CN109437221A - A kind of method of secondary growth method method preparation pure phase SSZ-13 molecular screen membrane - Google Patents
A kind of method of secondary growth method method preparation pure phase SSZ-13 molecular screen membrane Download PDFInfo
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- CN109437221A CN109437221A CN201811601552.2A CN201811601552A CN109437221A CN 109437221 A CN109437221 A CN 109437221A CN 201811601552 A CN201811601552 A CN 201811601552A CN 109437221 A CN109437221 A CN 109437221A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
- B01D53/228—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion characterised by specific membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
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- B01D2257/504—Carbon dioxide
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- 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
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- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
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Abstract
The invention proposes a kind of methods of secondary growth method preparation pure phase SSZ-13 molecular screen membrane, and before hydrothermal crystallizing, the seed layer loaded on porous support is made of unformed shape SAPO-34 molecular sieve and SSZ-13 molecular sieve；The seed layer be by SSZ-13 it is molecular sieve carried on porous support after it is again that the SAPO-34 of unformed shape is molecular sieve carried on porous support, then grow into the SSZ-13 molecular screen membrane of pure phase.Compared with the prior art, cost is relatively low for method according to the present invention, is conducive to subsequent industrial applications.
Description
Technical field
The present invention relates to a kind of preparation methods of film more particularly to a kind of mixing crystal seed method to prepare SSZ-13 molecular screen membrane
Method.
Background technique
Because terrestrial climate variation issue has caused the extensive concern of international community caused by carbon dioxide, coal-burning power plant is big
The important sources of CO2 in gas, carbon capture technology is the hot spot of current flue gas treatment after coal combustion, and numerous scientific research scholars are dedicated to
In the trapping work of CO2.In numerous CO2 trapping techniques, membrane separation technique is because it is with easy to operate and low energy consumption etc. advantages
The concern of more and more scholars is obtained.In numerous membrane materials applied to gas separation, high-silicon type zeolite molecular sieve film tool
There is good hydrothermal stability, is a kind of ideal membrane material of ideal mixed gas separation.SSZ-13 molecular screen membrane has rule
3 whole dimensions octatomic ring cellular structure (0. 37 nm*, 0.42 nm), and there is Preferential adsorption selectivity to CO2, therefore
SSZ-13 molecular screen membrane to from admixture of gas separate CO2 have potential application foreground.
The method for preparing SSZ-13 molecular screen membrane includes in-situ synthesis and secondary growth method, relative in situ synthesis,
Secondary growth method has controllability to parameters such as compactness, the thickness of film.Preparing SSZ-13 molecular screen membrane in the prior art is
It is coated in the SSZ-13 molecular sieve of preparation as crystal seed on supporter, but prepares SSZ-13 molecular sieve and need expensive N, N,
N- trimethyl -1- adamantyl ammonium hydroxide as template, therefore its as crystal seed preparation membrane material compared to conjunction in situ
The membrane material cost prepared at method is higher, to limit its industrial applications prospect.And for SSZ-13 molecular sieve, the prior art
Middle presence carries out induction synthesis as crystal seed using SAPO-34 prepared by cheap template (such as diethylamine, triethylamine), but
Be the applicant found in repeated experiment its preparation sieve particle qualification rate it is lower (being often accompanied by MOR stray crystal), and incite somebody to action
Substantially qualified SSZ-13 molecular screen membrane will not be prepared when SAPO-34 is supported on induction filming on carrier as crystal seed.Therefore,
It needs a kind of method and reduces secondary growth method to prepare the cost of SSZ-13 molecular screen membrane to improve its application prospect.
Summary of the invention
It is an object of the invention in the prior art using SSZ-13 system with molecular sieve for preparing for SSZ-13 molecular screen membrane price
Higher technical problem, providing the new preparation method of one kind reduces the cost of SSZ-13 molecular screen membrane and is substantially free of MOR
Stray crystal.
When technical solution of the present invention:
A kind of method of secondary growth method preparation pure phase SSZ-13 molecular screen membrane, it is characterised in that before hydrothermal crystallizing, be supported on
Seed layer on porous carrier is made of unformed shape SAPO-34 molecular sieve and SSZ-13 molecular sieve；The seed layer be by
SSZ-13 it is molecular sieve carried on porous support after it is again that the SAPO-34 of unformed shape is molecular sieve carried on porous support.
Preferably, it is by one of erasing, spin coating, dip-coating and vacuum suction or a variety of groups that crystal seed, which is supported on carrier,
It closes.
Preferably, SSZ-13 molecular sieve is loaded on porous support using erasing, and the SAPO-34 molecular sieve of unformed shape
On porous support by dip-coating load.
Preferably, the crystallization temperature that the hydrothermal crystallization process uses is 120-200 DEG C.
Preferably, the SSZ-13 molecular sieve is not fired removed template method.
Preferably, casting solution used by the hydrothermal crystallization process includes template, silicon source, silicon source, NaOH and water,
Wherein molar ratio, SIO2/Al2O3=20-400, SiO2/ template=1-10, H2O/SiO2=10-100, SiO2/NaOH=10-
200。
Preferably, the mixing of template N, N, N- trimethyl -1- adamantyl ammonium hydroxide (TMAdaOH) and triethylamine
The molar ratio of template, wherein N, N, N- trimethyl -1- adamantyl ammonium hydroxide and triethylamine is 1:1-20.
Preferably, the support shapes are tubulose, sheet, multichannel or doughnut, and the carrier medium is oxygen
Change aluminium, zirconium oxide, mullite or metal.
Preparation method of the present invention the following steps are included:
The method the following steps are included:
(1) processing of porous carrier: carrier is polishing to sand paper it is smooth, with deionized water ultrasonic vibration 2min-10,
6-24h is impregnated, is finally placed in baking oven and is dried for standby；
(2) synthesis of casting solution: template, silicon source, silicon source, NaOH and water being mixed, and are ultrasonically treated 20min, stir aging
6h, each material mol ratio in casting solution are as follows: SIO2/Al2O3=20-400, SiO2/ template=1-10, H2O/SiO2=10-100,
SiO2/NaOH=10-200；
(3) configuration of crystal seed suspension: SAPO-34 molecular sieve being mixed with water and is placed in bead mill tank, set grinding revolving speed as
300-450rpm, milling time 6-8h, grinding terminate after drying to obtain the SAPO-34 molecular sieve of amorphous state, by its with
Water mixing, is ultrasonically treated to obtain crystal seed suspension J1.In addition homemade SSZ-13 molecular sieve is taken to mix with water, after ultrasonic treatment
To obtain crystal seed suspension J2；
(4) crystal seed applies porous carrier: first load crystal seed is carried out to porous carrier using crystal seed suspension J1, using crystalline substance after drying
Kind suspension J2 carries out load crystal seed to porous carrier, and dries；
(5) crystallization: the carrier for loading crystal seed being placed in casting solution, and is fitted into stainless steel cauldron, is closed at 120 DEG C -200 DEG C
At 12-48h.After synthesis, by molecular screen membrane cleaning, impregnates and dry.
(6) it roasts: the molecular screen membrane of drying is placed in Muffle kiln roasting 4-18h, maturing temperature is 500-600 DEG C, is risen
Cooling rate is 0.2-1 DEG C/min to obtain SSZ-13 molecular screen membrane.
Beneficial effects of the present invention:
1. the present invention is mixed using the low SAPO-34 molecular sieve of synthesis cost with SSZ-13 molecular sieve, to be used as crystal seed to be supported on porous
On carrier, the generation of stray crystal in film further reduced on the basis of reducing film preparation cost, and pass through the crystal seed to two kinds
Coating method optimize, substantially avoid stray crystal MOR generate a possibility that.
2. discovery is in common template N, N, N- trimethyl -1- adamantyl hydrogen on the basis of the present invention is using crystal seed induction
A certain amount of triethylamine is added in amine-oxides equally can prepare the SSZ-13 molecular screen membrane of pure phase, further reduced membrane material
The preparation cost of material.
Detailed description of the invention
Fig. 1 is the XRD diagram of SSZ-13 molecular screen membrane prepared by the embodiment of the present invention.
Fig. 2 is the SEM figure on SSZ-13 molecular screen membrane surface prepared by the embodiment of the present invention.
Specific embodiment
Embodiment 1
(1) processing of porous carrier: the porous carrier that the present embodiment uses for alumina tube carrier (average pore size is 2.5 μm,
Porosity be 40%), tubular media is polishing to 800 mesh sand paper it is smooth, with deionized water ultrasonic vibration 10min, leaching
12h is steeped, is finally placed in 60 DEG C of baking ovens and is dried for standby.
(2) synthesis of casting solution: template, silicon source, silicon source, NaOH and water being mixed, and are ultrasonically treated 20min, stirred
Aging 6h, each material mol ratio is SIO2/Al2O3=40, SiO2/ template=10, H2O/SiO2=100, SiO2/ in casting solution
NaOH=10.For the template used in the present embodiment for TMAdaOH, silicon source is silica solution, and silicon source is sodium metaaluminate.
(3) homemade SAPO-34 molecular sieve the configuration of crystal seed suspension: is mixed into postposition according to the mass ratio of 5:95 with water
In bead mill tank, grinding revolving speed is set as 450rpm, milling time 6h, grinding terminates after drying to obtain amorphous state
SAPO-34 molecular sieve (XRD characterization finds that it is substantially completely unformed shape there is no SAPO-34 characteristic peak), by itself and water 2:
98 mass ratio mixing, is ultrasonically treated 10min to obtain crystal seed suspension J1.In addition homemade SSZ-13 molecular sieve and water 2 are taken:
98 mass ratio mixing, is ultrasonically treated 10min to obtain crystal seed suspension J2.
(4) crystal seed applies porous carrier
Spare porous carrier is loaded into crystal seed by the way of dip-coating, first porous carrier is placed in crystal seed suspension J2, is soaked
The stain time is 10s, is placed it in crystal seed suspension J1 again after 60 DEG C of drying in oven, dip time 10s, in 60 DEG C of baking ovens
Drying.
(5) crystallization
The carrier for loading crystal seed is placed in casting solution, and is fitted into stainless steel cauldron, synthesizes 36h at 155 DEG C.Synthesis terminates
Afterwards, molecular screen membrane cleaning, immersion are dried.
(6) it roasts
The molecular screen membrane of drying is placed in Muffle kiln roasting 15h, maturing temperature is 550 DEG C, and warming and cooling rate is 1 DEG C/min
To obtain SSZ-13 molecular screen membrane S1.
Embodiment 2
The embodiment and embodiment the difference is that the template used in step (2) for N, N, N- trimethyl -1- adamantane
The mixed templates (molar ratio 2:1) of base ammonium hydroxide (TMAdaOH) and triethylamine.The sample of embodiment preparation is denoted as
S2。
Comparative example 1
The comparative example is the difference from embodiment 1 is that step (3), (4):
(3) configuration of crystal seed suspension: homemade SSZ-13 molecular sieve is mixed with the mass ratio of water 2:98, is ultrasonically treated 10min
To obtain crystal seed suspension.
(4) crystal seed applies porous carrier: spare porous carrier being loaded crystal seed by the way of dip-coating, by porous carrier
It is placed in crystal seed suspension, dip time 10s, is placed it in crystal seed suspension again after 60 DEG C of drying in oven, when dipping
Between be 10s, 60 DEG C of drying in oven.The sample of comparative example preparation is denoted as D1.
Comparative example 2
The comparative example is the difference from embodiment 1 is that step (3), (4):
(3) configuration of crystal seed suspension: homemade SAPO-34 molecular sieve is mixed with water according to the mass ratio of 5:95 and is placed on pearl
In grinding jar, grinding revolving speed is set as 450rpm, milling time 6h, grinding terminates the SAPO- that amorphous state is obtained after drying
34 molecular sieves mix it with the mass ratio of water 2:98, are ultrasonically treated 10min to obtain crystal seed suspension.
(4) crystal seed applies porous carrier: spare porous carrier being loaded crystal seed by the way of dip-coating, by porous carrier
It is placed in crystal seed suspension, dip time 10s, is placed it in crystal seed suspension again after 60 DEG C of drying in oven, when dipping
Between be 10s, 60 DEG C of drying in oven.The sample of comparative example preparation is denoted as D2.
Comparative example 3
The comparative example is the difference from embodiment 1 is that step (3):
(3) configuration of crystal seed suspension: homemade SAPO-34 molecular sieve is mixed with the mass ratio of water 2:98, ultrasonic treatment
10min is to obtain crystal seed suspension J1.In addition it takes homemade SSZ-13 molecular sieve to mix with the mass ratio of water 2:98, is ultrasonically treated
10min is to obtain crystal seed suspension J2.The sample of comparative example preparation is denoted as D3.
Comparative example 4
The comparative example is the difference from embodiment 1 is that step (3):
(3) configuration of crystal seed suspension: homemade SAPO-34 molecular sieve is mixed with water according to the mass ratio of 5:95 and is placed on pearl
In grinding jar, grinding revolving speed is set as 150rpm, milling time 3h, grinding terminates after drying to obtain SAPO-34 molecular sieve
(XRD characterization finds that it still remains SAPO-34 characteristic peak) mixes it with the mass ratio of water 2:98, be ultrasonically treated 10min with
Obtain crystal seed suspension J1.In addition homemade SSZ-13 molecular sieve is taken to mix with the mass ratio of water 2:98, be ultrasonically treated 10min with
Obtain crystal seed suspension J2.The sample of comparative example preparation is denoted as D4.
Sample prepared by embodiment 1-2 and comparative example 1-4, which is carried out XRD characterization and SEM characterization to detect film surface, is
No is pure phase, the result is as follows:
The sample result of the different embodiment and comparative example preparations of table 1
| Sample | S1 | S2 | D1 | D2 | D3 | D4 |
| As a result | Pure phase SSZ-13 | Pure phase SSZ-13 | Pure phase SSZ-13 | Basic MOR | Basic MOR | MOR and SSZ-13 is simultaneously deposited |
Seen from table 1, the SSZ-13 molecular screen membrane (embodiment sample of pure phase can be prepared using method prepared by the present invention
XRD diagram referring to Fig. 1, SEM schemes referring to fig. 2), with use completely SSZ-13 as the SSZ- of crystal seed progress secondary growth method preparation
13 molecular screen membranes can be avoided the miscellaneous generation through MOR, and therefore, preparation method of the present invention is relative to using SSZ-13 points
Son sieve can significantly reduce production cost, be conducive to the subsequent industrial applications of SSZ-13 molecular screen membrane as crystal seed.
Based on the above description of the preferred embodiments of the present invention, by description, relevant staff completely can be with
On the basis of without departing from technical thought of the invention, various changes and amendments are carried out.Technical scope of the invention not office
It is limited to the content of specification record, it is necessary to which technical scope is determined with scope of the claims.
Claims (9)
1. a kind of method of secondary growth method preparation pure phase SSZ-13 molecular screen membrane, it is characterised in that before hydrothermal crystallizing, load
Seed layer on porous support is made of unformed shape SAPO-34 molecular sieve and SSZ-13 molecular sieve；The seed layer is
By SSZ-13 it is molecular sieve carried on porous support after it is again that the SAPO-34 of unformed shape is molecular sieve carried on porous support.
2. according to the method described in claim 1, it is characterized in that it is by erasing, spin coating, dip-coating that crystal seed, which is supported on carrier,
With vacuum suction one of or multiple combinations.
3. according to the method described in claim 1, it is characterized in that SSZ-13 molecular sieve using erasing load on porous support,
And the SAPO-34 molecular sieve of unformed shape is loaded on porous support by dip-coating.
4. according to the method described in claim 1, it is characterized in that the SSZ-13 molecular sieve is not fired removed template method.
5. according to the method described in claim 1, it is characterized in that the crystallization temperature that uses of the hydrothermal crystallization process for
120-200℃。
6. according to the method described in claim 1, it is characterized in that casting solution used by the hydrothermal crystallization process includes
Template, silicon source, silicon source, NaOH and water, wherein molar ratio, SIO2/Al2O3=20-400, SiO2/ template=1-10, H2O/
SiO2=10-100, SiO2/NaOH=10-200.
7. according to the method described in claim 4, it is characterized in that template is N, N, N- trimethyl -1- adamantyl hydroxide
The mixed templates of ammonium (TMAdaOH) and triethylamine, wherein N, N, N- trimethyl -1- adamantyl ammonium hydroxide and triethylamine
Molar ratio is 1-3:1.
8. according to the method described in claim 1, it is characterized in that the support shapes be tubulose, sheet, multichannel or in
Hollow fiber, the carrier medium are aluminium oxide, zirconium oxide, mullite or metal.
9. according to the method described in claim 1, it is characterized in that the method the following steps are included:
(1) processing of porous carrier: carrier is polishing to sand paper it is smooth, with deionized water ultrasonic vibration 2min-10,
6-24h is impregnated, is finally placed in baking oven and is dried for standby；
(2) synthesis of casting solution: template, silicon source, silicon source, NaOH and water being mixed, and are ultrasonically treated 20min, stir aging
6h, each material mol ratio in casting solution are as follows: SIO2/Al2O3=20-400, SiO2/ template=1-10, H2O/SiO2=10-100,
SiO2/NaOH=10-200；
(3) configuration of crystal seed suspension: SAPO-34 molecular sieve being mixed with water and is placed in bead mill tank, set grinding revolving speed as
300-450rpm, milling time 6-8h, grinding terminate after drying to obtain the SAPO-34 molecular sieve of amorphous state, by its with
Water mixing, is ultrasonically treated to obtain crystal seed suspension J1.In addition homemade SSZ-13 molecular sieve is taken to mix with water, after ultrasonic treatment
To obtain crystal seed suspension J2；
(4) crystal seed applies porous carrier: first load crystal seed is carried out to porous carrier using crystal seed suspension J1, using crystalline substance after drying
Kind suspension J2 carries out load crystal seed to porous carrier, and dries；
(5) crystallization: the carrier for loading crystal seed being placed in casting solution, and is fitted into stainless steel cauldron, is closed at 120 DEG C -200 DEG C
At 12-48h.After synthesis, by molecular screen membrane cleaning, impregnates and dry；
(6) it roasts: the molecular screen membrane of drying being placed in Muffle kiln roasting 4-18h, maturing temperature is 500-600 DEG C, heating and cooling
Speed is 0.2-1 DEG C/min to obtain SSZ-13 molecular screen membrane.
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|---|---|---|---|
| CN201811601552.2A CN109437221B (en) | 2018-12-26 | 2018-12-26 | Method for preparing pure-phase SSZ-13 molecular sieve membrane by secondary growth method |
| CN202010589193.4A CN111672461A (en) | 2018-12-26 | 2018-12-26 | Method for preparing pure-phase SSZ-13 molecular sieve membrane by secondary growth method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111056560A (en) * | 2019-11-26 | 2020-04-24 | 上海工程技术大学 | Economic synthesis method of ultrathin SSZ-13 molecular sieve membrane |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112499642B (en) * | 2020-12-02 | 2023-11-21 | 南京工业大学 | Preparation method of multichannel SSZ-13 molecular sieve membrane |
| CN114288871B (en) * | 2021-12-31 | 2023-06-16 | 武汉智宏思博环保科技有限公司 | Method for preparing molecular sieve membrane by dip-coating molecular sieve seed crystal method |
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| CN104289115A (en) * | 2014-08-25 | 2015-01-21 | 南京工业大学 | High silicon CHA type SSZ-13 zeolite membrane preparation method |
| CN106629761A (en) * | 2016-12-20 | 2017-05-10 | 上海卓悦化工科技有限公司 | Synthesis method of SSZ-13 molecular sieve |
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| CN104289115A (en) * | 2014-08-25 | 2015-01-21 | 南京工业大学 | High silicon CHA type SSZ-13 zeolite membrane preparation method |
| CN106629761A (en) * | 2016-12-20 | 2017-05-10 | 上海卓悦化工科技有限公司 | Synthesis method of SSZ-13 molecular sieve |
| 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 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111056560A (en) * | 2019-11-26 | 2020-04-24 | 上海工程技术大学 | Economic synthesis method of ultrathin SSZ-13 molecular sieve membrane |
| CN111056560B (en) * | 2019-11-26 | 2023-03-31 | 上海工程技术大学 | Economic synthesis method of ultrathin SSZ-13 molecular sieve membrane |
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| CN111672461A (en) | 2020-09-18 |
| CN109437221B (en) | 2020-12-11 |
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