CN106861451B - Heat-resistant filter membrane and preparation method and application thereof - Google Patents
Heat-resistant filter membrane and preparation method and application thereof Download PDFInfo
- Publication number
- CN106861451B CN106861451B CN201710127327.9A CN201710127327A CN106861451B CN 106861451 B CN106861451 B CN 106861451B CN 201710127327 A CN201710127327 A CN 201710127327A CN 106861451 B CN106861451 B CN 106861451B
- Authority
- CN
- China
- Prior art keywords
- carbon nitride
- nitride powder
- filter membrane
- graphite
- heat
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000012528 membrane Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000000843 powder Substances 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000005266 casting Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000002351 wastewater Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 22
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 239000004695 Polyether sulfone Substances 0.000 claims description 13
- 229920006393 polyether sulfone Polymers 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 10
- 239000003960 organic solvent Substances 0.000 claims description 9
- 238000007790 scraping Methods 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000004745 nonwoven fabric Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine powder Natural products NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 229920002521 macromolecule Polymers 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 43
- 239000010408 film Substances 0.000 description 33
- 230000004907 flux Effects 0.000 description 11
- 239000007787 solid Substances 0.000 description 9
- 229920000642 polymer Polymers 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 229910021389 graphene Inorganic materials 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 229920000728 polyester Polymers 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 238000001728 nano-filtration Methods 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000012695 Interfacial polymerization Methods 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 229920012266 Poly(ether sulfone) PES Polymers 0.000 description 2
- 229920002301 cellulose acetate Polymers 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000012760 heat stabilizer Substances 0.000 description 2
- 229920002492 poly(sulfone) Polymers 0.000 description 2
- 229920002239 polyacrylonitrile Polymers 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
Images
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
- B01D69/02—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
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
-
- 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
- B01D71/02—Inorganic material
- B01D71/021—Carbon
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/22—Thermal or heat-resistance properties
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a heat-resistant filter membrane and a preparation method and application thereof. Specifically, the preparation method comprises the following steps: 1) modifying graphite-like carbon nitride powder; 2) preparing a casting solution; 3) phase inversion to form a film. The preparation method has the advantages of simple process, convenient operation, high automation degree, easily obtained raw materials and easy realization of industrial production. The heat-resistant filter membrane prepared by the method has smooth and flat surface, has no obvious nano material agglomeration, and can be used as a filter membrane material for water treatment of high-temperature wastewater.
Description
Technical Field
The invention belongs to the technical field of membrane separation, and relates to a heat-resistant filter membrane, a preparation method thereof and application thereof in water treatment of high-temperature wastewater.
Background
The membrane separation technology is a novel separation technology, develops rapidly in recent decades, and is widely applied to the fields of water treatment, chemical industry, biology, medicines, foods and the like. Organic high polymers such as Polyethersulfone (PES), Polysulfone (PS), polyvinylidene fluoride (PVDF), Polyacrylonitrile (PAN), Cellulose Acetate (CA) are widely used as base film materials because of their excellent solubility, thermoplasticity and mechanical properties. However, as the greatest disadvantage of the organic film, the problem of poor thermal stability has also attracted a great deal of attention by those skilled in the art.
Interfacial polymerization is a typical method for preparing Nanofiltration (NF) membranes and Reverse Osmosis (RO) membranes, and has the advantages of mild conditions, easy control of reaction and the like. In the interfacial polymerization process, a base film is sequentially immersed in a water phase and an organic phase with certain compositions, organic monomers in the two phases react on the surface of the base film to form an ultrathin selection layer, and the finally prepared film needs to be heated for a certain time at a certain temperature so as to promote the completion of the polymerization reaction. Studies have shown that the temperature and time of the heat treatment will significantly affect the flux and rejection rate of the membrane.
In recent years, some work has been done by researchers to improve the thermal stability of polymers. Graphene is a single atomThe two-dimensional carbon structure with the thickness of the sub-layer has good mechanical property, electrical and thermal stability. Researches show that the thermal stability of the graphene can be remarkably improved by combining the graphene with a polymer. Graphite-like phase carbon nitride (g-C)3N4) And has a two-dimensional layered structure similar to graphene. It has attracted much attention because of its excellent chemical stability and visible light catalytic properties. However, no literature reports that graphite-like phase carbon nitride is introduced into a membrane material as a heat stabilizer to prepare a heat-resistant filter membrane.
Disclosure of Invention
Aiming at the technical problem that no heat-resistant filter membrane using graphite-like carbon nitride as a heat stabilizer exists at present, the invention aims to provide a heat-resistant filter membrane and a preparation method and application thereof.
Specifically, the invention adopts the following technical scheme:
a preparation method of a heat-resistant filter membrane comprises the following steps:
1) modification of graphite-like phase carbon nitride powder:
under the stirring condition, uniformly mixing graphite-like phase carbon nitride powder and strong acid according to the dosage proportion of 1g of strong acid to 20-40 mL, centrifuging, washing with water, and drying to obtain modified graphite-like phase carbon nitride powder;
2) preparing a casting solution:
mixing the modified graphite-like carbon nitride powder obtained in the step 1) with an organic solvent, performing ultrasonic dispersion uniformly, adding a base film macromolecular compound into the solution under the stirring condition, heating for dissolving, and then sealing, standing and defoaming to obtain a casting solution; wherein: the mass fraction of the modified graphite-like carbon nitride powder is 0.05-1.2%, and the mass fraction of the basal membrane macromolecular compound is 10-25%;
3) phase inversion film formation:
scraping the casting solution obtained in the step 2) into a film on a supporting layer by using a scraper, immediately immersing the film into a pure water bath at 25 ℃ after scraping to perform phase conversion film formation, and then immersing the prepared film into the pure water bath for more than 24 hours to remove the organic solvent, thereby finally obtaining the heat-resistant filter membrane.
In the above production method, the graphite-like phase carbon nitride powder in step 1) may be either commercially available or produced by the following method: heating melamine powder to 500-550 ℃ (preferably 500 ℃) and keeping for 2-3 hours (preferably 2 hours), then heating to 520-570 ℃ (preferably 520 ℃) at the speed of 10-15 ℃/min (preferably 10 ℃/min) and keeping for 2-3 hours (preferably 2 hours), stopping heating, naturally cooling to room temperature, and grinding to obtain the graphite-like phase carbon nitride powder.
In the above preparation method, the strong acid in step 1) is nitric acid, sulfuric acid or a mixture of the two, preferably a mixture of the two, and more preferably a mixture of nitric acid and sulfuric acid in a volume ratio of 1: 3.
In the preparation method, the using amount ratio of the graphite-like phase carbon nitride to the strong acid in the step 1) is 1g to 30 mL.
In the preparation method, the rotation speed of the centrifugation in the step 1) is 6000-8000 rpm (preferably 6000 rpm).
In the above preparation method, the water washing in step 1) is performed using deionized water.
In the preparation method, the drying temperature in the step 1) is 60-80 ℃ (preferably 60 ℃).
In the above preparation method, the organic solvent in step 2) is N, N-Dimethylformamide (DMF).
In the above preparation method, the base film polymer compound in step 2) is Polyethersulfone (PES).
In the preparation method, the mass fraction of the modified graphite-like phase carbon nitride powder in the casting solution in the step 2) is 0.25%, and the mass fraction of the base film polymer compound is 20%.
In the above preparation method, the support layer in step 3) is a non-woven fabric (preferably a polyester non-woven fabric).
In the above production method, the thickness of the thin film in the step 3) is controlled by a feeler gauge.
A heat-resistant filter membrane is prepared by the preparation method.
The heat-resistant filter membrane (as an ultrafiltration membrane or a nanofiltration membrane) is applied to water treatment of high-temperature wastewater (preferably high-temperature wastewater generated in the food or medical industry).
The preparation method of the heat-resistant filter membrane has the advantages of simple process, convenient operation, high automation degree, easily obtained raw materials and easy realization of industrial production. The heat-resistant filter membrane prepared by the method has smooth and flat surface and no obvious nano material agglomeration. Adding graphite-like carbon nitride (g-C) to base film polymer material3N4) Can improve the surface hydrophilicity and the section pore structure of the membrane, improve the pure water flux recovery rate of the membrane on the premise of not sacrificing the interception performance of the membrane, and show good thermal stability.
Drawings
FIG. 1 is a surface and cross-sectional profile of the heat-resistant filter membrane prepared in example 1, wherein (a) is a surface profile and (b) is a cross-sectional profile.
Fig. 2 is a schematic diagram showing the comparison of pure water flux recovery rates of a common polyethersulfone filter membrane and the heat-resistant filter membrane prepared in example 1 before and after being subjected to heat treatment for different periods of time, wherein PES is the common polyethersulfone filter membrane, and M2 is the heat-resistant filter membrane.
FIG. 3 is a thermogravimetric analysis of a common polyethersulfone filter and the heat-resistant filter obtained in example 1, wherein PES is a common polyethersulfone filter and M2 is a heat-resistant filter.
Detailed Description
The technical solution of the present invention will be further described with reference to the accompanying drawings and specific embodiments. Unless otherwise indicated, the instruments, materials, reagents and the like used in the following examples are all available by conventional commercial means.
Example 1: preparing a heat-resistant filter membrane and testing the performance of the heat-resistant filter membrane.
(1) Preparing graphite-like phase carbon nitride powder:
putting melamine powder (5g) into an alumina crucible with a cover, covering the crucible, putting the crucible into a muffle furnace, heating to 500 ℃, keeping the temperature for 2h, then heating to 520 ℃ at the speed of 10 ℃/min, keeping the temperature for 2h, stopping heating, naturally cooling the crucible to room temperature, and finally grinding the yellow blocky solid into faint yellow graphite-like carbon nitride powder (0.3g) by using an agate mortar.
(2) Modification of graphite-like phase carbon nitride powder:
placing the graphite-like phase carbon nitride powder (0.3g) obtained in the step (1) in a strong mixed acid (9mL, V)Nitric acid:VSulfuric acid1:3), the mixture was magnetically stirred overnight, centrifuged at 6000rpm using a centrifuge, and the resulting solid powder was washed with deionized water until neutral, and then dried in an oven at 60 ℃ overnight to give a modified graphite-like phase carbon nitride powder (0.25 g).
(3) Preparing a casting solution:
adding the modified graphite-like phase carbon nitride powder (0.25g) obtained in the step (2) into N, N-dimethylformamide (79.75g), performing ultrasonic treatment for 30min to disperse the modified graphite-like phase carbon nitride powder, adding polyether sulfone (20g), performing magnetic stirring to disperse the modified graphite-like phase carbon nitride powder, placing the mixture into an oven at 60 ℃ to dissolve solids, and sealing, standing and defoaming to obtain a casting solution (100 g).
(4) Phase inversion film formation:
pouring a certain amount of casting solution into a trough, controlling the thickness of the film to be 0.2mm by using a feeler gauge, scraping the casting solution on polyester non-woven fabric into a film by using a scraper, immediately immersing the film into a pure water bath at 25 ℃ for phase conversion to form the film, immersing the prepared film into the pure water bath for more than 24 hours to remove redundant organic solvent, and finally preparing the heat-resistant filter membrane, wherein the surface and the section appearance of the heat-resistant filter membrane are shown in figure 1.
The pure water flux of the heat-resistant filter membrane is 339L/(m) under the pressure of 0.1MPa2H), the pure water flux recovery rate after the heat treatment (heating at 60 ℃ for 2min) is 85.8% (as shown in FIG. 2, which is far superior to that of the ordinary PES filter membrane), wherein the pure water flux and the pure water flux recovery rate are calculated according to the following formulas:
in the formula: j. the design is a squarewIs pure water flux with the unit of L/(m)2H); v is the volume of the permeate, in units of L; a is the effective test area of the filter membrane, and the unit is m2(ii) a Δ t is the duration of the sampling in units of h.
In the formula: FRR is pure water flux recovery rate; j. the design is a squarew1Is the initial pure water flux in L/(m)2·h)；Jw2The pure water flux after heat treatment is expressed in L/(m)2·h)。
Under the protection of nitrogen, the heat-resistant filter membrane and the common PES filter membrane are respectively heated at the speed of 10 ℃ per minute within the temperature range of 40-800 ℃, and the thermogravimetric analysis result is shown in FIG. 3. As can be seen from FIG. 3, the mass reduction in the temperature range of 400-750 ℃ is mainly due to the degradation of the polymer, and the slight right shift of the thermogravimetric curve indicates that the addition of the graphite-like phase carbon nitride can improve the thermal stability of the polyethersulfone-based film.
Example 2: and (3) preparing a heat-resistant filter membrane.
(1) Preparing graphite-like phase carbon nitride powder:
putting melamine powder (5g) into an alumina crucible with a cover, covering the crucible cover, putting the crucible into a muffle furnace, heating to 520 ℃ and keeping the temperature for 2h, then heating to 550 ℃ at the speed of 12 ℃/min and keeping the temperature for 2h, stopping heating, naturally cooling the crucible to room temperature, and finally grinding the yellow blocky solid into faint yellow graphite-phase carbon nitride powder (0.25g) by using an agate mortar.
(2) Modification of graphite-like phase carbon nitride powder:
placing the graphite-like phase carbon nitride powder (0.25g) obtained in step (1) in a strong mixed acid (5mL, V)Nitric acid:VSulfuric acid1:3), the mixture was magnetically stirred overnight, centrifuged at 7000rpm using a centrifuge, and the resulting solid powder was washed with deionized water until neutral, and then dried in an oven at 70 ℃ overnight to give a modified graphite-like phase carbon nitride powder (0.2 g).
(3) Preparing a casting solution:
adding the modified graphite-like phase carbon nitride powder (0.2g) obtained in the step (2) into N, N-dimethylformamide (79.8g), performing ultrasonic treatment for 30min to disperse the modified graphite-like phase carbon nitride powder, adding polyether sulfone (20g), performing magnetic stirring to disperse the modified graphite-like phase carbon nitride powder, placing the mixture into an oven at 70 ℃ to dissolve solids, and sealing, standing and defoaming to obtain a casting solution (100 g).
(4) Phase inversion film formation:
pouring a certain amount of casting solution into a trough, controlling the thickness of the film to be 0.2mm by using a feeler gauge, scraping the casting solution on polyester non-woven fabric into a film by using a scraper, immediately immersing the film into a pure water bath at 25 ℃ for phase conversion to form the film after the scraping is finished, and immersing the prepared film into the pure water bath for more than 24 hours to remove redundant organic solvent, thus finally obtaining the heat-resistant filter membrane.
Example 3: and (3) preparing a heat-resistant filter membrane.
(1) Preparing graphite-like phase carbon nitride powder:
putting melamine powder (5g) into an alumina crucible with a cover, covering the crucible, putting the crucible into a muffle furnace, heating to 550 ℃, keeping the temperature for 3h, then heating to 570 ℃ at the speed of 15 ℃/min, keeping the temperature for 3h, stopping heating, naturally cooling the crucible to room temperature, and finally grinding the yellow blocky solid into faint yellow graphite-phase carbon nitride powder (0.4g) by using an agate mortar.
(2) Modification of graphite-like phase carbon nitride powder:
placing the graphite-like phase carbon nitride powder (0.4g) obtained in the step (1) in a strong mixed acid (16mL, V)Nitric acid:VSulfuric acid1:3), the mixture was centrifuged at 8000rpm using a centrifuge with magnetic stirring overnight, and the resulting solid powder was washed with deionized water until neutral, and then dried in an oven at 80 ℃ overnight to give a modified graphite-like phase carbon nitride powder (0.3 g).
(3) Preparing a casting solution:
adding the modified graphite-like phase carbon nitride powder (0.3g) obtained in the step (2) into N, N-dimethylformamide (79.7g), performing ultrasonic treatment for 30min to disperse the modified graphite-like phase carbon nitride powder, adding polyether sulfone (20g), performing magnetic stirring to disperse the modified graphite-like phase carbon nitride powder, placing the mixture into an oven at 80 ℃ to dissolve solids, and sealing, standing and defoaming to obtain a casting solution (100 g).
(4) Phase inversion film formation:
pouring a certain amount of casting solution into a trough, controlling the thickness of the film to be 0.2mm by using a feeler gauge, scraping the casting solution on polyester non-woven fabric into a film by using a scraper, immediately immersing the film into a pure water bath at 25 ℃ for phase conversion to form the film after the scraping is finished, and immersing the prepared film into the pure water bath for more than 24 hours to remove redundant organic solvent, thus finally obtaining the heat-resistant filter membrane.
Claims (8)
1. The preparation method of the heat-resistant filter membrane is characterized by comprising the following steps of:
1) modification of graphite-like phase carbon nitride powder:
under the stirring condition, uniformly mixing graphite-like phase carbon nitride powder and strong acid according to the dosage proportion of 1g of strong acid to 20-40 mL, centrifuging, washing with water, and drying to obtain modified graphite-like phase carbon nitride powder;
the strong acid in the step 1) is nitric acid, sulfuric acid or a mixture of the nitric acid and the sulfuric acid;
2) preparing a casting solution:
mixing the modified graphite-like carbon nitride powder obtained in the step 1) with an organic solvent, performing ultrasonic dispersion uniformly, adding a base film macromolecular compound into the solution under the stirring condition, heating for dissolving, and then sealing, standing and defoaming to obtain a casting solution; wherein: the mass fraction of the modified graphite-like carbon nitride powder is 0.05-1.2%, and the mass fraction of the basal membrane macromolecular compound is 10-25%;
the organic solvent in the step 2) is N, N-dimethylformamide;
3) phase inversion film formation:
scraping the casting solution obtained in the step 2) into a film on a supporting layer by using a scraper, immediately immersing the film into a pure water bath at 25 ℃ after scraping to perform phase conversion film formation, and then immersing the prepared film into the pure water bath for more than 24 hours to remove the organic solvent, thereby finally obtaining the heat-resistant filter membrane.
2. The method of claim 1, wherein:
the graphite-like phase carbon nitride powder in the step 1) is prepared by the following method: heating the melamine powder to 500-550 ℃, keeping the temperature for 2-3 hours, then heating to 520-570 ℃ at the speed of 10-15 ℃/min, keeping the temperature for 2-3 hours, stopping heating, naturally cooling to room temperature, and grinding to obtain the graphite-like phase carbon nitride powder.
3. The method of claim 1, wherein:
the rotating speed of the centrifugation in the step 1) is 6000-8000 rpm, the washing is completed by deionized water, and the drying temperature is 60-80 ℃.
4. The method of claim 1, wherein:
the base film high molecular compound in the step 2) is polyether sulfone.
5. The method of claim 1, wherein:
the supporting layer in the step 3) is non-woven fabric.
6. The method of claim 1, wherein:
the thickness of the film in step 3) is controlled by a feeler gauge.
7. A heat-resistant filter membrane produced by the production method according to any one of claims 1 to 6.
8. Use of a heat resistant filter membrane according to claim 7 in water treatment of high temperature wastewater.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710127327.9A CN106861451B (en) | 2017-03-06 | 2017-03-06 | Heat-resistant filter membrane and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710127327.9A CN106861451B (en) | 2017-03-06 | 2017-03-06 | Heat-resistant filter membrane and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106861451A CN106861451A (en) | 2017-06-20 |
| CN106861451B true CN106861451B (en) | 2020-02-14 |
Family
ID=59170508
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710127327.9A Active CN106861451B (en) | 2017-03-06 | 2017-03-06 | Heat-resistant filter membrane and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106861451B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109775798A (en) * | 2017-11-15 | 2019-05-21 | 天津淼宇科技发展有限公司 | Water purification method integrating photocatalysis and membrane filtration |
| CN109529638A (en) * | 2018-12-25 | 2019-03-29 | 武汉艾科滤膜技术有限公司 | A kind of high temperature resistant precision molecular cut off ultrafiltration membrane and preparation method thereof |
| CN113932950A (en) * | 2021-10-13 | 2022-01-14 | 中国科学院苏州纳米技术与纳米仿生研究所 | Flexible pressure sensor and manufacturing method thereof |
| CN114870654A (en) * | 2022-05-09 | 2022-08-09 | 广东工业大学 | Nano modified carbon sheet-based ultrafiltration membrane material and preparation method and application thereof |
| CN117225216B (en) * | 2023-08-10 | 2024-05-03 | 浙江大学 | Temperature-resistant thin-layer composite separation membrane and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103977718A (en) * | 2014-06-06 | 2014-08-13 | 中国科学技术大学 | High-water-flux forward-osmosis composite membrane and preparation method thereof |
| CN104772043A (en) * | 2015-04-07 | 2015-07-15 | 天津大学 | Sodium alginate-graphite phase carbon nitride nano-sheet hybridized composite membrane as well as preparation and application of composite membrane |
| CN105800953A (en) * | 2016-03-21 | 2016-07-27 | 中国科学院生态环境研究中心 | Visible-light response carbon @ graphite phase carbon nitride film electrode and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6214028B2 (en) * | 2013-04-05 | 2017-10-18 | 国立大学法人北海道大学 | Method for producing graphene oxide-containing liquid and use thereof |
| CN106215720B (en) * | 2016-04-18 | 2021-08-03 | 中国海洋大学 | Preparation method of graphene quantum dot doped organic solvent resistant ultrafiltration membrane, prepared ultrafiltration membrane and application of ultrafiltration membrane |
-
2017
- 2017-03-06 CN CN201710127327.9A patent/CN106861451B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103977718A (en) * | 2014-06-06 | 2014-08-13 | 中国科学技术大学 | High-water-flux forward-osmosis composite membrane and preparation method thereof |
| CN104772043A (en) * | 2015-04-07 | 2015-07-15 | 天津大学 | Sodium alginate-graphite phase carbon nitride nano-sheet hybridized composite membrane as well as preparation and application of composite membrane |
| CN105800953A (en) * | 2016-03-21 | 2016-07-27 | 中国科学院生态环境研究中心 | Visible-light response carbon @ graphite phase carbon nitride film electrode and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106861451A (en) | 2017-06-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106861451B (en) | Heat-resistant filter membrane and preparation method and application thereof | |
| CN106823863B (en) | Metal organic framework hybridized film, preparation method and application | |
| CN107029562B (en) | MXene-based composite nanofiltration membrane and preparation method thereof | |
| CN107344074B (en) | Preparation method of high-flux solvent-resistant organic/inorganic hybrid composite membrane doped with aminated graphene quantum dots | |
| CN105601317B (en) | A kind of SiCN aeroges and preparation method thereof | |
| CN103861480B (en) | The preparation method of a kind of hydrophilic polyvinylidene fluoride flat sheet membrane and hollow-fibre membrane | |
| CN107349787B (en) | Preparation method of forward osmosis membrane added with aminated graphene quantum dots, prepared forward osmosis membrane and application of forward osmosis membrane | |
| CN110559884B (en) | MIL-101@ PIM-1 composite pervaporation membrane and preparation method and application thereof | |
| WO2021248896A1 (en) | Preparation method for titania ceramic ultrafiltration membrane | |
| CN110935335A (en) | High-hydrophilicity polymer hybrid membrane and preparation method thereof | |
| JP6088932B2 (en) | Separation membrane comprising inorganic / organic hybrid compound and method for producing the same | |
| CN110559888B (en) | Amphipathic graphene oxide modified ultrathin composite nanofiltration membrane as well as preparation method and application thereof | |
| CN110559889A (en) | Hollow nano-particle composite nanofiltration membrane and preparation method and application thereof | |
| Rekik et al. | Development of an asymmetric ultrafiltration membrane from naturally occurring kaolin clays: Application for the cuttlefish effluents treatment | |
| Qin et al. | Formation kinetics of a polyphthalazine ether sulfone ketone membrane via phase inversion | |
| CN104785123A (en) | Hollow fiber ceramic membrane production method | |
| CN108310976B (en) | Preparation method of high-flux nano composite seawater desalination membrane | |
| CN105771704A (en) | Preparation method of novel anti-pollution high-selectivity sulfonated polysulfone nanofiltration membrane | |
| CN107871817A (en) | A kind of method for synthesizing organic inorganic hybridization perovskite crystallite | |
| CN115814617A (en) | Application of phytic acid-nitrogen doped carbon quantum dot composite as aqueous phase monomer in preparation of polyamide nanofiltration membrane | |
| CN104529411B (en) | A kind of microporous membrane and preparation method thereof | |
| CN108905626B (en) | Composite ultrafiltration membrane and preparation method and application thereof | |
| CN104785122A (en) | Polyether sulfone-nanocarbon combined gas separation membrane and preparation method thereof | |
| CN113797771B (en) | Graphene oxide-titanium dioxide-silver doped piperazine polyamide composite nanofiltration membrane and preparation method thereof | |
| CN101766958A (en) | Method for preparing porous membrane with intestine imitating structure |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20240219 Address after: 213000, No. 90 Gangqu Middle Road, Chunjiang Street, Xinbei District, Changzhou City, Jiangsu Province Patentee after: Pengtos (Changzhou) New Materials Technology Co.,Ltd. Country or region after: China Address before: 213001 No. 1801 Wu Cheng Road, Changzhou, Jiangsu Patentee before: JIANGSU University OF TECHNOLOGY Country or region before: China |
|
| TR01 | Transfer of patent right |