CN107686378A - Micro- mesoporous composite molecular sieve film and preparation method thereof - Google Patents
Micro- mesoporous composite molecular sieve film and preparation method thereof Download PDFInfo
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- CN107686378A CN107686378A CN201610636426.5A CN201610636426A CN107686378A CN 107686378 A CN107686378 A CN 107686378A CN 201610636426 A CN201610636426 A CN 201610636426A CN 107686378 A CN107686378 A CN 107686378A
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
- C04B41/5031—Alumina
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00793—Uses not provided for elsewhere in C04B2111/00 as filters or diaphragms
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/0081—Uses not provided for elsewhere in C04B2111/00 as catalysts or catalyst carriers
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- Silicates, Zeolites, And Molecular Sieves (AREA)
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Abstract
Micro- mesoporous composite molecular sieve film and preparation method thereof, micro- mesoporous composite molecular sieve film of the present invention, is made up of following raw material:Molecular sieve, aluminum oxide and sol-gel, the molecular sieve and aluminum oxide are solid powder, and molecular sieve has network-like structure, and aluminum oxide has micropore hole wall, and the ratio of molecular sieve, aluminum oxide and sol-gel is 1:1:1‑3:3:4.Present invention additionally comprises preparation method.Micro- mesoporous composite molecular sieve film heat endurance, chemical stability and the biological stability of the present invention is high, realizes integrated reaction and separation;Stability Analysis of Structures, hydrothermal stability is high, and specific surface area is big, more than 1100m2/ g, mesoporous pore size is uniform, and varying aperture has oxidation catalyst filter dual property between 2 50nm;Cost is low, and raw material are easy to get, and the preparation method of the present invention is simple, and equipment investment is few, and the cycle is short, beneficial to reducing cost and industrialized production.
Description
Technical field
The present invention relates to inorganic composite materials field, and in particular to a kind of micro- mesoporous composite molecular sieve film and its preparation side
Method.
Background technology
With the rapid development of every profession and trade, increase therewith for the demand of industrial ceramics product, it is notable that state
Reinforcing of the family to environmental protection policy, the manufacturing enterprise for meeting environmental requirement and scale level have vast potential for future development.In addition, stone
Oil, chemical industry, smelting, medical treatment, pharmacy, the purification of sewage, waste gas caused by food processing and production process are that China's current industrial is given up
The vital task of water, waste gas pollution control and treatment, but conventional filler tower absorption equipment volume is big, and weight is high, cost of manufacture is expensive, and vapour lock
Height, equipment operation energy consumption is big, is to restrict industrial wastewater, the larger obstacle for the treatment of tail gas progress, using high-performance ceramic membrane technology
This obstacle can preferably be overcome.For the present situation of China ceramic industry, it is necessary to carry out the improvement of ceramic production technology, carry out skill
Art is transformed or enterprise transformation, is integrated with international advanced energy consumption level standard, reduces environmental pollution and resources and energy consumption, ensures society
Meeting sustainable development, Speeding Up The Advancement of technology, takes part in international competition, improves the challenge of synthesized competitiveness.Country is formulating " ten
Three or five " when planning and distant view development plan, it has been determined that the actively production policy of the development high-tech ceramic industry of new technology.Progressively
The technique manufacturing enterprise backward with equipment is eliminated, encourages the production technology and equipment using new and high technology, existing enterprise is carried out
Transformation.Firmly contain low-level repeated construction, environmental protection, economize on resources, the development strategy of the Implement of sustainable development.
In recent years, due to mesopore molecular sieve even structure, can modulation pore structure, by the extensive concern of scientific research personnel.
But mesopore molecular sieve has the shortcomings of acid intensity is low, hydrothermal stability is poor, therefore it is not used widely.
The content of the invention
The technical problems to be solved by the invention are to overcome drawbacks described above existing for prior art, there is provided one kind has only
Special orderly physical and chemical performance, and the ratio of intermediary hole and microcellular structure can prepare hydro-thermal by controlling to adjust synthesis condition
Stability is high, specific surface area is big, the uniform composite membrane of mesoporous pore size, solves the problems, such as mesoporous part high hydrothermal stability difference,
The film is sprayed on oxidation aluminium surface, obtains excellent micro- mesoporous composite molecular sieve membrane filter tube, realizes reaction filtering integral
Micro- mesoporous composite molecular sieve film and preparation method thereof.
The technical solution adopted for the present invention to solve the technical problems is,
Micro- mesoporous composite molecular sieve film of the present invention, is made up of following raw material:Molecular sieve, aluminum oxide and sol-gel, described point
Son sieve and aluminum oxide are solid powder, and molecular sieve has network-like structure, and aluminum oxide has micropore hole wall, molecular sieve, oxidation
The ratio of aluminium and sol-gel is 1:1:1-3:3:4.
Further, the sol-gel is the one or more in phosphoric acid, Ludox, organic amine and deionized water.
Further, the solid powder size of the molecular sieve and aluminum oxide is nanoscale or micron order.
The preparation method of micro- mesoporous composite molecular sieve film of the present invention, it is characterised in that comprise the following steps:
(a)The raw material of aforementioned proportion is added in mixer and is well mixed, glue is made;
(b)By step(a)Manufactured glue is sprayed on alumina article surface and film is made;
(c)By step(b)Manufactured overlay film product is first dried in microwave, then carries out high-temperature calcination, high-temperature calcination temperature is
1200℃-1550℃(It is preferred that 1250-1500 DEG C), the high-temperature calcination time is 3-15h, cooling, is surface-treated, then be heat-treated
4-6h, the temperature of heat treatment is 40 DEG C -200 DEG C(It is preferred that 50 DEG C -120 DEG C), room temperature is naturally cooled to, that is, is made micro- composite mesoporous
Molecular screen membrane.
Compared with prior art, the invention has the advantages that:
(1)Micro- mesoporous composite molecular sieve film heat endurance, chemical stability and the biological stability of the present invention is high, has different
The perforated membrane of the high porosity of acid, hydrophily and catalytic performance, because the physical and chemical performance of ordered mesoporous material is unique, this
Kind inoranic membrane has huge application prospect in catalytic field and adsorbing separation, ion-exchange field, realizes Reaction Separation one
Body;
(2)Stability Analysis of Structures, hydrothermal stability is high, and specific surface area is big, typically larger than 1100m2/ g, mesoporous pore size is uniform, and aperture becomes
Change between 2-50nm, there is oxidation catalyst filter dual property;
(3)Cost is low, and raw material are easy to get, and the solid and solvent that the present invention selects all are ceramic convenient sources;
(4)The preparation method of the present invention is simple, and equipment investment is few, and the cycle is short, beneficial to reducing cost and industrialized production.
Embodiment
The invention will be further described with reference to embodiments.
Embodiment 1
Micro- mesoporous composite molecular sieve film of the present embodiment, is made up of following raw material:Molecular sieve, aluminum oxide and sol-gel, it is described
Molecular sieve and aluminum oxide are solid powder, and molecular sieve has network-like structure, and aluminum oxide has micropore hole wall, molecular sieve, oxygen
The ratio for changing aluminium and sol-gel is 1:1:1.
In the present embodiment, the sol-gel is phosphoric acid.
In the present embodiment, the solid powder size of the molecular sieve and aluminum oxide is nanoscale.
The preparation method of micro- mesoporous composite molecular sieve film of the present embodiment, it is characterised in that comprise the following steps:
(a)The raw material of aforementioned proportion is added in mixer and is well mixed, glue is made;
(b)By step(a)Manufactured glue is sprayed on alumina article surface and film is made;
(c)By step(b)Manufactured overlay film product is first dried in microwave, then carries out high-temperature calcination, high-temperature calcination temperature is
1450 DEG C, the high-temperature calcination time is 10h, cooling, is surface-treated, and reheating processing 5h, the temperature of heat treatment is 50 DEG C, natural
Room temperature is cooled to, that is, micro- mesoporous composite molecular sieve film is made.
Micro- mesoporous composite molecular sieve film heat endurance, chemical stability and the biological stability of the present invention is high, has difference
Acidity, hydrophily and catalytic performance high porosity perforated membrane, because the physical and chemical performance of ordered mesoporous material is unique,
This inoranic membrane has huge application prospect in catalytic field and adsorbing separation, ion-exchange field, realizes Reaction Separation
Integration;Stability Analysis of Structures, hydrothermal stability is high, and specific surface area is big, more than 1100m2/ g, mesoporous pore size is uniform, and varying aperture exists
Between 2-50nm, there is oxidation catalyst filter dual property;Cost is low, and raw material are easy to get, and the preparation method of the present invention is simple, and equipment is thrown
Money is few, and the cycle is short, beneficial to reducing cost and industrialized production.
Embodiment 2
Micro- mesoporous composite molecular sieve film of the present embodiment, is made up of following raw material:Molecular sieve, aluminum oxide and sol-gel, it is described
Molecular sieve and aluminum oxide are solid powder, and molecular sieve has network-like structure, and aluminum oxide has micropore hole wall, molecular sieve, oxygen
The ratio for changing aluminium and sol-gel is 3:3:4.
In the present embodiment, the sol-gel is the sol-gel mixed liquor of phosphoric acid and Ludox.
In the present embodiment, the solid powder size of the molecular sieve and aluminum oxide is micron order.
The preparation method of micro- mesoporous composite molecular sieve film of the present embodiment, comprises the following steps:
(a)The raw material of aforementioned proportion is added in mixer and is well mixed, glue is made;
(b)By step(a)Manufactured glue is sprayed on alumina article surface and film is made;
(c)By step(b)Manufactured overlay film product is first dried in microwave, then carries out high-temperature calcination, high-temperature calcination temperature is
1400 DEG C, the high-temperature calcination time is 8h, cooling, is surface-treated, and reheating processing 5h, the temperature of heat treatment is 100 DEG C, natural
Room temperature is cooled to, that is, micro- mesoporous composite molecular sieve film is made.
Micro- mesoporous composite molecular sieve film heat endurance, chemical stability and the biological stability of the present invention is high, has difference
Acidity, hydrophily and catalytic performance high porosity perforated membrane, because the physical and chemical performance of ordered mesoporous material is unique,
This inoranic membrane has huge application prospect in catalytic field and adsorbing separation, ion-exchange field, realizes Reaction Separation
Integration;Stability Analysis of Structures, hydrothermal stability is high, and specific surface area is big, more than 1100m2/ g, mesoporous pore size is uniform, and varying aperture exists
Between 2-50nm, there is oxidation catalyst filter dual property;Cost is low, and raw material are easy to get, and the preparation method of the present invention is simple, and equipment is thrown
Money is few, and the cycle is short, beneficial to reducing cost and industrialized production.
Embodiment 3
Micro- mesoporous composite molecular sieve film of the present embodiment, is made up of following raw material:Molecular sieve, aluminum oxide and sol-gel, it is described
Molecular sieve and aluminum oxide are solid powder, and molecular sieve has network-like structure, and aluminum oxide has micropore hole wall, molecular sieve, oxygen
The ratio for changing aluminium and sol-gel is 3:3:4.
In the present embodiment, the sol-gel is the sol-gel mixing of phosphoric acid, Ludox, organic amine and deionized water
Liquid.
In the present embodiment, the solid powder size of the molecular sieve and aluminum oxide includes nanoscale and micron order.
The preparation method of micro- mesoporous composite molecular sieve film of the present embodiment, comprises the following steps:
(a)The raw material of aforementioned proportion is added in mixer and is well mixed, glue is made;
(b)By step(a)Manufactured glue is sprayed on alumina article surface and film is made;
(c)By step(b)Manufactured overlay film product is first dried in microwave, then carries out high-temperature calcination, high-temperature calcination temperature is
1300 DEG C, the high-temperature calcination time is 6h, cooling, is surface-treated, and reheating processing 5h, the temperature of heat treatment is 60 DEG C, natural
Room temperature is cooled to, that is, micro- mesoporous composite molecular sieve film is made.
Micro- mesoporous composite molecular sieve film heat endurance, chemical stability and the biological stability of the present invention is high, has difference
Acidity, hydrophily and catalytic performance high porosity perforated membrane, because the physical and chemical performance of ordered mesoporous material is unique,
This inoranic membrane has huge application prospect in catalytic field and adsorbing separation, ion-exchange field, realizes Reaction Separation
Integration;Stability Analysis of Structures, hydrothermal stability is high, and specific surface area is big, more than 1100m2/ g, mesoporous pore size is uniform, and varying aperture exists
Between 2-50nm, there is oxidation catalyst filter dual property;Cost is low, and raw material are easy to get, and the preparation method of the present invention is simple, and equipment is thrown
Money is few, and the cycle is short, beneficial to reducing cost and industrialized production.
Claims (5)
1. micro- mesoporous composite molecular sieve film, it is characterised in that be made up of following raw material:Molecular sieve, aluminum oxide and sol-gel, institute
To state molecular sieve and aluminum oxide is solid powder, molecular sieve has a network-like structure, and aluminum oxide has a micropore hole wall, molecular sieve,
The ratio of aluminum oxide and sol-gel is 1:1:1-3:3:4.
2. micro- mesoporous composite molecular sieve film according to claim 1, it is characterised in that the sol-gel is phosphoric acid, silicon
One or more in colloidal sol, organic amine and deionized water.
3. micro- mesoporous composite molecular sieve film according to claim 1 or 2, it is characterised in that the molecular sieve and aluminum oxide
Solid powder size be nanoscale or micron order.
4. a kind of preparation method of micro- mesoporous composite molecular sieve film as described in any one of claim 1-3 claim, it is special
Sign is, comprises the following steps:
(a)The raw material of aforementioned proportion is added in mixer and is well mixed, glue is made;
(b)By step(a)Manufactured glue is sprayed on alumina article surface and film is made;
(c)By step(b)Manufactured overlay film product is first dried in microwave, then carries out high-temperature calcination, high-temperature calcination temperature is
1200 DEG C -1550 DEG C, the high-temperature calcination time is 3-15h, cooling, is surface-treated, reheating processing 4-6h, the temperature of heat treatment
For 40 DEG C -200 DEG C, room temperature is naturally cooled to, that is, micro- mesoporous composite molecular sieve film is made.
5. the preparation method of micro- mesoporous composite molecular sieve film according to claim 4, it is characterised in that the step(c)
In, high-temperature calcination temperature is 1250 DEG C -1500 DEG C, and the temperature of heat treatment is 50 DEG C -120 DEG C.
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103372379A (en) * | 2013-07-14 | 2013-10-30 | 浙江大学 | Preparation method of molecular sieve composite membrane by taking metallic oxide as carrier |
CN104785289A (en) * | 2015-03-14 | 2015-07-22 | 桂林理工大学 | Preparation method of molecular sieve coating layer on metal carrier |
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2016
- 2016-08-05 CN CN201610636426.5A patent/CN107686378A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103372379A (en) * | 2013-07-14 | 2013-10-30 | 浙江大学 | Preparation method of molecular sieve composite membrane by taking metallic oxide as carrier |
CN104785289A (en) * | 2015-03-14 | 2015-07-22 | 桂林理工大学 | Preparation method of molecular sieve coating layer on metal carrier |
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