CN108017065A - A kind of preparation method using the penetrating shape liquid crystal of two dimension as the mesoporous silicon oxide of masterplate - Google Patents
A kind of preparation method using the penetrating shape liquid crystal of two dimension as the mesoporous silicon oxide of masterplate Download PDFInfo
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- CN108017065A CN108017065A CN201810024022.XA CN201810024022A CN108017065A CN 108017065 A CN108017065 A CN 108017065A CN 201810024022 A CN201810024022 A CN 201810024022A CN 108017065 A CN108017065 A CN 108017065A
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P2006/14—Pore volume
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Abstract
The invention discloses a kind of preparation method using the penetrating shape liquid crystal of two dimension as the mesoporous silicon oxide of masterplate, change method with cetyl trimethylammonium bromide (CTAB) and the two-dimentional penetrating shape liquid crystal (LCs) that is self-assembly of of lauryl sodium sulfate (SDS) mixing cationic-anionic surfactants as template, tetraethoxysilane (TEOS) is inorganic precursors, under conditions of acidity, using collosol and gel method and by calcining the Metaporous silicon dioxide material for removing masterplate and being finally synthesizing the penetrating shape of two dimension.The present invention is easy to operate；Employ the liquid crystal of the surfactant formation of mixing reduces the use of single raw material for masterplate, so as to save cost and alleviate the influence to environment.
Description
Technical field
The present invention relates to field of inorganic material science, particularly a kind of mesoporous dioxy using the penetrating shape liquid crystal of two dimension as masterplate
The preparation method of SiClx.
Background technology
Mesoporous material is the virgin material system to grow up in 20th century, synthesizes M41s series materials from Mobil companies
Rise and just paid much attention to be subject to international chemistry, material and community of physicists.Since it is homogeneous adjustable etc. with high-specific surface area, aperture
Feature, it has a wide range of applications in fields such as absorption, catalysis, biologies.
What the synthesis of ordered mesoporous material relied on is supermolecule masterplate mechanism, is to utilize to have amphiphatic surfactant
Self assembly characteristic in aqueous and its interaction between inorganic precursor, obtain having having for specific mesoscopic structure
Machine-inorganic composite, roasting or extraction remove surfactant, obtain the side with the mesoporous material of orderly duct arrangement
Method.The function of wherein surfactant is to be self-assembly of various microcosmic knot as structure directing masterplate progress parents' molecule
Structure.Cationic surfactant, nonionic surfactant and anion surfactant are successively employed successfully in synthesising mesoporous
Silica, however, since single ionic surface active agent has higher critical micelle concentration (CMC), causes as mould
The amount of surfactant needed for version is larger, so that experimental cost is improved, and surface-active is relatively low, it is often more important that and it is hydrophilic
Synergistic effect between head base is relatively low, it is difficult to be self-assembled into various microstructure.
The content of the invention
To solve the above-mentioned problems, the present invention provides a kind of using the penetrating shape liquid crystal of two dimension as the mesoporous silicon oxide of masterplate
Preparation method.
The method proposed by the present invention for preparing mesoporous silicon oxide is to mix cationic and anionic surfactant cetyl
The two-dimentional penetrating shape liquid crystal that trimethylammonium bromide (CTAB) and lauryl sodium sulfate (SDS) are self-assembly of is masterplate, tetrem
Oxysilane (TEOS) is silicon source, and under conditions of acidity, the synthesis of mesoporous material is carried out by the method for sol-gel.This
Invention is the synthesising mesoporous material of masterplate using mixing cationic and anionic surfactant, and zwitterion table is mixed under appropriate ratio
Face activating agent illustrates the stronger synergistic effect not being separated, this is because hydrophilic head base effective dimensions reduce and it is hydrophobic
Partial volume increases, this will influence surfactant quantity, and it is logical that the micella resulted in is changed into plane polymolecular layer i.e. two dimension
The liquid crystal structure of saturating shape, the formation of liquid crystal structure result in the reduction of the surfactant total amount during synthesising mesoporous material
Then the cost for reducing experiment alleviates the influence of environment at the same time, and they can also reduce the formation concentration of liquid crystalline phase,
Change the viscosity of surfactant solution.
To achieve the above object, the present invention provides following technical solution：A kind of Jie using the penetrating shape liquid crystal of two dimension as masterplate
The preparation method of hole silica, comprises the following steps that：
(1) certain density CTAB and SDS solution is respectively configured with hydrochloric acid and is dissolved；
(2) TEOS solution is added in the SDS settled solutions dissolved, and the two mixed solution is added to immediately
In CTAB solution；
(3) mixed solution in step (2) is placed in thermostat water bath, heating stirring certain time, produces colloidal sol and coagulate
After glue, it stands under certain bath temperature to certain time obtains solid precipitation；
(4) product obtained by step (3) is filtered, is constantly washed with water during filtering, then drying is dry
It is dry；
(5) step (4) dried solid is calcined, removes template agent, then the solid after calcining is washed
Wash, filter, dry, finally obtain mesopore silicon dioxide nano material.
In a variety of cationic surfactants, CTAB can have good with anion, nonionic, amphoteric surfactant
Coordinating, chemical stability is good, heat-resisting, fast light, pressure-resistant, strong alkali-acid resistance.Compared to other cationic surfactants,
The price of CTAB is relatively low, and due to good compatibility, it is possible to reduce the use of chemical reagent, so as to reduce reality
Test cost.
Further, the concentration of CTAB and SDS solution is 0.015mol/L~0.3mol/L in the step (1), hydrochloric acid
PH value be 1~6.
As template agent concentration increases, the specific surface area of mesoporous material rises.This is because in low concentration, liquid in system
Brilliant (LCs) is loose, H between layer structure2The region increase of O, so that the mesoporous material wall thickness with synthesis, order is poor, compares table
Area is low, and LCs is fine and close after concentration increase, and order improves, specific surface area increase.After template agent concentration reaches certain value, than
Surface area has reached maximum, and order is high.As concentration continues to increase, specific surface area is on a declining curve, template agent concentration
The lifting of the excessive specific surface area for being also unfavorable for material, this is because system viscosity increases, LCs structures are difficult to reach balance and stability
State, so as to have impact on its order and the order of mesoporous material.
In strong acid solution, TEOS hydrolysis abilities are strong, but polycondensation reaction is slow, and silicate ion more can uniformly divide
Cloth is polycondensed into inorganic hole wall around template.Obtain having certain ordered and the higher mesoporous material of specific surface area
Material.As pH value is reduced, mesoporous material specific surface area significantly increases, and specific surface area reaches maximum during pH=2.
SDS is soluble easily in water, therefore during configuration SDS solution, it is easy to dissolve, so as to save the time.SDS and CTAB compatibilities
Performance is good, and dispersion performance is good.It is important that it is cheap, experimental cost can be saved.
Critical micelle concentration (CMC) value of CTAB and SDS is relatively low, therefore has saved template agent dosage, while both are one
Under fixed ratio, it is easy to form the liquid crystal of the penetrating shape of two dimension.And form the mild condition of liquid crystal, it is only necessary to adjust suitable
Temperature.During for synthesizing mesoporous silicon dioxide material, the simple acid that adds is catalyst, it is not necessary to high temperature and pressure
Environment, greatly saves manpower and materials.
Further, the molar ratio of mixed solution and TEOS (water silicon ratio) are 50~100 in the step (2).
Further, the temperature of water bath with thermostatic control is 40 DEG C~100 DEG C in the step (3), and the time of heating stirring is
24h.The bath temperature of standing is 40 DEG C~60 DEG C, time of repose 24h.
Further, drying temperature is 80 DEG C~100 DEG C in the step (4).
Further, calcining heat is 550 DEG C in the step (5), calcination time 6h.
Further, prepared mesoporous silicon oxide is characterized as：Specific surface area is 800m2/ g, pore size are
0.68cc/g, pore volume 3.5nm.
Compared with prior art, beneficial effect of the present invention：
(1) process of the present invention is simple, mild condition, due to providing acid condition, along with template agent charge effect, TEOS
With complete hydrolysis and silica can be aggregated into, and Silica Properties are stablized, therefore the yield of mesoporous silicon oxide is high.
(2) being used as masterplate and can save material by mixing cationic and anionic surfactant cost but also reduces to environment
Influence, the specific surface area of the mesoporous silicon oxide synthesized using liquid crystal as masterplate is bigger, order is higher, aperture size is equal
One, it can apply well in fields such as pollutant absorption, material transmission, sensor development, chromatography and electrophoretic separation.And closing
During by controlling synthesis condition factor such as reaction temperature, surfactant concentration, pH to obtain compared with Gao Bibiao
The homogeneous mesoporous material of area, pore-size distribution.
Brief description of the drawings
Fig. 1 is the polarisation photo of the penetrating shape liquid crystal of the two dimension of the embodiment of the present invention 1, the suction of the Metaporous silicon dioxide material of synthesis
Attached-desorption isotherm and scanning electron microscope (SEM) photograph.
Fig. 2 is the adsorption-desorption isothermal and scanning electron microscope for the Metaporous silicon dioxide material that the embodiment of the present invention 2 synthesizes
Figure.
Fig. 3 is the polarisation photo of the penetrating shape liquid crystal of the two dimension of the embodiment of the present invention 3 and the Metaporous silicon dioxide material of synthesis
Scanning electron microscope (SEM) photograph.
Fig. 4 is the adsorption/desorption isotherms and scanning electron microscope (SEM) photograph for the Metaporous silicon dioxide material that the embodiment of the present invention 4 synthesizes.
Fig. 5 is the adsorption/desorption isotherms and scanning electron microscope (SEM) photograph for the Metaporous silicon dioxide material that the embodiment of the present invention 5 synthesizes.
Embodiment
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other without making creative work
Embodiment, belongs to the scope of protection of the invention.
Embodiment 1
Configuration concentration is 0.2mol/L surfactant solutions, and the hydrochloric acid that the CTAB addition pH value for weighing 6.296g is 2 is molten
Liquid is to 86.4g；The SDS for similarly weighing 1.938g adds pH value in the hydrochloric acid solution for 2 to 33.6g, and heating stirring makes it respectively
Dissolving；Weigh 18.479g (water silicon ratio is 70) TEOS to be added in the good SDS solution of above-mentioned dissolving, quickly by both mixing
Solution is added in the CTAB solution dissolved, and Heating Water stirring 24h is carried out at 50 DEG C；Then stirring is stopped, at 50 DEG C
24h is stood under bath temperature；Then filtered, washed 3 times with hot water, be subsequently placed in 100 DEG C of baking ovens dry 24h；Will be dry
Solid after dry is placed in crucible, and removed template method is roasted in Muffle furnace by temperature programming, is risen to the speed of 2 DEG C/min
550 DEG C, 6h then is roasted at 550 DEG C, Muffle furnace is then shut off and cools down automatically.Product passes through washing, filters, is dry, grinding again
Mill can obtain final product mesoporous silicon oxide.
Fig. 1 a are to utilize the liquid crystal polarisation formed under the conditions of the example 1 gone out captured by homemade easy polarisation detection device
Photo, it was found from the polarisation phenomenon produced from figure, the liquid crystal structure for having densification is formed, and according to Fig. 1 b liquid crystal petrographic microscopes
It was observed that microphoto can obtain, the liquid crystal of formation has obvious " cruciate flower " structure to produce, and the structure is logical for obvious two dimension
The microstructure of saturating shape liquid crystal.Adsorption-desorption isothermal such as figure using liquid crystal for the Metaporous silicon dioxide material of masterplate synthesis
Shown in 1c, from isothermal type, the silica of synthesis has the obvious characteristic of mesoporous material, is closed under the conditions of example 1
Into mesoporous material hysteresis loop it is steeper, illustrate that its pore-size distribution is homogeneous, order is strong.Can also from Fig. 1 d scanning electron microscope (SEM) photographs
Prove the conclusion, Fig. 1 d are the scanning electron microscope (SEM) photograph of synthetic material under the conditions of example 1, obvious from electron microscope it can be seen that synthesis
Mesoporous silicon oxide be orderly two-dimentional penetrating shape structure, and consistency height, specific surface area is big, reaches 800m2/g.This is
Due to the first polycondensation speed with TEOS of Formation of liquid crystals speed, SiO at 50 DEG C2Life can be reacted in the LCs masterplates formed
Into so as to form orderly structure.
Embodiment 2
Configuration concentration is 0.2mol/L surfactant solutions, and the hydrochloric acid that the CTAB addition pH value for weighing 6.296g is 1 is molten
Liquid is to 86.4g；The SDS for similarly weighing 1.938g adds pH value in the hydrochloric acid solution for 1 to 33.6g, and heating stirring makes it respectively
Dissolving；Weigh 12.935g (water silicon ratio is 100) TEOS to be added in the SDS solution dissolved in step (1), quickly incite somebody to action both
Mixed solution be added in the CTAB solution dissolved, at 60 DEG C carry out Heating Water stirring 48h；Then stirring is stopped,
48h is stood under 60 DEG C of bath temperature；Then filtered, washed 3 times with hot water, is subsequently placed in 100 DEG C of baking ovens dry
24h；Dried solid is placed in crucible, removed template method is roasted in Muffle furnace by temperature programming, with 2 DEG C/min's
Speed rises to 550 DEG C, then roasts 6h at 550 DEG C, is then shut off Muffle furnace and cools down automatically.Product again by washing, filter,
Dry, grinding can obtain final product mesoporous silicon oxide.
Fig. 2 a are the adsorption/desorption isotherms of the Metaporous silicon dioxide material synthesized under the conditions of example 2, and the absorption of example 2 takes off
Attached thermoisopleth also has the feature of mesoporous material, but isothermal hysteresis loop, than shallower, the thermoisopleth compared to example 1 can
To find out, the structure of the material synthesized under the conditions of illustrated example 2 is more dispersed, heterogeneity.Synthesize and be situated between under the conditions of Fig. 2 b examples 2
The scanning electron microscope (SEM) photograph of hole earth silicon material can further confirm the conclusion.Under the conditions of the generation of the conclusion is due to example 2,
The amount of silicon source is fewer, and simultaneously synthesizing temperature is higher, and the liquid crystal energy comparison that surfactant molecule is formed is high, unstable,
The silica aggregated into be difficult completely with template agent electrostatic interaction, therefore formed structure it is more dispersed.
Embodiment 3
Configuration concentration is 0.2mol/L surfactant solutions, and the hydrochloric acid that the CTAB addition pH value for weighing 6.296g is 2 is molten
Liquid is to 86.4g；The SDS for similarly weighing 1.938g adds pH value in the hydrochloric acid solution for 2 to 33.6g, and heating stirring makes it respectively
Dissolving；Weigh 18.479g (water silicon ratio is 70) TEOS to be added in the SDS solution dissolved in step (1), quickly by both
Mixed solution is added in the CTAB solution dissolved, and Heating Water stirring 48h is carried out at 40 DEG C；Then stirring is stopped, 40
DEG C bath temperature under stand 48h；Then filtered, washed 3 times with hot water, be subsequently placed in 100 DEG C of baking ovens dry 24h；
Dried solid is placed in crucible, removed template method is roasted in Muffle furnace by temperature programming, with the speed of 2 DEG C/min
550 DEG C are risen to, then roasts 6h at 550 DEG C, Muffle furnace is then shut off and cools down automatically.Product is again by washing, filtering, dry
Dry, grinding can obtain final product mesoporous silicon oxide.
Fig. 3 a are using homemade polarisation detection device simply to observe whether template agent has partially under the conditions of 40 DEG C (example 3)
Optical phenomenon, from photo as can be seen that there is the generation of polarisation phenomenon under the conditions of being somebody's turn to do, but structure of polarized light is more dispersed.With under the conditions of this
The scanning electron microscope (SEM) photograph of Metaporous silicon dioxide material that synthesizes for masterplate of liquid crystal as shown in Figure 3b, as can be seen from the figure due to
Disperseing for liquid crystal structure, it is imperfect, therefore the two-dimentional penetrating shape structure of the material synthesized is also more dispersed.
Embodiment 4
Configuration concentration is 0.05mol/L surfactant solutions, and the hydrochloric acid that the CTAB addition pH value for weighing 3.935g is 6 is molten
Liquid is to 216g；The SDS for similarly weighing 1.211g adds pH value in the hydrochloric acid solution for 6 to 84g, and heating stirring makes its molten respectively
Solution；Weigh 25.871g (water silicon ratio is 50) TEOS to be added in the SDS solution dissolved in step (1), quickly by both mixed
Close solution to be added in the CTAB solution dissolved, Heating Water stirring 12h is carried out at 60 DEG C；Then stirring is stopped, at 60 DEG C
Bath temperature under stand 18h；Then filtered, washed 3 times with hot water, be subsequently placed in 80 DEG C of baking ovens dry 24h；Will be dry
Solid after dry is placed in crucible, and removed template method is roasted in Muffle furnace by temperature programming, is risen to the speed of 2 DEG C/min
300 DEG C, 5h then is roasted at 300 DEG C, Muffle furnace is then shut off and cools down automatically.Product passes through washing, filters, is dry, grinding again
Mill can obtain final product mesoporous silicon oxide.
Fig. 4 a show the absorption of the mesoporous material synthesized under the conditions of surfactant concentration 0.05mol/L (example 4)-de-
Attached thermoisopleth, the hysteresis loop shape facility of curve are totally different from the hysteresis loop of the mesoporous material of above-mentioned synthesis, this is because
During low concentration such as 0.05mol/L, liquid crystal structure is loose in system, the region increase of water layer between layer structure, and four ethoxies
The amount of base silane is more, and is synthesized under the conditions of partial neutral, and the polycondensation speed of silane is more than hydrolysis rate so that with synthesis
The speed-priority of mesoporous material and the speed of Formation of liquid crystals, the mesoporous material wall thickness resulted in, order is poor, specific surface area
It is low.The solvent area outside liquid crystal structure forms the unordered silica of bulk at the same time.Can be with by Fig. 4 b scanning electron microscope (SEM) photographs
Image observes this phenomenon.
Embodiment 5
Configuration concentration is 0.3mol/L surfactant solutions, and the hydrochloric acid that the CTAB addition pH value for weighing 9.444g is 2 is molten
Liquid weighs 2.907g SDS and adds hydrochloric acid solution that pH value is 2 to 33.6g to 86.4g.Heating stirring makes its dissolving respectively；Claim
18.479g (water silicon ratio is 70) TEOS is taken to be added in the SDS solution dissolved in step (1), it is quickly that both mixing is molten
Liquid is added in the CTAB solution dissolved, and Heating Water stirring 48h is carried out at 60 DEG C；Then stirring is stopped, in 60 DEG C of water
48h is stood under bath temperature；Then filtered, washed 3 times with hot water, be subsequently placed in 90 DEG C of baking ovens dry 24h；After dry
Solid be placed in crucible, removed template method is roasted in Muffle furnace by temperature programming, 650 are risen to the speed of 2 DEG C/min
DEG C, 7h then is roasted at 650 DEG C, Muffle furnace is then shut off and cools down automatically.Product passes through washing, filters, is dry, grinding again
It can obtain final product mesoporous silicon oxide.
Example 5 is the synthesizing mesoporous silicon dioxide material under the conditions of mixed surfactant concentration (0.3mol/L) is increased
, as shown in Figure 5 a, though thermoisopleth there are hysteresis loop feature possessed by mesoporous material, than shallower, illustrates to be formed
Material it is uneven.Fig. 5 b are scanning electron microscope (SEM) photograph, and the meso-porous titanium dioxide silicon layer of the two-dimentional penetrating shape synthesized shown in figure is thicker,
And it is scattered, it is uneven.Improved mainly due to surfactant concentration, the viscosity of mixed solution also increases, the liquid crystal of formation
It is not easy to scatter, accumulation together, forms thicker liquid crystal layer.
Obviously, those skilled in the art can carry out invention spirit of the various modification and variations without departing from the present invention
And scope.If in this way, these modifications and changes of the present invention belong to the claims in the present invention and its equivalent technologies scope it
Interior, then the present invention is also intended to comprising including these modification and variations.
Claims (7)
- A kind of 1. preparation method using the penetrating shape liquid crystal of two dimension as the mesoporous silicon oxide of masterplate, it is characterised in that specific steps It is as follows：(1) with hydrochloric acid be respectively configured certain density cetyl trimethylammonium bromide and sodium dodecyl sulfate solution and by its Dissolving；(2) tetraethoxysilane solution is added in the lauryl sodium sulfate settled solution dissolved, and the two is mixed Solution is closed to be added in cetyl trimethylammonium bromide solution immediately；(3) mixed solution in step (2) is placed in thermostat water bath, heating stirring certain time, produce collosol and gel it Afterwards, it is stood under certain bath temperature certain time obtain solid precipitation；(4) product obtained by step (3) is filtered, is constantly washed with water during filtering, then dries drying；(5) step (4) dried solid is calcined, removes template agent, then the solid after calcining is washed, is taken out Consider, drying, finally obtain mesopore silicon dioxide nano material.
- 2. the preparation method of mesoporous silicon oxide according to claim 1, it is characterised in that 16 in the step (1) The concentration of alkyl trimethyl ammonium bromide and sodium dodecyl sulfate solution is 0.05mol/L~0.3mol/L, and the pH value of hydrochloric acid is 1 ~6.
- 3. the preparation method of mesoporous silicon oxide according to claim 1, it is characterised in that 12 in the step (2) The molar ratio of sodium alkyl sulfate settled solution and tetraethoxysilane is 50~100.
- 4. the preparation method of mesoporous silicon oxide according to claim 1, it is characterised in that constant temperature in the step (3) The temperature of water-bath is 40 DEG C~60 DEG C, and the time of heating stirring is 12-48h, and the bath temperature of standing is 40 DEG C~60 DEG C, is stood Time is 18-48h.
- 5. the preparation method of mesoporous silicon oxide according to claim 1, it is characterised in that dry in the step (4) Temperature is 80 DEG C~100 DEG C.
- 6. the preparation method of mesoporous silicon oxide according to claim 1, it is characterised in that calcining in the step (5) Temperature is 300-650 DEG C, calcination time 5-7h.
- 7. according to the preparation method of claim 1-6 any one of them mesoporous silicon oxides, it is characterised in that prepared Jie Hole silicon dioxide features are：Specific surface area is 500-800m2/ g, pore size 0.68cc/g, pore volume 3.5nm.
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| CN110571392B (en) * | 2018-06-29 | 2020-12-08 | 华中科技大学 | Functional interlayer material of lithium-sulfur battery and preparation method thereof |
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