CN1375351A - Production process of hollow blended polyether sulphone fiber dialysis membrane - Google Patents
Production process of hollow blended polyether sulphone fiber dialysis membrane Download PDFInfo
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- CN1375351A CN1375351A CN 01139267 CN01139267A CN1375351A CN 1375351 A CN1375351 A CN 1375351A CN 01139267 CN01139267 CN 01139267 CN 01139267 A CN01139267 A CN 01139267A CN 1375351 A CN1375351 A CN 1375351A
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Abstract
The production method of new-type blended polyether sulphone hollow fiber dialysis membrane is characterized by that it uses polyether sulphone as main membrane-making material and uses other high polymers to make blending so as to obtain the invented hollow fibre dialysis membrane which possesses high strnegth, high compressive resistance, high disinfection resistance and good biological intermiscibility, and can change its property in large range, so that it can be suitable for the requirements of various dialyzation and superfilters.
Description
Technical field:
The present invention relates to macromolecular material dialysis membrane technical field.Be specifically related to a kind of manufacture method of novel blend polyethersulfone doughnut dialysis membrane.
Background of invention:
Tradition chemical process separation method commonly used has screening, filtration, centrifugation, concentrates, distillation, evaporation, extraction, recrystallization etc.But for higher level separation, as the separation of molecule or ion size, the separation of each component etc. in the biological solution is adopted traditional separation method to be difficult to realize, or is not reached precision, or big consumes energy and do not have practical value.Appearance and application with macromolecular material of Selective Separation function are readily solved an above-mentioned separation difficult problem.The membrane separation technique of setting up from nineteen sixties, obtain to develop rapidly, be widely used in the every field of liquid and gas separation at present because of having series of advantages.
Membrane separation technique can make fluid-mixing (liquid or gas) separate by the component difference, can purify or concentrate by convection cell again.It comes into one's own with flourish because of having following advantage: do not have phase-state change when separating, so needn't heat or freezing, also need not to add other reagent, so energy consumption reduces, and do not produce secondary pollution; Device structure is simple, and is easy to operate, and floor space is little, and cost is low, helps carrying out serialization production and control automatically; The material that can make some be difficult to separate by conventional method is achieved separation as the material of azeotropic mixture, boiling point approaching mixture, heat-sensitive substance or poor chemical stability.
Diffusion barrier has various ways, as flat sheet membrane, rolled film, tubular membrane, inverted pleat film and hollow-fibre membrane etc.Wherein the separation instrument that is assembled into by hollow-fibre membrane has the advantages that minimum volume is arranged under same membrane area.
Goal of the invention:
The objective of the invention is to develop have high strength, anti-compactibility, anti-sterilization, good biocompatibility and can in a big way, change the hollow-fibre membrane of the performance of film.
The present invention is the main material of preparing except that adopting polyether sulfone, also uses other high polymers to carry out blend with it.Polymer blend is polymer or copolymer or the cellulose and the ester class thereof of polyethylene base class.Most of polymer all is inconsistent, and promptly two kinds of polymer are dissolved in the solvent or when making membrane material, they are not to be that unit mixes mutually with the molecule jointly, but each self-forming phase farmland and mixing mutually independently.The size on phase farmland is relevant with the compatibility of two kinds of polymer: be separated into independently two-phase as complete incompatible its blend solution of two kinds of polymer; The high polymer that compatibility is fabulous can be dissolved into the solution of homogeneous phase; Compatibility is between the two above-mentioned, each self-forming phase farmland independently then, and be that unit is dispersed in the solution with the phase farmland, the better person of compatibility, the size on phase farmland is less, and the hole between the phase farmland is also less, so the pore size that forms after the film forming is also less; Compatibility chump, the independent phase farmland in the solution is bigger, and the hole between the phase farmland is also bigger, so the pore size that forms after the film forming is also bigger.Utilize this characteristics, select polymer blend, promptly can be made into the different serial hollow-fibre membrane of performance.
Summary of the invention:
The invention provides a kind of manufacture method of novel blend polyethersulfone doughnut dialysis membrane, this method comprises the following steps:
1. raw material and composition: (percentage by weight)
Polyether sulfone (η=0.4～0.8) 8～30%
Polymer blend 0.1～10%
Pore-foaming agent 1～30%
Solvent 50～90%
2. the preparation of spinning solution:
With above-mentioned raw materials by the prescription weighing after, be placed on earlier in the dissolution kettle, under the control of 50～90 ℃ temperature program(me)s, vigorous stirring 6～10 hours makes abundant swelling and dissolving, after filtration, after deaeration purifies, make spinning solution;
3. the spinning of doughnut:
The compressed air of spinning solution is pressed after spinning pipeline and the accurate metering of measuring pump from the spinning bucket, stoste enters candle filter and carries out last filtration together, the spinning head of forming through the circular concentric pipe is clamp-oned in the air again, and the stoste thread enters coagulating bath (coagulating bath is made up of solvent and water) and is frozen into nascent hollow-fibre membrane behind the air layer of certain altitude;
4. the manufacturing of doughnut dialysis membrane:
Nascent hollow-fibre membrane is blend polyethersulfone doughnut dialysis membrane of the present invention through 2～4 road biaxial tensiones with after protecting hole processing and drying.
In the inventive method: above-mentioned polymer blend is polymer or copolymer, cellulose and the ester class thereof of polyethylene base class; They can use separately, also can mix use; Pore-foaming agent is organic or inorganic compounds such as aluminium chloride, sodium nitrate such as PVP or PEG; Solvent is dimethylacetylamide, dimethyl formamide, dimethyl sulfoxide (DMSO) or N a---methyl pyrrolidone.
The technological parameter of spinning doughnut dialysis membrane is:
Measuring pump rotating speed (r/min) 6～40
Spinning pressure (Mpa) 0.3～0.6
Filling liquid pressure (Mpa) 0.001～0.06
Filling liquid concentration (wt%) 0～50
Dry-spinning path length (mm) 40～450
Coagulating bath concentration (wt%) 0.1～50
The former liquid temp of extruding spinning (℃) 30～60
Coagulation bath temperature (℃) 30～50
Coagulating bath internal circulating load (l/h) 5～40
Spinning speed (m/min) 10～50
Radial drawing rate (%) 0～100
Axial tension rate (%) 0～300
Need to be pressed into filling liquid at the spinning head inner chamber in above-mentioned spinning process, the filling liquid composition is the aqueous solution of the aqueous solution, aqueous acetone solution or the alcohols of solvent.
The component of above-mentioned coagulating bath is the aqueous solution of solvent.
In the above-mentioned spinning process, the present invention introduces new ideas " biaxial tension " and is put to process implementing.The spinning of traditional film does not generally stretch or carries out a spot of unidirectional (axially) stretching; Chemical fibre then must adopt powerful axial tension, the stretching result makes big molecule be orientated along draw direction, the longitudinal strength of fiber is obviously increased, transverse strength then reduces, because of fiber in use only utilizes its longitudinal strength, and very little with the transverse strength relation, therefore, the result of stretching improves the mechanical strength of fiber significantly.Hollow-fibre membrane is different with general fibre, and it not only needs higher longitudinal strength, needs good radial strength simultaneously.Therefore, it is inapt using traditional unidirectional (axially) to stretch, because it has but reduced transverse strength when strengthening longitudinal strength, whole film strength also thereby descend.That the present invention adopts is two-way (axially and radially) draws the method for stretching, and both can change the shortcoming of said method, and whole film strength is improved to some extent, and makes on the film micropore shape more regular, and draw ratio more approaches one.
It is main material of preparing that the present invention uses polyether sulfone, compares with traditional material of preparing polysulfones of function admirable, and polyether sulfone has following characteristics: the pore size of film is more easy to control, and higher selection separation property is arranged; Film strength is higher, has anti-destructive preferably; Sensitiveness under the better chemical stability, operating condition obviously reduces, and arranged long service life under load, and the chemical scope of application is wider; Excellent heat resistance energy, Tg are higher about 40 ℃ than polysulfones, so higher anti-moise-heat sterilization is arranged; Has better blood compatibility.
The apparent size of a kind of novel blend polyethersulfone doughnut dialysis membrane that the present invention makes, can be according to different purposes and regulated at will and determining: length be 300～1200mm; Thickness 30～250 μ m; External diameter 220～1400 μ m.
The blend polyethersulfone hollow-fibre membrane that the present invention makes can be assembled into various dialyzers, also can be made into multiple ultrafilter by its performance difference, is used separately as the processing of the purifying of various dialyzers, water and processor, various industrial wastes and recovery etc.
Embodiment 1
Prepare burden by following component and composition: polyether sulfone 16%; Acrylonitrile copolymer 2%; PVP4%; DMSO78%.Above-mentioned raw material add in the dissolvers, and under 40～90 ℃ of temperature program(me)s controls, spinning solution was made in swelling and dissolving in 6 hours, after filtration, be spun into film after the deaeration.The film-forming process parameter is: measuring pump volume 0.35ml/r, revolution speed 12r/min; Air bath length 160mm; Coagulating bath concentration is 10% solvent, one aqueous solution; Spinning speed is 30m/min.Make film through biaxial tension, washing and protect that the hole is handled and dry after, be assembled into the high flux artificial kidney dialyzer.The dialyzer water flux is 410ml/h.Kpa; Flesh liver transmitance is 90%; The urea transmitance is 93%
Embodiment 2
15 parts of polyether sulfones, 3 parts of polyacrylamides, 6 parts of PEG are dissolved in 76 parts of dimethylacetylamides.Swelling and be dissolved in the control of 40～80 ℃ of temperature program(me)s down, 7 hours time.Spinning solution spins film forming behind purification process such as deaeration, filtration.The film-forming process parameter is: measuring pump volume 0.35ml/r; Revolution speed 25r/min; Air bath length 200mm; The solvent of coagulating bath concentration 5%---the aqueous solution; Spinning speed 26m/min.Make hollow-fibre membrane after biaxial tension, washing and protecting hole processing and drying, be assembled into the terminal handler of sterile deionized water, this device is under the ultrafiltration pressure of 0.1Mpa, and water flux can reach 600l/h.
Claims (5)
1. the manufacture method of a novel blend polyethersulfone doughnut dialysis membrane is characterized in that this method comprises the following steps:
(1) raw material and composition: (percentage by weight)
Polyether sulfone (η=0.4～0.8) 8～30%
Polymer blend 0.1～10%
Pore-foaming agent 1～30%
Solvent 50～90%
(2) preparation of spinning solution:
With above-mentioned raw materials by the prescription weighing after, be placed on earlier in the dissolution kettle, under the control of 50～90 ℃ temperature program(me)s, vigorous stirring 6～10 hours makes abundant swelling and dissolving, after filtration, after deaeration purifies, make spinning solution;
(3) spinning of doughnut:
The compressed air of spinning solution is pressed after spinning pipeline and the accurate metering of measuring pump from the spinning bucket, stoste enters candle filter and carries out last filtration together, the spinning head of forming through the circular concentric pipe is clamp-oned in the air again, the stoste thread enters coagulating bath behind the air layer of certain altitude, be frozen into nascent hollow-fibre membrane;
(4) manufacturing of doughnut dialysis membrane:
Nascent hollow-fibre membrane is through 2～4 road biaxial tensiones and protect the hole processing, makes blend polyethersulfone doughnut dialysis membrane after the drying.
2. the manufacture method of a kind of novel blend polyethersulfone doughnut dialysis membrane according to claim 1 is characterized in that wherein said polymer blend is polymer or copolymer, cellulose and the ester class thereof of polyethylene base class; They can use separately, also can mix use; Pore-foaming agent is organic matter or inorganic compounds such as aluminium chloride, sodium nitrate such as PVP or PEG; Solvent is dimethylacetylamide, dimethyl formamide, dimethyl sulfoxide (DMSO) or N a---methyl pyrrolidone; Protecting the hole agent is monohydric alcohol, dihydroxylic alcohols or trihydroxylic alcohol, can use wherein a kind of separately, also can several mix and use.
3. the manufacture method of a kind of novel blend polyethersulfone doughnut dialysis membrane according to claim 1 is characterized in that the technological parameter that spins the doughnut dialysis membrane is:
Measuring pump rotating speed (r/min) 6～40
Spinning pressure (Mpa) 0.3～0.6
Filling liquid pressure (Mpa) 0.001～0.06
Filling liquid concentration (wt%) 0～50
Dry-spinning path length (mm) 40～450
Coagulating bath concentration (wt%) 0.1～50
The former liquid temp of extruding spinning (℃) 30～60
Coagulation bath temperature (℃) 30～50
Coagulating bath internal circulating load (l/h) 5～40
Spinning speed (m/min) 10～50
4. the manufacture method of a kind of novel blend polyethersulfone doughnut dialysis membrane according to claim 1 is characterized in that wherein said coagulating bath is made up of solvent and water.
5. the manufacture method of a kind of novel blend polyethersulfone doughnut dialysis membrane according to claim 1, the thickness that it is characterized in that film are 30～250 μ m; Length is 300～1200mm; External diameter is 220～1400 μ m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01139267 CN1375351A (en) | 2001-12-28 | 2001-12-28 | Production process of hollow blended polyether sulphone fiber dialysis membrane |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01139267 CN1375351A (en) | 2001-12-28 | 2001-12-28 | Production process of hollow blended polyether sulphone fiber dialysis membrane |
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| CN1375351A true CN1375351A (en) | 2002-10-23 |
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| CN 01139267 Pending CN1375351A (en) | 2001-12-28 | 2001-12-28 | Production process of hollow blended polyether sulphone fiber dialysis membrane |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004096418A1 (en) * | 2003-05-01 | 2004-11-11 | Tsinghua University | Hollow fiber ultrafilter membrane with poly(phthalazinone ether fulfone), poly(phthalazinone ether ketone) or poly(phthalazinone ether sulfone ketone) and preparation thereof |
| CN1317057C (en) * | 2005-01-31 | 2007-05-23 | 成都欧赛医疗器械有限公司 | Hollow fibrous membranes of modified poly(ether sulfone) and their production |
| CN100386136C (en) * | 2006-01-17 | 2008-05-07 | 亚美滤膜（南通）有限公司 | Method for producing porose semi-permeation filtering film |
| CN101209396B (en) * | 2006-12-31 | 2011-07-06 | 山西金泉合成纤维制造有限公司 | Blended polysulfone hollow fiber film and preparation method |
| CN103301759A (en) * | 2013-06-22 | 2013-09-18 | 威海威高血液净化制品有限公司 | Polysulfone hollow fiber dialysis membrane and preparation method thereof |
| CN105233711A (en) * | 2015-10-31 | 2016-01-13 | 宁波欧梵卫浴有限公司 | Preparation method for water-purifying polysulfone hollow fiber membrane |
| CN105233712A (en) * | 2015-10-31 | 2016-01-13 | 宁波欧梵卫浴有限公司 | Preparation method for water-purifying polyether sulfone hollow fiber membrane |
| CN105363358A (en) * | 2015-12-14 | 2016-03-02 | 苏州君康医疗科技有限公司 | Polyether sulfone/poly butylene carbonate hollow fiber blend membrane and preparation method thereof |
-
2001
- 2001-12-28 CN CN 01139267 patent/CN1375351A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004096418A1 (en) * | 2003-05-01 | 2004-11-11 | Tsinghua University | Hollow fiber ultrafilter membrane with poly(phthalazinone ether fulfone), poly(phthalazinone ether ketone) or poly(phthalazinone ether sulfone ketone) and preparation thereof |
| CN1317057C (en) * | 2005-01-31 | 2007-05-23 | 成都欧赛医疗器械有限公司 | Hollow fibrous membranes of modified poly(ether sulfone) and their production |
| CN100386136C (en) * | 2006-01-17 | 2008-05-07 | 亚美滤膜（南通）有限公司 | Method for producing porose semi-permeation filtering film |
| CN101209396B (en) * | 2006-12-31 | 2011-07-06 | 山西金泉合成纤维制造有限公司 | Blended polysulfone hollow fiber film and preparation method |
| CN103301759A (en) * | 2013-06-22 | 2013-09-18 | 威海威高血液净化制品有限公司 | Polysulfone hollow fiber dialysis membrane and preparation method thereof |
| CN103301759B (en) * | 2013-06-22 | 2016-01-13 | 威海威高血液净化制品有限公司 | A kind of hollow polysulfone fiber dialysis membrane and manufacture method thereof |
| CN105233711A (en) * | 2015-10-31 | 2016-01-13 | 宁波欧梵卫浴有限公司 | Preparation method for water-purifying polysulfone hollow fiber membrane |
| CN105233712A (en) * | 2015-10-31 | 2016-01-13 | 宁波欧梵卫浴有限公司 | Preparation method for water-purifying polyether sulfone hollow fiber membrane |
| CN105363358A (en) * | 2015-12-14 | 2016-03-02 | 苏州君康医疗科技有限公司 | Polyether sulfone/poly butylene carbonate hollow fiber blend membrane and preparation method thereof |
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