CN108211807A - A kind of processing method of molecular sieve - Google Patents
A kind of processing method of molecular sieve Download PDFInfo
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- CN108211807A CN108211807A CN201810036033.XA CN201810036033A CN108211807A CN 108211807 A CN108211807 A CN 108211807A CN 201810036033 A CN201810036033 A CN 201810036033A CN 108211807 A CN108211807 A CN 108211807A
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- screen membrane
- molecular screen
- molecular sieve
- processing method
- membrane
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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 22
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000003672 processing method Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000012670 alkaline solution Substances 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Inorganic materials [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 6
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 6
- 238000007654 immersion Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 229910017906 NH3H2O Inorganic materials 0.000 claims description 4
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 claims description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 2
- 150000007529 inorganic bases Chemical group 0.000 claims description 2
- 125000001453 quaternary ammonium group Chemical group 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 238000011010 flushing procedure Methods 0.000 claims 1
- ZMANZCXQSJIPKH-UHFFFAOYSA-O triethylammonium ion Chemical compound CC[NH+](CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-O 0.000 claims 1
- 239000012528 membrane Substances 0.000 abstract description 51
- 230000004907 flux Effects 0.000 abstract description 18
- 238000000926 separation method Methods 0.000 abstract description 18
- 230000008569 process Effects 0.000 abstract description 14
- 239000003513 alkali Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 238000012360 testing method Methods 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 8
- 230000008595 infiltration Effects 0.000 description 8
- 238000001764 infiltration Methods 0.000 description 8
- 238000001704 evaporation Methods 0.000 description 7
- 230000008020 evaporation Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000012466 permeate Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229920002379 silicone rubber Polymers 0.000 description 2
- 239000004945 silicone rubber Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 description 2
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 235000012489 doughnuts Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/10—Testing of membranes or membrane apparatus; Detecting or repairing leaks
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N2015/084—Testing filters
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The present invention discloses a kind of processing method of molecular sieve.The step of the method includes molecular sieve is made to be contacted with alkaline solution.By the method for simple alkali process, the permeation flux of molecular screen membrane can be improved, can even improve the permeation flux and separation selectivity of molecular screen membrane simultaneously in some cases.On the other hand, the used technological means is simple and practicable, of low cost, it is easy to accomplish commercial application.And it can be docked with existing simple production process, be conducive to upgrading of the manufacturing enterprise to product, increase the market competitiveness.
Description
Technical field
The invention belongs to technical field of membrane separation, specially molecular screen membrane field, are related to molecular screen membrane improved properties technology.
Background technology
Molecular screen membrane is a kind of novel inorganic separating film material, has the advantages of stability is good, and separating property is high, is oozing
Vaporization and Steam soak field achieve extensive use thoroughly.Two important indicators of characterization molecular screen membrane separating property are to permeate
Flux and separation selectivity.Usually by the optimization of synthesis condition, point with ideal infiltration flux and selectivity can be obtained
Sub- sieve membrane, but it is both relatively difficult to achieve in most cases while optimize.
The performance of molecular screen membrane can be improved using the method for post processing.For example pass through chemical liquid deposition, chemical gaseous phase
The defects of means such as deposition can be eliminated on molecular screen membrane, improves its separation selectivity.It can also be eliminated point by multi-stage synthesis
The defects of sub- sieve membrane, improves selectivity.But the above method normally results in the reduction of permeation flux.
The present invention has conducted a thorough research regarding to the issue above, it is expected to seek simple and practicable method to effectively improve molecule
The performance of sieve or molecular screen membrane.
Invention content
The object of the present invention is to provide a kind of methods of simple and practicable raising molecular screen membrane performance.In order to realize above-mentioned mesh
, the present invention discloses a kind of processing method of molecular sieve, and this method includes the step of molecular sieve is made to be contacted with alkaline solution.We
Research in find, by the method for simple alkali process, the permeation flux of molecular screen membrane can be improved, in some cases very
The permeation flux and separation selectivity of molecular screen membrane can be extremely improved simultaneously.On the other hand, the used technological means is simple
It is easy, of low cost, it is easy to accomplish commercial application.And it can be docked with existing simple production process, be conducive to produce
Enterprise increases the market competitiveness to the upgrading of product.
Description of the drawings
1 width of attached drawing of the present invention, i.e. Fig. 1 are schematic devices used by embodiment test parameter.
In figure：1 water bath with thermostatic control；2 head tanks；3 magnetic force circulating pumps；4 membrane modules；5 heaters；6 triple valves；7 collectors；8
Surge flask；9 diaphragm pumps.
Specific embodiment
The present invention provides a kind of processing method of molecular sieve, and this method includes making the step that molecular sieve is contacted with alkaline solution
Suddenly.
In specific embodiment, the alkaline solution pH is 8-13.It is it is preferred that saline and alkaline etc. with inorganic base or organic quaternary ammonium
Alkaline aqueous solution prepared by alkaline matter.More specifically, the alkaline matter preferably illustrate but be not limited to NaOH, KOH,
NH3H2O, TMAOH (tetramethylammonium hydroxide), TEAH (tetraethyl ammonium hydroxide), TPAOH (tetrapropylammonium hydroxide) or it is mixed
Close object.Wherein described mixture refers to mixture of one or more of the aforementioned substances according to arbitrary proportion.It is further preferable that
The alkaline matter is from NaOH, KOH, NH3H2O or its mixture.Wherein, using NaOH or KOH as most preferably.
In specific embodiment, the contact can understand according to common meaning.The most commonly used may be defined as
The processing mode of contact includes but not limited to impregnate or rinse.The time of immersion is generally in 5~60min, it is preferred to use 15~
40min.It rinses and should be guaranteed that coming into full contact with for molecular sieve and alkaline solution, used time general 15~60min, preferably 20~30min.
The above-mentioned molecular sieve after alkali process can be applied directly, be used after can also being rinsed with water to neutrality.Such as increase punching
Step is washed, then it is preferable to use deionized waters.Whether rinse and substantive influence is not generated to the property of molecular sieve.
Below in a manner of specific embodiment to it is of the present invention and technical solution and its effect do further, institute
The non-limiting example of display is understood not to any form of restriction to the content of present invention.
Unless otherwise specified, the acquisition of parameter and result uses following methods in this specification：
1st, test method
(1) flexural strength is performed by 5.4 regulations in HY/T064-2002.
(2) assay method of separating property is：Investigate the performance of molecular sieve film pervasion evaporating and dewatering, operation temperature 50
DEG C, material liquid is the ethanol water containing ethyl alcohol 90%.The composition of penetrant is measured by analysis and is collected in the unit interval
The quality of penetrant calculates water/separation of ethanol coefficient and permeation flux as follows.
Separation (separation factor)：Represent two kinds of substances in material by molecular screen membrane separation behaviour
The ratio of relative amount before and after work.It is defined as：
In formula, αi/jRepresent separation of the molecular screen membrane for i (preferentially through film) and j components；xi,p(xj,p) represent i
(j) mass fraction of the component in penetrant；xi,f(xj,f) represent the mass fraction of i (j) components in the feed.
Permeation flux (permeation flux)：By set point of temperature, pressure, material penetrates elementary membrane within the unit interval
The quality of area.It is defined as：
Wherein, J represents permeation flux (kgm-2h-1)；W represents the quality (kg) of infiltration component；When Δ t represents sampling interval
Between (h)；A represents the effective area (m that film surface plays centrifugation2)。
For above-mentioned parameter measure device as shown in Figure 1.
The step of test method is：
A) ethanol water containing ethyl alcohol 90% is prepared, molecular screen membrane is encapsulated in stainless steel membrane component with silicone rubber O-ring
In, according to exposed area effective separation area A.
B) regulating thermostatic water-bath and heater make system keep constant temperature at 50 DEG C.
C) material liquid is conveyed by magnetic force circulating pump to the feed side of membrane module, and the flow velocity in membrane module is not less than 0.1m/
s；Per-meate side is vacuumized (pressure is less than 1kPa) by diaphragm pump, and collector is placed in condensation in ice salt bath and collects penetrant.
D) stable rear certain interval of time switching collector sampling, weighs to penetrant, utilizes karl Fischer moisture
Analyzer detects the mass fraction of water and ethyl alcohol, substitutes into separation and permeation flux that formula calculates molecular screen membrane.Continuously take three
A sample calculates its average value.
Embodiment 1
It synthesizes to obtain A type molecular sieve film I (CN1467017A embodiments 1) using crystal seed method.Obtained molecular sieve will be synthesized
Film is immersed in the aqueous solution of NaOH, and the pH value of the solution is 10, soaking time 30min.After immersion neutrality is washed till with clear water.
Compare the separating property of molecular screen membrane before and after the processing using infiltration evaporation testing experiment.It is as follows to make process：
A) ethanol water containing ethyl alcohol 90% is prepared, molecular screen membrane is encapsulated in stainless steel membrane component with silicone rubber O-ring
In, according to exposed area effective separation area A.
B) regulating thermostatic water-bath and heater make system keep constant temperature at 50 DEG C.
C) material liquid is conveyed by magnetic force circulating pump to the feed side of membrane module, and the flow velocity in membrane module is not less than 0.1m/
s；Per-meate side is vacuumized (pressure is less than 1kPa) by diaphragm pump, and collector is placed in condensation in ice salt bath and collects penetrant.
D) stable rear certain interval of time switching collector sampling, weighs to penetrant, utilizes karl Fischer moisture
Analyzer detects the mass fraction of water and ethyl alcohol, substitutes into separation and permeation flux that formula calculates molecular screen membrane.Continuously take three
A sample calculates its average value.
The results are shown in Table 1 for above-mentioned testing experiment：
Table 1
| Molecular screen membrane | Permeation flux | Separation |
| Untreated molecular screen membrane I | 0.50kg/m2h | 600 |
| Alkali process molecular screen membrane I | 0.55kg/m2h | 650 |
Embodiment 2
It synthesizes to obtain A type molecular sieve film II (CN100337918C embodiments 3) using microwave process for synthesizing.It will synthesize what is obtained
Molecular screen membrane is immersed in the aqueous solution of NaOH, and the pH value of the solution is 8, soaking time 30min.In being washed till after immersion with clear water
Property.
Compare the separating property of molecular screen membrane before and after the processing using infiltration evaporation testing experiment.Infiltration evaporation operating process
Such as embodiment 1, the results are shown in Table 2 for above-mentioned testing experiment：
Table 2
| Molecular screen membrane | Permeation flux | Separation |
| Untreated molecular screen membrane II | 0.60kg/m2h | 1000 |
| Alkali process molecular screen membrane II | 0.70kg/m2h | 1250 |
Embodiment 3
Obtained point will be synthesized using mesoporous zeolite Opacity in lens NaA molecular sieve membrane III (CN104941451A embodiments 1)
Sub- sieve membrane is immersed in the aqueous solution of NaOH, and the pH value of the solution is 9, soaking time 30min.In being washed till after immersion with clear water
Property.
Compare the separating property of molecular screen membrane before and after the processing using infiltration evaporation testing experiment.Infiltration evaporation operating process
Such as embodiment 1, the results are shown in Table 3 for testing experiment：
Table 3
| Molecular screen membrane | Permeation flux | Separation |
| Untreated molecular screen membrane III | 0.60kg/m2h | 1000 |
| Alkali process molecular screen membrane III | 0.80kg/m2h | 950 |
Embodiment 4
Synthesizing compound MOR types molecular screen membrane IV (CN106823837A embodiments 1) as supporter using doughnut will
It synthesizes obtained molecular sieve hollow-fibre membrane to be immersed in the aqueous solution of KOH, the pH value of the solution is 10, impregnates 60min.It impregnates
Afterwards neutrality is washed till with clear water.Compare the separating property of molecular screen membrane before and after the processing using infiltration evaporation testing experiment.Permeate vapour
Change operating process such as embodiment 1, the results are shown in Table 4 for above-mentioned testing experiment：
Table 4
| Molecular screen membrane | Permeation flux | Separation |
| Untreated molecular screen membrane IV | 0.80kg/m2h | 500 |
| Alkali process molecular screen membrane IV | 1.00kg/m2h | 600 |
Embodiment 5
With reference to the method for Examples 1 to 4, different types of molecular screen membrane is synthesized, and use detection side described in embodiment 1
Method and condition are detected the property of molecular sieve that different alkaline conditions are disposed.With the molecule without alkali process under the same terms
Sieve as basic reference, calculate alkali process molecular sieve film pervasion variations of flux ratio (Δ x) and selectivity variation ratio (and Δ y), with
Percentage represents, such as table 5.
Table 5
In table 5, NaX, NaY, CHA, T and type ZSM 5 molecular sieve respectively refer to following document synthesis：J.Membr.Sci.,
337(2009)47-54；Sep.Sci.Tech.,40(2005)1047-1066；Sep.Sci.Tech.,40(2005)1047-
1066；AIChE J,39(2013)936-947；Korean Membr.J.,7(2005)51-57.
Claims (6)
1. a kind of processing method of molecular sieve, the step of including molecular sieve is made to be contacted with alkaline solution.
2. processing method according to claim 1, which is characterized in that the alkaline solution pH is 8-13.
3. processing method according to claim 1, which is characterized in that the alkaline solution is the water-soluble of alkaline matter
Liquid, the alkaline matter is selected from inorganic base or organic quaternary ammonium is saline and alkaline.
4. processing method according to claim 3, which is characterized in that the alkaline matter be selected from NaOH, KOH,
NH3H2O, TMAOH, TEAH, TPAOH or its mixture.
5. processing method method according to claim 3, which is characterized in that the alkaline matter be selected from NaOH, KOH,
NH3H2O or its mixture.
6. processing method according to claim 1, which is characterized in that the contact is immersion or flushing.
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| CN201810036033.XA CN108211807B (en) | 2018-01-15 | 2018-01-15 | Treatment method of molecular sieve membrane |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2021186412A1 (en) * | 2020-03-20 | 2021-09-23 | Terahertz Group Ltd. | Systems and methods for non-invasive determination of covid-19 coronavirus infection |
| US11510592B2 (en) | 2016-07-29 | 2022-11-29 | Terahertz Group Ltd. | Systems and methods for non-invasive determination of COVID-19 coronavirus infection |
| US11570971B2 (en) | 2016-07-29 | 2023-02-07 | Novatrans Group S.A. | System and method for in ovo sexing of avian embryos |
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|---|---|---|---|---|
| CN105727757A (en) * | 2016-03-18 | 2016-07-06 | 宁夏大学 | Preparation method of orientation LTL type molecular sieving membrane for gas separation |
| CN106378013A (en) * | 2016-11-10 | 2017-02-08 | 南京工业大学 | Preparation method and application of hierarchical porous molecular sieve membrane |
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2018
- 2018-01-15 CN CN201810036033.XA patent/CN108211807B/en active Active
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| CN105727757A (en) * | 2016-03-18 | 2016-07-06 | 宁夏大学 | Preparation method of orientation LTL type molecular sieving membrane for gas separation |
| CN106378013A (en) * | 2016-11-10 | 2017-02-08 | 南京工业大学 | Preparation method and application of hierarchical porous molecular sieve membrane |
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| Title |
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| 刘秀凤等: "ZSM-5和Fe-ZSM-5分子筛膜的合成与表面改性", 《化工学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11510592B2 (en) | 2016-07-29 | 2022-11-29 | Terahertz Group Ltd. | Systems and methods for non-invasive determination of COVID-19 coronavirus infection |
| US11570971B2 (en) | 2016-07-29 | 2023-02-07 | Novatrans Group S.A. | System and method for in ovo sexing of avian embryos |
| US11723343B2 (en) | 2016-07-29 | 2023-08-15 | Novatrans Group S.A. | System and method for in ovo sexing of avian embryos |
| WO2021186412A1 (en) * | 2020-03-20 | 2021-09-23 | Terahertz Group Ltd. | Systems and methods for non-invasive determination of covid-19 coronavirus infection |
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