CN103551040B - Online repairing method of NaA molecular sieve membrane - Google Patents
Online repairing method of NaA molecular sieve membrane Download PDFInfo
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- CN103551040B CN103551040B CN201310575304.6A CN201310575304A CN103551040B CN 103551040 B CN103551040 B CN 103551040B CN 201310575304 A CN201310575304 A CN 201310575304A CN 103551040 B CN103551040 B CN 103551040B
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- molecular sieve
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Abstract
The invention relates to an online repairing method of NaA molecular sieve membrane. The online repairing method is characterized by comprising the following steps of preparing a synthesized solution according to the molar ratio of (2-5) Na2o: 1Al2O3: (1.5-3) SiO2: (60-200) H2O; preparing a tubular membrane; separating, settling and storing the solution in a reactor after the membrane is synthesized to be used as membrane online repairing liquid; adding the membrane online repairing liquid into a membrane online repairing device at the temperature of 100DEG C through a flow rate of 50ml/min, cycling the membrane online repairing liquid for 3 to 10 hours by utilizing a cycling pump, so that the membrane online repairing liquid is precipitated and solidified on the surface of a to-be-repaired NaA membrane tube and washed, and the online repairing process is completed.
Description
Technical field
The present invention relates to technical field of molecular sieve, be specifically related to a kind of online restorative procedure of NaA molecular sieve membrane.
Background technology
In the past few decades, membrane technology emerges rapidly.Membrane separation technique make use of one or more materials and better reaches by film the object be separated containing two kinds and above incoming mixture than other material, and film has permeability for the certain ingredients in solution.The synthesis of most film is all directly carried out on carrier, and due to the difference of the coefficient of expansion, film is easily come off and occurs defect, the defect of molecular screen membrane makes separating effect decline, and have impact on effect and the progress of molecular screen membrane.
Because the aging of molecular screen membrane comes off or creep in molecular screen membrane separation process, under internal pressure, there is cracking or seepage, must repair as early as possible.In the process of rapid rush-repair, in order to make cracking position not expand further, must the position of ftractureing, damaging be repaired.
Main flow is carry out replacing process to the molecular screen membrane gone wrong in the market, because a set of molecular screen membrane separator is made up of many molecular screen membrane pipes, be not that every root goes wrong, because dismounting not only goes wrong to sealing further in the process changed, and due to the impact of unloading process, mechanical failure can be caused equally to intact molecular screen membrane pipe, cause and change and locking inconvenience.
Summary of the invention
Instant invention overcomes deficiency of the prior art, provide the simple and online restorative procedure of the molecular screen membrane pipe that breaks of highly versatile of a kind of structure.
In order to realize above-mentioned object, adopt following technical scheme:
The transparent colloidal sol of synthesis liquid utilizing the molecular screen membrane of reparation of the present invention to use, and stability can maintain January more than, the molecular screen membrane repaired by it has good permeance property, does not have the defect that foreign matter causes completely.
The present invention is a kind of online restorative procedure of NaA molecular sieve membrane; It is characterized in that:
Processing step is as follows:
1) be that the NaA molecular sieve crystal of 0.2 ~ 2.5 μm is coated in as crystal seed the α-Al that supporter is 0.2 ~ 2.5 μm, aperture using particle diameter
2o
3porous carrier on, obtain the α-Al with crystal seed layer
2o
3supporter;
2) tubular membrane adopts intermediate water thermal synthesis method to obtain, according to 2 ~ 5Na
2o:1Al
2o
3: 1.5 ~ 3SiO
2: (60 ~ 200) H
2the mol ratio preparation synthesis liquid of O; Wherein aluminium source uses aluminium isopropoxide or sodium aluminate, and silicon source uses white carbon or activated silica gel, and deionized water and NaOH are that raw material obtains Hydrothermal Synthesis liquid; The supporter of seeded layer in step 1) is loaded in high-pressure synthesis reactor, then pours Hydrothermal Synthesis liquid into, hydrothermal synthesis reaction 3 ~ 10 hours at 60 ~ 110 DEG C;
3) by step 2) supporter takes out washing drying and obtains NaA molecular sieve membrane in reactor, and synthesize the settled solution that the solution in the reactor after film obtains after centrifugation molecular sieve and preserve, repair liquid online as film.
4) the NaA film pipe (film pipe 90 ~ 95% separation of ethanol coefficient declines less than 5000) repeatedly using the rear needs producing certain defect to repair sealing installed, is positioned over the online prosthetic device of film inner;
5) by 3) in clarify the film that obtains and repair liquid online and at 100 DEG C, be passed into 4 with the flow rate of 50ml/min) the online prosthetic device of film in, circulate 3 ~ 10 hours under the circulation of circulating pump, make film repair liquid deposition online and solidify the NaA film tube-surface repaired in needs, thus completing online repair process, then taking-up deionized water water cleans.
6) the NaA film after reparation is carried out to the separating property test of 95% ethanol water, separation brings up to 10000.
Accompanying drawing explanation
Fig. 1 is online prosthetic device schematic diagram provided by the invention.
1, liquid is synthesized, 2, inlet, 3, circulation fluid outlet, 4, discharging opening, 5, gas vent, 6, tubular membrane, 7, fluororubber pad;
Beneficial effect of the present invention:
(1) this method operation can conservation, effectively utilizes the waste liquid after synthesis, reduces the pollution to environment.
(2) compared with prior art, highly versatile of the present invention, easy to use and flexible, reduces unloading process.
(3) operating condition is simple, effectively improves membrane separating property.
(4) can Fast Measurement repairing performance, easy to detect.
Detailed description of the invention
Embodiment 1
1) be that the NaA molecular sieve crystal of 0.2 μm is coated in as crystal seed the α-Al that supporter is 0.2 μm, aperture using particle diameter
2o
3porous carrier on, obtain the α-Al with crystal seed layer
2o
3supporter;
2) tubular membrane adopts intermediate water thermal synthesis method to obtain, and this experimental program is according to 2Na
2o:1Al
2o
3: 2SiO
2: 120H
2the mol ratio preparation synthesis liquid of O; Wherein aluminium source uses aluminium isopropoxide or sodium aluminate, and silicon source uses white carbon or activated silica gel, and deionized water and NaOH are that raw material obtains Hydrothermal Synthesis liquid; The supporter of seeded layer in step 1) is loaded in high-pressure synthesis reactor, then pours Hydrothermal Synthesis liquid into, hydrothermal synthesis reaction 4 hours at 100 DEG C;
3) by step 2) supporter takes out washing drying and obtains NaA molecular sieve membrane in reactor, and synthesize the settled solution that the solution in the reactor after film obtains after centrifugation molecular sieve and preserve, repair liquid online as film.
4) the NaA film pipe (film pipe 95% separation of ethanol coefficient drops to 5000) repeatedly using the rear needs producing certain defect to repair sealing installed, is positioned over the online prosthetic device of film inner;
5) by 3) in clarify the film that obtains and repair liquid online and at 100 DEG C, be passed into 4 with the flow rate of 50ml/min) the online prosthetic device of film in, circulate 4 hours under the circulation of circulating pump, make film repair liquid deposition online and solidify the NaA film tube-surface repaired in needs, thus completing online repair process, then taking-up deionized water water cleans.
6) the NaA film after reparation is carried out to the separating property test of 95% ethanol water, separation brings up to 10000.
Embodiment 2
1) be that the NaA molecular sieve crystal of 0.8 ~ 1 μm is coated in as crystal seed the α-Al that supporter is 1 μm, aperture using particle diameter
2o
3porous carrier on, obtain the α-Al with crystal seed layer
2o
3supporter;
2) tubular membrane adopts intermediate water thermal synthesis method to obtain, and this experimental program is according to 2Na
2o:1Al
2o
3: 2SiO
2: 120H
2the mol ratio preparation synthesis liquid of O; Wherein aluminium source uses aluminium isopropoxide or sodium aluminate, and silicon source uses white carbon or activated silica gel, and deionized water and NaOH are that raw material obtains Hydrothermal Synthesis liquid; The supporter of seeded layer in step 1) is loaded in high-pressure synthesis reactor, then pours Hydrothermal Synthesis liquid into, hydrothermal synthesis reaction 6 hours at 80 DEG C;
3) by step 2) supporter takes out washing drying and obtains NaA molecular sieve membrane in reactor, and synthesize the settled solution that the solution in the reactor after film obtains after centrifugation molecular sieve and preserve, repair liquid online as film.
4) the NaA film pipe (film pipe 95% separation of ethanol coefficient drops to 3000) repeatedly using the rear needs producing certain defect to repair sealing installed, is positioned over the online prosthetic device of film inner;
5) by 3) in clarify the film that obtains and repair liquid online and at 90 DEG C, be passed into 4 with the flow rate of 50ml/min) the online prosthetic device of film in, circulate 5 hours under the circulation of circulating pump, make film repair liquid deposition online and solidify the NaA film tube-surface repaired in needs, thus completing online repair process, then taking-up deionized water water cleans.
6) the NaA film after reparation is carried out to the separating property test of 90% ethanol water.Separation brings up to 8000.
Embodiment 3
1) be that the NaA molecular sieve crystal of 1.5 μm is coated in as crystal seed the α-Al that supporter is 2 μm, aperture using particle diameter
2o
3porous carrier on, obtain the α-Al with crystal seed layer
2o
3supporter;
2) tubular membrane adopts intermediate water thermal synthesis method to obtain, and this experimental program is according to 2Na
2o:1Al
2o
3: 2SiO
2: 120H
2the mol ratio preparation synthesis liquid of O; Wherein aluminium source uses aluminium isopropoxide or sodium aluminate, and silicon source uses white carbon or activated silica gel, and deionized water and NaOH are that raw material obtains Hydrothermal Synthesis liquid; The supporter of seeded layer in step 1) is loaded in high-pressure synthesis reactor, then pours Hydrothermal Synthesis liquid into, hydrothermal synthesis reaction 4 hours at 110 DEG C;
3) by step 2) supporter takes out washing drying and obtains NaA molecular sieve membrane in reactor, and synthesize the settled solution that the solution in the reactor after film obtains after centrifugation molecular sieve and preserve, repair liquid online as film.
4) the NaA film pipe (film pipe 90% separation of ethanol coefficient drops to 5000) repeatedly using the rear needs producing certain defect to repair sealing installed, is positioned over the online prosthetic device of film inner;
5) by 3) in clarify the film that obtains and repair liquid online and at 80 DEG C, be passed into 4 with the flow rate of 50ml/min) the online prosthetic device of film in, circulate 6 hours under the circulation of circulating pump, make film repair liquid deposition online and solidify the NaA film tube-surface repaired in needs, thus completing online repair process, then taking-up deionized water water cleans.
6) the NaA film after reparation is carried out to the separating property test of 90% ethanol water.Separation brings up to 10000.
The present invention includes but be not limited to above embodiment, every any equivalent replacement of carrying out under the principle of spirit of the present invention or local improvement, all will be considered as within protection scope of the present invention.
Claims (1)
1. the online restorative procedure of a NaA molecular sieve membrane; It is characterized in that:
Processing step is as follows:
1) be that the NaA molecular sieve crystal of 0.2 ~ 2.5 μm is coated in as crystal seed the α-Al that supporter is 0.2 ~ 2.5 μm, aperture using particle diameter
2o
3porous carrier on, obtain the α-Al with crystal seed layer
2o
3supporter;
2) tubular membrane adopts intermediate water thermal synthesis method to obtain, according to 2 ~ 5Na
2o:1Al
2o
3: 1.5 ~ 3SiO
2: 60 ~ 200H
2the mol ratio preparation synthesis liquid of O; Wherein aluminium source uses aluminium isopropoxide or sodium aluminate, and silicon source uses white carbon or activated silica gel, and deionized water and NaOH are that raw material obtains Hydrothermal Synthesis liquid; By step 1) in the supporter of seeded layer load in high-pressure synthesis reactor, then pour Hydrothermal Synthesis liquid into, hydrothermal synthesis reaction 3 ~ 10 hours at 60 ~ 110 DEG C, obtained tubular membrane;
3) by step 2) tubular membrane is taken out in reactor, and washing drying obtains NaA molecular sieve membrane, and synthesizes the settled solution that the solution in the reactor after film obtains after centrifugation molecular sieve and preserve, and repairs liquid online as film;
4) the NaA film pipe repeatedly using the rear needs producing certain defect to repair sealing installed, now film pipe 90 ~ 95% separation of ethanol coefficient test value drops to less than 5000, is positioned over the online prosthetic device of film inner;
5) by 3) in clarify the film that obtains and repair liquid online and at 100 DEG C, be passed into 4 with the flow rate of 50ml/min) the online prosthetic device of film in, circulate 3 ~ 10 hours under the circulation of circulating pump, make film repair liquid deposition online and solidify the NaA film tube-surface repaired in needs, then taking-up deionized water is cleaned, thus completes online repair process; Now repair caudacoria pipe 90 ~ 95% separation of ethanol coefficient test value at 8000-10000.
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|---|---|---|---|
| CN201310575304.6A CN103551040B (en) | 2013-11-15 | 2013-11-15 | Online repairing method of NaA molecular sieve membrane |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310575304.6A CN103551040B (en) | 2013-11-15 | 2013-11-15 | Online repairing method of NaA molecular sieve membrane |
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|---|---|
| CN103551040A CN103551040A (en) | 2014-02-05 |
| CN103551040B true CN103551040B (en) | 2015-06-24 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343067A (en) * | 2008-09-04 | 2009-01-14 | 天津大学 | Method for renovating molecular sieve membrane defection by means of liquid-liquid interfacial chemical liquid deposition |
| CN101874990A (en) * | 2009-11-16 | 2010-11-03 | 南京工业大学 | Repair method of intergranular pore channel of molecular sieve membrane |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5454975A (en) * | 1977-10-07 | 1979-05-01 | Kobe Steel Ltd | Operation of tubular membrane separator |
| US20080034453A1 (en) * | 1999-05-06 | 2008-02-07 | Nordine Cheikh | Annotated Plant Genes |
| US8715392B2 (en) * | 2009-05-21 | 2014-05-06 | Battelle Memorial Institute | Catalyzed CO2-transport membrane on high surface area inorganic support |
| EP4245370A3 (en) * | 2010-07-12 | 2023-11-29 | University of Southern California | Biocompatible substrate for facilitating interconnections between stem cells and target tissues and methods for implanting same |
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2013
- 2013-11-15 CN CN201310575304.6A patent/CN103551040B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343067A (en) * | 2008-09-04 | 2009-01-14 | 天津大学 | Method for renovating molecular sieve membrane defection by means of liquid-liquid interfacial chemical liquid deposition |
| CN101874990A (en) * | 2009-11-16 | 2010-11-03 | 南京工业大学 | Repair method of intergranular pore channel of molecular sieve membrane |
Non-Patent Citations (1)
| Title |
|---|
| 沸石分子筛膜缺陷的形成及修复;王聪等;《化学进展》;20081224(第12期);第1861-1867页 * |
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Address after: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Patentee after: CHINA NATIONAL OFFSHORE OIL Corp. Patentee after: CNOOC TIANJIN CHEMICAL RESEARCH & DESIGN INSTITUTE Co.,Ltd. Patentee after: CNOOC ENERGY TECHNOLOGY & SERVICES Ltd. Address before: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Patentee before: CHINA NATIONAL OFFSHORE OIL Corp. Patentee before: CNOOC TIANJIN CHEMICAL RESEARCH & DESIGN INSTITUTE Patentee before: CNOOC ENERGY TECHNOLOGY & SERVICES Ltd. |
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Effective date of registration: 20161010 Address after: No. three road 300131 Tianjin city Hongqiao District dingzigu No. 85 Patentee after: CNOOC TIANJIN CHEMICAL RESEARCH & DESIGN INSTITUTE Co.,Ltd. Patentee after: CNOOC ENERGY TECHNOLOGY & SERVICES Ltd. Address before: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Patentee before: CHINA NATIONAL OFFSHORE OIL Corp. Patentee before: CNOOC TIANJIN CHEMICAL RESEARCH & DESIGN INSTITUTE Co.,Ltd. Patentee before: CNOOC ENERGY TECHNOLOGY & SERVICES Ltd. |