CN103665832B - Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film and photocuring preparation method thereof - Google Patents
Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film and photocuring preparation method thereof Download PDFInfo
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- CN103665832B CN103665832B CN201310556512.1A CN201310556512A CN103665832B CN 103665832 B CN103665832 B CN 103665832B CN 201310556512 A CN201310556512 A CN 201310556512A CN 103665832 B CN103665832 B CN 103665832B
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- block amide
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- 239000007788 liquid Substances 0.000 title claims abstract description 91
- 229920002614 Polyether block amide Polymers 0.000 title claims abstract description 71
- 229920000642 polymer Polymers 0.000 title claims abstract description 48
- 229920000831 ionic polymer Polymers 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000000016 photochemical curing Methods 0.000 title claims abstract description 13
- 230000000873 masking effect Effects 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000002608 ionic liquid Substances 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 14
- 238000001291 vacuum drying Methods 0.000 claims abstract description 12
- 239000000178 monomer Substances 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 9
- -1 1-octyl Chemical group 0.000 claims description 30
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical group CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 24
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- 239000004809 Teflon Substances 0.000 claims description 11
- 229920006362 Teflon® Polymers 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000012956 1-hydroxycyclohexylphenyl-ketone Substances 0.000 claims description 9
- MQDJYUACMFCOFT-UHFFFAOYSA-N bis[2-(1-hydroxycyclohexyl)phenyl]methanone Chemical group C=1C=CC=C(C(=O)C=2C(=CC=CC=2)C2(O)CCCCC2)C=1C1(O)CCCCC1 MQDJYUACMFCOFT-UHFFFAOYSA-N 0.000 claims description 9
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 6
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 5
- 238000004132 cross linking Methods 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- FQTUOJOWQBMFTM-UHFFFAOYSA-N 1-butyl-3-ethenyl-2h-imidazole Chemical compound CCCCN1CN(C=C)C=C1 FQTUOJOWQBMFTM-UHFFFAOYSA-N 0.000 claims 1
- QGHDLJAZIIFENW-UHFFFAOYSA-N 4-[1,1,1,3,3,3-hexafluoro-2-(4-hydroxy-3-prop-2-enylphenyl)propan-2-yl]-2-prop-2-enylphenol Chemical group C1=C(CC=C)C(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C(CC=C)=C1 QGHDLJAZIIFENW-UHFFFAOYSA-N 0.000 claims 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- 239000003999 initiator Substances 0.000 claims 1
- 229910052698 phosphorus Inorganic materials 0.000 claims 1
- 239000011574 phosphorus Substances 0.000 claims 1
- 238000000926 separation method Methods 0.000 abstract description 15
- 229920006254 polymer film Polymers 0.000 abstract description 10
- 238000012805 post-processing Methods 0.000 abstract description 10
- 239000012528 membrane Substances 0.000 abstract description 6
- 230000002045 lasting effect Effects 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract 1
- 238000007711 solidification Methods 0.000 abstract 1
- 230000008023 solidification Effects 0.000 abstract 1
- 238000001764 infiltration Methods 0.000 description 18
- 230000008595 infiltration Effects 0.000 description 9
- 239000004952 Polyamide Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 150000002148 esters Chemical class 0.000 description 4
- AXNBHOOQHIIQFA-UHFFFAOYSA-N [S].C(F)(F)F Chemical compound [S].C(F)(F)F AXNBHOOQHIIQFA-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- VPRUMANMDWQMNF-UHFFFAOYSA-N phenylethane boronic acid Chemical compound OB(O)CCC1=CC=CC=C1 VPRUMANMDWQMNF-UHFFFAOYSA-N 0.000 description 3
- 229920002647 polyamide Polymers 0.000 description 3
- 229920000570 polyether Polymers 0.000 description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920002292 Nylon 6 Polymers 0.000 description 1
- 238000003848 UV Light-Curing Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 125000002883 imidazolyl group Chemical group 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004879 molecular function Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229920001748 polybutylene Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000909 polytetrahydrofuran Polymers 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 239000012855 volatile organic compound Substances 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
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
- B01D71/80—Block polymers
-
- 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
- B01D67/0006—Organic membrane manufacture by chemical reactions
-
- 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
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0095—Drying
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F226/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
- C08F226/06—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a heterocyclic ring containing nitrogen
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention belongs to gas separation membrane preparation field, particularly relate to a kind of Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film and photocuring preparation method thereof.The preparation method following processing step of employing of described film: 1) prepare masking feed liquid: after polyether block amide (PEBA2533), solvent, ionic liquid monomer uniformly being mixed at 65 DEG C, form masking feed liquid；2) it is cross-linked to form interpenetrating net polymer film: in described masking feed liquid, add cross-linking agent, light trigger, is cured to after supersound process cross-link film forming in photo solidification machine；3) post processing: prepared Semi-IPN film is dried 24 hours in atmosphere, proceeds to vacuum drying oven and is dried 24 hours at 30 DEG C.The one of which component that the film using the present invention to prepare uses polymerisable ionic liquid monomer to be semi-interpenetrating polymer network film, the compatibility with other component is good, stablizes and not easily runs off, can guarantee that the physical arrangement of film and the lasting stability of performance.
Description
Technical field
The invention belongs to gas separation membrane preparation field, particularly relate to a kind of polyether block amide/poly ion liquid semi-interpenetrating polymer
Network film and photocuring preparation method thereof.
Background technology
In the past few decades, along with a large amount of uses of Fossil fuel, the CO in air2Content sharply increase, exacerbate
The greenhouse effect in the whole world.At present, for CO in segregated combustion tail gas2Method and technology have absorption, absorb, condensation at low temperature and
Membrance separation etc..Membrane separation technique is low with its energy consumption, and equipment scale is little, it is easy to advantages such as other technologies combine, becomes current
Research CO2The focus separated.
Polyether block amide (polyether block amide, PEBA) is a kind of rubbery state high-molecular copolymer membrane material, this material
Material is to carry out polycondensation reaction generation when melted with the polyamide containing double hydroxyls and PTMEG, straight at polyamide
Line chain part embedded in polyether components.From structure, it substantially belongs to a kind of linear chain structure, and wherein-PA-represents fat
The block polyamide of fat race rigidity, they are often highly polar, such as nylon-6 (PA-6), PA-12 (PA-12) etc., have poly-
Amide (PA) material hard, provides mechanical strength for PEBA, can overcome excessive adsorption volatile organic matter (VOCs) and
Gas and the film that causes swelling ,-PE-then represents soft low pole polyethers, such as poly(ethylene oxide) (PEO), polybutylene oxide
(PTMEO) etc., soft polyether segment provides bigger free volume, and the most this rigid flexible system is that some is had by PEBA film
Machine thing, gas have good permeability and lay a good foundation.
Ionic liquid, as eco-friendly " cleaning " solvent and emerging catalyst system and catalyzing, has been increasingly becoming chemical industry and association area has been ground
The focus studied carefully；And, it has been found that ionic liquid is to CO2There is special affinity so that it is become for gas separation membrane
Ideal material.But ionic liquid is relatively strong due to segment rigidity, and himself film property is poor.It is big in order to improve poly ion liquid film fragility,
CO2 permeation flux is little and reduces the micron-scale phase separation phenomenon of poly ion liquid copolymer membrane, is prepared for poly ion liquid and plasticity bullet
Gonosome semi-interpenetrating polymer network film (Semi-Interpenetrating Polymer Network, S-IPN or Semi-IPN).Half
Interpenetrating polymer networks is distinctive to force mutual tolerance effect that two kinds of performance differences can be made very big or has the polymer of difference in functionality and formed surely
Fixed combination, thus realize producing special synergism at macro property between component.
Summary of the invention
It is an object of the invention to provide a kind of Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network separated for gas
Film and photocuring preparation method thereof, to overcome the defect of prior art.
A kind of Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film photocuring preparation method that the present invention proposes, it is special
Levy and be to comprise the steps:
A, by polyether block amide 4.5-10 part, solvent 85.3-88.8 part, ionic liquid monomer 1.2-10.2 part at 65 DEG C all
After even mixing, form masking feed liquid；
B, adds the cross-linking agent of 0.2-1.2 part, 0.1-0.3 part light trigger mix homogeneously at 30 DEG C in described masking feed liquid,
Mixed masking feed liquid supersound process is placed on Teflon mold for 10 minutes, at plane UV-curing after standing 10min
Change machine solidifies 1 hour to being cross-linked into film.
The Semi-IPN film that C prepares is dried 24 hours in atmosphere, then proceeds to vacuum drying oven and is dried 24 hours at 30 DEG C
Obtain the Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film that thickness is 130 microns.
Preferably, described solvent is n-butyl alcohol, normal propyl alcohol or isopropanol.
Preferably, described ionic liquid monomer is 1-octyl group-3-vinyl imidazole hexafluorophosphate, 1-octyl group-3-vinyl imidazole four
Borofluoride or 1-octyl group-3-vinyl imidazole bis-trifluoromethylsulfoandimide salt.
Preferably, described cross-linking agent is 1,6-hexanediyl ester, Ethylene glycol dimethacrylate or divinylbenzene.
Preferably, described light trigger is 1-hydroxycyclohexyl phenyl ketone or 2-hydroxy-2-methyl-1-phenyl-1-acetone.
The present invention also proposes a kind of Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film, it is characterised in that formula includes
Following component: polyether block amide 4.5-10 part, solvent 85.3-88.8 part, ionic liquid monomer 1.2-10.2 part, cross-linking agent 0.2-1.2
Part, light trigger 0.1-0.3 part.
Preferably, described solvent is n-butyl alcohol, normal propyl alcohol or isopropanol.
Preferably, described ionic liquid monomer is 1-octyl group-3-vinyl imidazole hexafluorophosphate, 1-octyl group-3-vinyl imidazole four
Borofluoride or 1-octyl group-3-vinyl imidazole bis-trifluoromethylsulfoandimide salt.
Preferably, described cross-linking agent is 1,6-hexanediyl ester, Ethylene glycol dimethacrylate or divinylbenzene.
Preferably, described light trigger is 1-hydroxycyclohexyl phenyl ketone or 2-hydroxy-2-methyl-1-phenyl-1-acetone.
The Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film that the present invention provides, internal crosslinking three-dimensional ionic liquid
Body skeletal support, improves the mechanical strength of film to a certain extent, and the anti-pressure ability of film is strong；In addition the ionic liquid of crosslinking condition is steady
Qualitative well, it is not easy to run off, and high to the adsorption/desorption efficiency of gas.It addition, the CO of polarity2Molecule and poly ion liquid
In imidazole ring on active H have strong interaction so that CO2In film internal ratio N2There is more preferable permeability, it is adaptable to
CO2/ N2Gas separate.
In sum, the preparation method of the Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film of the present invention, be based on
Interpenetrating networks principle is formed, and has the advantage that
1, the present invention uses photocuring processes, and polymerization efficiency is high, and technique is simple, easy to operate, produces reproducible.
2, the one of which component that the present invention uses polymerisable ionic liquid monomer to be semi-interpenetrating polymer network film, itself and other
The compatibility of component is good；Film-forming process has good stability, not easily runs off, can guarantee that the physical arrangement of film and the lasting of performance
Stability.
3, Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film prepared by the inventive method is used, due to film self
Chemical constitution and the impact of molecular function group, to CO2The permeance property of gas is good, to CO2/ N2Separation factor high.
The following is the embodiment of Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film and preparation method thereof, but described reality
Execute example not to be construed as limiting the invention.
Detailed description of the invention
The following is Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film and the embodiment of photocuring preparation method thereof, but
Described embodiment is not construed as limiting the invention.
Embodiment one:
1) masking feed liquid is prepared:
By polyether block amide (PEBA2533) 10 parts, n-butyl alcohol 88.8 parts, 1-octyl group-3-vinyl imidazole hexafluorophosphate
After 1.2 parts uniformly mix at 65 DEG C, form masking feed liquid.
2) interpenetrating net polymer film it is cross-linked to form:
In above-mentioned masking feed liquid, add the 1 of 0.2 part, 6-hexanediyl ester, 0.1 part of 1-hydroxycyclohexyl phenyl ketone in
Mix homogeneously at 30 DEG C, is placed on mixed masking feed liquid supersound process on Teflon mold for 10 minutes, stands 10min
After in plane uv cure machine solidify 1 hour to being cross-linked into film.
3) post processing:
The Semi-IPN film prepared is dried 24 hours in atmosphere, then proceeds to vacuum drying oven and is dried 24 hours thick at 30 DEG C
Degree is the Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film of 130 microns.
It is used for separating CO by above-mentioned Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film2/ N2, CO2Infiltration system
Property more preferable, infiltration coefficient is 198.34barrer, CO2/ N2Separation factor be 24.5.
Embodiment two:
1) masking feed liquid is prepared:
By polyether block amide (PEBA2533) 10 parts, isopropanol 88.8 parts, 1-octyl group-3-vinyl imidazole tetrafluoroborate
After 1.2 parts uniformly mix at 65 DEG C, form masking feed liquid.
2) interpenetrating net polymer film it is cross-linked to form:
The 1 of 0.2 part is added, 6-hexanediyl ester, 0.15 part of 1-hydroxycyclohexyl phenyl ketone in above-mentioned masking feed liquid
Mix homogeneously at 30 DEG C, is placed on mixed masking feed liquid supersound process on Teflon mold for 10 minutes, stands
In plane uv cure machine, 1 hour is solidified to being cross-linked into film after 10min.
3) post processing:
The Semi-IPN film prepared is dried 24 hours in atmosphere, then proceeds to vacuum drying oven and is dried 24 hours thick at 30 DEG C
Degree is the Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film of 130 microns.
It is used for separating CO by above-mentioned Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film2/ N2, CO2Infiltration system
Property more preferable, infiltration coefficient is 213.87barrer, CO2/ N2Separation factor be 26.1.
Embodiment three:
1) masking feed liquid is prepared:
By polyether block amide (PEBA2533) 8.8 parts, n-butyl alcohol 87.4 parts, 1-octyl group-3-vinyl imidazole hexafluorophosphate
After 3.8 parts uniformly mix at 65 DEG C, form masking feed liquid.
2) interpenetrating net polymer film it is cross-linked to form:
In above-mentioned masking feed liquid, add the 1 of 0.4 part, 6-hexanediyl ester, 0.2 part of 1-hydroxycyclohexyl phenyl ketone in
Mix homogeneously at 30 DEG C, is placed on mixed masking feed liquid supersound process on Teflon mold for 10 minutes, stands 10min
After in plane uv cure machine solidify 1 hour to being cross-linked into film.
3) post processing:
The Semi-IPN film prepared is dried 24 hours in atmosphere, then proceeds to vacuum drying oven and is dried 24 hours thick at 30 DEG C
Degree is the Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film of 130 microns.
It is used for separating CO by above-mentioned Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film2/ N2, CO2Infiltration system
Property more preferable, infiltration coefficient is 186.5barrer, CO2/ N2Separation factor be 21.3.
Embodiment four:
1) masking feed liquid is prepared:
By polyether block amide (PEBA2533) 8.8 parts, normal propyl alcohol 87.4 parts, the double fluoroform sulphur of 1-octyl group-3-vinyl imidazole
Imide salts 3, after 8 parts uniformly mix at 65 DEG C, forms masking feed liquid.
2) interpenetrating net polymer film it is cross-linked to form:
The Ethylene glycol dimethacrylate of 0.5 part, 0.25 part of 2-hydroxy-2-methyl-1-phenyl-1-is added in above-mentioned masking feed liquid
Acetone is mix homogeneously at 30 DEG C, mixed masking feed liquid supersound process is placed on Teflon mold for 10 minutes, quiet
In plane uv cure machine, 1 hour is solidified to being cross-linked into film after putting 10min.
3) post processing:
The Semi-IPN film prepared is dried 24 hours in atmosphere, then proceeds to vacuum drying oven and is dried 24 hours thick at 30 DEG C
Degree is the Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film of 130 microns.
It is used for separating CO by above-mentioned Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film2/ N2, CO2Infiltration system
Property more preferable, infiltration coefficient is 227.8barrer, CO2/ N2Separation factor be 24.9.
Embodiment five:
1) masking feed liquid is prepared:
By polyether block amide (PEBA2533) 4.5 parts, n-butyl alcohol 85.3 parts, 1-octyl group-3-vinyl imidazole hexafluorophosphate
After 10.2 parts uniformly mix at 65 DEG C, form masking feed liquid.
2) interpenetrating net polymer film it is cross-linked to form:
The 1 of 1.1 parts is added, 6-hexanediyl ester, 0.25 part of 1-hydroxycyclohexyl phenyl ketone in above-mentioned masking feed liquid
Mix homogeneously at 30 DEG C, is placed on mixed masking feed liquid supersound process on Teflon mold for 10 minutes, stands
In plane uv cure machine, 1 hour is solidified to being cross-linked into film after 10min.
3) post processing:
The Semi-IPN film prepared is dried 24 hours in atmosphere, then proceeds to vacuum drying oven and is dried 24 hours thick at 30 DEG C
Degree is the Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film of 130 microns.
It is used for separating CO by above-mentioned Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film2/N2, CO2Infiltration system
Property more preferable, infiltration coefficient is 172.3barrer, CO2/N2Separation factor be 18.9.
Embodiment six:
1) masking feed liquid is prepared:
By polyether block amide (PEBA2533) 4.5 parts, isopropanol 85.3 parts, 1-octyl group-3-vinyl imidazole tetrafluoroborate
After 10.2 parts uniformly mix at 65 DEG C, form masking feed liquid.
2) interpenetrating net polymer film it is cross-linked to form:
The Ethylene glycol dimethacrylate of 1.2 parts, 0.3 part of 2-hydroxy-2-methyl-1-phenyl-1-is added in above-mentioned masking feed liquid
Acetone is mix homogeneously at 30 DEG C, mixed masking feed liquid supersound process is placed on Teflon mold for 10 minutes, quiet
In plane uv cure machine, 1 hour is solidified to being cross-linked into film after putting 10min.
3) post processing:
The Semi-IPN film prepared is dried 24 hours in atmosphere, then proceeds to vacuum drying oven and is dried 24 hours thick at 30 DEG C
Degree is the Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film of 130 microns.
It is used for separating CO by above-mentioned Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film2/N2, CO2Infiltration system
Property more preferable, infiltration coefficient is 183.6barrer, CO2/N2Separation factor be 20.2.
Embodiment seven:
1) masking feed liquid is prepared:
By polyether block amide (PEBA2533) 10 parts, n-butyl alcohol 88.8 parts, the double fluoroform sulphur of 1-octyl group-3-vinyl imidazole
After imide salts 1.2 parts uniformly mixes at 65 DEG C, form masking feed liquid.
2) interpenetrating net polymer film it is cross-linked to form:
The divinylbenzene, the 0.15 part of 1-hydroxycyclohexyl phenyl ketone that add 0.2 part in above-mentioned masking feed liquid are mixed at 30 DEG C
Close uniformly, mixed masking feed liquid supersound process is placed on Teflon mold for 10 minutes, in plane after standing 10min
Uv cure machine solidifies 1 hour to being cross-linked into film.
3) post processing:
The Semi-IPN film prepared is dried 24 hours in atmosphere, then proceeds to vacuum drying oven and is dried 24 hours thick at 30 DEG C
Degree is the Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film of 130 microns.
It is used for separating CO by above-mentioned Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film2/ N2, CO2Infiltration system
Property more preferable, infiltration coefficient is 259.8barrer, CO2/N2Separation factor be 28.5.
Embodiment eight:
1) masking feed liquid is prepared:
By polyether block amide (PEBA2533) 8.8 parts, isopropanol 87.4 parts, 1-octyl group-3-vinyl imidazole tetrafluoroborate
After 3.8 parts uniformly mix at 65 DEG C, form masking feed liquid.
2) interpenetrating net polymer film it is cross-linked to form:
The divinylbenzene of 0.6 part, 0.2 part of 2-hydroxy-2-methyl-1-phenyl-1-acetone is added in 30 DEG C in above-mentioned masking feed liquid
Lower mix homogeneously, is placed on mixed masking feed liquid supersound process on Teflon mold for 10 minutes, stand after 10min
Plane uv cure machine solidifies 1 hour to being cross-linked into film.
3) post processing:
The Semi-IPN film prepared is dried 24 hours in atmosphere, then proceeds to vacuum drying oven and is dried 24 hours thick at 30 DEG C
Degree is the Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film of 130 microns.
It is used for separating CO by above-mentioned Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film2/ N2, CO2Infiltration system
Property more preferable, infiltration coefficient is 196.8barrer, CO2/ N2Separation factor be 22.4.
Embodiment nine:
1) masking feed liquid is prepared:
By polyether block amide (PEBA2533) 4.5 parts, n-butyl alcohol 85.3 parts, the double fluoroform sulphur of 1-octyl group-3-vinyl imidazole
After imide salts 10.2 parts uniformly mixes at 65 DEG C, form masking feed liquid.
2) interpenetrating net polymer film it is cross-linked to form:
The divinylbenzene of 1.2 parts, 0.25 part of 2-hydroxy-2-methyl-1-phenyl-1-acetone is added in 30 DEG C in above-mentioned masking feed liquid
Lower mix homogeneously, is placed on mixed masking feed liquid supersound process on Teflon mold for 10 minutes, stand after 10min
Plane uv cure machine solidifies 1 hour to being cross-linked into film.
3) post processing:
The Semi-IPN film prepared is dried 24 hours in atmosphere, then proceeds to vacuum drying oven and is dried 24 hours thick at 30 DEG C
Degree is the Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film of 130 microns.
It is used for separating CO by above-mentioned Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film2/ N2, CO2Infiltration system
Property more preferable, infiltration coefficient is 192.89barrer, CO2/ N2Separation factor be 23.0.
The description of above-described embodiment should be considered explanation, it is easy to is understood by, can be without departing from illustrating the most in detail in the claims
The present invention in the case of use many changes and the combination of feature described above, this kind of change has been not to be regarded as a departure from this
Bright spirit and scope, and all such change be included in the range of claims below.
Claims (10)
1. a Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film photocuring preparation method, it is characterised in that comprise the steps:
After polyether block amide 4.5-10 part, solvent 85.3-88.8 part, ionic liquid monomer 1.2-10.2 part are uniformly mixed at 65 DEG C by A, formed
Masking feed liquid；
B adds the cross-linking agent of 0.2-1.2 part, 0.1-0.3 part light trigger mix homogeneously at 30 DEG C in described masking feed liquid, by mixed masking
Feed liquid supersound process is placed on Teflon mold for 10 minutes, solidifies 1 hour to crosslinking after standing 10min in plane uv cure machine
Film forming；
The Semi-IPN film that C prepares is dried 24 hours in atmosphere, then proceed to vacuum drying oven be dried 24 hours at 30 DEG C thickness is 130 micro-
Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film about meter.
Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film photocuring preparation method the most according to claim 1, it is characterised in that
Described solvent is n-butyl alcohol, normal propyl alcohol or isopropanol.
Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film photocuring preparation method the most according to claim 1, it is characterised in that
Described ionic liquid monomer is 1-octyl group-3-vinyl imidazole hexafluorophosphate, 1-octyl group-3-vinyl imidazole tetrafluoroborate or 1-octyl group-3-second
Thiazolinyl imidazoles bis-trifluoromethylsulfoandimide salt.
Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film photocuring preparation method the most according to claim 1, it is characterised in that
Described cross-linking agent is 1,6-hexanediyl ester, Ethylene glycol dimethacrylate or divinylbenzene.
5., according to Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film photocuring preparation method described in any one of claim 1-4, it is special
Levying and be, described light trigger is 1-hydroxycyclohexyl phenyl ketone or 2-hydroxy-2-methyl-1-phenyl-1-acetone.
6. a Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film, it is characterised in that formula includes following component: polyether block amide
4.5-10 part, solvent 85.3-88.8 part, ionic liquid monomer 1.2-10.2 part, cross-linking agent 0.2-1.2 part, light trigger 0.1-0.3 part.
Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film the most according to claim 6, it is characterised in that described solvent is positive fourth
Alcohol, normal propyl alcohol or isopropanol.
Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film the most according to claim 6, it is characterised in that described ionic liquid list
Body is 1-octyl group-3-vinyl imidazole hexafluorophosphate, 1-hexyl-3-vinyl imidazole hexafluorophosphate or 1-butyl-3-vinyl imidazole hexafluoro phosphorus
Hydrochlorate.
Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film the most according to claim 6, it is characterised in that described cross-linking agent is 1,
6-hexanediyl ester, Ethylene glycol dimethacrylate or divinylbenzene.
10. according to Polyether block amide/polyion liquid semi-interpenetratinpolymer polymer network film described in any one of claim 6-9, it is characterised in that described light
Initiator is 1-hydroxycyclohexyl phenyl ketone or 2-hydroxy-2-methyl-1-phenyl-1-acetone.
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| CN105879721A (en) * | 2014-12-16 | 2016-08-24 | 江南大学 | Preparation method of light-chemical crosslinking and hyperbranched-polysiloxane pervaporation membrane |
| CN105879726B (en) * | 2014-12-16 | 2019-01-18 | 江南大学 | A kind of sandwich structure polyether block amide gel mould and preparation method thereof |
| GB201513020D0 (en) * | 2015-07-23 | 2015-09-09 | Fujifilm Mfg Europe Bv | Radiation-curable compositions, membranes and the manufacture and use of such membranes |
| CN105968279B (en) * | 2016-06-27 | 2018-05-04 | 杭州圣传新材料科技有限公司 | One kind can remold recyclable poly ion liquid network material and preparation method |
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