CN102897844B - 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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- CN102897844B CN102897844B CN201210394722.0A CN201210394722A CN102897844B CN 102897844 B CN102897844 B CN 102897844B CN 201210394722 A CN201210394722 A CN 201210394722A CN 102897844 B CN102897844 B CN 102897844B
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- hydrotalcite
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- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 title claims abstract description 46
- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 46
- 229910001701 hydrotalcite Inorganic materials 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000004005 microsphere Substances 0.000 title abstract description 13
- 239000004094 surface-active agent Substances 0.000 title abstract 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000007787 solid Substances 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000013543 active substance Substances 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000002425 crystallisation Methods 0.000 claims description 8
- 230000008025 crystallization Effects 0.000 claims description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 210000002969 egg yolk Anatomy 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 150000002505 iron Chemical class 0.000 claims description 4
- 229910001960 metal nitrate Inorganic materials 0.000 claims description 4
- 238000010276 construction Methods 0.000 claims description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 239000012876 carrier material Substances 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000008685 targeting Effects 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 11
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 6
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 6
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 6
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 4
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 3
- 239000013335 mesoporous material Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 238000005194 fractionation Methods 0.000 description 2
- 239000008204 material by function Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000010406 interfacial reaction Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000002648 laminated material Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
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 under a kind of tensio-active agent guiding, prepare the method for Multilevel-structure hydrotalcite microballoon.
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, bring 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 multilevel hierarchy micro-sphere material, have template duplicating method, microemulsion method, template-interfacial reaction method, spray method and supersonic method etc.As prepared the inorganicss such as Si, Al, Ti, metal and oxide compound and sulfide, macromole or high molecular polymer etc. by template duplicating method.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 controlling yardstick, condition of surface, the inner structural features of nanoparticle, thereby obtain New Type of Mesoporous complex body functional materials.Therefore, the research of mesoporous material has in recent years 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 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 existing easily, assembles the hydrotalcite that traditional synthetic method of preparing hydrotalcite obtains, the deficiencies such as microtexture lack of alignment, and this has limited its functional giving full play to greatly.The controlled preparation that realizes hydrotalcite microballoon not only can realize the making full use of of hydrotalcite self property, and can bring into play its special constructional feature.The present invention is to Development of Novel functional materials and realize making full use of of material property and have great importance.
Summary of the invention
The object of this invention is to provide a kind of prepare Multilevel-structure hydrotalcite microballoon under tensio-active agent guiding method.
Technical scheme of the present invention is: in ethylene glycol solution, take tensio-active agent as directed agents, take divalence, trivalent metal salts solution is raw material, carries out the Nano microsphere that hydro-thermal reaction obtains hydrotalcite under alkaline environment.Wherein, by the content of modulation tensio-active agent realize hydrotalcite microballoon by solid construction to yolk formula structure again to the modulation of hollow structure.
The concrete steps of method of preparing Multilevel-structure hydrotalcite microballoon under tensio-active agent of the present invention guiding 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 is poured in A solution and stirred, and then crystallization 12-24 hour at 120-160 ℃, uses dehydrated alcohol centrifuge washing, and 50-80 ℃ of dry 6-12 hour obtains 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 is 0.2-0.4g, the hydrotalcite microballoon obtaining is solid construction.
When above-mentioned tensio-active agent add-on is 0.5-0.7g, the hydrotalcite microballoon obtaining is yolk formula structure.
When above-mentioned tensio-active agent add-on is 0.8-1.0g, the hydrotalcite microballoon obtaining is hollow structure.
The present invention has realized the preparation of the adjustable magnetic hydrotalcite microballoon of internal structure first, the hydrotalcite microballoon obtaining 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 obtaining 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.
Accompanying drawing explanation
Fig. 1 is the projection electromicroscopic photograph of the Multilevel-structure hydrotalcite microballoon that obtains of the embodiment of the present invention 1.
Fig. 2 is the stereoscan photograph of the Multilevel-structure hydrotalcite microballoon that obtains of the embodiment of the present invention 1.
Fig. 3 is the XRD spectra of the Multilevel-structure hydrotalcite microballoon that obtains of the embodiment of the present 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
-1; Ordinate zou is transmitance.
Embodiment
[embodiment 1]
1). the preparation of solid MgFe hydrotalcite microballoon:
The sodium laurylsulfonate of the iron trichloride of the magnesium nitrate of 0.396g, 0.18g and 0.3g is added in the ethylene glycol of 10ml, stirs, 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 is poured in A solution and stirred, and then crystallization 24 hours at 160 ℃, uses dehydrated alcohol centrifuge washing, 60 ℃ dry 10 hours, obtain finely dispersed core-shell type hydrotalcite microballoon.
2). the preparation of yolk formula MgFe hydrotalcite microballoon:
The sodium laurylsulfonate of the iron trichloride of the magnesium nitrate of 0.396g, 0.18g and 0.6g is added in the ethylene glycol of 10ml, stirs, 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 is poured in A solution and stirred, and then crystallization 24 hours at 160 ℃, uses dehydrated alcohol centrifuge washing, 60 ℃ dry 10 hours, obtain finely dispersed yolk formula hydrotalcite microballoon.
3). the preparation of open core type MgFe hydrotalcite microballoon:
The sodium laurylsulfonate of the iron trichloride of the magnesium nitrate of 0.396g, 0.18g and 1.0g is added in the ethylene glycol of 10ml, stirs, 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 is poured in A solution and stirred, and then crystallization 24 hours at 160 ℃, uses dehydrated alcohol centrifuge washing, 60 ℃ dry 10 hours, obtain finely dispersed open core type hydrotalcite microballoon.
[embodiment 2]
1). the preparation of solid NiFe hydrotalcite microballoon:
The sodium laurylsulfonate of the iron trichloride of the nickelous nitrate of 0.317g, 0.12g and 0.3g is added in the ethylene glycol of 10ml, stirs, 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 is poured in A solution and stirred, and then crystallization 24 hours at 160 ℃, uses dehydrated alcohol centrifuge washing, 60 ℃ dry 10 hours, obtain finely dispersed core-shell type hydrotalcite microballoon.
2). the preparation of yolk formula NiFe hydrotalcite microballoon:
The sodium laurylsulfonate of the iron trichloride of the nickelous nitrate of 0.317g, 0.12g and 0.6g is added in the ethylene glycol of 10ml, stirs, 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 is poured in A solution and stirred, and then crystallization 24 hours at 160 ℃, uses dehydrated alcohol centrifuge washing, 60 ℃ dry 10 hours, obtain finely dispersed yolk formula hydrotalcite microballoon.
3). the preparation of open core type NiFe hydrotalcite microballoon:
The sodium laurylsulfonate of the iron trichloride of the nickelous nitrate of 0.317g, 0.12g and 1.0g is added in the ethylene glycol of 10ml, stirs, 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 is poured in A solution and stirred, and then crystallization 24 hours at 160 ℃, uses dehydrated alcohol centrifuge washing, 60 ℃ dry 10 hours, obtain finely dispersed open core type hydrotalcite microballoon.
Claims (4)
1. under tensio-active agent guiding, prepare a method for Multilevel-structure hydrotalcite microballoon, it 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 is poured in A solution and stirred, and then crystallization 12-24 hour at 120-160 ℃, uses dehydrated alcohol centrifuge washing, and 50-80 ℃ of dry 6-12 hour obtains finely dispersed hydrotalcite microballoon;
When described tensio-active agent add-on is 0.2-0.4g, the hydrotalcite microballoon obtaining is solid construction;
When described tensio-active agent add-on is 0.5-0.7g, the hydrotalcite microballoon obtaining is yolk formula structure;
When described tensio-active agent add-on is 0.8-1.0g, the hydrotalcite microballoon obtaining is hollow structure.
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.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104762101B (en) * | 2015-04-17 | 2017-01-25 | 北京化工大学 | Method for oxidative desulfurization of fuel oil by adopting polyacid intercalation trihydroxymethyl hydrotalcite and ionic liquid extraction catalysis |
| CN110538648B (en) * | 2018-12-21 | 2022-08-23 | 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 |
| 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 |
| CN113104872B (en) * | 2021-05-24 | 2022-10-21 | 北京化工大学 | Method for preparing organic molecule intercalation hydrotalcite array by one-step method |
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| CN100542966C (en) * | 2006-11-28 | 2009-09-23 | 山东大学 | Rod hydrotalcite-like compound and preparation method thereof |
| CN101972631A (en) * | 2010-09-17 | 2011-02-16 | 北京化工大学 | Multilevel-structure hydrotalcite adsorbent and preparation method thereof |
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