CN107930411A - The preparation method and device of a kind of molecular screen membrane - Google Patents
The preparation method and device of a kind of molecular screen membrane Download PDFInfo
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- CN107930411A CN107930411A CN201711380381.0A CN201711380381A CN107930411A CN 107930411 A CN107930411 A CN 107930411A CN 201711380381 A CN201711380381 A CN 201711380381A CN 107930411 A CN107930411 A CN 107930411A
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- molecular screen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/36—Pervaporation; Membrane distillation; Liquid permeation
- B01D61/362—Pervaporation
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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
- B01D67/0051—Inorganic membrane manufacture by controlled crystallisation, e,.g. hydrothermal growth
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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
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2475—Membrane reactors
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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
- C01B39/14—Type A
- C01B39/16—Type A from aqueous solutions of an alkali metal aluminate and an alkali metal silicate excluding any other source of alumina or silica but seeds
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
- B01J2219/00081—Tubes
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Water Supply & Treatment (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The present invention relates to the preparation method and device of a kind of molecular screen membrane, belong to molecular screen membrane preparing technical field.Porous supporting body is fixed in the reaction kettle tubulation of membrane reactor；Molecular sieve seed suspension is delivered to the inner cavity of porous supporting body in membrane reactor afterwards, and is flowed 1~60 second in speed loop of the surface of internal cavity using speed as 50~200mL/min；The crystal seed suspension of reverse circulation discharge afterwards, drying；Film making solution is finally sent into membrane reactor, crystallization synthetic reaction is carried out, porous supporting body is taken out after reaction and washs and dries, that is, obtains NaA molecular sieve inner membrance.The problem of brilliant process and the relatively independent process of film-forming process are applied when preparing molecular screen membrane is this method solve, the molecular screen membrane of this method synthesis, repeatability is high, function admirable.
Description
Technical field
The invention belongs to the painting in molecular screen membrane preparing technical field, more particularly to a kind of preparation process by molecular screen membrane is brilliant
Process and the integrated method of film making process.
Background technology
Molecular sieve infiltration evaporation membrane separation technique is a kind of new separation technology, have it is energy-efficient, process is easily controllable,
It is easy to operate, easy to amplifying and the advantages that industrialization, played in new energy development, optimizing network resource utilization and environmental protection etc.
More and more important effect, is one of 21 century most promising new and high technology.Molecular screen membrane is used for dehydration of organic solvent
Research start from last century the nineties, realized the large-scale industrial application of NaA molecular sieve membrane at present, built up about in the whole world
400 sets of industrial dehydration devices.The synthesis of the molecular screen membrane of the prior art will apply in brilliant process and building-up process in operation
Separately carry out, add artificial influence factor, cause film building-up process batch quality unstable, particularly in industrialized production
When, performance has different, such as flux, separation factor and microstructural difference between the finished product of each batch, this is also to restrict
One of Pinch technology of its large-scale industrial production.
The content of the invention
The technical problems to be solved by the invention are to realize the brilliant process of painting and crystallization process one in the same apparatus
Change and carry out, reduce the influence that human factor synthesizes film, improve the lot stability of film synthesis, specific technical solution
It is：
A kind of integral preparation method of supporter inner surface molecular screen membrane, this method comprise the following steps：
1st step：Porous supporting body is fixed in the reaction kettle tubulation of membrane reactor；
2nd step：Molecular sieve seed suspension is delivered to the inner cavity of porous supporting body in membrane reactor, and in surface of internal cavity
Flowed 1~60 second for the speed loop of 50~200mL/min with speed DEG C；The crystal seed suspension of reverse circulation discharge afterwards, drying；
3rd step：Film making solution is sent into membrane reactor, crystallization synthetic reaction is carried out, after reaction by porous supporting body
Take out and wash and dry, that is, obtain NaA molecular sieve inner membrance.
In technical solution of the present invention：The configuration of the porous supporting body is the doughnut of single hose, multi-channel type.
In technical solution of the present invention：The porous supporting body is horizontally or vertically fixed in membrane reactor tubulation.
In technical solution of the present invention：The drying of 2nd step, which uses heat source, to be conduction oil, hot water or water vapour.
In technical solution of the present invention：The drying temperature DEG C of 2nd step is 30-120 DEG C；As preferred：The drying temperature DEG C of 2nd step is
50-70℃。
In technical solution of the present invention：The temperature DEG C of 3rd step synthetic reaction is 30-180 DEG C；As preferred：3rd step synthetic reaction
Temperature DEG C be 80-120 DEG C.
In some preferred technical solutions：Synthetic reaction, which uses heat source, to be conduction oil, hot water or water vapour.
In technical solution of the present invention：Solution used in film is that addition sodium hydroxide and deionized water are abundant in sodium metaaluminate
Stirring, forms aluminum solutions, sodium metasilicate is added after clarification, is formed after stirring and prepares NaA type molecular screen membranes.
In technical solution of the present invention：The proportioning of film making solution is：Al2O3:SiO2:Na2O:H2O=1：1：1~5：100~
200。
A kind of device for being used for realization the method, the device include membrane reactor and the envelope positioned at reactor both ends
Head, reaction kettle tubulation are located in the inner cavity of membrane reactor, and porous supporting body is fixed on membrane reactor by O-ring and pressing plate
Reaction kettle tubulation surface, is equipped with heat source fluidized bed between reaction kettle tubulation and membrane reactor inner wall.
Beneficial effect：
Use technical solution of the present invention to synthesize NaA type molecular sieve inner membrance of the length for 800mm, be used to separate at 70 DEG C
When feed liquid is the ethanol/water solution system that water content is 5wNaA.%, the separation factor of film>1000, flux>2.0kg·h–1·
m–2, with high selectivity and permeation flux.Compared with prior art, the present invention innovatively proposes that brilliant process and crystallization will be applied
Process integration system is standby, eliminates influence of the human factor to seeding carrier after painting crystalline substance, reduces the loading and unloading of film, and the party
Method is simple, easy, during the preparation for the molecular sieve inner membrance being applied to, can make into film uniformity raising, film properties are improved.Profit
The NaA type molecular sieve inner membrances synthesized with the method for the present invention are compared with the performance of existing market molecular screen membrane, and repeatability is high, performance
It is excellent, it is adapted to scale industrial production.
Brief description of the drawings
Fig. 1 is the preparation facilities schematic diagram of the molecular screen membrane of the present invention；
Fig. 2 is the film surface field emission scanning electron microscope (SEM) photograph for the molecular screen membrane that the embodiment of the present invention 1 synthesizes；
Fig. 3 is the film section field emission scanning electron microscope (SEM) photograph for the molecular sieve inner membrance that the embodiment of the present invention 1 synthesizes；
Wherein, 1, end socket；2nd, heat source fluidized bed；3rd, reaction kettle tubulation；4th, O-ring；5th, pressing plate；6th, porous supporting body.
Embodiment
With reference to embodiment, the invention will be further described, but protection scope of the present invention not limited to this：
A kind of preparation facilities of molecular screen membrane, the device include membrane reactor and the end socket (1) positioned at reactor both ends,
Reaction kettle tubulation (3) is located in the inner cavity of membrane reactor, and porous supporting body (6) is fixed on by O-ring (4) and pressing plate (5)
The reaction kettle tubulation surface of membrane reactor, is equipped with heat source fluidized bed (2) between reaction kettle tubulation (3) and membrane reactor inner wall.
Embodiment 1
The fixation of step 1, supporter
The single tube porous supporting body 6 of two end seal glaze is fixed in reaction kettle tubulation using O-ring 4 and pressing plate 5, and is sealed
Both ends end socket 1.
Step 2：The preparation of seeding supporter
As shown in Figure 1, porous supporting body is fixed in the reaction kettle tubulation of membrane reactor.Crystal seed 10g is weighed afterwards, point
Dissipate in 990g deionized waters, and in the crystal seed tank being contained on blender, stir and ultrasonic, obtain molecular sieve seed suspension
Liquid；A type molecular sieve crystal seed suspension is then delivered to supporter 6 by conveying device constant flow pump with 100mL/min flow velocitys
Inner cavity, circulates 5s, next circulates middle seed-solution in emptying 6 inner cavity of supporter and reaction kettle with reverse direction, then
Open conduction oil heat source and set heat conduction oil temperature as 60 DEG C, dry 5h, it is rear spare
Step 3：Prepare NaA type molecular screen membranes
Sodium metaaluminate is added into sodium hydroxide and deionized water is sufficiently stirred, aluminum solutions is formed, silicic acid is added after clarification
Sodium, forms the film making solution for preparing NaA type molecular screen membranes, its component is that mol ratio is after stirring：Al2O3：SiO2：Na2O：H2O
=1:1:3.5:155.Pumped using slurries and film making solution is delivered to sealing reaction kettle, later on heat-conducting oil heating system makes system
Coating solution temperature, which reaches, carries out Hydrothermal Synthesiss at 80 DEG C.Taken out after reaction 4h, then seal off first 1, pressing plate 5, O-ring 4, unload porous
Supporter membrane tube, cleaning and dipping membrane tube to pH are put into 50 DEG C of oven for drying after being 7-8 or so.
Repeat aforesaid operations 5 times, prepare 5 single tube NaA molecular sieve inner membrances.
Embodiment 2
The fixation of step 1, supporter
The four-way supporter 6 of two end seal glaze is fixed in reaction kettle tubulation using O-ring 4 and pressing plate 5, and seals two
End seal first 1.
Step 2：The preparation of seeding supporter
As shown in Figure 1, weighing crystal seed 10g, it is scattered in 990g deionized waters, and the crystal seed tank being contained on blender
In, stir and ultrasonic, obtain molecular sieve seed suspension；A type molecular sieve crystal seed suspension is then passed through into conveying device constant current
Pump is delivered to the inner cavity of supporter 6 with 150mL/min flow velocitys, circulates 15s, next circulates emptying support with reverse direction
Middle seed-solution in 6 inner cavity of body and reaction kettle, later on conduction oil heat source set heat conduction oil temperature as 50 DEG C, dry 5h, after
It is spare.
Step 3：Prepare NaA type molecular screen membranes
Sodium metaaluminate is added into sodium hydroxide and deionized water is sufficiently stirred, aluminum solutions is formed, silicic acid is added after clarification
Sodium, forms the film making solution for preparing NaA type molecular screen membranes, its component is that mol ratio is after stirring：Al2O3：SiO2：Na2O：H2O
=1:1:2:150.Pumped using slurries and film making solution is delivered to sealing reaction kettle, later on heat-conducting oil heating system makes film
Solution temperature, which reaches, carries out Hydrothermal Synthesiss at 100 DEG C.Taken out after reaction 4h, then seal off first 1, pressing plate 5, O-ring 4, unload porous
Supporter membrane tube, cleaning and dipping membrane tube to pH are put into 50 DEG C of oven for drying after being 7-8 or so.
Repeat aforesaid operations 5 times, prepare 5 four-way NaA molecular sieve inner membrances.
Embodiment 3
The fixation of step 1, supporter
7 channel support bodies 6 of two end seal glaze are fixed in reaction kettle tubulation using O-ring 4 and pressing plate 5, and seal two
End seal first 1.
Step 2：The preparation of seeding supporter
As shown in Figure 1, weighing crystal seed 10g, it is scattered in 990g deionized waters, and the crystal seed tank being contained on blender
In, stir and ultrasonic, obtain molecular sieve seed suspension；A type molecular sieve crystal seed suspension is then passed through into conveying device constant current
Pump is delivered to the inner cavity of supporter 6 with 180mL/min flow velocitys, circulates 45s, next circulates emptying support with reverse direction
Middle seed-solution in 6 inner cavity of body and reaction kettle, later on conduction oil heat source set heat conduction oil temperature as 70 DEG C, dry 5h, after
It is spare
Step 3：Prepare NaA type molecular screen membranes
Sodium metaaluminate is added into sodium hydroxide and deionized water is sufficiently stirred, aluminum solutions is formed, silicic acid is added after clarification
Sodium, forms the film making solution for preparing NaA type molecular screen membranes, its component is that mol ratio is after stirring：Al2O3：SiO2：Na2O：H2O
=1:1:2:120.Pumped using slurries and film making solution is delivered to sealing reaction kettle, later on heat-conducting oil heating system makes film
Solution temperature, which reaches, carries out Hydrothermal Synthesiss at 120 DEG C.Taken out after reaction 4h, then seal off first 1, pressing plate 5, O-ring 4, unload porous
Supporter membrane tube, cleaning and dipping membrane tube to pH are put into 50 DEG C of oven for drying after being 7-8 or so.
Repeat aforesaid operations 5 times, prepare 7 four-way NaA molecular sieve inner membrances.
Reference examples 1：
The fixation of step 1, supporter
The single tube porous supporting body of two end seal glaze is fixed in the brilliant component of painting.
Step 2：The preparation of seeding supporter
As shown in Figure 1, weighing crystal seed 10g, it is scattered in 990g deionized waters, and the crystal seed tank being contained on blender
In, stir and ultrasonic, obtain molecular sieve seed suspension；A type molecular sieve crystal seed suspension is then passed through into conveying device constant current
Pump is delivered to the inner cavity of supporter 6 with 100mL/min flow velocitys, circulates 5s, next circulates emptying support with reverse direction
Middle seed-solution in 6 inner cavity of body and reaction kettle, removes and applies brilliant component, draw off seeding porous supporting body, be put into baking oven and dry
5h, it is rear spare
Step 3：Prepare NaA type molecular screen membranes
Sodium metaaluminate is added into sodium hydroxide and deionized water is sufficiently stirred, aluminum solutions is formed, silicic acid is added after clarification
Sodium, forms the film making solution for preparing NaA type molecular screen membranes, its component is that mol ratio is after stirring：Al2O3：SiO2：Na2O：H2O
=1:1:2:120.Then seeding porous supporting body is put into reaction kettle tubulation, is pumped using slurries and is delivered to film making solution
Reaction kettle is sealed, later on heat-conducting oil heating system reaches film making solution temperature to carry out Hydrothermal Synthesiss at 80 DEG C.React 4h
After take out, then, take out porous supporting body membrane tube cleaning and dipping membrane tube to pH to be put into 50 DEG C of oven for drying after 7-8 or so.
Repeat aforesaid operations 5 times, prepare 5 single tube NaA molecular sieve inner membrances.
The NaA molecular sieve of 1~embodiment of embodiment 3 and the gained of reference examples 1 is subjected to infiltration evaporation, experimental condition is：Behaviour
Make 70 DEG C of temperature DEG C, separation system is the ethanol/water solution of 5wNaA.%.Acquired results are as follows.
The infiltration evaporation performance of film synthesized by the present invention is more excellent, separation factor in the film synthesized by 1~embodiment of embodiment 3
>1000, flux>2kg·h–1·m–2.Meet the requirement of industrial applications.
The field emission scanning electron microscope (SEM) photograph for the NaA type molecular screen membranes being prepared by embodiment 1 as shown in Figures 2 and 3, from
It can be seen from the figure that, the molecular sieve even film layer being prepared, it is perfect fall into.
Claims (10)
- A kind of 1. integral preparation method of supporter inner surface molecular screen membrane, it is characterised in that：This method comprises the following steps：1st step：Porous supporting body is fixed in the reaction kettle tubulation of membrane reactor；2nd step：Molecular sieve seed suspension is delivered to the inner cavity of porous supporting body in membrane reactor, and in surface of internal cavity with speed DEG C for 50~200mL/min speed loop flow 1~60 second；The crystal seed suspension of reverse circulation discharge afterwards, drying；3rd step：Film making solution is sent into membrane reactor, crystallization synthetic reaction is carried out, after reaction takes out porous supporting body And wash and dry, that is, obtain NaA molecular sieve inner membrance.
- A kind of 2. integral preparation method of supporter inner surface molecular screen membrane according to claim 1, it is characterised in that： The configuration of the porous supporting body is the doughnut of single hose, multi-channel type.
- 3. a kind of integral preparation method of supporter inner surface molecular screen membrane according to claim 1, is characterized in that：Institute The porous supporting body stated horizontally or vertically is fixed in membrane reactor tubulation.
- A kind of 4. integral preparation method of supporter inner surface molecular screen membrane according to claim 1, it is characterised in that： The drying of 2nd step, which uses heat source, to be conduction oil, hot water or water vapour.
- A kind of 5. integral preparation method of supporter inner surface molecular screen membrane according to claim 1, it is characterised in that： The drying temperature DEG C of 2nd step is 30-120 DEG C.
- A kind of 6. integral preparation method of supporter inner surface molecular screen membrane according to claim 5, it is characterised in that： The drying temperature DEG C of 2nd step is 50-70 DEG C.
- A kind of 7. integral preparation method of supporter inner surface molecular screen membrane according to claim 1, it is characterised in that： The temperature DEG C of 3rd step synthetic reaction is 30-180 DEG C.
- A kind of 8. integral preparation method of supporter inner surface molecular screen membrane according to claim 7, it is characterised in that： The temperature DEG C of 3rd step synthetic reaction is 80-120 DEG C.
- 9. a kind of integral preparation method of supporter inner surface molecular screen membrane according to claim 7 or 8, its feature exist In：Synthetic reaction, which uses heat source, to be conduction oil, hot water or water vapour.
- A kind of 10. device for being used for realization claim 1 the method, it is characterised in that：The device include membrane reactor and End socket (1) positioned at reactor both ends, reaction kettle tubulation (3) are located in the inner cavity of membrane reactor, and porous supporting body (6) passes through O Type circle (4) and pressing plate (5) are fixed on the reaction kettle tubulation surface of membrane reactor, in reaction kettle tubulation (3) and membrane reactor Heat source fluidized bed (2) is equipped between wall.
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| CN201711380381.0A CN107930411A (en) | 2017-12-20 | 2017-12-20 | The preparation method and device of a kind of molecular screen membrane |
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| CN201711380381.0A CN107930411A (en) | 2017-12-20 | 2017-12-20 | The preparation method and device of a kind of molecular screen membrane |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109012196A (en) * | 2018-07-04 | 2018-12-18 | 华东理工大学 | The doughnut inner wall NaA type molecular sieve infiltrating and vaporizing membrane and its synthetic method dynamically synthesized in a kind of continuous current system |
| CN110860268A (en) * | 2018-08-28 | 2020-03-06 | 美国分子工程股份有限公司 | Structural material hydrothermal growth reactor |
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| CN101402022A (en) * | 2007-06-22 | 2009-04-08 | 中科院嘉兴中心成都有机所分中心 | Novel methods for producing type A molecular sieve film in current system |
| CN103055716A (en) * | 2013-01-09 | 2013-04-24 | 江苏九天高科技股份有限公司 | NaA molecular sieve membrane element internal membrane preparation method |
| CN103446896A (en) * | 2013-09-02 | 2013-12-18 | 中国海洋石油总公司 | Method for rapidly preparing supported zeolite inner-membranes |
| CN107335343A (en) * | 2017-09-06 | 2017-11-10 | 李晨舒 | A kind of synthesizer and synthetic method of doughnut NaA molecular sieve membrane |
| CN207694612U (en) * | 2017-12-20 | 2018-08-07 | 江苏九天高科技股份有限公司 | A kind of device preparing molecular screen membrane |
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2017
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101402022A (en) * | 2007-06-22 | 2009-04-08 | 中科院嘉兴中心成都有机所分中心 | Novel methods for producing type A molecular sieve film in current system |
| CN103055716A (en) * | 2013-01-09 | 2013-04-24 | 江苏九天高科技股份有限公司 | NaA molecular sieve membrane element internal membrane preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109012196A (en) * | 2018-07-04 | 2018-12-18 | 华东理工大学 | The doughnut inner wall NaA type molecular sieve infiltrating and vaporizing membrane and its synthetic method dynamically synthesized in a kind of continuous current system |
| CN109012196B (en) * | 2018-07-04 | 2021-07-30 | 华东理工大学 | Hollow fiber inner wall NaA type molecular sieve pervaporation membrane dynamically synthesized in continuous flow system and synthesis method thereof |
| CN110860268A (en) * | 2018-08-28 | 2020-03-06 | 美国分子工程股份有限公司 | Structural material hydrothermal growth reactor |
| CN110860268B (en) * | 2018-08-28 | 2021-10-08 | 美国分子工程股份有限公司 | Structural material hydrothermal growth reactor |
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