CN108545751A - Ordered mesoporous silica dioxide super-thin sheet-shaped material of one type graphene-structured and preparation method thereof - Google Patents
Ordered mesoporous silica dioxide super-thin sheet-shaped material of one type graphene-structured and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to ordered mesoporous silica dioxide super-thin sheet-shaped materials of a type graphene-structured and preparation method thereof, belong to silicon-based mesoporous material preparing technical field.The present invention is using cheap melamine as hard template, block copolymer is surfactant, ethyl orthosilicate is silicon source, block copolymer surfactant is dissolved in ethanol water in preparation process and adjusts pH value to acidity, then ethyl orthosilicate is added to stir to form uniform mesopore silicon oxide precursor solution, it grinds this precursor solution and melamine hard template to obtain the mixture of mesopore silicon oxide presoma and melamine, then the mixture of mesopore silicon oxide presoma and melamine is placed in culture dish to be evaporated at room temperature induces self assembly to obtain solid powder, by this solid powder, successively high-temperature calcination is handled under nitrogen and air atmosphere, natural cooling, which cools down, can be obtained the ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured.
Description
Technical field
The present invention relates to the materials of a type graphene-structured, more particularly to order mesoporous the two of a type graphene-structured
Silica super-thin sheet-shaped material and preparation method thereof, belongs to silicon-based mesoporous material preparing technical field.
Background technology
From Univ Manchester UK An Deliegaimu professors in 2010 and Constantine's Nuo Woxiao loves because in stone
Remarkable research in terms of black alkene and since having shared Nobel Prize in physics, using graphene as the two-dimentional class graphene superthin section of representative
The nano material of shape structure receives the extensive concern of people.It is similar with graphene, class graphene two-dimensional ultrathin flaky material
It is multiple in photoelectricity, catalyst, transistor etc. with much very excellent characteristic, such as high-specific surface area, high Young's modulus
Field has potential application.
Another aspect pore size between 2-50nm ordered meso-porous silicon oxide material due to big specific surface area, height
Pore volume, uniform adjustable aperture the features such as have in catalysis, absorption, sensing, drug delivery and nano-reactor etc.
Wide application prospect.Prepared by ordered meso-porous silicon oxide material generally use surfactant soft template method, i.e., first surface is lived
Property agent be dissolved in the solution of certain pH value, silicon precursor, which is added, makes it hydrolyze self assembly at a certain temperature, then in certain condition
Lower removal organic surface active agent template obtains the target product with ordered mesopore structure.However this method can not obtain it is super
The ordered meso-porous silicon oxide material of flaky texture limits application of the mesoporous material in two-dimentional scale field.Therefore research and development one
The preparation method of the novel ordered mesoporous silica dioxide super-thin sheet-shaped material with class graphene-structured of kind is with great research
And practical value.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide it is a kind of it is novel effectively, production process it is simple and at
The ordered mesoporous silica dioxide super-thin sheet-shaped material of this lower class graphene-structured.
The present invention also provides a kind of preparation methods of the material.
The technical solution adopted by the present invention to solve the technical problems is：
The preparation method of the ordered mesoporous silica dioxide super-thin sheet-shaped material of one type graphene-structured, this method include such as
Lower step：
(a) block copolymer surfactant is dissolved in ethanol solution and adjusts pH value to 0.2-3.0, so with acid solution
Afterwards be added ethyl orthosilicate stir to form uniform mesopore silicon oxide precursor solution, wherein block copolymer surfactant with
The mass ratio of ethyl orthosilicate is 0.2-1.2：1；
(b) the mesopore silicon oxide precursor solution for preparing step (a) is ground with melamine hard template, obtains mesoporous oxygen
Then the mixture of mesopore silicon oxide presoma and melamine is placed in culture by the mixture of SiClx presoma and melamine
Induction self assembly is evaporated in ware at room temperature and obtains solid powder；
(c) the first calcination processing hot under nitrogen atmosphere of the solid powder for preparing step (b), then switches to air atmosphere again
Heat treatment removal organic formwork is carried out under enclosing, and the order mesoporous titanium dioxide of class graphene-structured is can be obtained after natural cooling cooling
Silicon super-thin sheet-shaped material.
Preferably, in step (a), the block copolymer surfactant is P123 (EO20PO70EO20), F127
(EO106PO70EO106) one or both of mixture.
Preferably, in step (a), the acid solution is the aqueous solution of nitric acid or hydrochloric acid, a concentration of 0.5-2mol/L.
Preferably, the mass ratio of the mesopore silicon oxide precursor solution and melamine described in step (b) is 1-5：
1, the meso pore silicon oxide material synthesized under the proportional region has more perfect class graphene super-thin sheet-shaped structure.
Preferably, the evaporation-induced self-assembly time described in step (b) is 6-24h.
Preferably, the hot calcination temperature in nitrogen atmosphere of the solid powder described in step (c) is 400-600 DEG C, forge
Burn time 1-8h.
Preferably, the heat treatment temperature in air atmosphere of the solid powder described in step (c) is 500-800 DEG C, forge
Burn time 2-10h.
Preferably, the optimum quality ratio of block copolymer surfactant and ethyl orthosilicate is 0.4-0.8:1, the ratio
The silica material synthesized under example range has more regular ordered mesopore structure.
Made from the preparation method of the ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured described in a kind of
Ordered mesoporous silica dioxide super-thin sheet-shaped material.
The preparation method of the ordered mesoporous silica dioxide super-thin sheet-shaped material of type graphene-structured provided by the invention,
Using cheap melamine as hard template, mesopore silicon oxide precursor solution and melamine hard template are first passed through in preparation process
Simple ground and mixed is crossed, after evaporation-induced self-assembly air-dries at room temperature again respectively under nitrogen and air atmosphere at high-temperature calcination
It is obtained after reason.Therefore the preparation method of the present invention is relatively easy, and production cost is relatively low.
The ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured provided by the invention has high specific surface
Product (500-1100m2g-1), big Kong Rong (0.8-2.5cm3g-1), unified and adjustable mesoporous pore size (2-10nm).
The beneficial effects of the invention are as follows：The ordered mesoporous silica dioxide of type graphene-structured provided by the invention is ultra-thin
Flaky material not only has the meso-hole structure of high-sequential, but also maintains two-dimentional class graphene super-thin sheet-shaped structure.It compares
In ordered mesoporous silicon-dioxide material prepared by conventional method, (its specific surface area is generally 300-700m2g-1, pore volume 0.4-
1.2cm3g-1), the ordered mesoporous silica dioxide super-thin sheet-shaped material of the class graphene-structured of present invention gained has higher ratio
The pore volume of surface area and bigger makes it have broader practice foreground in fields such as absorption, separation, catalysis.
Description of the drawings
Fig. 1 is the ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured prepared by the embodiment of the present invention 1
Stereoscan photograph；
Fig. 2 is the ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured prepared by the embodiment of the present invention 1
Transmission electron microscope photo (a) and low-angle XRD spectra (b).
Specific implementation mode
Below by specific embodiment, technical scheme of the present invention will be further explained in detail.It should be appreciated that this hair
Bright implementation is not limited to the following examples, and the accommodation in any form made to the present invention and/or changed will all be fallen
Enter the scope of the present invention.
In the present invention, if not refering in particular to, all parts, percentage are unit of weight, used equipment and raw material etc.
It is commercially available or commonly used in the art.Method in following embodiments is unless otherwise instructed the normal of this field
Rule method.
Embodiment1
The ordered mesoporous silica dioxide super-thin sheet-shaped material of one type graphene-structured, the material are by system as described below
Preparation Method is made：
(1), 2.3g block copolymer P123 surfactants are dissolved in 15mL ethanol solutions and with the HNO of 1mol/L3
PH value is adjusted to 0.5,4.2g ethyl orthosilicates are then added and continuously stir to form uniform mesopore silicon oxide precursor solution.
(2), mesopore silicon oxide precursor solution and 20g melamine hard templates prepared by step 1 are ground to obtain mesoporous
Then the mixture of mesopore silicon oxide presoma and melamine is placed in training by the mixture of siliconoxide precursor and melamine
Supporting to be evaporated at room temperature in ware induces self assembly 8h to obtain solid powder.
(3), by solid powder prepared by step 2 be transferred to tube furnace first be warming up under nitrogen atmosphere 500 DEG C calcining when
Between 3h, then switch to again and be warming up to 550 DEG C of remaining organic formworks of heat treatment 10h removals, natural cooling drop under air atmosphere
Temperature can be obtained the ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured.
Using Bei Shide, 3H-2000PS4 types specific surface area and Porosimetry are to the class graphene-structured of above-mentioned gained
Ordered mesoporous silica dioxide super-thin sheet-shaped material is measured, specific surface area 568m2/ g, aperture 2.4nm, pore volume are
1.5cm3/g。
The scanning electron microscope of the ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured manufactured in the present embodiment is shone
Piece is as shown in Figure 1, it will be clear that the material has three-dimensional class graphene super-thin sheet-shaped structure from figure；
The transmission electron microscope photo of the ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured prepared by this implementation
(a) and low-angle XRD spectra (b) is shown in Fig. 2, can be clear that from Fig. 2 a in silica super-thin sheet-shaped material surface
With the order mesoporous of many queueing disciplines, and the apparent diffraction maximum occurred on low-angle XRD spectra (Fig. 2 b)
The silica super-thin sheet-shaped material for demonstrating synthesis has orderly meso-hole structure.
Embodiment 2
The ordered mesoporous silica dioxide super-thin sheet-shaped material of one type graphene-structured, the material are by system as described below
Preparation Method is made：
(1), 2.3g block copolymer P123 surfactants are dissolved in 15mL ethanol solutions and with the HNO of 2mol/L3
PH value is adjusted to 1.2,6.8g ethyl orthosilicates are then added and continuously stir to form uniform mesopore silicon oxide precursor solution.
(2), mesopore silicon oxide precursor solution and 16g melamine hard templates prepared by step 1 are ground to obtain mesoporous
Then the mixture of mesopore silicon oxide presoma and melamine is placed in training by the mixture of siliconoxide precursor and melamine
Supporting to be evaporated at room temperature in ware induces self assembly 12h to obtain solid powder.
(3), by solid powder prepared by step 2 be transferred to tube furnace first be warming up under nitrogen atmosphere 550 DEG C calcining when
Between 4h, then switch to again and be warming up to 600 DEG C of remaining organic formworks of heat treatment 6h removals, natural cooling cooling under air atmosphere
It can be obtained the ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured.
Using Bei Shide, 3H-2000PS4 types specific surface area and Porosimetry are to the class graphene-structured of above-mentioned gained
Ordered mesoporous silica dioxide super-thin sheet-shaped material is measured, specific surface area 760m2/ g, aperture 3.6nm, pore volume are
1.9cm3/g。
Embodiment3
The ordered mesoporous silica dioxide super-thin sheet-shaped material of one type graphene-structured, the material are by system as described below
Preparation Method is made：
(1), 2.3g block copolymer F127 surfactants are dissolved in 15mL ethanol solutions and with the HCl of 0.5mol/L
PH value is adjusted to 1.8,4.8g ethyl orthosilicates are then added and continuously stir to form uniform mesopore silicon oxide precursor solution.
(2), mesopore silicon oxide precursor solution and 12g melamine hard templates prepared by step 1 are ground to obtain mesoporous
Then the mixture of mesopore silicon oxide presoma and melamine is placed in training by the mixture of siliconoxide precursor and melamine
Supporting to be evaporated at room temperature in ware induces self assembly 10h to obtain solid powder.
(3), by solid powder prepared by step 2 be transferred to tube furnace first be warming up under nitrogen atmosphere 450 DEG C calcining when
Between 7h, then switch to again and be warming up to 650 DEG C of remaining organic formworks of heat treatment 4h removals, natural cooling cooling under air atmosphere
It can be obtained the ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured.
Using Bei Shide, 3H-2000PS4 types specific surface area and Porosimetry are to the class graphene-structured of above-mentioned gained
Ordered mesoporous silica dioxide super-thin sheet-shaped material is measured, specific surface area 820m2/ g, aperture 5.6nm, pore volume are
2.1cm3/g。
Embodiment4
The ordered mesoporous silica dioxide super-thin sheet-shaped material of one type graphene-structured, the material are by system as described below
Preparation Method is made：
(1), 2.3g block copolymer F127 surfactants are dissolved in 15mL ethanol solutions and with the HCl tune of 2mol/L
PH value is saved to 2.5,7.6g ethyl orthosilicates are then added and continuously stir to form uniform mesopore silicon oxide precursor solution.
(2), mesopore silicon oxide precursor solution and 10g melamine hard templates prepared by step 1 are ground to obtain mesoporous
Then the mixture of mesopore silicon oxide presoma and melamine is placed in training by the mixture of siliconoxide precursor and melamine
Supporting to be evaporated at room temperature in ware induces self assembly 18h to obtain solid powder.
(3), by solid powder prepared by step 2 be transferred to tube furnace first be warming up under nitrogen atmosphere 600 DEG C calcining when
Between 2h, then switch to again and be warming up to 700 DEG C of remaining organic formworks of heat treatment 2h removals, natural cooling cooling under air atmosphere
It can be obtained the ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured.
Using Bei Shide, 3H-2000PS4 types specific surface area and Porosimetry are to the class graphene-structured of above-mentioned gained
Ordered mesoporous silica dioxide super-thin sheet-shaped material is measured, specific surface area 1080m2/ g, aperture 5.3nm, pore volume
For 2.38cm3/g。
Embodiment5
The ordered mesoporous silica dioxide super-thin sheet-shaped material of one type graphene-structured, the material are by system as described below
Preparation Method is made：
(1), that 0.8g block copolymer P123 and 1.5g block copolymer F127 surfactants are dissolved in 15mL ethyl alcohol is molten
In liquid and with the HNO of 1mol/L3PH value is adjusted to 0.6,5.8g ethyl orthosilicates are then added and continuously stir to form uniform Jie
Hole siliconoxide precursor solution.
(2), it grinds mesopore silicon oxide precursor solution and 8g melamine hard templates prepared by step 1 to obtain mesoporous oxygen
Then the mixture of mesopore silicon oxide presoma and melamine is placed in culture by the mixture of SiClx presoma and melamine
Induction self assembly is evaporated in ware at room temperature and obtains solid powder for 24 hours.
(3), by solid powder prepared by step 2 be transferred to tube furnace first be warming up under nitrogen atmosphere 550 DEG C calcining when
Between 5h, then switch to again and be warming up to 750 DEG C of remaining organic formworks of heat treatment 2h removals, natural cooling cooling under air atmosphere
It can be obtained the ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured.
Using Bei Shide, 3H-2000PS4 types specific surface area and Porosimetry are to the class graphene-structured of above-mentioned gained
Ordered mesoporous silica dioxide super-thin sheet-shaped material is measured, specific surface area 920m2/ g, aperture 4.6nm, pore volume are
1.98cm3/g。
Embodiment6
The ordered mesoporous silica dioxide super-thin sheet-shaped material of one type graphene-structured, the material are by system as described below
Preparation Method is made：
(1), 1.5g block copolymer P123 and 1g block copolymer F127 surfactants are dissolved in 15mL ethanol solutions
In and with the HCl of 2mol/L adjust pH value to 1.5,8g ethyl orthosilicates are then added and continuously stir to form uniform mesoporous oxidation
Silicon precursor solution.
(2), it grinds mesopore silicon oxide precursor solution and 8g melamine hard templates prepared by step 1 to obtain mesoporous oxygen
Then the mixture of mesopore silicon oxide presoma and melamine is placed in culture by the mixture of SiClx presoma and melamine
Induction self assembly 16h is evaporated in ware at room temperature and obtains solid powder.
(3), by solid powder prepared by step 2 be transferred to tube furnace first be warming up under nitrogen atmosphere 600 DEG C calcining when
Between 2h, then switch to again and be warming up to 800 DEG C of remaining organic formworks of heat treatment 2h removals, natural cooling cooling under air atmosphere
It can be obtained the ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured.
Using Bei Shide, 3H-2000PS4 types specific surface area and Porosimetry are to the class graphene-structured of above-mentioned gained
Ordered mesoporous silica dioxide super-thin sheet-shaped material is measured, specific surface area 770m2/ g, aperture 8.2nm, pore volume are
1.22cm3/g。
Embodiment7
The ordered mesoporous silica dioxide super-thin sheet-shaped material of one type graphene-structured, the material are by system as described below
Preparation Method is made：
(1), 2g block copolymer P123 and 0.3g block copolymer F127 surfactants are dissolved in 15mL ethanol solutions
In and with the HNO of 2mol/L3PH value is adjusted to 0.2,2g ethyl orthosilicates are then added and continuously stir to form uniform mesoporous oxygen
SiClx precursor solution.
(2), it grinds mesopore silicon oxide precursor solution and 5g melamine hard templates prepared by step 1 to obtain mesoporous oxygen
Then the mixture of mesopore silicon oxide presoma and melamine is placed in culture by the mixture of SiClx presoma and melamine
Induction self assembly 6h is evaporated in ware at room temperature and obtains solid powder.
(3), by solid powder prepared by step 2 be transferred to tube furnace first be warming up under nitrogen atmosphere 400 DEG C calcining when
Between 8h, then switch to again and be warming up to 500 DEG C of remaining organic formworks of heat treatment 10h removals, natural cooling drop under air atmosphere
Temperature can be obtained the ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured.
Using Bei Shide, 3H-2000PS4 types specific surface area and Porosimetry are to the class graphene-structured of above-mentioned gained
Ordered mesoporous silica dioxide super-thin sheet-shaped material is measured, specific surface area 820m2/ g, aperture 3.9nm, pore volume are
0.88cm3/g。
Above-mentioned embodiment is only a preferred solution of the present invention, not the present invention is made in any form
Limitation, on the premise of not exceeding the technical scheme recorded in the claims also other variations and modifications.
Claims (9)
1. the preparation method of the ordered mesoporous silica dioxide super-thin sheet-shaped material of a type graphene-structured, it is characterised in that the party
Method includes the following steps：
（a）Block copolymer surfactant is dissolved in ethanol solution and adjusts pH value to 0.2-3.0 with acid solution, is then added
Enter ethyl orthosilicate to stir to form uniform mesopore silicon oxide precursor solution, wherein block copolymer surfactant and positive silicon
The mass ratio of acetoacetic ester is 0.2-1.2：1；
（b）By step（a）The mesopore silicon oxide precursor solution of preparation is ground with melamine hard template, obtains mesopore silicon oxide
Then the mixture of mesopore silicon oxide presoma and melamine is placed in culture dish by the mixture of presoma and melamine
It is evaporated induction self assembly at room temperature and obtains solid powder；
（c）By step（b）The first calcination processing hot under nitrogen atmosphere of the solid powder of preparation, then switches under air atmosphere again
Heat treatment removal organic formwork is carried out, the ordered mesoporous silica dioxide that class graphene-structured is can be obtained after natural cooling cooling is super
Lamellar material.
2. preparation method according to claim 1, it is characterised in that：Step（a）In, the block copolymer surfactant
Agent is P123（EO20PO70EO20）, F127（EO106PO70EO106）One or both of mixture.
3. preparation method according to claim 1, it is characterised in that：Step（a）In, the acid solution is nitric acid or salt
The aqueous solution of acid, a concentration of 0.5-2 mol/L.
4. preparation method according to claim 1, it is characterised in that：Step（b）Described in mesopore silicon oxide presoma
The mass ratio of solution and melamine is 1-5：1.
5. preparation method according to claim 1, it is characterised in that：Step（b）Described in evaporation-induced self-assembly when
Between be 6-24 h.
6. preparation method according to claim 1, it is characterised in that：Step（c）Described in solid powder in nitrogen atmosphere
It is 400-600 DEG C to enclose middle hot calcination temperature, calcination time 1-8h.
7. preparation method according to claim 1, it is characterised in that：Step（c）Described in solid powder in air atmosphere
It is 500-800 DEG C to enclose middle heat treatment temperature, calcination time 2-10h.
8. preparation method according to claim 1, it is characterised in that：Block copolymer surfactant and ethyl orthosilicate
Mass ratio be 0.4-0.8:1.
9. a kind of preparation of the ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured according to claim 1
Ordered mesoporous silica dioxide super-thin sheet-shaped material made from method.
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| CN113769703A (en) * | 2021-08-20 | 2021-12-10 | 绍兴蓝竹新材料科技有限公司 | Preparation method of amino functionalized ordered mesoporous silica adsorbent |
| CN114572989A (en) * | 2022-05-06 | 2022-06-03 | 北洋研创(天津)科技有限公司 | Silicon dioxide nanosheet and preparation method and laminated structure thereof |
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| CN205106377U (en) * | 2015-09-25 | 2016-03-30 | 河南中烟工业有限责任公司 | Add aerobic fossil china ink alkene - mesoporous silica combined material's cigarette filter rod |
| CN107541208A (en) * | 2017-08-21 | 2018-01-05 | 徐州医科大学 | A kind of preparation method of hud typed graphene quantum dot@mesopore silicon dioxide nano materials |
| CN108439419A (en) * | 2018-04-02 | 2018-08-24 | 深圳元颉新材料科技有限公司 | Preparation method of mesoporous silica nano hemispherical material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113769703A (en) * | 2021-08-20 | 2021-12-10 | 绍兴蓝竹新材料科技有限公司 | Preparation method of amino functionalized ordered mesoporous silica adsorbent |
| CN114572989A (en) * | 2022-05-06 | 2022-06-03 | 北洋研创(天津)科技有限公司 | Silicon dioxide nanosheet and preparation method and laminated structure thereof |
| CN114572989B (en) * | 2022-05-06 | 2022-09-16 | 北洋研创(天津)科技有限公司 | Silicon dioxide nanosheet and preparation method and laminated structure thereof |
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