CN104528754A - Synthesis method of nanorod-shaped AlPO4-15 - Google Patents
Synthesis method of nanorod-shaped AlPO4-15 Download PDFInfo
- Publication number
- CN104528754A CN104528754A CN201410649136.5A CN201410649136A CN104528754A CN 104528754 A CN104528754 A CN 104528754A CN 201410649136 A CN201410649136 A CN 201410649136A CN 104528754 A CN104528754 A CN 104528754A
- Authority
- CN
- China
- Prior art keywords
- urea
- alpo
- shape
- solution
- nano bar
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/36—Aluminium phosphates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a synthesis method of nanorod-shaped AlPO4-15, and belongs to the field of nanomaterials. The method comprises the following steps: 1, dissolving an aluminum salt in water to prepare an aluminum salt solution with the concentration of 0.8-3mol/L; 2, adding urea to the aluminum salt solution according to a molar ratio of the aluminum salt to urea of 4:1-15:1, and stirring for 10-60min; 3, adding phosphate to a solution obtained in step 2 according to a molar ratio of Al:P of 1:1, and stirring for 10-60min; and 4, transferring a solution obtained in step 3 to a hydrothermal reaction kettle, reacting at 130-160DEG C for 30-72h, filtering after the reaction ends, washing the obtained filter cake, and drying to obtain nanorod-shaped AlPO4-15 powder. AlPO4-15 nanorods are formed through self-assembling under hydrothermal synthesis conditions by changing the content of urea, prolonging the reaction time and adjusting the reaction temperature.
Description
Technical field
The present invention relates to technical field of nano material, particularly a kind of nano bar-shape AlPO
4the synthetic method of-15.
Background technology
In recent years due to the potential application of material in scientific and technological of nanorod structure, it causes the interest of investigators.Nanometer rod represents the material of a series of space one dimension, and presents very important photochemistry, optical physics and transfer transport character.These are all different with the material of other structures.
Phosphoric acid salt is because its special structural unit MPO
4obtain very large concern.In this structural unit, M is a trivalent metal ion, can increase different types of skeleton construction like this.Bellitto Carlo etc. has inferred these phosphatic structure formation, and be exactly in the octahedral coordination of a distortion, each atoms metal is surrounded by six Sauerstoffatoms, constitutes four abutments, end another from water molecules; Aluminum phosphate material can use gentle condition to implement the optionally acid catalyzed chemical conversion of Br nsted with high transformation efficiency and selectivity, such as, alcohol is converted into alkene (CN 102361693 A).In addition phosphaljel can alleviate the symptoms such as the sour regurgitation that hyperchlorhydria causes, and is applicable to the antiacid treatment of the acid-related disease such as gastric and duodenal ulcer and reflux esophagitis.Nanjing Normal University Yang Jin flies seminar in CN103145110A, CN102786041A, describes a kind of method preparing hypo-aluminum orthophosphate respectively, but Hypophosporous Acid, 50 decomposes produces the phosphine gas of severe toxicity, hypophosphite is wayward, and to cause obtaining impurity in products many.
Adopt eco-friendly method, the problem that phosphate material needs overcome prepared by the material of preparation specific morphology.
Summary of the invention
In order to make up the deficiencies in the prior art, the invention provides a kind of nano bar-shape AlPO
4the environmental protection synthetic method of-15.
Technical scheme of the present invention is:
A kind of nano bar-shape AlPO
4the synthetic method of-15, comprises the following steps:
1) by water-soluble for aluminium salt, the aluminum salt solution of preparation 0.8-3mol/L;
2) be that 4:1-15:1 adds urea in aluminum salt solution according to the mol ratio of aluminium salt and urea, stir 10-60min;
3) be that 1:1 is to step 2 according to the mol ratio of Al:P) add phosphoric acid salt in the solution of gained, stir 10-60min;
4) be transferred in hydrothermal reaction kettle by step 3) gained solution, and to arrange temperature of reaction be 130-160 DEG C, the reaction times is 30-72h, after question response terminates, filters, and washing leaching cake is also dry, obtains nano bar-shape AlPO
4-15 powder.
Preferably, aluminium salt described in step 1) is aluminum chloride, Tai-Ace S 150 or aluminum nitrate.
Further, the concentration of aluminium salt is 1-2mol/L.
Preferably, step 2) in the mol ratio of aluminium salt and urea be 6:1-10:1.
Preferably, the phosphoric acid salt described in step 3) is triammonium phosphate or tertiary sodium phosphate.
Beneficial effect of the present invention is:
The present invention adopts the influence condition such as content, prolongation reaction times, adjustment temperature of reaction changing urea, and under hydrothermal synthesizing condition, autonomous dress defines AlPO4-15 nanometer rod.Wherein, urea provides hydroxide radical for reaction system, provides condition for preparing mono-dispersed nano particle, and hydroxide radical in conjunction with the proton in phosphate solution, thus forms the buffer system of an acid base equilibrium, is conducive to the formation of nanometer rod; The formation of concentration to aluminum phosphate nanometer rod of urea soln is most important; Also there is impact in reaction times for bar-shaped growth, reaction times in short-term, obtain as small particle, along with the reaction times extends, obtain nano bar-shape structure, this provides condition for preparing mono-dispersed nano particle, for the nano material preparing specific morphology provides foundation, provides a kind of eco-friendly preparation method.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is that embodiment 1 contrasts X-ray diffraction (XRD) figure of powder with standard card number;
Transmission electron microscope (TEM) figure of Fig. 2 aluminum phosphate obtained by embodiment 1;
Transmission electron microscope (TEM) figure of Fig. 3 aluminum phosphate obtained by embodiment 2;
Transmission electron microscope (TEM) figure of Fig. 4 aluminum phosphate obtained by embodiment 3;
Transmission electron microscope (TEM) figure of Fig. 5 aluminum phosphate obtained by embodiment 4;
Transmission electron microscope (TEM) figure of Fig. 6 aluminum phosphate obtained by comparative example.
Embodiment
Comparative example
0.08mol aluminum nitrate is dissolved in the deionized water of 80ml, after violent stirring 20min, again 0.08mol tertiary sodium phosphate is dissolved in above-mentioned solution, continue to stir 30min, then solution is transferred in the stainless hydrothermal reaction kettle of teflon-lined of 100 ml, sealing, arranging temperature of reaction is 150 DEG C, after question response 35h, off-response, when reactor cool to room temperature, with vacuum filter by white precipitate and solution separating, then by white precipitate ethanol and distilled water wash.The sample obtained is dry 24 h at 60 DEG C.Gained sample does tem study (result as shown in Figure 6).
Embodiment 1
0.08mol aluminum nitrate and 1.21g urea are dissolved in the deionized water of 80ml, after violent stirring 20min, again 0.08mol tertiary sodium phosphate is dissolved in above-mentioned solution, continue to stir 30min, then solution is transferred in the stainless hydrothermal reaction kettle of teflon-lined of 100 ml, sealing, arranging temperature of reaction is 150 DEG C, after question response 35h, off-response, when reactor cool to room temperature, with vacuum filter by white precipitate and solution separating, then by white precipitate ethanol and distilled water wash.The sample obtained is dry 24 h at 60 DEG C.Gained sample does X-ray diffraction analysis (result as shown in Figure 1) and tem study (result as shown in Figure 2).The present embodiment obtains nano bar-shape AlPO
4-15 powder.
As can be seen from Figure 1, the XRD figure shape of sample, (-101), (110), (101), (200), the characteristic peak of (130) and (-132) can easily from pure monoclinic crystal AlPO4-15 phase (JCPDS 45-0183, spatial group P21/n (no. 14)) middle index, from XRD spectrogram, the diffraction peak of other impurity do not detected.Further, the XRD collection of illustrative plates of more various sample, urea decomposition makes (-101) increase with the ratio diffraction peak intensity of (101).
Comparison diagram 2 and Fig. 6, can find out, adding the formation of aluminum phosphate nanometer rod of urea is most important.When not adding urea, the particle obtained is sheet structure, is of a size of 1 μm.When a certain amount of urea of interpolation; The nano bar-shape structure that TEM only observes.
Embodiment 2
0.16mol aluminum nitrate and 2.0g urea are dissolved in the deionized water of 80ml, after violent stirring 20min, again 0.16mol tertiary sodium phosphate is dissolved in above-mentioned solution, continue to stir 30min, then solution is transferred in the stainless hydrothermal reaction kettle of teflon-lined of 100 ml, sealing, arranging temperature of reaction is 150 DEG C, after question response 30h, off-response, when reactor cool to room temperature, with vacuum filter by white precipitate and solution separating, then by white precipitate ethanol and distilled water wash.The sample obtained is dry 24 h at 60 DEG C.Gained sample does tem study (result as shown in Figure 3).
Embodiment 3
0.16mol aluminum nitrate and 2.0g urea are dissolved in the deionized water of 80ml, after violent stirring 20min, again 0.16mol tertiary sodium phosphate is dissolved in above-mentioned solution, continue to stir 30min, then solution is transferred in the stainless hydrothermal reaction kettle of teflon-lined of 100 ml, sealing, arranging temperature of reaction is 150 DEG C, after question response 50h, off-response, when reactor cool to room temperature, with vacuum filter by white precipitate and solution separating, then by white precipitate ethanol and distilled water wash.The sample obtained is dry 24 h at 60 DEG C.Gained sample does tem study (result as shown in Figure 4).
As can be seen from Figure 4, there is certain influence in the reaction times for bar-shaped growth, the reaction times in short-term, obtain as small particle, along with the reaction times extend, as shown in Figure 4, mean length and the width of the growth of nanometer rod are about 85nm and 35nm respectively.Embodiment of comparing 2 gained nano particle has good club shaped structure.
Embodiment 4
0.16mol aluminum nitrate and 0.9g urea are dissolved in the deionized water of 80ml, after violent stirring 20min, again 0.08mol tertiary sodium phosphate is dissolved in above-mentioned solution, continue to stir 30min, then solution is transferred in the stainless hydrothermal reaction kettle of teflon-lined of 100 ml, sealing, arranging temperature of reaction is 150 DEG C, after question response 35h, off-response, when reactor cool to room temperature, with vacuum filter by white precipitate and solution separating, then by white precipitate ethanol and distilled water wash.The sample obtained is dry 24 h at 60 DEG C.Gained sample does tem study (result as shown in Figure 5).
As can be seen from Figure 5, when the amount of urea is less than finite concentration, has the aluminum phosphate of a small amount of sheet structure around, illustrate that the concentration of urea plays most important effect in the reaction.
Embodiment 5
0.16mol Tai-Ace S 150 and 1.5g urea are dissolved in the deionized water of 80ml, after violent stirring 20min, again 0.16mol triammonium phosphate is dissolved in above-mentioned solution, continue to stir 30min, then solution is transferred in the stainless hydrothermal reaction kettle of teflon-lined of 100 ml, sealing, arranging temperature of reaction is 160 DEG C, after question response 33h, off-response, when reactor cool to room temperature, with vacuum filter by white precipitate and solution separating, then by white precipitate ethanol and distilled water wash.The sample obtained is dry 24 h at 60 DEG C, obtained nano bar-shape AlPO
4-15 powder.
Embodiment 6
0.2mol Tai-Ace S 150 and 1.52g urea are dissolved in the deionized water of 80ml, after violent stirring 40min, again 0.16mol triammonium phosphate is dissolved in above-mentioned solution, continue to stir 20min, then solution is transferred in the stainless hydrothermal reaction kettle of teflon-lined of 100 ml, sealing, arranging temperature of reaction is 140 DEG C, after question response 60h, off-response, when reactor cool to room temperature, with vacuum filter by white precipitate and solution separating, then by white precipitate ethanol and distilled water wash.The sample obtained is dry 24 h at 60 DEG C, obtained nano bar-shape AlPO
4-15 powder.
Claims (5)
1. a nano bar-shape AlPO
4the synthetic method of-15, is characterized in that: comprise the following steps:
1) by water-soluble for aluminium salt, the aluminum salt solution of preparation 0.8-3mol/L;
2) be that 4:1-15:1 adds urea in aluminum salt solution according to the mol ratio of aluminium salt and urea, stir 10-60min;
3) be that 1:1 is to step 2 according to the mol ratio of Al:P) add phosphoric acid salt in the solution of gained, stir 10-60min;
4) be transferred in hydrothermal reaction kettle by step 3) gained solution, and to arrange temperature of reaction be 130-160 DEG C, the reaction times is 30-72h, after question response terminates, filters, and washing leaching cake is also dry, obtains nano bar-shape AlPO
4-15 powder.
2. nano bar-shape AlPO as claimed in claim 1
4the synthetic method of-15, is characterized in that: aluminium salt described in step 1) is aluminum chloride, Tai-Ace S 150 or aluminum nitrate.
3. nano bar-shape AlPO as claimed in claim 2
4the synthetic method of-15, is characterized in that: the concentration of aluminium salt is 1-2mol/L.
4. nano bar-shape AlPO as claimed in claim 1
4the synthetic method of-15, is characterized in that: step 2) in the mol ratio of aluminium salt and urea be 6:1-10:1.
5. nano bar-shape AlPO as claimed in claim 1
4the synthetic method of-15, is characterized in that: the phosphoric acid salt described in step 3) is triammonium phosphate or tertiary sodium phosphate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410649136.5A CN104528754B (en) | 2014-11-17 | 2014-11-17 | A kind of nano bar-shape AlPO4the synthetic method of-15 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410649136.5A CN104528754B (en) | 2014-11-17 | 2014-11-17 | A kind of nano bar-shape AlPO4the synthetic method of-15 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104528754A true CN104528754A (en) | 2015-04-22 |
| CN104528754B CN104528754B (en) | 2016-08-24 |
Family
ID=52844449
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410649136.5A Active CN104528754B (en) | 2014-11-17 | 2014-11-17 | A kind of nano bar-shape AlPO4the synthetic method of-15 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104528754B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112028087A (en) * | 2020-08-14 | 2020-12-04 | 深圳技术大学 | Transition metal element doped AlPO-15 molecular sieve and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003183020A (en) * | 2001-10-11 | 2003-07-03 | Mitsubishi Chemicals Corp | Production method for zeolite, zeolite prepared thereby, and steam-adsorptive material containing the zeolite |
| CN103539202A (en) * | 2013-08-23 | 2014-01-29 | 中山大学 | Method for preparing titanium dioxide nanowire through self-reaction of single reagent |
-
2014
- 2014-11-17 CN CN201410649136.5A patent/CN104528754B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003183020A (en) * | 2001-10-11 | 2003-07-03 | Mitsubishi Chemicals Corp | Production method for zeolite, zeolite prepared thereby, and steam-adsorptive material containing the zeolite |
| CN103539202A (en) * | 2013-08-23 | 2014-01-29 | 中山大学 | Method for preparing titanium dioxide nanowire through self-reaction of single reagent |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112028087A (en) * | 2020-08-14 | 2020-12-04 | 深圳技术大学 | Transition metal element doped AlPO-15 molecular sieve and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104528754B (en) | 2016-08-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101559979B (en) | Method for preparing extrafine anatase titanium dioxide nano rods | |
| CN101319371B (en) | Production method of spindle-shaped nano ZnO monocrystal | |
| CN103771485B (en) | A kind of controllable method for preparing of cupric oxide three-dimensional manometer self-assembly | |
| CN104591301B (en) | Porous nano CoFe2O4Preparation method of (1) | |
| CN105923657B (en) | A kind of preparation method of monoclinic form tungstic acid | |
| CN103523824B (en) | The preparation method of nano-sheet ferroelectric material for a kind of photocatalysis | |
| CN110104623B (en) | Preparation method of phosphorus-rich transition metal phosphide cobalt tetraphosphate with different morphologies | |
| Wu et al. | Template-free synthesis of mesoporous anatase yttrium-doped TiO 2 nanosheet-array films from waste tricolor fluorescent powder with high photocatalytic activity | |
| CN103754935B (en) | Method for synthesizing lead molybdate tower crystal at room temperature | |
| CN103787296B (en) | A kind of disc-shaped aluminum phosphate and preparation method thereof | |
| CN102616840B (en) | Method for preparing transition metal oxide nano single crystal with specific exposed crystal faces through stripping nanosheets | |
| CN104528754A (en) | Synthesis method of nanorod-shaped AlPO4-15 | |
| CN102897723A (en) | Hydrothermal method for preparing selenium-copper-based nano-crystals | |
| CN108676018B (en) | Organic-inorganic hybrid perovskite nano material and preparation method thereof | |
| CN113353908A (en) | Preparation method of rod-shaped nano iron phosphate material | |
| Manseki et al. | Structure identification of Ti (iv) clusters in low-temperature TiO 2 crystallization: Creating high-surface area brush-shaped rutile TiO 2 | |
| CN101774603B (en) | Preparation method of mesoporous magnesium borate microsphere | |
| CN107033907B (en) | Rare earth doped nanocrystals and methods of making the same | |
| CN102557055A (en) | Preparation method of zirconium silicate powder | |
| CN109908871A (en) | A kind of magnetic Fe3O4The preparation method and applications of@MIL-100 | |
| CN105970281B (en) | A kind of simple preparation method of cadmium vanadate monocrystal nanowire | |
| CN106995209B (en) | A kind of ψ-type Zirconium phosphate crystal nanometer sheet and its preparation and application | |
| CN103754929A (en) | Preparation method for TiO2/InVO4 composite porous micro-sphere | |
| CN110002494B (en) | Superfine anatase type TiO2Nanowire and method for preparing same | |
| CN108163895B (en) | Preparation method of cation-modified molybdenum oxide or tungsten oxide nanowire with large specific surface area |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |