CN106315611A - SSZ -13 molecular sieve preparing method - Google Patents
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- CN106315611A CN106315611A CN201610708823.9A CN201610708823A CN106315611A CN 106315611 A CN106315611 A CN 106315611A CN 201610708823 A CN201610708823 A CN 201610708823A CN 106315611 A CN106315611 A CN 106315611A
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- 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
- C01B39/04—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 using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound
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- 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
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
The invention discloses a SSZ -13 molecular sieve preparing method comprising the steps of (1) evenly mixing and putting N,N,N- trimethyl adamantane ammonium hydroxide and crystal growth agent into high-pressure reaction kettle, then adding silicon source, aluminium source and water successively into it and obtaining initial gel after mixing; (2) crystallizing the initial gel obtained in step (1) under 155-175oC for 17-72 hours and obtaining crystallized product; (3) centrifugalizing the crystallized product obtained in step (2) to obtain filter cake and filtrate, washing the obtained filter cake by deionized water to pH 7-8, then drying it for 10-13 hours under 100-120oC to obtain the SSZ -13 molecular sieve; the SSZ -13 molecular sieve preparing method in the invention may realize the free modulation for partical size of SSZ -13 molecular sieve from 0. 3-17Mum through adding crystal growth agent; the addition of crystal growth agent in the invention makes more even dispersion of molecular sieve crystal.
Description
Technical field
The present invention relates to technical field of molecular sieve, specifically the preparation method of SSZ-13 molecular sieve.
Background technology
SSZ-13 molecular sieve has elliposoidal cage and the three dimensional intersection pore passage structure of octatomic ring structure, and its specific surface area is the highest
Can reach 700m2/ g, owing to its tradable cation and surface plasmon acid centre are many, thus is often used as adsorbent or urges
Agent, but the template that synthesis SSZ-13 molecular sieve is conventional at present is N, N, N-trimethyl diamantane (obsolete) ammonium hydroxide SDA, price
Costliness, seriously constrains its process of industrialization, the synthesis cost of SSZ-13 molecular sieve, is restriction SSZ-13 molecular sieve commercial production
Principal element.For molecular sieve, size is a critically important quality index, and usual small particle molecular sieve is by relatively
Good micropore diffusion ability and there is of a relatively high reactivity, but there is the problem separating difficulty；Big particle diameter molecular sieve leads to
Paradoxical reaction activity is the highest, but is easily isolated.How to take into account the separation in catalytic performance and real process, certainly will require molecular sieve
Particle size adjustment propose higher requirement.By the end of so far, how the particle diameter to SSZ-13 molecular sieve realizes freely regulating,
There is no open report.
The main method reducing SSZ-13 Zeolite synthesis cost at present is to reduce N, N, N-trimethyl diamantane (obsolete) hydroxide
The use of ammonium, conventional method is to use to find suitable template replacement SDA, as organic formwork agent tetraethyl ammonium hydroxide can
Partly or entirely to substitute the SDA pure phase SSZ-13 molecular sieve of synthesis, but the crystal formation of the SSZ-13 molecular sieve of the method synthesis is relatively
Difference, size is uneven, has had a strong impact on the catalytic performance of molecular sieve.
Summary of the invention
For solving the problems referred to above, it is an object of the invention to provide the preparation method of SSZ-13 molecular sieve.
The present invention for achieving the above object, is achieved through the following technical solutions:
The preparation method of a kind of SSZ-13 molecular sieve, comprises the following steps:
1. by N, N, N-trimethyl diamantane (obsolete) ammonium hydroxide and crystal growth agent mix homogeneously, add in autoclave, then
It is sequentially added into silicon source, aluminum source and water wherein, after stirring, obtains Primogel；N in described Primogel, N, N-trimethyl Buddha's warrior attendant
Alkane ammonium hydroxide: crystal growth agent: SiO2: Al2O3: H2The mol ratio of O is 0.06～0.25:0.00085～0.025:1:
0.017～0.063:20～40；Described crystal growth agent is piperazine；
2. by Primogel crystallization 17 ~ 72 hours at 155 ~ 175 DEG C of step 1. gained, crystallization product is obtained；
3. by the crystallization product centrifugation of step 2. gained, obtain filter cake and filtrate, gained filter cake is washed with deionized
To pH to 7 ~ 8, then it is dried 10 ~ 13 hours at 100 ~ 120 DEG C, obtains SSZ-13 molecular sieve.
Preferably, silicon source is Ludox, white carbon, c-type silica gel or tetraethyl orthosilicate.
Preferably, aluminum source is boehmite, aluminium hydroxide, aluminum sulfate or aluminum isopropylate..
Preferably, N in Primogel, N, N-trimethyl diamantane (obsolete) ammonium hydroxide: crystal growth agent: SiO2: Al2O3: H2O
Mol ratio be 0.15～0.20:0.005～0.01:1:0.02～0.06:25～35.
Preferably, N in Primogel, N, N-trimethyl diamantane (obsolete) ammonium hydroxide: crystal growth agent: SiO2: Al2O3: H2O
Mol ratio be 0.15:0.025:1:0.04:30.
Preferably, 2. step is by Primogel crystallization 24 ~ 60 hours at 160 ~ 170 DEG C of step 1. gained, obtains
Crystallization product.
Preferably, aluminum source is boehmite.
Preferably, silicon source is Ludox.
Further preferred preparation method, comprises the following steps:
1. by N, N, N-trimethyl diamantane (obsolete) ammonium hydroxide and crystal growth agent mix homogeneously, add in autoclave, then
It is sequentially added into silicon source, aluminum source and water wherein, after stirring, obtains Primogel；N in described Primogel, N, N-trimethyl Buddha's warrior attendant
Alkane ammonium hydroxide: crystal growth agent: SiO2: Al2O3: H2The mol ratio of O is 0.15:0.025:1:0.04:30；Described crystal
Growth stimulator is piperazine；Source of aluminium is boehmite；Described silicon source is Ludox；
2. by Primogel crystallization 50 hours at 165 DEG C of step 1. gained, crystallization product is obtained；
3. by the crystallization product centrifugation of step 2. gained, obtain filter cake and filtrate, gained filter cake is washed with deionized
To pH to 7, then it is dried 12 hours at 110 DEG C, obtains SSZ-13 molecular sieve.
The present invention has the advantage that compared to existing technology
The preparation method of the SSZ-13 molecular sieve of the present invention is by adding crystal growth agent so that it is and template N, N, N-trimethyl
Diamantane (obsolete) ammonium hydroxide coordinates, and can realize the particle diameter free modulation from 0.3 ~ 17 μm of SSZ-13 molecular sieve, simple to operate, easily
In industrial operation；The addition of the crystal growth agent of the application, can not only promote the growth of molecular sieve, and avoid between crystal
Cluster so that molecular sieve crystal is scattered more uniform；Crystal growth agent (PA) is dissolved in the aobvious alkalescence of water, instead of and is conventionally synthesized
The sodium hydroxide solution that SSZ-13 molecular sieve uses so that the SSZ-13 molecular sieve sodium content finally synthesized is extremely low, with Na2O%
Meter is between 0.01 ~ 0.05%, and the Na of conventional method synthesis2O% counts 2.0～6.0%, thus avoids in commercial production
Ammonium exchange process, simplifies production technology, effectively reduces synthesis cost.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of embodiment 1 gained sample；
Fig. 2 is the X ray diffracting spectrum of embodiment 2 gained sample；
Fig. 3 is the X ray diffracting spectrum of embodiment 3 gained sample；
Fig. 4 is the X ray diffracting spectrum of embodiment 1 gained sample；
Fig. 5 is the scanning electron microscope (SEM) photograph of embodiment 1 gained sample；
Fig. 6 is the scanning electron microscope (SEM) photograph of embodiment 2 gained sample；
Fig. 7 is the scanning electron microscope (SEM) photograph of embodiment 3 gained sample；
Fig. 8 is the scanning electron microscope (SEM) photograph of embodiment 4 gained sample.
Detailed description of the invention
It is an object of the invention to provide the preparation method of SSZ-13 molecular sieve, be achieved through the following technical solutions:
The preparation method of a kind of SSZ-13 molecular sieve, comprises the following steps:
1. by N, N, N-trimethyl diamantane (obsolete) ammonium hydroxide and crystal growth agent mix homogeneously, add in autoclave, then
It is sequentially added into silicon source, aluminum source and water wherein, after stirring, obtains Primogel；N in described Primogel, N, N-trimethyl Buddha's warrior attendant
Alkane ammonium hydroxide: crystal growth agent: SiO2: Al2O3: H2The mol ratio of O is 0.06～0.25:0.00085～0.025:1:
0.017～0.063:20～40；Described crystal growth agent is piperazine；
2. by Primogel crystallization 17 ~ 72 hours at 155 ~ 175 DEG C of step 1. gained, crystallization product is obtained；
3. by the crystallization product centrifugation of step 2. gained, obtain filter cake and filtrate, gained filter cake is washed with deionized
To pH to 7 ~ 8, then it is dried 10 ~ 13 hours at 100 ~ 120 DEG C, obtains SSZ-13 molecular sieve.
Preferably, silicon source is Ludox, white carbon, c-type silica gel or tetraethyl orthosilicate.
Preferably, aluminum source is boehmite, aluminium hydroxide, aluminum sulfate or aluminum isopropylate..
Preferably, N in Primogel, N, N-trimethyl diamantane (obsolete) ammonium hydroxide: crystal growth agent: SiO2: Al2O3: H2O
Mol ratio be 0.15～0.20:0.005～0.01:1:0.02～0.06:25～35.
Preferably, N in Primogel, N, N-trimethyl diamantane (obsolete) ammonium hydroxide: crystal growth agent: SiO2: Al2O3: H2O
Mol ratio be 0.15:0.025:1:0.04:30.
Preferably, 2. step is by Primogel crystallization 24 ~ 60 hours at 160 ~ 170 DEG C of step 1. gained, obtains
Crystallization product.
Preferably, aluminum source is boehmite.
Preferably, silicon source is Ludox.
Further preferred preparation method, comprises the following steps:
1. by N, N, N-trimethyl diamantane (obsolete) ammonium hydroxide and crystal growth agent mix homogeneously, add in autoclave, then
It is sequentially added into silicon source, aluminum source and water wherein, after stirring, obtains Primogel；N in described Primogel, N, N-trimethyl Buddha's warrior attendant
Alkane ammonium hydroxide: crystal growth agent: SiO2: Al2O3: H2The mol ratio of O is 0.15:0.025:1:0.04:30；Described crystal
Growth stimulator is piperazine；Source of aluminium is boehmite；Described silicon source is Ludox；
2. by Primogel crystallization 50 hours at 165 DEG C of step 1. gained, crystallization product is obtained；
3. by the crystallization product centrifugation of step 2. gained, obtain filter cake and filtrate, gained filter cake is washed with deionized
To pH to 7, then it is dried 12 hours at 110 DEG C, obtains SSZ-13 molecular sieve.
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
1. by 31.3kgN, N, N-trimethyl diamantane (obsolete) ammonium hydroxide (SDA 25wt%) and 0.01kg crystal growth agent Piperazine anhydrous
(100wt%) mix homogeneously, adds in autoclave, is sequentially added into 13.3kg aluminum sulfate solution (Al the most wherein2O3
7.16wt%), 35.6kg Ludox (SiO2 25wt%) with 71.1kg water, after stirring, obtain Primogel；2. by step 1. gained
Primogel crystallization 72 hours at 155 DEG C, obtain crystallization product；
3. by the crystallization product centrifugation of step 2. gained, obtain filter cake and filtrate, gained filter cake is washed with deionized
To pH to 7, being then dried 13 hours at 100 DEG C, obtain SSZ-13 molecular sieve, wherein sodium content is with Na2O% counts, its numerical value model
Enclosing is 0.01%, and gained SSZ-13 molecular sieve verifies as pure phase SSZ-13 molecular sieve, the X-ray of sample through X-ray diffraction (XRD)
Shown in diffracting spectrum as accompanying drawing 1, shown in scanning electron microscope (SEM) photograph as accompanying drawing 5, its crystallite dimension is about 350nm.
Embodiment 2
1. by 12.1kgN, N, N-trimethyl diamantane (obsolete) ammonium hydroxide (SDA 25wt%) and 0.03kg crystal growth agent Piperazine anhydrous
(100wt%) mix homogeneously, adds in autoclave, is sequentially added into 0.56kg boehmite (Al the most wherein2O3
66.1wt%), 19.2kg tetraethyl orthosilicate (SiO2 25wt%) with 120.2kg water, after stirring, obtain Primogel；
2. by Primogel crystallization 17 hours at 175 DEG C of step 1. gained, crystallization product is obtained；
3. by the crystallization product centrifugation of step 2. gained, obtain filter cake and filtrate, gained filter cake is washed with deionized
To pH to 8, being then dried 10 hours at 130 DEG C, obtain SSZ-13 molecular sieve, wherein sodium content is with Na2O% counts, its numerical value model
Enclosing is 0.02%, and gained SSZ-13 molecular sieve verifies as pure phase SSZ-13 molecular sieve, the X-ray of sample through X-ray diffraction (XRD)
Shown in diffracting spectrum as accompanying drawing 2, shown in scanning electron microscope (SEM) photograph as accompanying drawing 6, its crystallite dimension is about 2.2 μm.
Embodiment 3
1. by 22.5kgN, N, N-trimethyl diamantane (obsolete) ammonium hydroxide (SDA 25wt%) and 0.29kg crystal growth agent Piperazine anhydrous
(100wt%) mix homogeneously, adds in autoclave, is sequentially added into 0.93kg aluminum isopropylate. (Al the most wherein2O3
24.8wt%), 10kgC type silica gel (SiO2 80.8wt%) with 130.5kg water, after stirring, obtain Primogel；
2. by Primogel crystallization 17 hours at 170 DEG C of step 1. gained, crystallization product is obtained；
3. by the crystallization product centrifugation of step 2. gained, obtain filter cake and filtrate, gained filter cake is washed with deionized
To pH to 7, being then dried 13 hours at 130 DEG C, obtain SSZ-13 molecular sieve, wherein sodium content is with Na2O% counts, its numerical value model
Enclosing is 0.03%, and gained SSZ-13 molecular sieve line verifies as pure phase SSZ-13 molecular sieve, the X-ray of sample through X ray diffraction (XRD)
Shown in diffracting spectrum as accompanying drawing 3, shown in scanning electron microscope (SEM) photograph as accompanying drawing 7, its crystallite dimension is about 17.0 μm.
Embodiment 4
1. by 15.3kgN, N, N-trimethyl diamantane (obsolete) ammonium hydroxide (SDA 25%) and 0.25kg crystal growth agent Piperazine anhydrous
(100wt%) mix homogeneously, adds in autoclave, is sequentially added into 29.06kg Ludox (SiO the most wherein2 25wt%
), 0.747kg boehmite (Al2O366.1wt%) with 151.2kg water, after stirring, obtain Primogel；
2. by Primogel crystallization 50 hours at 165 DEG C of step 1. gained, crystallization product is obtained；
3. by the crystallization product centrifugation of step 2. gained, obtain filter cake and filtrate, gained filter cake is washed with deionized
To pH to 7, being then dried 12 hours at 110 DEG C, obtain SSZ-13 molecular sieve, wherein sodium content is with Na2O% counts, its numerical value model
Enclosing is 0.01%, and gained SSZ-13 molecular sieve verifies as pure phase SSZ-13 molecular sieve, the X-ray of sample through X-ray diffraction (XRD)
Shown in diffracting spectrum as accompanying drawing 4, shown in scanning electron microscope (SEM) photograph as accompanying drawing 8, its crystallite dimension is about 5.0 μm.
Claims (9)
1. the preparation method of a SSZ-13 molecular sieve, it is characterised in that: comprise the following steps:
1. by N, N, N-trimethyl diamantane (obsolete) ammonium hydroxide and crystal growth agent mix homogeneously, add in autoclave, then
It is sequentially added into silicon source, aluminum source and water wherein, after stirring, obtains Primogel；N in described Primogel, N, N-trimethyl Buddha's warrior attendant
Alkane ammonium hydroxide: crystal growth agent: SiO2: Al2O3: H2The mol ratio of O is 0.06～0.25:0.00085～0.025:1:
0.017～0.063:20～40；Described crystal growth agent is piperazine；
2. by Primogel crystallization 17 ~ 72 hours at 155 ~ 175 DEG C of step 1. gained, crystallization product is obtained；
3. by the crystallization product centrifugation of step 2. gained, obtain filter cake and filtrate, gained filter cake is washed with deionized
To pH to 7 ~ 8, then it is dried 10 ~ 13 hours at 100 ~ 120 DEG C, obtains SSZ-13 molecular sieve.
The preparation method of SSZ-13 molecular sieve the most according to claim 1, it is characterised in that: described silicon source be Ludox,
White carbon, c-type silica gel or tetraethyl orthosilicate.
The preparation method of SSZ-13 molecular sieve the most according to claim 1, it is characterised in that: source of aluminium is for intending thin water aluminum
Stone, aluminium hydroxide, aluminum sulfate or aluminum isopropylate..
The preparation method of SSZ-13 molecular sieve the most according to claim 1, it is characterised in that: N, N in described Primogel,
N-trimethyl diamantane (obsolete) ammonium hydroxide: crystal growth agent: SiO2: Al2O3: H2The mol ratio of O be 0.15～0.20:0.005～
0.01:1:0.02～0.06:25～35.
The preparation method of SSZ-13 molecular sieve the most according to claim 1, it is characterised in that: N, N in described Primogel,
N-trimethyl diamantane (obsolete) ammonium hydroxide: crystal growth agent: SiO2: Al2O3: H2The mol ratio of O is 0.15:0.025:1:0.04:
30。
The preparation method of SSZ-13 molecular sieve the most according to claim 1, it is characterised in that: step is 2. for by step 1. institute
Primogel crystallization 24 ~ 60 hours at 160 ~ 170 DEG C obtained, obtain crystallization product.
The preparation method of SSZ-13 molecular sieve the most according to claim 1, it is characterised in that: described silicon source is Ludox.
The preparation method of SSZ-13 molecular sieve the most according to claim 1, it is characterised in that: source of aluminium is for intending thin water aluminum
Stone.
The preparation method of SSZ-13 molecular sieve the most according to claim 1, it is characterised in that: comprise the following steps:
1. by N, N, N-trimethyl diamantane (obsolete) ammonium hydroxide and crystal growth agent mix homogeneously, add in autoclave, then
It is sequentially added into silicon source, aluminum source and water wherein, after stirring, obtains Primogel；N in described Primogel, N, N-trimethyl Buddha's warrior attendant
Alkane ammonium hydroxide: crystal growth agent: SiO2: Al2O3: H2The mol ratio of O is 0.15:0.025:1:0.04:30；Described crystal
Growth stimulator is piperazine；Source of aluminium is boehmite；Described silicon source is Ludox；
2. by Primogel crystallization 50 hours at 165 DEG C of step 1. gained, crystallization product is obtained；
3. by the crystallization product centrifugation of step 2. gained, obtain filter cake and filtrate, gained filter cake is washed with deionized
To pH to 7, then it is dried 12 hours at 110 DEG C, obtains SSZ-13 molecular sieve.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108059172A (en) * | 2017-12-13 | 2018-05-22 | 山东齐鲁华信高科有限公司 | The preparation method of H-SSZ-13 molecular sieves |
| CN110436478A (en) * | 2019-07-22 | 2019-11-12 | 东北大学 | A kind of lamelliform CHA type SSZ-13 zeolite molecular sieve material and preparation method thereof |
| CN111592011A (en) * | 2020-05-21 | 2020-08-28 | 浙江大学 | Method for directly synthesizing SSZ-13 zeolite molecular sieve by using TEAOH as organic template agent |
| CN112495429A (en) * | 2021-01-14 | 2021-03-16 | 福州大学 | Method for synthesizing Cu-CHA molecular sieve with high SCR activity without template agent |
| CN112661170A (en) * | 2021-01-18 | 2021-04-16 | 中化学科学技术研究有限公司 | Synthesis method of low template agent SSZ-13 molecular sieve |
| US20210339233A1 (en) * | 2018-10-29 | 2021-11-04 | Pacific Industrial Development Corporation | Method of making ssz-13 zeolites with high acidity and low silica to alumina ratio (sar) |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108059172A (en) * | 2017-12-13 | 2018-05-22 | 山东齐鲁华信高科有限公司 | The preparation method of H-SSZ-13 molecular sieves |
| CN108059172B (en) * | 2017-12-13 | 2020-07-10 | 山东齐鲁华信高科有限公司 | Preparation method of H-SSZ-13 molecular sieve |
| US20210339233A1 (en) * | 2018-10-29 | 2021-11-04 | Pacific Industrial Development Corporation | Method of making ssz-13 zeolites with high acidity and low silica to alumina ratio (sar) |
| US11883804B2 (en) * | 2018-10-29 | 2024-01-30 | Pacific Industrial Development Corporation | Method of making SSZ-13 zeolites with high acidity and low silica to alumina ratio (SAR) |
| CN110436478A (en) * | 2019-07-22 | 2019-11-12 | 东北大学 | A kind of lamelliform CHA type SSZ-13 zeolite molecular sieve material and preparation method thereof |
| CN110436478B (en) * | 2019-07-22 | 2021-06-11 | 东北大学 | Lamellar CHA type SSZ-13 zeolite molecular sieve material and preparation method thereof |
| CN111592011A (en) * | 2020-05-21 | 2020-08-28 | 浙江大学 | Method for directly synthesizing SSZ-13 zeolite molecular sieve by using TEAOH as organic template agent |
| CN112495429A (en) * | 2021-01-14 | 2021-03-16 | 福州大学 | Method for synthesizing Cu-CHA molecular sieve with high SCR activity without template agent |
| CN112495429B (en) * | 2021-01-14 | 2021-11-02 | 福州大学 | Method for synthesizing Cu-CHA molecular sieve with high SCR activity without template agent |
| CN112661170A (en) * | 2021-01-18 | 2021-04-16 | 中化学科学技术研究有限公司 | Synthesis method of low template agent SSZ-13 molecular sieve |
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