CN108545751B - 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
- Publication number
- CN108545751B CN108545751B CN201810757986.5A CN201810757986A CN108545751B CN 108545751 B CN108545751 B CN 108545751B CN 201810757986 A CN201810757986 A CN 201810757986A CN 108545751 B CN108545751 B CN 108545751B
- Authority
- CN
- China
- Prior art keywords
- preparation
- structured
- melamine
- thin sheet
- silica dioxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Carbon And Carbon Compounds (AREA)
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 preparation 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, in particular 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 preparation technical field.
Background technique
From Univ Manchester UK An Deliegaimu professors in 2010 and Constantine Nuo Woxiao love because in stone
Brilliant 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 catalysis, absorption, sensing, drug delivery and in terms of have
Wide application prospect.Ordered meso-porous silicon oxide material generallys use the preparation of surfactant soft template method, i.e., first that surface is living
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 mesoporous material in the application 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 has great research
And practical value.
Summary of the invention
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 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 of step (a) preparation and melamine hard template are ground, 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) by the first calcination processing hot under nitrogen atmosphere of the solid powder of step (b) preparation, air atmosphere is then switched to again
Heat treatment removal organic formwork is carried out under enclosing, and the order mesoporous titanium dioxide of class graphene-structured can be obtained after natural cooling cooling
Silicon super-thin sheet-shaped material.
Preferably, the block copolymer surfactant is P123 (EO in step (a)20PO70EO20), F127
(EO106PO70EO106) one or both of mixture.
Preferably, the acid solution is the aqueous solution of nitric acid or hydrochloric acid, concentration 0.5-2mol/L in step (a).
Preferably, the mass ratio of 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 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 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 preparation method of the 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 present invention are: the ordered mesoporous silica dioxide of type graphene-structured provided by the invention is ultra-thin
Flaky material not only with 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 resulting class graphene-structured of the present invention has higher ratio
Surface area and bigger pore volume make it have broader practice prospect in fields such as absorption, separation, catalysis.
Detailed description of the invention
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 embodiment
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 by 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 surfactant is dissolved in 15mL ethanol solution and with the HNO of 1mol/L3
PH value is adjusted to 0.5,4.2g ethyl orthosilicate is then added and continuously stirs to form uniform mesopore silicon oxide precursor solution.
(2), mesopore silicon oxide precursor solution and 20g melamine hard template 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), the solid powder for preparing step 2 is transferred to tube furnace first when being warming up to 500 DEG C of calcinings under nitrogen atmosphere
Between 3h, then switch to again and be warming up to 550 DEG C of remaining organic formworks of heat treatment 10h removal, natural cooling drop under air atmosphere
The ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured can be obtained in temperature.
Using Bei Shide, 3H-2000PS4 type specific surface area and Porosimetry are to above-mentioned resulting class graphene-structured
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 the class graphene-structured of this implementation preparation
(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 obvious 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 surfactant is dissolved in 15mL ethanol solution and with the HNO of 2mol/L3
PH value is adjusted to 1.2,6.8g ethyl orthosilicate is then added and continuously stirs to form uniform mesopore silicon oxide precursor solution.
(2), mesopore silicon oxide precursor solution and 16g melamine hard template 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), the solid powder for preparing step 2 is transferred to tube furnace first when being warming up to 550 DEG C of calcinings under nitrogen atmosphere
Between 4h, then switch to again and be warming up to 600 DEG C of remaining organic formworks of heat treatment 6h removal, natural cooling cooling under air atmosphere
The ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured can be obtained.
Using Bei Shide, 3H-2000PS4 type specific surface area and Porosimetry are to above-mentioned resulting class graphene-structured
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 surfactant is dissolved in 15mL ethanol solution and with the HCl of 0.5mol/L
PH value is adjusted to 1.8,4.8g ethyl orthosilicate is then added and continuously stirs to form uniform mesopore silicon oxide precursor solution.
(2), mesopore silicon oxide precursor solution and 12g melamine hard template 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), the solid powder for preparing step 2 is transferred to tube furnace first when being warming up to 450 DEG C of calcinings under nitrogen atmosphere
Between 7h, then switch to again and be warming up to 650 DEG C of remaining organic formworks of heat treatment 4h removal, natural cooling cooling under air atmosphere
The ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured can be obtained.
Using Bei Shide, 3H-2000PS4 type specific surface area and Porosimetry are to above-mentioned resulting class graphene-structured
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 surfactant is dissolved in 15mL ethanol solution and with the HCl tune of 2mol/L
PH value is saved to 2.5,7.6g ethyl orthosilicate is then added and continuously stirs to form uniform mesopore silicon oxide precursor solution.
(2), mesopore silicon oxide precursor solution and 10g melamine hard template 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), the solid powder for preparing step 2 is transferred to tube furnace first when being warming up to 600 DEG C of calcinings under nitrogen atmosphere
Between 2h, then switch to again and be warming up to 700 DEG C of remaining organic formworks of heat treatment 2h removal, natural cooling cooling under air atmosphere
The ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured can be obtained.
Using Bei Shide, 3H-2000PS4 type specific surface area and Porosimetry are to above-mentioned resulting class graphene-structured
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 surfactant is 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 orthosilicate is then added and continuously stirs to form uniform Jie
Hole siliconoxide precursor solution.
(2), it grinds mesopore silicon oxide precursor solution and 8g melamine hard template 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), the solid powder for preparing step 2 is transferred to tube furnace first when being warming up to 550 DEG C of calcinings under nitrogen atmosphere
Between 5h, then switch to again and be warming up to 750 DEG C of remaining organic formworks of heat treatment 2h removal, natural cooling cooling under air atmosphere
The ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured can be obtained.
Using Bei Shide, 3H-2000PS4 type specific surface area and Porosimetry are to above-mentioned resulting class graphene-structured
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 surfactant is dissolved in 15mL ethanol solution
In and with the HCl of 2mol/L adjust pH value to 1.5,8g ethyl orthosilicate is then added and continuously stirs to form uniform mesoporous oxidation
Silicon precursor solution.
(2), it grinds mesopore silicon oxide precursor solution and 8g melamine hard template 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), the solid powder for preparing step 2 is transferred to tube furnace first when being warming up to 600 DEG C of calcinings under nitrogen atmosphere
Between 2h, then switch to again and be warming up to 800 DEG C of remaining organic formworks of heat treatment 2h removal, natural cooling cooling under air atmosphere
The ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured can be obtained.
Using Bei Shide, 3H-2000PS4 type specific surface area and Porosimetry are to above-mentioned resulting class graphene-structured
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 surfactant is dissolved in 15mL ethanol solution
In and with the HNO of 2mol/L3PH value is adjusted to 0.2,2g ethyl orthosilicate is then added and continuously stirs to form uniform mesoporous oxygen
SiClx precursor solution.
(2), it grinds mesopore silicon oxide precursor solution and 5g melamine hard template 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), the solid powder for preparing step 2 is transferred to tube furnace first when being warming up to 400 DEG C of calcinings under nitrogen atmosphere
Between 8h, then switch to again and be warming up to 500 DEG C of remaining organic formworks of heat treatment 10h removal, natural cooling drop under air atmosphere
The ordered mesoporous silica dioxide super-thin sheet-shaped material of class graphene-structured can be obtained in temperature.
Using Bei Shide, 3H-2000PS4 type specific surface area and Porosimetry are to above-mentioned resulting class graphene-structured
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, there are also other variations and modifications on the premise of not exceeding the technical scheme recorded in the claims.
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, then plus
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) the mesopore silicon oxide precursor solution of step (a) preparation and melamine hard template are ground, 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) it by the first calcination processing hot under nitrogen atmosphere of the solid powder of step (b) preparation, then switches under air atmosphere again
Heat treatment removal organic formwork is carried out, the ordered mesoporous silica dioxide that class graphene-structured can be obtained after natural cooling cooling is super
Lamellar material.
2. preparation method according to claim 1, it is characterised in that: in step (a), 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: in step (a), the acid solution is nitric acid or salt
The aqueous solution of acid, concentration are 0.5-2 mol/L.
4. preparation method according to claim 1, it is characterised in that: mesopore silicon oxide presoma described in step (b)
The mass ratio of solution and melamine is 1-5:1.
5. preparation method according to claim 1, it is characterised in that: when evaporation-induced self-assembly described in step (b)
Between be 6-24 h.
6. preparation method according to claim 1, it is characterised in that: solid powder described in step (c) is in nitrogen atmosphere
Enclosing middle hot calcination temperature is 400-600 DEG C, calcination time 1-8h.
7. preparation method according to claim 1, it is characterised in that: solid powder described in step (c) is in air atmosphere
Enclosing middle heat treatment temperature is 500-800 DEG C, 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810757986.5A CN108545751B (en) | 2018-07-11 | 2018-07-11 | Ordered mesoporous silica dioxide super-thin sheet-shaped material of one type graphene-structured and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810757986.5A CN108545751B (en) | 2018-07-11 | 2018-07-11 | Ordered mesoporous silica dioxide super-thin sheet-shaped material of one type graphene-structured and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108545751A CN108545751A (en) | 2018-09-18 |
| CN108545751B true CN108545751B (en) | 2019-10-08 |
Family
ID=63492140
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810757986.5A Active CN108545751B (en) | 2018-07-11 | 2018-07-11 | Ordered mesoporous silica dioxide super-thin sheet-shaped material of one type graphene-structured and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108545751B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113769703B (en) * | 2021-08-20 | 2024-07-12 | 绍兴蓝竹新材料科技有限公司 | Preparation method of amino-functionalized ordered mesoporous silica adsorbent |
| 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 |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102909005B (en) * | 2012-10-24 | 2014-02-05 | 中国科学院理化技术研究所 | Graphene-based composite material with surface coated with mesoporous silica and loaded with precious metal nanoparticles, and preparation method and application thereof |
| CN104155357B (en) * | 2014-05-23 | 2015-08-19 | 济南大学 | The preparation method of a kind of three-dimensional cubic duct mesoporous silicon oxide sensor and application |
| US20180065859A1 (en) * | 2015-03-19 | 2018-03-08 | The Regents Of The University Of California | Silica nanostructures, large-scale fabrication methods, and applications thereof |
| 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 |
| CN107541208B (en) * | 2017-08-21 | 2020-08-14 | 徐州医科大学 | Preparation method of core-shell graphene quantum dot @ mesoporous silica nanomaterial |
| CN108439419B (en) * | 2018-04-02 | 2019-11-12 | 深圳元颉新材料科技有限公司 | Preparation method of mesoporous silica nano hemispherical material |
-
2018
- 2018-07-11 CN CN201810757986.5A patent/CN108545751B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN108545751A (en) | 2018-09-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Chen et al. | Preparation and characterization of ZrO2: Eu3+ phosphors | |
| CN107151029B (en) | A kind of sol-gel self-combustion synthesis preparation process of tetra phase barium titanate powder | |
| CN101935877B (en) | Method for synthesizing mullite whiskers by normal pressure sintering | |
| CN108545751B (en) | Ordered mesoporous silica dioxide super-thin sheet-shaped material of one type graphene-structured and preparation method thereof | |
| Liu et al. | A simple and efficient synthetic route for preparation of NaYF 4 upconversion nanoparticles by thermo-decomposition of rare-earth oleates | |
| CN101153051A (en) | Ordered mesoporous material with ultra-large bore diameter and method of producing the same | |
| CN104211388B (en) | One is suitable for low sintering M-type strontium ferrite SrFe 12o 19preparation method | |
| CN108339562B (en) | Preparation method of iron ion doped carbon nitride nanotube and obtained product | |
| CN104292236A (en) | Preparation method of three-dimensional porous g-C3N4 material | |
| CN108706637A (en) | A kind of preparation method of the adjustable magnetic iron oxide mesomorphic material of size uniform | |
| CN102951669B (en) | Method for preparing CeO2 nano solid spheres by microwave-assisted urea hydrolysis | |
| CN104973615A (en) | Microwave burning preparation method of nano gadolinium oxide powder | |
| CN101891209A (en) | Method for preparing nano powder of spherical silicon dioxide | |
| CN102502821A (en) | Mixed organic solvent-thermal method for preparing spherical or hollow spherical BiVO4 | |
| CN104495944A (en) | Method for preparing nitrogen-doped bismuth ferrite nano powder | |
| Wu et al. | Microwave hydrothermal synthesis of boehmite hollow microspheres | |
| CN105036148B (en) | Preparation method for flowerlike Li2Si2O5 powder | |
| CN104477976A (en) | Preparation method of calcium titanate powder with controllable micro/nano structures | |
| Wang et al. | An innovative process for synthesis of superfine nanostructured Li2TiO3 tritium breeder ceramic pebbles via TBOT hydrolysis–solvothermal method | |
| CN101891210A (en) | Preparation method of nano silicon dioxide powder | |
| CN105236468B (en) | Alumina doped mesoporous zinc oxide material with uniform duct and preparation method thereof | |
| Zhang et al. | Sol–gel synthesis of titania hollow spheres | |
| CN108046217A (en) | The preparation method of nano composite metal oxide | |
| CN101538063B (en) | Method for synthesising mesoporous tin oxide by three-dimensional mesoporous silicon dioxide hard template | |
| CN101774603B (en) | Preparation method of mesoporous magnesium borate microsphere |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20221116 Address after: Room 1923-1, Building 2, Jianan Meidi, Jiaxing Economic and Technological Development Zone, Zhejiang 314000 Patentee after: Jiaxing Qianyi Trading Co.,Ltd. Address before: 314001 No. 56 South Yuexiu Road, Zhejiang, Jiaxing Patentee before: JIAXING University |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20230828 Address after: 314001 Room 102-2-2, Block A, Building 7, No. 36, Changsheng South Road, Jiaxing Economic and Technological Development Zone, Zhejiang Province Patentee after: Jiaxing'an Yijia Intelligent Technology Co.,Ltd. Address before: Room 1923-1, Building 2, Jianan Meidi, Jiaxing Economic and Technological Development Zone, Zhejiang 314000 Patentee before: Jiaxing Qianyi Trading Co.,Ltd. |
|
| TR01 | Transfer of patent right |