CN106179000A - A kind of preparation method of solvent resistant NF membrane - Google Patents
A kind of preparation method of solvent resistant NF membrane Download PDFInfo
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- CN106179000A CN106179000A CN201610687032.2A CN201610687032A CN106179000A CN 106179000 A CN106179000 A CN 106179000A CN 201610687032 A CN201610687032 A CN 201610687032A CN 106179000 A CN106179000 A CN 106179000A
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- 239000012528 membrane Substances 0.000 title claims abstract description 70
- 239000002904 solvent Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 210000004379 membrane Anatomy 0.000 claims abstract description 68
- -1 siloxanes Chemical class 0.000 claims abstract description 35
- 210000002469 basement membrane Anatomy 0.000 claims abstract description 34
- 238000005266 casting Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- 229920002492 poly(sulfone) Polymers 0.000 claims description 13
- 229920002379 silicone rubber Polymers 0.000 claims description 12
- 239000004945 silicone rubber Substances 0.000 claims description 11
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 10
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 10
- 239000003960 organic solvent Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 7
- 238000004132 cross linking Methods 0.000 claims description 7
- 238000007654 immersion Methods 0.000 claims description 7
- 238000000935 solvent evaporation Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000003431 cross linking reagent Substances 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 4
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 4
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 3
- 239000004695 Polyether sulfone Substances 0.000 claims description 3
- 229920006393 polyether sulfone Polymers 0.000 claims description 3
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 2
- 239000002033 PVDF binder Substances 0.000 claims description 2
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 2
- ZJKABZNFELLAQQ-UHFFFAOYSA-N octane Chemical compound CCCCCCCC.CCCCCCCC ZJKABZNFELLAQQ-UHFFFAOYSA-N 0.000 claims description 2
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims 4
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 2
- 238000006555 catalytic reaction Methods 0.000 claims 2
- 239000000377 silicon dioxide Substances 0.000 claims 2
- RZYKUPXRYIOEME-UHFFFAOYSA-N CCCCCCCCCCCC[S] Chemical compound CCCCCCCCCCCC[S] RZYKUPXRYIOEME-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 26
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 20
- 229940012189 methyl orange Drugs 0.000 description 20
- 238000012360 testing method Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 6
- 239000012530 fluid Substances 0.000 description 5
- 230000004907 flux Effects 0.000 description 5
- 230000003204 osmotic effect Effects 0.000 description 5
- 230000000149 penetrating effect Effects 0.000 description 5
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 5
- 239000011550 stock solution Substances 0.000 description 5
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 238000001728 nano-filtration Methods 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- DGYMCGCIUWHSNH-UHFFFAOYSA-N C(CCC)[Sn]CCCC.C(CCCCCCCCCCC)[S] Chemical compound C(CCC)[Sn]CCCC.C(CCCCCCCCCCC)[S] DGYMCGCIUWHSNH-UHFFFAOYSA-N 0.000 description 1
- USEBIPUIVPERGC-UHFFFAOYSA-N Dibutylone Chemical compound CCC(N(C)C)C(=O)C1=CC=C2OCOC2=C1 USEBIPUIVPERGC-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- 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
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
-
- 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
- B01D67/0002—Organic membrane manufacture
-
- 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
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
-
- 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
- B01D71/06—Organic material
- B01D71/40—Polymers of unsaturated acids or derivatives thereof, e.g. salts, amides, imides, nitriles, anhydrides, esters
- B01D71/42—Polymers of nitriles, e.g. polyacrylonitrile
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses the preparation method of a kind of solvent resistant NF membrane, the method includes: preparation siloxanes casting solution, guarantor hole pretreatment, the preparation of solvent resistant NF membrane of basement membrane.By the solvent resistant NF membrane that a process for preparing, have that separating property is good, intensity advantages of higher, in preparation process, especially add the guarantor hole pretreatment of basement membrane, make the solvent resistant NF membrane prepared effectively avoid hole and ooze phenomenon, significantly improve the stability of solvent resistant NF membrane performance.
Description
Technical field
The present invention relates to organic solvent nanofiltration technical field, be specifically related to the preparation method of a kind of solvent resistant NF membrane.
Background technology
Macromolecular nano filtering membrane is the pressure-actuated Novel separation film of the one between reverse osmosis membrane and ultrafilter membrane, exists
Each industrial circle and scientific research are used widely, presently mainly concentrate on water solution system, and actual industrial flow process
The significant portion related to is organic solvent system.The plurality of advantages of nanofiltration process, if separation process is without phase transformation, without adding
Agent, temperature impact are little etc. so that it is have the most potential in the non-aqueous solution system in the fields such as petrochemical industry, medicine and food
Using value, and traditional NF membrane is difficult to widen in non-aqueous solution system use, therefore research and development is resistance to molten further
Agent NF membrane has extremely important function and significance for widening the application of its process.
At present, solvent resistant NF membrane many employings cladding process prepares.Cladding process is that casting solution is attached to porous basement membrane
On, it is allowed to fully crosslinked by heat treatment etc. and obtains.Due to the effect of capillary force, in dip coating process, at open support
Internal hole can be occurred to ooze phenomenon.Although coating only has a few micrometers thick, but has penetrated in hole due to casting solution so that the biography of supporting layer
Matter resistance increases, especially for glassy polymers.Therefore, be reduced or avoided that hole oozes for solvent resistant NF membrane performance is steady
Fixed and lifting has great importance and is worth.
Summary of the invention
For solving above-mentioned technical problem, the invention provides the preparation method of a kind of solvent resistant NF membrane.
The present invention is achieved by the following technical programs:
A kind of preparation method of solvent resistant NF membrane, the method comprises the following steps:
A, preparation siloxanes casting solution: siloxanes is dissolved in organic solvent, magnetic agitation 30min, add cross-linking agent and
Catalyst stirs, and obtains siloxanes casting solution after filtering deaeration；
B, the guarantor hole pretreatment of basement membrane: basement membrane is put into immersion 30min in the guarantor hole liquid of 15%, and by it in temperature is
Heat treatment 10min in the baking oven of 50-60 DEG C, stand-by after being cooled to room temperature after being taken out from baking oven by basement membrane；
C, the preparation of solvent resistant NF membrane: the siloxanes casting solution prepared in step a is coated in step b after pretreatment
Basement membrane on, room temperature in air stop 10-60min, until solvent evaporation and tentatively cross-link after, 90-100 DEG C of heat treatment in an oven
100min, prepares solvent resistant NF membrane.
Siloxanes in described step a is the one in 107 silicone rubber or polydimethylsiloxane.
In described step a, siloxanes mass concentration is 20-25%.
Organic solvent in described step a is one or more in toluene, normal hexane, hexamethylene, normal heptane or octane.
Cross-linking agent in described step a is tetraethyl orthosilicate, γ aminopropyltriethoxy silane, phenyl trimethoxy
One or more in silane or octyl group trimethoxy silane.
Catalyst in described step a is dibutyl tin dilaurate, stannous octoate, two (dodecyl sulfur) dibutyl tin
Or one or more in dibutyltin diacetate.
The mass ratio of siloxanes, cross-linking agent and catalyst in described step a is 10:1:0.5,10:2:0.5,10:1:1,
One in 10:2:1,10:2:2.
Hole liquid of protecting in described step b is one or more in glycerol, isopropanol, n-butyl alcohol, deionized water.
The basement membrane of described step b is that polysulfone porous membrane, polyethersulfone porous membrane, polyvinylidene fluoride porous film or polyacrylonitrile are many
One in pore membrane.
The beneficial effects of the present invention is: by the solvent resistant NF membrane that a process for preparing, there is separating property good, strong
Degree advantages of higher, especially adds the guarantor hole pretreatment of basement membrane so that the solvent resistant NF membrane prepared in preparation process
Effectively avoid hole and ooze phenomenon, significantly improve the stability of solvent resistant NF membrane performance.
Accompanying drawing explanation
Fig. 1 is the surface topography map of solvent resistant NF membrane of the present invention；
Fig. 2 is the cross-section morphology figure of solvent resistant NF membrane of the present invention.
Detailed description of the invention
Below in conjunction with drawings and Examples, technical scheme is further described, but claimed scope is also
It is not limited to described.
Embodiment 1
A, preparation siloxanes casting solution: polydimethylsiloxane is dissolved in normal hexane, magnetic agitation 30min, is just adding
Silester and dibutyl tin dilaurate stir, and obtain siloxanes casting solution, the most poly-diformazan after filtering deaeration
The mass concentration of radical siloxane is 25%, and polydimethylsiloxane, tetraethyl orthosilicate, the mass ratio of dibutyl tin dilaurate are
10:1:0.5；
B, the guarantor hole pretreatment of basement membrane: polysulfones basement membrane is put into immersion 30min in the guarantor hole liquid of 15%, and by it in temperature
It is heat treatment 10min in the baking oven of 60 DEG C, stand-by after being cooled to room temperature after being taken out from baking oven by basement membrane；
C, the preparation of solvent resistant NF membrane: the siloxanes casting solution that step a prepares is coated in step b pretreated
On polysulfone porous basement membrane, room temperature in air stops 30min, after solvent evaporation tentatively cross-linking, and 100 DEG C of heat treatments in an oven
100min, prepares solvent resistant NF membrane.
As depicted in figs. 1 and 2, the surface topography of obtained solvent resistant NF membrane and the scanning electricity of cross-section morphology it are respectively
Mirror picture.The surface of solvent resistant NF membrane is that even compact does not has defect as seen from Figure 1, obtained as seen from Figure 2
The cross-linked layer of solvent resistant NF membrane be coated uniformly on polysulfones basement membrane, cross-linked layer does not infiltrate through in polysulfone porous membrane.
The solvent resistant NF membrane preparing the present embodiment carries out organic solvent solution separating property test: by methyl orange/different
Propanol stock solution is 25 DEG C at feeding temperature, and feed pressure is to flow through solvent resistant NF membrane surface under 3MPa, under the effect of the pressure,
Isopropanol and a small amount of methyl orange overcome osmotic pressure to pass through NF membrane surface, obtain the penetrating fluid containing very small amount methyl orange, after testing
Permeation flux is 0.867L/m2h, and the rejection to methyl orange is 95.7%.
Embodiment 2
A, preparation siloxanes casting solution: 107 silicone rubber are dissolved in normal hexane, magnetic agitation 30min, add positive silicic acid second
Ester and dibutyl tin dilaurate stir, and obtain siloxanes casting solution, the wherein matter of 107 silicone rubber after filtering deaeration
Amount concentration is 20%, and 107 silicone rubber, tetraethyl orthosilicate, the mass ratio of dibutyl tin dilaurate are 10:1:0.5；
B, the guarantor hole pretreatment of basement membrane: polysulfones basement membrane is put into immersion 30min in the guarantor hole liquid of 15%, and by it in temperature
It is heat treatment 10min in the baking oven of 50 DEG C, stand-by after being cooled to room temperature after being taken out from baking oven by basement membrane；
C, the preparation of solvent resistant NF membrane: the siloxanes casting solution that step a prepares is coated in step b pretreated
On polyether sulfone porous basement membrane, room temperature in air stops 30min, after solvent evaporation tentatively cross-linking, in an oven at 90 DEG C of heat
Reason 100min, prepares solvent resistant NF membrane.
The solvent resistant NF membrane preparing the present embodiment carries out organic solvent solution separating property test: by methyl orange/different
Propanol stock solution is 25 DEG C at feeding temperature, and feed pressure is to flow through solvent resistant NF membrane surface under 3MPa, under the effect of the pressure,
Isopropanol and a small amount of methyl orange overcome osmotic pressure to pass through NF membrane surface, obtain the penetrating fluid containing very small amount methyl orange, after testing
Permeation flux is 1.308L/m2h, and the rejection to methyl orange is 93%.
Embodiment 3
A, preparation siloxanes casting solution: 107 silicone rubber are dissolved in normal hexane, magnetic agitation 30min, add positive silicic acid second
Ester and dibutyl tin dilaurate stir, and obtain siloxanes casting solution, the wherein matter of 107 silicone rubber after filtering deaeration
Amount concentration is 20%, and 107 silicone rubber, tetraethyl orthosilicate, the mass ratio of dibutyl tin dilaurate are 0:2:0.5；
B, the guarantor hole pretreatment of basement membrane: polysulfones basement membrane is put into immersion 30min in the guarantor hole liquid of 15%, and by it in temperature
It is heat treatment 10min in the baking oven of 50 DEG C, stand-by after being cooled to room temperature after being taken out from baking oven by basement membrane；
C, the preparation of solvent resistant NF membrane: the siloxanes casting solution that step a prepares is coated in step b pretreated
On polysulfone porous basement membrane, room temperature in air stops 30min, after solvent evaporation tentatively cross-linking, and 90 DEG C of heat treatments in an oven
100min, prepares solvent resistant NF membrane.
The solvent resistant NF membrane preparing the present embodiment carries out organic solvent solution separating property test: by methyl orange/different
Propanol stock solution is 25 DEG C at feeding temperature, and feed pressure is to flow through solvent resistant NF membrane surface under 3MPa, under the effect of the pressure,
Isopropanol and a small amount of methyl orange overcome osmotic pressure to pass through NF membrane surface, obtain the penetrating fluid containing very small amount methyl orange, after testing
Permeation flux is 0.987L/m2h, and the rejection to methyl orange is 94%.
Embodiment 4
A, preparation siloxanes casting solution: 107 silicone rubber are dissolved in normal hexane, magnetic agitation 30min, add phenyl front three
TMOS and dibutyl tin dilaurate stir, and obtain siloxanes casting solution, wherein 107 silicon rubber after filtering deaeration
The mass concentration of glue is 20%, and 107 silicone rubber, phenyltrimethoxysila,e, the mass ratio of dibutyl tin dilaurate are 10:2:
0.5；
B, the guarantor hole pretreatment of basement membrane: polysulfones basement membrane is put into immersion 30min in the guarantor hole liquid of 15%, and by it in temperature
It is heat treatment 10min in the baking oven of 50 DEG C, stand-by after being cooled to room temperature after being taken out from baking oven by basement membrane；
C, the preparation of solvent resistant NF membrane: the siloxanes casting solution that step a prepares is coated in step b pretreated
On polysulfone porous basement membrane, room temperature in air stops 30min, after solvent evaporation tentatively cross-linking, and 90 DEG C of heat treatments in an oven
100min, prepares solvent resistant NF membrane.
The solvent resistant NF membrane preparing the present embodiment carries out organic solvent solution separating property test: by methyl orange/different
Propanol stock solution is 25 DEG C at feeding temperature, and feed pressure is to flow through solvent resistant NF membrane surface under 3MPa, under the effect of the pressure,
Isopropanol and a small amount of methyl orange overcome osmotic pressure to pass through NF membrane surface, obtain the penetrating fluid containing very small amount methyl orange, after testing
Permeation flux is 0.987L/m2h, and the rejection to methyl orange is 94%.
Embodiment 5
A, preparation siloxanes casting solution: polydimethylsiloxane is dissolved in normal heptane, magnetic agitation 30min, adds benzene
Base trimethoxy silane and stannous octoate stir, and obtain siloxanes casting solution after filtering deaeration.Wherein 107 silicone rubber
Mass concentration be 20%, polydimethylsiloxane, phenyltrimethoxysila,e, the mass ratio of stannous octoate are 10:2:1；
B, the guarantor hole pretreatment of basement membrane: polysulfones basement membrane is put into immersion 30min in the guarantor hole liquid of 15%, and by it in temperature
It is heat treatment 10min in the baking oven of 50 DEG C, stand-by after being cooled to room temperature after being taken out from baking oven by basement membrane；
B, the preparation of solvent resistant NF membrane: the siloxanes casting solution that step a prepares is coated in step b pretreated
On polysulfone porous basement membrane, room temperature in air stops 30min, after solvent evaporation tentatively cross-linking, and 90 DEG C of heat treatments in an oven
100min, prepares solvent resistant NF membrane.
The solvent resistant NF membrane preparing the present embodiment carries out organic solvent solution separating property test: by methyl orange/different
Propanol stock solution is 25 DEG C at feeding temperature, and feed pressure is to flow through solvent resistant NF membrane surface under 3MPa, under the effect of the pressure,
Isopropanol and a small amount of methyl orange overcome osmotic pressure to pass through NF membrane surface, obtain the penetrating fluid containing very small amount methyl orange, after testing
Permeation flux is 0.734L/m2h, and the rejection to methyl orange is 92.5%.
Above example only in order to illustrate that technical scheme is not intended to limit, to without departing from the present invention spirit and
Any amendment of scope or equivalent, it all should be contained in the middle of scope of the presently claimed invention.
Claims (9)
1. the preparation method of a solvent resistant NF membrane, it is characterised in that: the method comprises the following steps:
A, preparation siloxanes casting solution: siloxanes is dissolved in organic solvent, magnetic agitation 30min, adds cross-linking agent and catalysis
Agent stirs, and obtains siloxanes casting solution after filtering deaeration；
B, the guarantor hole pretreatment of basement membrane: basement membrane is put in the guarantor hole liquid of 15% immersion 30min, and be 50-60 by it in temperature
DEG C baking oven in heat treatment 10min, stand-by after being cooled to room temperature after being taken out from baking oven by basement membrane；
C, the preparation of solvent resistant NF membrane: the siloxanes casting solution prepared in step a is coated on pretreated base in step b
On film, room temperature in air stops 10-60min, after solvent evaporation tentatively cross-linking, and 90-100 DEG C of heat treatment in an oven
100min, prepares solvent resistant NF membrane.
The preparation method of solvent resistant NF membrane the most according to claim 1, it is characterised in that: the silica in described step a
Alkane is the one in 107 silicone rubber or polydimethylsiloxane.
The preparation method of solvent resistant NF membrane the most according to claim 1, it is characterised in that: siloxanes in described step a
Mass concentration is 20-25%.
The preparation method of solvent resistant NF membrane the most according to claim 1, it is characterised in that: organic in described step a
Solvent is one or more in toluene, normal hexane, hexamethylene, normal heptane or octane.
The preparation method of solvent resistant NF membrane the most according to claim 1, it is characterised in that: the crosslinking in described step a
Agent is in tetraethyl orthosilicate, γ aminopropyltriethoxy silane, phenyltrimethoxysila,e or octyl group trimethoxy silane
One or more.
The preparation method of solvent resistant NF membrane the most according to claim 1, it is characterised in that: the catalysis in described step a
Agent is the one in dibutyl tin dilaurate, stannous octoate, two (dodecyl sulfur) dibutyl tins or dibutyltin diacetate
Or it is several.
The preparation method of solvent resistant NF membrane the most according to claim 1, it is characterised in that: the silica in described step a
The mass ratio of alkane, cross-linking agent and catalyst is the one in 10:1:0.5,10:2:0.5,10:1:1,10:2:1,10:2:2.
The preparation method of solvent resistant NF membrane the most according to claim 1, it is characterised in that: the guarantor hole in described step b
Liquid is one or more in glycerol, isopropanol, n-butyl alcohol, deionized water.
The preparation method of solvent resistant NF membrane the most according to claim 1, it is characterised in that: the basement membrane of described step b is
One in polysulfone porous membrane, polyethersulfone porous membrane, polyvinylidene fluoride porous film or polyacrylonitrile porous membrane.
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| CN201610687032.2A CN106179000A (en) | 2016-08-18 | 2016-08-18 | A kind of preparation method of solvent resistant NF membrane |
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| CN201610687032.2A CN106179000A (en) | 2016-08-18 | 2016-08-18 | A kind of preparation method of solvent resistant NF membrane |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108636118A (en) * | 2018-05-16 | 2018-10-12 | 南京帝膜净水材料开发有限公司 | A kind of preparation method of complex reverse osmosis membrane |
| CN109046035A (en) * | 2018-08-28 | 2018-12-21 | 浙江工业大学 | A kind of hydrophilic modifying Kynoar filter membrane and its application |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102794117A (en) * | 2012-07-29 | 2012-11-28 | 北京工业大学 | Preparation method of silazane-modified silicalite-1 molecular sieve filling silicon rubber composite membrane |
| CN102921311A (en) * | 2012-10-30 | 2013-02-13 | 北京化工大学 | Preparation method of type-priority ethanol permeable membrane |
| CN103463999A (en) * | 2013-09-06 | 2013-12-25 | 烟台绿水赋膜材料有限公司 | Preparation method of novel ultrathin salt-cutting separation membrane |
| CN104437141A (en) * | 2014-11-17 | 2015-03-25 | 清华大学 | Preparation method of solvent resistant nanofiltration membrane |
| CN105169959A (en) * | 2015-07-20 | 2015-12-23 | 北京工业大学 | Method for rapid and environmentally-friendly production of compact separation membrane |
| CN105396472A (en) * | 2015-12-24 | 2016-03-16 | 北京碧水源膜科技有限公司 | Preparation method of composite base-membrane nanofiltration membrane |
| CN105771705A (en) * | 2014-12-23 | 2016-07-20 | 北京化工大学常州先进材料研究院 | Application of modified polyvinyl triethoxysilane membrane material in separating of butanol/water system |
-
2016
- 2016-08-18 CN CN201610687032.2A patent/CN106179000A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102794117A (en) * | 2012-07-29 | 2012-11-28 | 北京工业大学 | Preparation method of silazane-modified silicalite-1 molecular sieve filling silicon rubber composite membrane |
| CN102921311A (en) * | 2012-10-30 | 2013-02-13 | 北京化工大学 | Preparation method of type-priority ethanol permeable membrane |
| CN103463999A (en) * | 2013-09-06 | 2013-12-25 | 烟台绿水赋膜材料有限公司 | Preparation method of novel ultrathin salt-cutting separation membrane |
| CN104437141A (en) * | 2014-11-17 | 2015-03-25 | 清华大学 | Preparation method of solvent resistant nanofiltration membrane |
| CN105771705A (en) * | 2014-12-23 | 2016-07-20 | 北京化工大学常州先进材料研究院 | Application of modified polyvinyl triethoxysilane membrane material in separating of butanol/water system |
| CN105169959A (en) * | 2015-07-20 | 2015-12-23 | 北京工业大学 | Method for rapid and environmentally-friendly production of compact separation membrane |
| CN105396472A (en) * | 2015-12-24 | 2016-03-16 | 北京碧水源膜科技有限公司 | Preparation method of composite base-membrane nanofiltration membrane |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108636118A (en) * | 2018-05-16 | 2018-10-12 | 南京帝膜净水材料开发有限公司 | A kind of preparation method of complex reverse osmosis membrane |
| CN109046035A (en) * | 2018-08-28 | 2018-12-21 | 浙江工业大学 | A kind of hydrophilic modifying Kynoar filter membrane and its application |
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