CN107587267A - One kind is used for water-oil emulsion separation nano fibrous membrane and preparation method thereof - Google Patents
One kind is used for water-oil emulsion separation nano fibrous membrane and preparation method thereof Download PDFInfo
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- CN107587267A CN107587267A CN201610530561.1A CN201610530561A CN107587267A CN 107587267 A CN107587267 A CN 107587267A CN 201610530561 A CN201610530561 A CN 201610530561A CN 107587267 A CN107587267 A CN 107587267A
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- 239000012528 membrane Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000002569 water oil cream Substances 0.000 title claims abstract description 18
- 238000000926 separation method Methods 0.000 title claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 40
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000005253 cladding Methods 0.000 claims abstract description 18
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 17
- 239000011591 potassium Substances 0.000 claims abstract description 17
- 239000002121 nanofiber Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 6
- 229920000642 polymer Polymers 0.000 claims abstract description 6
- 238000002604 ultrasonography Methods 0.000 claims abstract description 6
- 238000009987 spinning Methods 0.000 claims description 19
- 238000001523 electrospinning Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 229920001661 Chitosan Polymers 0.000 claims description 4
- 229920000747 poly(lactic acid) Polymers 0.000 claims description 4
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 4
- 238000010041 electrostatic spinning Methods 0.000 claims description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- NCWQJOGVLLNWEO-UHFFFAOYSA-N methylsilicon Chemical compound [Si]C NCWQJOGVLLNWEO-UHFFFAOYSA-N 0.000 claims description 2
- 229920001610 polycaprolactone Polymers 0.000 claims description 2
- 239000004632 polycaprolactone Substances 0.000 claims description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 229920000954 Polyglycolide Polymers 0.000 claims 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- 239000004633 polyglycolic acid Substances 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 4
- 238000004945 emulsification Methods 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract 2
- 238000000576 coating method Methods 0.000 abstract 2
- 239000000835 fiber Substances 0.000 description 17
- 239000003921 oil Substances 0.000 description 7
- 235000019198 oils Nutrition 0.000 description 6
- XTIIITNXEHRMQL-UHFFFAOYSA-N tripotassium methoxy(trioxido)silane Chemical compound [K+].[K+].[K+].CO[Si]([O-])([O-])[O-] XTIIITNXEHRMQL-UHFFFAOYSA-N 0.000 description 5
- 239000011324 bead Substances 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 230000000873 masking effect Effects 0.000 description 3
- 239000004626 polylactic acid Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 238000005352 clarification Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011083 cement mortar Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000019476 oil-water mixture Nutrition 0.000 description 1
- 239000010451 perlite Substances 0.000 description 1
- 235000019362 perlite Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/204—Keeping clear the surface of open water from oil spills
Abstract
The invention discloses a kind of nano fibrous membrane of poly- methane-siliconic acid alcohol cladding for water-oil emulsion separation and preparation method thereof, comprise the following steps：Prepared polymer solution first, then utilize electrospun nanofibers film；The nano fibrous membrane of preparation is immersed in methane-siliconic acid potassium solution again；Acid-conditioning solution pH to 7 or so is used under ultrasound condition, the nano fibrous membrane of poly- methane-siliconic acid alcohol cladding is made after drying.The present invention is by the strata methane-siliconic acid alcohol of nano fibrous membrane Surface coating one, allow and break the profit drop of emulsification when profit filters so as to improve water-oil separating efficiency and repeat usage, on the other hand improved by coating poly- methane-siliconic acid alcohol in the use intensity of nanofiber surface filter membrane, the preparation method has simple to operate, the advantages that cost is cheap, and technique is relatively easy to control.
Description
Technical field
The invention belongs to water-oil emulsion separation membrane material field, more particularly to a kind of gathering for water-oil emulsion separation
The preparation of the micro/nano fibrous membrane material of methane-siliconic acid alcohol cladding.
Background technology
Due to growing industry oil waste water, the seawater of pollution and frequently oil leakage, such as the deep water oil in the Gulf of Mexico
Leakage, water-oil separating turn into global problem.For example oil skimmer, centrifuge, depth-type filtration, precipitation and floating rotation separation can for conventional method
For insoluble oil aqueous mixtures, but it is invalid to the oil water mixture of emulsification, especially in the presence of the microemulsion (liquid of surfactant
Drip 20 μm of size ＜).The forward position of the advanced spinning material of Electrospun nano-fibers, combine good wetability, connectedness, compared with
Strong mechanical performance, good adaptability, larger specific surface area and easily extended from multiple material (polymer, ceramics, carbon etc.)
Synthesis, is to bear larger desired superior nanometer materials.The film prepared with nanofiber possesses and has water-oil emulsion separation
Potentiality, addition modification, preferable separating effect can be obtained after clad.Potassium methyl silicate can be with the CO in air2Or its
He reacts at acid compound, forms one layer of undissolvable netted waterproof ventilated membrane on base material top layer, there is outstanding waterproof to imitate
Fruit and antiseepage, protection against the tide, effect are lasting, resistance to scrub, the advantages that high-low temperature resistant (- 50~150 DEG C), antipollution.The poly- methyl of generation
Silicic acid alcohol structural formula is as follows：
Potassium methyl silicate is mainly used in stone material, brick and tile, ceramics, concrete, cement mortar, perlite, gypsum and stone at present
Water repellent treatments such as cream plate, timber, but be seldom related in terms of membrane filtration, the particularly separating treatment of water-oil emulsion.
The content of the invention
The technical problems to be solved by the invention, which are to provide one kind, has super oleophylic, hydrophobicity, can efficiently separate profit
The nanofiber membrane preparation method of the poly- methane-siliconic acid alcohol cladding of emulsion.
Realizing the technical solution of the object of the invention is：A kind of nanofiber film preparation for water-oil emulsion separation
Method, including step in detail below：
Step 1：The preparation of nano fibrous membrane
Spinning material is dissolved in DMF solution, stir to solution clarify it is homogeneous, stand, gathered
Polymer solution, nano fibrous membrane is made using electrostatic spinning technique；
Step 2：It is prepared by methane-siliconic acid potassium solution
Take potassium methyl silicate raw material to add and methane-siliconic acid potassium solution is prepared in pure water；
Step 3：The preparation of poly- methane-siliconic acid alcohol cladding nano fibrous membrane
The nano fibrous membrane of preparation is immersed in the methane-siliconic acid potassium solution of preparation, is slowly dropped under ultrasound condition dilute
Sulfuric acid, pH value of solution is adjusted to 7 or so, is standing and soak for, poly- methyl silicon is finally dried to obtain at 30 DEG C with pure water three times
The nano fibrous membrane of acid alcohol cladding.
Preferably, in described step 1, spinning material is polyacrylonitrile, chitosan, PLA, polycaprolactone, poly- hydroxyl
Any one in acetate multipolymer.
Preferably, in described step 1, the quality volume fraction that spinning material accounts for total system is 10%~16%.
Preferably, in described step 1, electrospinning parameters are：Spinneret needle diameter is 0.5~0.8mm, voltage is 10~
16kV, it is 8~18cm to receive distance, and fltting speed is 0.5~1.5mL/h.
Preferably, in described step 2, potassium methyl silicate liquid quality fraction is 5%~40%.
Preferably, in described step 3, the mass fraction of dilute sulfuric acid is 1~10%.
Preferably, in described step 3, the pH value of solution is 6~8, and soak time is 3 minutes.
The nanofiber membrane structure that prepared by the above method be used for water-oil emulsion separation is netted more of nano fibrous membrane
Poly- methane-siliconic acid alcohol is filled in hole, and thickness is 0.05~1 millimeter, and weight per square meter is 50~200 grams.
Compared with prior art, the present invention has following remarkable advantage：
(1) nano fibrous membrane of poly- methane-siliconic acid alcohol cladding is successfully prepared using the method for cladding, is made originally hydrophilic
Nano fibrous membrane possesses super lipophilic-hydrophobic property.
(2) simple to operate using electrostatic spinning technique, cost is cheap, and reaction condition is gentle.
(3) manufacture craft of the invention is simple, is easy to industrialized production.
Brief description of the drawings
Fig. 1 is the hydrophobic angle figure of the nano fibrous membrane of poly- methane-siliconic acid alcohol cladding produced by the present invention.
Fig. 2 is the scanning electron microscope (SEM) photograph of the nano fibrous membrane of poly- methane-siliconic acid alcohol cladding produced by the present invention.
Embodiment
With reference to specific implementation example, the present invention is expanded on further.
Embodiment 1
Poly- methane-siliconic acid alcohol is prepared in being soaked in mass fraction as 20% methane-siliconic acid potassium solution using polyacrylonitrile fibre membrane
The nano fibrous membrane of cladding
(1) polyacrylonitrile is dissolved in DMF solution and is configured to spinning solution, spinning material accounts for total system
Mass fraction be 12.5%, and under magnetic stirring to solution clarify it is homogeneous, then stand 24 hours.
(2) electrospinning, electrospinning parameters are carried out in the electric spinning equipment of self assembly：Spinneret needle diameter is 0.8mm, in 15kV electricity
Pressure, it is 15cm to receive distance, carries out electrospinning with 0.8mL/h fltting speed, masking foil is used to receive, each tunica fibrosa spinning
Solution body accumulated amount is 0.5mL.By the electro spinning nanometer fiber membrane drying for standby of collection.The fiber of the electro spinning nanometer fiber membrane of preparation with
Monodisperse status is presented between fiber, fiber surface is smooth, and thickness is homogeneous, no bead structure.
(3) methane-siliconic acid potassium solution 2g is taken, adds 8g pure water, the methane-siliconic acid potassium solution that mass fraction is 20% is made.
(4) nano fibrous membrane of preparation is soaked in 20% methane-siliconic acid potassium solution, slowly dripped under ultrasound condition
Entering 2% dilute sulfuric acid, regulation solution ph is 7.0, then stands 3 minutes, finally with pure water rinsing 3 times, is dried at 30 DEG C,
The nano fibrous membrane of poly- methane-siliconic acid alcohol cladding is obtained, as shown in figure 1, the hydrophobic angle of its super large shows that hydrophobic oleophilic oil is preferable,
Its surface topography is as shown in Fig. 2 nano fibrous membrane surface mesh is filled by poly- methane-siliconic acid alcohol.
Embodiment 2
Poly- methane-siliconic acid is prepared in being soaked in mass fraction as 10% methane-siliconic acid potassium solution using polylactic acid nano fiber film
The nano fibrous membrane of alcohol cladding
(1) PLA is dissolved in DMF solution and is configured to spinning solution, spinning material accounts for total system
Mass fraction is 12.5%, and homogeneous to solution clarification under magnetic stirring, then stands 24 hours.
(2) electrospinning, electrospinning parameters are carried out in the electric spinning equipment of self assembly：Spinneret needle diameter is 0.5mm, in 16kV electricity
Pressure, it is 12cm to receive distance, carries out electrospinning with 0.8mL/h fltting speed, masking foil is used to receive, each tunica fibrosa spinning
Solution body accumulated amount is 0.5mL.By the electro spinning nanometer fiber membrane drying for standby of collection.The fiber of obtained electro spinning nanometer fiber membrane with
Monodisperse status is presented between fiber, fiber surface is smooth, and thickness is homogeneous, no bead structure.
(3) methane-siliconic acid potassium solution 1g is taken, adds 9g pure water, the methane-siliconic acid potassium solution that mass fraction is 10% is made.
(4) it is in 10% methane-siliconic acid potassium solution, in ultrasound condition the nano fibrous membrane of preparation to be soaked in into mass fraction
Under slowly instill 2% dilute sulfuric acid, then regulation solution ph stands 3 minutes to 7.5, finally with pure water rinsing 3 times,
Dried at 30 DEG C, obtain the nano fibrous membrane of poly- methane-siliconic acid alcohol cladding.
Embodiment 3
It is soaked in chitosan nano fiber membrane and receiving for poly- methane-siliconic acid alcohol cladding is prepared in 30% methane-siliconic acid potassium solution
Rice tunica fibrosa
(1) chitosan is dissolved in DMF solution and is configured to spinning solution, spinning material accounts for total system
Mass fraction is 12.5%, and homogeneous to solution clarification under magnetic stirring, then stands 24h.
(2) electrospinning, electrospinning parameters are carried out in homemade electric spinning equipment：Spinneret needle diameter is 0.5mm, in 12kV voltage
Under, it is 15cm to receive distance, carries out electrospinning with 1.0mL/h fltting speed, nanofiber is spun onto masking foil, each fiber
Film spinning solution volume is 0.5mL.By the electro spinning nanometer fiber membrane drying for standby of collection.Obtained electro spinning nanometer fiber membrane
Monodisperse status is presented between fiber and fiber, fiber surface is smooth, and thickness is homogeneous, no bead structure.
(3) raw material methane-siliconic acid potassium solution 1g is taken, adds 9g pure water, it is molten that the potassium methyl silicate that mass fraction is 10% is made
Liquid.
(4) nano fibrous membrane of preparation is soaked in 30% methane-siliconic acid potassium solution, slowly dripped under ultrasound condition
Entering 2% dilute sulfuric acid, regulation solution ph is 7.0, then stands 5 minutes, finally with pure water rinsing 3 times, is dried at 30 DEG C,
Obtain the nano fibrous membrane of poly- methane-siliconic acid alcohol cladding.
Claims (8)
1. the preparation method of a kind of nano fibrous membrane for water-oil emulsion separation, it is characterised in that including walking in detail below
Suddenly：
Step 1：The preparation of polymer solution
Spinning material is dissolved in DMF solution, stir to solution clarify it is homogeneous, stand 1~5 hour, obtain
Polymer solution；
Step 2：The preparation of nano fibrous membrane
By the polymer solution in step 1 by electrostatic spinning, nano fibrous membrane is made；
Step 3：The preparation of poly- methane-siliconic acid alcohol cladding nano fibrous membrane
The nano fibrous membrane of preparation is immersed in the methane-siliconic acid potassium solution of preparation, dilute sulphur is slowly dropped under ultrasound condition
Acid, pH value of solution is adjusted to 6-8, is standing and soak for, with pure water repeated washing, after finally being dried at 30 DEG C, obtain poly- methyl silicon
The nano fibrous membrane of acid alcohol cladding.
2. the preparation method of the nano fibrous membrane separated as claimed in claim 1 for water-oil emulsion, it is characterised in that
In step 1, spinning material is polyacrylonitrile, chitosan, PLA, polycaprolactone, any one in polyglycolic acid copolymers
Kind.
3. the preparation method of the nano fibrous membrane separated as claimed in claim 1 for water-oil emulsion, it is characterised in that step
In rapid 1, the quality volume fraction that spinning material accounts for total system is 10%~16%.
4. the preparation method of the nano fibrous membrane separated as claimed in claim 1 for water-oil emulsion, it is characterised in that step
In rapid 1, electrospinning parameters are：Spinneret needle diameter is 0.4~0.8mm, and voltage is 10~16kV, and it is 8~18cm to receive distance, is pushed away
It is 0.5~1.5mL/h to enter speed.
5. the preparation method of the nano fibrous membrane separated as claimed in claim 1 for water-oil emulsion, it is characterised in that step
In rapid 2, the mass fraction of methane-siliconic acid potassium solution is 5%~40%.
6. the preparation method of the nano fibrous membrane separated as claimed in claim 1 for water-oil emulsion, it is characterised in that step
In rapid 3, the mass fraction of dilute sulfuric acid is 1~10%.
7. the preparation method of the nano fibrous membrane separated as claimed in claim 1 for water-oil emulsion, it is characterised in that step
In rapid 3, soak time is 3~20 minutes.
It is 8. a kind of based on the nano fibrous membrane for being used for water-oil emulsion separation made from claim 1-7 methods describeds, its feature
It is, the described nanofiber membrane structure for being used for water-oil emulsion separation is the netted poly- methyl of porous filling of nano fibrous membrane
Silicic acid alcohol, thickness are 0.05~1 millimeter, and weight per square meter is 50~200 grams.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610530561.1A CN107587267A (en) | 2016-07-06 | 2016-07-06 | One kind is used for water-oil emulsion separation nano fibrous membrane and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610530561.1A CN107587267A (en) | 2016-07-06 | 2016-07-06 | One kind is used for water-oil emulsion separation nano fibrous membrane and preparation method thereof |
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Family
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108754873A (en) * | 2018-05-30 | 2018-11-06 | 齐鲁工业大学 | A kind of super-hydrophobicity CdS/CS/PLA nanofiber composites and the preparation method and application thereof |
| CN108950863A (en) * | 2018-09-21 | 2018-12-07 | 大连瑞源非织造布有限公司 | Wet process spun lacing oily filter cloth and preparation method thereof |
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| EP2589693A1 (en) * | 2010-06-29 | 2013-05-08 | Kao Corporation | Nanofibre |
| CN103866492A (en) * | 2014-03-31 | 2014-06-18 | 北京服装学院 | Efficient oil and water separation composite fiber film and preparation method thereof |
| CN104436760A (en) * | 2014-10-27 | 2015-03-25 | 北京服装学院 | Magnetic response type high-efficiency oil-water separation fiber membrane and preparation method thereof |
| CN104831415A (en) * | 2015-05-18 | 2015-08-12 | 中国石油大学(华东) | Porous fiber membrane with oil-water emulsion separation capacity and preparation method thereof |
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- 2016-07-06 CN CN201610530561.1A patent/CN107587267A/en active Pending
Patent Citations (5)
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|---|---|---|---|---|
| CN101100821A (en) * | 2007-07-04 | 2008-01-09 | 中国科学院长春应用化学研究所 | Preparation method and use for ultra-hydrophobic cotton fibrous material or ultra-hydrophobic paper fibrous material |
| EP2589693A1 (en) * | 2010-06-29 | 2013-05-08 | Kao Corporation | Nanofibre |
| CN103866492A (en) * | 2014-03-31 | 2014-06-18 | 北京服装学院 | Efficient oil and water separation composite fiber film and preparation method thereof |
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| CN108754873B (en) * | 2018-05-30 | 2020-02-04 | 齐鲁工业大学 | Super-hydrophobic CdS/CS/PLA nanofiber composite and preparation method and application thereof |
| CN108950863A (en) * | 2018-09-21 | 2018-12-07 | 大连瑞源非织造布有限公司 | Wet process spun lacing oily filter cloth and preparation method thereof |
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