CN104310449B - A kind of preparation method of laminated double hydroxide nanometer rod - Google Patents
A kind of preparation method of laminated double hydroxide nanometer rod Download PDFInfo
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Abstract
A kind of preparation method of laminated double hydroxide nanometer rod, weigh divalence and trivalent metal soluble-salt respectively, the mol ratio of divalence and trivalent metal soluble-salt is 1-3:1, the soluble-salt of divalence and trivalent metal is dissolved in deionized water and is made into salting liquid, weigh urea again, urea is 7:1-9:1 with the mol ratio of the soluble-salt of trivalent metal, urea is dissolved in salting liquid formation mixed solution, mixed solution is placed in reaction kettle for reaction, form suspension, cool down again, washing, precipitation, suction filtration, it is dried to obtain hexagon shape layered double-hydroxide powder, double-hydroxide powder is dissolved in alcohol liquid, ultrasonically treated, alcoholic solution pH is adjusted with nitric acid, continue ultrasonically treated rear suction filtration, it is dried to obtain powder, above-mentioned powder is dissolved in ultrasonic in formamide after i.e. obtain laminated double hydroxide nanometer rod.The present invention has synthesized the laminated double hydroxide nanometer rod that draw ratio is bigger under the conditions of not having template, and technique is simple, easy to operate, easy control of structure.
Description
Technical field
The invention belongs to chemical field, particularly relate to a kind of layered double-hydroxide, the specifically double hydrogen of a kind of stratiform
The preparation method of oxide nano-rod.
Background technology
Layered double-hydroxide (Layered Double Hydroxides, be abbreviated as LDH) be a kind of typical cloudy from
Subtype lamellar compound is also called houghite stratified material, and its formula is [M2+ 1−xM3+ x (OH) 2][An−] x/n·mH2O, this
Plant material to be made up of the laminate being parallel to each other, the divalent metal M being positioned on laminate2+Can be at certain proportion
The interior trivalent metal cation M close by ionic radius3+Same order elements so that laminate band permanent positive charge；Interlayer has can be handed over
The anion changed is to maintain charge balance.Can be at the different group of intercalation by ion exchange, the many functional materials of preparation,
Wide application prospect has been shown in fields such as absorption, catalysis, medicine, electrochemistry, photochemistry, agricultural chemicals and military project materials.Cause
And the preparation research of LDH material has obtained paying close attention to widely in recent years.
Monodimension nanometer material mainly has nano wire, nanometer rods, and nanobelt, nanotube etc. not only have usual nanometer due to it
Skin effect, quantum size effect and small-size effect etc. that material is had also have the heat endurance of its uniqueness, mechanicalness
Energy, optical property etc. make it have wide application prospect.A lot of scholars utilize Template synthesis such as threadiness, wire ((a)
Li Bo. the preparation of anionic type laminated material hydrotalcite controls research [D] with crystal morphology. [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.) layered hydroxide of different-shape such as, but it exists as when removing template, structure such as is easily caved at the problem.Rarely has synthesis
The report of laminated double hydroxide nanometer rod.
Summary of the invention
For drawbacks described above present in prior art, it is double that the technical problem to be solved is to provide a kind of stratiform
The preparation method of hydroxide nanorod, the preparation method of described this laminated double hydroxide nanometer rod to solve existing skill
When removing template in the laminated double hydroxide nanometer rod preparation process in art, structure such as is easily caved at the technical problem.
A kind of laminated double hydroxide nanometer of the present invention rod preparation method, weigh respectively divalent metal soluble-salt and
Trivalent metal soluble-salt, the soluble-salt of described divalent metal and the mol ratio of trivalent metal soluble-salt are 1-3:1, will
The soluble-salt of divalent metal and the soluble-salt of trivalent metal are dissolved in deionized water and are made into salting liquid, then weigh urea,
Described urea is 7:1-9:1 with the mol ratio of the soluble-salt of trivalent metal, and urea is dissolved in described salting liquid formation
Mixed solution, is placed in mixed solution in polytetrafluoroethylene (PTFE) reactor, reacts 8-15 hour, formed suspended at 120-140 DEG C
Liquid, after cooling, is washed with deionized precipitation, and then suction filtration is dried to obtain hexagon shape layered double-hydroxide powder, by six limits
Shape layered double-hydroxide powder is dissolved in alcohol liquid, ultrasonically treated 0.5-3 hour, then adjusts alcoholic solution pH to 1.5-with nitric acid
3.5, suction filtration after continuing ultrasonically treated 0.5-3 hour, it is dried and to obtain powder, above-mentioned powder is dissolved in ultrasonic 0.5-3 in formamide
Laminated double hydroxide nanometer rod is i.e. obtained after hour.
Further, the pH of described salpeter solution is 1 ~ 3.
Further, described alcohol liquid is methyl alcohol or ethanol or isopropanol or glycerine.
Further, described divalent ion is Mg2+, or Zn2+, or Mn2+。
Further, described trivalent metal ion is Al3+, or Fe3+The combination of the one or two kinds of in for.
Further, the soluble-salt of described divalent metal and the soluble-salt of trivalent metal are dissolved in deionized water
The concentration of the salting liquid of rear formation is 0.05 ~ 0.15mol/L.
The present invention compares with prior art, and its technological progress is significant.It is an advantage of the current invention that there is no template condition
Lower synthesized the laminated double hydroxide nanometer rod that aspect ratio is bigger, and this invention to have technique simple, easy to operate, structure
The advantage such as easily-controllable.
Accompanying drawing explanation
Fig. 1 is the TEM figure of the laminated double hydroxide nanometer rod that the method by the present invention prepares.
Detailed description of the invention
Embodiment 1:
(1) setting Mg/ (Al+Fe) mol ratio as 2, Al/Fe mol ratio is 3, and the mol ratio (R) of urea/(Al+Fe) is 7,
Weigh raw material Mg(NO by a certain percentage3)2·6H2O, Al(NO3)3·9 H2O, Fe(NO3)3·9 H2O is dissolved in deionized water and is made into
0.1mol/L salting liquid, simultaneously weighs the urea of respective quality according to R value and is dissolved in this salting liquid.Above-mentioned mixed solution is added poly-
In tetrafluoroethene reactor, set reaction temperature as 120 DEG C of reaction time as 12h, formation suspension.After cooling, spend from
Sub-water washing precipitation, be dried at 80 DEG C suction filtration hexagon shape layered double-hydroxide powders A.
(2) salpeter solution that appropriate powders A is dissolved in ultrasonically treated rear pH=2 in absolute ethyl alcohol adjusts alcohol liquid to pH=2, continues
Continuous ultrasonic rear suction filtration, it is dried and to obtain powder B.
(3) a certain amount of powder B is dissolved in formamide ultrasonically treated i.e. obtain flower-like nanometer rod.Nanometer rods is about 500nm,
Diameter about 100nm.
Embodiment 2:
(1) setting Zn/ (Al+Fe) mol ratio as 2, Al/Fe mol ratio is 3, and the mol ratio (R) of urea/(Al+Fe) is 9,
Weigh raw material Zn(NO by a certain percentage3)2·6H2O, Al(NO3)3·9 H2O, Fe(NO3)3·9 H2O is dissolved in deionized water and is made into
0.1mol/L salting liquid, simultaneously weighs the urea of respective quality according to R value and is dissolved in this salting liquid.Above-mentioned mixed solution is added poly-
In tetrafluoroethene reactor, set reaction temperature as 140 DEG C of reaction time as 12h, formation suspension.After cooling, spend from
Sub-water washing precipitation, be dried at 80 DEG C suction filtration hexagon shape layered double-hydroxide powders A.
(2) appropriate powders A is dissolved in ultrasonically treated rear pH=1.5 in absolute ethyl alcohol salpeter solution adjust alcohol liquid to pH=2,
Continue ultrasonic rear suction filtration, be dried to obtain powder B.
(3) a certain amount of powder B is dissolved in formamide ultrasonically treated i.e. obtain flower-like nanometer rod.Nanometer rods is about 400nm,
Diameter about 50nm.
Embodiment 3:
(1) setting Mn/ (Al+Fe) mol ratio as 3, Al/Fe mol ratio is 3, and the mol ratio (R) of urea/(Al+Fe) is 8,
Weigh raw material Mn(NO by a certain percentage3)2·6H2O, Al(NO3)3·9 H2O, Fe(NO3)3·9 H2O is dissolved in deionized water and is made into
0.1mol/L salting liquid, simultaneously weighs the urea of respective quality according to R value and is dissolved in this salting liquid.Above-mentioned mixed solution is added poly-
In tetrafluoroethene reactor, set reaction temperature as 140 DEG C of reaction time as 12h, formation suspension.After cooling, spend from
Sub-water washing precipitation, be dried at 80 DEG C suction filtration hexagon shape layered double-hydroxide powders A.
(2) salpeter solution that appropriate powders A is dissolved in ultrasonically treated rear pH=1 in glycerine adjusts alcohol liquid to pH=2, continues
Ultrasonic rear suction filtration, be dried to obtain powder B.
(3) a certain amount of powder B is dissolved in formamide ultrasonically treated i.e. obtain flower-like nanometer rod.Nanometer rods is about 550nm,
Width about 120nm.
Embodiment 4:
(1) setting Mg/Al mol ratio as 2, the mol ratio (R) of urea/Al is 7, weighs raw material Mg by a certain percentage
(NO3)2·6H2O, Al(NO3)3·9 H2O is dissolved in deionized water and is made into 0.1mol/L salting liquid, weighs accordingly according to R value simultaneously
The urea of quality is dissolved in this salting liquid.Above-mentioned mixed solution is added in polytetrafluoroethylene (PTFE) reactor, sets reaction temperature as 140
DEG C reaction time is 12h, forms suspension.After cooling, it is washed with deionized precipitation, at 80 DEG C, is dried suction filtration
Hexagon shape layered double-hydroxide powders A.
(2) appropriate powders A is dissolved in ultrasonically treated rear pH=1.5 in absolute ethyl alcohol salpeter solution adjust alcohol liquid to pH=3,
Continue ultrasonic rear suction filtration, be dried to obtain powder B.
(3) a certain amount of powder B is dissolved in formamide ultrasonically treated i.e. obtain flower-like nanometer rod.Nanometer rods is about 350nm,
Width about 50nm.
Embodiment 5:
(1) setting Zn/Al mol ratio as 3, the mol ratio (R) of urea/Al is 8, weighs raw material Mg by a certain percentage
(NO3)2·6H2O, Al(NO3)3·9 H2O is dissolved in deionized water and is made into 0.1mol/L salting liquid, weighs accordingly according to R value simultaneously
The urea of quality is dissolved in this salting liquid.Above-mentioned mixed solution is added in polytetrafluoroethylene (PTFE) reactor, sets reaction temperature as 120
DEG C reaction time is 12h, forms suspension.After cooling, it is washed with deionized precipitation, at 80 DEG C, is dried suction filtration
Hexagon shape layered double-hydroxide powders A.
(2) appropriate powders A is dissolved in ultrasonically treated rear pH=3 in absolute ethyl alcohol salpeter solution adjust alcohol liquid to pH=2.5,
Continue ultrasonic rear suction filtration, be dried to obtain powder B.
(3) a certain amount of powder B is dissolved in formamide ultrasonically treated i.e. obtain flower-like nanometer rod.Nanometer rods is about 500nm,
Width about 150nm.
Claims (4)
1. the preparation method of a laminated double hydroxide nanometer rod, it is characterised in that: weigh the solubility of divalent metal respectively
Salt and trivalent metal soluble-salt, 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 salting liquid, then weigh urine
Element, described urea is 7:1-9:1 with the mol ratio of the soluble-salt of trivalent metal, and urea is dissolved in shape in described salting liquid
Become mixed solution, mixed solution is placed in polytetrafluoroethylene (PTFE) reactor, react 8-15 hour at 120-140 DEG C, formed outstanding
Turbid liquid, after cooling, is washed with deionized precipitation, and then suction filtration is dried to obtain hexagon shape layered double-hydroxide powder, by six
Limit shape layered double-hydroxide powder is dissolved in alcohol liquid, ultrasonically treated 0.5-3 hour, then adjusts alcoholic solution pH extremely with nitric acid
1.5-3.5, suction filtration after continuing ultrasonically treated 0.5-3 hour, is dried and to obtain powder, is dissolved in formamide ultrasonic by above-mentioned powder
Layered double-hydroxide flower-like nanometer rod is i.e. obtained after 0.5-3 hour.
The preparation method of a kind of laminated double hydroxide nanometer the most as claimed in claim 1 rod, it is characterised in that: described alcohol liquid
For methyl alcohol or ethanol or isopropanol or glycerin solution.
The preparation method of a kind of laminated double hydroxide nanometer the most as claimed in claim 1 rod, it is characterised in that: described two
Valence metal ion is Mg2+, or Zn2+, or Mn2 +。
The preparation method of a kind of laminated double hydroxide nanometer the most as claimed in claim 1 rod, it is characterised in that: described trivalent
Metal ion is Al3+, or Fe3+In the combination of one or two kinds of.
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| US10138199B2 (en) * | 2016-03-17 | 2018-11-27 | Saudi Arabian Oil Company | High aspect ratio layered double hydroxide materials and methods for preparation thereof |
| GB201610663D0 (en) * | 2016-06-17 | 2016-08-03 | Scg Chemicals Co Ltd | Layered double hydroxides |
| 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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| CN101318687A (en) * | 2008-06-06 | 2008-12-10 | 北京化工大学 | Method for preparing micrometre level flocculus shaped layered bi-metal hydroxide |
| WO2012150460A1 (en) * | 2011-05-04 | 2012-11-08 | Isis Innovation Limited | Method for the preparation of layered double hydroxides |
| CN103274437A (en) * | 2013-06-21 | 2013-09-04 | 北京化工大学 | Three-dimensional flower-like layered double hydroxide and preparation method thereof |
| JP2013212937A (en) * | 2012-03-30 | 2013-10-17 | Kao Corp | Method for producing layered double hydroxide |
| CN103552988A (en) * | 2013-09-30 | 2014-02-05 | 东南大学 | Layered double hydroxide based composite material with fiber hierarchical structure and preparation method thereof |
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2014
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Patent Citations (6)
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|---|---|---|---|---|
| CN101318687A (en) * | 2008-06-06 | 2008-12-10 | 北京化工大学 | Method for preparing micrometre level flocculus shaped layered bi-metal hydroxide |
| WO2012150460A1 (en) * | 2011-05-04 | 2012-11-08 | Isis Innovation Limited | Method for the preparation of layered double hydroxides |
| JP2013212937A (en) * | 2012-03-30 | 2013-10-17 | Kao Corp | Method for producing layered double hydroxide |
| CN103964391A (en) * | 2013-01-28 | 2014-08-06 | 北京化工大学 | Flaky structure layered composite hydroxide and preparation method thereof |
| CN103274437A (en) * | 2013-06-21 | 2013-09-04 | 北京化工大学 | Three-dimensional flower-like layered double hydroxide and preparation method thereof |
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