CN114669194B - Preparation method of single-multivalent ion high-resolution nanofiltration membrane - Google Patents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
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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
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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
- B01D69/12—Composite membranes; Ultra-thin membranes
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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
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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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
- B01D2325/02—Details relating to pores or porosity of the membranes
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- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
Abstract
A preparation method of a single-multivalent ion high-resolution nanofiltration membrane belongs to the technical field of membrane separation materials. The method comprises the following steps: preparing an aqueous solution: piperazine 0.8-2.0g/l, specific bi-component surfactant 0.1-5g/l, buffer salt 10-50g/l, pH range 8-11; configuration with organic phase solution: adding trimesoyl chloride monomer into isodecaalkane solvent oil and mixing; preparing a composite membrane: and (3) completely immersing the porous polysulfone supporting layer into the aqueous solution or coating the aqueous solution on one surface of the porous polysulfone supporting layer, removing the surface water, coating the organic solution on the other surface of the porous polysulfone supporting layer, and drying. According to the preparation method of the single-multivalent ion high-resolution nanofiltration membrane, the specific bi-component surfactant is added into the aqueous phase solution to precisely regulate and control the nanometer size of the formed polypiperazine amide particles, so that the high-resolution nanofiltration membrane has extremely high resolution on monovalent ions such as chloride ions and multivalent ions such as sulfate radicals and has high water production efficiency.
Description
Technical Field
The invention belongs to the technical field of membrane separation materials, and particularly relates to a preparation method of a single-multivalent ion high-resolution nanofiltration membrane.
Background
The nanofiltration membrane separation material is a novel separation membrane material in recent years, and is obviously different from the traditional reverse osmosis membrane separation material. The greatest difference is that for different feed components, such as the anionic mixed component system: chloride/sulfate, as cationic mixed component system: calcium magnesium ions/lithium sodium ions, etc., exhibit distinct separation characteristics, i.e., high ion permselectivity. In recent years, the separation process of the nanofiltration membrane can also keep the pure physical property of the membrane separation process, so that the method is particularly suitable for the material concentration and purification processes in the industrial field, and particularly for the purification and separation processes which do not support the thermal process.
The great difference of the nanofiltration composite membrane and the reverse osmosis composite membrane in the separation selectivity comes from the separation mechanism. The separation mechanism of composite membranes, which generally have rejection characteristics for salt ions, is generally considered to be: charge repulsion, pore size sieving, solution diffusion, etc. For the charge repulsion separation, the membrane material has the lowest desalting performance and the best pollution resistance when the surface is at zero potential, and the charge repulsion has more obvious influence on the separation performance of the nanofiltration composite membrane and the reverse osmosis composite membrane.
Chinese patent CN 109224865A discloses a preparation method of a nanofiltration membrane with high selective separation property. The separation selectivity of the nanofiltration composite membrane is improved by adjusting the surface charge property of the prepared nanofiltration composite membrane. However, the high-selectivity nanofiltration composite membrane prepared by adopting the dendritic membrane material as the water phase additive to prepare the low-rejection-rate nanofiltration composite base membrane and then adopting the method of electronegativity regulating the surface of the base membrane by adopting the strong electronegativity compound realizes lower removal rate of chloride ions, but the removal rate of sulfate radicals is remarkably lower, the separation requirement of a chlor-alkali working condition system which has the requirement of higher removal rate of the sulfate radicals at the same time cannot be met, and the use breadth is limited. In addition, the process is complex, when the hydrophilic dendritic polymer material is used as a water phase additive, the difficulty of removing residual water on the surface of the hydrophilic dendritic polymer material is increased, and the removal rate of multivalent salt ions such as sulfate radical and the like is obviously low, and the firmness of the surface charge regulated by the surface negatively charged group compound in the operation period, the medicament cleaning link and the like is required to be verified.
Chinese patent CN 111330450A discloses a preparation method of a composite membrane with high flux and high desalination rate and the prepared composite membrane. The morphology structure of the prepared composite membrane is adjusted by adding a specific inorganic salt additive into a water phase system, so that the water flux of the reverse osmosis composite membrane is greatly improved on the premise of not damaging the desalination rate. The addition of specific inorganic salts thereof alters the monomer diffusion process of the interfacial polymerization reaction. The method is suitable for industrial batch preparation, but the salt rejection rate of the prepared reverse osmosis membrane is still low, and whether the effect of the interfacial polymerization process of the nanofiltration composite membrane, which is similar to a piperazine system, is obviously higher than that of the reverse osmosis membrane forming process and has extremely strong hydrophilicity of the nanofiltration membrane water-phase monomer piperazine and extremely short diffusion depth to an organic phase, needs to be verified.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to design and provide a technical scheme of a preparation method of a single-multivalent ion high-resolution nanofiltration membrane, and the preparation method adopts a specific bi-component surfactant to cooperatively regulate and control an interfacial polymerization reaction field of piperazine and trimesoyl chloride on a similar porous support membrane from the comprehensive consideration of a reaction mechanism and a separation mechanism of the nanofiltration composite membrane, so that the high-selectivity nanofiltration composite separation membrane material with more uniform granularity, smaller surface separation holes and wider surface charge zero-charge pH interval is realized in one step; the prepared nanofiltration composite membrane material has low interception performance on monovalent salt and extremely high desalination performance on multivalent salt such as sulfate ions and calcium and magnesium ions.
The preparation method of the single-multivalent salt high-resolution nanofiltration composite membrane is characterized by comprising the following steps of:
1) Preparing a polysulfone/dimethylformamide membrane casting solution, coating a layer of membrane casting solution on a PET non-woven fabric in a scraping manner, and curing and rinsing to obtain a porous polysulfone supporting layer;
2) Completely immersing the porous polysulfone supporting layer into the aqueous solution or coating the aqueous solution on one side of the porous polysulfone supporting layer, and removing surface water for later use;
preparing the aqueous phase solution, wherein in the aqueous phase solution: piperazine 0.8-2.0g/l, bi-component surfactant 0.1-5g/l, buffer salt 10-50g/l, and pH 8-11; the bi-component surfactant is prepared by mixing the components in a concentration ratio of 0.5-2.5: sodium lauryl sulfate of 1: mixing sodium hexadecyl sulfate; the buffer salt is at least one of sodium citrate, sodium camphorsulfonate, triethylamine hydrochloride and sodium phosphate;
3) Coating an organic phase solution on one surface of the porous polysulfone supporting layer containing the water phase monomer formed in the step 2), and drying to obtain a nanofiltration composite membrane;
the organic phase solution is formed by adding trimesoyl chloride monomer into isodecaalkane solvent oil and mixing, and the concentration of the trimesoyl chloride in the organic phase solution is 0.6-1.5g/l.
The preparation method of the high-resolution nanofiltration composite membrane of mono-and multivalent salts is characterized in that the preparation method comprises the following steps of 1): adding polysulfone and dimethylformamide into a batching kettle, setting the interlayer heat conduction oil temperature of the batching kettle to be 45-55 ℃, starting a stirrer to stir for 1-2 hours at the rotation speed of 200-250rpm, raising the interlayer heat conduction oil temperature of the batching kettle to 85-95 ℃, continuously keeping stirring, filtering and removing impurities of feed liquid through a filter after the whole casting liquid is transparent, transferring the feed liquid to a storage tank, defoaming the casting liquid in the storage tank by using a vacuum pump, and keeping constant temperature when the casting liquid temperature is slowly reduced to 20-30 ℃ for later use; and (3) blade-coating a layer of casting solution with the thickness of 30-50 microns on the PET non-woven fabric, and carrying out primary curing through a gel bath and fully rinsing through a rinsing tank to obtain the porous polysulfone supporting layer.
The preparation method of the high-resolution nanofiltration composite membrane of mono-and multivalent salts is characterized in that the preparation method comprises the following steps of 1): the porous polysulfone support layer is prepared by slit preset amount coating or doctor blade casting coating and a wet phase inversion method.
The preparation method of the high-resolution nanofiltration composite membrane of mono-and multivalent salts is characterized in that the preparation method comprises the following steps of 1): the weight ratio of the polysulfone to the dimethylformamide is 10-20, preferably 15.
The preparation method of the high-resolution nanofiltration composite membrane of mono-and multivalent salts is characterized in that the step 2) is that: 1-1.8g/l of piperazine, 0.5-4g/l of bi-component surfactant, 15-45g/l of buffer salt and 8.5-10.5 of pH; preferably 1.2-1.6g/l of piperazine, 1-3g/l of bi-component surfactant, 20-40g/l of buffer salt and 9-10 of pH; more preferably 1.4-1.5g/l piperazine, 2-2.5g/l bi-component surfactant, 25-30g/l buffer salt, and pH 9.3-9.5.
The preparation method of the high-resolution nanofiltration composite membrane of mono-and multivalent salts is characterized in that in the step 2): sodium lauryl sulfate: the concentration ratio of the sodium hexadecyl sulfate is 1-2:1, preferably 1.5:1.
the preparation method of the high-resolution nanofiltration composite membrane of mono-and multivalent salts is characterized in that in the step 2): the concentration of trimesoyl chloride in the solution of the organic phase is from 0.8 to 1.3g/l, preferably from 1 to 1.1g/l.
The preparation method of the single-multivalent ion high-resolution nanofiltration membrane has the technical effects that:
1) On a porous polysulfone support membrane, obtaining a composite nanofiltration membrane by using a water phase containing a specific bi-component surfactant, piperazine and sodium citrate and isomeric decaalkane solvent oil containing trimesoyl chloride through a traditional interfacial polymerization mode and oven heat treatment; the invention precisely adjusts and controls the nanometer size of the formed polypiperazine amide particles by adding the specific bi-component surfactant into the aqueous phase solution, thereby realizing the nanofiltration composite membrane which has extremely high resolution ratio on monovalent ions such as chloride ions and multivalent ions such as sulfate radicals and has higher water production efficiency.
2) The nanofiltration composite membrane obtained by the invention has the high-selectivity nanofiltration composite separation membrane material with more uniform granularity, smaller surface separation holes and wider surface charge zero-charge pH interval, thereby realizing the high-selectivity separation of multivalent/monovalent salt ions and extremely high removal rate of the multivalent salt ions, meeting the application of high-concentration salt working conditions, and being widely applied to the industry fields of pharmacy, petrifaction, chlor-alkali, food and the like which have requirements on material separation and purification operations.
Drawings
FIG. 1 is a SEM photograph of example 3 of the present invention;
fig. 2 is a surface particle size distribution diagram of the composite nanofiltration membrane in example 3 of the present invention;
fig. 3 is a surface contact angle diagram of the composite nanofiltration membrane in example 3 of the present invention.
Detailed Description
The present invention will now be described more fully hereinafter with reference to the accompanying specific examples and comparative examples, in which some, but not all examples of the invention are shown. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Examples 1-8 and comparative examples, the configuration is given in table 1.
1) Putting 15wt% of Suwei p3500 polysulfone and 85 wt% of dimethylformamide into a batching kettle, setting the temperature of interlayer heat conduction oil of the batching kettle to be 50 ℃, starting a stirrer to stir for 1.5 hours, rotating at 220rpm, increasing the temperature of interlayer heat conduction oil of the batching kettle to be 90 ℃, continuing stirring, filtering and removing impurities of feed liquid through a filter after the whole casting solution is transparent, transferring the feed liquid to a storage tank, defoaming the casting solution in the storage tank by using a vacuum pump, and keeping constant temperature when the temperature of the casting solution is slowly reduced to 25 ℃ for later use; a layer of casting solution with the thickness of 40 microns is blade-coated on a PET non-woven fabric with the width of 1100mm, and is subjected to 15wt% of dimethylacetamide aqueous solution to form a gel bath, the gel bath is carried out at 25 ℃, the gel bath is fully soaked and primarily cured for 20 seconds, and the gel bath is fully rinsed with warm water at 50 ℃ to obtain the porous polysulfone supporting layer.
2) Completely immersing the porous polysulfone supporting layer into the aqueous solution or coating the aqueous solution on one side of the porous polysulfone supporting layer, extruding the porous polysulfone supporting layer by using an extrusion roller, setting the pressure of the extrusion roller to be 0.3Mpa, and blowing off residual liquid drops on the film surface by using a dehumidified air knife for later use;
preparing the aqueous phase solution, wherein in the aqueous phase solution: 1.5g/l of piperazine, 2g/l of bi-component surfactant, 20g/l of buffer salt and pH of 9; the bi-component surfactant is prepared by mixing sodium dodecyl sulfate and sodium hexadecyl sulfate, wherein the ratio of the sodium dodecyl sulfate: the concentration ratio of sodium hexadecyl sulfate is 1.5:1; the buffer salt is at least one of sodium citrate, sodium camphorsulfonate, triethylamine hydrochloride and sodium phosphate; the temperature of the aqueous phase was 25 ℃.
3) Coating an organic phase solution on one side of the porous polysulfone supporting layer containing the water-phase monomer formed in the step 2), performing heat treatment for 5 minutes in a 90 ℃ oven to complete the interfacial polymerization process of the composite membrane, thus obtaining the high-resolution nanofiltration membrane, and storing the prepared nanofiltration membrane in deionized water for later use.
The organic phase solution is formed by adding trimesoyl chloride monomer into isodecaalkane solvent oil and mixing, the concentration of the trimesoyl chloride in the organic phase solution is 1.0g/L, and the temperature is 25 ℃.
In the invention: setting the temperature of the interlayer heat conduction oil of the batching kettle at 45 ℃, 48 ℃, 52 ℃ or 55 ℃, starting a stirrer to stir for 1 or 2 hours at the rotation speed of 200 rpm or 250rpm, raising the temperature of the interlayer heat conduction oil of the batching kettle to 85 ℃, 92 ℃ or 95 ℃, slowly reducing the temperature of the casting solution to 20 ℃, 23 ℃, 28 ℃ or 30 ℃ and keeping the constant temperature; the doctor blade coating thickness of the casting solution is 35 micrometers, 45 micrometers or 50 micrometers.
In the aqueous phase solution: 1.5g/l of piperazine, 4.0g/l of bi-component surfactant and 10g/l of sodium phosphate, wherein the pH value is 12; or 1g/l of piperazine, 2g/l of bi-component surfactant and 40g/l of buffer salt, and the pH value is 10.5; or 1.8g/l of piperazine, 0.8g/l of bi-component surfactant, 20g/l of buffer salt and 8.7 of pH. Sodium lauryl sulfate: the concentration ratio of sodium hexadecyl sulfate is 0.5:1 or 2.5:1. the concentration of trimesoyl chloride in the organic phase solution is 0.6g/l, 1.5g/l or 1.2g/l. The performance test of the prepared nanofiltration membrane can also achieve the beneficial effects of the invention by the same steps as the examples 1-5.
The advantageous effects of the present invention are further illustrated by the corresponding test data below.
The composite nanofiltration membranes of examples 1 to 8 and comparative example 1 were tested for desalination and water permeation performance at an operating temperature of 25 ℃ and an operating pressure of 0.5MPa in a sodium chloride solution of 2000ppm and a sodium sulfate solution of 2000ppm, as shown in table 2.
Table 2 shows that: compared with comparative example 1 with zero surfactant addition, examples 1-8 of the present invention using a two-component surfactant had better resolution for typical mono/multivalent salt ions consisting of chloride/sulfate groups, while having extremely high removal performance for the removal rate of multivalent salt ions.
The embodiments described in this specification are merely exemplary of implementations of the inventive concepts and are provided for illustrative purposes only. The scope of the present invention should not be construed as being limited to the particular forms set forth in the embodiments, but is to be accorded the widest scope consistent with the principles and equivalents thereof as contemplated by those skilled in the art.
Claims (12)
1. A preparation method of a single-multivalent salt high-resolution nanofiltration composite membrane is characterized by comprising the following steps:
1) Preparing a polysulfone/dimethylformamide membrane casting solution, coating a layer of membrane casting solution on a PET non-woven fabric in a scraping manner, and curing and rinsing to obtain a porous polysulfone supporting layer;
2) Completely immersing the porous polysulfone supporting layer into the aqueous solution or coating the aqueous solution on one side of the porous polysulfone supporting layer, and removing surface water for later use;
preparing the aqueous phase solution, wherein in the aqueous phase solution: piperazine 0.8-2.0g/l, bi-component surfactant 0.1-5g/l, buffer salt 10-50g/l, pH 8-11; the bi-component surfactant is prepared by mixing the components in a concentration ratio of 0.5-2.5: sodium lauryl sulfate of 1: mixing sodium hexadecyl sulfate; the buffer salt is at least one of sodium citrate, sodium camphorsulfonate, triethylamine hydrochloride and sodium phosphate;
3) Coating an organic phase solution on one side of the porous polysulfone supporting layer containing the water phase monomer formed in the step 2), and drying to obtain a nanofiltration composite membrane;
the organic phase solution is formed by adding trimesoyl chloride monomer into isodecaalkane solvent oil and mixing, and the concentration of the trimesoyl chloride in the organic phase solution is 0.6-1.5g/l.
2. The method for preparing a high-resolution nanofiltration composite membrane of mono-and multivalent salts according to claim 1, wherein the step 1) comprises: adding polysulfone and dimethylformamide into a batching kettle, setting the interlayer heat conduction oil temperature of the batching kettle to be 45-55 ℃, starting a stirrer to stir for 1-2 hours at the rotation speed of 200-250rpm, raising the interlayer heat conduction oil temperature of the batching kettle to 85-95 ℃, continuously keeping stirring, filtering and removing impurities of feed liquid through a filter after the whole casting liquid is transparent, transferring the feed liquid to a storage tank, defoaming the casting liquid in the storage tank by using a vacuum pump, and keeping constant temperature when the casting liquid temperature is slowly reduced to 20-30 ℃ for later use; and (3) blade-coating a layer of casting solution with the thickness of 30-50 microns on the PET non-woven fabric, and carrying out primary curing through a gel bath and fully rinsing through a rinsing tank to obtain the porous polysulfone supporting layer.
3. The method for preparing a high-resolution nanofiltration composite membrane of mono-and multivalent salts according to claim 1, wherein the step 1) comprises: the porous polysulfone support layer is prepared by slit preset amount coating or doctor blade casting coating and a wet phase inversion method.
4. The method for preparing a high-resolution nanofiltration composite membrane of mono-and multivalent salts according to claim 1, wherein the step 1) comprises: the weight ratio of the polysulfone to the dimethylformamide is 10-20.
5. The method for preparing a high-resolution nanofiltration composite membrane of mono-and multivalent salts according to claim 1, wherein the step 1) comprises: the weight ratio of polysulfone to dimethylformamide is 15.
6. The method for preparing a high-resolution nanofiltration composite membrane of mono-and multivalent salts according to claim 1, wherein the step 2) comprises the following steps: 1-1.8g/l of piperazine, 0.5-4g/l of bi-component surfactant, 15-45g/l of buffer salt and 8.5-10.5 of pH.
7. The method for preparing a high-resolution nanofiltration composite membrane of mono-and multivalent salts according to claim 1, wherein the step 2) comprises the following steps: 1.2-1.6g/l of piperazine, 1-3g/l of bi-component surfactant, 20-40g/l of buffer salt and pH of 9-10.
8. The method for preparing a high-resolution nanofiltration composite membrane of mono-and multivalent salts according to claim 1, wherein the step 2) comprises the following steps: 1.4-1.5g/l of piperazine, 2-2.5g/l of bi-component surfactant, 25-30g/l of buffer salt and 9.3-9.5 of pH.
9. The method for preparing a high-resolution nanofiltration composite membrane of mono-and multivalent salts according to claim 1, wherein in the step 2): sodium lauryl sulfate: the concentration ratio of the sodium hexadecyl sulfate is 1-2:1.
10. the method for preparing a mono-and multivalent-salt high-resolution nanofiltration composite membrane according to claim 1, wherein in the step 2): sodium lauryl sulfate: the concentration ratio of sodium hexadecyl sulfate was 1.5:1.
11. the method for preparing a mono-and multivalent-salt high-resolution nanofiltration composite membrane according to claim 1, wherein in the step 2): the concentration of trimesoyl chloride in the organic phase solution is 0.8-1.3g/l.
12. The method for preparing a high-resolution nanofiltration composite membrane of mono-and multivalent salts according to claim 1, wherein in the step 2): the concentration of trimesoyl chloride in the organic phase solution is 1-1.1g/l.
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