CN101920970A - Preparation method of silicate nano hollow structure material - Google Patents
Preparation method of silicate nano hollow structure material Download PDFInfo
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- CN101920970A CN101920970A CN 201010111591 CN201010111591A CN101920970A CN 101920970 A CN101920970 A CN 101920970A CN 201010111591 CN201010111591 CN 201010111591 CN 201010111591 A CN201010111591 A CN 201010111591A CN 101920970 A CN101920970 A CN 101920970A
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Abstract
The invention relates to a preparation method of a silicate nano hollow structure material, which comprises the following steps: (1) orderly adding 0.2 mol/L nitrate solution and 0.2 mol/L sodium silicate solution into mixed liquor of ethanol and polyethylene glycol to form a mixed solution, wherein the mixed solution respectively comprises 20-30 parts of ethanol, 2-3 parts of polyethylene glycol, 1 part of nitrate solution and 1-2 parts of sodium silicate solution in parts by volume; (2) adding NaOH solution into the mixed solution obtained in step (1), wherein the volume ratio of NaOH solution to nitrate solution is 1:0.03-0.2; and after conducting magnetic stirring, transferring the mixed solution to a hydrothermal kettle, reacting under the hydrothermal condition of 100-200 DEG C, filtering and drying to obtain the silicate nano hollow structure material. The obtained silicate hollow material can be used for heavy metal ion absorption, and can also be used in the fields of catalysis, medicines, environmental pollution treatment and the like.
Description
Technical field
The present invention relates to a kind of preparation method of hollow material, particularly a kind of preparation method of silicate nano hollow structure material.
Background technology
At present developed a lot of methods that prepare hollow material both at home and abroad, the most general method has with inorganics, metal, polymer billet etc. as the hard template method of template with the soft template method as template such as microemulsion, vesica.For example, Yoon S.B. etc. reported on the AdvancedMaterials magazine and use the solid-surface mesoporous silico-aluminate bead of submicron-scale as template in 2002, made surface mesoporous carbon material Capsules (Adv.Mater., 2002,14:19-21).Djojoputro H. etc. reported use vesica and liquid crystal dual mould plate method in 2006 on Journal of The AmericanChemical Society magazine, made the mesoporous organosilicon hollow material (J.Am.Chem.Soc. of the rule of adjustable wall thickness, 2006,128:6320-6321).Therefore hard template method and soft template method all can obtain uniformly meso-porous hollow material, yet hard template method is to the removal of template particles very expensive and consuming time always, and for the effective preparation of soft template more complicated usually in the soft template method.
Summary of the invention
In order to overcome the defective of above-mentioned prior art, the object of the present invention is to provide a kind of preparation method of silicate nano hollow structure material, nitrate and sodium silicate solution are joined in ethanol and the polyoxyethylene glycol mixed solvent, regulate the pH value with NaOH, be transferred to liquid phase reaction in the closed reaction vessel tetrafluoroethylene autoclave, the silicate hollow material that obtains can be used aspect heavy metal ion adsorbed to some extent, can be used for fields such as catalysis, medicine, environmental pollution improvement.
In order to achieve the above object, technical scheme of the present invention is achieved in that
A kind of preparation method of silicate nano hollow structure material may further comprise the steps:
One, in the mixed solution of ethanol and polyoxyethylene glycol, add the nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, nitrate solution and sodium silicate solution is respectively 20-30 part, 2-3 part, 1 part and 1-2 part in this mixing solutions;
Two, in the mixing solutions that step 1 makes, add 4mol/L NaOH solution, NaOH solution is 1 with nitrate solution volume parts ratio in the step 1: 0.03-0.2, behind the magnetic agitation 15-30min, be transferred in the water heating kettle, react 12-48h under 100 ℃～200 ℃ hydrothermal conditions, filtration drying obtains silicate nano hollow structure material.
The resulting silicate hollow structure material of the present invention is to heavy metal ion, as Pb
2+, Cr
3+, Cd
2+And Fe
3+Deng good exchange absorption property is arranged, this is because the nano-scale of material and hollow structure have increased the specific surface that silicate can be used for ion-exchange and absorption, no matter and be silicate stratiform or chain-like structure, be free between the silica casing ply or metal ion that interchain can move freely can more touch external environment, and replaced by other metal ion.So the silicate hollow structure material that the present invention obtains is bigger than the ion-exchange performance of silicate minerals material in the past.
Description of drawings
Fig. 1 is that the XRD of embodiment 1,2 prepared Magnesium Silicate q-agent hollow balls and nucleocapsid ball product characterizes, and wherein: a is that the XRD of hollow ball characterizes the XRD phenogram of b nucleocapsid ball product.
Fig. 2 is the TEM phenogram of embodiment 1 prepared Magnesium Silicate q-agent nucleocapsid ball product.
Fig. 3 is the SEM phenogram of embodiment 2 prepared Magnesium Silicate q-agent hollow ball products.
Fig. 4 is the EDS composition analysis figure of embodiment 1 and 2 prepared Magnesium Silicate q-agent hollow balls and nucleocapsid ball product
Fig. 5 is the TEM phenogram and the SEM phenogram of embodiment 3 and 4 prepared zinc silicates, hollow aluminosilicate ball product, and wherein: a, b are zinc silicate, and c, d are pure aluminium silicate.
Embodiment
Embodiment one
The preparation method of present embodiment may further comprise the steps:
One, in the mixed solution of ethanol and polyoxyethylene glycol, add the magnesium nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, magnesium nitrate solution and sodium silicate solution is respectively 30 parts, 3 parts, 1 part and 1 part in this mixing solutions;
Two, in the mixing solutions that step 1 makes, add 4mol/LNaOH solution, NaOH solution is 1: 0.03 with nitrate solution volume parts ratio in the step 1, behind the magnetic agitation 15min, be transferred in the water heating kettle, react 12h under 190 ℃ of hydrothermal conditions, filtration drying obtains Magnesium Silicate q-agent core-shell particles product.
Among Fig. 1: the b curve is that the XRD of embodiment 1 prepared nucleocapsid ball product characterizes, main diffraction peak 2 θ=19.493,24.366,35.307 and 60.414 ° and Mg
3Si
2O
5(OH)
4(JCPDS no.52-1562) is consistent for standard diagram, has illustrated that product is a Magnesium Silicate q-agent.
Fig. 2 is that the TEM of embodiment 1 prepared nucleocapsid ball product characterizes, and picture shows that almost 90% sample is made up of hollow ball shell and kernel, and the diameter of nucleocapsid ball is between 100～200nm.
Embodiment two
The preparation method of present embodiment may further comprise the steps:
One, in the mixed solution of ethanol and polyoxyethylene glycol, add the magnesium nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, magnesium nitrate solution and sodium silicate solution is respectively 30 parts, 3 parts, 1 part and 1 part in this mixing solutions;
Two, in the mixing solutions that step 1 makes, add 4mol/LNaOH solution, NaOH solution is 1: 0.1 with nitrate solution volume parts ratio in the step 1, behind the magnetic agitation 15min, be transferred in the water heating kettle, react 12h under 190 ℃ of hydrothermal conditions, filtration drying obtains Magnesium Silicate q-agent tiny balloon product.
Among Fig. 1: a curve is that the XRD of embodiment 2 prepared Magnesium Silicate q-agent hollow balls characterizes, main diffraction peak 2 θ=19.493,24.366,35.307 and 60.414 ° and Mg
3Si
2O
5(OH)
4(JCPDS no.52-1562) is consistent for standard diagram, has illustrated that product is a Magnesium Silicate q-agent.
Fig. 3 is that the TEM of example 2 prepared Magnesium Silicate q-agent hollow balls characterizes, and as can be seen from the figure, institute's synthetic product is homogeneous (almost 90% is hollow ball) comparatively, and the diameter dimension of hollow ball is between 100～200nm, and the Magnesium Silicate q-agent hollow ball is made up of small pieces.
As can be seen from Figure 1, the difference of two embodiment degree of crystallinity that is Magnesium Silicate q-agent hollow ball product good than nucleocapsid ball product.And Fig. 4 EDS collection of illustrative plates shows, no matter be hollow structure or nucleocapsid structure, all contains elements such as Mg, Si and O in the product sample, and by more as can be seen, the Mg/Si value of Magnesium Silicate q-agent hollow ball is bigger than nucleocapsid ball, illustrates that hollow ball contains more Mg element.
Embodiment three
The preparation method of present embodiment may further comprise the steps:
One, in the mixed solution of ethanol and polyoxyethylene glycol, add the zinc nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, zinc nitrate solution and sodium silicate solution is respectively 25 parts, 2 parts, 1 part and 1 part in this mixing solutions;
Two, in the mixing solutions that step 1 makes, add 4mol/LNaOH solution, NaOH solution is 1: 0.15 with nitrate solution volume parts ratio in the step 1, behind the magnetic agitation 30min, be transferred in the water heating kettle, react 24h under 120 ℃ of hydrothermal conditions, filtration drying obtains the zinc silicate hollow ball material.
Among Fig. 5: a-b is that the TEM and the SEM of embodiment 3 prepared zinc silicate products characterizes, and as can be seen from the figure the pattern of product is a hollow ball structure.
Embodiment four
The preparation method of present embodiment may further comprise the steps:
One, in the mixed solution of ethanol and polyoxyethylene glycol, add the aluminum nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, aluminum nitrate solution and sodium silicate solution is respectively 27 parts, 2 parts, 1 part and 1.5 parts in this mixing solutions;
Two, in the mixing solutions that step 1 makes, add 4mol/LNaOH solution, NaOH solution is 1: 0.12 with nitrate solution volume parts ratio in the step 1, behind the magnetic agitation 15min, be transferred in the water heating kettle, react 12h under 160 ℃ of hydrothermal conditions, filtration drying obtains the hollow aluminosilicate ball material.
Among Fig. 5: c-d is that the TEM and the SEM of embodiment 4 prepared pure aluminium silicate products characterizes, and as can be seen from the figure the pattern of product is a hollow ball structure.
It is 106.42mg/L that the 0.05g Magnesium Silicate q-agent sample ultrasonic of embodiment one preparation is scattered in 10ml concentration, and pH value is 2 Pb (II) deionized water solution, is adsorbed on surperficial OH with nitre acid for adjusting pH value to 7 with neutralization again
-, when stirring, it is joined in the Pb that 10ml concentration is 106.42mg/L (II) solution then, stir after 3 hours, solid is separated from solution, and the concentration of staying Pb in the solution (II) is detected.
The sample of embodiment two preparation is detected as stated above equally, and as can be seen from Table 1, Magnesium Silicate q-agent hollow ball product and nucleocapsid ball product are respectively 64.79 and 47.51mg g to Pb (II) ionic removal ability
-1Nucleocapsid ball product is littler than hollow ball product to Pb (II) ionic exchange adsorptive power, this is because the nucleocapsid ball product of equivalent is compared with the hollow ball product and contained less Mg (II) ion (the EDS collection of illustrative plates can prove), makes it possible to that Mg (II) ion that replaced by Pb (II) ion exchange is less to be caused.
The BET data and the ion adsorption capacity of the prepared Magnesium Silicate q-agent product of table 1
In addition, table 2 has proved that Magnesium Silicate q-agent hollow ball product all has ion-exchange absorption effect to Cr (III), Cd (II) and Fe (III) plasma.
The prepared Magnesium Silicate q-agent hollow ball product of table 2 is to the absorption of different ions
Claims (5)
1. the preparation method of a silicate nano hollow structure material, it is characterized in that, may further comprise the steps: one, in the mixed solution of ethanol and polyoxyethylene glycol, add the nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, nitrate solution and sodium silicate solution is respectively 20-30 part, 2-3 part, 1 part and 1-2 part in this mixing solutions; Two, in the mixing solutions that step 1 makes, add 4mol/L NaOH solution, NaOH solution is 1 with nitrate solution volume parts ratio in the step 1: 0.03-0.2, behind the magnetic agitation 15-30min, be transferred in the water heating kettle, react 12-48h under 100 ℃～200 ℃ hydrothermal conditions, filtration drying obtains silicate nano hollow structure material.
2. the preparation method of a kind of silicate nano hollow structure material according to claim 1, it is characterized in that, may further comprise the steps: one, in the mixed solution of ethanol and polyoxyethylene glycol, add the magnesium nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, magnesium nitrate solution and sodium silicate solution is respectively 30 parts, 3 parts, 1 part and 1 part in this mixing solutions; Two, in the mixing solutions that step 1 makes, add 4mol/LNaOH solution, NaOH solution is 1: 0.03 with nitrate solution volume parts ratio in the step 1, behind the magnetic agitation 15min, be transferred in the water heating kettle, react 12h under 190 ℃ of hydrothermal conditions, filtration drying obtains Magnesium Silicate q-agent core-shell particles product.
3. the preparation method of a kind of silicate nano hollow structure material according to claim 1, it is characterized in that, may further comprise the steps: one, in the mixed solution of ethanol and polyoxyethylene glycol, add the magnesium nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, magnesium nitrate solution and sodium silicate solution is respectively 30 parts, 3 parts, 1 part and 1 part in this mixing solutions; Two, in the mixing solutions that step 1 makes, add 4mol/LNaOH solution, NaOH solution is 1: 0.1 with nitrate solution volume parts ratio in the step 1, behind the magnetic agitation 15min, be transferred in the water heating kettle, react 12h under 190 ℃ of hydrothermal conditions, filtration drying obtains Magnesium Silicate q-agent tiny balloon product.
4. the preparation method of a kind of silicate nano hollow structure material according to claim 1, it is characterized in that, may further comprise the steps: one, in the mixed solution of ethanol and polyoxyethylene glycol, add the zinc nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, zinc nitrate solution and sodium silicate solution is respectively 25 parts, 2 parts, 1 part and 1 part in this mixing solutions; Two, in the mixing solutions that step 1 makes, add 4mol/LNaOH solution, NaOH solution is 1: 0.15 with nitrate solution volume parts ratio in the step 1, behind the magnetic agitation 30min, be transferred in the water heating kettle, react 24h under 120 ℃ of hydrothermal conditions, filtration drying obtains the zinc silicate hollow ball material.
5. the preparation method of a kind of silicate nano hollow structure material according to claim 1, it is characterized in that, may further comprise the steps: one, in the mixed solution of ethanol and polyoxyethylene glycol, add the aluminum nitrate solution of 0.2mol/L and the sodium silicate solution of 0.2mol/L successively, form mixing solutions, the volume parts of ethanol, polyoxyethylene glycol, aluminum nitrate solution and sodium silicate solution is respectively 27 parts, 2 parts, 1 part and 1.5 parts in this mixing solutions; Two, in the mixing solutions that step 1 makes, add 4mol/LNaOH solution, NaOH solution is 1: 0.12 with nitrate solution volume parts ratio in the step 1, behind the magnetic agitation 15min, be transferred in the water heating kettle, react 12h under 160 ℃ of hydrothermal conditions, filtration drying obtains the hollow aluminosilicate ball material.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103071438A (en) * | 2013-01-07 | 2013-05-01 | 中国科学院合肥物质科学研究院 | Preparation method of core-shell structured micro-nanosphere comprising magnetic core and magnesium silicate nano-sheet shell |
| CN103359749A (en) * | 2013-07-22 | 2013-10-23 | 东北师范大学 | Preparation method for porous rare earth silicate hollow spheres |
| CN103635426A (en) * | 2011-03-11 | 2014-03-12 | 日立化成株式会社 | Aluminum silicate, metal ion adsorbent, and method for producing same |
| CN104445228A (en) * | 2014-10-21 | 2015-03-25 | 中国建筑材料科学研究总院 | Hollow spherical type serpentine superfine powder and preparation method thereof |
| CN106237975A (en) * | 2016-08-09 | 2016-12-21 | 北京化工大学 | A kind of high-ratio surface big pore volume adsorption of magnesium silicate material and its preparation method and application |
| CN107500303A (en) * | 2017-08-14 | 2017-12-22 | 曲阜师范大学 | A kind of mesoporous magnesium silicate microballoon and its hydro-thermal thermal transition preparation method |
| CN109796021A (en) * | 2019-04-04 | 2019-05-24 | 河北工业大学 | Utilize the method for iron tailings preparation ellipsoid zinc silicate compound adsorbent |
| CN113716576A (en) * | 2021-07-29 | 2021-11-30 | 浙江工业大学 | Method for preparing hollow spherical zeolite by using natural zeolite |
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| CN1211155C (en) * | 2003-07-18 | 2005-07-20 | 清华大学 | Preparation method of silicate nano tube for adsorbing and separating gas |
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2010
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Patent Citations (1)
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| CN1211155C (en) * | 2003-07-18 | 2005-07-20 | 清华大学 | Preparation method of silicate nano tube for adsorbing and separating gas |
Non-Patent Citations (1)
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| 《J. Phys. Chem. C》 20090521 Yuan Zhuang, et al. Magnesium Silicate Hollow Nanostructures as Highly Efficient Absorbents for Toxic Metal Ions 10441-10445 1-5 第113卷, 第24期 2 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103635426A (en) * | 2011-03-11 | 2014-03-12 | 日立化成株式会社 | Aluminum silicate, metal ion adsorbent, and method for producing same |
| CN103635426B (en) * | 2011-03-11 | 2017-03-01 | 日立化成株式会社 | Aluminosilicate, metal ion adsorbent and their manufacture method |
| CN103071438A (en) * | 2013-01-07 | 2013-05-01 | 中国科学院合肥物质科学研究院 | Preparation method of core-shell structured micro-nanosphere comprising magnetic core and magnesium silicate nano-sheet shell |
| CN103359749A (en) * | 2013-07-22 | 2013-10-23 | 东北师范大学 | Preparation method for porous rare earth silicate hollow spheres |
| CN104445228A (en) * | 2014-10-21 | 2015-03-25 | 中国建筑材料科学研究总院 | Hollow spherical type serpentine superfine powder and preparation method thereof |
| CN106237975A (en) * | 2016-08-09 | 2016-12-21 | 北京化工大学 | A kind of high-ratio surface big pore volume adsorption of magnesium silicate material and its preparation method and application |
| CN107500303A (en) * | 2017-08-14 | 2017-12-22 | 曲阜师范大学 | A kind of mesoporous magnesium silicate microballoon and its hydro-thermal thermal transition preparation method |
| CN107500303B (en) * | 2017-08-14 | 2019-10-08 | 曲阜师范大学 | A kind of mesoporous magnesium silicate microballoon and its hydro-thermal-thermal transition preparation method |
| CN109796021A (en) * | 2019-04-04 | 2019-05-24 | 河北工业大学 | Utilize the method for iron tailings preparation ellipsoid zinc silicate compound adsorbent |
| CN109796021B (en) * | 2019-04-04 | 2022-04-05 | 河北工业大学 | Method for preparing ellipsoidal zinc silicate composite adsorbent by using iron tailings |
| CN113716576A (en) * | 2021-07-29 | 2021-11-30 | 浙江工业大学 | Method for preparing hollow spherical zeolite by using natural zeolite |
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Application publication date: 20101222 |