CN108408737A - A method of quickly preparing Y type molecular sieve - Google Patents
A method of quickly preparing Y type molecular sieve Download PDFInfo
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- CN108408737A CN108408737A CN201810532833.0A CN201810532833A CN108408737A CN 108408737 A CN108408737 A CN 108408737A CN 201810532833 A CN201810532833 A CN 201810532833A CN 108408737 A CN108408737 A CN 108408737A
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- ball
- molecular sieve
- type molecular
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- ball milling
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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
- C01B39/20—Faujasite type, e.g. type X or Y
- C01B39/24—Type Y
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- 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
Abstract
A method of Y type molecular sieve quickly being prepared, is included the following steps：Weigh suitable aluminum sulfate, it is put into mortar and is adequately ground, load weighted sodium hydroxide is added thereto again, it is stirred mixing using glass bar, after mixing, suitable Ludox and Y type molecular sieve crystal seed are added, said mixture, which is put into ball mill, after stirring carries out ball milling, after ball milling, mixture is isolated from ball grinder, it is put into reaction kettle and carries out crystallization, the reaction time is 0.5 1d, and reaction temperature is 120 150 DEG C, after reaction, product is washed, wherein the additive amount of each reactant presses SiO2：Al2O3：Na2O：H2The molar ratio range of O is 4 15：1：12‑20：50‑100；The addition of crystal seed is the 3% of Ludox quality.This method is simple, manufacturing cost is low and can fast implement the batch preparation of Y type molecular sieve.
Description
Technical field
The present invention relates to a kind of molecular sieve preparation fields, and in particular to a method of quickly preparing Y type molecular sieve.
Background technology
Y type molecular sieve belongs to cubic system, and the skeleton structure with faujasite, space group Fd-3m is tied substantially
Structure unit is β cages.Y type molecular sieve shape is an octahedron, and each vertex is a silicon（Aluminium）Oxygen tetrahedron, adjacent β cages
Between two kinds of new cages are interconnected to form with six oxygen bridges by hexatomic ring, one is hexagon prism cage, volume ratio β cages are small；
Another kind is octahedral zeolite cage, it is to surround the big cage formed by hexagon prism cage and β cages, is the oikocryst cave of Y type molecular sieve.Octahedral
It is connected by twelve-ring between zeolite cages, twelve-ring is the oikocryst hole of octahedral zeolite cage, and aperture is about 0.7-0.9nm.Its
It is widely used in fields such as cracking of oil catalysis, hydrocracking, absorption, separation, fine chemistry and organic syntheses.
Currently, the preparation method about Y type molecular sieve mainly has hydrothermal crystallization method, addition directing agent method, microwave crystallization method
Deng, but above-mentioned preparation method all has some limitations, and such as hydrothermal crystallization method, the silica alumina ratio for the Y type molecular sieve prepared
It is relatively low；Addition directing agent method cost is higher, technique is also more complicated, and post-processing is complicated, needs to consume more detergent；Microwave
Although crystallization method improves reaction efficiency, but its reaction controllability is poor.
Invention content
In view of above-mentioned disadvantage existing in the prior art, the purpose of the present invention is to provide a kind of methods simply, is prepared into
This relatively low, simple and rapid Y type molecular sieve preparation method.
In order to reach foregoing invention purpose, the present invention uses following method.
A method of Y type molecular sieve quickly being prepared, is included the following steps：
Suitable aluminum sulfate is weighed, is put into mortar and is adequately ground, then load weighted sodium hydroxide is added thereto, is made
It is stirred mixing with glass bar, after mixing, adds suitable Ludox and Y type molecular sieve crystal seed, it will be upper after stirring
It states mixture and is put into ball mill and carry out ball milling, after ball milling, mixture is isolated from ball grinder, is put into reaction kettle and carries out
Crystallization, reaction time 0.5-1d, reaction temperature are 120-150 DEG C, after reaction, are washed to product,
Wherein, the additive amount of each reactant presses SiO2：Al2O3：Na2O：H2The molar ratio range of O is 4-15：1：12-20：50-100；It is brilliant
The addition of kind is the 3% of Ludox quality.
Preferably, heretofore described ball mill is planetary ball mill, ball milling speed 200-300rpm, ratio of grinding media to material
It is 2.43, mill ball is zirconia ball.
Compared with prior art, the present invention achieves following beneficial technique effect：
1, we teach preparation method of the seminar about solventless method synthesis of molecular sieve with reference to Zhejiang University Xiao Fengshou, especially
It is that it is published in May, 2018《Accounts of Chemical Research》On related experimental methods, for the first time at
The realizing of work(, which does not add any solvent, can prepare Y type molecular sieve；
2, this method is simple, manufacturing cost is low and can fast implement the batch preparation of Y type molecular sieve.
3, in the present invention, after reaction raw materials mixing, the final product of ball milling pair has a significant impact, we, which analyze, may be
Because mixed reactant passes through ball milling, it is equivalent to and has carried out preliminary pre- crystallization, to be more favorable for subsequent direct crystalline substance
Change process just cannot obtain final target product if omitting this step.
Description of the drawings
The XRD spectrum for the Y type molecular sieve that Fig. 1 present invention is quickly prepared；
The SEM photograph for the Y type molecular sieve that Fig. 2 present invention is quickly prepared.
Specific implementation mode
Embodiment 1
Suitable aluminum sulfate is weighed, is put into mortar and is adequately ground, then load weighted sodium hydroxide is added thereto, is made
It is stirred mixing with glass bar, after mixing, adds suitable Ludox and Y type molecular sieve crystal seed, it will be upper after stirring
It states mixture and is put into ball mill progress ball milling, rotational speed of ball-mill 200rpm, Ball-milling Time 10min；After ball milling, from ball milling
Mixture is isolated in tank, is put into reaction kettle and carries out crystallization, and reaction time 0.5d, reaction temperature is 120 DEG C, reaction
After, product is washed, wherein the additive amount of each reactant presses SiO2：Al2O3：Na2O：H2The molar ratio of O is
4：1：15：80；The addition of crystal seed is the 3% of Ludox quality.
Embodiment 2
Suitable aluminum sulfate is weighed, is put into mortar and is adequately ground, then load weighted sodium hydroxide is added thereto, is made
It is stirred mixing with glass bar, after mixing, adds suitable Ludox and Y type molecular sieve crystal seed, it will be upper after stirring
It states mixture and is put into ball mill progress ball milling, rotational speed of ball-mill 250rpm, Ball-milling Time 8min；After ball milling, from ball milling
Mixture is isolated in tank, is put into reaction kettle and carries out crystallization, and reaction time 0.5d, reaction temperature is 150 DEG C, reaction
After, product is washed, wherein the additive amount of each reactant presses SiO2：Al2O3：Na2O：H2The molar ratio of O is
6：1：16：100；The addition of crystal seed is the 3% of Ludox quality.
Embodiment 3
Suitable aluminum sulfate is weighed, is put into mortar and is adequately ground, then load weighted sodium hydroxide is added thereto, is made
It is stirred mixing with glass bar, after mixing, adds suitable Ludox and Y type molecular sieve crystal seed, it will be upper after stirring
It states mixture and is put into ball mill progress ball milling, rotational speed of ball-mill 250rpm, Ball-milling Time 8min；After ball milling, from ball milling
Mixture is isolated in tank, is put into reaction kettle and carries out crystallization, and reaction time 1d, reaction temperature is 130 DEG C, reaction knot
Shu Hou washs product, wherein the additive amount of each reactant presses SiO2：Al2O3：Na2O：H2The molar ratio of O is 4：
1：15：80；The addition of crystal seed is the 3% of Ludox quality.
Embodiment 4
Suitable aluminum sulfate and ferric nitrate are weighed, is put into mortar and is adequately ground, then load weighted hydrogen is added thereto
Sodium oxide molybdena is stirred mixing using glass bar, after mixing, adds suitable Ludox and Y type molecular sieve crystal seed, stirs
Said mixture is put into ball mill after mixing and carries out ball milling, rotational speed of ball-mill 250rpm, Ball-milling Time 8min；Ball milling terminates
Afterwards, mixture is isolated from ball grinder, is put into reaction kettle and is carried out crystallization, reaction time 1d, reaction temperature 130
DEG C, after reaction, washing is carried out to product and can be obtained Fe-Y molecular sieves, wherein the additive amount of each reactant presses SiO2：
FeO：Al2O3：Na2O：H2The molar ratio of O is 4：0.5：1：15：80；The addition of crystal seed is the 3% of Ludox quality.
Claims (2)
1. a kind of method quickly preparing Y type molecular sieve, it is characterised in that：Include the following steps,
Suitable aluminum sulfate is weighed, is put into mortar and is adequately ground, then load weighted sodium hydroxide is added thereto, is made
It is stirred mixing with glass bar, after mixing, adds suitable Ludox and Y type molecular sieve crystal seed, it will be upper after stirring
It states mixture and is put into ball mill and carry out ball milling, after ball milling, mixture is isolated from ball grinder, is put into reaction kettle and carries out
Crystallization, reaction time 0.5-1d, reaction temperature are 120-150 DEG C, after reaction, are washed to product,
Wherein, the additive amount of each reactant presses SiO2：Al2O3：Na2O：H2The molar ratio range of O is 4-15：1：12-20：50-100；It is brilliant
The addition of kind is the 3% of Ludox quality.
2. according to the method described in claim 1, it is characterized in that：The ball mill is planetary ball mill, ball milling speed
For 200-300rpm, ratio of grinding media to material 2.43, mill ball is zirconia ball.
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| CN201810532833.0A CN108408737A (en) | 2018-05-29 | 2018-05-29 | A method of quickly preparing Y type molecular sieve |
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| CN201810532833.0A CN108408737A (en) | 2018-05-29 | 2018-05-29 | A method of quickly preparing Y type molecular sieve |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111825104A (en) * | 2019-04-18 | 2020-10-27 | 中国科学院大连化学物理研究所 | Method for preparing high-silicon Y molecular sieve by seed crystal method |
| CN113683962A (en) * | 2021-08-31 | 2021-11-23 | 马惠琪 | Preparation method of silicon dioxide grinding and polishing agent |
| CN116102032A (en) * | 2023-02-06 | 2023-05-12 | 淄博恒亿化工科技有限公司 | Preparation method of ZSM-5 molecular sieve |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1354134A (en) * | 2001-10-19 | 2002-06-19 | 中国石油化工股份有限公司 | Method for synthesizing small-grain Y-type molecular sieve |
| US20090036294A1 (en) * | 2004-01-29 | 2009-02-05 | Younes Bouizi | Catalyst in the form of grains comprising an acidic porous core surrounded by a uniform outer layer |
| CN102951656A (en) * | 2012-10-16 | 2013-03-06 | 大连瑞克科技有限公司 | Method for synthesizing even-grained ZSM-5 molecular sieves |
| CN103269978A (en) * | 2010-12-01 | 2013-08-28 | 南方化学Ip股份有限责任公司 | Mechanochemical production of zeolites |
-
2018
- 2018-05-29 CN CN201810532833.0A patent/CN108408737A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1354134A (en) * | 2001-10-19 | 2002-06-19 | 中国石油化工股份有限公司 | Method for synthesizing small-grain Y-type molecular sieve |
| US20090036294A1 (en) * | 2004-01-29 | 2009-02-05 | Younes Bouizi | Catalyst in the form of grains comprising an acidic porous core surrounded by a uniform outer layer |
| CN103269978A (en) * | 2010-12-01 | 2013-08-28 | 南方化学Ip股份有限责任公司 | Mechanochemical production of zeolites |
| CN102951656A (en) * | 2012-10-16 | 2013-03-06 | 大连瑞克科技有限公司 | Method for synthesizing even-grained ZSM-5 molecular sieves |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111825104A (en) * | 2019-04-18 | 2020-10-27 | 中国科学院大连化学物理研究所 | Method for preparing high-silicon Y molecular sieve by seed crystal method |
| CN111825104B (en) * | 2019-04-18 | 2022-08-19 | 中国科学院大连化学物理研究所 | Method for preparing high-silicon Y molecular sieve by seed crystal method |
| CN113683962A (en) * | 2021-08-31 | 2021-11-23 | 马惠琪 | Preparation method of silicon dioxide grinding and polishing agent |
| CN113683962B (en) * | 2021-08-31 | 2022-06-07 | 马惠琪 | Preparation method of silicon dioxide grinding and polishing agent |
| CN116102032A (en) * | 2023-02-06 | 2023-05-12 | 淄博恒亿化工科技有限公司 | Preparation method of ZSM-5 molecular sieve |
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Application publication date: 20180817 |