CN110228813A - A method of preparing y-type zeolite membrane - Google Patents
A method of preparing y-type zeolite membrane Download PDFInfo
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- CN110228813A CN110228813A CN201910654796.5A CN201910654796A CN110228813A CN 110228813 A CN110228813 A CN 110228813A CN 201910654796 A CN201910654796 A CN 201910654796A CN 110228813 A CN110228813 A CN 110228813A
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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
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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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- 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
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- 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
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- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The present invention provides a kind of methods for preparing y-type zeolite membrane, belong to the technical field of molecular screen membrane.Its technical solution are as follows: the following steps are included: step 1: the preparation of nano Y-shaped molecular sieve；Step 2: the pretreatment of carrier；Step 3: secondary growth method prepares y-type zeolite membrane.The invention has the benefit that the present invention, which is utilized, is polished to Al for nano Y-shaped molecular sieve crystal seed2O3On ceramic ring carrier surface, with the pre- plant nano Y-shaped molecular sieve crystal seed and Al after corona treatment2O3Ceramic ring carrier directly passes through in-site secondary hydrothermal synthesis and obtains fine and close y-type zeolite membrane.Reaction time is short, and preparation method is convenient.The y-type zeolite membrane compactness prepared is fine, and thickness is also 5 μm very uniformly.In view of the property of Y type molecular sieve, which can be used for the separation of the mixture of bigger molecule, and the size of molecular sieve bore diameter is adjusted by method further physically or chemically, can be had broad application prospects in terms of separation.
Description
Technical field
The present invention relates to the preparation technical field of molecular screen membrane more particularly to a kind of methods for preparing y-type zeolite membrane.
Background technique
Molecular screen membrane has the characteristics that cellular structure is uniform, the easy modulation of acid-base property, in gas as a kind of Novel inorganic membrane
Separation and membrane reactor field have broad application prospects.Y type molecular sieve has three-dimensional cellular structure, and maximum diameter of hole is
0.74nm is grown on cellular ceramic substrate the Large pore molecular sieve membrane for then being formed and being different from other zeolite membranes, is suitable for pair
The separation of bigger molecule and petrochemical industry, field of fine chemical.
It records in the prior art and goes out continuous the eight of different-thickness by planting crystal seed and then secondary hydrothermal synthesis in advance on carrier
Face zeolite membrane, it is also on the books differently to plant crystal seed in advance on carrier for separating gas and organic matter, then pass through microwave
Synthesize faujasite film, and the y-type zeolite membrane of continuous densification is obtained by multi-stage synthesis.
Recently, domestic and international scientific circles conduct extensive research the synthesis of y-type zeolite membrane with application, develop a variety of
Synthetic method specifically includes that Vacuum-assisted method method, gas phase synthesis method etc..Wherein surface of the Vacuum-assisted method method to carrier
Property requirements are stringenter, cause its repeatability and applicability poor.Gas phase synthesis method is complicated for operation, and crystallization degree is not high, unfavorable
In the molecular screen membrane that formation is stable.
Summary of the invention
The present invention in view of the above problems, in order to overcome raw water position thermal synthesis method repeatability and applicability it is poor and
Meteorological synthetic method is unfavorable for forming the defect of stable molecular screen membrane, and the purpose of the present invention is to provide one kind in Al2O3Ceramic ring
The method for preparing y-type zeolite membrane using nano Y-shaped molecular sieve guiding growth method on carrier.
The molecular screen membrane continuity that the synthetic method known to scanning spectrogram obtains is high, and compactness is strong, can be used for optics device
Part, membrane separator etc., in sensor, lithium battery etc. is had potential application.
The present invention is realized by following measure: a method of preparing y-type zeolite membrane, comprising the following steps:
Step 1: the preparation of nano Y-shaped molecular sieve:
By nNa2O:nSiO2: nAl2O3: nH2The molar ratio of O=16:16:1:210 prepares directed agents, by directed agents aging
After 19h, sulfuric acid solution is instilled into directed agents, is formed gel, is configured to nNa2O:nSiO2:nAl2O3:nH2O=7.8:16:1:
Reaction solution is packed into reaction kettle by 400 reaction solution, and reaction kettle is put into insulating box, and crystallization 8h at 100 DEG C will be in reaction kettle
Product takes out, and product is put into 120 DEG C of Muffle furnace drying, obtains nano Y-shaped molecular sieve, molecular sieve one after suction filtration and washing
Secondary preparation can be in molecular screen membrane preparation using multiple；
Step 2: the pretreatment of carrier:
Alkali process: the sodium hydroxide solution of aluminium oxide ceramics ring carrier and 7mol/L are placed in flask, are heated to 110 DEG C
Reflow treatment 1h is cleaned 2-3 times under ultrasonic wave, (each 10min) with deionized water, is then placed in Muffle furnace and is burnt for 600 DEG C
Burn 1h；
Corona treatment: first will be nano Y-shaped by one layer of aluminium oxide ceramics ring carrier surface polishing after alkali process
Then molecular sieve is loaded with the carrier of nano Y-shaped molecular sieve using Microwave plasma treatment；
Step 3: secondary growth method prepares y-type zeolite membrane:
Nano Y-shaped molecular sieve is planted in advance to porous Al using polishing mode2O3On ceramic ring carrier, and nanometer Y will be planted in advance
After the carrier Microwave plasma treatment of type molecular sieve, by Al2(SO4)3·18H2O, silica solution, sodium hydroxide and deionization
Water is according to n (Na2O): n (SiO2)/n(Al2O3)/n(H2O)=14:10:1:800 proportion is in room temperature and intense mechanical stirring bar
It is uniformly mixed into glue under part and is aged 9h respectively, the Al of nano Y-shaped molecular sieve will be planted in advance2O3Carrier passes through corona treatment
Afterwards, it being vertically put into the stainless steel cauldron of polytetrafluoro liner, injection reaction glue seals reaction kettle to carrier is flooded completely,
It is placed in constant temperature, is taken out in 90 DEG C of crystallization 9h, be washed with deionized to filtrate and be in neutrality, it is dry at 120 DEG C, Y is made
Type molecular screen membrane.
Further, reflow treatment refers to condensing reflux, i.e. sodium hydroxide solution after by thermal evaporation, from heating end from
Open, reach and be converted into drop again after by cold end, heating end with by cold end, in the same flask, and heated end position is lower,
Drop, which just converges, flows back to heating end, is formed and is condensed back.
Further, deionized water refers to the pure water eliminated in after ionic species impurity.
Further, cleaning refers to and utilizes ultrasonic wave cavitation in a liquid, acceleration effect and straight under ultrasonic wave
Influent stream effect to liquid and dirt directly, indirectly effect, make crud layer by dispersion, emulsification, removing and reach cleaning purpose.
Further, corona treatment refers to Microwave plasma treatment.
Further, the time of Microwave plasma treatment is 15min.
Further, polishing mode refers to: by the nano Y-shaped molecular sieve of preparation directly in Al2O3Ceramic ring carrier rings front
Upper grinding homogeneity is rinsed with deionized water to remove Al2O3The unattached firm nano Y-shaped molecular sieve of ceramic ring carrier ring surface
Particle.
Further, it is vertically put into and refers to and will smear the Al of nano Y-shaped molecular sieve2O3Ceramic ring carrier is put vertically down
Into in reaction kettle, to prevent molecular sieve powder from depositing in carrier side.
The invention has the benefit that the present invention, which is utilized, is polished to Al for nano Y-shaped molecular sieve crystal seed2O3Ceramic ring carrier
It is brilliant with the pre- plant nano Y-shaped molecular sieve after corona treatment after then handling carrier with microwave plasma device on surface
Kind and Al2O3Ceramic ring carrier directly passes through in-site secondary hydrothermal synthesis and obtains fine and close y-type zeolite membrane.Reaction time is short, system
Preparation Method is convenient.Keep the y-type zeolite membrane compactness prepared fine, thickness is also 5 μm very uniformly, reproducible.In view of Y
The property of type molecular sieve, the film can be used for the separation of the mixture of bigger molecule, pass through method further physically or chemically
The size for adjusting molecular sieve bore diameter, can have broad application prospects in terms of separation.
Detailed description of the invention
Fig. 1 is the XRD spectra of synthesized sample.
Fig. 2 is sample surface morphology SEM photograph.
Fig. 3 is plasma producing apparatus.
Fig. 4 is the pre- XRD spectra for planting the molecular screen membrane prepared after crystal seed of polishing.
Fig. 5 is the surface that molecular screen membrane is prepared using polishing crystal seed.
Fig. 6 is surface and the side view that molecular screen membrane is prepared using polishing crystal seed.
Wherein: it will be seen from figure 1 that 2 θ=6.19 (°) of sample, 10.11 (°), 12.39 (°), 15.6l (°), 23.72
There is apparent diffraction maximum in (°) and 27.70 (°), belong to the characteristic peak of micropore FAU type Y zeolite, compared complete with standard spectrogram
It is consistent.
Fig. 2 is the SEM spectrogram of synthesized and application Y type molecular sieve crystal seed, can be seen that crystal seed is pure by scanning electron microscope (SEM) photograph
Phase, particle is more uniform, and crystal seed size is about 100 nanometers.
Fig. 3 microwave plasma emission device figure, this device are setting for the carrier that Microwave plasma treatment plants crystal seed in advance
It is standby.
Fig. 4 pre- XRD spectra for planting the molecular screen membrane prepared after crystal seed of polishing.
Using ceramic ring as the XRD diffraction spectrogram of Y shape molecular screen membrane synthesized by carrier.2 θ=6.19 (°), 10.11 in figure
There is the series of features of Y shape molecular sieve crystal in the positions such as (°), 12.39 (°), 15.6l (°), 23.72 (°) and 27.70 (°)
Peak, it was demonstrated that it is y-type zeolite membrane, wherein 18.02 °, 29.4 °, the 35.04 ° and 37.66 ° characteristic peaks for potsherd carrier, wherein
A is molecular sieve, and b, which is that polishing is pre-, plants the molecular screen membrane prepared after crystal seed.
Fig. 5 is the surface that molecular screen membrane is prepared using polishing crystal seed, and the Y type molecular sieve film surface grows very as seen from the figure
Densification, continuity are preferable.
Fig. 6 is surface and the side view that molecular screen membrane is prepared using polishing crystal seed, from side view, y-type zeolite membrane
Thickness is uniform, with a thickness of 5 μm of fine and close y-type zeolite membrane.
Specific embodiment
In order to clarify the technical characteristics of the invention, being illustrated below by specific embodiment to this programme.
The present invention is the preparation method of y-type zeolite membrane, is included the following steps:
Step 1: taking silica solution (wt30%) 30.05g, and 9.75g sodium hydroxide is added, and is uniformly mixed, and forms solution 1.,
6.25gAl2 (SO4) 318H2O is dissolved with 21g water, is uniformly mixed, 4.5g sodium hydroxide is then added, is uniformly mixed, is formed
Solution is 2..Wherein silica solution is silicon source, and aluminum sulfate is silicon source, and sodium hydroxide is alkali source.
2. 1. solution is slowly dropped into solution, be uniformly mixed, form gel, place aging 19h, forms directed agents, guiding
The molar ratio of agent forms: nNa2O:nSiO2:nAl2O3:nH2O=16:16:1:210.98% concentrated sulfuric acid 7.7g is taken to delay the concentrated sulfuric acid
It is slow to instill in 17.8g water, it stirs while adding, is uniformly mixed.Configured sulfuric acid solution is instilled in directed agents, when being added
Stirring is uniformly mixed.Then reaction kettle is added, the molar ratio of reaction kettle reaction solution is added are as follows: nNa2O:nSiO2:nAl2O3:nH2O
Reaction kettle is put into crystallization 10h in 100 DEG C of insulating boxs by=7.8:16:1:400.Reaction kettle is taken out, cooling, centrifuge separation washing
To neutrality, it is put into 120 DEG C of Muffle furnace drying.Obtain nano Y-shaped molecular sieve.
Step 2: the pretreatment of carrier
Alkali process: the sodium hydroxide solution of carrier and 7mol/L are placed in flask, reflow treatment at 110 DEG C is heated to
1h is cleaned 2-3 times under ultrasonic wave, (each 10min) with deionized water, is then placed in 600 DEG C of calcination 1h in Muffle furnace.
Corona treatment: it first by by the aluminium oxide ceramics ring carrier surface one layer crystal kind of polishing after alkali process, applies
The crystal seed smeared uniformly, and will not will fall crystal seed powder easily.Then the load of crystal seed is loaded with using Microwave plasma treatment
Body, microwave plasma emission device figure as shown in Figure 3:
Specific step is as follows for Microwave plasma treatment:
1. all channels of closed system and atmosphere start vacuum pump, vacuum degree is evacuated to less than 133Pa；
2. connecting discharge-type vacuum meter, pressure regulator knob is reconciled, makes the quartz glass tube vacuumized that glow discharge occur, and
Vacuum is detected to 100-200Pa；
3. connecting microwave plasma-generator installation's power source；
4.) the setting processing time be 15min；
5. pressing start button, pressure regulator rotating handle is adjusted, is located at " demodulating voltage " on threshold voltage (150V), until
Arc discharge occurs, generates plasma.Vacuum degree is high, and arcing voltage is low；Conversely, the starting the arc is difficult.Etc. vacuum degrees reach 100-
When 200Pa stablizes, arcing voltage 155-160V, power 110-140W；
6. being passed through reaction gas air, 20ml/min, electric arc maintenance voltage are controlled by flowmeter or mass flowmenter
200-220V, flow 0.04m3/ h, electric arc maintenance voltage are greater than 200V；Power is 400W.
7. after reaction, pressure regulator knob is returned to zero, microwave plasma-generator installation's power source is cut off；
8. cutting off discharge-type vacuum meter power supply, communicate system with atmosphere, stops vacuum pump.
Step 3: the preparation of Y molecular screen membrane:
It takes silica solution 22.5435g that 8.463g sodium hydroxide is added, stirs evenly, form solution 3.,
Aluminum sulfate 6.6477g is dissolved with 95.89965g water, 3.906g sodium hydroxide is then added, stirs evenly, is formed molten
Liquid 4., then 4. solution is slowly dropped into solution 3. in, form gel before this, then become white solution.It is stirred until homogeneous.It is old
Change 9h, is then stirred to react liquid half an hour, will be put into reaction kettle, poured into the carrier for being loaded with crystal seed after corona treatment
Reaction solution.Seal reaction kettle.It is put into oven, 90 DEG C of crystallization 9h.Reaction kettle is taken out, reaction solution and carrier are poured out, by carrier ultrasound
It washs to neutrality.It is put into 120 DEG C of drying 8h of crucible.
Technical characteristic of the present invention without description can realize that details are not described herein by or using the prior art, certainly,
The above description is not a limitation of the present invention, and the present invention is also not limited to the example above, the ordinary skill of the art
The variations, modifications, additions or substitutions that personnel are made within the essential scope of the present invention also should belong to protection model of the invention
It encloses.
Claims (9)
1. a kind of method for preparing y-type zeolite membrane, which comprises the following steps:
Step 1: the preparation of nano Y-shaped molecular sieve:
By nNa2O:nSiO2: nAl2O3: nH2The molar ratio of O=16:16:1:210 prepares directed agents, after directed agents aging 19h,
Sulfuric acid solution is instilled into directed agents, is formed gel, is configured to nNa2O:nSiO2:nAl2O3:nH2O=7.8:16:1:400's is anti-
Liquid is answered, reaction solution is packed into reaction kettle, reaction kettle is put into insulating box, crystallization 8h at 100 DEG C takes the product in reaction kettle
Out, product is put into 120 DEG C of Muffle furnace drying, obtains diameter 100nm nano Y-shaped molecular sieve, molecular sieve after suction filtration and washing
Primary preparation can be in molecular screen membrane preparation using multiple；
Step 2: the pretreatment of carrier:
Alkali process: the sodium hydroxide solution of aluminium oxide ceramics ring carrier and 7mol/L are placed in flask, are heated to 110 DEG C of reflux
1h is handled, is cleaned 2-3 times under ultrasonic wave with deionized water, (each 10min), 600 DEG C of calcination 1h in Muffle furnace are then placed in；
Corona treatment: first will be by aluminium oxide ceramics ring carrier surface one layer of nano Y-shaped molecule of polishing after alkali process
Then sieve is loaded with the carrier of nano Y-shaped molecular sieve using Microwave plasma treatment；
Step 3: secondary growth method prepares y-type zeolite membrane:
Nano Y-shaped molecular sieve is planted in advance to porous Al using polishing mode2O3On ceramic ring carrier, and nano Y-shaped point will be planted in advance
After the carrier Microwave plasma treatment of son sieve, by Al2(SO4)3·18H2O, silica solution, sodium hydroxide and deionized water are pressed
According to n (Na2O): n (SiO2)/n(Al2O3)/n(H2O)=14:10:1:800 proportion is under room temperature and intense mechanical stirring condition
It is uniformly mixed into glue and is aged 9h respectively, the Al of nano Y-shaped molecular sieve will be planted in advance2O3Carrier hangs down after corona treatment
It is directly put into the stainless steel cauldron of polytetrafluoro liner, injection reaction glue seals reaction kettle, be placed in carrier is flooded completely
In constant temperature, is taken out in 90 DEG C of crystallization 9h, be washed with deionized to filtrate and be in neutrality, it is dry at 120 DEG C, Y type molecule is made
Sieve membrane.
2. the method according to claim 1 for preparing y-type zeolite membrane, which is characterized in that reflow treatment, which refers to, to be condensed back to
Stream, i.e., sodium hydroxide solution leaves after by thermal evaporation from heating end, reaches and is converted into drop again after by cold end, heating end with
By cold end in the same flask, and heated end position is lower, and drop, which just converges, flows back to heating end, and formation is condensed back to
Stream.
3. the method according to claim 1 for preparing y-type zeolite membrane, which is characterized in that deionized water, which refers to, to be eliminated
In the pure water after ionic species impurity.
4. the method according to claim 1 for preparing y-type zeolite membrane, which is characterized in that cleaning refers to benefit under ultrasonic wave
Liquid and dirt directly, are indirectly acted on cavitation, acceleration effect and the direct flow effect of ultrasonic wave in a liquid,
Make crud layer by dispersion, emulsification, removing and reach cleaning purpose.
5. the method according to claim 1 for preparing y-type zeolite membrane, which is characterized in that corona treatment refers to micro-
Wave corona treatment.
6. the method according to claim 5 for preparing y-type zeolite membrane, which is characterized in that Microwave plasma treatment
Time is 15min.
7. the method according to claim 1 for preparing y-type zeolite membrane, which is characterized in that polishing mode refers to: will prepare
Nano Y-shaped molecular sieve directly in Al2O3Grinding homogeneity on ceramic ring carrier rings front is rinsed with deionized water to remove Al2O3
The unattached firm nano Y-shaped molecular sieve particle of ceramic ring carrier ring surface.
8. the method according to claim 1 for preparing y-type zeolite membrane, which is characterized in that be vertically put into and refer to and will smear
The Al of nano Y-shaped molecular sieve2O3Ceramic ring carrier is put into reaction kettle vertically down, to prevent molecular sieve powder in carrier side
Upper deposition.
9. the method according to claim 1 for preparing y-type zeolite membrane, which is characterized in that y-type zeolite membrane is with a thickness of 5 μ
m。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113387370A (en) * | 2020-03-11 | 2021-09-14 | 中国科学院深圳先进技术研究院 | Method for adjusting crystal morphology and structure of zeolite molecular sieve by using low-temperature plasma technology |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279208A (en) * | 2008-05-20 | 2008-10-08 | 吉林大学 | Method for preparing Y type molecular sieve film |
| CN101696018A (en) * | 2009-10-27 | 2010-04-21 | 华南理工大学 | Method for synthesizing silicalite-1 zeolite membranes |
-
2019
- 2019-07-19 CN CN201910654796.5A patent/CN110228813A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279208A (en) * | 2008-05-20 | 2008-10-08 | 吉林大学 | Method for preparing Y type molecular sieve film |
| CN101696018A (en) * | 2009-10-27 | 2010-04-21 | 华南理工大学 | Method for synthesizing silicalite-1 zeolite membranes |
Non-Patent Citations (1)
| Title |
|---|
| 甄铁丽: "纳米 NaY 型分子筛及分子筛膜的制备", 《中国学位论文全文数据库》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113387370A (en) * | 2020-03-11 | 2021-09-14 | 中国科学院深圳先进技术研究院 | Method for adjusting crystal morphology and structure of zeolite molecular sieve by using low-temperature plasma technology |
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Application publication date: 20190913 |