CN107149883A - A kind of graphene modified PVDF hollow fiber ultrafilter membrane and preparation method - Google Patents
A kind of graphene modified PVDF hollow fiber ultrafilter membrane and preparation method Download PDFInfo
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- CN107149883A CN107149883A CN201710538596.4A CN201710538596A CN107149883A CN 107149883 A CN107149883 A CN 107149883A CN 201710538596 A CN201710538596 A CN 201710538596A CN 107149883 A CN107149883 A CN 107149883A
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- hollow fiber
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Abstract
The invention discloses a kind of graphene modified PVDF hollow fiber ultrafilter membrane and preparation method, milipore filter is made up of the system of following mass ratio：Kynoar 20~45%, graphene 0.01~1%, graphite powder 1~5%, iron powder 0~1%, composite coupler 0.02~0.5%, hydrophilizing agent 1~25%, diluent 30~70%, pore former 2~20%.The overall preparation method of milipore filter is：Graphene and graphite powder premixing, microwave drying；Add composite coupler, iron powder, Kynoar, mixed at high speed；Add other raw materials and be fabricated to film material；Milipore filter is prepared using thermic phase method.The present invention utilizes graphene or its property formed with iron powder, the milipore filter with functions such as catalysis, microelectrode, antibacterials is produced, when applied to sewage disposal, there is filtration, the oxidative degradation of pollutant is can speed up again, so as to greatly improve sewage treating efficiency and stain resistance.
Description
Technical field
The present invention relates to a kind of hollow fiber ultrafiltration membrane and preparation method, more particularly to a kind of graphene modified polyvinilidene fluorine second
Alkene hollow fiber ultrafiltration membrane and preparation method, belong to technical field of membrane.
Background technology
Hollow fiber ultrafiltration membrane technique is a kind of purification for being widely used in water, and solution is separated, concentration, and is carried from waste water
Utility is taken, purification of waste water recycles the new and high technology in field.The current preferable hollow fiber ultrafiltration membrane of industrialization prepares skill
Art is mainly solution spinning, melt spinning pulling method and thermally induced phase separation.Wherein, solution spinning is due to needing to use
Substantial amounts of solvent (account for film forming system more than 80%) to solvent, it is necessary to be reclaimed, separated and recycled, it is easy to be caused
Environmental pollution simultaneously deteriorates working condition, therefore development is restricted；Melt spinning pulling method is not required to molten compared with solution spinning
Agent and its removal process, technique is relatively simple, production efficiency is higher, but because its drilling process is to as-spun fibre aggregated structure
Requirement it is more harsh, exist spinning, post-tensioning stretching process and tunica fibrosa microcellular structure control difficulty it is larger the problem of；Thermic
Phase separation method is to control different polymeric systems to be separated by changing system temperature, so as to reach to form microcellular structure
Purpose, the method has the advantages that tunica fibrosa micropore size is smaller, mechanical property is strong compared with the former two, it has also become from theory to
The focus of study on the industrialization.But in the existing discussion that hollow fiber ultrafiltration membrane is prepared to thermally induced phase separation, most of scientific research people
Research emphasis has been placed on the filter effect and mechanical strength for how improving milipore filter by member, is also rarely had at present to urging
The report of the graphene modified PVDF hollow fiber ultrafilter membrane of change, microelectrode and antibacterial action.
The content of the invention
In order to solve the weak point present in above-mentioned technology, the invention provides a kind of graphene modified polyvinilidene fluoride
Hollow fiber ultrafiltration membrane and preparation method.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of graphene modified polyvinilidene fluoride
Hollow fiber ultrafiltration membrane, is made up of the film forming system of following mass ratio：
Wherein, composite coupler is by waiting the silane coupler and titanate coupling agent of mass ratio to mix.
Hydrophilizing agent is polyvinylpyrrolidone or polyethylene glycol.
Diluent is dibutyl phthalate, dioctyl phthalate, paraxylene, tributyl phosphate, tetrahydrochysene furan
One or more combinations in muttering.
Pore former is sodium chloride or lithium chloride or calcium chloride or calcium carbonate.
Graphite powder, iron powder are nanoscale.
A kind of preparation method of graphene modified PVDF hollow fiber ultrafilter membrane, is concretely comprised the following steps：
By 0.01~1% graphene with 1~5% graphite powder premix merges microwave drying, then addition 0.02~
0.5% composite coupler, 0~1% iron powder, 20~45% Kynoar, mixed at high speed；
Sequentially added into the dispensing after above-mentioned mixed at high speed 1~25% hydrophilizing agent, 2~20% pore former, 30
~70% diluent, it is well mixed to be fabricated to film material；
Film material is poured onto in 200~400 DEG C of twin-screw extrusion forming machine, it is heated to molten condition；Melting
Film material afterwards is cooled to hollow fiber conduit after being extruded through hollow-fibre membrane die orifice；
Compressed air or higher boiling non-solvent are passed through into hollow fiber conduit as core liquid, then hollow fiber conduit is sent into
In gas phase or liquid phase separation groove, the diluent being film-made in material, pore former are separated, graphene modified polyvinilidene fluoride is obtained
Hollow fiber ultrafiltration membrane.
The present invention mainly uses graphene or itself and property-catalysis of iron powder formation, antibacterial, microelectrode, pre-
The milipore filter of property is manufactured that after mixing using thermic phase method.This product when in applied to sewage disposal process,
There is filtration, there is the functions such as catalysis, microelectrode, antibacterial again, the oxidative degradation of pollutant is can speed up, so that
Greatly improve sewage treating efficiency and stain resistance.
Embodiment
With reference to embodiment, the present invention is further detailed explanation.
In the present invention, a kind of graphene modified polyvinilidene fluoride hollow-fibre membrane is passed through by the film forming system of following mass ratio
Prepared after premixing by thermic phase method：
Wherein, composite coupler is by waiting the silane coupler and titanate coupling agent of mass ratio to mix.
Hydrophilizing agent is polyvinylpyrrolidone or polyethylene glycol.
Diluent is high boiling organic diluent, such as dibutyl phthalate, dioctyl phthalate, to diformazan
One or more combinations in benzene, tributyl phosphate, tetrahydrofuran.
Pore former is sodium chloride or the inorganic salts such as lithium chloride or calcium chloride or calcium carbonate.
Graphite powder, iron powder are nanoscale.
A kind of preparation method of graphene modified PVDF hollow fiber ultrafilter membrane, is concretely comprised the following steps：
In order that graphene can be effectively dispersed among Kynoar, and also to reduce cost, first will
0.01~1% graphene merges microwave drying with 1~5% graphite powder premix, then adds 0.02~0.5% compound idol
Join agent, 0~1% iron powder, 20~45% Kynoar, mixed at high speed；
Sequentially added into the dispensing after above-mentioned mixed at high speed 1~25% hydrophilizing agent, 2~20% pore former, 30
~70% diluent, it is well mixed to be fabricated to film material；
Hollow fiber ultrafiltration membrane is prepared using thermic phase method, will be film-made material be poured onto 200~400 DEG C of twin-screw extrusion into
In type machine, it is set to be heated to molten condition；Film material after melting is cooled to doughnut after being extruded through hollow-fibre membrane die orifice
Pipe；
Compressed air or higher boiling non-solvent are passed through into hollow fiber conduit as core liquid, then hollow fiber conduit is sent into
In gas phase or liquid phase separation groove, the diluent being film-made in material, pore former are separated, graphene modified polyvinilidene fluoride is obtained
Hollow fiber ultrafiltration membrane.
This method can be such that graphene is effectively evenly dispersed in Kynoar, will not cause graphene produce reunite and
Failure or reduction effectiveness.
Graphene is added in Kynoar and graphene modified polyvinilidene fluoride doughnut is made by the present invention to be surpassed
Filter membrane so that the film is provided with the functions such as catalysis, antibacterial functions and its microelectrode formed with iron powder of graphene, therefore,
The oxidative degradation for accelerating pollutant can be played in sewage disposal process, and can effectively suppress breeding of the bacterium on film surface,
So as to greatly improve film antifouling property and wastewater treatment efficiency.
Beneficial effects of the present invention are：
1) filtration of milipore filter can be played, while having the functions such as catalysis, microelectrode again, can be promoted dirty in sewage
Contaminate thing oxidative degradation so that greatly improve with wastewater treatment efficiency and speed, with the multi-functional advantage of a film；
2) antibiotic property preferably, can prevent bacterium from being bred on film surface；Antifouling property is good, easy cleaning；
3) hollow fiber ultrafiltration membrane that this formula and method are prepared has stronger tensile strength, not fracture of wire；
4) produced using thermic phase method, therefore the scope of selectable raw material, additive is also very wide, production technology is fitted
Answering property is good, and expansion is stronger.
The whole structure of the present invention is further elaborated below by five specific embodiments.
Embodiment one,
0.2% graphene is merged into microwave drying with 5% graphite powder premix, 0.5% compound coupling is then added
Agent, 0% iron powder, 20% Kynoar, mixed at high speed；
Sequentially added into the dispensing after above-mentioned mixed at high speed 10% hydrophilizing agent, 2% pore former, 30~62.3%
Diluent, it is well mixed to be fabricated to film material；
Film material is poured onto in 200 DEG C of twin-screw extrusion forming machine, it is heated to molten condition；System after melting
Coating materials is cooled to hollow fiber conduit after being extruded through hollow-fibre membrane die orifice；
Compressed air or higher boiling non-solvent are passed through into hollow fiber conduit as core liquid, then hollow fiber conduit is sent into
In gas phase or liquid phase separation groove, the diluent being film-made in material, pore former are separated, graphene modified polyvinilidene fluoride is obtained
Hollow fiber ultrafiltration membrane.
The external diameter of hollow fiber ultrafiltration membrane obtained by the present embodiment is 1.3mm, and internal diameter is 0.6mm, and porosity is 56%, film
It is 0.03 micron to separate aperture, in 0.1MPa, 25 DEG C of test condition (detection normative reference：People's Republic of China's ocean row
Industry standard HY/T112-2008 " milipore filter and its component " requirement) under, pure water water-flowing amount is 720L/m2*hr；For usual
Sanitary sewage disposal normally in operation, influent COD (COD) is 350mg/L, and production water COD is 60mg/L, and COD is removed
Rate is 82.9%.
Embodiment two,
1% graphene is merged into microwave drying with 2% graphite powder premix, 0.15% compound coupling is then added
Agent, 0.5% iron powder, 45% Kynoar, mixed at high speed；
Sequentially added into the dispensing after above-mentioned mixed at high speed 5% hydrophilizing agent, 16.35% pore former, 30%
Diluent, it is well mixed to be fabricated to film material；
Film material is poured onto in 400 DEG C of twin-screw extrusion forming machine, it is heated to molten condition；System after melting
Coating materials is cooled to hollow fiber conduit after being extruded through hollow-fibre membrane die orifice；
Compressed air or higher boiling non-solvent are passed through into hollow fiber conduit as core liquid, then hollow fiber conduit is sent into
In gas phase or liquid phase separation groove, the diluent being film-made in material, pore former are separated, graphene modified polyvinilidene fluoride is obtained
Hollow fiber ultrafiltration membrane.
The external diameter of hollow fiber ultrafiltration membrane obtained by the present embodiment is 1.3mm, and internal diameter is 0.6mm, and porosity is 53%, film
It is 0.05 micron to separate aperture, under 0.1MPa, 25 DEG C of test condition, and pure water water-flowing amount is 700L/m2*hr；For leading to
Normal sanitary sewage disposal is normally in operation, and influent COD (COD) is 350mg/L, and production water COD is 35mg/L, and COD is gone
Except rate is 90%.
Embodiment three,
0.01% graphene is merged into microwave drying with 0.1% graphite powder premix, then addition 0.02% is compound
Coupling agent, 1% iron powder, 21% Kynoar, mixed at high speed；
Sequentially added into the dispensing after above-mentioned mixed at high speed 25% hydrophilizing agent, 20% pore former, 31.97%
Diluent, it is well mixed to be fabricated to film material；
Film material is poured onto in 300 DEG C of twin-screw extrusion forming machine, it is heated to molten condition；System after melting
Coating materials is cooled to hollow fiber conduit after being extruded through hollow-fibre membrane die orifice；
Compressed air or higher boiling non-solvent are passed through into hollow fiber conduit as core liquid, then hollow fiber conduit is sent into
In gas phase or liquid phase separation groove, the diluent being film-made in material, pore former are separated, graphene modified polyvinilidene fluoride is obtained
Hollow fiber ultrafiltration membrane.
The external diameter of hollow fiber ultrafiltration membrane obtained by the present embodiment is 1.3mm, and internal diameter is 0.6mm, and porosity is 71%, film
It is 0.05 micron to separate aperture, under 0.1MPa, 25 DEG C of test condition, and pure water water-flowing amount is 720L/m2*hr；For leading to
Normal sanitary sewage disposal is normally in operation, and influent COD (COD) is 350mg/L, and production water COD is 50mg/L, and COD is gone
Except rate is 85.7%.
Example IV,
0.2% graphene is merged into microwave drying with 1.4% graphite powder premix, 0.3% compound idol is then added
Join agent, 0.1% iron powder, 25% Kynoar, mixed at high speed；
Sequentially added into the dispensing after above-mentioned mixed at high speed 1% hydrophilizing agent, 2% pore former, 70% dilution
Agent, it is well mixed to be fabricated to film material；
Film material is poured onto in 350 DEG C of twin-screw extrusion forming machine, it is heated to molten condition；System after melting
Coating materials is cooled to hollow fiber conduit after being extruded through hollow-fibre membrane die orifice；
Compressed air or higher boiling non-solvent are passed through into hollow fiber conduit as core liquid, then hollow fiber conduit is sent into
In gas phase or liquid phase separation groove, the diluent being film-made in material, pore former are separated, graphene modified polyvinilidene fluoride is obtained
Hollow fiber ultrafiltration membrane.
The external diameter of hollow fiber ultrafiltration membrane obtained by the present embodiment is 1.3mm, and internal diameter is 0.6mm, and porosity is 67%, film
It is 0.05 micron to separate aperture, under 0.1MPa, 25 DEG C of test condition, and pure water water-flowing amount is 680L/m2*hr；For leading to
Normal sanitary sewage disposal is normally in operation, and influent COD (COD) is 350mg/L, and production water COD is 45mg/L, and COD is gone
Except rate is 87.1%.
Embodiment five,
0.5% graphene is merged into microwave drying with 3.5% graphite powder premix, 0.25% compound idol is then added
Join agent, 0.2% iron powder, 30% Kynoar, mixed at high speed；
Sequentially added into the dispensing after above-mentioned mixed at high speed 25% hydrophilizing agent, 5% pore former, 35.55%
Diluent, it is well mixed to be fabricated to film material；
Film material is poured onto in 250 DEG C of twin-screw extrusion forming machine, it is heated to molten condition；System after melting
Coating materials is cooled to hollow fiber conduit after being extruded through hollow-fibre membrane die orifice；
Compressed air or higher boiling non-solvent are passed through into hollow fiber conduit as core liquid, then hollow fiber conduit is sent into
In gas phase or liquid phase separation groove, the diluent being film-made in material, pore former are separated, graphene modified polyvinilidene fluoride is obtained
Hollow fiber ultrafiltration membrane.
The external diameter of hollow fiber ultrafiltration membrane obtained by the present embodiment is 1.3mm, and internal diameter is 0.6mm, and porosity is 67%, film
It is 0.05 micron to separate aperture, under 0.1MPa, 25 DEG C of test condition, and pure water water-flowing amount is 720L/m2*hr；For leading to
Normal sanitary sewage disposal is normally in operation, and influent COD (COD) is 350mg/L, and production water COD is 40mg/L, and COD is gone
Except rate is 83%.
Graphene modified PVDF hollow fiber ultrafilter membrane obtained by above-described embodiment meets the People's Republic of China (PRC)
Ocean professional standard HY/T112-2008 " milipore filter and its component " requirement.
Above-mentioned embodiment is not limitation of the present invention, and the present invention is also not limited to the example above, this technology neck
The variations, modifications, additions or substitutions that the technical staff in domain is made in the range of technical scheme, also belong to this hair
Bright protection domain.
Claims (7)
1. a kind of graphene modified PVDF hollow fiber ultrafilter membrane, it is characterised in that：It by following mass ratio film forming
System is constituted：
2. graphene modified PVDF hollow fiber ultrafilter membrane according to claim 1, it is characterised in that：It is described multiple
Coupling agent is closed by waiting the silane coupler and titanate coupling agent of mass ratio to mix.
3. graphene modified PVDF hollow fiber ultrafilter membrane according to claim 1, it is characterised in that：The parent
Aqua is polyvinylpyrrolidone or polyethylene glycol.
4. graphene modified PVDF hollow fiber ultrafilter membrane according to claim 1, it is characterised in that：It is described dilute
It is one kind in dibutyl phthalate, dioctyl phthalate, paraxylene, tributyl phosphate, tetrahydrofuran to release agent
Or a variety of combinations.
5. graphene modified PVDF hollow fiber ultrafilter membrane according to claim 1, it is characterised in that：It is described into
Hole agent is sodium chloride or lithium chloride or calcium chloride or calcium carbonate.
6. graphene modified PVDF hollow fiber ultrafilter membrane according to claim 1, it is characterised in that：The stone
Ink powder, iron powder are nanoscale.
7. a kind of preparation method of graphene modified PVDF hollow fiber ultrafilter membrane, it is characterised in that：Methods described
Concretely comprise the following steps：
0.01~1% graphene is merged into microwave drying with 1~5% graphite powder premix, 0.02~0.5% is then added
Composite coupler, 0~1% iron powder, 20~45% Kynoar, mixed at high speed；
Sequentially added into the dispensing after above-mentioned mixed at high speed 1~25% hydrophilizing agent, 2~20% pore former, 30~
70% diluent, it is well mixed to be fabricated to film material；
Film material is poured onto in 200~400 DEG C of twin-screw extrusion forming machine, it is heated to molten condition；After melting
Film material is cooled to hollow fiber conduit after being extruded through hollow-fibre membrane die orifice；
Compressed air or higher boiling non-solvent are passed through into hollow fiber conduit as core liquid, hollow fiber conduit is then sent into gas phase
Or in liquid phase separation groove, the diluent being film-made in material, pore former are separated, graphene modified polyvinilidene fluoride is obtained hollow
Fiber ultrafiltration membrane.
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Cited By (3)
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| CN108786495A (en) * | 2018-06-13 | 2018-11-13 | 南通强生石墨烯科技有限公司 | A kind of antibacterial graphene oxide is modified PVDF hollow-fibre membranes and preparation method thereof |
| CN109395591A (en) * | 2018-10-12 | 2019-03-01 | 南京龙源环保有限公司 | A kind of preparation method of reinforced graphite alkene polyvinylidene fluoride microporous film |
| CN113600039A (en) * | 2021-07-23 | 2021-11-05 | 北京中电加美环保科技有限公司 | Polyvinylidene fluoride ultrafiltration membrane and preparation method thereof |
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| CN106492644A (en) * | 2016-11-18 | 2017-03-15 | 北京建筑大学 | A kind of ultrafilter membrane process for purifying water based on microemulsion modified Nano Zero-valent Iron Carbon Materials precoated shet |
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| CN108786495A (en) * | 2018-06-13 | 2018-11-13 | 南通强生石墨烯科技有限公司 | A kind of antibacterial graphene oxide is modified PVDF hollow-fibre membranes and preparation method thereof |
| CN109395591A (en) * | 2018-10-12 | 2019-03-01 | 南京龙源环保有限公司 | A kind of preparation method of reinforced graphite alkene polyvinylidene fluoride microporous film |
| CN113600039A (en) * | 2021-07-23 | 2021-11-05 | 北京中电加美环保科技有限公司 | Polyvinylidene fluoride ultrafiltration membrane and preparation method thereof |
| CN113600039B (en) * | 2021-07-23 | 2022-05-24 | 北京中电加美环保科技有限公司 | Polyvinylidene fluoride ultrafiltration membrane and preparation method thereof |
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