CN109569320A - A method of mixing crystal seed method prepares pure phase SSZ-13 molecular screen membrane - Google Patents
A method of mixing crystal seed method prepares pure phase SSZ-13 molecular screen membrane Download PDFInfo
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- CN109569320A CN109569320A CN201811601519.XA CN201811601519A CN109569320A CN 109569320 A CN109569320 A CN 109569320A CN 201811601519 A CN201811601519 A CN 201811601519A CN 109569320 A CN109569320 A CN 109569320A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/028—Molecular sieves
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0046—Inorganic membrane manufacture by slurry techniques, e.g. die or slip-casting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0067—Inorganic membrane manufacture by carbonisation or pyrolysis
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Abstract
The invention proposes a kind of methods of mixing crystal seed method preparation pure phase SSZ-13 molecular screen membrane, it passes through before hydrothermal crystallizing, the seed layer of load on porous support is made of SAPO-34 molecular sieve and SSZ-13 molecular sieve, wherein, the mass ratio of SAPO-34 molecular sieve and SSZ-13 molecular sieve is 1:3-3:1；The seed layer is that seed layer is formed on carrier with not ground SSZ-13 molecular sieve mixing back loading at after unformed shape by SAPO-34 sieve particle is ground, then the SSZ-13 molecular screen membrane of pure phase is grown into, 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 preparation method of pure phase SSZ-13 molecular screen membrane loads seed layer on porous support before hydrothermal crystallizing
It is made of SAPO-34 molecular sieve and SSZ-13 molecular sieve, wherein SAPO-34 molecular sieve and the mass ratio of SSZ-13 molecular sieve are
1:3-3:1；The seed layer is mixed with SSZ-13 molecular sieve at after unformed shape by SAPO-34 sieve particle is ground
Back loading forms seed layer on carrier.
It is by one of erasing, spin coating, dip-coating and vacuum suction or a variety of groups that preferred crystal seed, which is supported on carrier,
It closes.
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:
(1) processing of porous carrier: carrier is polishing to sand paper it is smooth, with deionized water ultrasonic vibration 2min-10, leaching
6-24h 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 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: homemade SAPO-34 molecular sieve being mixed with water and is placed in bead mill tank, setting
Grinding revolving speed is 300-450rpm, milling time 6-8h, and grinding terminates the SAPO-34 molecule that amorphous state is obtained after drying
It (is passed through the molecule using TMAdaOH as template, not prepared with the template with homemade SSZ-13 molecular sieve by sieve
Sieve ineffective) be 1:3-3:1 mixing according to mass ratio after, mixed according still further to molecular sieve with the mass ratio of water 1:99-5:95, it is super
Sonication 2-10min is to obtain crystal seed suspension.
(4) crystal seed applies porous carrier
Spare porous carrier is loaded by the way of one of erasing, spin coating, dip-coating and vacuum suction or multiple combinations
Crystal seed, and in 60 DEG C of drying in oven.
(5) crystallization
The carrier for loading crystal seed is placed in casting solution, and is fitted into stainless steel cauldron, synthesizes 12- at 120 DEG C -200 DEG C
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, and warming and cooling rate is
0.2-1 DEG C/min is 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 by grinding SAPO-34
It is mixed at amorphous state with the SSZ-13 molecular sieve without any processing, substantially avoids a possibility that stray crystal MOR is generated.
2. discovery is in common template N, N, N- trimethyl -1- adamantane on the basis of the present invention is using crystal seed induction
A certain amount of triethylamine is added in base ammonium hydroxide equally can prepare the SSZ-13 molecular screen membrane of pure phase, further reduced
The preparation cost of membrane 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 it, and there is no SAPO-34 characteristic peaks, are substantially completely unformed shape), by itself and self-control
SSZ-13 molecular sieve (by using TMAdaOH as template, average grain diameter is 1 μm, non-removed template method) according to quality
It after for 1:1 mixing, is mixed according still further to molecular sieve 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 is loaded into crystal seed by the way of dip-coating, dip time non-10s is repeated once, 60 DEG C after drying
Drying in oven.
(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): homemade SSZ-13 molecular sieve and the mass ratio of water 2:98 are mixed
It closes, is ultrasonically treated 10min to obtain crystal seed suspension.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): by homemade SAPO-34 molecular sieve and water according to the matter of 5:95
Amount is placed in bead mill tank than mixing, sets grinding revolving speed as 450rpm, milling time 6h is ground after terminating drying to obtain
The SAPO-34 molecular sieve of amorphous state mixes it with the mass ratio of water 2:98, is ultrasonically treated 10min to obtain crystal seed suspension
Liquid.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): by homemade SAPO-34 molecular sieve and homemade SSZ-13 points
Son sieve is after 1:1 is mixed, to mix according still further to molecular sieve with the mass ratio of water 2:98 according to mass ratio, is ultrasonically treated 10min to obtain
Obtain crystal seed suspension.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): by homemade SAPO-34 molecular sieve and water according to the matter of 5:95
Amount is placed in bead mill tank than mixing, sets grinding revolving speed as 150rpm, milling time 3h is ground after terminating drying to obtain
The SAPO-34 molecular sieve (XRD characterization finds that it still remains SAPO-34 characteristic peak) of amorphous state, by itself and homemade SSZ-
13 molecular sieves (by the way that using TMAdaOH as template, average grain diameter is 1 μm, non-removed template method) are 1:1 according to mass ratio
It after mixing, is mixed according still further to molecular sieve with the mass ratio of water 2:98, is ultrasonically treated 10min to obtain crystal seed suspension.The comparison
The sample of 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 (8)
1. a kind of method of mixing crystal seed 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 SAPO-34 molecular sieve and SSZ-13 molecular sieve, wherein SAPO-34 molecular sieve with
The mass ratio of SSZ-13 molecular sieve is 1:3-3:1；The seed layer is that SAPO-34 sieve particle is ground at unformed
Seed layer is formed on carrier with not ground SSZ-13 molecular sieve mixing back loading after state.
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 the SSZ-13 molecular sieve is not fired removed template method.
4. 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℃。
5. 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.
6. 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.
7. 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.
8. 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: homemade SAPO-34 molecular sieve being mixed with water and is placed in bead mill tank, setting grinding
Revolving speed is 300-450rpm, milling time 6-8h, and grinding terminates the SAPO-34 molecular sieve that amorphous state is obtained after drying,
After it is mixed with homemade SSZ-13 molecular sieve according to mass ratio for 1:3-3:1, according still further to molecular sieve with water 1:99-5:95's
Mass ratio mixing is ultrasonically treated 2-10min to obtain crystal seed suspension；
(4) crystal seed applies porous carrier: by spare porous carrier using one of erasing, spin coating, dip-coating and vacuum suction
Or the mode of multiple combinations loads crystal seed, and in drying in oven；
(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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| 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 |
| CN116002709A (en) * | 2023-01-31 | 2023-04-25 | 南京工业大学 | Preparation method of SSZ-13 molecular sieve membrane |
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