CN102897844A - Method for preparing hydrotalcite microspheres with multilevel structures under guide of surfactant - Google Patents
Method for preparing hydrotalcite microspheres with multilevel structures under guide of surfactant Download PDFInfo
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Abstract
The invention discloses a method for preparing hydrotalcite microspheres with multilevel structures under guide of surfactant and belongs to the field of synthesis of inorganic nano materials. The method for preparing the hydrotalcite microspheres with the multilevel structures has the advantages of: performing hydrothermal reaction on divalent and trivalent metal salt solutions which are used as raw materials under alkaline environment in an ethylene glycol solution by taking the surfactant as a guiding agent to obtain the hydrotalcite nano microspheres. By adjusting the content of the surfactant, the solid structures of the hydrotalcite microspheres are changed from yolk-type structures to hollow structures. The prepared hydrotalcite microspheres are magnetic, and the internal microstructures of the hydrotalcite microspheres can be adjusted; and the method for preparing hydrotalcite materials and the application field of the method are expanded, and the obtained microspheres with the multilevel structures have the important application prospect in the aspects of medicine targeting delivery, high-performance catalytic carrier materials and the like. The nano microspheres with the adjustable internal structures have the important application value in the fields of adsorption separation, catalysis and the like.
Description
Technical field
The invention belongs to the synthetic field of inorganic nano material, particularly the lower method for preparing the Multilevel-structure hydrotalcite microballoon of a kind of tensio-active agent guiding.
Background technology
The preparation of multilevel hierarchy micro-sphere material and application are one of the study hotspot of current physics, chemistry and Material Field and emphasis.Microballoon preparation and Functionalization that research and probe is new are brought into play its constructional feature, and excavating its using value becomes focus and the main direction of studying that people pay close attention to.According to its geometry, people have designed several different methods and have prepared the multilevel hierarchy micro-sphere material, and template duplicating method, microemulsion method, template-interfacial reaction method, spray method and supersonic method etc. are arranged.As by the standby inorganicss such as Si, Al, Ti, metal and oxide compound and sulfide, macromole or the high molecular polymer etc. of obtaining of template duplicating legal system.The assembling of nano particle and mesoporous material not only makes many characteristics of nano particle be not fully exerted, but also has produced nano particle and the not available special property of mesoporous material itself.In addition, this approach also becomes people's design, synthetic novel material, realizes the effective ways of performance regulation and control, as: can realize the position of optical absorption edge and absorption band is significantly regulated by yardstick, condition of surface, the inner structural features of control nanoparticle, thereby obtain New Type of Mesoporous complex body functional materials.Therefore, the in recent years research of mesoporous material has become the study hotspot of chemistry, physics, material subject, has cultivated new vegetative point for multidisciplinary intersection simultaneously.
It is a kind of typical anionic type laminated material that LDHs is called again hydrotalcite (Layered Double Hydroxides is abbreviated as LDHs), and it is adjustable that it has the laminate metallic element, and interlayer object anion species the is adjustable structural advantage of Denging.In recent years, hydrotalcite-like material has been realized industrial application in fields such as fire-retardant, anti-ultraviolet aging, fractionation by adsorption.But the hydrotalcite that traditional synthetic method for preparing hydrotalcite obtains exists easily and assembles, the deficiencies such as microtexture lack of alignment, and this has limited its functional giving full play to greatly.The controlled preparation that realizes the hydrotalcite microballoon not only can realize the taking full advantage of of hydrotalcite self property, and can bring into play its special constructional feature.The present invention is to the Development of Novel functional materials and realize that taking full advantage of of material property has great importance.
Summary of the invention
The purpose of this invention is to provide the lower method for preparing the Multilevel-structure hydrotalcite microballoon of a kind of tensio-active agent guiding.
Technical scheme of the present invention is: in ethylene glycol solution, take tensio-active agent as directed agents, take divalence, trivalent metal salts solution as raw material, carry out the Nano microsphere that hydro-thermal reaction obtains hydrotalcite under alkaline environment.Wherein, the content by the modulation tensio-active agent realize the hydrotalcite microballoon by solid construction to yolk formula structure again to the modulation of hollow structure.
Tensio-active agent of the present invention guiding is lower, and to prepare the concrete steps of method of Multilevel-structure hydrotalcite microballoon as follows:
The divalent metal nitrate of 0.1-0.4g, the trivalent iron salt of 0.1-0.5g and the tensio-active agent of 0.2-1.0g are added in the ethylene glycol of 10-30ml, stir, be designated as A solution; The sodium hydroxide of 0.1-0.2g is joined in the ethylene glycol of 10-30ml, stir, be designated as B solution; B solution poured in the A solution stir, then at 120-160 ℃ of lower crystallization 12-24 hour, use the dehydrated alcohol centrifuge washing, 50-80 ℃ dry 6-12 hour, obtain finely dispersed hydrotalcite microballoon.
Described divalent metal nitrate is selected from Mg (NO
3)
2, Co (NO
3)
2, Ni (NO
3)
2In a kind of.
Described trivalent iron salt is FeCl
3, Fe (NO
3)
3, Fe
2(SO
4)
3In a kind of.
Described tensio-active agent is cetyl trimethylammonium bromide, Sodium dodecylbenzene sulfonate or sodium cetanesulfonate.
When above-mentioned tensio-active agent add-on was 0.2-0.4g, the hydrotalcite microballoon that obtains was solid construction.
When above-mentioned tensio-active agent add-on was 0.5-0.7g, the hydrotalcite microballoon that obtains was yolk formula structure.
When above-mentioned tensio-active agent add-on was 0.8-1.0g, the hydrotalcite microballoon that obtains was hollow structure.
The present invention has realized the preparation of the magnetic hydrotalcite microballoon that internal structure is adjustable first, the hydrotalcite microballoon that obtains has magnetic and internal microstructure is adjustable, the present invention has expanded preparation method and the Application Areas of hydrotalcite-like material, and the multilevel hierarchy microballoon that obtains has important application prospect at aspects such as drug targeting transportation, high-performance catalytic carrier materials.The Nano microsphere that this internal structure is adjustable has important using value in fields such as fractionation by adsorption, catalysis.
Description of drawings
Fig. 1 is the projection electromicroscopic photograph of the Multilevel-structure hydrotalcite microballoon that obtains of the embodiment of the invention 1.
Fig. 2 is the stereoscan photograph of the Multilevel-structure hydrotalcite microballoon that obtains of the embodiment of the invention 1.
Fig. 3 is the XRD spectra of the Multilevel-structure hydrotalcite microballoon that obtains of the embodiment of the invention 1; X-coordinate is 2 θ, unit: degree; Ordinate zou is intensity.
Fig. 4 is the infrared spectrum of the Multilevel-structure hydrotalcite microballoon that obtains of example 1 of the present invention; X-coordinate is wave number, unit: cm
-1Ordinate zou is transmitance.
Embodiment
[embodiment 1]
1). the preparation of solid MgFe hydrotalcite microballoon:
The magnesium nitrate of 0.396g, the iron trichloride of 0.18g and the sodium laurylsulfonate of 0.3g are added in the ethylene glycol of 10ml, stir, be designated as A solution; The sodium hydroxide of 0.16g is joined in the ethylene glycol of 10ml, stir, be designated as B solution; B solution poured in the A solution stir, then 160 ℃ of lower crystallization 24 hours, use the dehydrated alcohol centrifuge washing, 60 ℃ of dryings 10 hours obtain finely dispersed core-shell type hydrotalcite microballoon.
2). the preparation of yolk formula MgFe hydrotalcite microballoon:
The magnesium nitrate of 0.396g, the iron trichloride of 0.18g and the sodium laurylsulfonate of 0.6g are added in the ethylene glycol of 10ml, stir, be designated as A solution; The sodium hydroxide of 0.16g is joined in the ethylene glycol of 10ml, stir, be designated as B solution; B solution poured in the A solution stir, then 160 ℃ of lower crystallization 24 hours, use the dehydrated alcohol centrifuge washing, 60 ℃ of dryings 10 hours obtain finely dispersed yolk formula hydrotalcite microballoon.
3). the preparation of open core type MgFe hydrotalcite microballoon:
The magnesium nitrate of 0.396g, the iron trichloride of 0.18g and the sodium laurylsulfonate of 1.0g are added in the ethylene glycol of 10ml, stir, be designated as A solution; The sodium hydroxide of 0.16g is joined in the ethylene glycol of 10ml, stir, be designated as B solution; B solution poured in the A solution stir, then 160 ℃ of lower crystallization 24 hours, use the dehydrated alcohol centrifuge washing, 60 ℃ of dryings 10 hours obtain finely dispersed open core type hydrotalcite microballoon.
[embodiment 2]
1). the preparation of solid NiFe hydrotalcite microballoon:
The nickelous nitrate of 0.317g, the iron trichloride of 0.12g and the sodium laurylsulfonate of 0.3g are added in the ethylene glycol of 10ml, stir, be designated as A solution; The sodium hydroxide of 0.16g is joined in the ethylene glycol of 10ml, stir, be designated as B solution; B solution poured in the A solution stir, then 160 ℃ of lower crystallization 24 hours, use the dehydrated alcohol centrifuge washing, 60 ℃ of dryings 10 hours obtain finely dispersed core-shell type hydrotalcite microballoon.
2). the preparation of yolk formula NiFe hydrotalcite microballoon:
The nickelous nitrate of 0.317g, the iron trichloride of 0.12g and the sodium laurylsulfonate of 0.6g are added in the ethylene glycol of 10ml, stir, be designated as A solution; The sodium hydroxide of 0.16g is joined in the ethylene glycol of 10ml, stir, be designated as B solution; B solution poured in the A solution stir, then 160 ℃ of lower crystallization 24 hours, use the dehydrated alcohol centrifuge washing, 60 ℃ of dryings 10 hours obtain finely dispersed yolk formula hydrotalcite microballoon.
3). the preparation of open core type NiFe hydrotalcite microballoon:
The nickelous nitrate of 0.317g, the iron trichloride of 0.12g and the sodium laurylsulfonate of 1.0g are added in the ethylene glycol of 10ml, stir, be designated as A solution; The sodium hydroxide of 0.16g is joined in the ethylene glycol of 10ml, stir, be designated as B solution; B solution poured in the A solution stir, then 160 ℃ of lower crystallization 24 hours, use the dehydrated alcohol centrifuge washing, 60 ℃ of dryings 10 hours obtain finely dispersed open core type hydrotalcite microballoon.
Claims (7)
1. the lower method for preparing the Multilevel-structure hydrotalcite microballoon of tensio-active agent guiding is characterized in that, its concrete steps are as follows:
The divalent metal nitrate of 0.1-0.4g, the trivalent iron salt of 0.1-0.5g and the tensio-active agent of 0.2-1.0g are added in the ethylene glycol of 10-30ml, stir, be designated as A solution; The sodium hydroxide of 0.1-0.2g is joined in the ethylene glycol of 10-30ml, stir, be designated as B solution; B solution poured in the A solution stir, then at 120-160 ℃ of lower crystallization 12-24 hour, use the dehydrated alcohol centrifuge washing, 50-80 ℃ dry 6-12 hour, obtain finely dispersed hydrotalcite microballoon.
2. method according to claim 1 is characterized in that, described divalent metal nitrate is selected from Mg (NO
3)
2, Co (NO
3)
2, Ni (NO
3)
2In a kind of.
3. method according to claim 1 is characterized in that, described trivalent iron salt is FeCl
3, Fe (NO
3)
3, Fe
2(SO
4)
3In a kind of.
4. method according to claim 1 is characterized in that, described tensio-active agent is cetyl trimethylammonium bromide, Sodium dodecylbenzene sulfonate or sodium cetanesulfonate.
5. arbitrary described method is characterized in that according to claim 1-4, and when described tensio-active agent add-on was 0.2-0.4g, the hydrotalcite microballoon that obtains was solid construction.
6. arbitrary described method is characterized in that according to claim 1-4, and when described tensio-active agent add-on was 0.5-0.7g, the hydrotalcite microballoon that obtains was yolk formula structure.
7. arbitrary described method is characterized in that according to claim 1-4, and when described tensio-active agent add-on was 0.8-1.0g, the hydrotalcite microballoon that obtains was hollow structure.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145202A (en) * | 2013-03-18 | 2013-06-12 | 燕山大学 | Synthetic method of layered flower type shell powder based nickel aluminum hydrotalcite |
| CN103241752A (en) * | 2013-05-29 | 2013-08-14 | 肇庆学院 | Preparation method of surface-modified hydrotalcite |
| CN104762101A (en) * | 2015-04-17 | 2015-07-08 | 北京化工大学 | Method for oxidative desulfurization of fuel oil by adopting polyacid intercalation trihydroxymethyl hydrotalcite and ionic liquid extraction catalysis |
| CN110467225A (en) * | 2019-09-03 | 2019-11-19 | 大连理工大学 | A kind of preparation method of the hollow sandwich microballoon of monodisperse cobalt sulfide |
| CN110538648A (en) * | 2018-12-21 | 2019-12-06 | 天津大学 | Flower-shaped hierarchical pore structure hydrotalcite-like material, preparation method of catalyst and application of catalyst in propane dehydrogenation |
| CN111498876A (en) * | 2020-05-20 | 2020-08-07 | 中铝山东有限公司 | Preparation method of guiding agent and preparation method of magnesium-aluminum hydrotalcite |
| CN113104872A (en) * | 2021-05-24 | 2021-07-13 | 北京化工大学 | Method for preparing organic molecule intercalation hydrotalcite array by one-step method |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103145202A (en) * | 2013-03-18 | 2013-06-12 | 燕山大学 | Synthetic method of layered flower type shell powder based nickel aluminum hydrotalcite |
| CN103145202B (en) * | 2013-03-18 | 2014-07-23 | 燕山大学 | Synthetic method of layered flower type shell powder based nickel aluminum hydrotalcite |
| CN103241752A (en) * | 2013-05-29 | 2013-08-14 | 肇庆学院 | Preparation method of surface-modified hydrotalcite |
| CN104762101A (en) * | 2015-04-17 | 2015-07-08 | 北京化工大学 | Method for oxidative desulfurization of fuel oil by adopting polyacid intercalation trihydroxymethyl hydrotalcite and ionic liquid extraction catalysis |
| CN110538648A (en) * | 2018-12-21 | 2019-12-06 | 天津大学 | Flower-shaped hierarchical pore structure hydrotalcite-like material, preparation method of catalyst and application of catalyst in propane dehydrogenation |
| CN110467225A (en) * | 2019-09-03 | 2019-11-19 | 大连理工大学 | A kind of preparation method of the hollow sandwich microballoon of monodisperse cobalt sulfide |
| CN111498876A (en) * | 2020-05-20 | 2020-08-07 | 中铝山东有限公司 | Preparation method of guiding agent and preparation method of magnesium-aluminum hydrotalcite |
| CN111498876B (en) * | 2020-05-20 | 2022-08-02 | 中铝山东有限公司 | Preparation method of guiding agent and preparation method of magnesium-aluminum hydrotalcite |
| CN113104872A (en) * | 2021-05-24 | 2021-07-13 | 北京化工大学 | Method for preparing organic molecule intercalation hydrotalcite array by one-step method |
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