CN105013337A - Method for quickly synthesizing Y-type molecular sieve membrane and application of Y-type molecular sieve membrane in biological alcohol and water mixed solution separation - Google Patents
Method for quickly synthesizing Y-type molecular sieve membrane and application of Y-type molecular sieve membrane in biological alcohol and water mixed solution separation Download PDFInfo
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- CN105013337A CN105013337A CN201410156691.4A CN201410156691A CN105013337A CN 105013337 A CN105013337 A CN 105013337A CN 201410156691 A CN201410156691 A CN 201410156691A CN 105013337 A CN105013337 A CN 105013337A
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- molecular sieve
- supporter
- type molecular
- sieve membrane
- zeolite membrane
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Abstract
The invention provides a preparation method for quickly synthesizing a Y-type molecular sieve membrane and application of the Y-type molecular sieve membrane in biological alcohol and water mixed solution separation. The method is characterized in a novel microwave synthesis method is adopted to uniformly synthesize a densely continuous NaY-type molecular sieve membrane on the outer surface of a mullite and stainless steel tubular supporting body. In the preparation process, the synthesis time is short, the membrane forming process is simple, and the defects of the prepared membrane can be suppressed and greatly reduced. By adoption of a customized pervaporation device, the synthesized NaY-type molecular sieve membrane is used for separating a biological alcohol and water mixed solution. The separation process is simple and easy to operate and control, and the separation performance is excellent. When applied to a butanol/water mixture and an ethyl alcohol/water mixture, the molecular sieve membrane is high in permeation flux and large in separation factor, and particularly the NaY-type molecular sieve membrane synthesized by the stainless steel supporting body is extremely high in permeation flux.
Description
Technical field
The invention provides Fast back-projection algorithm y-type zeolite membrane and the application in bio-alcohol water mixed solution is separated thereof, belong to inorganic material permeability and separation field.
Background technology
Membrane separation technique is one of important separation method of Recent study.Due to the more economic environmental protection of separating technology that membrane separation process is more traditional, and have desirable Energy Efficiency Ratio, membrane separation technique is widely used in the water treatment field in chemical industry, oil, environment and food, electronics industry by work.In the past few decades, various organic film and inoranic membrane are used for the practical technical fields such as micro-filtration, nanofiltration, dialysis, counter-infiltration, infiltration evaporation, Steam soak and gas separaion.
Infiltration evaporation and Steam soak technology are the important means of industrial separation and azeotropic azeotropic mixture.Apply the important component part that this technology water deviate from organic matter or mixed solvent has become application of membrane separation technology.And the organic mixture utilizing infiltration evaporation to be separated with Steam soak mainly contains a few class mixtures such as alcohol-water mixture, alcohol-ether mixture, aromatic hydrocarbon isomers, aromatic hydrocarbon and alkane.
Microwave heating method utilizes microwave to heat to synthesis liquid the method carrying out synthesis zeolite film.Compared with traditional heating method, microwave heating method can heat Reactive Synthesis liquid rapidly, equably, shorten crystallization time, can within the scope of wider synthesis condition synthesis zeolite film, and be conducive to synthesizing that purity is high, crystal size is homogeneous, crystal layer is thinner zeolite molecular sieve film.At present, the zeolite molecular sieve film of microwave heating method synthesis is adopted to have NaA type, FAU type (NaX and NaY), MFI type, T-shaped, ALPO-5 type etc.
Weh etc. (Micropor. Mesopor. Mater, 2002,54:27-36) adopt microwave heating method, are 10SiO in gel proportioning
2: 1Al
2o
3: 14Na
2o:840H
2in the system of O, at synthesis temperature 120
ounder C, generated time 2 h, prepare the FAU type molecular sieve crystal rete that thickness is about l ~ 2 um; Repeat synthesis, obtain the FAU type molecular sieve crystal rete that thickness is about 5.0 ~ 6.0 um, this film is applied to N respectively
2/ CO
2and CH
4/ CO
2mixed system, 23
oduring C, separation selectivity is respectively 5.5,3.5.Shen Yongde (Nanjing University of Technology, 2006,6) adopts microwave heating method, mole is consisting of 25SiO
2: 1Al
2o
3: 22Na
2o:990H
2in the synthesized gel rubber of O, 100
ounder C, crystallization 40 min, obtained thickness is about the NaY type molecular screen membrane of 10 um, and time this film infiltration evaporation Separation of Water/ethanol system (10/90 wt%), separation factor reaches 104, and the permeation flux of its correspondence is 1.31 kg m
-2h
-1.Compared with traditional heating method, microwave heating method not only substantially reduces generated time, and has synthesized the NaY type molecular screen membrane with thinner crystal layer.At present, about the Microwave synthesize of NaY type molecular screen membrane mainly concentrates on OH
-route, adopts fluorine route in microwave, synthesize NaY type molecular screen membrane and is not reported so far, and in colloidal sol regulation and control, fluorine route synthesis of molecular sieve is important means, and it has a lot of advantage: F
-mainly play mineralizer or template effect, the formation of framework of molecular sieve Si-O-Si key can be promoted.The synthesis of fluorine route also improves the degree of crystallinity of crystal and decreases crystal defect (Zeolites, 12 (8), 929-35,1992).In addition report fluoride is had also can to change molecular sieve crystal skeleton
nsi/
nal (Chem. J. Chinese U., 19 (6), 930-933,1986), the hydrophily of regulatory molecule sieve plane of crystal.
The present invention adopts microwave hydrothermal Fast back-projection algorithm condition in fluorine-containing system to prepare Y molecular sieve film, improves crystal structure degree and shortens generated time, decreasing the thickness of rete, add the stability of film under high-temperature operation condition.And preparation flow is very simple, quick.The supporter mechanical strength adopted is high, is suitable for commercial Application.The membrane surface molecule sieve crystal growth synthesized under optimal conditions is good, and defect is considerably less.The Y molecular sieve film of gained has good separation selectivity in bio-alcohol water mixed solution is separated.
Summary of the invention
The object of this invention is to provide a kind of high-performance infiltration evaporation NaY type molecular screen membrane preparation method and its separation process in organic mixture.The present invention is optimized the composition of raw materials in the preparation of NaY type molecular screen membrane, synthesis condition, by high-temperature water thermal synthesis, shortens the generated time of film.Utilize this method on porous supporting body, synthesized high-purity, growth continuous print molecular screen membrane, and have that generated time is short, the simple feature of preparation process.This molecular screen membrane can realize methyl alcohol/methyl tertiary butyl ether(MTBE), ethanol/ethyl tert-butyl ether (ETBE), and benzene/cyclohexane organic mixture high selectivity is separated.
The method of Fast back-projection algorithm y-type zeolite membrane of the present invention is as follows:
1, be silicon source with waterglass, take sodium metaaluminate as aluminium source, aluminium source, as alkali raw material, is dissolved in sodium hydroxide solution by NaOH, then adds silicon source under stirring state, finally adds fluorine source, preparation raw material liquid SiO
2-Al
2o
3---Na
2o-MF-H
2o (M=NH
4, Li, Na, K) system, each component mol ratio is:
SiO
2/Al
2O
3=15～30,
Na
2O/SiO
2=0.5～2.5,
H
2O/Na
2O=25～80，
MF/SiO
2 =0.1～0.8
2, continue stirring 1 ~ 3 h, be then placed in still aging 6 ~ 12 h of airtight polytetrafluoroethylcontainer container room temperature.
3, aging good colloidal sol adds in stainless steel cauldron, and is vertically inserted in colloidal sol by the tubular porous supporter of precoating kind, and colloidal sol liquid level needs submergence supporter.Insert in microwave reactor, temperature 100 ~ 150
oc synthesizes, hydro-thermal reaction time 2 ~ 9 h; This supporter is tubular porous mullite or stainless steel.
4, reacted rear taking-up, washed away surperficial alkali lye, washed with de-ionized water 24 h, dried.
In the present invention, supporter average pore size is 0.1 ~ 10 μm, supporter porosity 30 % ~ 60 %; Pipe external diameter 8 ~ 15 mm of supporter, supporter thickness of pipe wall 1 ~ 3 mm.
There are silica flour, Ludox and sodium metasilicate in the silicon source that the inventive method material liquid adopts; There are aluminium hydroxide, sodium metaaluminate in the aluminium source adopted; The alkali adopted is NaOH; There is NH in the fluorine source adopted
4f, NaF, KF, LiF.
In the present invention, hydro-thermal reaction optimum condition is: temperature 100
oduring C, reaction time 4.5 ~ 8 h; Temperature 120
oduring C, reaction time 3.0 ~ 5 h.
The NaY type molecular screen membrane average thickness synthesized is at 8 ~ 13 μm.Coating growth is good, continuously and be evenly distributed, the defect such as free of pinholes, crack.
The present invention adopts water/organic admixture to characterize the performance of synthesis film.Water/the butanol mixture of the water/organic matter adopted to be moisture be 5 wt%, operating temperature is 75
oc.Because this system is simple to operate, in film synthesis optimizing process, adopt this system characterization of membrane, instructed the optimization of film by permeation data.
Water/organic admixture the system adopted has:
Material liquid 1: the mass fraction containing butanols is the butanol/water mixture of 95 wt%, operating temperature is 75 ° of C.
Material liquid 2: the mass fraction containing ethanol is the ethanol/water mixture of 10 wt%, operating temperature is 75 ° of C.
Accompanying drawing explanation
Fig. 1 is the installation drawing of the infiltration evaporation performance of the NaY type molecular screen membrane detecting synthesis.
Fig. 2 is at the NaY type molecular screen membrane surface Electronic Speculum figure that porous mullite supporter outer surface is formed.
Fig. 3 is the NaY type molecular screen membrane section Electronic Speculum figure formed at porous mullite supporter outer surface.
Fig. 4 is mullite supporter (a), fluorine-containing NaY type molecular screen membrane (b) of system synthesis of microwave, (c) XRD of NaY type molecular screen membrane crystal seed scheme.
In order to further describe the present invention, shown below is several concrete case study on implementation, but patent right is not limited to these examples.
Specific embodiment
Embodiment 1
Adopt waterglass to be silicon source, aluminium hydroxide is aluminium source, and NaOH and deionized water are synthesis liquid raw material.
The supporter that the porous mullite pipe adopting Japanese Nikkato Co., Ltd. to produce synthesizes as film, mullite consists of 67 wt%Al
2o
3with 33 wt%SiO
2.Supporter, after 800 order sand paperings and ultrasonic cleaning, applies one deck NaY type molecular sieve crystal seed.
Aluminium hydroxide and NaOH are dissolved in deionized water, and adding waterglass formation mol ratio is under agitation 25SiO
2: 1Al
2o
3: 22Na
2o:7.5NH
4f:990H
2the mixed liquor of O, continues stirring 2 h colloidal sol.This colloidal sol is placed in airtight polytetrafluoroethylcontainer container at room temperature still aging 12 h.Colloidal sol after ageing is poured in airtight stainless steel cauldron, and the supporter scribbling NaY molecular sieve crystal seed in advance is vertically put into reactor, and ensures that colloidal sol liquid level is higher than supporter.And insert in the baking oven of 100 ° of C and react 6.5 h.
The film of synthesis, with first repeatedly rinsing by deionized water, to wash the alkali lye adsorbed in the amorphous substance of the surperficial and inwall of film and supporter, then continues to wash 24 h by deionized water, film under 100 ° of C dry 12 h with for subsequent use.
The infiltration evaporation performance of the film of synthesis is undertaken measuring by the device shown in Fig. 1.Film pipe is placed in tubular type stainless steel mould, with the seal with elastometic washer of O shape.This mould is placed in oven environment, and feeding liquid flows through the outer surface of molecular screen membrane.This tubular membrane inner chamber connects vacuum plant.The admixture of gas of infiltration is collected in cold-trap by liquid nitrogen condensation.Infiltration evaporation is adopted to detect infiltration evaporation flux, the separation that directly can obtain film, thus direct evaluated for film performance.
The infiltration evaporation performance of film is by permeation flux
jand separation
αtwo Parametric Representations.Permeation flux
jthe material gross mass of the film of unit are is penetrated through in the representation unit time.
j=unit interval interior the quality through thing/(unit interval × membrane area), unit is kg/m
2h; Separation
αfor the height of evaluated for film separative efficiency,
α=(Y
a / Y
b )/(X
a / X
b ), wherein Y
a with Y
b be illustrated respectively in penetrant
awith
bthe mass concentration of two kinds of components, X
a with X
b be illustrated respectively in material liquid
awith
bthe mass percent concentration of two kinds of components.Component
a,
bcontent adopt GC-14 type gas chromatographic detection.
The film of synthesis is applied to 75 ° of C, the infiltration evaporation of water/butanols (5/95 wt%) system.The infiltration evaporation performance of the NaY type molecular screen membrane that table 1 is prepared under showing different condition.
Embodiment 2:
Synthetic ratio is identical with embodiment 1 with preparation process.Unlike crystallization temperature being increased to 110 ° of C.The film that generated time is reduced to 5 h synthesis investigates the infiltration evaporation performance of film after treatment.Its result performance is as shown in table 1.
Embodiment 3:
Synthetic ratio is identical with embodiment 1 with preparation process.Unlike crystallization temperature being increased to 120 ° of C, generated time is reduced to 4 h.The film of synthesis after treatment, investigates the infiltration evaporation performance of film.Its result performance is as shown in table 1.
Effective XRD and the SEM instrument of film after supporter before synthesis, synthesis is characterized, the JSM-6350 of XRD to be Japanese Shimadzu (SHIMADZU) company XRD-6100, SEM be NEC (JEOL) company.
Fig. 2 shows the surface microstructure of the NaY type molecular screen membrane synthesized on porous mullite supporter.Supporting body surface is covered by one deck NaY type molecular sieve crystal, and molecular sieve crystal is staggered, compact growth.
Fig. 3 shows the cross-section morphology synthesizing the NaY type molecular screen membrane of film on mullite supports.As seen from the figure, grown one deck molecular sieve rete fine and close continuously at open support external surface, there is more fine and close intermediate layer between film top layer and supporter, rete gross thickness is about 8 ~ 12 μm.
Fig. 4 is X-ray diffraction (XRD) comparison diagram of porous mullite supporter, synthesis NaY type molecular screen membrane, NaY type molecular sieve crystal.As shown in the figure, the film of synthesis has obvious NaY type molecular sieve crystal seed characteristic peak, shows that the outer surface of porous supporting body grown one deck continuous print NaY molecular sieve crystal.
Embodiment 4:
Changing synthesis colloidal sol proportioning is 25SiO
2: 1Al
2o
3: 22Na
2o:7.5NH
4f:1540H
2o, preparation process is identical with embodiment 1.Crystallization condition is crystallization 9 h under 120 ° of C hydrothermal conditions.The infiltration evaporation performance of synthesis film to water/ethanol (10/90 wt%) system is as shown in table 1.
Embodiment 5:
Changing synthesis colloidal sol proportioning is 25SiO
2: 1Al
2o
3: 22Na
2o:12.5NH
4f:990H
2o, preparation process is identical with embodiment 1.Crystallization condition is crystallization 4 h under 120 ° of C hydrothermal conditions.The infiltration evaporation performance of synthesis film to water/butanols (5/95 wt%) system is as shown in table 1.
Embodiment 6:
Changing synthesis colloidal sol proportioning is 30SiO
2: 1Al
2o
3: 22Na
2o:7.5NH
4f:990H
2o, preparation process is identical with embodiment 1.Crystallization condition is crystallization 4 h under 120 DEG C of hydrothermal conditions.The infiltration evaporation performance of synthesis film to water/ethanol (10/90 wt%) system is as shown in table 1.
Embodiment 7:
Adopt the tubulose α-Al that German Schumacker GmbH company produces
2o
3as the matrix of film synthesis.Supporter, after 800 order sand paperings and ultrasonic cleaning, applies one deck NaY type molecular sieve powder.Synthesis colloidal sol proportioning is identical with embodiment 1 with preparation process.Under 100 ° of C hydrothermal conditions, crystallization 6.5 h, rinses repeatedly by deionized water after taking-up.Synthesis film is applied to 75 DEG C, and the infiltration evaporation performance of water/ethanol (10/90 wt%) system is as shown in table 1.
Embodiment 8:
The tubulose stainless steel that supporter adopts Mott company of the U.S. to produce.Supporter dries after the pretreatment such as ultrasonic cleaning, for subsequent use after supporter outer surface mechanical application skim NaY type molecular sieve powder.
Synthesis colloidal sol proportioning is identical with embodiment 1 with preparation process.Crystallization 6.5 h under 100 ° of C hydrothermal conditions.Synthesis film is applied to 75 ° of C, and the infiltration evaporation performance of water/ethanol (10/90 wt%) system is as shown in table 1.
Embodiment 9(applies):
The molecular screen membrane synthesized under embodiment 1 condition is applied to the osmotic system of material liquid 1 and material liquid 2, investigates the vaporization permeance property of film.Its result is as shown in table 2.
Embodiment 10(applies):
The molecular screen membrane synthesized under embodiment 8 condition is applied to the osmotic system of material liquid 1 and material liquid 2, investigates the vaporization permeance property of film.Its result is as shown in table 2.
The synthesis condition of table 1 embodiment 1-8 and permeance property
| SiO 2/Al 2O 3 | Na 2O/SiO 2 | H 2O/ Na 2O | Supporter | Synthesis temperature/ oC | Generated time/h | Flux J / kg/m 2·h | Separation factor α | |
| Embodiment 1 | 25 | 0.88 | 45 | Mullite | 100 | 6.5 | 3.50 | 2500 |
| Embodiment 2 | 25 | 0.88 | 45 | Mullite | 110 | 5.0 | 3.19 | 1800 |
| Embodiment 3 | 25 | 0.88 | 45 | Mullite | 120 | 4.0 | 3.45 | 2040 |
| Embodiment 4 | 25 | 0.88 | 70 | Mullite | 120 | 9.0 | 2.56 | 1090 |
| Embodiment 5 | 25 | 0.88 | 45 | Mullite | 120 | 4.0 | 3.70 | 1010 |
| Embodiment 6 | 30 | 0.73 | 45 | Mullite | 120 | 4.0 | 3064 | 45 |
| Embodiment 7 | 25 | 0.88 | 45 | Aluminium oxide | 100 | 6.5 | 3.14 | 3050 |
| Embodiment 8 | 25 | 0.88 | 45 | Stainless steel | 100 | 6.5 | 6.80 | 1050 |
Note: osmotic system: 75 DEG C, water/butanols (5/95 wt%);
The film that table 2 synthesizes is applied to infiltration evaporation (vaporization infiltration) performance under different infiltration condition
Claims (7)
1. the method for a Fast back-projection algorithm y-type zeolite membrane, it is characterized in that adopting homemade high activity Y zeolite crystal seed, by secondary growth method, form the Y type molecular formula film of one deck Thief zone performance at perforated tubular supporter outer surface fast, it is prepared as follows:
Be silicon source with waterglass, take sodium metaaluminate as aluminium source, aluminium source, as alkali raw material, is dissolved in sodium hydroxide solution by NaOH, then adds silicon source under stirring state, finally adds fluorine source, preparation raw material liquid SiO
2-Al
2o
3---Na
2o-MF-H
2o (M=NH
4, Li, Na, K) system, each component mol ratio is:
SiO
2/Al
2O
3=20～50，
Na
2O/SiO
2=0.5～3，
H
2O/Na
2O=20～80
MF/SiO
2 =0.1～1；
Continue stirring 1 ~ 3 h, be then placed in still aging 6 ~ 12 h of airtight polytetrafluoroethylcontainer container room temperature;
The colloidal sol prepared adds in Microwave synthesize reactor, and is vertically inserted in colloidal sol by the tubular porous supporter of precoating kind, and colloidal sol liquid level needs submergence supporter.
2. temperature 100 ~ 150
oc synthesizes, hydro-thermal reaction time 2 ~ 9 h;
Reacted rear taking-up, deionized water is rinsed repeatedly, to film surface in neutral, dries.
3. the method for Fast back-projection algorithm y-type zeolite membrane according to claim 1, is characterized in that hydrothermal temperature is 100 ~ 120
oc, Hydrothermal Synthesis 3 ~ 7 h.
4. the method for Fast back-projection algorithm y-type zeolite membrane according to claim 1, is characterized in that: each component mol ratio is: SiO
2/ Al
2o
3=15 ~ 30, Na
2o/SiO
2=0.5 ~ 2.5, H
2o/Na
2o=25 ~ 80, MF/SiO
2=0.1 ~ 0.8
According to the method for the Fast back-projection algorithm y-type zeolite membrane described in claim 1, it is characterized in that: the average pore size adopting porous pipe type supporter is 0.1 ~ 10 μm, and porosity is 30% ~ 60%, and pipe external diameter is 8 ~ 15 mm, and thickness of pipe wall is 0.5 ~ 3 mm.
5. the method for the Fast back-projection algorithm y-type zeolite membrane according to claim 1-4, is characterized in that: the y-type zeolite membrane that mullite supporter synthesizes, is applied to 75
oflux and the separation factor of C, butanol/water mixture (95/5 wt%) system are respectively 3.50 kg/m
2h and 2500.
6. the method for the Fast back-projection algorithm y-type zeolite membrane according to claim 1-4, is characterized in that: the y-type zeolite membrane that mullite supporter synthesizes, is applied to 75
oflux and the separation factor of C, ethanol/water mixture (90/10 wt%) system are respectively 1.9 kg/m
2h and 900.
7. the method for Fast back-projection algorithm y-type zeolite membrane according to claim 1, it is characterized in that tubular type support body material is porous stainless steel, mullite and aluminium oxide, porous stainless steel supporter is that preferably flux stainless steel supporter synthesizing film is more than 2 times of mullite supporter.
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|---|---|---|---|
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|---|---|---|---|
| CN201410156691.4A CN105013337A (en) | 2014-04-18 | 2014-04-18 | Method for quickly synthesizing Y-type molecular sieve membrane and application of Y-type molecular sieve membrane in biological alcohol and water mixed solution separation |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108786478A (en) * | 2018-05-04 | 2018-11-13 | 河南工程学院 | The preparation method of membrane distillation composite membrane |
| CN110508158A (en) * | 2019-08-12 | 2019-11-29 | 上海工程技术大学 | A method of preparing ultra-thin SAPO-34 molecular screen membrane |
| CN112808028A (en) * | 2020-12-23 | 2021-05-18 | 华南理工大学 | Method for rapidly preparing ultrathin UiO-66 film under assistance of microwaves and ultrathin UiO-66 film prepared by method |
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| CN101716470A (en) * | 2009-11-05 | 2010-06-02 | 江西师范大学 | Method for preparing fluorine-containing mordenite zeolite membrane |
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2014
- 2014-04-18 CN CN201410156691.4A patent/CN105013337A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101716470A (en) * | 2009-11-05 | 2010-06-02 | 江西师范大学 | Method for preparing fluorine-containing mordenite zeolite membrane |
Non-Patent Citations (1)
| Title |
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| 沈永德: "NaY型分子筛膜的制备", 《中国优秀博硕士学位论文全文数据库 (硕士)工程科技Ⅰ辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108786478A (en) * | 2018-05-04 | 2018-11-13 | 河南工程学院 | The preparation method of membrane distillation composite membrane |
| CN110508158A (en) * | 2019-08-12 | 2019-11-29 | 上海工程技术大学 | A method of preparing ultra-thin SAPO-34 molecular screen membrane |
| CN110508158B (en) * | 2019-08-12 | 2021-10-08 | 上海工程技术大学 | Method for preparing ultrathin SAPO-34 molecular sieve membrane |
| CN112808028A (en) * | 2020-12-23 | 2021-05-18 | 华南理工大学 | Method for rapidly preparing ultrathin UiO-66 film under assistance of microwaves and ultrathin UiO-66 film prepared by method |
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