CN108744995A - A kind of antibacterial composite hollow fiber membrane and preparation method thereof - Google Patents
A kind of antibacterial composite hollow fiber membrane and preparation method thereof Download PDFInfo
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- CN108744995A CN108744995A CN201810571375.1A CN201810571375A CN108744995A CN 108744995 A CN108744995 A CN 108744995A CN 201810571375 A CN201810571375 A CN 201810571375A CN 108744995 A CN108744995 A CN 108744995A
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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
- B01D69/12—Composite membranes; Ultra-thin membranes
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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
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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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
- B01D71/06—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
- B01D2325/00—Details relating to properties of membranes
- B01D2325/48—Antimicrobial properties
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Abstract
A kind of antibacterial composite hollow fiber membrane and preparation method thereof.The present invention provides a kind of modified hollow fibre membrane, including following mass percent prepares raw material：The modified inorganic nano-particle of the polysulfones of 12-14%, the pore-foaming agent of 8%-12%, the polyethylene glycol of 2-4% and 1-4%, surplus are organic solvent.The present invention increases the bacteriostasis rate of tunica fibrosa by selecting silver ion nanometer doped zinc oxide and silver ion doped nano titanium dioxide to be modified tunica fibrosa.The present invention improves the permeability to water and the removal effect to β2-microglobulin, reduces the loss of human serum albumins by adding a small amount of PEG-10000 and PEG-8000.
Description
Technical field
The present invention relates to a kind of antibacterial composite hollow fiber membranes and preparation method thereof.
Background technology
Nano anti-biotic material is a kind of new material for having bacteriostasis property.Due to the high-specific surface area of antiseptic in material
With the special effects of high reaction activity, whole antibacterial effect is substantially increased, it includes bacterium, fungi, ferment that can make microorganism
The growth and breeding of female bacterium, algae and virus etc. keep lower level.Nano anti-biotic material can be divided into 3 again by Antibacterial Mechanism
Class：1st class is metal molds nano antibacterial agents such as silver-colored (Ag)；2nd class is quaternary ammonium salt or quaternary alkylphosphonium salt modification inorganic nanoparticles；
3rd class is nano zine oxide (ZnO), the photocatalyst-types nano anti-biotic material such as nano-titanium dioxide (TiO2).
The membrane for purifying blood product clinically applied is required to sterile, the sterilizings such as generally use irradiation, steam, ethylene oxide
Mode keeps product sterile, wherein irradiation is the preferred sterilization method of domestic and international manufacturer, including gamma irradiation and electron beam spoke
According to.The parameter of most critical is sterilizing dose in irradiation, and sterilizing dose is excessively high, the membrane structure of destructible product and the support knot of membrane material
Structure (such as shell), sterilizing dose are insufficient, cannot meet the requirement of sterility assurance level, and when treatment, content of microorganisms is exceeded, Yi Fa
Raw malpractice.The height of sterilizing dose, it is directly related with the quantity of the biological load of product or initial contaminating bacteria, therefore,
In the raw material for forming product, anti-biotic material is added, can effectively inhibit the breeding of microorganism, the sterilizing dose of product is made to keep
In low-level, it is more advantageous to the performance for keeping product and material.
The core starting materials of membrane for purifying blood product are membrane materials, and common membrane material is the synthesis film such as polysulfones and polyether sulfone,
Middle PS membrane has an excellent mechanical performance, chemical property, it is cheap the features such as, but its antibiotic property is poor.
Chinese patent (Publication No. CN 103572507A) discloses a kind of antibacterial ultraviolet-resistannanofiber silk fibroin nano-fiber film
Preparation method improve the antibiotic property of PS membrane by the way that inorganic nano-particle is added in this article, however it is still not ideal enough.
Invention content
On this basis, a kind of antibacterial composite hollow fiber membrane of present invention offer and preparation method thereof.
To achieve the above object, the technical solution used in the present invention：A kind of antibacterial composite hollow fiber membrane, including it is following
Mass percent prepares raw material：The polysulfones of 12-14%, the pore-foaming agent of 8%-12%, the polyethylene glycol of 2-4% and 1-4%
Modified inorganic nano-particle, surplus are organic solvent.
Preferably, the modified hollow fibre membrane includes that following mass percent prepares raw material：13% polysulfones, 9%
Pore-foaming agent, 3% polyethylene glycol, 1% inorganic nano-particle and 73% organic solvent.
Preferably, the polyethylene glycol is the mixture of PEG-10000 and PEG-8000.
Preferably, the mass ratio of the PEG-10000 and PEG-8000 is 5:1.
Preferably, the modified inorganic nano-particle be by inorganic nano-particle through lauryl sodium sulfate blending and modifying and
?.
It is highly preferred that the modified inorganic nano-particle is prepared by following methods：
Inorganic nano-particle is added in a concentration of 25g/L sodium dodecyl sulfate solutions and is modified, vinegar is then used
The pH of modified mixed liquor is adjusted to 4.5 by acid, is filtered using 300 mesh filter screens after then stirring evenly mixed liquor,
The dilute acetic acid solution for being again 6% with mass fraction is washed, then the vacuum drying at 55 DEG C, is obtained the modified inorganic and is received
Rice corpuscles powder.
Preferably, the inorganic nano-particle is silver ion nanometer doped zinc oxide and silver ion doped nano titanium dioxide
Mixture.
Preferably, the mass ratio of the silver ion nanometer doped zinc oxide and silver ion doped nano titanium dioxide is 1:1.
Preferably, the pore-foaming agent is polyvinylpyrrolidone.
Preferably, the organic solvent is in n-methyl-2-pyrrolidone, dimethylformamide, dimethylacetylamide
It is at least one.
The present invention provides the preparation methods of modified hollow fibre membrane described above, include the following steps：
(1) polysulfones and pore-foaming agent are added in organic solvent, fully dissolving is stirred at 55~65 DEG C；
(2) modified inorganic nano-particle is added into mixed solution under agitation and spinning original is made in polyethylene glycol
Liquid；
(3) vacuumizing and defoaming is carried out at vacuum degree -0.7~-0.85bar and obtains spinning solution, and spinning solution is true through filtering, taking out
Empty deaeration, dry-wet spinning, washing, stretching and dry obtained antibacterial composite hollow fiber membrane.
The beneficial effects of the present invention are：
(1) present invention is by selecting silver ion nanometer doped zinc oxide and silver ion doped nano titanium dioxide to tunica fibrosa
It is modified, increases the bacteriostasis rate of tunica fibrosa.
(2) present invention improves membrane material and is produced to the permeability and film of water by adding a small amount of PEG-10000 and PEG-8000
Product reduce the loss of human serum albumins to the removal effect of β2-microglobulin.
Specific implementation mode
Embodiment 1
A kind of embodiment of antibacterial composite hollow fiber membrane of the present invention, including following mass percent prepare raw material：
13% polysulfones, 9% pore-foaming agent, 3% polyethylene glycol, 1% inorganic nano-particle and 74% organic solvent.Wherein institute
It is polyvinylpyrrolidone to state pore-foaming agent.The polyethylene glycol is the mixture of PEG-10000 and PEG-8000, the PEG-
The mass ratio of 10000 and PEG-8000 is 5:1.The modified inorganic nano-particle be silver ion nanometer doped zinc oxide and silver from
The mixture of sub- doped nano titanium dioxide, the doping of silver ion is 1wt% in silver ion nanometer doped zinc oxide, silver from
The doping of silver ion is 1wt% in sub- doped nano titanium dioxide, and the silver ion nanometer doped zinc oxide and silver ion are mixed
The mass ratio of miscellaneous nano-titanium dioxide is 1:1.The organic solvent is dimethylformamide.
The modified inorganic nano-particle is prepared by following methods：
Inorganic nano-particle is added in a concentration of 25g/L sodium dodecyl sulfate solutions and is modified, vinegar is then used
The pH of modified mixed liquor is adjusted to 4.5 by acid, is filtered using 300 mesh filter screens after then stirring evenly mixed liquor,
The dilute acetic acid solution for being again 6% with mass fraction is washed, then the vacuum drying at 55 DEG C, is obtained the modified inorganic and is received
Rice corpuscles powder.
The preparation method of antibacterial composite hollow fiber membrane described above, includes the following steps：
(1) polysulfones and pore-foaming agent are added in organic solvent, fully dissolving is stirred at 60 DEG C；
(2) polyethylene glycol is added into mixed solution under agitation and spinning solution is made；
(3) vacuumizing and defoaming being carried out at vacuum degree -0.85bar and obtaining spinning solution, spinning solution is de- through filtering, vacuumizing
Bubble, dry-wet spinning, washing, stretching and dry obtained antibacterial composite hollow fiber membrane.
Embodiment 2
A kind of embodiment of antibacterial composite hollow fiber membrane of the present invention, including following mass percent prepare raw material：
13% polysulfones, 9% pore-foaming agent, 3% polyethylene glycol, 1% inorganic nano-particle and 74% organic solvent.Wherein institute
It is polyvinylpyrrolidone to state pore-foaming agent.The polyethylene glycol is the mixture of PEG-10000 and PEG-8000, the PEG-
The mass ratio of 10000 and PEG-8000 is 5:1.The modified inorganic nano-particle be silver ion nanometer doped zinc oxide, silver from
The doping of silver ion is 1wt% in sub- nanometer doped zinc oxide.The organic solvent is dimethylformamide.
The antibacterial composite nano inoganic particle is prepared by following methods：
Inorganic nano-particle is added in a concentration of 25g/L sodium dodecyl sulfate solutions and is modified, vinegar is then used
The pH of modified mixed liquor is adjusted to 4.5 by acid, is filtered using 300 mesh filter screens after then stirring evenly mixed liquor,
The dilute acetic acid solution for being again 6% with mass fraction is washed, then the vacuum drying at 55 DEG C, is obtained the modified inorganic and is received
Rice corpuscles powder.
The preparation method of antibacterial composite hollow fiber membrane described above, includes the following steps：
(1) polysulfones and pore-foaming agent are added in organic solvent, fully dissolving is stirred at 60 DEG C；
(2) modified inorganic nano-particle is added into mixed solution under agitation and spinning original is made in polyethylene glycol
Liquid；
(3) vacuumizing and defoaming being carried out at vacuum degree -0.85bar and obtaining spinning solution, spinning solution is de- through filtering, vacuumizing
Bubble, dry-wet spinning, washing, stretching and dry obtained antibacterial composite hollow fiber membrane.
Embodiment 3
A kind of embodiment of antibacterial composite hollow fiber membrane of the present invention, including following mass percent prepare raw material：
13% polysulfones, 9% pore-foaming agent, 3% polyethylene glycol, 1% inorganic nano-particle and 74% organic solvent.Wherein institute
It is polyvinylpyrrolidone to state pore-foaming agent.The polyethylene glycol is the mixture of PEG-10000 and PEG-8000, the PEG-
The mass ratio of 10000 and PEG-8000 is 5:1.Inorganic nano-particle in the modified inorganic nano-particle adulterates for silver ion
Nano-titanium dioxide, the doping of silver ion is 1wt% in silver ion doped nano titanium dioxide.The organic solvent is diformazan
Base formamide.
The modified inorganic nano-particle is prepared by following methods：
Inorganic nano-particle is added in a concentration of 25g/L sodium dodecyl sulfate solutions and is modified, vinegar is then used
The pH of modified mixed liquor is adjusted to 4.5 by acid, is filtered using 300 mesh filter screens after then stirring evenly mixed liquor,
The dilute acetic acid solution for being again 6% with mass fraction is washed, then the vacuum drying at 55 DEG C, is obtained the modified inorganic and is received
Rice corpuscles powder.
The preparation method of antibacterial composite hollow fiber membrane described above, includes the following steps：
(1) polysulfones and pore-foaming agent are added in organic solvent, fully dissolving is stirred at 60 DEG C；
(2) modified inorganic nano-particle is added into mixed solution under agitation and spinning original is made in polyethylene glycol
Liquid；
(3) vacuumizing and defoaming being carried out at vacuum degree -0.85bar and obtaining spinning solution, spinning solution is de- through filtering, vacuumizing
Bubble, dry-wet spinning, washing, stretching and dry obtained antibacterial composite hollow fiber membrane.
Embodiment 4
A kind of embodiment of antibacterial composite hollow fiber membrane of the present invention, including following mass percent prepare raw material：
13% polysulfones, 9% pore-foaming agent, 3% polyethylene glycol, 1% inorganic nano-particle and 74% organic solvent.Wherein institute
It is polyvinylpyrrolidone to state pore-foaming agent.The polyethylene glycol is PEG-10000.The modified inorganic nano-particle is silver ion
The mixture of nanometer doped zinc oxide and silver ion doped nano titanium dioxide, silver ion in silver ion nanometer doped zinc oxide
Doping be 1wt%, the doping of silver ion is 1wt% in silver ion doped nano titanium dioxide, the silver ion doping
The mass ratio of nano zine oxide and silver ion doped nano titanium dioxide is 1:1.The organic solvent is dimethylformamide.
The modified inorganic nano-particle is prepared by following methods：
Inorganic nano-particle is added in a concentration of 25g/L sodium dodecyl sulfate solutions and is modified, vinegar is then used
The pH of modified mixed liquor is adjusted to 4.5 by acid, is filtered using 300 mesh filter screens after then stirring evenly mixed liquor,
The dilute acetic acid solution for being again 6% with mass fraction is washed, then the vacuum drying at 55 DEG C, is obtained the modified inorganic and is received
Rice corpuscles powder.
The preparation method of antibacterial composite hollow fiber membrane described above, includes the following steps：
(1) polysulfones and pore-foaming agent are added in organic solvent, fully dissolving is stirred at 60 DEG C；
(2) polyethylene glycol is added into mixed solution under agitation and spinning solution is made；
(3) vacuumizing and defoaming being carried out at vacuum degree -0.85bar and obtaining spinning solution, spinning solution is de- through filtering, vacuumizing
Bubble, dry-wet spinning, washing, stretching and dry obtained antibacterial composite hollow fiber membrane.
Comparative example 1
This comparative example hollow-fibre membrane includes that following mass percent prepares raw material：13% polysulfones, 9% pore
Agent, 3% polyethylene glycol, 1% inorganic nano-particle and 74% organic solvent.The wherein described pore-foaming agent is polyvinyl pyrrole
Alkanone.The polyethylene glycol is PEG-20000.The modified inorganic nano-particle be silver ion nanometer doped zinc oxide and silver from
The mixture of sub- doped nano titanium dioxide, the doping of silver ion is 1wt% in silver ion nanometer doped zinc oxide, silver from
The doping of silver ion is 1wt% in sub- doped nano titanium dioxide, and the silver ion nanometer doped zinc oxide and silver ion are mixed
The mass ratio of miscellaneous nano-titanium dioxide is 1:1.The organic solvent is dimethylformamide.
The modified inorganic nano-particle is prepared by following methods：
Inorganic nano-particle is added in a concentration of 25g/L sodium dodecyl sulfate solutions and is modified, vinegar is then used
The pH of modified mixed liquor is adjusted to 4.5 by acid, is filtered using 300 mesh filter screens after then stirring evenly mixed liquor,
The dilute acetic acid solution for being again 6% with mass fraction is washed, then the vacuum drying at 55 DEG C, is obtained the modified inorganic and is received
Rice corpuscles powder.
The preparation method of hollow-fibre membrane described above, includes the following steps：
(1) polysulfones and pore-foaming agent are added in organic solvent, fully dissolving is stirred at 60 DEG C；
(2) polyethylene glycol is added into mixed solution under agitation and spinning solution is made；
(3) vacuumizing and defoaming being carried out at vacuum degree -0.85bar and obtaining spinning solution, spinning solution is de- through filtering, vacuumizing
Bubble, dry-wet spinning, washing, stretching and dry obtained hollow-fibre membrane.
Performance test
Using 1-4 antibacterials composite hollow fiber membrane of the embodiment of the present invention and comparative example doughnut film preparation haemodialysis
The raw material of device, each embodiment is shown in Table 1, then carries out simulated experiment, characterizes the performance of membrane material and performance (the screening system of film product
Number), the results are shown in Table 2.
1 raw material of table
2 the performance test results of table
As can be seen from Table 2, the present invention is by selecting silver ion nanometer doped zinc oxide and silver ion dopen Nano
Titanium dioxide is modified tunica fibrosa, increases the bacteriostasis rate of tunica fibrosa.
By table 2 it is also seen that by adding a small amount of PEG-10000 and PEG-8000, permeability of the membrane material to water is improved
With film product to the screening efficiency of β2-microglobulin, screening efficiency of the film product to human serum albumins is reduced, is illustrated a small amount of
PEG-10000 and PEG-8000 be conducive to remove the middle molecule toxins such as β2-microglobulin, and inhibit human serum albumins etc. to have
The loss of beneficial substance.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than is protected to the present invention
The limitation of range is protected, although being explained in detail to the present invention with reference to preferred embodiment, those skilled in the art should
Understand, technical scheme of the present invention can be modified or replaced equivalently, without departing from the essence of technical solution of the present invention
And range.
Claims (10)
1. a kind of antibacterial composite hollow fiber membrane, which is characterized in that prepare raw material including following mass percent：12-14%
Polysulfones, the pore-foaming agent of 8%-12%, the polyethylene glycol of 2-4% and 1-4% modified inorganic nano-particle, surplus be it is organic molten
Agent.
2. antibacterial composite hollow fiber membrane according to claim 1, which is characterized in that include the system of following mass percent
Standby raw material：13% polysulfones, 9% pore-foaming agent, 3% polyethylene glycol, 1% inorganic nano-particle and 73% it is organic molten
Agent.
3. antibacterial composite hollow fiber membrane according to claim 1 or 2, which is characterized in that the polyethylene glycol is PEG-
The mixture of 10000 and PEG-8000.
4. antibacterial composite hollow fiber membrane according to claim 3, which is characterized in that the PEG-10000 and PEG-
8000 mass ratio is 5:1.
5. antibacterial composite hollow fiber membrane according to claim 1, which is characterized in that the modified inorganic nano-particle is
By inorganic nano-particle through obtained by lauryl sodium sulfate blending and modifying.
6. antibacterial composite hollow fiber membrane according to claim 5, which is characterized in that the inorganic nano-particle be silver from
The mixture of sub- nanometer doped zinc oxide and silver ion doped nano titanium dioxide.
7. antibacterial composite hollow fiber membrane according to claim 6, which is characterized in that the silver ion dopen Nano oxidation
The mass ratio of zinc and silver ion doped nano titanium dioxide is 1:1.
8. antibacterial composite hollow fiber membrane according to claim 1, which is characterized in that the pore-foaming agent is polyvinyl pyrrole
Alkanone.
9. antibacterial composite hollow fiber membrane according to claim 1, which is characterized in that the organic solvent is N- methyl-
At least one of 2-Pyrrolidone, dimethylformamide, dimethylacetylamide.
10. a kind of preparation method of antibacterial composite hollow fiber membrane as described in claim 1-9 is any, which is characterized in that packet
Include following steps：
(1) polysulfones and pore-foaming agent are added in organic solvent, fully dissolving is stirred at 55~65 DEG C；
(2) modified inorganic nano-particle is added into mixed solution under agitation and spinning solution is made in polyethylene glycol；
(3) vacuumizing and defoaming being carried out at vacuum degree -0.7~-0.85bar and obtaining spinning solution, spinning solution is de- through filtering, vacuumizing
Bubble, dry-wet spinning, washing, stretching and dry obtained antibacterial composite hollow fiber membrane.
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| CN201810571375.1A CN108744995B (en) | 2018-06-06 | 2018-06-06 | A kind of antibacterial composite hollow fiber membrane and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112143306A (en) * | 2020-09-17 | 2020-12-29 | 鹤山市顺鑫实业有限公司 | Covering base film and preparation method thereof |
| CN114917769A (en) * | 2022-05-24 | 2022-08-19 | 江苏诺莱智慧水务装备有限公司 | Antibacterial hollow fiber membrane and preparation method thereof |
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| CN101711954A (en) * | 2009-11-06 | 2010-05-26 | 江苏朗生生命科技有限公司 | Blending modified hollow polysulfone fiber film, preparation method and application thereof |
| CN103572507A (en) * | 2012-07-24 | 2014-02-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for antibiosis ultraviolet prevention silk fibroin nanofiber membrane |
| CN105251370A (en) * | 2015-11-24 | 2016-01-20 | 江润生 | Super-hydrophobic air filtering membrane as well as preparation method and application thereof |
| CN105903360A (en) * | 2016-06-17 | 2016-08-31 | 安庆市天虹新型材料科技有限公司 | Antibacterial stain-resistant polyvinylidene fluoride composite film |
| CN106268371A (en) * | 2016-08-08 | 2017-01-04 | 贵阳时代沃顿科技有限公司 | A kind of polyacrylonitrile hollow fiber ultrafilter membrane and preparation method thereof |
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| CN101711954A (en) * | 2009-11-06 | 2010-05-26 | 江苏朗生生命科技有限公司 | Blending modified hollow polysulfone fiber film, preparation method and application thereof |
| CN103572507A (en) * | 2012-07-24 | 2014-02-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for antibiosis ultraviolet prevention silk fibroin nanofiber membrane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112143306A (en) * | 2020-09-17 | 2020-12-29 | 鹤山市顺鑫实业有限公司 | Covering base film and preparation method thereof |
| CN114917769A (en) * | 2022-05-24 | 2022-08-19 | 江苏诺莱智慧水务装备有限公司 | Antibacterial hollow fiber membrane and preparation method thereof |
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| CN108744995B (en) | 2019-04-23 |
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