CN106064024B - Polysulfones-graphene oxide hollow-fibre membrane and preparation method thereof - Google Patents
Polysulfones-graphene oxide hollow-fibre membrane and preparation method thereof Download PDFInfo
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- CN106064024B CN106064024B CN201610469322.XA CN201610469322A CN106064024B CN 106064024 B CN106064024 B CN 106064024B CN 201610469322 A CN201610469322 A CN 201610469322A CN 106064024 B CN106064024 B CN 106064024B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/08—Hollow fibre membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/021—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/24—Mechanical properties, e.g. strength
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Abstract
The invention discloses a kind of polysulfones-graphene oxide hollow-fibre membranes and preparation method thereof.The present invention is directed to polysulfones（PSF）The problem of doughnut film properties, introduce graphene oxide, surface modification is carried out to graphene oxide using super critical CO 2 technology, can it is fully dispersed in a polymer matrix, and it is arranged in pairs or groups using specific component, both the toughness of ps hollow fiber uf membrane had been improved, increase the application range of polysulfones base hollow-fibre membrane, under the premise of so that ps hollow fiber uf membrane is kept preferable water flux and rejection again, the comprehensive mechanical performance and antifouling property of ps hollow fiber uf membrane, the more stable doughnut film composite material of forming properties can be improved.
Description
Technical field
The present invention relates to technical field of polymer materials, especially a kind of polysulfones-graphene oxide hollow-fibre membrane and its
Preparation method.
Background technology
Polysulfones is due to its good chemical stability, water resistance, heat resistance, dimensional stability and preferable film forming
And mechanical strength, it has been obtained widely in micro-filtration, reverse osmosis, ultrafiltration, electrodialysis, gas separation, bioengineering, medical treatment etc.
Using being particularly suitable for application to the excellent hemodialysis membrane of processability, polysulfones material is a kind of membrane material for applying very much
Material.But existing ps hollow fiber uf membrane there is also hydrophilies problem not high, easy to pollute, water is handled in practical applications
It is inefficient, while film is easy to be contaminated, and the service life of film is caused to reduce.
Invention content
The purpose of the present invention is：A kind of polysulfones-graphene oxide hollow-fibre membrane and preparation method thereof is provided, it is significantly carried
The hydrophily of PS membrane has been supplied, and has improved mechanical strength and hardness, permeability and resistance tocrocking are also very excellent, to overcome
The deficiencies in the prior art.
The invention is realized in this way：Polysulfones-graphene oxide hollow-fibre membrane, is calculated, including according to the mass fraction with 15-
20 parts of polysulfones, 1.2-1.7 parts of sulfonated polysulfone, 33-37 parts of polyethylene glycol, 42-48 parts of DMAC N,N' dimethyl acetamides and 0.01-1
Part graphene oxide.
The preparation method of polysulfones-graphene oxide hollow-fibre membrane takes each component, by above-mentioned quality by above-mentioned mass fraction
Number takes each component, includes the following steps：
1) polysulfones and sulfonated polysulfone are dried in vacuo 12-24 hours at 65-75 DEG C respectively；
2) processed graphene oxide is added in n,N-dimethylacetamide, then oxidation stone is made by ultrasonic power
Black alkene is dispersed in DMAC N,N' dimethyl acetamide；
3) then be included in it is dry after sulfonated polysulfone, polyethylene glycol and it is dry after polysulfones filled under conditions of 65-75 DEG C
Divide stirring 10-15h, form it into homogeneous casting solution, and carry out vacuum defoamation, then passes through spinneret and form dynamic analysis of spinning, warp
It crosses the air gap between spinneret and coagulating bath to immerse in coagulating bath, passes through solvent n,N-dimethylacetamide and non-solvent water
Mass transfer exchange and form hollow-fibre membrane.
Air gap length between the spinneret and coagulating bath is 1-5cm, and the temperature of the air gap is 20-50
DEG C, humidity 50-80%.The temperature and humidity for ensureing the air gap, exclude the influence of environment.Control the warm and humid of the air gap
Degree, being capable of effective solution environment temperature and influence of the humidity to hollow fiber film structure and performance.
The graphene oxide by graphene oxide, modifying agent and cosolvent before use, be first put into overcritical dioxy
Change in carbon reaction kettle, carries out, reacted under conditions of reaction temperature is 40 DEG C, reaction pressure >=20MPa, reaction time are 2h
Cheng Hou, fast pressure relief 3-5 times repeatedly, obtain the graphene oxide of supercritical carbon dioxide treatment, using by overcritical dioxy
Change graphene oxide and the preparation of carbon processing.
The ultrasonic power of the ultrasonic power is 50-300W, time 0.5-2h.
The polyethylene glycol polymeric degree is 400-6000, and the sulfonation degree of sulfonated polysulfone is 15-30%.
When using supercritical carbon dioxide treatment graphene oxide, modifying agent is added, modifier used is：Quaternary ammonium salt
The mass ratio of Lei, phosphonium salts classes or silane coupling agent, the modifying agent of addition and graphene oxide to be modified is 1-100: 10-100.
The quaternary ammonium salt is cetyl ammonium bromide；Suo Shu phosphonium salt classes are cetyl phosphonium chloride or ethoxy three
Ben Ji phosphonium chlorides；The silane coupling agent is KH550 or KH560.
The homogeneous casting solution of the formation is specifically that under 60-75 DEG C of temperature condition, the polyethylene glycol of half is added
It in the n,N-dimethylacetamide solution evenly dispersed to graphene oxide, is sufficiently stirred, then by the polysulfones and sulphur after drying
Change polysulfones to be uniformly mixed by high-speed mixer, is divided into tripartite, in mass ratio example 4: 3: 3, puts into solution in batches, often
Minor tick 1.5-2.5h, while solution is added in remaining polyethylene glycol incessantly, it is sufficiently stirred 10-15h, is formed it into
The casting solution of phase.
By adopting the above-described technical solution, compared with prior art, the present invention is directed to polysulfones (PSF) doughnut film property
The problem of energy, introduces graphene oxide, and surface modification is carried out to graphene oxide using super critical CO 2 technology,
It fully dispersed and can be arranged in pairs or groups in a polymer matrix using specific component, both improve ps hollow fiber uf membrane
Toughness, increase the application range of polysulfones base hollow-fibre membrane, and ps hollow fiber uf membrane is made to keep preferable water flux and cut
Under the premise of staying rate, the comprehensive mechanical performance and antifouling property of ps hollow fiber uf membrane can be improved, forming properties are more steady
Fixed doughnut film composite material.
Specific implementation mode
The present invention is further described specifically by the following examples.In following embodiment, each component
Dosage is weight consumption.It is necessarily pointed out that following embodiment is served only for, the present invention is described further, no
It can be interpreted as limiting the scope of the invention, field technology skilled person is the present invention according to aforementioned present invention content
Go out some nonessential modifications and adaptations, still falls within protection scope of the present invention.
The embodiment of the present invention 1：Polysulfones-graphene oxide hollow-fibre membrane, is calculated according to the mass fraction, including with 18.5 parts
Polysulfones, 1.5 parts of sulfonated polysulfone, 35.6 parts of polyethylene glycol 400,44.4 parts of DMAC N,N' dimethyl acetamides and 0.05 part of graphite oxide
Alkene.
The preparation method of polysulfones-graphene oxide hollow-fibre membrane takes each component by above-mentioned mass fraction, including walks as follows
Suddenly：
1) polysulfones and sulfonated polysulfone are dried in vacuo 24 hours at 70 DEG C respectively；
2) graphene oxide described in before use, first graphene oxide is put into supercritical carbon dioxide reaction kettle,
It carries out under conditions of reaction temperature is 40 DEG C, reaction pressure >=20MPa, reaction time are 2h, after the completion of reaction, quickly unloads
Pressure, 3-5 times repeatedly, obtains the graphene oxide of supercritical carbon dioxide treatment, using by supercritical carbon dioxide treatment
Graphene oxide and preparation；It adds graphene oxide into n,N-dimethylacetamide, then oxidation stone is made by ultrasonic power
Black alkene is dispersed in DMAC N,N' dimethyl acetamide；The ultrasonic power of the ultrasonic power is 200W, time 1h；
3) then be included in it is dry after sulfonated polysulfone, polyethylene glycol 400 and it is dry after polysulfones filled under conditions of 70 DEG C
Divide stirring 12h, form it into homogeneous casting solution, and carry out vacuum defoamation, then dynamic analysis of spinning is formed by spinneret, by spray
The air gap between filament plate and coagulating bath is immersed in coagulating bath, and the biography of solvent n,N-dimethylacetamide and non-solvent water is passed through
Mass transter and form hollow-fibre membrane；The temperature of the air gap between the spinneret and coagulating bath is 30 DEG C, humidity≤
20%.
After testing, the performance indicator of the product of embodiment 1 is：Internal diameter 500-700um, wall thickness 200-300um, pure water flux
≥180L·m-2·h-1, to rejection >=98% of bovine serum albumin (67000).
The embodiment of the present invention 2：Polysulfones-thermoplastic elastomer (TPE)-organo montmorillonite blend hollow fiber membrane, by mass fraction
Calculate, include with 15 parts of polysulfones, 1.7 parts of sulfonated polysulfone, 33 parts of polyethylene glycol 400,48 parts of n,N-dimethylacetamide and
0.01 part of graphene oxide.
The preparation method is the same as that of Example 1.
After testing, the performance indicator of the product of embodiment 1 is：Internal diameter 1000-1200um, wall thickness 100-150um, pure water are logical
Amount >=250Lm-2·h-1, to rejection >=90% of bovine serum albumin (67000).
The embodiment of the present invention 3：Polysulfones-thermoplastic elastomer (TPE)-organo montmorillonite blend hollow fiber membrane, by mass fraction
Calculate, include with 20 parts of polysulfones, 1.2 parts of sulfonated polysulfone, 37 parts of polyethylene glycol 400,42 parts of n,N-dimethylacetamide and
0.01 part of graphene oxide.
The preparation method is the same as that of Example 1.
After testing, the performance indicator of the product of embodiment 1 is：Internal diameter 500-700um, wall thickness 200-250um, pure water flux
≥180L·m-2·h-1, to rejection >=95% of bovine serum albumin (67000).
Comparative example 1
By comparing a kind of patent of invention " preparation method of permanent hydrophilic type polysulfone ultrafiltration membrane " embodiment seven, solid content
For the pure water flux 130Lm of 20% polysulfone ultrafiltration membrane-2·h-1, bovine serum albumin rejection 96%, by add it is modified
Graphene oxide, under the conditions of identical solid content, using this patent preparation method, the pure water of polysulfones/graphene oxide of preparation
Flux >=180Lm-2·h-1, 38.5% is improved, to rejection >=98% of bovine serum albumin (67000), performance is obviously excellent
In comparison PS membrane.
The experimental result of experimental data and comparative example according to the embodiment is it is known that technical scheme of the present invention improves
The toughness of ps hollow fiber uf membrane, increase polysulfones base hollow-fibre membrane application range, and make ps hollow fiber uf membrane keep compared with
Under the premise of good water flux and rejection, the comprehensive mechanical performance and antifouling property of ps hollow fiber uf membrane can be improved,
The more stable doughnut film composite material of forming properties.
Claims (9)
1. a kind of polysulfones-graphene oxide hollow-fibre membrane, it is characterised in that：It calculates according to the mass fraction, including poly- with 15-20 parts
Sulfone, 1.2-1.7 part sulfonated polysulfone, 33-37 parts of polyethylene glycol, 42-48 parts of N, N- dimethylacetylamides and 0.01-1 parts of oxidations
Graphene；It is prepared as follows：
Each component is taken by above-mentioned mass fraction, is included the following steps：
1）Polysulfones and sulfonated polysulfone are dried in vacuo 12-24 hours at 65-75 DEG C respectively；
2）Processed graphene oxide is added to N, in N- dimethylacetylamides, then graphite oxide is made by ultrasonic power
Alkene is dispersed in N, in N- dimethylacetylamides；
3）Then the polysulfones after addition is dry after sulfonated polysulfone, polyethylene glycol and drying fully stirs under conditions of 65-75 DEG C
10-15h is mixed, forms it into homogeneous casting solution, and carry out vacuum defoamation, then dynamic analysis of spinning is formed by spinneret, by spray
The air gap between filament plate and coagulating bath is immersed in coagulating bath, by solvent N, N- dimethylacetylamides and non-solvent water
Mass transfer exchanges and forms hollow-fibre membrane；
The graphene oxide by graphene oxide, modifying agent and cosolvent before use, be first put into supercritical carbon dioxide
In reaction kettle, carried out under conditions of reaction temperature is 40 DEG C, reaction pressure >=20MPa, reaction time are 2h, reaction is completed
Afterwards, fast pressure relief 3-5 times repeatedly, obtains the graphene oxide of supercritical carbon dioxide treatment, using by overcritical titanium dioxide
The graphene oxide of carbon processing participates in preparing；
When using supercritical carbon dioxide treatment graphene oxide, modifying agent is added, modifier used is：Quaternary ammonium salt,
The mass ratio of phosphonium salt class or silane coupling agent, the modifying agent of addition and graphene oxide to be modified is 1-100：10-100.
2. a kind of preparation method of polysulfones as described in claim 1-graphene oxide hollow-fibre membrane, it is characterised in that：It presses
Above-mentioned mass fraction takes each component, includes the following steps：
1）Polysulfones and sulfonated polysulfone are dried in vacuo 12-24 hours at 65-75 DEG C respectively；
2）Processed graphene oxide is added to N, in N- dimethylacetylamides, then graphite oxide is made by ultrasonic power
Alkene is dispersed in N, in N- dimethylacetylamides；
3）Then the polysulfones after addition is dry after sulfonated polysulfone, polyethylene glycol and drying fully stirs under conditions of 65-75 DEG C
10-15h is mixed, forms it into homogeneous casting solution, and carry out vacuum defoamation, then dynamic analysis of spinning is formed by spinneret, by spray
The air gap between filament plate and coagulating bath is immersed in coagulating bath, by solvent N, N- dimethylacetylamides and non-solvent water
Mass transfer exchanges and forms hollow-fibre membrane.
3. the preparation method of polysulfones according to claim 2-graphene oxide hollow-fibre membrane, it is characterised in that：It is described
Spinneret and coagulating bath between air gap length be 1-5cm, the temperature of the air gap is 20-50 DEG C, humidity 50-
80%。
4. the preparation method of polysulfones according to claim 2-graphene oxide hollow-fibre membrane, it is characterised in that：It is described
Graphene oxide before use, first graphene oxide, modifying agent and cosolvent are put into supercritical carbon dioxide reaction kettle,
It carries out under conditions of reaction temperature is 40 DEG C, reaction pressure >=20MPa, reaction time are 2h, after the completion of reaction, quickly unloads
Pressure, 3-5 times repeatedly, obtains the graphene oxide of supercritical carbon dioxide treatment, using by supercritical carbon dioxide treatment
Graphene oxide participates in preparing.
5. the preparation method of polysulfones according to claim 2-graphene oxide hollow-fibre membrane, it is characterised in that：It is described
Ultrasonic power ultrasonic power be 50-300W, time 0.5-2h.
6. the preparation method of polysulfones according to claim 2-graphene oxide hollow-fibre membrane, it is characterised in that：It is described
Polyethylene glycol polymeric degree be 400-6000, the sulfonation degree of sulfonated polysulfone is 15-30%.
7. the preparation method of polysulfones according to claim 4-graphene oxide hollow-fibre membrane, it is characterised in that：It is adopting
When with supercritical carbon dioxide treatment graphene oxide, modifying agent is added, modifier used is：Quaternary ammonium salt, phosphonium salts class or
The mass ratio of silane coupling agent, the modifying agent of addition and graphene oxide to be modified is 1-100：10-100.
8. the preparation method of polysulfones according to claim 7-graphene oxide hollow-fibre membrane, it is characterised in that：It is described
Quaternary ammonium salt be cetyl ammonium bromide；Suo Shu phosphonium salt classes are cetyl phosphonium chloride or hydroxyethyl triphenyl phosphonium chloride；
The silane coupling agent is KH550 or KH560.
9. the preparation method of polysulfones according to claim 2-graphene oxide hollow-fibre membrane, it is characterised in that：It is described
The homogeneous casting solution of formation be specifically that under 60-75 DEG C of temperature condition, the polyethylene glycol of half is added to graphene oxide
In evenly dispersed N, N- dimethylacetamide solution, be sufficiently stirred, then by after drying polysulfones and sulfonated polysulfone pass through height
Fast mixing machine is uniformly mixed, and is divided into tripartite, in mass ratio example 4：3：3, it puts into solution in batches, per minor tick 1.5-
2.5h, while solution is added in remaining polyethylene glycol incessantly, it is sufficiently stirred 10-15h, forms it into homogeneous casting film
Liquid.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106582298A (en) * | 2016-12-09 | 2017-04-26 | 西安建筑科技大学 | Three-dimensional GO sheet sphere particle modified organic composite ultra/micro filtering membrane preparing method |
| CN107570021B (en) * | 2017-01-17 | 2021-09-10 | 贵州师范大学 | Hydrophilic polysulfone/silicon dioxide blended hollow fiber membrane and preparation method thereof |
| IT201800010402A1 (en) * | 2018-11-16 | 2020-05-16 | Consiglio Nazionale Ricerche | METHOD FOR THE TREATMENT OF A POROUS SUBSTRATE |
| CN110813110B (en) * | 2019-11-14 | 2021-06-25 | 泰州清润环保科技有限公司 | Graphene composite photocatalytic ultrafiltration membrane and preparation method thereof |
| CN112642308A (en) * | 2019-12-03 | 2021-04-13 | 贵州省材料技术创新基地 | Polysulfone-biochar blending separation membrane and preparation method thereof |
| CN112175177B (en) * | 2020-10-15 | 2023-01-20 | 贵州省材料技术创新基地 | Catalyst and preparation method thereof, and preparation method of polylactic acid |
| CN112403291A (en) * | 2020-11-12 | 2021-02-26 | 杭州艾珀耐特工程科技有限公司 | High-performance PVDF film and preparation method thereof |
| CN112774468A (en) * | 2020-12-18 | 2021-05-11 | 任国峰 | Graphene polysulfone ultrafiltration membrane and preparation method thereof |
| CN112844082A (en) * | 2020-12-30 | 2021-05-28 | 桐乡市艾维科技有限公司 | Porous graphene grafted polysulfone high-flux gas separation membrane material and preparation method thereof |
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| CN104096488A (en) * | 2014-08-01 | 2014-10-15 | 天津工业大学 | Preparation method of polymer/graphene oxide composite separating membrane |
| CN105582821A (en) * | 2016-02-22 | 2016-05-18 | 国家海洋局第三海洋研究所 | Membrane casting solution of functionalized graphene composite ultrafiltration membrane and preparation method of functionalized graphene composite ultrafiltration membrane |
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| CN104096488A (en) * | 2014-08-01 | 2014-10-15 | 天津工业大学 | Preparation method of polymer/graphene oxide composite separating membrane |
| CN105582821A (en) * | 2016-02-22 | 2016-05-18 | 国家海洋局第三海洋研究所 | Membrane casting solution of functionalized graphene composite ultrafiltration membrane and preparation method of functionalized graphene composite ultrafiltration membrane |
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