CN102730646A - Preparation method of layered double-hydroxide nanobelt - Google Patents
Preparation method of layered double-hydroxide nanobelt Download PDFInfo
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- CN102730646A CN102730646A CN2012101791862A CN201210179186A CN102730646A CN 102730646 A CN102730646 A CN 102730646A CN 2012101791862 A CN2012101791862 A CN 2012101791862A CN 201210179186 A CN201210179186 A CN 201210179186A CN 102730646 A CN102730646 A CN 102730646A
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Abstract
The invention relates to a preparation method of a layered double-hydroxide nanobelt. The method comprises the following steps: mixing divalent ions Mg<2+>, Zn<2+>, Ni<2+>, Mn<2+> and Cu<2+> with trivalent metal ions Al<3+>, Fe<3+> and Cr<3+> according to ratio of 1:1-3:1 to prepare a solution A, mixing and dissolving sodium hydroxide or potassium hydroxide and sodium carbonate or potassium carbonate according to a ratio of hydroxide ions to carbonate ions of 1:1-3:1 to prepare a solution B, rapidly mixing the solution A with the solution B with the molar concentration ratio of a divalent metal salt solution to a strong alkaline solution being 1:1-1:3 at 10-50DEG C, and continuously stirring at 10-50DEG C for 0.5-4h; ageing at 50-150DEG C for 8-72h; and washing the resulting products with deionized water, and drying or directly dispersing in ethanol to obtain the one-dimensional layered double-hydroxide nanobelt. The preparation method has an advantage that the one-dimensional nanobelt with a large aspect ratio is synthesized through using a mild method without templates and surfactants. The preparation method has the characteristics of simple process, convenient operation, easily control structure and the like.
Description
Technical field
The present invention relates to the preparation method of layered double-hydroxide, particularly a kind of preparation method of laminated double hydroxide nanometer band.
Background technology
Monodimension nanometer material mainly comprises nano wire, nanometer rod, nano belt, nanotube, nano-cable etc.; Because it not only has surface effects, quantum size effect and the small-size effect etc. that common nano material has; Also have its unique thermostability, mechanical property, electric transmission and photon transmission property, optical property, photoconduction and field emission effect etc., it is with a wide range of applications.Nano belt is as a kind of typical monodimension nanometer material, and all existing relevant report ((a) Pan, Z. W. are synthesized in the success of oxide compound, sulfide and simple substance nano belt that some homogeneity are good; Dai, Z. R.; Wang, Z. L.
Science 2001,
291, 1947 – 1949. (b) Kim, F.; Song, J. H.; Yang, P. D.
J. Am. Chem. Soc. 2002,
124, 14316 – 14317. (c) Nakayama, Y.; Pauzauskie, P. J.; Radenovic, A.; Onorato, R. M.; Saykally, R. J.; Liphardt, J.; Yang, P. D.
Nature 2007,
447, 1098 – 1101.).), but rarely have bibliographical information about one dimension laminated double hydroxide nanometer band.
Layered double-hydroxide and natural hydrotalcite have similar structures, and its general structure is [M (II)
1 xM (III)
x(OH)
2]
X+[A
n]
X/n, wherein M (II) refers to that divalent metal M (III) refers to trivalent metal cation A
nBut be the negatively charged ion of stable existence in the basic soln, this structure is by M (OH)
6Octahedra shared prismatic becomes unit layer, and part M (II) is substituted by M (III) and produces positive polarity, and comes balance by interlayer anion, and layer component has variety in the layered double-hydroxide, can hold multiple positively charged ion such as Mg
2+, Ni
2+, Co
2+, Zn
2+, Cu
2+And Al
3+, Cr
3+, Fe
3+, Sc
3+, Ga
3+Deng.The negatively charged ion that is between the layered double-hydroxide structural sheet can be by other anionresin, thereby have excellent anionresin performance.Can regulation and control in a big way, particular structural and character and have a wide range of applications just because of the composition of layered double-hydroxide.And the research of laminated double hydroxide nanometer structured material has also attracted lot of domestic and foreign scholar's concern.A lot of scholars utilize the template or the method for tensio-active agent to synthesize such as ring-type, tubulose, flower-shaped ((a) Yang, M. S.; Liu, J. F.; Chang, Z.; Williams, G. R.; O ' Hare, D.; Zheng, X. H.; Sun, X.M. Duan, X.
J. Mater. Chem. 2011,
21, 14741-14746. (b) Zhao, Y.; Xiao, F. F.; Jiao, Q. Z.
Journalof Nanotechnology 2011, 646409. (c) Xiao, T. Tang, Y. W.; Jia, Z. Y.; Li, D. W.; Hu, X.Y.; Li, B.H.; Luo, L. J.
Nanotechnology,
2009,
20, 475603.) etc. the layered double-hydroxide of different-shape, but in the last handling process of preparation, problem such as can cause that structure is caved in when removing template and the tensio-active agent wash-out is not clean.
Summary of the invention
The objective of the invention is to overcome the problem that exists in the prior art, provide a kind of under gentle relatively condition, the method for the laminated double hydroxide nanometer band that the preparation aspect ratio is bigger under the situation of no template and tensio-active agent.
For achieving the above object, the present invention adopts following technical scheme:
A kind of preparation method of laminated double hydroxide nanometer band is characterized in that the concrete steps of this method are:
A, the soluble salt of divalence and trivalent metal is dissolved in the deionized water, divalence and trivalent metal ion mol ratio are 1:1 ~ 3:1, obtain solution A;
B, highly basic and carbonate is dissolved in is mixed with mixed ammonium/alkali solutions in the deionized water; Described highly basic is a kind of in sodium hydroxide or the Pottasium Hydroxide, and carbonate is a kind of in yellow soda ash or the salt of wormwood, and the mol ratio of hydroxide ion and carbanion is 1:1 ~ 3:1, obtains solution B;
C, under 10 ~ 50 ° of C temperature condition, step a gained solution A and step b gained solution B are mixed rapidly, divalent metal soluble salt and alkaline mol ratio are 1:1 ~ 1:3, stirring reaction 0.5 ~ 4h; At 50 ~ 150 ° of C ageing 8h ~ 72h; Product with gained filters with deionized water wash at last, and is dry or directly be dispersed in and just can obtain unidimensional laminated double hydroxide nanometer band in the alcohol.
Above-mentioned divalent ion is Mg
2+, Zn
2+, Ni
2+, Mn
2+Or Cu
2+Described trivalent ion is Al
3+, Fe
3+Or Cr
3+Described soluble salt is muriate, vitriol or nitrate salt.
The length of the one dimension laminated double hydroxide nanometer band of gained of the present invention is 500 ~ 2000nm, and width is 50 ~ 150nm.Digestion time and ageing temperature have fundamental influence to the formation of one dimension laminated double hydroxide nanometer band in the inventive method, and time and temperature control are the keys that obtains one dimension layered hydroxide nano belt.
Advantage of the present invention is to utilize comparatively gentle method, under the condition that does not have template and tensio-active agent, and the 1-dimention nano band that the synthetic aspect ratio is bigger.And characteristics such as technology is simple, easy to operate, easy control of structure that this invention has.And the cost of material material benefit, can be widely used in each association area.
Description of drawings
Fig. 1 is the XRD spectra of the embodiment of the invention one gained sample
Fig. 2 is the embodiment of the invention one gained sample transmission electron microscope (TEM) photo.
Embodiment
After specific embodiment of the present invention being described at present.
Embodiment one:A certain amount of MgCl
2And AlCl
3(Mg
2+/ Al
3+Mol ratio=2/1) is dissolved in the 30mL deionized water, is designated as solution A.Then with a certain amount of NaOH and Na
2CO
3(OH
-/ CO
3 2-=2/1) is dissolved in the deionized water of other a 30mL, is designated as solution B.Next solution A, B are added in the middle of the three-necked bottle together; The divalent metal salts solution is 1:2 with the ratio of the volumetric molar concentration of strong base solution; Under 10 ° of C, stir 60 min; Then mixed turbid liquid is shifted into autoclave, putting into temperature is the baking oven ageing 8h of 50 ° of C, can obtain the zonal whisker of high aspect ratio nano.At last the product that obtains is dispersed in to be tested and application in the absolute ethyl alcohol.Sample can know that through XRD analysis the nano belt that obtains is purified, and well-crystallized's layered double-hydroxide is shown in accompanying drawing 1.The length of nano belt is 600 ~ 800nm, and width is 50 ~ 80nm, shown in accompanying drawing 2.
Embodiment two:A certain amount of ZnCl
2And AlCl
3(Zn
2+/ Al
3+Mol ratio=3/1) is dissolved in the 30mL deionized water, is designated as solution A.Then with a certain amount of KOH and K
2CO
3(OH
-/ CO
3 2-=3/1) is dissolved in the deionized water of other a 30mL, is designated as solution B.Next solution A, B are added in the middle of the three-necked bottle together; The divalent metal salts solution is 1:1 with the ratio of the volumetric molar concentration of strong base solution; Under 20 ° of C, stir 40 min, then mixed turbid liquid is shifted into autoclave, putting into temperature is the baking oven ageing 18h of 90 ° of C.At last with the to be tested and application of product washing, oven dry that obtains.Sample can know that through XRD analysis the nano belt that obtains is purified, well-crystallized's layered double-hydroxide.The length of nano belt is 800 ~ 1000nm, and width is 80 ~ 100nm.
Embodiment three:A certain amount of Mg (SO
4)
2And Al
2(SO
4)
3(Mg
2+/ Al
3+Mol ratio=1/1) is dissolved in the 50mL deionized water, is designated as solution A.Then with a certain amount of NaOH and Na
2CO
3(OH
-/ CO
3 2-=2/1) is dissolved in the deionized water of other a 10mL, is designated as solution B.Next solution A, B are added in the middle of the three-necked bottle together; The divalent metal salts solution is 1:2 with the ratio of the volumetric molar concentration of strong base solution; Under 30 ° of C, stir 120 min, then mixed turbid liquid is shifted into autoclave, putting into temperature is the baking oven ageing 48h of 150 ° of C.At last the product that obtains is dispersed in to be tested and application in the absolute ethyl alcohol.Sample can know that through XRD analysis the nano belt that obtains is purified, well-crystallized's layered double-hydroxide.The length of nano belt is 500 ~ 600nm, and width is 90 ~ 120nm.
Embodiment four:A certain amount of Ni (NO
3)
2And Fe (NO
3)
3(Ni
2+/ Fe
3+Mol ratio=3/1) is dissolved in the 40mL deionized water, is designated as solution A.Then with a certain amount of KOH and K
2CO
3(OH
-/ CO
3 2-=1/1) is dissolved in the deionized water of other a 20mL, is designated as solution B.Next solution A, B are added in the middle of the three-necked bottle together; The divalent metal salts solution is 1:3 with the ratio of the volumetric molar concentration of strong base solution; Under 50 ° of C, stir 4h; Then mixed turbid liquid is shifted into autoclave, putting into temperature is the baking oven ageing 72h of 120 ° of C, at last with the to be tested and application of product washing, oven dry that obtains.Sample can know that through XRD analysis the nano belt that obtains is purified, well-crystallized's layered double-hydroxide.The length of nano belt is 1200 ~ 1500nm, and width is 120 ~ 150nm.
Claims (2)
1. the preparation method of a laminated double hydroxide nanometer band is characterized in that the concrete steps of this method are:
A, the soluble salt of divalence and trivalent metal is dissolved in the deionized water, divalence and trivalent metal ion mol ratio are 1:1 ~ 3:1, obtain solution A;
B, highly basic and carbonate is dissolved in is mixed with mixed ammonium/alkali solutions in the deionized water; Described highly basic is a kind of in sodium hydroxide or the Pottasium Hydroxide, and carbonate is a kind of in yellow soda ash or the salt of wormwood, and the mol ratio of hydroxide ion and carbanion is 1:1 ~ 3:1, obtains solution B;
C, under 10 ~ 50 ° of C temperature condition, step a gained solution A and step b gained solution B are mixed rapidly, divalent metal soluble salt and alkaline mol ratio are 1:1 ~ 1:3, stirring reaction 0.5 ~ 4h; At 50 ~ 150 ° of C ageing 8h ~ 72h; Product with gained filters with deionized water wash at last, and is dry or directly be dispersed in and just can obtain unidimensional laminated double hydroxide nanometer band in the alcohol.
2. the preparation method of laminated double hydroxide nanometer band according to claim 1 is characterized in that described divalent ion is Mg
2+, Zn
2+, Ni
2+, Mn
2+Or Cu
2+Described trivalent ion is Al
3+, Fe
3+Or Cr
3+Described soluble salt is muriate, vitriol or nitrate salt.
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Cited By (2)
| 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 |
| CN110436532A (en) * | 2019-07-16 | 2019-11-12 | 河北工业大学 | A kind of laminated double hydroxide nanometer material, preparation method and applications |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101516781A (en) * | 2006-09-21 | 2009-08-26 | 阿克佐诺贝尔股份有限公司 | Process for preparing layered double hydroxide comprising carbonate |
| CN102180614A (en) * | 2011-03-21 | 2011-09-14 | 北京化工大学 | Magnelium base layer-shaped double-hydroxide ultraviolet barrier material used in anti-aging asphalt |
-
2012
- 2012-06-04 CN CN2012101791862A patent/CN102730646A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101516781A (en) * | 2006-09-21 | 2009-08-26 | 阿克佐诺贝尔股份有限公司 | Process for preparing layered double hydroxide comprising carbonate |
| CN102180614A (en) * | 2011-03-21 | 2011-09-14 | 北京化工大学 | Magnelium base layer-shaped double-hydroxide ultraviolet barrier material used in anti-aging asphalt |
Non-Patent Citations (2)
| Title |
|---|
| JAE-MIN OH ET AL.: "The effect of synthetic conditions on tailoring the size of hydrotalcite particles", 《SOLID STATE INOICS 151》 * |
| 曹楠: "层状双金属氢氧化物及其衍生复合氧化物制备及吸附效能的研究", <中国优秀硕士学位论文全文数据库> * |
Cited By (4)
| 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 |
| CN110436532A (en) * | 2019-07-16 | 2019-11-12 | 河北工业大学 | A kind of laminated double hydroxide nanometer material, preparation method and applications |
| CN110436532B (en) * | 2019-07-16 | 2023-11-28 | 河北工业大学 | Layered double hydroxide nano material, preparation method and application thereof |
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Application publication date: 20121017 |