CN109701399A - A kind of corona treatment multi-layer gas composite membrane and its preparation method and application - Google Patents
A kind of corona treatment multi-layer gas composite membrane and its preparation method and application Download PDFInfo
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- CN109701399A CN109701399A CN201711016701.4A CN201711016701A CN109701399A CN 109701399 A CN109701399 A CN 109701399A CN 201711016701 A CN201711016701 A CN 201711016701A CN 109701399 A CN109701399 A CN 109701399A
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Abstract
The invention discloses a kind of corona treatment multi-layer gas composite membranes and its preparation method and application, belong to gas separation membrane field.Atmospheric low-temperature plasma treatment is carried out to composite membrane middle layer, can conveniently and efficiently improve its surface energy and the compatibility with separating layer.There is good compatibility by the middle layer and separating layer of plasma treatment; low concentration coating solution can be coated; and obtain ultra-thin zero defect separating layer and excellent permeability and separation performance; it can avoid the use of essential protective layer in routine film-forming method; reduce painting hierachy number, the preparation efficiency of composite membrane can be effectively improved.
Description
Technical field
The invention belongs to gas separation membrane technical fields, and in particular to a kind of corona treatment multi-layer gas composite membrane and
Preparation method and application.
Background technique
In the energy resource structure in the whole world, there is no in the case where basic variation, the development of social economy is big there is still a need for consuming
The fossil energy of amount, and the use of fossil energy can bring a large amount of pollutants and CO2、SO2、H2The discharge of the acidity such as S, leads to one
Serial environmental problem, such as CO2A large amount of excess emissions will lead to greenhouse effects.For CO2The separation of equal sour gas, UF membrane
Technology has that low energy consumption, and occupied area is few, easy to operate, and easily amplification and control is easy to the combination of other processes, invests less, item
The advantages that part is mild is a kind of very with application prospect separation method.
In CO2Separation in, ether oxygen (EO) group is with it to CO2Wide pass is obtained with excellent permeability and separation performance
Therefore note, the material of the group containing EO also become UF membrane field focus of attention.Polyether block amide (Pebax), polyoxyethylene
Alkene-polybutylene terephthalate (PBT) (Polyactive), polyethylene glycol oxide-polyimide block copolymer, polyethylene glycol oxide-
Polyetherimide blocks' copolymer etc. is all the copolymer containing polyethylene glycol oxide (PEO) block.In addition to EO group, ester group, itrile group,
Amino groups are also to CO2With biggish dissolubility, it can be used to improve membrane material to CO2Solubility.Currently, gas separates
One important development direction of film is the structure optimization of composite membrane.In composite membrane, in order to obtain bigger permeation flux, often
It is required that gas separation membrane has relatively thin separating layer, most of materials cannot keep enough mechanical strengths at this time, therefore, usually
It needs to support counterdie.But be directly coated on separation layer materials on support counterdie, it is easy to the generation of bleed hole infiltration in this way,
Cause film properties poor.The polyether sulfone PES/Pebax-MWNTs composite membrane of the preparations such as Murali, selective separating > 10 μm, CO2
Permeation flux is less than 25GPU (Ind.Eng.Chem.Res., 49 (2010) 6530-6538).Although by counterdie and separating layer
Between introduce dimethyl silicone polymer (PDMS) middle layer can prevent hole seep generation, but due to the surface PDMS can it is lower,
Interfacial effect to hardly result in relatively thin zero defect separating layer on its surface.Currently, most of researchs are by repeatedly coating
PDMS is repaired, i.e., coats one layer of PDMS again in separating layer as protective layer, film-forming process is relatively complicated.
The present invention carries out processing modification to composite membrane middle layer by plasma technique, easily and effectively improves its surface
Can, be conducive to the coating for eliminating interfacial effect and ultra-thin zero defect separating layer, reduction applies hierachy number less, improves the preparation of composite membrane
Efficiency and its separating property.
Summary of the invention
The purpose of the present invention is to provide a kind of composite membrane middle layer method of modifying, reduce and apply hierachy number, improve composite membrane
Preparation efficiency and its separating property.
A kind of corona treatment multi-layer gas composite membrane, the composite membrane are bottom/middle layer/separating layer structure multilayer
Composite membrane;Bottom is porous support layer, 50-200 μm of thickness;Middle layer be high osmosis material, 0.1-10 μm of thickness;Separation
Layer is has the membrane material of good intrinsic separating property to specific gas component, and 10nm-5 μm of thickness.
The primer includes but is not limited to poly (aryl ether sulfone ketone), polyimides, polyetherimide, polysulfones, polyether sulfone, gathers
Acrylonitrile or Kynoar.
The middle layer is silicon rubber or derivatives thereof.
The separation layer materials include but is not limited to the block copolymer containing polyether segment, polyurethane, polyphenylene oxide, polyamides
Amine, polyimides, polyether sulfone, polyether ethersulfone;
Or above-mentioned material and contain ether oxygen, ester group, itrile group, the small organic molecule of amino group or ionic liquid;
Or the blending that constitutes of above-mentioned radical functino ionic liquid, metal organic frame, molecular sieve or carbon nanotube and mixed-matrix
Membrane material;
The block copolymer containing polyether segment includes but is not limited to polyethers-b- amide, polyethers-poly terephthalic acid
Butanediol ester block copolymer, polyethers-polyimide block copolymer, polyethers-polyetherimide blocks' copolymer, polyethers-are poly-
Urethane, polyethers-polylauryllactam, thermoplastic polyurethane and other polyether block copolymers.
A kind of preparation method of corona treatment multi-layer gas composite membrane, multilayer complex films use immersion coating legal system
It is standby, the specific steps are as follows:
(1) bottom is immersed into intermediate layer solution, prepares bottom/interlayer film;
(2) corona treatment is carried out to bottom/middle layer composite membrane;Corona treatment voltage is 0-200V, electric current
For 0-3A, processing speed 1-50cm/s;
(3) by treated, bottom/middle layer composite membrane is impregnated in concentration as in 0.1-10% separating layer solution, dipping is applied
The pull rate covered is 0.1-40cm/s, then by evaporation of solvent, forms bottom/middle layer/separating layer MULTILAYER COMPOSITE
Film.
The intermediate layer solution is the solution of described silicon rubber or derivatives thereof, and wherein solvent includes but is not limited to positive penta
Alkane, hexamethylene, normal heptane, chloroform, methylene chloride, toluene, benzene.
The separating layer Solutions Solution is the solution of separation layer materials, and wherein solvent includes but is not limited to N, N- dimethyl methyl
Amide, DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone, 1-1-2- trichloroethanes, formic acid, acetic acid, n-butyl alcohol, n-butyl alcohol and
1- propanol solvent mixture, ethyl alcohol and water mixed solvent, chloroform, tetrafluoroacetate.
The separation layer materials include but is not limited to the block copolymer containing polyether segment, polyurethane, polyphenylene oxide, polyamides
Amine, polyimides, polyether sulfone, polyether ethersulfone;
Or above-mentioned material and contain ether oxygen, ester group, itrile group, the small organic molecule of amino group or ionic liquid;
Or the blending that constitutes of above-mentioned radical functino ionic liquid, metal organic frame, molecular sieve or carbon nanotube and mixed-matrix
Membrane material;
The block copolymer containing polyether segment includes but is not limited to polyethers-b- amide, polyethers-poly terephthalic acid
Butanediol ester block copolymer, polyethers-polyimide block copolymer, polyethers-polyetherimide blocks' copolymer, polyethers-are poly-
Urethane, polyethers-polylauryllactam, thermoplastic polyurethane and other polyether block copolymers.
The corona treatment is atmospheric low-temperature plasma processing;Low-temperature plasma is generated by glow discharge, is put
Dielectric is air, Ar, He, Ne, Kr, Xe, H2、N2Or O2One of.
A kind of application of corona treatment multi-layer gas composite membrane, it is characterised in that the multilayer complex films are applied to
Gas separation.
The multilayer complex films are applied to sour gas CO2、SO2And H2The separation of S.
Corona treatment acts on middle layer, can effectively improve its surface energy, and decrease even is eliminated interfacial effect, avoids
The use of essential protective layer in conventional film-forming method reduces and applies hierachy number, improves production efficiency.
It is plasma-treated, the compatibility of middle layer and separating layer be improved significantly, can be without using protective layer
In the case of and obtain close to intrinsic selective separating property, that is, obtain ultra-thin zero defect separating layer.
The present invention has the advantages that using plasma processing middle layer is modified have the advantages that it is convenient and efficient,
The modified surface energy that middle layer can be improved, is conducive to the coating of zero defect separating layer.It is separated with traditional bottom/middle layer/
Layer/protective layer structure compares the use for eliminating protective layer, reduces painting hierachy number, can effectively improve production efficiency.
Specific embodiment
Comparative example 1
Polyethers-b- amide (Pebax1657) is dissolved in ethanol/water and obtains 5wt% casting solution, is obtained through casting filming therapy
Pebax homogeneous membrane, 35 DEG C, the film is to CO when 0.5MPa2Selectivity be shown in Table 1.
Table 1.
CO2Infiltration coefficient (Barrer) | CO2/N2 | |
Pure Pebax | 129 | 51 |
Comparative example 2
Polysulfones (Psf) counterdie is impregnated in the pentane solution of middle layer dimethyl silicone polymer (PDMS), will be dried
After wait until Psf/PDMS film.Not plasma treated Psf/PDMS is impregnated in the Pebax1657 ethanol/water separation of 1wt%
In layer solution, composite membrane is taken out from coating solution with the pull rate of 0.5cm/s, then in 40 DEG C of solvent flashing 1d, is obtained
Psf/PDMS/Pebax composite membrane.Room temperature, the performance of the film is shown in Table 3 when 0.5MPa.
Comparative example 3
Polysulfones (Psf) counterdie is impregnated in the pentane solution of middle layer dimethyl silicone polymer (PDMS), will be dried
After wait until Psf/PDMS film.Not plasma treated Psf/PDMS is impregnated in the Pebax1657 ethanol/water separation of 5wt%
In layer solution, composite membrane is taken out from coating solution with the pull rate of 2cm/s, then in 40 DEG C of solvent flashing 1d, is obtained
Psf/PDMS/Pebax composite membrane.Room temperature, the performance of the film is shown in Table 3 when 0.5MPa.
Embodiment 1
Polysulfones (Psf) counterdie is impregnated in the pentane solution of middle layer dimethyl silicone polymer (PDMS), will be dried
After wait until Psf/PDMS film.The Psf/PDMS of (voltage 50V, electric current 1.8A, processing speed 20cm/s) is denoted as after plasma treatment
Psf/PDMS-plasme is impregnated in the Pebax1657 ethanol/water separating layer solution of 1wt%, with the lifting of 20cm/s
Speed takes out composite membrane from coating solution, and then in 40 DEG C of solvent flashing 1d, it is compound to obtain Psf/PDMS-plasme/Pebax
Film, the performance of the film is shown in Table 2 when 0.5MPa.
Table 2.
Embodiment 2
Polysulfones (Psf) counterdie is impregnated in the pentane solution of middle layer dimethyl silicone polymer (PDMS), will be dried
After wait until Psf/PDMS film.Psf/PDMS after plasma treatment (voltage 100V, electric current 2A, processing speed 50cm/s) is denoted as
Psf/PDMS-plasme is impregnated in the Pebax1657 ethanol/water separating layer solution of 1wt%, with the lifting of 40cm/s
Speed takes out composite membrane from coating solution, and then in 40 DEG C of solvent flashing 1d, it is compound to obtain Psf/PDMS-plasme/Pebax
Film, CO2 flux are higher than 150GPU, and CO2/N2 is selectively greater than 35, function admirable.
Embodiment is analyzed as follows with comparative example data:
Table 3.
CO2Permeation flux (GPU) | CO2/N2 | |
Pure Pebax | 129Barrer | 51 |
Psf/PDMS/Pebax (1wt%) | 1536 | 10 |
Psf/PDMS/Pebax (5wt%) | 8 | 50 |
The intrinsic CO of PDMS and Pebax2/N2Selectivity is respectively 10 and 51.It can by the comparison of 3 comparative example 1,2,3 of table
Know, misaligns interbed and carry out corona treatment, when separating layer solution concentration is lower, since interlayer surfaces can be larger, with
Separating layer compatibility is poor, can not obtain complete separating layer, causes prepared multilayer complex films without separating property.Work as separating layer
Solution concentration increases, and viscosity increases, and the bonding force between middle layer also increases with it, and can obtain complete separation at this time
Layer, acquisition and the comparable selectivity of intrinsic separation property, but separating layer is thicker at this time, the CO of acquisition2Permeation flux is extremely low.
Table 4.
CO2Permeation flux (GPU) | CO2/N2 | |
Psf/PDMS/Pebax (1wt%) | 1536 | 10 |
Psf/PDMS-plasme/Pebax (1wt%) | 152 | 50 |
Psf/PDMS/Pebax (5wt%) | 8 | 50 |
Table 4 is comparative example 2,3, the comparison of embodiment 1, it can be seen that after corona treatment, composite membrane be can get and this
The comparable selectivity of separation property is levied, shows that separating layer is complete, while separating layer is again relatively thin, so that permeation flux is larger.
Table 5.
CO2Permeability | CO2/N2 | |
Pure Pebax | 129Barrer | 51 |
Psf/PDMS-plasme/Pebax (1wt%) | 218GPU | 38 |
Table 5 is the comparison of comparative example 1, embodiment 1, under the same test conditions, after corona treatment, composite membrane
The available and comparable selectivity of intrinsic separation property, and permeation flux is larger, shows there is ultra-thin complete separating layer, separating layer
Know that separating layer is at this time with a thickness of 0.6 μm by calculating.
It is modified to composite membrane middle layer by plasma, ultra-thin zero defect can be obtained in unprotected situation
Separating layer reduces painting hierachy number, can effectively improve production efficiency.
Claims (10)
1. a kind of corona treatment multi-layer gas composite membrane, it is characterised in that: the composite membrane is bottom/middle layer/separating layer
The multilayer complex films of structure;Bottom is porous support layer, 50-200 μm of thickness;Middle layer is the material of high osmosis, thickness
0.1-10μm;Separating layer is the membrane material for having good intrinsic separating property to specific gas component, 10nm-5 μm of thickness.
2. a kind of corona treatment multi-layer gas composite membrane according to claim 1, it is characterised in that: the backsheet
Material includes but is not limited to poly (aryl ether sulfone ketone), polyimides, polyetherimide, polysulfones, polyether sulfone, polyacrylonitrile or polyvinylidene fluoride
Alkene.
3. a kind of corona treatment multi-layer gas composite membrane according to claim 1, it is characterised in that: the middle layer
For silicon rubber or derivatives thereof.
4. a kind of corona treatment multi-layer gas composite membrane according to claim 1, it is characterised in that: the separating layer
Material includes but is not limited to the block copolymer containing polyether segment, polyurethane, polyphenylene oxide, polyamide, polyimides, polyether sulfone
Or polyether ethersulfone;
Or above-mentioned material and contain ether oxygen, ester group, itrile group, the small organic molecule of amino group or ionic liquid;Or
The blending and mixed-matrix membrane material that above-mentioned radical functino ionic liquid, metal organic frame, molecular sieve or carbon nanotube are constituted
Material.
5. a kind of corona treatment multi-layer gas composite membrane according to claim 4, it is characterised in that: described containing poly-
The block copolymer of ether segment includes but is not limited to polyethers-b- amide, polyethers-polybutylene terephthalate (PBT) block copolymerization
Object, polyethers-polyimide block copolymer, polyethers-polyetherimide blocks' copolymer, polyether-polyurethane, polyethers-polyoxyethylene lauryl
Base lactams, thermoplastic polyurethane and other polyether block copolymers.
6. a kind of preparation of corona treatment multi-layer gas composite membrane described in any claim in -5 according to claim 1
Method, it is characterised in that: multilayer complex films are prepared using dip-coating method, the specific steps are as follows:
(1) bottom is immersed into intermediate layer solution, prepares bottom/interlayer film;
(2) corona treatment is carried out to bottom/middle layer composite membrane;Corona treatment voltage is 0-200V, electric current 0-
3A, processing speed 1-50cm/s;
(3) will treated that bottom/middle layer composite membrane is impregnated in that concentration is in 0.1-10% separating layer solution, immersion coating
Pull rate is 0.1-40cm/s, then by evaporation of solvent, forms bottom/middle layer/separating layer multilayer complex films.
7. a kind of preparation method of corona treatment multi-layer gas composite membrane according to claim 6, it is characterised in that:
The intermediate layer solution is the solution of silicon rubber or derivatives thereof, and wherein solvent includes but is not limited to pentane, hexamethylene, positive heptan
Alkane, chloroform, methylene chloride, toluene or benzene;
The separating layer Solutions Solution is the solution of separation layer materials, and wherein solvent includes but is not limited to N, N- dimethyl formyl
Amine, DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone, 1-1-2- trichloroethanes, formic acid, acetic acid, n-butyl alcohol, n-butyl alcohol and 1-
Propanol solvent mixture, ethyl alcohol and water mixed solvent, chloroform or tetrafluoroacetate;
The separation layer materials include but is not limited to the block copolymer containing polyether segment, polyurethane, polyphenylene oxide, polyamide,
Polyimides, polyether sulfone or polyether ethersulfone;
Or above-mentioned material and contain ether oxygen, ester group, itrile group, the small organic molecule of amino group or ionic liquid;Or
The blending and mixed-matrix membrane material that above-mentioned radical functino ionic liquid, metal organic frame, molecular sieve or carbon nanotube are constituted
Material.
8. a kind of preparation method of corona treatment multi-layer gas composite membrane according to claim 6, it is characterised in that
The corona treatment is atmospheric low-temperature plasma processing;Low-temperature plasma is generated by glow discharge, and discharge medium is
Air, Ar, He, Ne, Kr, Xe, H2、N2Or O2One of.
9. a kind of application of corona treatment multi-layer gas composite membrane described in -5 any claims according to claim 1,
It is characterized in that the multilayer complex films are separated applied to gas.
10. a kind of application of corona treatment multi-layer gas composite membrane according to any claim of claim 9,
It is characterized in that the multilayer complex films are applied to sour gas CO2、SO2And H2The separation of S.
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CN111111479A (en) * | 2020-01-02 | 2020-05-08 | 中国科学院大连化学物理研究所 | Mixed matrix membrane for gas separation and preparation method and application thereof |
CN112023730A (en) * | 2020-09-18 | 2020-12-04 | 天津工业大学 | Preparation of block polyether amide-photosensitive copper organic framework film and gas separation application |
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