CN114873603B - Photo-induced self-assembly synthesis method of one-dimensional mesoporous composite molecular sieve material - Google Patents
Photo-induced self-assembly synthesis method of one-dimensional mesoporous composite molecular sieve material Download PDFInfo
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- CN114873603B CN114873603B CN202210562771.4A CN202210562771A CN114873603B CN 114873603 B CN114873603 B CN 114873603B CN 202210562771 A CN202210562771 A CN 202210562771A CN 114873603 B CN114873603 B CN 114873603B
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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 39
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 239000000463 material Substances 0.000 title claims abstract description 30
- 238000001338 self-assembly Methods 0.000 title claims abstract description 22
- 238000001308 synthesis method Methods 0.000 title claims abstract description 9
- 229960000892 attapulgite Drugs 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 25
- 229910052625 palygorskite Inorganic materials 0.000 claims abstract description 25
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 15
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 14
- 239000006185 dispersion Substances 0.000 claims abstract description 11
- 239000011521 glass Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims description 16
- -1 polydimethylsiloxane Polymers 0.000 claims description 13
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- 229910000077 silane Inorganic materials 0.000 claims description 8
- 238000005286 illumination Methods 0.000 claims description 7
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 abstract description 10
- 238000007747 plating Methods 0.000 abstract 1
- 239000011148 porous material Substances 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000002444 silanisation Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
- C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Composite Materials (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention relates to the field of synthesis of molecular sieve materials, and discloses a photoinduced self-assembly synthesis method of a one-dimensional mesoporous composite molecular sieve material. Under the condition of 30-100% humidity, the high-dispersion film-plating gel is uniformly coated on a glass slide, the thickness of a liquid film is 5-10 mu m, and the light-induced self-assembly synthesis of the one-dimensional mesoporous composite molecular sieve material is realized by irradiation of an ultraviolet light source. The invention can construct mesoporous molecular sieve shell layer on the surface of one-dimensional attapulgite in one step without using any additional structure directing agent, and the synthesized one-dimensional mesoporous composite molecular sieve material has the advantages of large specific surface area, adjustable mesoporous aperture, high composite degree and the like.
Description
Technical Field
The invention relates to the field of synthesis of one-dimensional mesoporous composite molecular sieve materials, in particular to a photoinduced self-assembly synthesis method for preparing a mesoporous composite molecular sieve material by taking one-dimensional attapulgite as a hard template to replace a mesoporous structure guiding agent.
Background
Because the mesoporous molecular sieve has larger specific surface area and adjustable aperture, the mesoporous molecular sieve is often used as a carrier of a catalyst, and in order to further improve the catalytic activity of the catalyst, mesoporous composite technology, pore wall thickness increasing technology and silanization hydrophobic technology are generally adopted to improve the stability of the molecular sieve. Wherein the mesoporous and microporous composite can directly improve the physical and chemical stability of the catalyst. Common synthesis methods of mesoporous and microporous composite include a nano assembly method, a pore wall crystallization method, a soft template agent method and a hard template agent method. The hard template method has the advantages of simple operation, stable structure, easy realization and the like. The traditional mesoporous molecular sieve is synthesized by introducing a surfactant such as P123 as a structure directing agent to induce the hydrolytic polymerization of silane and removing a template agent. Then, the mesoporous and microporous composite of the molecular sieve is realized by means of nano assembly, hole wall crystallization and the like. The method has the advantages of complex operation process, difficult parameter control, long reaction period and huge energy consumption.
Disclosure of Invention
The invention aims to: aiming at the problems in the prior art, the invention provides a photoinduced self-assembly synthesis method of a one-dimensional mesoporous composite molecular sieve material. The invention can realize the synthesis of the mesoporous molecular sieve material in one step, and the synthesis strategy is that a mesoporous shell layer is constructed on the surface of the attapulgite by a photoinduction self-assembly method, so that the mesoporous composite is realized in one step. The one-step photoinduction self-assembly synthesis of the one-dimensional mesoporous composite molecular sieve material has the advantages of high synthesis speed, adjustable thickness and aperture of a mesoporous shell layer, capability of being carried out at normal temperature and normal pressure, and the like.
The technical scheme is as follows: the invention provides a photoinduced self-assembly synthesis method of a one-dimensional mesoporous composite molecular sieve material, which comprises the following steps: s1: the attapulgite is treated with,The neutral silane and the photoacid generator PAG are prepared into a high-dispersion coating gel; wherein the mass ratio of the attapulgite to the neutral silane to the photoacid generator PAG is 10-25:60-130:1-5; s2: uniformly coating the film-coated gel on a glass sheet to form a layer of liquid film with the thickness of 5-10 mu m; s3, in a narrow wave band with a wave band of 310-400nm, the illumination intensity is 4-6 mW/cm 2 Under the illumination condition, the liquid film is irradiated for 1-20min, thus realizing the photoinduction self-assembly synthesis of the one-dimensional mesoporous composite molecular sieve material.
Preferably, the neutral silane is polydimethylsiloxane PDMOS.
Preferably, each step is carried out under an environment of normal temperature and pressure of 30-100% humidity.
Preferably, the attapulgite clay is attapulgite clay.
Preferably, the photoacid generator PAG is diphenyliodonium hexafluorophosphate.
The beneficial effects are that: the invention provides a photoinduction self-assembly synthesis method of a one-dimensional mesoporous composite molecular sieve material, which takes attapulgite as a hard template and successfully builds a mesoporous shell layer on the surface of the attapulgite by a photoinduction self-assembly method. The preparation of the one-dimensional mesoporous composite molecular sieve material with the attapulgite surface coated with the mesoporous molecular sieve shell layer is realized. The preparation of the one-dimensional mesoporous composite molecular sieve material is that an acidic substance is generated by using a photoacid generator PAG under the irradiation of ultraviolet light to induce the silane to carry out hydrolytic polymerization, so that the surface of the attapulgite is coated with a mesoporous shell layer with a regular pore structure.
The one-dimensional mesoporous composite molecular sieve material prepared by the invention has the advantages of high synthesis rate, high order degree of mesoporous shell layers, controllable optical parameters, realization at normal temperature and normal pressure and the like. According to the invention, the parameters such as mesoporous shell layer, mesoporous shell layer aperture and mesoporous shell layer thickness are accurately regulated and controlled by regulating the proportion of the raw materials such as attapulgite, PDMOS, PAG and the like.
The invention provides abundant micropore channels for the composite material by using the attapulgite, provides a structure guiding agent for the formation of the mesoporous molecular sieve by using the attapulgite as a hard template agent, eliminates the defect that the structure guiding property of the conventional template agent is difficult to control, and simultaneously achieves the functions of capacity expansion and reaming. The attapulgite is used as a hard template agent, and the stronger adsorption effect of the attapulgite is utilized, so that the composite material can have better performance in the fields of adsorption catalysis and the like. The mesoporous molecular sieve shell layer with high specific surface and the micropore pore canal inside the shell layer cooperate with each other to provide a reaction container for catalytic reaction, fully exert the synergistic effect of the micropore structure of the attapulgite and the mesoporous pore canal of the mesoporous molecular sieve, and the abundant pore canal structure is beneficial to rapid in-out of reactants and products and forward generation of catalytic reaction.
When the one-dimensional mesoporous composite molecular sieve material is prepared, the pore channel order of the composite material can be increased by increasing the amount of attapulgite, and the specific surface area and the pore size of the composite material are effectively improved. Therefore, the order of the specific surface and mesoporous shell pore canal of the material and the pore size thereof can be regulated by regulating the dosage of the attapulgite.
Drawings
FIG. 1 is a flow chart of a photo-induced self-assembly synthesis process of a one-dimensional mesoporous composite molecular sieve material.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
Embodiment 1:
uniformly mixing 0.1g of attapulgite, 0.04g of diphenyl iodonium hexafluorophosphate and 1.1g of polydimethylsiloxane in a brown glass bottle to obtain high-dispersion coated gel;
uniformly coating the dispersion liquid on a glass sheet under the condition of 60% of humidity to form a uniform liquid film, wherein the thickness of the liquid film is controlled to be 5-10 mu m;
transferring the liquid film into an environment with humidity of 30%, and using a narrow band with wavelength of 310nm and intensity of 5 mW/cm 2 The ultraviolet irradiation liquid film is reacted for 5 min; the preparation of the one-dimensional mesoporous composite molecular sieve material can be completed by a one-step photoinduction self-assembly method.
Embodiment 2:
uniformly mixing 0.2g of attapulgite, 0.04g of diphenyl iodonium hexafluorophosphate and 1.1g of polydimethylsiloxane in a brown glass bottle to obtain high-dispersion coated gel;
uniformly coating the dispersion liquid on a glass plate under the condition of 60% of humidity to form a uniform liquid film, wherein the thickness of the liquid film is controlled to be 5-10 mu m;
transferring the liquid film into an environment with humidity of 30%, and using a narrow band with wavelength of 310nm and intensity of 5 mW/cm 2 The ultraviolet irradiation liquid film is reacted for 5 min; the preparation of the one-dimensional mesoporous composite molecular sieve material can be completed by a one-step photoinduction self-assembly method.
Embodiment 3:
uniformly mixing 0.1g of attapulgite, 0.03g of diphenyl iodonium hexafluorophosphate and 1.1g of polydimethylsiloxane in a brown glass bottle to obtain high-dispersion coated gel;
uniformly coating the dispersion liquid on a glass plate under the condition of 60% of humidity to form a uniform liquid film, wherein the thickness of the liquid film is controlled to be 5-10 mu m;
transferring the liquid film into an environment with humidity of 30%, and using a narrow band with wavelength of 310nm and intensity of 5 mW/cm 2 The ultraviolet irradiation liquid film is reacted for 5 min; the preparation of the one-dimensional mesoporous composite molecular sieve material can be completed by a one-step photoinduction self-assembly method.
Embodiment 4:
uniformly mixing 0.1g of attapulgite, 0.04g of diphenyl iodonium hexafluorophosphate and 1.2g of polydimethylsiloxane in a brown glass bottle to obtain high-dispersion coated gel;
uniformly coating the dispersion liquid on a glass plate under the condition of 60% of humidity to form a uniform liquid film, wherein the thickness of the liquid film is controlled to be 5-10 mu m;
transferring the liquid film into an environment with humidity of 30%, and using a narrow band with wavelength of 310nm and intensity of 5 mW/cm 2 The ultraviolet irradiation liquid film is reacted for 5 min; the preparation of the one-dimensional mesoporous composite molecular sieve material can be completed by a one-step photoinduction self-assembly method.
Embodiment 5:
the present embodiment is substantially the same as embodiment 1, and differs from this embodiment only in that the humidity environment at the time of illumination is 50%.
Embodiment 6:
the present embodiment is substantially the same as embodiment 1, and differs from this embodiment only in that the illumination wavelength is a narrow band of 360 nm.
Embodiment 7:
the present embodiment is substantially the same as embodiment 1, except that the illumination intensity is different from the present embodiment in that the lighting intensity is 10 mW/cm 2 。
The performance parameters of the low-valence metal doped one-dimensional mesoporous composite molecular sieve materials prepared in the above embodiments 1 to 7 are as follows:
the foregoing embodiments are merely illustrative of the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the present invention and to implement the same, not to limit the scope of the present invention. All equivalent changes or modifications made according to the spirit of the present invention should be included in the scope of the present invention.
Claims (4)
1. A light-induced self-assembly synthesis method of a one-dimensional mesoporous composite molecular sieve material is characterized by comprising the following steps:
s1: preparing attapulgite, neutral silane and a photoacid generator PAG into high-dispersion coating gel; wherein the mass ratio of the attapulgite to the neutral silane to the photoacid generator PAG is 10-25:60-130:1-5;
s2: uniformly coating the film-coated gel on a glass sheet to form a layer of liquid film with the thickness of 5-10 mu m;
s3, in a narrow wave band with a wave band of 310-400nm, the illumination intensity is 4-6 mW/cm 2 Under the illumination condition, the liquid film is irradiated for 1-20min, thus realizing the photoinduction self-assembly synthesis of the one-dimensional mesoporous composite molecular sieve material.
2. The method for photoinduced self-assembly synthesis of a one-dimensional mesoporous composite molecular sieve material according to claim 1, wherein the neutral silane is polydimethylsiloxane PDMOS.
3. The method for photo-induced self-assembly synthesis of one-dimensional mesoporous composite molecular sieve material according to claim 1, wherein each step is performed under the environment of normal temperature and normal pressure with humidity of 30-100%.
4. The method for photoinduced self-assembly synthesis of a one-dimensional mesoporous composite molecular sieve material according to claim 1, wherein the photoacid generator PAG is diphenyliodonium hexafluorophosphate.
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Application publication date: 20220809 Assignee: XUYI OUBAITE CLAY MATERIALS Co.,Ltd. Assignor: HUAIYIN INSTITUTE OF TECHNOLOGY Contract record no.: X2023980053928 Denomination of invention: Photoinduced self-assembly synthesis method of one-dimensional mesoporous composite molecular sieve materials Granted publication date: 20230929 License type: Common License Record date: 20231225 |