CN104310449A - Method for preparing layered double hydroxide nanorod - Google Patents
Method for preparing layered double hydroxide nanorod Download PDFInfo
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- CN104310449A CN104310449A CN201410543801.2A CN201410543801A CN104310449A CN 104310449 A CN104310449 A CN 104310449A CN 201410543801 A CN201410543801 A CN 201410543801A CN 104310449 A CN104310449 A CN 104310449A
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- double hydroxide
- trivalent metal
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/009—Compounds containing, besides iron, two or more other elements, with the exception of oxygen or hydrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
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- C—CHEMISTRY; METALLURGY
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- C01G9/00—Compounds of zinc
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- 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
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- 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
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing a layered double hydroxide nanorod. The method comprises the following steps: respectively weighing divalent and trivalent metal soluble salts, wherein the molar ratio of the divalent and trivalent metal soluble salts is 1-3:1; dissolving the divalent and trivalent metal soluble salts in deionized water to prepare a salt solution; weighing urea, wherein the molar ratio of the urea to the trivalent metal soluble salts is 7:1-9:1; dissolving the urea in the salt solution to form a mixed solution; reacting the mixed solution in a reaction kettle to form turbid liquid; cooling, washing, precipitating, performing suction filtration and drying, thus obtaining hexagonal layered double hydroxide powder, dissolving the double hydroxide powder in alcohol fluid, performing ultrasonic treatment, regulating the pH value of the alcohol solution by using nitric acid, continuously performing ultrasonic treatment, performing suction filtration, drying to obtain powder, dissolving the powder in formamide, and performing ultrasonic treatment, thus obtaining the layered double hydroxide nanorod. According to the method disclosed by the invention, the layered double hydroxide nanorod with a large draw ratio is synthesized under the condition that no template is used, the process is simple, the operation is convenient, and the structure is easily controlled.
Description
Technical field
The invention belongs to chemical field, particularly relate to a kind of layered double-hydroxide, specifically a kind of preparation method of laminated double hydroxide nanometer rod.
Background technology
Layered double-hydroxide (Layered Double Hydroxides, is abbreviated as LDH) is that a kind of typical anion type laminated compound is also called houghite stratified material, and its general formula is [M
2+ 1 xm
3+ x(OH)
2] [A
n]
x/nmH
2o, this material is made up of the laminate be parallel to each other, and is positioned at the divalent metal M on laminate
2+can by trivalent metal cation M that ionic radius is close in certain proportional range
3+isomorphous substitution, makes laminate band permanent positive charge; Interlayer has tradable negatively charged ion to maintain charge balance.At the different group of intercalation, many functional materialss can be prepared, shown wide application prospect in fields such as absorption, catalysis, medicine, electrochemistry, photochemistry, agricultural chemicals and military project materials by ion-exchange.Thus the preparation research of LDH material obtains and pays close attention to widely in recent years.
Monodimension nanometer material mainly contains nano wire, nanometer rod, nano belt, nanotube etc. make it have wide application prospect because it not only has the thermostability, mechanical property, optical property etc. that surface effects, quantum size effect and small-size effect etc. that usual nano material has also have its uniqueness.A lot of scholar utilizes Template synthesis such as threadiness, wire ((a) Li Bo. the preparation of anionic type laminated material hydrotalcite and crystal morphology control to study [D]. [master thesis]. Beijing: Beijing University of Chemical Technology, 2008. (b) Hongyu Wu, Qingze Jiao, Yun Zhao, Silu Huang, Xuefei Li, Hongbo Liu, Mingji Zhou.J. Materials Character zation, 61 (2010) 227 – 232.) etc. the layered hydroxide of different-shape, but it exists as structure during removing template such as easily to be caved at the problem.Rarely has the report of synthesis laminated double hydroxide nanometer rod.
Summary of the invention
For the above-mentioned defect existed in prior art, technical problem to be solved by this invention is to provide a kind of preparation method of laminated double hydroxide nanometer rod, and the preparation method of described this laminated double hydroxide nanometer rod will solve in laminated double hydroxide nanometer of the prior art rod preparation process structure when removing template and the technical problem such as easily cave in.
The preparation method of a kind of laminated double hydroxide nanometer rod of the present invention, take soluble salt and the trivalent metal soluble salt of divalent metal respectively, the soluble salt of described divalent metal and the mol ratio of trivalent metal soluble salt are 1-3:1, the soluble salt of divalent metal and the soluble salt of trivalent metal are dissolved in deionized water and are made into salts solution, take urea again, the mol ratio of described urea and the soluble salt of trivalent metal is 7:1-9:1, urea is dissolved in described salts solution and forms mixing solutions, mixing solutions is placed in tetrafluoroethylene reactor, 8-15 hour is reacted at 120-140 DEG C, form suspension liquid, after cooling, precipitate with deionized water wash, then suction filtration is dry obtains hexagon shape layered double-hydroxide powder, hexagon shape layered double-hydroxide powder is dissolved in alcohol liquid, supersound process 0.5-3 hour, then alcoholic solution pH to 1.5-3.5 is adjusted with nitric acid, continue suction filtration after supersound process 0.5-3 hour, dry powder, above-mentioned powder is dissolved in methane amide and namely obtains laminated double hydroxide nanometer rod after ultrasonic 0.5-3 hour.
Further, the pH of described salpeter solution is 1 ~ 3.
Further, described alcohol liquid is methyl alcohol or ethanol or Virahol or glycerol.
Further, described divalent ion is Mg
2+, or Zn
2+, or Mn
2+.
Further, described trivalent metal ion is Al
3+, or Fe
3+for in a kind of or combination of two kinds.
Further, the concentration that the soluble salt of described divalent metal and the soluble salt of trivalent metal are dissolved in the salts solution formed after in deionized water is 0.05 ~ 0.15mol/L.
The present invention compares with prior art, and its technical progress is significant.The invention has the advantages that and under there is no template condition, to have synthesized the larger laminated double hydroxide nanometer rod of aspect ratio, and the advantages such as this invention to have technique simple, easy to operate, easy control of structure.
Accompanying drawing explanation
Fig. 1 is the TEM figure of the laminated double hydroxide nanometer rod prepared by method of the present invention.
Embodiment
Embodiment 1:
(1) setting Mg/ (Al+Fe) mol ratio is 2, Al/Fe mol ratio is 3, and the mol ratio (R) of urea/(Al+Fe) is 7, raw materials weighing Mg(NO by a certain percentage
3)
26H
2o, Al(NO
3)
39 H
2o, Fe(NO
3)
39 H
2o is dissolved in deionized water and is made into 0.1mol/L salts solution, and the urea simultaneously taking respective quality according to R value is dissolved in this salts solution.Added by above-mentioned mixing solutions in tetrafluoroethylene reactor, setting temperature of reaction is 120 DEG C of reaction times is 12h, forms suspension liquid.After cooling, by deionized water wash precipitation, at 80 DEG C, dry suction filtration is dry obtains hexagon shape layered double-hydroxide powders A.
(2) appropriate powders A being dissolved in dehydrated alcohol after supersound process adjusts alcohol liquid to pH=2 with the salpeter solution of pH=2, continues ultrasonic rear suction filtration, dry powder B.
(3) a certain amount of powder B is dissolved in supersound process in methane amide and namely obtains flower-like nanometer rod.Nanometer rod is about 500nm, and diameter is about 100nm.
Embodiment 2:
(1) setting Zn/ (Al+Fe) mol ratio is 2, Al/Fe mol ratio is 3, and the mol ratio (R) of urea/(Al+Fe) is 9, raw materials weighing Zn(NO by a certain percentage
3)
26H
2o, Al(NO
3)
39 H
2o, Fe(NO
3)
39 H
2o is dissolved in deionized water and is made into 0.1mol/L salts solution, and the urea simultaneously taking respective quality according to R value is dissolved in this salts solution.Added by above-mentioned mixing solutions in tetrafluoroethylene reactor, setting temperature of reaction is 140 DEG C of reaction times is 12h, forms suspension liquid.After cooling, by deionized water wash precipitation, at 80 DEG C, dry suction filtration is dry obtains hexagon shape layered double-hydroxide powders A.
(2) appropriate powders A being dissolved in dehydrated alcohol after supersound process adjusts alcohol liquid to pH=2 with the salpeter solution of pH=1.5, continues ultrasonic rear suction filtration, dry powder B.
(3) a certain amount of powder B is dissolved in supersound process in methane amide and namely obtains flower-like nanometer rod.Nanometer rod is about 400nm, and diameter is about 50nm.
Embodiment 3:
(1) setting Mn/ (Al+Fe) mol ratio is 3, Al/Fe mol ratio is 3, and the mol ratio (R) of urea/(Al+Fe) is 8, raw materials weighing Mn(NO by a certain percentage
3)
26H
2o, Al(NO
3)
39 H
2o, Fe(NO
3)
39 H
2o is dissolved in deionized water and is made into 0.1mol/L salts solution, and the urea simultaneously taking respective quality according to R value is dissolved in this salts solution.Added by above-mentioned mixing solutions in tetrafluoroethylene reactor, setting temperature of reaction is 140 DEG C of reaction times is 12h, forms suspension liquid.After cooling, by deionized water wash precipitation, at 80 DEG C, dry suction filtration is dry obtains hexagon shape layered double-hydroxide powders A.
(2) appropriate powders A being dissolved in glycerol after supersound process adjusts alcohol liquid to pH=2 with the salpeter solution of pH=1, continues ultrasonic rear suction filtration, dry powder B.
(3) a certain amount of powder B is dissolved in supersound process in methane amide and namely obtains flower-like nanometer rod.Nanometer rod is about 550nm, wide about 120nm.
Embodiment 4:
(1) setting Mg/Al mol ratio is 2, and the mol ratio (R) of urea/Al is 7, raw materials weighing Mg(NO by a certain percentage
3)
26H
2o, Al(NO
3)
39 H
2o is dissolved in deionized water and is made into 0.1mol/L salts solution, and the urea simultaneously taking respective quality according to R value is dissolved in this salts solution.Added by above-mentioned mixing solutions in tetrafluoroethylene reactor, setting temperature of reaction is 140 DEG C of reaction times is 12h, forms suspension liquid.After cooling, by deionized water wash precipitation, at 80 DEG C, dry suction filtration is dry obtains hexagon shape layered double-hydroxide powders A.
(2) appropriate powders A being dissolved in dehydrated alcohol after supersound process adjusts alcohol liquid to pH=3 with the salpeter solution of pH=1.5, continues ultrasonic rear suction filtration, dry powder B.
(3) a certain amount of powder B is dissolved in supersound process in methane amide and namely obtains flower-like nanometer rod.Nanometer rod is about 350nm, wide about 50nm.
Embodiment 5:
(1) setting Zn/Al mol ratio is 3, and the mol ratio (R) of urea/Al is 8, raw materials weighing Mg(NO by a certain percentage
3)
26H
2o, Al(NO
3)
39 H
2o is dissolved in deionized water and is made into 0.1mol/L salts solution, and the urea simultaneously taking respective quality according to R value is dissolved in this salts solution.Added by above-mentioned mixing solutions in tetrafluoroethylene reactor, setting temperature of reaction is 120 DEG C of reaction times is 12h, forms suspension liquid.After cooling, by deionized water wash precipitation, at 80 DEG C, dry suction filtration is dry obtains hexagon shape layered double-hydroxide powders A.
(2) appropriate powders A being dissolved in dehydrated alcohol after supersound process adjusts alcohol liquid to pH=2.5 with the salpeter solution of pH=3, continues ultrasonic rear suction filtration, dry powder B.
(3) a certain amount of powder B is dissolved in supersound process in methane amide and namely obtains flower-like nanometer rod.Nanometer rod is about 500nm, wide about 150nm.
Claims (4)
1. the preparation method of a laminated double hydroxide nanometer rod, it is characterized in that: the soluble salt and the trivalent metal soluble salt that take divalent metal respectively, the soluble salt of described divalent metal and the mol ratio of trivalent metal soluble salt are 1-3:1, the soluble salt of divalent metal and the soluble salt of trivalent metal are dissolved in deionized water and are made into salts solution, take urea again, the mol ratio of described urea and the soluble salt of trivalent metal is 7:1-9:1, urea is dissolved in described salts solution and forms mixing solutions, mixing solutions is placed in tetrafluoroethylene reactor, 8-15 hour is reacted at 120-140 DEG C, form suspension liquid, after cooling, precipitate with deionized water wash, then suction filtration is dry obtains hexagon shape layered double-hydroxide powder, hexagon shape layered double-hydroxide powder is dissolved in alcohol liquid, supersound process 0.5-3 hour, then alcoholic solution pH to 1.5-3.5 is adjusted with nitric acid, continue suction filtration after supersound process 0.5-3 hour, dry powder, above-mentioned powder is dissolved in methane amide and namely obtains laminated double hydroxide nanometer rod after ultrasonic 0.5-3 hour.
2. the preparation method of a kind of laminated double hydroxide nanometer rod as claimed in claim 1, is characterized in that: described alcohol liquid is methyl alcohol or ethanol or Virahol or glycerin solution.
3. the preparation method of a kind of laminated double hydroxide nanometer rod as claimed in claim 1, is characterized in that: described divalent-metal ion is Mg
2+, or Zn
2+, or Mn
2+.
4. the preparation method of a kind of laminated double hydroxide nanometer rod as claimed in claim 1, is characterized in that: described trivalent metal ion is Al
3+, or Fe
3+for in a kind of or combination of two kinds.
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| CN201410543801.2A CN104310449B (en) | 2014-10-15 | 2014-10-15 | A kind of preparation method of laminated double hydroxide nanometer rod |
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| CN104310449B CN104310449B (en) | 2016-07-06 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109414686A (en) * | 2016-03-17 | 2019-03-01 | 沙特阿拉伯石油公司 | High aspect ratio layered double-hydroxide material and preparation method |
| CN109641761A (en) * | 2016-06-17 | 2019-04-16 | Scg化学有限公司 | Layered double-hydroxide |
| CN115155507A (en) * | 2022-07-07 | 2022-10-11 | 浙江大学 | Magnesium oxycarbonate-loaded green embroidery nanocomposite, preparation method and application thereof |
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2014
- 2014-10-15 CN CN201410543801.2A patent/CN104310449B/en not_active Expired - Fee Related
Patent Citations (6)
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Non-Patent Citations (4)
| Title |
|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109414686A (en) * | 2016-03-17 | 2019-03-01 | 沙特阿拉伯石油公司 | High aspect ratio layered double-hydroxide material and preparation method |
| CN109414686B (en) * | 2016-03-17 | 2021-09-28 | 沙特阿拉伯石油公司 | High aspect ratio layered double hydroxide materials and methods of making the same |
| CN109641761A (en) * | 2016-06-17 | 2019-04-16 | Scg化学有限公司 | Layered double-hydroxide |
| CN115155507A (en) * | 2022-07-07 | 2022-10-11 | 浙江大学 | Magnesium oxycarbonate-loaded green embroidery nanocomposite, preparation method and application thereof |
| CN115155507B (en) * | 2022-07-07 | 2023-07-07 | 浙江大学 | Magnesium oxide-loaded green embroidery nanocomposite, preparation method and application thereof |
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| CN104310449B (en) | 2016-07-06 |
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