CN113019141B - Preparation method of monovalent selective cation exchange membrane with charge Janus structure - Google Patents
Preparation method of monovalent selective cation exchange membrane with charge Janus structure Download PDFInfo
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- CN113019141B CN113019141B CN202110363180.XA CN202110363180A CN113019141B CN 113019141 B CN113019141 B CN 113019141B CN 202110363180 A CN202110363180 A CN 202110363180A CN 113019141 B CN113019141 B CN 113019141B
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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
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0093—Chemical modification
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/14—Membrane materials having negatively charged functional groups
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/16—Membrane materials having positively charged functional groups
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/42—Ion-exchange membranes
Abstract
The invention discloses a preparation method of a monovalent selective cation exchange membrane with a charge Janus structure, which comprises the following steps: firstly, soaking a base material to swell the base material; fixing the swelled base material and spreading the surface of the base material flatly; thirdly, immersing the coating liquid 1 into the substrate to carry out surface treatment on the substrate; fourthly, removing the coating liquid 1 and drying the surface of the membrane until the membrane is clean and dry; fifthly, immersing the coating liquid 2 into the substrate to carry out surface treatment on the substrate; sixthly, removing the coating liquid 2 and drying the surface of the membrane by blowing till the membrane is clean and dry; and seventhly, placing the six dried membranes in an oven for heat treatment to obtain the monovalent selective cation exchange membrane with the charge Janus structure. The invention constructs the surface selection layer with positive charges on the surface of the cation exchange membrane with sulfonic acid groups by utilizing the interface reaction, thereby realizing the Na-ion exchange of the surface selection layer + /Mg 2+ With Li + /Mg 2+ The Li/Mg separation coefficient higher than that of the commercial film is suitable for extracting lithium from salt lake water.
Description
Technical Field
The invention relates to a preparation method of a monovalent selective cation exchange membrane with a charge Janus structure.
Background
The membrane separation method has the advantages of small occupied area, good stability, easiness in operation, greenness, no pollution, low energy consumption and the like, and has huge development potential and good application background. Ion exchange membranes play an important role in the fields of electrodialysis, reverse electrodialysis, redox flow batteries, and the like. However, for some specific fields, such as redox flow batteries, production of edible salts, extraction of lithium ions, etc., the common cation exchange membranes cannot meet the application requirements. Therefore, the preparation and application of monovalent selective cation exchange membranes with higher ion permselectivity are the focus of current research. It is worth noting that the screening principle of the current monovalent selective ion exchange membrane is mainly the size screening effect and the donnan effect. In one aspect, a surface selective layer with smaller pore sizes may be used to separate the larger radius hydrated ions. On the other hand, monovalent and multivalent ions can be separated by the donnan effect after the surface selective layer with opposite charges is constructed. At present, common membrane surface modification methods mainly comprise layer-by-layer self-assembly, surface grafting and interfacial polymerization. Although these methods can improve the permselectivity of ions, they inevitably cause problems such as an increase in the membrane surface resistance and a decrease in the current efficiency.
On one hand, the monovalent selective cation exchange membrane with the charge Janus structure can overcome the problem of current efficiency reduction caused by anion leakage existing in the porous ion exchange membrane; on the other hand, the membrane surface resistance of the monovalent selective cation exchange membrane with the charge Janus structure is only slightly increased due to the fact that the selection layer is thin, and therefore high current efficiency can be guaranteed while energy consumption is reduced. The construction of a positively charged selection layer on the surface of a negatively charged basement membrane is a common method for preparing a monovalent selective cation exchange membrane with a charge Janus structure, but the practical application of materials commonly used for constructing a positively charged selection layer, such as polypyrrole and polyaniline, is limited due to the high cost. In addition, the surface of the cation exchange membrane is coated with polyethyleneimine with highly branched polyamino groups, so that the osmotic selectivity can be remarkably improved, the monovalent selective cation exchange membrane with the positively charged selective layer can be widely applied in the fields of environmental remediation, energy enrichment and the like, and the stability of the constructed selective layer needs to be further improved.
Disclosure of Invention
The invention aims to provide a preparation method of a monovalent selective cation exchange membrane with a charge Janus structure, which is characterized in that the interface reaction of an amino-containing substance and a cross-linking agent is utilized on the surface of the cation exchange membrane with a sulfonic group, the high cross-linking degree of the amino-containing substance and the cross-linking agent and the electrostatic interaction between the amino-containing substance and a base membrane are utilized to improve the stability of the membrane, and finally, the monovalent selective cation exchange membrane with the charge Janus structure with excellent performance and good stability is obtained and is used for the fields of environmental remediation, energy enrichment and the like.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a monovalent selective cation exchange membrane with a charge Janus structure comprises the following steps of placing a substrate with negative electricity in a plate frame, and forming a selection layer with positive charge on one side of the substrate, so that the Janus monovalent selective cation exchange membrane with different charge properties on two sides is prepared, wherein the preparation method specifically comprises the following steps:
soaking a base material to swell the base material, wherein the base material is a cation exchange membrane with a sulfonic group;
fixing the swelled base material and spreading the surface of the base material flatly;
step three, immersing the coating liquid 1 into a substrate to perform surface treatment on the substrate, wherein:
the coating liquid 1 contains surfactant molecules and a cross-linking agent;
the surfactant is sodium dodecyl benzene sulfonate or sodium dodecyl sulfate, and the concentration is 0.1-0.3 wt.%;
the cross-linking agent is 1,3, 5-benzene tricarboxylic acid or polyphenols such as tannic acid and dopamine, and the concentration is 0.05-0.5 wt.%;
the surface treatment time is 1-10 min;
step four, removing the coating liquid 1 and drying the surface of the membrane until the membrane is clean and dry;
step five, immersing the coating liquid 2 into the substrate to perform surface treatment on the substrate, wherein:
the coating liquid 2 contains amino substances;
the amino substances are polyethyleneimine, triethylene tetramine or tetraethylene pentamine and the like, and the concentration is 0.1-2 wt.%;
the surface treatment time is 1-10 min;
sixthly, removing the coating liquid 2 and drying the surface of the membrane until the membrane is clean and dry;
and step seven, placing the membrane dried in the step six into an oven for heat treatment to obtain the monovalent selective cation exchange membrane with the charge Janus structure, wherein:
the heat treatment temperature is 50-120 ℃, and the heat treatment time is 5-30 min.
Compared with the prior art, the invention has the following advantages:
1. the Janus monovalent selective cation exchange membrane prepared by the invention has different charge properties on two sides, and the difference of the charge properties on the two sides of the membrane is realized by forming a positively charged selection layer on one side of a negatively charged base membrane through an interface reaction.
2. The invention constructs the surface selection layer with positive charges on the surface of the cation exchange membrane with sulfonic acid groups by utilizing the interface reaction, thereby realizing the Na-ion exchange of the surface selection layer + /Mg 2+ With Li + /Mg 2+ The Li/Mg separation coefficient higher than that of the commercial membrane can be suitable for extracting lithium from salt lake water.
3. The method for preparing the monovalent selective cation exchange membrane with the charge Janus structure does not need special equipment, and is simple and easy to operate.
Drawings
FIG. 1 is a process for preparing a monovalent selective cation exchange membrane having a charged Janus structure;
FIG. 2 is a digital photograph of a plate frame mold during film preparation;
FIG. 3 shows Li in example 1 + /Mg 2+ Separating the experimental results of the pilot experiment;
FIG. 4 shows Na in example 1 + /Mg 2+ Experimental results of the system separation stability experiment.
Detailed Description
The technical solutions of the present invention are further described below with reference to the following examples, but the present invention is not limited thereto, and any modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Example 1:
the embodiment provides a preparation method of a monovalent selective cation exchange membrane with a charge Janus structure, which comprises the following steps:
soaking a base material to swell the base material, wherein the base material is a sulfonated polypropylene film;
fixing the swelled base material and spreading the surface of the base material flatly by using a plate frame mold;
step three, immersing the substrate in a coating solution 1 containing 0.15 wt.% of sodium dodecyl benzene sulfonate and 0.10 wt.% of 1,3, 5-benzene tricarboxylic acid for 5min for surface treatment;
step four, removing the coating liquid 1 and drying the surface of the membrane until the membrane is clean and dry;
step five, immersing the base material in the coating liquid 2 containing 0.8wt.% of polyethyleneimine for surface treatment for 2 min;
sixthly, removing the coating liquid 2 and drying the surface of the membrane until the membrane is clean and dry;
step seven, placing the membrane dried in the step six in an oven to carry out heat treatment for 10min at the temperature of 90 ℃;
and step eight, removing the plate frame mould from the film after heat treatment and storing the film in deionized water.
As can be seen from FIG. 3, the monovalent selective cation exchange membrane with charge Janus structure prepared in the example significantly reduces Mg 2+ And improves Li + /Mg 2+ Permselectivity of (a).
As can be seen from FIG. 4, the monovalent selective cation exchange membrane with charge Janus structure prepared in this example has the effect of Na + /Mg 2+ The system has high separation selectivity and operation stability.
Example 2:
the embodiment provides a preparation method of a monovalent selective cation exchange membrane with a charge Janus structure, which comprises the following steps:
soaking a base material to swell the base material, wherein the base material is a sulfonated polypropylene film;
fixing the swelled base material and spreading the surface of the base material flatly by using a plate frame mold;
immersing the substrate in a coating solution 1 containing 0.15 wt.% of sodium dodecyl benzene sulfonate and 0.10 wt.% of 1,3, 5-benzene tricarboxylic acid to perform surface treatment on the substrate for 5 min;
step four, removing the coating liquid 1 and drying the surface of the membrane until the membrane is clean and dry;
step five, immersing the base material in the coating liquid 2 containing 0.6wt.% of polyethyleneimine for surface treatment for 2 min;
sixthly, removing the coating liquid 2 and drying the surface of the membrane until the membrane is clean and dry;
step seven, placing the membrane dried in the step six in an oven to carry out heat treatment for 10min at the temperature of 90 ℃;
and step eight, removing the plate frame mould from the film after heat treatment and storing the film in deionized water.
Example 3:
the embodiment provides a preparation method of a monovalent selective cation exchange membrane with a charge Janus structure, which comprises the following steps:
soaking a base material to swell the base material, wherein the base material is a sulfonated polypropylene film;
fixing the swelled base material and spreading the surface of the base material flatly by using a plate frame mold;
immersing the substrate in a coating solution 1 containing 0.15 wt.% of sodium dodecyl benzene sulfonate and 0.2 wt.% of 1,3, 5-benzene tricarboxylic acid for 5min for surface treatment;
step four, removing the coating liquid 1 and drying the surface of the membrane until the membrane is clean and dry;
step five, immersing the base material in the coating liquid 2 containing 0.6wt.% of polyethyleneimine for surface treatment for 2 min;
sixthly, removing the coating liquid 2 and drying the surface of the membrane until the membrane is clean and dry;
step seven, placing the membrane dried in the step six in an oven to carry out heat treatment for 10min at the temperature of 80 ℃;
and step eight, removing the plate frame mould from the film after heat treatment and storing the film in deionized water.
Example 4:
the embodiment provides a preparation method of a monovalent selective cation exchange membrane with a charge Janus structure, which comprises the following steps:
soaking a base material to swell the base material, wherein the base material is a sulfonated polypropylene film;
fixing the swelled base material and spreading the surface of the base material flatly by using a plate frame mold;
immersing the substrate in a coating solution 1 containing 0.15 wt.% of sodium dodecyl benzene sulfonate and 0.25 wt.% of 1,3, 5-benzene tricarboxylic acid to perform surface treatment on the substrate for 10 min;
step four, removing the coating liquid 1 and drying the surface of the membrane until the membrane is clean and dry;
step five, immersing the substrate in the coating liquid 2 containing 1 wt.% of polyethyleneimine for surface treatment for 2 min;
sixthly, removing the coating liquid 2 and drying the surface of the membrane by blowing till the membrane is clean and dry;
step seven, placing the membrane dried in the step six in an oven to carry out heat treatment for 10min at the temperature of 70 ℃;
and step eight, removing the plate frame mould from the film after heat treatment and storing the film in deionized water.
Example 5:
the embodiment provides a preparation method of a monovalent selective cation exchange membrane with a charge Janus structure, which comprises the following steps:
soaking a base material to swell the base material, wherein the base material is a sulfonated polypropylene film;
fixing the swelled base material and spreading the surface of the base material flatly by using a plate frame mold;
immersing the substrate in a coating solution 1 containing 0.1 wt.% of sodium dodecyl benzene sulfonate and 0.15 wt.% of 1,3, 5-benzene tricarboxylic acid for surface treatment for 5 min;
step four, removing the coating liquid 1 and drying the surface of the membrane until the membrane is clean and dry;
step five, immersing the substrate in the coating liquid 2 containing 1.5 wt.% of polyethyleneimine for 5min for surface treatment;
sixthly, removing the coating liquid 2 and drying the surface of the membrane until the membrane is clean and dry;
step seven, placing the membrane dried in the step six in an oven to carry out heat treatment for 30min at the temperature of 80 ℃;
and step eight, removing the plate frame mould from the film after heat treatment and storing the film in deionized water.
Claims (6)
1. A preparation method of a monovalent selective cation exchange membrane with a charge Janus structure is characterized by comprising the following steps:
soaking a base material to swell the base material, wherein the base material is a sulfonated polypropylene film;
fixing the swelled base material and spreading the surface of the base material flatly;
immersing a substrate in a coating solution 1 to perform surface treatment on the substrate, wherein the coating solution 1 contains surfactant molecules and a cross-linking agent, and the cross-linking agent is 1,3, 5-benzenetricarboxylic acid, tannic acid or dopamine;
step four, removing the coating liquid 1 and drying the surface of the membrane until the membrane is clean and dry;
immersing the substrate in coating liquid 2 to perform surface treatment on the substrate, wherein the coating liquid 2 contains amino substances, and the amino substances are polyethyleneimine, triethylene tetramine or tetraethylene pentamine;
sixthly, removing the coating liquid 2 and drying the surface of the membrane until the membrane is clean and dry;
and step seven, placing the membrane dried in the step six in an oven for heat treatment to obtain the monovalent selective cation exchange membrane with the charge Janus structure.
2. The method according to claim 1, wherein the concentration of the surfactant in the coating solution 1 is 0.1-0.3 wt.%, and the concentration of the cross-linking agent in the coating solution is 0.05-0.5 wt.%.
3. The method of claim 1 or 2, wherein the surfactant is sodium dodecylbenzene sulfonate or sodium dodecyl sulfonate.
4. The method according to claim 1, wherein the concentration of the amino group-containing substance in the coating solution 2 is 0.1 to 2 wt.%.
5. The method according to claim 1, wherein the surface treatment time is 1-10 min.
6. The method according to claim 1, wherein the heat treatment temperature is 50 to 120 ℃ and the heat treatment time is 5 to 30 min.
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| CN113522042A (en) * | 2021-08-07 | 2021-10-22 | 南开大学 | Preparation method and application of homogeneous cation exchange membrane containing alkylbenzene sulfonate |
| CN114100374B (en) * | 2021-11-26 | 2023-09-29 | 山东浩然特塑股份有限公司 | Monovalent ion selective cation exchange membrane and preparation method and application thereof |
| CN114177775B (en) * | 2022-01-11 | 2023-02-28 | 江苏巨之澜科技有限公司 | Salt lake lithium extraction nanofiltration membrane and preparation method and application thereof |
| CN114749031B (en) * | 2022-03-29 | 2023-04-07 | 杭州水处理技术研究开发中心有限公司 | Positively charged nanofiltration membrane and preparation method and application thereof |
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