CN117504617A - Pump-free household nanofiltration membrane and preparation method thereof - Google Patents
Pump-free household nanofiltration membrane and preparation method thereof Download PDFInfo
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- 239000012528 membrane Substances 0.000 title claims abstract description 63
- 238000001728 nano-filtration Methods 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000012071 phase Substances 0.000 claims abstract description 30
- 238000001035 drying Methods 0.000 claims abstract description 17
- 238000005266 casting Methods 0.000 claims abstract description 14
- 239000004695 Polyether sulfone Substances 0.000 claims abstract description 13
- 229920002492 poly(sulfone) Polymers 0.000 claims abstract description 13
- 229920006393 polyether sulfone Polymers 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000004745 nonwoven fabric Substances 0.000 claims abstract description 7
- 238000007493 shaping process Methods 0.000 claims abstract description 7
- 239000008346 aqueous phase Substances 0.000 claims abstract description 6
- 238000012695 Interfacial polymerization Methods 0.000 claims abstract description 3
- 238000012216 screening Methods 0.000 claims abstract 2
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 30
- 239000002202 Polyethylene glycol Substances 0.000 claims description 17
- 229920001223 polyethylene glycol Polymers 0.000 claims description 17
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 15
- UWCPYKQBIPYOLX-UHFFFAOYSA-N benzene-1,3,5-tricarbonyl chloride Chemical compound ClC(=O)C1=CC(C(Cl)=O)=CC(C(Cl)=O)=C1 UWCPYKQBIPYOLX-UHFFFAOYSA-N 0.000 claims description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 8
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000010410 layer Substances 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000002344 surface layer Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 238000007790 scraping Methods 0.000 claims description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 abstract description 8
- 238000000746 purification Methods 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 35
- 238000012360 testing method Methods 0.000 description 18
- 238000001223 reverse osmosis Methods 0.000 description 8
- 238000001914 filtration Methods 0.000 description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 238000000108 ultra-filtration Methods 0.000 description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 description 5
- 239000011707 mineral Substances 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000010612 desalination reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003651 drinking water Substances 0.000 description 2
- 235000020188 drinking water Nutrition 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 241000195493 Cryptophyta Species 0.000 description 1
- 229920000604 Polyethylene Glycol 200 Polymers 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000035622 drinking Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 244000052769 pathogen Species 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920006316 polyvinylpyrrolidine Polymers 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
Classifications
-
- 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
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
- B01D69/1251—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction by interfacial polymerisation
-
- 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
-
- 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
- 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
- B01D67/0013—Casting processes
-
- 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
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
- B01D69/105—Support pretreatment
-
- 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
- B01D69/10—Supported membranes; Membrane supports
- B01D69/107—Organic support material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/46—Impregnation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/22—Eliminating or preventing deposits, scale removal, scale prevention
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2307/00—Location of water treatment or water treatment device
- C02F2307/10—Location of water treatment or water treatment device as part of a potable water dispenser, e.g. for use in homes or offices
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Water Supply & Treatment (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Organic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention belongs to the technical field of new material household water purification and separation membranes, and particularly relates to a pump-free household nanofiltration membrane and a preparation method thereof. Embedding a blending membrane casting solution of polyether sulfone and polysulfone into a reverse layer of a non-woven fabric to prepare a rough base membrane layer, shaping through a drying tunnel with the temperature of 50 ℃, performing interfacial polymerization on three phases (aqueous phase, amphiphilic phase and oil phase), and finally performing post-treatment to obtain a membrane with screening function, wherein monovalent ions and divalent ions can be selectively separated, so that the household nanofiltration membrane with satisfactory water outlet under the condition of no pump is prepared.
Description
Technical Field
The invention belongs to the technical field of new material household water purification and separation membranes, and particularly relates to a pump-free household nanofiltration membrane and a preparation method thereof.
Background
Along with the increasing popularization of treatment of drinking water at the tail end of families, water purifiers are widely used in the household water purification industry. In the application aspect of membrane materials in the household water purifier, the technology of reverse osmosis filtration and ultrafiltration filtration are mainly relied on, and the technology of reverse osmosis membrane and the technology of ultrafiltration membrane are used for terminal drinking water as two membrane filtration modes which exist in parallel.
The reverse osmosis membrane has the advantages that the water at the tail end is completely water molecules, the water is pure and free of ions, and the reverse osmosis membrane plays a certain role in removing the caking and the dirt of water in areas with higher minerals and high salt areas. However, the use of reverse osmosis membranes is also obvious, and the intake of mineral demands of people is affected to a certain extent due to the fact that effluent water is free of minerals. So that the natural properties of municipal water supply are not exerted. Meanwhile, due to the compact structure of the reverse osmosis membrane. So that a high pressure pump is required as a driving force during the application of the water purifier. Thus, there is a lazy nature to the electrical energy and the ends often need to be press-fitted with pressure barrels as water reservoirs. Thus, a large space is occupied for the household kitchen, and thus, the use of the reverse osmosis water purifier is also limited by these factors.
The other end filtering ultrafiltration membrane has the advantages of blocking pathogens, pathogenic bacteria, colloid, blue algae, dirt particles and the like in water, ensuring the sanitation and safety of the end effluent quality, and achieving the direct drinking effect. Is an energy-saving, sanitary and safe instant on-line water making mode. Is very popular in the market. However, the characteristics of the micropores of the ultrafiltration membrane determine that the ultrafiltration mode does not intercept mineral ions in water, so that the problem of softening of high-hardness water quality cannot be solved.
Based on the current situation of the water treatment modes of the two filtering membranes, the end water purification treatment of the water purification industry at present needs a novel household filtering mode of the water treatment membrane.
Disclosure of Invention
Aiming at the confusion of the existing household water purification tail end water treatment, the invention provides a pump-free household nanofiltration membrane and a preparation method thereof, and fills the defects of the existing ultrafiltration membrane and reverse osmosis membrane.
The pump-free household nanofiltration membrane is prepared by embedding a blending membrane casting solution of polyethersulfone and polysulfone into a reverse side layer of non-woven fabric to prepare a rough base membrane layer, shaping through a drying tunnel at 50 ℃, performing interfacial polymerization through aqueous phase solution, amphiphilic phase solution and oil phase solution, and finally performing cleaning, drying and shaping again.
The specific preparation method of the pump-free household nanofiltration membrane comprises the following steps:
(1) Adding an organic solvent, polysulfone and polyether sulfone into a dissolving tank, stirring and mixing uniformly, and then adding polyvinylpyrrolidone until the polyvinylpyrrolidone is thoroughly dissolved to obtain a casting solution;
the casting film liquid comprises the following components in parts by mass: 20-25 parts of polysulfone and polyether sulfone blending material, 7-10 parts of polyvinylpyrrolidone K90 and 65-85 parts of organic solvent.
Wherein, the mass ratio of polysulfone to polyethersulfone is 3-5: 5 to 8.
The organic solvent is: one of N, N-dimethylformamide, dimethylacetamide, N-methylpyrrolidone or dimethylsulfoxide.
(2) Coating the casting film liquid prepared in the step (1) on a reverse surface layer of a non-woven fabric by using a scraper in a film scraping machine at room temperature, and shaping and forming a film by using a drying channel at 50 ℃ to prepare a nanofiltration base film;
(3) Soaking the base film in a water-phase solution tank containing piperazine for 8-15 minutes at room temperature; the aqueous phase solution containing piperazine comprises the following components in percentage by mass: piperazine 1.0-1.5%, sodium carbonate 1.0-1.5%, polyvinyl alcohol 0.6-1.0%, and water in balance.
(4) Soaking the base film in the step (3) in an amphiphilic phase solution tank containing polyethylene glycol at room temperature for 8-15; the amphiphilic polyethylene glycol solution comprises the following components in percentage by mass: 30-50% of polyethylene glycol, 30-50% of polyethylene glycol methyl ether, 10% of water and 10% of normal hexane.
(5) Transferring the membrane treated in the step (4) into an oil phase solution tank containing trimesoyl chloride for soaking for 3-5 minutes, and then cleaning and drying to obtain a pump-free household nanofiltration membrane;
the oil phase solution containing trimesoyl chloride is normal hexane solution of trimesoyl chloride with mass concentration of 0.4-0.6%.
The drying temperature is as follows: the drying time is 5-8 minutes at 40-60 ℃.
The beneficial effects are that:
(1) The casting film material liquid prepared from the polyether sulfone and polysulfone blending material is embedded into the non-woven fabric rough reverse surface layer to form a water-passing layer which is tightly combined and loose in structure. And then the base film layer is fully polymerized through three phases of hydrophilic phase, amphiphilic phase and oleophylic phase. The pump-free ultralow-pressure household nanofiltration membrane which has better water permeability and can fully screen monovalent ions and divalent ions in water is formed.
(2) The nanofiltration membrane is soaked in the amphiphilic phase solution, is more hydrophilic and better combined with the polymer, so that the prepared nanofiltration membrane can realize separation without pressurization.
(3) The product of the invention has the characteristics that no pump is driven, and the lazy operation of a power supply is avoided by the water supply pressure of tap water. Secondly, the product has higher mineral ion removal rate for generating caking in water, and more ions beneficial to human bodies are reserved while the caking is avoided. Thirdly, the water outlet flux is larger under the condition of no pump, so that the household water has better experience. And fourthly, the filter is obtained online, and the non-storage pressure barrel ensures the saving of kitchen space and is relatively suitable for household application.
Description of the drawings:
FIG. 1 is an electron microscope image of a plate nanofiltration membrane prepared according to the present invention.
Detailed Description
The invention is further described in detail below with reference to examples:
example 1
(1) 70g of N, N-dimethylformamide, 10g of polysulfone and 15g of polyethersulfone are put into a dissolving tank, stirred and mixed uniformly, and then 8g of polyvinylpyrrolidone is added until the mixture is completely dissolved, thus obtaining casting solution;
(2) Coating the casting film liquid prepared in the step (1) on a reverse surface layer of a non-woven fabric by using a scraper in a film scraping machine at room temperature, and shaping and forming a film by using a drying channel at 50 ℃ to prepare a nanofiltration base film;
(3) Soaking the base film in an aqueous phase solution tank containing piperazine for 10 minutes at room temperature;
the composition of the aqueous solution containing piperazine was: piperazine 1.2%, sodium carbonate 1.2%, polyvinyl alcohol 0.8%, and water the rest.
(4) At room temperature, soaking the base film in the step (3) in an amphiphilic solution tank containing polyvinyl alcohol for 10 minutes;
the composition of the amphiphilic polyethylene glycol solution is as follows: 40% of polyethylene glycol, 40% of polyethylene glycol methyl ether, 10% of water and 10% of normal hexane.
(5) Transferring the membrane treated in the step (4) into an oil phase solution tank containing trimesoyl chloride for soaking for 5 minutes, and then performing post-treatment cleaning and drying to obtain a pump-free household nanofiltration membrane;
the oil phase solution containing trimesoyl chloride is n-hexane solution of trimesoyl chloride with mass concentration of 0.5%.
Example 2
In comparison to example 1, step (1) was changed to: 70g of N, N-dimethylformamide, 7.2g of polysulfone and 16.8g of polyether sulfone are put into a dissolving tank, stirred and mixed uniformly, and then 8g of polyvinylpyrrolidone is added until the mixture is thoroughly dissolved, thus obtaining the casting solution.
The rest of the procedure is the same as in example 1.
Example 3
In comparison to example 1, step (1) was changed to: 70g of N, N-dimethylformamide, 12.5g of polysulfone and 12.5g of polyether sulfone are put into a dissolving tank, stirred and mixed uniformly, and then 8g of polyvinylpyrrolidone is added until the mixture is thoroughly dissolved, thus obtaining the casting solution.
The rest of the procedure is the same as in example 1.
Example 4
In comparison with example 1, the composition of the aqueous piperazine-containing solution of step (3) was changed to: piperazine 1.0%, sodium carbonate 1.0%, polyvinyl alcohol 0.6%, and water the rest.
The rest of the procedure is the same as in example 1.
Example 5
In comparison with example 1, the composition of the aqueous piperazine-containing solution of step (3) was changed to: piperazine 1.5%, sodium carbonate 1.5%, polyvinyl alcohol 1.0%, and water in balance.
The rest of the procedure is the same as in example 1.
Example 6
In comparison with example 1, the composition of the amphiphilic phase solution containing polyvinyl alcohol in step (4) was changed to: 30% of polyethylene glycol, 50% of polyethylene glycol methyl ether, 10% of water and 10% of n-hexane.
The rest of the procedure is the same as in example 1.
Example 7
In comparison with example 1, the composition of the amphiphilic phase solution containing polyvinyl alcohol in step (4) was changed to: 50% of polyethylene glycol, 30% of polyethylene glycol methyl ether, 10% of water and 10% of n-hexane.
The rest of the procedure is the same as in example 1.
Example 8
The concentration of the oil phase solution of step (5) was changed to 0.4% compared to example 1.
The rest of the procedure is the same as in example 1.
Comparative example 1
Steps (1) - (3) are the same as in example 1.
(4) Transferring the membrane treated in the step (3) into an oil phase solution tank containing trimesoyl chloride for soaking for 5 minutes, and then performing post-treatment cleaning and drying to obtain a pump-free household nanofiltration membrane;
the oil phase solution containing trimesoyl chloride is n-hexane solution of trimesoyl chloride with mass concentration of 0.5%.
Comparative example 2
Steps (1) - (2) are the same as in example 1.
(3) Soaking the base film in a solution tank containing piperazine for 10 minutes at room temperature;
the composition of the aqueous solution containing piperazine was: piperazine 1.2%, sodium carbonate 1.2%, polyvinyl alcohol 0.8%, polyethylene glycol 40% and water the rest.
(4) Transferring the membrane treated in the step (3) into an oil phase solution tank containing trimesoyl chloride for soaking for 5 minutes, and then performing post-treatment cleaning and drying to obtain a pump-free household nanofiltration membrane;
the oil phase solution containing trimesoyl chloride is 40% of trimesoyl chloride and polyethylene glycol methyl ether with the mass concentration of 0.5%, and the balance is normal hexane solution.
The testing method comprises the following steps:
and (3) connecting the nanofiltration membrane component to a testing device, connecting pure water, adjusting the water pressure to 0.3MPa, running for 30min, then connecting filtrate, timing for 10min, and calculating the flow.
Divalent salt rejection: analytically pure MgSO 4 Preparing stock solution, adding standard to 1000-2000 us/cm, operating and filtering under 0.3MPa, taking filtrate, measuring conductivity and calculating desalination rate.
Monovalent desalination rate: analyzing pure NaCl, preparing stock solution, adding standard to 1000-2000 us/cm, operating and filtering under 0.3MPa, taking filtrate, measuring conductivity and calculating desalination rate.
Test conditions
The test should be carried out under the following conditions, except for the special provisions, and the specific conditions are shown in Table 1.
TABLE 1
Configuration of test raw water
According to the test conditions, pure water with conductivity less than 10 mu S/cm and a reagent with purity of analytical purity are used for preparing a test raw solution with a certain concentration, and the pH value is regulated by adopting NaOH or HCl. The prepared test raw water should be stored in a light-proof closed container and should be prepared for use at present.
Testing
a) And filling the nanofiltration membrane component to be tested into a membrane shell, and flushing with pure water with the conductivity less than 10 mu S/cm according to the pressure and the recovery rate in the test conditions for 30min.
b) And (3) connecting the washed nanofiltration membrane component with a testing device according to B.2 in an annex B of GB/T30306-2013, and introducing conductivity (standard solution) under testing conditions. After the system stably operates for 10min, a certain amount of raw water of conductivity (standard liquid) test liquid and water from a water outlet of the nanofiltration membrane component are collected by a beaker, and the conductivity is tested according to a conductivity measurement method. And the conductivity is tested, meanwhile, the total hardness of raw water and produced water can be tested by using a sampling water sample, and the removal rate is calculated. Total hardness test method is referred to GB/T5750.4-2006.
c) Connecting MgSO 4 After the system stably operates for 10min, the test solution is respectively collected by a beaker to obtain a certain amount of MgSO 4 Testing the raw water of the liquid and the water outlet of the nanofiltration membrane component, and testing electricity according to a conductivity measurement methodConductivity.
d) And connecting NaCl test liquid, collecting a certain amount of raw water of the NaCl test liquid and water from a water outlet of the nanofiltration membrane component by using a beaker after the system stably runs for 10min, and testing the conductivity according to a conductivity measurement method.
e) Alternative freshly unpacked nanofiltration membrane elements were tested for PEG200 removal rate, performed with reference to the methods in the GB/T34242-2017 standard.
The results of the performance tests of the inventive and comparative examples are shown in Table 2
TABLE 2
Claims (9)
1. A pump-free domestic nanofiltration membrane is characterized in that a blend casting membrane solution of polyethersulfone and polysulfone is embedded into a reverse side layer of non-woven fabric to form a rough base membrane layer, the rough base membrane layer is shaped through a drying channel with the temperature of 50 ℃, and then is subjected to interfacial polymerization of aqueous phase solution, amphiphilic phase solution and oil phase solution, and finally is subjected to cleaning, drying and shaping again to obtain the nanofiltration membrane with a screening function.
2. The pump-free household nanofiltration membrane as claimed in claim 1, wherein the blending casting solution comprises the following components in parts by mass: 20-25 parts of polysulfone and polyether sulfone blending material, 907-10 parts of polyvinylpyrrolidone and 65-85 parts of organic solvent.
3. The pump-free household nanofiltration membrane according to claim 2, wherein the mass ratio of polysulfone to polyethersulfone in the blend material is 3-5: 5 to 8.
4. The pumpless domestic nanofiltration membrane of claim 2, wherein the organic solvent is: one of N, N-dimethylformamide, dimethylacetamide, N-methylpyrrolidone or dimethylsulfoxide.
5. The pumpless domestic nanofiltration membrane of claim 1, wherein the aqueous phase solution comprises, in mass percent: piperazine 1.0-1.5%, sodium carbonate 1.0-1.5%, polyvinyl alcohol 0.6-1.0% and water the rest.
6. The pumpless domestic nanofiltration membrane of claim 1, wherein the amphiphilic phase solution comprises, in mass percent: 30-50% of polyethylene glycol, 30-50% of polyethylene glycol methyl ether, 10% of water and 10% of normal hexane.
7. The pumpless domestic nanofiltration membrane of claim 1, wherein the oil phase solution is an n-hexane solution of trimesoyl chloride with a mass concentration of 0.4-0.6%.
8. A method for preparing the pump-free household nanofiltration membrane as claimed in claim 1, wherein the preparation method comprises the following steps:
(1) Adding an organic solvent, polysulfone and polyethersulfone into a dissolving tank, fully stirring and uniformly mixing, and then adding polyvinylpyrrolidone until the polyvinylpyrrolidone is thoroughly dissolved to obtain a casting solution;
(2) Coating the casting film liquid prepared in the step (1) on a reverse surface layer of a non-woven fabric by using a scraper in a film scraping machine at room temperature, and shaping and forming a film by using a drying channel at 50 ℃ to prepare a nanofiltration base film;
(3) Soaking the base film in a water-phase solution tank containing piperazine for 8-15 minutes at room temperature;
(4) At room temperature, soaking the base film in the step (3) in a amphiphilic phase solution tank containing polyethylene glycol and polyethylene glycol methyl ether for 8-15;
(5) Transferring the membrane treated in the step (4) into an oil phase solution tank containing trimesoyl chloride for soaking for 3-5 minutes, and then cleaning and drying to obtain the pump-free household nanofiltration membrane.
9. The method for preparing a pump-free household nanofiltration membrane according to claim 8, wherein the drying temperature is: the drying time is 5-8 minutes at 40-60 ℃.
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