CN109867288A - Mesoporous monox nanometer carrying material and preparation method thereof - Google Patents
Mesoporous monox nanometer carrying material and preparation method thereof Download PDFInfo
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- CN109867288A CN109867288A CN201811086064.2A CN201811086064A CN109867288A CN 109867288 A CN109867288 A CN 109867288A CN 201811086064 A CN201811086064 A CN 201811086064A CN 109867288 A CN109867288 A CN 109867288A
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Abstract
The present invention relates to a kind of mesoporous monox nanometer carrying materials and preparation method thereof.The mesoporous monox nanometer band has relatively orderly mesopore orbit, and for length between 1 ~ 1.5 μm, width is 45 ~ 50 nm.It can be seen that the resulting mesoporous silicon oxide nanomaterial of the present invention from SEM picture and unique kinky-like structure be presented.TEM also confirms that edge of materials is crimped, and be observed that apparent mesopore orbit structure the results show that the edge of materials and internal light and shade are clearly demarcated.The invention preparation band-like mesoporous silicon oxide nanomaterial, due to its with surfaces externally and internally can functional modification unique texture, be all with a wide range of applications in fields such as environmental catalysis, absorption and biomedicines.
Description
Technical field
The present invention relates to a kind of mesoporous monox nanometer carrying materials and preparation method thereof.
Background technique
Mesoporous silicon oxide nanomaterial is prominent due to its high specific area, adjustable aperture and diversified appearance structure etc.
Advantage, since 1992 report MCM-41 for the first time by Mobil company, always by the extensive of material circle and chemists
Concern especially controls, in terms of structure regulating and growth mechanism in its pattern.The institute of mesoporous silicon oxide nanomaterial
To show many excellent physico-chemical properties, in addition to having outside the Pass with the unique mesopore orbit of material, also with the macroscopic view of material itself
Form is related with microscopic appearance.In recent years, scientists be dedicated to regulate and control mesopore silicon oxide internal gutter structure while,
Its exterior appearance abundant of growing interest.Currently, the mesoporous silicon oxide nanomaterial of various patterns and different structure is reported in succession
Road, such as it is spherical, bowl-shape, rodlike and flower-shaped, and they play important work in fields such as absorption, catalysis and biological medicines
With.
It is noted that in these structures, the meso pore silicon oxide material for possessing banded structure is unique each by its
The features such as anisotropy cause the special attention of scholars.However, as far as we know, current research, which focuses mostly on, is utilizing chiral table
Face activating agent prepares chiral mesoporous monox nanometer band, and use the anionic/cationic surfactant of routine be total
Template is but rarely reported to prepare mesoporous monox nanometer band.What cationic surfactant and anionic surfactant were constituted
Binary surfactant system can form a plurality of types of micro-structures due to the controllability of its head group opposite charges,
Such as vesica, stratiform, spherical shape and club shaped structure.
Summary of the invention
One of the objects of the present invention is to provide a kind of mesoporous monox nanometer carrying materials.
The second object of the present invention is to provide the preparation method of the mesoporous monox nanometer band.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of mesoporous monox nanometer carrying material, it is characterised in that the mesoporous monox nanometer band has relatively orderly mesoporous hole
Road, for length between 1 ~ 1.5 μm, width is 45 ~ 50 nm.
A method of preparing above-mentioned mesoporous monox nanometer carrying material, it is characterised in that the specific steps of this method
Are as follows:
A. cetyl trimethylammonium bromide is dissolved in deionized water, being configured to molar concentration is 0.0015 ~ 0.002
The solution of mol/L is then added ethyl acetate (EA), continues to stir evenly；The ethyl acetate and cetyl trimethyl
The molar ratio of ammonium bromide are as follows: 6 ~ 8；
B. lauryl sodium sulfate is added in step a acquired solution, and stirred evenly, the ammonia of 25 ~ 28 wt.% is added later
Water continues to stir evenly；The molar ratio of the lauryl sodium sulfate and cetyl trimethylammonium bromide are as follows: 0.9 ~ 1, pH
Value is between 8 ~ 10；
C. tetraethyl orthosilicate is added in step b acquired solution as silicon source, 15~24 h of sustained response, after the reaction was completed,
Reactant is centrifugated, and is washed with deionized, dries, obtains mesoporous monox nanometer carrying material；The positive silicic acid
The molar ratio of tetra-ethyl ester and lauryl sodium sulfate are as follows: 0.4 ~ 0.5.
The present invention for silicon source, is used as by using anion/cation surfactant and is mixed with tetraethyl orthosilicate (TEOS)
Template, ethyl acetate (EA) help template action under, common guiding prepares the mesopore silicon oxide with unique coiled structure
Nanobelt material.
In synthesis process of the present invention, the addition of ethyl acetate plays a dual role of cosolvent and helps template, in micro emulsion
Under system, single cationic surfactant cetyl trimethylammonium bromide (CTAB) forms rod-shaped micelle, and assembling is formed
The spherical shape of stable structure.After anionic (SDS) is added, zwitterion double-template
Collective effect is in micella, and the rod-shaped micelle length of formation is longer and stacking number reduces, so that stability reduces, structure tends to
It is formed by bending cyclic structure；When continuing to improve SDS dosage to 0.08 g, the rod-shaped micelle of stacking starts avalanche and forms stratiform knot
Structure, with the progress of reaction, material, which reduces direction towards Gibbs free energy, to be carried out, therefore surface crimps, and then forms volume
Curved banded structure.
Compared with existing synthetic technology, the technology of the present invention have it is following it is significant a little: use two distinct types of table
For face activating agent as hybrid template, synthetic method is simple, mild condition, morphology controllable, due to its unique curly nano junction
Structure has potential application prospect in fields such as environmental catalysis, absorption and biomedicines.
Detailed description of the invention
Fig. 1 is the SEM picture of gained mesoporous monox nanometer band in the embodiment of the present invention 1.
Fig. 2 is the TEM picture of gained mesoporous monox nanometer band in the embodiment of the present invention 1.
Fig. 3 is the TEM picture of gained mesoporous monox nanometer stick in the embodiment of the present invention 2.
Fig. 4 is the TEM photo of gained mesoporous monox nanometer ball in comparative example of the present invention.
Specific embodiment
The operating procedure of all embodiments according to the above technical scheme is operated.
Embodiment 1
A. 0.1 g cetyl trimethylammonium bromide (CTAB) is dissolved in 137 mL deionized waters, until solution clarify, with
After 1.32 mL ethyl acetate (EA) are added, continue to stir evenly；
B. 0.08 g lauryl sodium sulfate (SDS) is added in above-mentioned solution, is 1 with CTAB molar ratio, and stir evenly, it
The ammonium hydroxide (25 ~ 28 wt.%) of 2.7 mL is added afterwards, continues to stir evenly；
C. finally, 275 μ L tetraethyl orthosilicates (TEOS), which are added, is used as silicon source, 20 h of sustained response after the reaction was completed will be anti-
It answers object to be centrifugated, and is washed repeatedly with deionized water, dried, obtained white powder is mesoporous monox nanometer band.
Products obtained therefrom is subjected to physical property characterization, partial results are as shown in the picture.Gained mesopore silicon oxide product length is 1
Between ~ 1.5 μm, wide about 45 nm, are the banded structure of edge curl.Meanwhile TEM is the results show that the material has obviously
The mesopore orbit along banded structure radial direction, pattern is uniform.
Embodiment 2
The preparation process and step of the present embodiment are substantially the same manner as Example 1, and difference is b step:
The dosage of lauryl sodium sulfate (SDS) is 0.04 g.
Acquired results all have apparent difference in pattern and configuration aspects with embodiment 1, and products obtained therefrom part presents and closes
The cyclic structure of conjunction, the structure are mainly 400 nm or so by length, and the nanometer rods of about 43 nm of diameter form, and have good
Duct feature.
Embodiment 3
The preparation process and step of the present embodiment are substantially the same manner as Example 1, and difference is a step:
Ethyl acetate (EA) dosage is 0.5 mL.
Acquired results have apparent difference compared with Example 1, and obtaining product is layer structure, and still there is slight volume at edge
Song, but relatively thick and bad dispersibility.
Embodiment 4
The preparation process and step of the present embodiment are substantially the same manner as Example 1, and difference is a step:
Ethyl acetate (EA) changes isometric ether into.
Compared with Example 1, structure is significantly different for acquired results, obtains the club shaped structure that curling folds.
Comparative example: the preparation process and step of the present embodiment are identical with embodiment 1, and difference is b step:
Lauryl sodium sulfate (SDS) is not added.
Acquired results and 1 topographical difference of embodiment are larger, obtain the uniform mesoporous monox nanometer of pattern after the reaction was completed
Ball, monodispersity is good, and partial size is 150 ~ 200 nm.
Referring to attached drawing, Fig. 1 is the scanning electron microscope (SEM) of 1 gained mesoporous silicon dioxide nano carrying material of the embodiment of the present invention
Picture.Sem analysis: material morphology is observed using Japan Electronics Corporation JSM-6700F type transmitting scanning electron microscope.From SEM
For picture it is found that meso pore silicon oxide material produced by the present invention, pattern is more uniform, has unique curly nanostructure.
Referring to attached drawing, Fig. 2 is the transmission electron microscope (TEM) of 1 gained mesoporous silicon dioxide nano carrying material of the embodiment of the present invention
Picture.Tem analysis: Jeol Ltd. JEOL-200CX type transmission electron microscope observation material morphology and knot are used
Structure.It can be seen that Metaporous silicon dioxide material produced by the present invention from TEM picture, there is apparent banded structure and mesoporous hole
Road, width are 45 ~ 50 nm, and 5 nm of lamellar spacing or so, length is between 1 ~ 1.5 μm.
Referring to attached drawing, Fig. 3 is transmission electron microscope (TEM) figure of 2 gained mesoporous monox nanometer bar material of the embodiment of the present invention
Piece.There it can be seen that mesopore silicon oxide made from the present embodiment is the class diamond structure of rodlike connection, the diameter of stick is 43
Nm or so.
Referring to attached drawing, Fig. 4 is transmission electron microscope (TEM) picture of mesoporous silica nanospheres obtained by comparative example of the present invention.
From TEM picture it is found that oxidation silicon nano material made from comparative example have uniform spherical morphology and it is relatively orderly it is mesoporous with
And good monodispersity, partial size are 150 ~ 200 nm.
Claims (2)
1. a kind of mesoporous monox nanometer carrying material, it is characterised in that the mesoporous monox nanometer band has relatively orderly mesoporous
Duct, for length between 1 ~ 1.5 μm, width is 45 ~ 50 nm.
2. a kind of method for preparing mesoporous monox nanometer carrying material according to claim 1, it is characterised in that this method
Specific steps are as follows:
A. cetyl trimethylammonium bromide is dissolved in deionized water, being configured to molar concentration is 0.0015 ~ 0.002
The solution of mol/L is then added ethyl acetate (EA), continues to stir evenly；The ethyl acetate and cetyl trimethyl
The molar ratio of ammonium bromide are as follows: 6 ~ 8；
B. lauryl sodium sulfate is added in step a acquired solution, and stirred evenly, the ammonia of 25 ~ 28 wt.% is added later
Water continues to stir evenly；The molar ratio of the lauryl sodium sulfate and cetyl trimethylammonium bromide are as follows: 0.9 ~ 1, pH
Value is between 8 ~ 10；
C. tetraethyl orthosilicate is added in step b acquired solution as silicon source, 15~24 h of sustained response, after the reaction was completed,
Reactant is centrifugated, and is washed with deionized, dries, obtains mesoporous monox nanometer carrying material；The positive silicic acid
The molar ratio of tetra-ethyl ester and lauryl sodium sulfate are as follows: 0.4 ~ 0.5.
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| CN101166573A (en) * | 2005-03-07 | 2008-04-23 | 金斯顿女王大学 | Sol gel functionalized silicate catalyst and scavenger |
| JP2011020023A (en) * | 2009-07-14 | 2011-02-03 | Dic Corp | Method for producing photocatalyst and photocatalyst |
| CN102502660A (en) * | 2011-10-18 | 2012-06-20 | 苏州大学 | Spiral mesoporous silicon dioxide nanofiber with cracked surface and preparation method thereof |
| CN103224239A (en) * | 2013-04-08 | 2013-07-31 | 天津大学 | Chiral mesoporous silica nano-rod and preparation method thereof |
| CN104386699A (en) * | 2014-11-05 | 2015-03-04 | 上海大学 | Method for preparing multi-shell mesoporous silicon oxide nanomaterial by dual-template method |
| CN105692625A (en) * | 2014-11-24 | 2016-06-22 | 中国科学院上海硅酸盐研究所 | Preparation method of oxide nanotube and nanobelt |
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2018
- 2018-09-18 CN CN201811086064.2A patent/CN109867288B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101166573A (en) * | 2005-03-07 | 2008-04-23 | 金斯顿女王大学 | Sol gel functionalized silicate catalyst and scavenger |
| JP2011020023A (en) * | 2009-07-14 | 2011-02-03 | Dic Corp | Method for producing photocatalyst and photocatalyst |
| CN102502660A (en) * | 2011-10-18 | 2012-06-20 | 苏州大学 | Spiral mesoporous silicon dioxide nanofiber with cracked surface and preparation method thereof |
| CN103224239A (en) * | 2013-04-08 | 2013-07-31 | 天津大学 | Chiral mesoporous silica nano-rod and preparation method thereof |
| CN104386699A (en) * | 2014-11-05 | 2015-03-04 | 上海大学 | Method for preparing multi-shell mesoporous silicon oxide nanomaterial by dual-template method |
| CN105692625A (en) * | 2014-11-24 | 2016-06-22 | 中国科学院上海硅酸盐研究所 | Preparation method of oxide nanotube and nanobelt |
Non-Patent Citations (1)
| Title |
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| CHEN, YUXIA ET AL.: "Formation of Left-handed Double Twisted Silica Nanoribbons", 《CHIN. J. CHEM》 * |
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