CN107511082A - A kind of PES hollow cored fibre dialysis membrane and preparation method thereof - Google Patents
A kind of PES hollow cored fibre dialysis membrane and preparation method thereof Download PDFInfo
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- CN107511082A CN107511082A CN201710927626.0A CN201710927626A CN107511082A CN 107511082 A CN107511082 A CN 107511082A CN 201710927626 A CN201710927626 A CN 201710927626A CN 107511082 A CN107511082 A CN 107511082A
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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
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
- A61M1/00—Suction or pumping devices for medical purposes; Devices for carrying-off, for treatment of, or for carrying-over, body-liquids; Drainage systems
- A61M1/14—Dialysis systems; Artificial kidneys; Blood oxygenators ; Reciprocating systems for treatment of body fluids, e.g. single needle systems for hemofiltration or pheresis
- A61M1/16—Dialysis systems; Artificial kidneys; Blood oxygenators ; Reciprocating systems for treatment of body fluids, e.g. single needle systems for hemofiltration or pheresis with membranes
- A61M1/1621—Constructional aspects thereof
-
- 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
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0013—Casting processes
-
- 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
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
Abstract
The present invention relates to a kind of PES hollow cored fibre dialysis membrane and preparation method thereof, belongs to characterized by shape, structure or performance, using the hollow fibre technical field of membrane typically either physically or chemically separated.The casting solution of the PES hollow cored fibre dialysis membrane is mainly made up of polyethersulfone resin, diatomite, amphipathic copolymer, organic pore-foaming agent, the polymer of good biocompatibility and solvent.The application is applied to the fields such as haemodialysis, there is high mechanical properties, good biocompatibility, permanent hydrophily, high ultrafiltrate coefficient and high clearance rate.
Description
Technical field
The present invention relates to a kind of PES hollow cored fibre dialysis membrane and preparation method thereof, belong to shape, structure or performance
It is characterized, using the hollow fibre technical field of membrane typically either physically or chemically separated.
Background technology
Haemodialysis is developed so far existing more than 90 years history, and haemodialysis is acute or chronic renal failure patient's replacement therapy
One of mode.It by by internal blood drainage to external, by the new old generation in membrane removal blood of being dialysed in haemodialysis control unit
Waste, impurity and moisture are thanked, then the blood purified is transmitted back in vivo.Dialysis membrane by being formed without several hollow fibres, when
When blood is flowed through on the inside of these hollow fibres, pass through more to the electrolyte similar to body concentration on the outside of hollow fibre
Dissipate, convection current progress mass exchange, so as to remove internal metabolic waste, maintain electrolyte and acid-base balance, remove simultaneously
Excessive moisture.
Dialysis membrane is the most crucial part of haemodialyser, and dialysis membrane material is the key for influenceing effects of hemodialysis in treating
Factor.At present, clinical conventional dialysis membrane can be divided into three classes：Unmodified cellulose membrane, modification or regenerated cellulose film and
Synthesize film.This three classes dialysis membrane has larger difference in biocompatibility, Water permeability, uremic toxins's removing etc.,
Removing solute and ultrafiltration are two major functions of dialyzer, and clearance rate and ultrafiltrate coefficient are that the key of evaluation dialysis film quality refers to
Mark.The transmission characteristic of dialysis membrane determines the clearance rate of solute and the clearance to moisture, and the surface nature of dialysis membrane determines
The characteristic and degree of the interphase interaction of blood and film, include absorption, complement activation and the immune response etc. of protein.
Polyether sulfone is because of its high mechanical strength, glass transition temperature is high, physicochemical stability is good, solute permeability height etc. is excellent
Performance and the dialysis membrane for being used as haemodialyser.But polyether sulfone materials belong to hydrophobic material, therefore before as dialysis membrane, need
Hydrophilicity-imparting treatment is carried out to it.And therefore polyether sulfone, is ensuring solute also there is the defects of certain in terms of biocompatibility
Also certain biocompatibility is taken into account while clearance rate, phenomena such as avoiding that blood coagulation occurs in blood dialysis.In addition,
Existing dialysis membrane can only remove the metabolic waste in blood by way of disperse, convection current, lead to if dialysis membrane can be assigned
The function of part metabolic waste can also be removed by crossing absorption, then will greatly improve the clearance rate of metabolic waste.
Based on this, the application is made.
The content of the invention
For the drawbacks described above present in existing dialysis membrane, it is steady that the application provide firstly a kind of high mechanical strength, chemistry
Qualitative and good biocompatibility, ultrafiltrate coefficient are high, Solute removal rate is high, the PES hollow cored fibre of complement activation can be avoided to dialyse
Film.
To achieve the above object, the technical scheme that the application takes is as follows：
A kind of PES hollow cored fibre dialysis membrane, its casting solution form as follows by weight percentage：
Polyethersulfone resin 10-25%；
Diatomite 1-4%；
Amphipathic copolymer 1-5%；
Organic pore-foaming agent 4-12%；
The polymer 2-6% of good biocompatibility；
Solvent：According to the content of above each component, fluid infusion to 100%.
Further, as preferred：
Described polyether sulfone number-average molecular weight is 20000-60000.
Described polyethersulfone resin weight percent content is 15-20%.
Described diatomite is the diatomite with nano micropore structure.Research is found：Diatomite has porous, more equal
The property such as even particle diameter distribution and pore-size distribution, absorption, added in casting solution provided herein with above-mentioned characteristic
Diatomite, can not only improve the mechanical strength and ultrafiltrate coefficient of hollow fibre dialysis membrane, and can also optionally adsorption section
Divide metabolic waste, the i.e. absorption of the third reset mode of dialysis membrane is assigned, so as to effectively increase its clearance rate.
Described diatomaceous weight percent content is 2-3%.
Described amphipathic copolymer is polyoxyethylene-poly-oxypropylene polyoxyethylene, polyether modified silicon oil, poly- methyl-prop
Any of e pioic acid methyl ester-polystyrene or several mixtures.Amphipathic copolymer is to contain hydrophilic segment simultaneously and dredge
The block copolymer of water segment, hydrophilic segment are enriched in the surface of film in the preparation process of film, can significantly improve the parent of film
Water-based and ultrafiltrate coefficient, its hydrophilicity is assigned from membrane structure, without carrying out extra hydrophilic treated；And hydrophobic segment
In the presence of making amphipathic copolymer and polyether sulfone that there is good compatibility, ensure that the stability and persistence of membrane structure.
The weight percent content of described amphipathic copolymer is 2-4%.
Described organic pore-foaming agent be selected from polyethylene glycol, polyoxyethylene, PEO, polyvinyl alcohol, methylcellulose,
Any of ethylene glycol, propane diols, glycerine or several mixtures, organic pore-foaming agent can effectively improve the hollow fibre of polyether sulfone
Tie up the performances such as microcellular structure, porosity and the infiltration of dialysis membrane.
The weight percent content of organic pore-foaming agent is preferably 6-12%.
Any of the polymer of the good biocompatibility in polyvinylpyrrolidone, polymethyl methacrylate
Kind.
The weight percent content of the polymer of described good biocompatibility is 3-5%.
Described solvent is selected from dimethylformamide, dimethyl acetamide, dimethyl sulfoxide (DMSO), 1-METHYLPYRROLIDONE, phosphorus
One or more in sour trimethyl, triethyl phosphate.
The internal diameter of described PES hollow cored fibre dialysis membrane is 400-500um, wall thickness 50-100um.
Present invention also provides a kind of preparation method of PES hollow cored fibre dialysis membrane as characterized above, and it prepares step
It is rapid as follows：
（1）The casting solution each component of above-mentioned PES hollow cored fibre dialysis membrane is put into agitator tank in proportion, in 55-85 DEG C of temperature
Stirred under degree, standing and defoaming, the casting solution of 40-70 DEG C of acquisition；
（2）Dry-wet spinning technique spinning hollow fiber dialysis membrane：Above-mentioned casting solution is extruded by spinning head, by 5-500mm's
Dry-spinning path, coagulation system solidification, cleaning device cleaning, drying unit drying, are finally collected by filament winding device.
Further, as preferred：
Step（2）In, in described solidification process, its coagulation bath temperature is controlled at 25-55 DEG C, and coagulating bath is water or water and solvent
Mixed solution.
Step（2）In, two kinds of solution are extruded in described spinning head simultaneously, one kind is casting solution, and another kind is with 25-55
DEG C water or 25-55 DEG C of water and casting solution in solvent composition formed mixed solution, 25-55 DEG C of the water or its with
The mixed solution that solvent is formed is also referred to as core liquid, and the core liquid passes through spinning nozzle simultaneously with casting solution.
Step（2）In, in described matting, cleaning bath water temperature control is at 30-90 DEG C, stroke 5-20m.
The operation principle of the application and have the beneficial effect that：
（1）The application carries out the processing of hollow fibre dialysis membrane using dry-wet spinning technique, and whole process only prepares casting
Film liquid and the step of spinning two can be completed, and preparation method is simple, and production efficiency is high；Above-mentioned technique, can without extra scrap build
Completed in the dry-wet spinning equipment of routine, and propose particularly harsh want between two procedures in itself to equipment
Ask, thus universality is strong, cost is relatively low, is suitable for industrialized production.
（2）The casting solution of the application is mainly by polyethersulfone resin, diatomite, amphipathic copolymer, organic pore-foaming agent, biology
The good polymer of compatibility and solvent are formed, and while it gives full play to polyethersulfone resin good mechanical properties, are equipped with diatom
Native and organic pore, its new absorption property is assigned, improve its clearance rate, and gather by amphipathic copolymer, biocompatibility
The setting of compound and solvent, its hydrophily and biocompatibility are assigned from structure, so as to make obtained hollow fibre dialysis membrane
Itself has high mechanical properties, good biocompatibility, permanent hydrophily, high ultrafiltrate coefficient and high clearance rate.
（3）In the application, diatomite using having nano level microcellular structure, its have highly uniform particle diameter distribution and
The properties such as pore-size distribution, absorption, therefore, diatomite is added in casting solution, can not only improve the machine of hollow fibre dialysis membrane
Tool intensity, ultrafiltrate coefficient, and can also optionally absorbed portion metabolic waste, improve clearance rate.
（4）It is the block copolymer containing hydrophilic segment and hydrophobic segment simultaneously using amphipathic copolymer in the application,
Hydrophilic segment is enriched in the surface of film in film forming procedure, is blended into PES hollow cored fibre dialysis membrane a small amount of amphipathic
Copolymer is the hydrophily for being remarkably improved film；And according to similar compatibility principle, the presence of hydrophobic segment, make amphipathic copolymer
There is good compatibility with polyether sulfone, and adhesion is strong, and amphipathic copolymer not easily runs off during film use, ensures
The durable hydrophilic property of film.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, those skilled in the art
Various changes or modification can be made to the present invention, these equivalent form of values equally fall within the model that the application appended claims are limited
Enclose.
First, the mixing that the present embodiment is carried out to each technological parameter in preparation process between single factor test and blocking factor is real
Test, the results showed that：Spray two kinds of solution in spinning head at the same time, i.e. casting solution and during core liquid, good hollow aperture can be achieved
Control, therefore, core liquid are particularly suitable for use in " 25-55 DEG C of water " and " 25-55 DEG C of water+solvent " two ways, itself and casting film liquid temperature
Degree is different, and different film-formation results can be achieved；There is similar principle with spinneret, be applied equally to solidify in process is solidified
Liquid is particularly suitable for use in " 25-55 DEG C of water " and " 25-55 DEG C of water+solvent " two ways.
Secondly, the application also tests to the component of casting solution, the results showed that：When polyethersulfone resin 10-25%, diatom
Native 1-4%, amphipathic copolymer 1-5%, organic pore-foaming agent 4-12%, the polymer 2-6% of good biocompatibility, surplus are mended with solvent
When liquid is to 100%, good using effect can be achieved, especially as polyethersulfone resin 15-20%, diatomite 2-3%, amphipathic common
Polymers 2-4%, organic pore-foaming agent 6-12%, the polymer 3-5% of good biocompatibility, surplus with solvent fluid infusion to 100% when, gained
To mechanical performance, biocompatibility, hydrophily, ultrafiltrate coefficient and the clearance rate of PES hollow cored fibre dialysis membrane reach most
It is good.
The method of testing of the related performance indications of PES hollow cored fibre dialysis membrane is referring to document：Zou Wet.al.,
Journal of Membrane Science, 2010,358：76.
Application scheme is specifically described with three embodiments below.
Embodiment 1
(1) it is used for casting solution raw material by following component and weight percent to be uniformly dissolved in agitator tank, whipping temp 70
DEG C, standing and defoaming obtains casting solution, and casting solution temperature is 50 DEG C.
Component：Polyethersulfone resin 15%, diatomite 3%, amphipathic copolymer（It is preferably polyether-modified silicon in the present embodiment
Oil）4%th, organic pore-foaming agent（It is preferably polyethylene glycol in the present embodiment）8%th, the polymer of good biocompatibility（In the present embodiment
Preferably polyvinylpyrrolidone）4%th, solvent（It is preferably dimethyl acetamide in the present embodiment）66%.
(2) with conventional dry-wet spinning processing line spinning hollow fiber dialysis membrane.Casting solution is after filter screen, and core
Liquid is together extruded by spinning head, after the 10cm that walks in atmosphere, is cleaned through coagulating bath shaping, cleaner bath, drying machine drying, finally
Collected by filament winding device.Wherein, core liquid is 30% dimethylacetamide amine aqueous solution, and temperature is 30 DEG C；Coagulating bath is the two of 20%
Methyl vinyl amine aqueous solution, temperature are 40 DEG C；It is 60 DEG C to clean bath temperature, and cleaning stroke is 12m；Gained PES hollow cored fibre
The internal diameter of dialysis membrane is 450um, wall thickness 60um.
(3) gained PES hollow cored fibre dialysis membrane measures pure water contact angle 50o；After filtering albumin solution, pure water leads to
The response rate of amount is 90%；The mL/m of ultrafiltrate coefficient 322·h·mmHg；To β2The clearance rate of microglobulin is 82%.
Embodiment 2
(1) it is used for casting solution raw material by following component and weight percent to be uniformly dissolved in agitator tank, whipping temp 70
DEG C, standing and defoaming obtains casting solution, and casting solution temperature is 50 DEG C.
Component：Polyethersulfone resin 16%, diatomite 2%, amphipathic copolymer（It is preferably polymethylacrylic acid in the present embodiment
Methyl esters-polystyrene）3%th, organic pore-foaming agent（It is preferably in the present embodiment：Polyethylene glycol 5%+ glycerine 3%）8%th, bio-compatible
The good polymer of property（It is preferably polyvinylpyrrolidone in the present embodiment）4%th, solvent（It is preferably dimethyl second in the present embodiment
Acid amides）67%.
(2) with conventional dry-wet spinning technique spinning hollow fiber dialysis membrane.Casting solution is after filter screen, and core liquid
Together extruded by spinning head, in atmosphere walk 25cm after, through coagulating bath shaping, cleaner bath cleaning, drying machine drying, finally by
Filament winding device is collected.Wherein, core liquid is 30% dimethylacetamide amine aqueous solution, and temperature is 30 DEG C；Coagulating bath is 10% diformazan
The yl acetamide aqueous solution, temperature are 40 DEG C；It is 70 DEG C to clean bath temperature, and cleaning stroke is 16m；Gained PES hollow cored fibre is saturating
The internal diameter for analysing film is 450um, wall thickness 50um.
(3) gained PES hollow cored fibre dialysis membrane measures pure water contact angle 48o；After filtering albumin solution, pure water leads to
The response rate of amount is 92%；The mL/m of ultrafiltrate coefficient 302·h·mmHg；To β2The clearance rate of microglobulin is 79%.
Embodiment 3
(1) it is used for casting solution raw material by following component and weight percent to be uniformly dissolved in agitator tank, whipping temp 75
DEG C, standing and defoaming obtains casting solution, and casting solution temperature is 55 DEG C.
Component：Polyethersulfone resin 18%, diatomite 2%, amphipathic copolymer（It is preferably polyether-modified silicon in the present embodiment
Oil）2%th, organic pore-foaming agent（It is preferably polyethylene glycol in the present embodiment）10%th, the polymer of good biocompatibility（In the present embodiment
Preferably polymethyl methacrylate）3%th, solvent（It is preferably dimethyl sulfoxide (DMSO) in the present embodiment）65%.
(2) with conventional dry-wet spinning technique spinning hollow fiber dialysis membrane.Casting solution is after filter screen, and core liquid
Together extruded by spinning head, in atmosphere walk 30cm after, through coagulating bath shaping, cleaner bath cleaning, drying machine drying, finally by
Filament winding device is collected.Wherein, core liquid is 20% dimethyl sulphoxide aqueous solution, and temperature is 30 DEG C；Coagulating bath is 10% dimethyl
The sulfoxide aqueous solution, temperature are 50 DEG C；It is 80 DEG C to clean bath temperature, and cleaning stroke is 20m；Gained PES hollow cored fibre dialysis membrane
Internal diameter be 500um, wall thickness 50um.
(3) gained PES hollow cored fibre dialysis membrane measures pure water contact angle 52o；After filtering albumin solution, pure water leads to
The response rate of amount is 89%；The mL/m of ultrafiltrate coefficient 352·h·mmHg；To β2The clearance rate of microglobulin is 86%.
Claims (10)
1. a kind of PES hollow cored fibre dialysis membrane, it is characterised in that its casting solution forms as follows by weight percentage：
Polyethersulfone resin 10-25%,
Diatomite 1-4%,
Amphipathic copolymer 1-5%,
Organic pore-foaming agent 4-12%,
The polymer 2-6% of good biocompatibility,
Solvent：According to the content of above each component, fluid infusion to 100%；
The internal diameter for the PES hollow cored fibre dialysis membrane that the casting solution film forming is formed is 400-500um, wall thickness 50-100um.
A kind of 2. PES hollow cored fibre dialysis membrane as claimed in claim 1, it is characterised in that：Described polyether sulfone number is divided equally
Son amount is 20000-60000.
A kind of 3. PES hollow cored fibre dialysis membrane as claimed in claim 1, it is characterised in that：Described amphipathic copolymer
For any of polyoxyethylene-poly-oxypropylene polyoxyethylene, polyether modified silicon oil, polymethyl methacrylate-polystyrene
Or several mixture.
A kind of 4. PES hollow cored fibre dialysis membrane as claimed in claim 1, it is characterised in that：Described organic pore-foaming agent choosing
From appointing in polyethylene glycol, polyoxyethylene, PEO, polyvinyl alcohol, methylcellulose, ethylene glycol, propane diols, glycerine
One or more of mixtures.
A kind of 5. PES hollow cored fibre dialysis membrane as claimed in claim 1, it is characterised in that：The good biocompatibility
Polymer is selected from any of polyvinylpyrrolidone, polymethyl methacrylate.
A kind of 6. PES hollow cored fibre dialysis membrane as claimed in claim 1, it is characterised in that：Described solvent is selected from diformazan
One kind in base formamide, dimethyl acetamide, dimethyl sulfoxide (DMSO), 1-METHYLPYRROLIDONE, trimethyl phosphate, triethyl phosphate
It is or several.
7. the preparation method of PES hollow cored fibre dialysis membrane as claimed in claim 1, it is characterised in that：
（1）The casting solution each component of above-mentioned PES hollow cored fibre dialysis membrane is put into agitator tank in proportion, in 55-85 DEG C of temperature
Stirred under degree, standing and defoaming, the casting solution of 40-70 DEG C of acquisition；
（2）Dry-wet spinning technique spinning hollow fiber dialysis membrane：Above-mentioned casting solution is extruded by spinning head, by 5-500mm's
Dry-spinning path, coagulation system solidification, cleaning device cleaning, drying unit drying, are finally collected by filament winding device.
8. the preparation method of PES hollow cored fibre dialysis membrane as claimed in claim 7, it is characterised in that：Step（2）In, institute
In the solidification process stated, its coagulation bath temperature is controlled at 25-55 DEG C, and coagulating bath is water or the mixed solution of water and solvent.
9. the preparation method of PES hollow cored fibre dialysis membrane as claimed in claim 7, it is characterised in that：Step（2）In, institute
In the spinning head stated while two kinds of solution are extruded, one kind is casting solution, and another kind is with 25-55 DEG C of water or 25-55 DEG C
The mixed solution that water is formed with the solvent composition in casting solution.
10. the preparation method of PES hollow cored fibre dialysis membrane as claimed in claim 7, it is characterised in that：Step（2）In,
In described matting, cleaning bath water temperature control is at 30-90 DEG C, stroke 5-20m.
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Cited By (6)
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| CN108816062A (en) * | 2018-06-27 | 2018-11-16 | 苏州市贝克生物科技有限公司 | polyamide-alginate fibre dialysis membrane and preparation method thereof |
| CN112121645A (en) * | 2020-10-09 | 2020-12-25 | 江西三鑫医疗科技股份有限公司 | Preparation method of hollow fiber membrane for dialysate filter |
| CN112221361A (en) * | 2020-09-15 | 2021-01-15 | 大连理工大学 | Polyether sulfone/copolyether sulfone blended hollow fiber hemodialysis membrane with phthalazinone structure and preparation method thereof |
| CN112221360A (en) * | 2020-09-15 | 2021-01-15 | 大连理工大学 | Copolymerized ether sulfone hemodialysis membrane containing phthalazinone structure and preparation method thereof |
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| CN112121645A (en) * | 2020-10-09 | 2020-12-25 | 江西三鑫医疗科技股份有限公司 | Preparation method of hollow fiber membrane for dialysate filter |
| CN113072714A (en) * | 2021-04-02 | 2021-07-06 | 齐鲁工业大学 | Method for preparing nano lignin balls from corn straws |
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