CN112619434A - Preparation and application of polyether amine blending modified rubbery polymer blending membrane - Google Patents
Preparation and application of polyether amine blending modified rubbery polymer blending membrane Download PDFInfo
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- CN112619434A CN112619434A CN202011389620.0A CN202011389620A CN112619434A CN 112619434 A CN112619434 A CN 112619434A CN 202011389620 A CN202011389620 A CN 202011389620A CN 112619434 A CN112619434 A CN 112619434A
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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
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- 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
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- 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
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- 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
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- 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
Abstract
The invention discloses preparation and application of a polyether amine blending modified rubbery polymer blending membrane, and relates to the technical field of polymer material membrane preparation. The invention comprises polyether amine (PEA, molecular weight 400) and a blend membrane, wherein the blend membrane is added into the PEA, the blend membrane takes a polyamide-polyether block copolymer Pebax as a membrane matrix, and the PEA is doped into the membrane matrix. The permeation selectivity data of the Pebax/PEA blended membrane prepared by the method exceeds the permeation selectivity of a single Pebax membrane, and the separation performance of a single material is improved, so that the method for improving the gas permeability and the selectivity of the membrane by utilizing the special molecular structure of PEA is an effective method for improving the performance of the blended membrane.
Description
Technical Field
The invention belongs to the technical field of preparation of high polymer material films, and particularly relates to preparation and application of a polyether amine blending modified rubbery high polymer blending film.
Background
The biological methane is taken as an important renewable clean energy at the present stage, the use of the biological methane is popularized, the effort value of non-renewable natural gas can be effectively increased, and the environmental problem brought by biological waste is relieved; however, newly collected biogas usually contains acidic impurity gases such as CO2, and the like, and the acidic impurity gas of CO2 not only affects the calorific value and quality of methane and blocks the pipeline, but also seriously corrodes the pipeline and equipment, so before the biogas is used, the acidic impurity gas of CO2 must be removed, therefore, the separation of CO2 becomes a necessary and critical industrial process, the high-efficiency, low-energy consumption and environment-friendly CO2 separation technology is the key to solve the problem of biogas gas purification, the membrane separation technology has the characteristics of high efficiency, low energy consumption, environmental protection and the like, and has good development prospects in the field of CO2 separation, the key of the CO2 separation technology is a CO2 separation membrane material, and the CO2 separation membrane material is a material having selective permeability to substances; therefore, the development of the CO2 separation membrane material with high permeability and high selectivity has important theoretical value and practical significance;
the CO2 separation membrane material is generally divided into two categories, namely a polymer membrane and an inorganic membrane, and the polymer membrane as the CO2 separation membrane material has the following characteristics: good film forming property, thermal stability, permeability and flexibility, and low price of organic materials; therefore, the polymer membrane is a good selection object, the single polymer membrane material has certain limitation on performance, higher benefit can be brought by modifying the single polymer membrane material, and the blending method has the characteristics of simplicity and easiness in operation, so that the polymer membrane material is one of common modification methods for the polymer membrane material, and the blending membrane has the main characteristic of phase shape for separating CO2, can enhance the plasticity resistance of the membrane, and can promote the transmission of CO2 in the membrane by adjusting the blending ratio of the additive;
in recent years, with the development of research on blend membranes by researchers, the idea of enhancing the transfer promoting effect of CO2 in membranes has attracted attention as an effective separation method, and the additives of small-molecule substances which are used for preparing blend membranes and can react with CO2 are: polyethylene glycol (PEG), Triethanolamine (TEA), amino acid salt, ionic liquid and other materials, but the materials have insufficient CO2 separation performance brought by a rubbery polymer membrane and still have certain limitations.
Disclosure of Invention
The invention aims to provide preparation of a polyether amine blending modified rubbery polymer blending membrane, and solves the problems of insufficient CO2 separation performance and the like of the existing application materials on the rubbery polymer membrane.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention relates to a preparation method of a polyether amine blending modified rubbery polymer blending membrane, which comprises polyether amine (PEA, molecular weight 400) and a blending membrane, wherein the blending membrane is added into the PEA, the blending membrane takes a polyamide-polyether block copolymer Pebax as a membrane matrix, and the PEA is doped into the membrane matrix;
preferably, the method comprises the steps of preparing a Pebax solution and physically blending the prepared Pebax solution with the existing PEA;
the preparation method of the Pebax solution comprises the following steps:
step 1: weighing a certain amount of Pebax particles;
step 2: adding the Pebax particles weighed in the step into 70% ethanol/30% water solution by mass fraction to prepare 4% solution by mass concentration, and then stirring at 80 ℃ for 2 hours to completely dissolve the Pebax to obtain Pebax solution;
the preparation method of the PEA additive blend membrane comprises the following steps:
step 1: adding a certain amount of PEA into the prepared Pebax solution, and stirring for 3 hours at room temperature until the additive is uniformly mixed in the solution to obtain a casting solution;
and step 3: and (3) putting the dried membrane casting solution into a vacuum oven at 40 ℃ to remove residual solvent, thus obtaining the Pebax/PEA blended membrane.
Preferably, the mass ratio of Pebax to PEA is 1: 0.01-0.04.
Preferably, the thickness of the blend film is 40 to 90 μm.
Preferably, the Pebax/PEA blend membrane is used for CO2 and CH4 mixed gas permeability tests, the CO2 flux of the membrane is 128-195Barrer (1Barrer is 10-10cm3 cm/cm2 s cmHg), and the CO2/CH4 selectivity is 20-23.
The invention has the following beneficial effects:
in the method, polyether amine (PEA) is used as an additive, a polyamide-polyether block copolymer (Pebax) is used as a membrane substrate to prepare a blend membrane for separating CO2/CH4 mixed gas, and a high-speed CO2 transfer channel is constructed in the blend membrane by utilizing the special molecular structure of the PEA in the blend membrane, so that the CO2 separation performance of the membrane is enhanced;
the Pebax/PEA blend membrane is used for CO2 and CH4 permeability tests, the CO2 flux of the blend membrane is 128-substituted 195Barrer (1Barrer is 10-10cm3 cm/cm2 s cmHg), and the CO2/CH4 selectivity is 20-23;
the permeation selectivity data of the Pebax/PEA blended membrane exceeds the permeation selectivity of a single Pebax membrane, and the separation performance of a single material is improved, so that the method for improving the gas permeability and selectivity of the membrane by utilizing the special molecular structure of PEA is an effective method for improving the performance of the blended membrane.
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
FIG. 1 is a cross-sectional view of a scanning electron microscope of the Pebax/PEA-1 blend film prepared in example 1;
FIG. 2 is a cross-sectional view of a scanning electron microscope of the Pebax/PEA-2 blend film prepared in example 2;
FIG. 3 is a cross-sectional view of a scanning electron microscope of the Pebax/PEA-3 blend film prepared in example 3;
FIG. 4 is a cross-sectional view of a scanning electron microscope of the Pebax/PEA-4 blend film prepared in example 4;
fig. 5 is a cross-sectional view of a Pebax film prepared in the comparative example under a scanning electron microscope.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
The invention relates to a preparation method of a polyether amine blending modified rubbery polymer blending film, which comprises polyether amine (PEA, molecular weight 400) and a blending film, wherein the blending film is added into the PEA, the blending film takes polyamide-polyether block copolymer Pebax as a film matrix, and the PEA is doped into the film matrix.
Further, the method comprises the steps of preparing a Pebax solution, and physically blending the prepared Pebax solution with the existing PEA;
the preparation method of the Pebax solution comprises the following steps:
step 1: weighing a certain amount of Pebax particles;
step 2: adding the Pebax particles weighed in the step into 70% ethanol/30% water solution by mass fraction to prepare 4% solution by mass concentration, and then stirring at 80 ℃ for 2 hours to completely dissolve the Pebax to obtain Pebax solution;
the preparation method of the PEA addition blending film comprises the following steps:
step 1: adding a certain amount of PEA into the prepared Pebax solution, and stirring for 3 hours at room temperature until the additive is uniformly mixed in the solution to obtain a casting solution;
and step 3: and (3) putting the dried membrane casting solution into a vacuum oven at 40 ℃ to remove residual solvent, thus obtaining the Pebax/PEA blended membrane.
Further, the mass ratio of Pebax to PEA is 1: 0.01-0.04.
Further, the thickness of the blend film is 40 to 90 μm.
Further, the Pebax/PEA blend membrane is used for CO2 and CH4 mixed gas permeability tests, the CO2 flux of the blend membrane is 128-195Barrer (1Barrer is 10-10cm3 cm/cm2 s cmHg), and the selectivity of CO2/CH4 is 20-23.
Example 1:
preparing a Pebax/PEA-1 blended film with the thickness of 50 μm, wherein the Pebax is used as a film matrix, and PEA is added into the film matrix, wherein the mass ratio of the Pebax to the PEA 400 is 1: 0.01, the preparation method of the blend film comprises the following steps:
And 2, weighing 0.0035g of PEA, adding the PEA into the Pebax solution with the mass fraction of 4% prepared in the step 1, stirring for 3 hours at room temperature, pouring the obtained casting solution on a clean super-flat dish for casting, drying for 48 hours at 25 ℃, then putting the casting solution into a vacuum oven at 40 ℃ to remove residual solvent, thus obtaining a Pebax/PEA-1 blend membrane, and obtaining the blend membrane with the thickness of 50 mu m.
FIG. 1 is a cross-sectional view of a scanning electron microscope of the Pebax/PEA-1 film obtained in example 1.
The Pebax/PEA-1 blend membrane is used for CO2 and CH4 mixed gas permeability tests under the conditions of 25 ℃ and 2bar, the CO2 flux is 128 Barrer, and the CO2/CH4 selectivity is 20.
Example 2:
a Pebax/PEA-2 blend membrane was prepared, differing from the Pebax/PEA-1 blend membrane of example 1 by: the thickness of the film is 60 μm, wherein the mass ratio of Pebax to PEA is 1: 0.02, the preparation of this blend film differs from the preparation of example 1 only in that: in the step 2, 0.0035g of PEA is changed into 0.007g of PEA; finally, a blended film having a thickness of 60 μm was obtained.
FIG. 2 is a cross-sectional view of a scanning electron microscope of the Pebax/PEA-2 film obtained in example 2.
The Pebax/PEA-2 blend membrane prepared in example 2 is used for CO2 and CH4 mixed gas permeability test under the conditions of 25 ℃ and 2bar, the CO2 flux is 142 Barrer, and the CO2/CH4 selectivity is 22.
Example 3:
a Pebax/PEA-3 blend film was prepared, differing from the blend film of example 1: the thickness of the film is 80 μm, wherein the mass ratio of Pebax to PEA is 1: 0.03 preparation of the blend film with example 1
The preparation method of (a) differs only in that: in the step 2, the PEA weighing 0.0035g is changed into the PEA weighing 0.0105 g; finally, a blended film having a thickness of 80 μm was obtained.
FIG. 3 is a cross-sectional view of a scanning electron microscope of the Pebax/PEA-3 film obtained in example 3.
The Pebax/PEA-3 blend membrane prepared in example 3 was used for CO2 and CH4 mixed gas permeability test at 25 ℃ and 2bar, and the CO2 flux was 195Barrer and the CO2/CH4 selectivity was 23.
Example 4:
a Pebax/PEA-4 blend film was prepared, differing from the blend film of example 1: the thickness of the film is 90 μm, wherein the mass ratio of Pebax to PEA is 1: 0.04, the preparation of this blend film differs from the preparation of example 1 only in that: in step 2, the weight of 0.0035g of PEA is changed into the weight of 0.014g of PEA; finally, a blended film having a thickness of 90 μm was obtained.
FIG. 4 is a cross-sectional view of a scanning electron microscope of the Pebax/PEA-4 film obtained in example 4.
The Pebax/PEA-4 blend membrane prepared in example 4 is used for CO2 and CH4 mixed gas permeability test at 25 ℃ and 2bar, and has the CO2 flux of 183 Barrer and the CO2/CH4 selectivity of 22.
Comparative example:
preparing a Pebax film with the film thickness of 40 mu m; the preparation method comprises the following steps: 0.35g 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 40 microns is obtained.
FIG. 5 is a cross-sectional view of a pure Pebax film prepared in the comparative example under a scanning electron microscope.
The Pebax membrane prepared in the comparative example is used for the permeability test of CO2 and CH4 mixed gas at 25 ℃ and 2bar, the CO2 flux is 80Barrer, and the selectivity of CO2/CH4 is 18.
The scheme of the patent selects an organic material of polyether amine as an additive to be doped into a rubber polymer film (polyamide-polyether block copolymer) for physical blending modification, and brings better CO2 separation performance for the rubber polymer film through the interaction of the two materials, wherein the polyether amine (PEA) is a polymer with a polyether structure as a main chain and an amino group as a terminal active functional group; wherein, the amino group is used as a fixed carrier of CO2, interacts with CO2 in the membrane to form a compound and HCO 3-easy to diffuse, promotes the transfer of CO2 in the membrane, and enhances the separation performance of CO 2; the ether oxygen unit is a CO2 affinity group, and can preferentially select CO2 to generate dipole quadrupole effect with the CO2 affinity group, so that the selectivity and the permeability of CO2 are enhanced, therefore, the invention prepares the blending membrane based on polyether amine blending modified rubbery high molecular material, and enhances the CO2 separation performance in the blending membrane through the special effect of the amine carrier and the ether oxygen unit in the blending membrane on CO 2.
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 (5)
1. The preparation method of the polyether amine blending modified rubbery polymer blending film comprises the following steps of preparing polyether amine (PEA, molecular weight 400) and a blending film, and is characterized in that: adding a blend film to PEA, wherein the blend film takes a polyamide-polyether block copolymer Pebax as a film matrix, and PEA is doped in the film matrix.
2. The preparation method of the polyether amine blending modified rubbery polymer blending film according to claim 1, wherein the polyether amine blending modified rubbery polymer blending film comprises the following steps: the method comprises the steps of preparing a Pebax solution, and physically blending the prepared Pebax solution with the existing PEA;
the preparation method of the Pebax solution comprises the following steps:
step 1: weighing a certain amount of Pebax particles;
step 2: adding the Pebax particles weighed in the step into an ethanol/30% aqueous solution with the mass fraction of 70% to prepare a solution with the mass concentration of 4%, and then stirring at 80 ℃ for 2 hours to completely dissolve the Pebax to obtain a Pebax solution;
the preparation method of the PEA additive blend membrane comprises the following steps:
step 1: adding a certain amount of PEA into the prepared Pebax solution, and stirring for 3 hours at room temperature until the additive is uniformly mixed in the solution to obtain a casting solution;
step 2, pouring the casting solution obtained in the step on a clean super-flat surface dish for casting, and drying at 25 ℃ for 48 hours;
and step 3: and (3) putting the dried membrane casting solution into a vacuum oven with the temperature of 40 ℃ to remove residual solvent, thus obtaining the Pebax/PEA blend membrane.
3. The preparation method of the polyether amine blending modified rubbery polymer blending membrane as claimed in claim 2, wherein the mass ratio of Pebax to PEA is 1: 0.01-0.04.
4. The preparation method of the polyether amine blending modified rubbery polymer blending film as claimed in claim 3, wherein the thickness of the blending film is 40-90 μm.
5. The preparation method of the polyether amine blended and modified rubbery polymer blend membrane as claimed in claim 4, wherein said Pebax/PEA blend membrane is used for CO2, CH4 mixed gas permeability test, and has CO2 flux of 128-195Barrer (1Barrer = 10-10cm3 cm/cm2 s cmHg) and CO2/CH4 selectivity of 20-23.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
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| CN202011389620.0A CN112619434A (en) | 2020-12-02 | 2020-12-02 | Preparation and application of polyether amine blending modified rubbery polymer blending membrane |
| ZA2021/08736A ZA202108736B (en) | 2020-12-02 | 2021-11-08 | Method for preparing rubbery polymer blend membrane modified by polyetheramine blending and application thereof |
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| CN202011389620.0A CN112619434A (en) | 2020-12-02 | 2020-12-02 | Preparation and application of polyether amine blending modified rubbery polymer blending membrane |
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| ZA202108736B (en) | 2022-02-23 |
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Application publication date: 20210409 |