CN112915821A - Preparation method of amphiphilic polymer blending modified rubbery polymer blending membrane - Google Patents

Preparation method of amphiphilic polymer blending modified rubbery polymer blending membrane Download PDF

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Publication number
CN112915821A
CN112915821A CN202110142602.0A CN202110142602A CN112915821A CN 112915821 A CN112915821 A CN 112915821A CN 202110142602 A CN202110142602 A CN 202110142602A CN 112915821 A CN112915821 A CN 112915821A
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pebax
membrane
pedot
solution
pss
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李雪琴
王江南
吕侠
黄路
李珑
张金利
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Shihezi University
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Shihezi University
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    • 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
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
    • B01D53/228—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion characterised by specific membranes
    • 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
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002—Organic membrane manufacture
    • B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
    • B01D67/0011—Casting solutions therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
    • 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
    • B01D71/82—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74 characterised by the presence of specified groups, e.g. introduced by chemical after-treatment

Abstract

The invention discloses a preparation method of a rubber-state polymer blend membrane based on blending modification of an amphiphilic polymer, and relates to the technical field of polymer material membrane preparation. The invention comprises the following steps: and (3) doping PEDOT into the film matrix, and blending with PSS to obtain a blended film, namely a Pebax/PEDOT/PSS blended film. The permeation selectivity data of the blend membrane of the PEDOT and the PSS prepared by the method exceeds that of a single Pebax membrane, the separation performance of a single material is improved, and the gas permeability and selectivity of the blend membrane are improved by utilizing the special molecular structure of the PEDOT and the PSS.

Description

Preparation method of amphiphilic polymer blending modified rubbery polymer blending membrane
Technical Field
The invention belongs to the technical field, and particularly relates to a preparation method of a rubbery polymer blend membrane modified based on blending of amphiphilic polymers.
Background
Since the 21 st century, the severe climate change, the rise of sea level, global warming, frequent extreme weather and other ecological environment deterioration phenomena are caused by excessive deforestation of human beings, damage to vegetation, consumption of resources and fossil energy. CO 22Is the main gas causing greenhouse effect, mainly comes from the combustion of fossil fuel, so energy conservation and emission reduction are strived for all the world. Meanwhile, natural gas usually also contains a certain amount of CO2When acidic gases are used, the transportation cost is increased, the heat value is reduced, and CO is required to be removed2The product quality is improved, the corrosion of equipment and pipelines is reduced, and the transportation cost and the storage cost of the natural gas are reduced. In addition, CO2And is an important carbon resource, which is widely applied to various fields of bioengineering, fire fighting, carbonated beverage, refrigerant, medical treatment and health, high polymer material synthesis and the like. Thus, the pair of CO is realized2The efficient capture of (A) is a global efficient CO capture2The key steps of emission reduction, transformation and utilization technology relate to the living environment, energy structure and economic development of the whole human society. The membrane separation technology has the characteristics of high efficiency, low energy consumption, environmental protection and the like in CO2The separation field shows good development prospect, CO2The key of the membrane separation technology is CO2Separating membrane material, CO2The separation membrane material is a material having selective permeability to a substance; thus, the development of highly permeable and highly selective CO2The separation membrane material has important theoretical value and practical significance;
CO2separation membrane materials are generally classified into two major types, i.e., a polymer membrane as CO and an inorganic membrane2The separation membrane material has the following characteristics: good film forming property, thermal stability, permeability and flexibility, and low price of organic materials; thus, polymer membranes are a good choice, considering a single polymerThe membrane material has certain limitation on performance, higher benefit can be brought by modifying a single polymer membrane material, and the blending method has the characteristics of simplicity and easiness in operation, so that the blending membrane is one of common modification methods for polymer membrane materials, and is used for CO (carbon monoxide) blending2The main characteristic of the separation is that the additive can enhance the plasticity resistance of the membrane and can promote CO by adjusting the blending ratio of the additive2(ii) delivery within the membrane;
in recent years, with the development of researches on blended membranes by researchers, intensified CO is built in the membranes2The idea of facilitating transport has attracted the attention of researchers as an effective separation method, which is currently used for preparing blend membranes and can be used with CO2The additives of the small molecular substances which act are as follows: polyethylene glycol (PEG), Triethanolamine (TEA), amino acid salt, ionic liquid and other materials, but the materials bring CO to the rubbery polymer membrane2The separation performance is insufficient and still has certain limitations.
Disclosure of Invention
The invention aims to provide a preparation method of a rubbery polymer blend membrane modified based on blending of amphiphilic polymers, which solves the problem that CO brought by the existing application materials to the rubbery polymer membrane is solved2Insufficient separation performance, etc.
In order to solve the technical problems, the invention is realized by the following technical scheme:
a preparation method of a modified rubbery polymer blend membrane based on blending of amphiphilic polymers comprises the following steps: and (3) doping PEDOT (PSS) (poly (3, 4-ethylenedioxythiophene) -poly (styrenesulfonic acid)) into a film matrix, and blending to obtain a blended film.
Preferably, a preparation method of a membrane matrix and a blending method of a blended membrane based on the membrane matrix are included;
the membrane matrix is a polyamide-polyether block copolymer Pebax solution;
the preparation method of the blend membrane comprises the steps of firstly preparing a Pebax solution, and physically blending the prepared Pebax solution with a PEDOT/PSS aqueous solution.
The preparation method of the Pebax solution comprises the following steps:
step S01: weighing Pebax particles;
step S02: adding the weighed Pebax particles into an ethanol/30% water solution with the mass fraction of 70% to prepare a solution with the mass concentration of 6%, and then stirring at the temperature of 80 ℃ for 2 hours to completely dissolve the Pebax to obtain a Pebax solution;
the blending method of the blended film based on the film matrix is to physically blend the prepared Pebax solution and a PEDOT/PSS aqueous solution, wherein the weight ratio of the PEDOT: the mass fraction of the PSS is 1.4%, and the method comprises the following steps:
step S11: adding a PEDOT (Poly ethylene terephthalate) PSS aqueous solution into a Pebax solution, and stirring for 4 hours at room temperature until the mixture is uniformly mixed to obtain a casting solution;
step S12, pouring the casting solution on a clean super-flat dish for casting, and drying at 25 ℃ for 48 h;
step S13: and (3) putting the dried membrane casting solution into a vacuum oven at 40 ℃ to remove residual solvent, thus obtaining the blend membrane.
Preferably, the mass ratio of Pebax to PEDOT: PSS in the blended film is 1: 0.03 to 1: 0.09.
preferably, the thickness of the blend film is 100-120 μm.
The invention has the following beneficial effects:
the invention takes poly (3, 4-ethylenedioxythiophene) -poly (styrenesulfonic acid) (PEDOT: PSS) as an additive and takes polyamide-polyether block copolymer (Pebax) as a membrane matrix to prepare a blended membrane for separating CO2/CH4The mixed gas utilizes the special molecular structure of PEDOT and PSS in the blended film to construct high-speed CO in the film2Transfer channel, membrane-enhanced CO2Separation performance;
the permeation selectivity data of the blend membrane of the Pebax/PEDOT and PSS exceeds the permeation selectivity of a single Pebax membrane, the separation performance of a single material is improved, the gas permeability and the selectivity of the blend membrane are improved by utilizing the special molecular structure of the PEDOT and PSS, and the performance of the blend membrane is effectively improved.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a cross-sectional view of a scanning electron microscope of a blended film of Pebax/PEDOT and PSS-3 prepared in example 1;
FIG. 2 is a cross-sectional view of a scanning electron microscope of the blended film of Pebax/PEDOT and PSS-5 prepared in example 2;
FIG. 3 is a cross-sectional view of a scanning electron microscope of the blended film of Pebax/PEDOT: PSS-7 prepared in example 3;
FIG. 4 is a cross-sectional view of a scanning electron microscope of the blended film of Pebax/PEDOT: PSS-9 prepared in example 4;
FIG. 5 is a cross-sectional view of a Pebax film obtained in the comparative example, taken by scanning electron microscopy.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A preparation method of a modified rubbery polymer blend membrane based on blending of amphiphilic polymers comprises the following steps: and (3) doping PEDOT (PSS) (poly (3, 4-ethylenedioxythiophene) -poly (styrenesulfonic acid)) into a film matrix, and blending to obtain a blended film.
The preparation method comprises a preparation method of a membrane matrix and a blending method of a blended membrane based on the membrane matrix;
the film matrix is a polyamide-polyether block copolymer Pebax solution;
the preparation method of the blend membrane comprises the steps of firstly preparing a Pebax solution, and physically blending the prepared Pebax solution with a PEDOT (Poly ethylene glycol Ether-Co-monomer) PSS (PolyEthyl Ether-Ether
The preparation method of the Pebax solution comprises the following steps:
step S01: weighing Pebax particles;
step S02: adding the weighed Pebax particles into an ethanol/30% water solution with the mass fraction of 70% to prepare a solution with the mass concentration of 6%, and then stirring at the temperature of 80 ℃ for 2 hours to completely dissolve the Pebax to obtain a Pebax solution;
the blending method of the blended film based on the film matrix comprises the step of physically blending the prepared Pebax solution with a PEDOT/PSS aqueous solution, wherein the weight ratio of the PEDOT: the mass fraction of the PSS is 1.4%, and the method comprises the following steps:
step S11: adding a PEDOT (Poly ethylene terephthalate) PSS aqueous solution into a Pebax solution, and stirring for 4 hours at room temperature until the mixture is uniformly mixed to obtain a casting solution;
step S12, pouring the casting solution on a clean super-flat dish for casting, and drying at 25 ℃ for 48 h;
step S13: and (3) putting the dried membrane casting solution into a vacuum oven at 40 ℃ to remove residual solvent, thus obtaining the blend membrane.
Wherein the mass ratio of Pebax to PEDOT to PSS in the blended film is 1: 0.03 to 1: 0.09.
wherein the thickness of the blend film is 100-120 μm.
Wherein the Pebax/PEDOT/PSS blended membrane is used for separating CO under wet condition2/CH4Mixed gas of CO2Flux 276 + 440Barrer (1 Barrer-10)-10cm3cm/cm2s cmHg)，CO2/CH4The selectivity is 24-28.
Example 1:
preparing a Pebax/PEDOT: PSS-3 blended film, wherein the thickness of the blended film is 100 mu m, the Pebax is used as a film substrate of the blended film, and the PEDOT: PSS is added into the film substrate, wherein the mass ratio of the Pebax to the PEDOT: PSS is 1: 0.03, the preparation method of the blend film comprises the following steps:
step 1, weighing 0.54g of Pebax, dissolving the Pebax into 70% ethanol/30% water solution by mass fraction, stirring the mixture for 2 hours at 80 ℃ to completely dissolve Pebax particles, and preparing to obtain a Pebax solution with the mass fraction of 6% for later use.
And 2, weighing 0.0162g of PEDOT: PSS, adding the weighed PEDBAX solution with the mass fraction of 6% prepared in the step 1, stirring the solution for 4 hours at room temperature, pouring the obtained casting solution on a clean super-flat dish for casting, drying the casting solution for 48 hours at 25 ℃, and then putting the casting solution into a vacuum oven at 40 ℃ to remove residual solvent to obtain a blended film of the PEDBAX/PEDOT: PSS-3, so as to obtain the blended film with the thickness of 100 mu m.
FIG. 1 is a cross-sectional view of a scanning electron microscope of a film of Pebax/PEDOT: PSS-3 prepared in this example.
The blend film of Pebax/PEDOT and PSS-3 is used for CO under wet condition at 25 ℃ and 2bar220% by volume of CO2/CH4Mixed gas separation test of CO2Flux 314Barrer, CO2/CH4The selectivity was 26.
Example 2:
a blend film of Pebax/PEDOT: PSS-5 was prepared, as opposed to the blend film of Pebax/PEDOT: PSS-3 of example 1: the thickness of the film is 105 μm, wherein the mass ratio of Pebax to PEDOT: PSS is 1: 0.05, the preparation of this blend film differs from the preparation of example 1 only in that: in the step 2, 0.0162g of PEDOT to PSS is changed into 0.027g of PEDOT to PSS; finally, a blended film having a thickness of 105 μm was obtained.
FIG. 2 is a cross-sectional view of a scanning electron microscope of a film of Pebax/PEDOT: PSS-5 prepared in this example.
The blend film of Pebax/PEDOT PSS-5 obtained in example 2 was used in wet CO conditions at 25 ℃ and 2bar220% by volume of CO2/CH4Mixed gas separation test of CO2Flux 393Barrer, CO2/CH4The selectivity was 28.
Example 3:
preparation of Pebax/PEDOT PSS-7 blend film, in contrast to the blend film of example 1: the thickness of the film is 120 μm, wherein the mass ratio of Pebax to PEDOT: PSS is 1: 0.07, the preparation of this blend film differs from the preparation method of example 1 only in that: in the step 2, 0.0162g of PEDOT and PSS are changed into 0.0378g of PEDOT and PSS; finally, a blended film having a thickness of 120 μm was obtained.
FIG. 3 is a cross-sectional view of a scanning electron microscope of a film of Pebax/PEDOT: PSS-7 prepared in this example.
The blend film of Pebax/PEDOT: PSS-7 obtained in example 3 was used in wet CO conditions at 25 ℃ and 2bar220% by volume of CO2/CH4Mixed gas separation test of CO2Flux 440Barrer, CO2/CH4The selectivity was 28.
Example 4:
preparation of Pebax/PEDOT PSS-9 blend film, in contrast to the blend film of example 1: the thickness of the film is 114 μm, wherein the mass ratio of Pebax to PEDOT: PSS is 1: 0.09, the preparation of this blend film differs from the preparation of example 1 only in that: in the step 2, changing the weighing of 0.0162g of PEDOT to PSS into the weighing of 0.0486g of PEDOT to PSS; finally, a blended film having a thickness of 114 μm was obtained.
FIG. 4 is a cross-sectional view of a scanning electron microscope of a film of Pebax/PEDOT: PSS-9 prepared in this example.
The blend film of Pebax/PEDOT PSS-9 from example 4 was used in wet CO conditions at 25 ℃ and 2bar220% by volume of CO2/CH4Mixed gas separation test of CO2Flux of 406Barrer, CO2/CH4The selectivity was 28.
Comparative example:
preparing a Pebax film with the film thickness of 110 mu m; the preparation method comprises the following steps: 0.54g of Pebax particles are weighed and dissolved in 70% ethanol/30% aqueous solution by mass fraction, the mixture is stirred at 80 ℃ for 2 hours, the obtained casting solution is poured on a clean super-flat dish for casting, the casting solution is dried at room temperature for 48 hours, and then the casting solution is placed in a vacuum oven at 40 ℃ for 24 hours to remove residual solvent, so that a Pebax film with the thickness of 110 microns is obtained.
FIG. 5 is a cross-sectional view of a pure Pebax film prepared in this comparative example under a scanning electron microscope.
The Pebax membrane prepared in the comparative example was used for CO in the wet state at 25 ℃ under 2bar220% by volume of CO2/CH4Mixed gas separation test of CO2Flux 276Barrer, CO2/CH4The selectivity was 24.
The invention selects an organic material of poly (3, 4-ethylenedioxythiophene) -poly (styrenesulfonic acid) as an additive to be doped into a rubbery polymer film (polyamide-polyether block copolymer) for physical blending modification, and through the interaction of the two materials, better CO is brought to the rubbery polymer film2The separation performance was that poly (3, 4-ethylenedioxythiophene) -poly (styrenesulfonic acid) (PEDOT: PSS) was an aqueous solution of a high molecular polymer with a content of 1.4%, wherein PEDOT was a hydrophobic polymer, PSS was a hydrophilic polymer, and the hydrophilic group promoted CO2Adsorption, hydrophobic group promoting CO2Desorption, and the amphiphilic groups jointly construct high-speed CO2A delivery channel. Water in CO2The PSS contains abundant hydrophilic group sulfonic groups, can effectively adjust the water content in the membrane, and further improves the CO content of the membrane2Permeability of (2). And hydrated proton ions generated from sulfonic acid groups in the polymer can be used as CO2The selective transmission channel can promote the CO-mixed membrane to react with the CO2Selective delivery of (a). Therefore, the blend film is prepared by blending and modifying the rubbery high molecular material based on the PEDOT-PSS polymer, and the amphiphilic group in the blend film is used for CO2Strengthening CO in the blended film2Separation performance.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims (4)

1. A preparation method of a modified rubbery polymer blend membrane based on blending of an amphiphilic polymer is characterized by comprising the following steps: and (3) doping PEDOT into the film matrix, and blending PSS to obtain the blended film.
2. The preparation method of the amphiphilic polymer blending modified rubbery polymer blend membrane according to claim 1, wherein: a blending method comprising a preparation method of a membrane substrate and a blended membrane based on the membrane substrate;
the membrane matrix is a polyamide-polyether block copolymer Pebax solution;
the preparation method of the blend membrane comprises the steps of firstly preparing a Pebax solution, and physically blending the prepared Pebax solution with a PEDOT/PSS aqueous solution.
The preparation method of the Pebax solution comprises the following steps:
step S01: weighing Pebax particles;
step S02: adding the weighed Pebax particles into an ethanol/30% water solution with the mass fraction of 70% to prepare a solution with the mass concentration of 6%, and then stirring at the temperature of 80 ℃ for 2 hours to completely dissolve the Pebax to obtain a Pebax solution;
the blending method of the blended film based on the film matrix is to physically blend the prepared Pebax solution and a PEDOT/PSS aqueous solution, wherein the weight ratio of the PEDOT: the mass fraction of the PSS is 1.4%, and the method comprises the following steps:
step S11: adding a PEDOT (Poly ethylene terephthalate) PSS aqueous solution into a Pebax solution, and stirring for 4 hours at room temperature until the mixture is uniformly mixed to obtain a casting solution;
step S12, pouring the casting solution on a clean super-flat dish for casting, and drying at 25 ℃ for 48 h;
step S13: and (3) putting the dried membrane casting solution into a vacuum oven at 40 ℃ to remove residual solvent, thus obtaining the blend membrane.
3. The preparation method of the amphiphilic polymer blending modified rubbery polymer blending film according to claim 2, wherein: the mass ratio of Pebax to PEDOT to PSS in the blended film is 1: 0.03 to 1: 0.09.
4. the preparation method of the amphiphilic polymer blending modified rubbery polymer blending film according to claim 3, wherein: the thickness of the blend film is 100-120 μm.
CN202110142602.0A 2021-02-02 2021-02-02 Preparation method of amphiphilic polymer blending modified rubbery polymer blending membrane Pending CN112915821A (en)

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Application publication date: 20210608