CN106861451A - A kind of heat resistant type filter membrane and its preparation method and application - Google Patents
A kind of heat resistant type filter membrane and its preparation method and application Download PDFInfo
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- CN106861451A CN106861451A CN201710127327.9A CN201710127327A CN106861451A CN 106861451 A CN106861451 A CN 106861451A CN 201710127327 A CN201710127327 A CN 201710127327A CN 106861451 A CN106861451 A CN 106861451A
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- 239000012528 membrane Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 42
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 37
- 239000010439 graphite Substances 0.000 claims abstract description 37
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000005266 casting Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 13
- 230000004048 modification Effects 0.000 claims abstract description 13
- 238000012986 modification Methods 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 8
- 239000002351 wastewater Substances 0.000 claims abstract description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 239000004695 Polyether sulfone Substances 0.000 claims description 11
- 210000002469 basement membrane Anatomy 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- 229920006393 polyether sulfone Polymers 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229920002521 macromolecule Polymers 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 239000004745 nonwoven fabric Substances 0.000 claims description 6
- 238000007654 immersion 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
- 238000010792 warming Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims 3
- 238000001035 drying Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 43
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 230000004907 flux Effects 0.000 description 10
- 239000007787 solid Substances 0.000 description 9
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 210000004379 membrane Anatomy 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 239000000428 dust Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 150000007513 acids Chemical class 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
- 230000008859 change Effects 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 238000001728 nano-filtration Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000012695 Interfacial polymerization Methods 0.000 description 2
- 229920012266 Poly(ether sulfone) PES Polymers 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 229920002301 cellulose acetate Polymers 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
- 238000011160 research Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012876 topography Methods 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
- B01D69/02—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 kind of heat resistant type filter membrane and its preparation method and application.Specifically, the preparation method comprises the following steps：1) modification of class graphite phase carbon nitride powder；2) preparation of casting solution；3) inversion of phases film forming.The preparation method process is simple, easy to operate, high degree of automation, raw material are easy to get, and easily realize industrialized production.The surface of the heat resistant type filter membrane prepared using the method is smooth, has no that obvious nano material is reunited, and the water process of hot waste water can be applied to as filter membrane material.
Description
Technical field
The invention belongs to technical field of membrane separation, it is related to a kind of heat resistant type filter membrane, its preparation method, and its in hot waste water
Water process in application.
Background technology
Membrane separation technique is a kind of new isolation technics, and recent decades quickly grow, in water process, chemical industry, life
It is used widely in the fields such as thing, medicine, food.Polyether sulfone (PES), polysulfones (PS), Kynoar (PVDF), polyacrylonitrile
(PAN), the organic polymer such as cellulose acetate (CA) has excellent dissolubility, thermoplasticity and mechanical performance and extensive because of it
As basal lamina material.However, used as the maximum shortcoming of organic film, the problem of heat endurance difference also result in the extensive of professional
Concern.
Interfacial polymerization is a kind of typical method for preparing nanofiltration (NF) film and counter-infiltration (RO) film, with condition temperature
The advantages of with, easy control of reaction.In interfacial polymerization process, basement membrane is dipped into water phase and organic phase with definite composition successively
In, the Orqanics Monomer in two-phase reacts in membrane surface, and then forms one layer of ultra-thin selection layer, the final film for preparing
Need to heat certain hour at a certain temperature, to promote the completion of polymerisation.Research shows, the temperature of heat treatment and when
Between will significantly affect the flux and rejection of film.
In recent years, researcher has made a few thing to improve the heat endurance of polymer.Graphene is a kind of single
The two-dimentional carbon structure of atomic layer level thickness, with good mechanical performance, electrically and thermally stability.There are some researches show, by Graphene with
Polymer combination can significantly improve its heat endurance.Class graphite phase carbon nitride (g-C3N4), with the two dimension similar with Graphene
Layer structure.Because it has excellent chemical stability and visible light catalytic performance, therefore obtain extensive concern.But, extremely
The present does not have document report to be introduced into membrane material class graphite phase carbon nitride as heat stabilizer to be used to prepare heat resistant type filter membrane.
The content of the invention
For heat resistant type filter membrane this technical problem, this hair that there is no at present using class graphite phase carbon nitride as heat stabilizer
It is bright to aim to provide a kind of heat resistant type filter membrane and its preparation method and application.
Specifically, the present invention is adopted the following technical scheme that：
A kind of preparation method of heat resistant type filter membrane, it comprises the following steps：
1) modification of class graphite phase carbon nitride powder：
Under agitation, according to class graphite phase carbon nitride powder:Strong acid=1g:The usage ratio of 20~40mL, by class
Graphite phase carbon nitride powder is well mixed with strong acid, through centrifugation, washing, dries, the class graphite phase carbon nitride powder after being modified
End；
2) preparation of casting solution：
By step 1) in class graphite phase carbon nitride powder after the modification that obtains mix with organic solvent, ultrasonic disperse is equal
Even, then under agitation, to basement membrane macromolecular compound is added in solution, closed standing and defoaming, obtains after heating for dissolving
Casting solution；Wherein：The mass fraction of the class graphite phase carbon nitride powder after modification is 0.05%~1.2%, basement membrane producing high-molecular
The mass fraction of compound is 10%~25%；
3) inversion of phases film forming：
Using scraper on the supporting layer by step 2) in the casting solution striking that obtains into film, striking at once will be thin after finishing
Film immerses carries out inversion of phases film forming in 25 DEG C of pure water baths, then will be carried out within more than 24 hours in the immersion pure water bath of obtained film organic molten
The removal of agent, finally gives heat resistant type filter membrane.
In above-mentioned preparation method, step 1) described in class graphite phase carbon nitride powder can both be obtained by commercial sources
, it is also possible to prepared by following method：Melamine powder is heated to 500~550 DEG C (preferably 500 DEG C), and holding 2~
3 hours (preferably 2 hours), are then warming up to 520~570 DEG C (preferably with the speed of 10~15 DEG C/min (preferably 10 DEG C/min)
520 DEG C), and keep 2~3 hours (preferably 2 hours), after stopping heating, naturally cooling to room temperature, class graphite-phase is obtained after grinding
Nitridation carbon dust.
In above-mentioned preparation method, step 1) described in strong acid be nitric acid, sulfuric acid or the mixture of the two, preferably the two
Mixture, more preferably nitric acid are 1 with the volume ratio of sulfuric acid:3 mixture.
In above-mentioned preparation method, step 1) described in the usage ratio of class graphite phase carbon nitride and the strong acid be 1g:
30mL。
In above-mentioned preparation method, step 1) described in the rotating speed that is centrifuged be 6000~8000rpm (preferably 6000rpm).
In above-mentioned preparation method, step 1) described in wash using deionized water and complete.
In above-mentioned preparation method, step 1) described in dry temperature be 60~80 DEG C (preferably 60 DEG C).
In above-mentioned preparation method, step 2) described in organic solvent be DMF (DMF).
In above-mentioned preparation method, step 2) described in basement membrane macromolecular compound be polyether sulfone (PES).
In above-mentioned preparation method, step 2) described in modify in casting solution after class graphite phase carbon nitride powder quality
Fraction is 0.25%, and the mass fraction of basement membrane macromolecular compound is 20%.
In above-mentioned preparation method, step 3) described in supporting layer be non-woven fabrics (preferably polyester non-woven fabric).
In above-mentioned preparation method, step 3) described in the thickness of film controlled by clearance gauge.
A kind of heat resistant type filter membrane, it is obtained by above-mentioned preparation method.
In hot waste water, (preferably food or medical industry are produced above-mentioned heat resistant type filter membrane (as milipore filter or NF membrane)
Hot waste water) water process in application.
The preparation method process is simple of heat resistant type filter membrane, easy to operate, high degree of automation, raw material are easy to get in the present invention,
Easily realize industrialized production.The surface of the heat resistant type filter membrane prepared using the above method is smooth, has no obvious nanometer
Material is reunited.To addition class graphite phase carbon nitride (g-C in basement membrane macromolecular material3N4) film surface hydrophilicity can be improved and broken
Pore structure, improves the pure water flux recovery rate of film on the premise of not expendable film cutoff performance, and shows good heat
Stability.
Brief description of the drawings
Fig. 1 is surface and the cross-section morphology figure of obtained heat resistant type filter membrane in embodiment 1, wherein (a) is surface topography map,
B () is cross-section morphology figure.
Fig. 2 is that common polyether sulfone filter membrane is receiving the heat treatment of different time with obtained heat resistant type filter membrane in embodiment 1
Front and rear pure water flux recovery rate contrast schematic diagram, wherein PES is common polyether sulfone filter membrane, and M2 is heat resistant type filter membrane.
Fig. 3 is the thermogravimetric analysis figure of common polyether sulfone filter membrane and obtained heat resistant type filter membrane in embodiment 1, and wherein PES is
Common polyether sulfone filter membrane, M2 is heat resistant type filter membrane.
Specific embodiment
Further description is made to the technical scheme in the present invention below in conjunction with the drawings and specific embodiments.Except as otherwise
Illustrate outer, instrument, material, reagent used in the following example etc. can be obtained by routine business means.
Embodiment 1：The preparation and performance test of heat resistant type filter membrane.
(1) preparation of class graphite phase carbon nitride powder：
Melamine powder (5g) is placed in alumina crucible with cover, after covering crucible cover, crucible Muffle is put into
500 DEG C, and keeping temperature 2h are heated in stove, then 520 DEG C is warming up to the speed of 10 DEG C/min, and keep 2h, stop adding
After heat, crucible is naturally cooled to room temperature, yellow blocks of solid is finally ground to form into faint yellow class graphite-phase nitrogen with agate mortar
Change carbon dust (0.3g).
(2) modification of class graphite phase carbon nitride powder：
Class graphite phase carbon nitride powder (0.3g) that will be obtained in step (1) is placed in mixed strong acids (9mL, VNitric acid:VSulfuric acid=1:
3) in, mixture overnight, uses centrifuge to be centrifuged with the rotating speed of 6000rpm, the solid powder for obtaining under magnetic stirring
It is washed with deionized until neutrality, is then dried overnight, the class graphite phase carbon nitride powder after being modified in 60 DEG C of baking ovens
Last (0.25g).
(3) preparation of casting solution：
Class graphite phase carbon nitride powder (0.25g) after the modification that will be obtained in step (2) is added to N, N- dimethyl methyls
In acid amides (79.75g), ultrasonic 30min disperses it, adds polyether sulfone (20g), disperses it by magnetic agitation, by this
Mixture is placed in 60 DEG C of baking ovens, to make solid dissolving, casting solution (100g) is obtained after closed standing and defoaming.
(4) inversion of phases film forming：
A certain amount of casting solution is poured into hopper, it is 0.2mm to control the thickness of film using clearance gauge, using scraper poly-
By casting solution striking into film on ester non-woven fabrics, striking finish after at once will film immerse carried out in the bath of 25 DEG C of pure water inversion of phases into
Film, then by more than 24h in the immersion pure water bath of obtained film, to remove unnecessary organic solvent, heat resistant type filter membrane is finally obtained, its
Surface and cross-section morphology are as shown in Figure 1.
Under 0.1MPa pressure, the pure water flux of the heat resistant type filter membrane is 339L/ (m2H), by heating (60 DEG C
Heating 2min) after, pure water flux recovery rate is 85.8% (as shown in Fig. 2 far superior to common PE S filter membrane), and wherein pure water leads to
The computing formula of amount and pure water flux recovery rate is as follows：
In formula：JwIt is pure water flux, unit is L/ (m2·h)；V is the volume of permeate, and unit is L；A has for filter membrane
Effect test area, unit is m2；Δ t is the duration of sampling, and unit is h.
In formula：FRR is pure water flux recovery rate；Jw1It is initial pure water flux, unit is L/ (m2·h)；Jw2It is heating
Pure water flux after treatment, unit is L/ (m2·h)。
Under nitrogen protection, in 40~800 DEG C of temperature ranges, the heat resistant type is filtered respectively with 10 DEG C per minute of speed
Film and common PE S filter membranes are heated, and its thermal gravimetric analysis results is as shown in Figure 3.From the figure 3, it may be seen that in 400~750 DEG C of temperature
Quality reduction in the range of degree is mainly due to the degraded of polymer, and the small of thermogravimetric curve moves to right, and shows class graphite-phase nitrogen
Changing the addition of carbon can improve the heat endurance of polyether sulfone basement membrane.
Embodiment 2：The preparation of heat resistant type filter membrane.
(1) preparation of class graphite phase carbon nitride powder：
Melamine powder (5g) is placed in alumina crucible with cover, after covering crucible cover, crucible Muffle is put into
520 DEG C, and keeping temperature 2h are heated in stove, then 550 DEG C is warming up to the speed of 12 DEG C/min, and keep 2h, stop adding
After heat, crucible is naturally cooled to room temperature, yellow blocks of solid is finally ground to form into faint yellow class graphite-phase nitrogen with agate mortar
Change carbon dust (0.25g).
(2) modification of class graphite phase carbon nitride powder：
Class graphite phase carbon nitride powder (0.25g) that will be obtained in step (1) is placed in mixed strong acids (5mL, VNitric acid:VSulfuric acid=
1:3) in, mixture overnight, uses centrifuge to be centrifuged with the rotating speed of 7000rpm under magnetic stirring, the solid powder for obtaining
End is washed with deionized until neutrality, is then dried overnight, the class graphite phase carbon nitride after being modified in 70 DEG C of baking ovens
Powder (0.2g).
(3) preparation of casting solution：
Class graphite phase carbon nitride powder (0.2g) after the modification that will be obtained in step (2) is added to N, N- dimethyl formyls
In amine (79.8g), ultrasonic 30min disperses it, adds polyether sulfone (20g), and it is disperseed by magnetic agitation, and this is mixed
Thing is placed in 70 DEG C of baking ovens, to make solid dissolving, casting solution (100g) is obtained after closed standing and defoaming.
(4) inversion of phases film forming：
A certain amount of casting solution is poured into hopper, it is 0.2mm to control the thickness of film using clearance gauge, using scraper poly-
By casting solution striking into film on ester non-woven fabrics, striking finish after at once will film immerse carried out in the bath of 25 DEG C of pure water inversion of phases into
Film, then by more than 24h in the immersion pure water bath of obtained film, to remove unnecessary organic solvent, heat resistant type filter membrane is finally obtained.
Embodiment 3：The preparation of heat resistant type filter membrane.
(1) preparation of class graphite phase carbon nitride powder：
Melamine powder (5g) is placed in alumina crucible with cover, after covering crucible cover, crucible Muffle is put into
550 DEG C, and keeping temperature 3h are heated in stove, then 570 DEG C is warming up to the speed of 15 DEG C/min, and keep 3h, stop adding
After heat, crucible is naturally cooled to room temperature, yellow blocks of solid is finally ground to form into faint yellow class graphite-phase nitrogen with agate mortar
Change carbon dust (0.4g).
(2) modification of class graphite phase carbon nitride powder：
Class graphite phase carbon nitride powder (0.4g) that will be obtained in step (1) is placed in mixed strong acids (16mL, VNitric acid:VSulfuric acid=
1:3) in, mixture overnight, uses centrifuge to be centrifuged with the rotating speed of 8000rpm under magnetic stirring, the solid powder for obtaining
End is washed with deionized until neutrality, is then dried overnight, the class graphite phase carbon nitride after being modified in 80 DEG C of baking ovens
Powder (0.3g).
(3) preparation of casting solution：
Class graphite phase carbon nitride powder (0.3g) after the modification that will be obtained in step (2) is added to N, N- dimethyl formyls
In amine (79.7g), ultrasonic 30min disperses it, adds polyether sulfone (20g), and it is disperseed by magnetic agitation, and this is mixed
Thing is placed in 80 DEG C of baking ovens, to make solid dissolving, casting solution (100g) is obtained after closed standing and defoaming.
(4) inversion of phases film forming：
A certain amount of casting solution is poured into hopper, it is 0.2mm to control the thickness of film using clearance gauge, using scraper poly-
By casting solution striking into film on ester non-woven fabrics, striking finish after at once will film immerse carried out in the bath of 25 DEG C of pure water inversion of phases into
Film, then by more than 24h in the immersion pure water bath of obtained film, to remove unnecessary organic solvent, heat resistant type filter membrane is finally obtained.
Claims (10)
1. a kind of preparation method of heat resistant type filter membrane, it comprises the following steps：
1) modification of class graphite phase carbon nitride powder：
Under agitation, according to class graphite phase carbon nitride powder:Strong acid=1g:The usage ratio of 20~40mL, by class graphite
Phase carbon nitride powder is well mixed with strong acid, through centrifugation, washing, dries, the class graphite phase carbon nitride powder after being modified；
2) preparation of casting solution：
By step 1) in class graphite phase carbon nitride powder after the modification that obtains mix with organic solvent, ultrasonic disperse is uniform, so
Afterwards under agitation, to basement membrane macromolecular compound is added in solution, closed standing and defoaming, obtains casting film after heating for dissolving
Liquid；Wherein：The mass fraction of the class graphite phase carbon nitride powder after modification is 0.05%~1.2%, basement membrane macromolecular compound
Mass fraction be 10%~25%；
3) inversion of phases film forming：
Using scraper on the supporting layer by step 2) in the casting solution striking that obtains into film, striking at once soaks film after finishing
Entering during 25 DEG C of pure water are bathed carries out inversion of phases film forming, then will carry out organic solvent within more than 24 hours in the immersion pure water bath of obtained film
Removal, finally gives heat resistant type filter membrane.
2. preparation method according to claim 1, it is characterised in that：
Step 1) described in class graphite phase carbon nitride powder prepared by following method：Melamine powder is heated to 500~
550 DEG C, and kept for 2~3 hours, 520~570 DEG C then are warming up to the speed of 10~15 DEG C/min, and kept for 2~3 hours,
After stopping heating, room temperature is naturally cooled to, class graphite phase carbon nitride powder is obtained after grinding.
3. preparation method according to claim 1, it is characterised in that：
Step 1) described in strong acid be nitric acid, sulfuric acid or the mixture of the two.
4. preparation method according to claim 1, it is characterised in that：
Step 1) described in the rotating speed that is centrifuged be 6000~8000rpm, the washing completed using deionized water, the drying
Temperature be 60~80 DEG C.
5. preparation method according to claim 1, it is characterised in that：
Step 2) described in organic solvent be N,N-dimethylformamide.
6. preparation method according to claim 1, it is characterised in that：
Step 2) described in basement membrane macromolecular compound be polyether sulfone.
7. preparation method according to claim 1, it is characterised in that：
Step 3) described in supporting layer be non-woven fabrics.
8. preparation method according to claim 1, it is characterised in that：
Step 3) described in the thickness of film controlled by clearance gauge.
9. a kind of heat resistant type filter membrane, it is obtained by preparation method according to any one of claim 1 to 8.
10. application of the heat resistant type filter membrane according to claim 9 in the water process of hot waste water.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710127327.9A CN106861451B (en) | 2017-03-06 | 2017-03-06 | Heat-resistant filter membrane and preparation method and application thereof |
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| 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 |
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| Publication Number | Publication Date |
|---|---|
| CN106861451A true CN106861451A (en) | 2017-06-20 |
| CN106861451B CN106861451B (en) | 2020-02-14 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| 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 |
| CN117225216A (en) * | 2023-08-10 | 2023-12-15 | 浙江大学 | Temperature-resistant thin-layer composite separation membrane and preparation method and application thereof |
Citations (5)
| 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 |
| JP2014201492A (en) * | 2013-04-05 | 2014-10-27 | 国立大学法人北海道大学 | Method for manufacturing a graphene oxide-containing liquid and uses of the same |
| 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 |
| CN106215720A (en) * | 2016-04-18 | 2016-12-14 | 中国海洋大学 | Preparation method, prepared ultrafilter membrane and the application of this ultrafilter membrane of a kind of doped graphene quantum dot organic solvent-resistant ultrafilter membrane |
-
2017
- 2017-03-06 CN CN201710127327.9A patent/CN106861451B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014201492A (en) * | 2013-04-05 | 2014-10-27 | 国立大学法人北海道大学 | Method for manufacturing a graphene oxide-containing liquid and uses of the same |
| 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 |
| CN106215720A (en) * | 2016-04-18 | 2016-12-14 | 中国海洋大学 | Preparation method, prepared ultrafilter membrane and the application of this ultrafilter membrane of a kind of doped graphene quantum dot organic solvent-resistant ultrafilter membrane |
Cited By (6)
| 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 |
| CN117225216A (en) * | 2023-08-10 | 2023-12-15 | 浙江大学 | Temperature-resistant thin-layer composite separation membrane 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 |
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