6H2The molar ratio of O is 2 ︰ 1.
3) after magnetic stirring apparatus rotating speed is 450 revs/min of stirring 8h, compound complex agent solution is added drop-wise to dress dropwise
Have in the mortar of mixed powder, the grinding of side edged, after being added dropwise to complete, continue to grind 25min, obtain the sticky intermediate of paste.
4) the sticky intermediate of the paste of gained is placed in the baking oven that temperature has been preheated with 70 DEG C, dry 3h evaporates water
Point, obtain gel piece.
5) gel piece of acquisition is placed in Muffle furnace, 20min is handled at a temperature of 400 DEG C, obtain fluffy block, so
5min is ground in agate mortar afterwards, is subsequently placed in the Muffle furnace for being preheating to 650 DEG C of temperature, is heat-treated 2h, you can obtain mesh
Mark product zirconic acid yttrium (Y2Zr2O7)。
Embodiment 4
1) the analytically pure Y (NO of 8mmol are weighed respectively3)3·6H2O and ZrO (NO3)2·H2O is placed in agate mortar fully
Grinding obtains mixed powder.
2) by the molar ratio of tartaric acid ︰ EDTA=1 ︰ 1.5, quantitative analysis pure tartaric acid and ethylenediamine tetra-acetic acid are weighed
(EDTA), the compound complex agent that tartaric acid concentration is 0.2mol/L is prepared, and compound complex agent pH=2 is adjusted with concentrated ammonia liquor, is obtained
To compound complex agent solution；Wherein, tartaric acid and Y (NO3)3·6H2The molar ratio of O is 2 ︰ 1.
3) after magnetic stirring apparatus rotating speed is 500 revs/min of stirring 6h, compound complex agent solution is added drop-wise to dress dropwise
Have in the mortar of mixed powder, the grinding of side edged, after being added dropwise to complete, continue to grind 30min, obtain the sticky intermediate of paste.
4) the sticky intermediate of the paste of gained is placed in the baking oven that temperature has been preheated with 80 DEG C, dry 3h evaporates water
Point, obtain gel piece.
5) gel piece of acquisition is placed in Muffle furnace, 30min is handled at a temperature of 400 DEG C, obtain fluffy block, so
5min is ground in agate mortar afterwards, is subsequently placed in the Muffle furnace for being preheating to 700 DEG C of temperature, is heat-treated 1h, you can obtain mesh
Mark product zirconic acid yttrium (Y2Zr2O7)。
The present invention has the following advantages：
1) product made from the method is in porous block pattern, and crystallinity is high, good dispersion.
2) the method does not need to special installation, and simple for process easy to operate, manufacturing cost is relatively low.
3) the method is when tartaric acid and EDTA compound complex agents burn, the CO of release2Can zirconic acid yttrium ratio be promoted with pore-creating
The expansion of surface area is conducive to the raising of the photocatalytic activity of powder.
4) heat of compound complex agent burning short time release, can promote the quickly synthesis in low temperature of material, compare existing
High temperature solid-state method has the advantages that energy conservation and environmental protection.
Claims (6)
1. the method that a kind of tartaric acid-nitrate combustion method prepares zirconic acid yttrium, which is characterized in that include the following steps：
1) by Y (NO3)3·6H2O and ZrO (NO3)2·H2O grinds after mixing, obtains mixed powder；Wherein, Y (NO3)3·6H2O
With ZrO (NO3)2·H2The molar ratio of O is 1:1；
2) tartaric acid and ethylenediamine tetra-acetic acid are mixed, then adjusts pH value to 2~7, obtain compound complex agent solution；
3) it after compound complex agent solution is stirred, is added drop-wise to dropwise in the mortar equipped with mixed powder, edged grinding in side drips
Cheng Hou continues grinding uniformly, obtains the sticky intermediate of paste；Its mesotartaric acid and Y (NO3)3·6H2The molar ratio of O is 2 ︰ 1；
4) the sticky intermediate drying of paste is obtained into gel piece；
5) gel piece is heated at high temperature to obtain fluffy block, fluffy block at 500 DEG C~700 DEG C is heat-treated 1~3h, is obtained
Zirconic acid yttrium；
It is mixed in step 2) by the molar ratio of tartaric acid ︰ ethylenediamine tetra-acetic acids=(1~2) ︰ 1；
Dry temperature is 60~80 DEG C in step 4), and the time is 2~3h.
2. the method that a kind of tartaric acid-nitrate combustion method according to claim 1 prepares zirconic acid yttrium, which is characterized in that
PH value is adjusted to 2~7 using ammonium hydroxide in step 2).
3. the method that a kind of tartaric acid-nitrate combustion method according to claim 1 prepares zirconic acid yttrium, which is characterized in that
The rotating speed stirred in step 3) is 350~500 revs/min, and the time is 6~12h.
4. the method that a kind of tartaric acid-nitrate combustion method according to claim 1 prepares zirconic acid yttrium, which is characterized in that
The time that drop is ground after finishing in step 3) is 15~30min.
5. the method that a kind of tartaric acid-nitrate combustion method according to claim 1 prepares zirconic acid yttrium, which is characterized in that
It is 10~30min that the temperature of step 5) high temperature heating, which is 300~400 DEG C of times,.
6. the method that a kind of tartaric acid-nitrate combustion method according to claim 1 prepares zirconic acid yttrium, which is characterized in that
It is ground before being heat-treated.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1548227A (en) * | 2003-05-16 | 2004-11-24 | 中国科学院成都有机化学研究所 | Catalyst for preparing carbon nanotube and its prepn |
| CN102923765A (en) * | 2012-10-08 | 2013-02-13 | 中山大学 | Indium tin oxide (ITO) nano powder and preparation method thereof |
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2017
- 2017-04-11 CN CN201710234022.8A patent/CN107010663B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1548227A (en) * | 2003-05-16 | 2004-11-24 | 中国科学院成都有机化学研究所 | Catalyst for preparing carbon nanotube and its prepn |
| CN102923765A (en) * | 2012-10-08 | 2013-02-13 | 中山大学 | Indium tin oxide (ITO) nano powder and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| (Y,Ce)2Zr2O7纳米粉体的制备及其发光性能的研究;王蕾等;《中国计量学院学报》;20160331;第27卷(第1期);第108-112、120页 * |
| 有机前驱体低温燃烧制备Ba0.8Sr0.2TiO3纳米粉体;刘塞珠;《陕西师范大学学报(自然科学版)》;20090331;第37卷(第2期);第57-59页 * |
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