CN101288831B - Forming method and device of hollow fiber blood filtering membrane - Google Patents

Forming method and device of hollow fiber blood filtering membrane Download PDF

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CN101288831B
CN101288831B CN2008101239090A CN200810123909A CN101288831B CN 101288831 B CN101288831 B CN 101288831B CN 2008101239090 A CN2008101239090 A CN 2008101239090A CN 200810123909 A CN200810123909 A CN 200810123909A CN 101288831 B CN101288831 B CN 101288831B
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pressure
container
distributing pipe
filtering membrane
blood filtering
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CN101288831A (en
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张亚琴
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Abstract

The invention relates to a forming method of a hollow fibre blood filter film; spinning solution with given rotation viscosity is delivered to a sealed container; clean gas with the pressure of 0.01-0.10MPa is pumped into the container; the spinning solution is sprayed out of an external hole of a dual-hole spinneret with the flux of 0.1-10ml/min through a distribution pipe that is horizontally arranged under the gas pressure; the filling liquid is sprayed out of an internal hole with the flux of 0.05-5ml/min under the pressure of 0.01-0.10MPa; after being solidified by air, the primary fibre enters water bath and is solidified, formed and wound to gain the filter film; meanwhile, a pressure sensor feeds the fluid pressure signals at the distribution pipe back to a controller which controls the air inlet pressure of the container, thus keeping stable liquid outlet flux of the dual-hole spinneret. The forming method of the invention keeps stable liquid outlet flux of the dual-hole spinneret by controlling the pressure in the container, which has simple technology, uniform and smooth film wall of the product and good continuity, and facilitates the industrialized production.

Description

The manufacturing process of doughnut blood filtering membrane and device thereof
Technical field
The present invention relates to a kind of manufacturing process and device thereof of doughnut blood filtering membrane, belong to the tunica fibrosa manufacture technology field.
Background technology
Polyether sulfone or polysulfones are special engineering plastics, and because of its vitrification point height, physical and chemical performance is stable, and through for many years improvement and perfect, are blood purification at present with one of main material of film.The hollow-fibre membrane made from polyether sulfone or polysulfones has nontoxic, anti-several different methods sterilization, the biocompatibility excellence, and the property removed is better than characteristics such as general hollow-fibre membrane.But the doughnut film production that is used for haemodialysis requires to require height than common hollow-fibre membrane, not only require hollow-fibre membrane to have suitable inside and outside footpath ratio, but also requirement has the membranous wall surface of uniform wall thickness and smooth rounding, to guarantee good withstand voltage properties and ultrafiltration performance.This in the throwing forming process, makes the spinning solution flow reach continuously with even with regard to the inevitable requirement hollow-fibre membrane as far as possible.But both at home and abroad on the make during the hollow fiber film, be the flow of controlling spinning solution by measuring pump at present, there is following problem in this spinning process: the hollow-fibre membrane wall unevenness of 1, making is even.Because the diameter of hollow-fibre membrane is less, no matter the measuring pump that adopts is gear pump or plunger displacement pump, in operation process, the liquid of output all can produce pulsation, and this pulsation causes pressure fluctuation, cause the flow and the pressure of the spinning solution of delivering to the spinning head place often to change, therefore cause spinning solution can not be consistent from the filter membrane wall thickness that spinning head is crushed to, and filter membrane surface fineness is not high, cause filter membrane micropore size inhomogeneous, cause the clearance rate of filter membrane not high, so that made hollow-fibre membrane is used for the haemodialysis effect is undesirable.On the other hand, because the pulsating nature of spinning solution feed flow makes the continuity of throwing descend,, increased manufacturing cost so the filter membrane yield rate is low.The clearance rate of the hollow-fibre membrane of 2, making is low.Because forming technology all adopts measuring pump that spinning solution is measured, carries, liquid is behind measuring pump, the pressure basic controlling of measuring pump is about 0.1~0.4Mpa, because pressure is relatively large, not only easily cause the leakage of spinning solution, noise is big, and because of spinning solution by the spinneret hole extrusion speed very fast, make between the fiber molecule and arrange after the extruding closely, so ultrafiltrate coefficient is generally at 10~20ml/hmmHg.3, be difficult for realizing industrialization production.It is a container with a measuring pump that present doughnut blood filtering membrane is shaped, and to a diplopore spinning head feed, because the production efficiency reduction is difficult to realize suitability for industrialized production.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of manufacturing process of doughnut blood filtering membrane is provided, directly controlling spinning solution with the steady pressure in the container is shaped from the diplopore spinning head, not only technology is simple, and the tunica fibrosa wall thickness that of being shaped is more even, membranous wall is more smooth, continuity is good, is convenient to industrialized production.
And the building mortion of doughnut blood filtering membrane provided by the present invention is simple in structure, can guarantee the quality of system film, and can the serialization industrial production.
The present invention is that the technical scheme that achieves the above object is: a kind of manufacturing process of doughnut blood filtering membrane is characterized in that: the spinning solution that rotary viscosity 600cp~9000cp (40 ℃) is contained polyether sulfone or polysulfones is delivered in the airtight container; In container, feed the clean gas of 0.01MPa~0.10MPa; Under the pressure of clean gas, spinning solution is through being horizontally set on the distributing pipe of external container, flow with 0.1~10ml/min sprays from the outer hole of concentric diplopore spinning head more than six on the distributing pipe, filling liquid is under the pressure of 0.01MPa~0.10MPa simultaneously, with the endoporus ejection of the flow of 0.05~5ml/min from the diplopore spinning head, as-spun fibre enters the water-bath solidification forming again behind air setting, reel, form the doughnut blood filtering membrane, pressure sensor feeds back to controller with the fluid pressure signal at distributing pipe place, controller with detected force value and setup pressure value relatively after, controller output signal control container admission pressure, keep the diplopore spinning head stable go out flow quantity.
The present invention makes the building mortion of above-mentioned doughnut blood filtering membrane, comprise airtight container, feed tube and filling pipe and concentric diplopore spinning head, it is characterized in that: described external container has horizontally disposed distributing pipe, and the container bottom distributing pipe communicates, six above diplopore spinning heads are housed on the distributing pipe, pressure sensor is housed on the distributing pipe, the air inlet pipeline on container top communicates with clean compressed gas source, and the control valve of regulator solution surface pressure is housed on the air inlet pipeline, filling pipe communicates with the endoporus of diplopore spinning head, the output of pressure sensor is connected with the input of controller, the output termination control valve of controller.
The present invention has the following advantages after adopting technique scheme: 1, doughnut blood filtration film properties improves.The present invention feeds the clean gas of pressure stability in closed container, spinning solution is under the effect of clean gas pressure, extrusion spinning liquid is to outside horizontally disposed distributing pipe place, outer hole from the diplopore spinning head sprays again, and the pressure sensor at distributing pipe place can in time feed back the pressure signal of spinning solution, in time regulate the admission pressure of container by controller, and keep spinning solution to go out the stability of flow quantity.Therefore the present invention can make spinning solution pass through the diplopore spinning head equably, continuously, makes smooth, even, the good spinnability of doughnut blood filtering membrane membranous wall of shaping.Because the filter membrane micropore of made of the present invention size evenly, the filtration film strength is higher, therefore has anti-destructive preferably, better chemical stability and good withstand voltage heat resistance, blood compatibility is further improved, and makes the performance of hollow-fibre membrane that bigger improvement arranged.2, clearance rate is good.The present invention is because spinning solution is even by the stability of flow at diplopore spinning head place, so it is even to make ground doughnut blood filtering membrane wall thickness, polyether sulfone or polysulfones molecular structure are arranged loose, and clearance rate is good, ultrafiltration rate height, its ultrafiltrate coefficient are that former measuring pump makes more than 5 times of filter membrane.3, easily realize suitability for industrialized production.The present invention has been owing to cancelled measuring pump, not only can solve to reveal and the problem of noise, and a container can realize a plurality of diplopore spinning head material sprays that production efficiency obviously improves, and can reduce production costs the realization industrialized production.4, building mortion is rational in infrastructure, simple, can improve spinning quality.The present invention is provided with pressure sensor at the distributing pipe place, make pressure sensor in time detect the flow of spinning solution by the diplopore spinning head, controller with detected force value and setup pressure value relatively after, the aperture of control and regulation valve, keep the interior liquid level pressure of container at 0.01MPa~0.10MPa, make the spinning solution rate of discharge keep stable and uniform, can make the uniform fibers film continuously, not only yield rate height, and spinning quality excellence.
Description of drawings
Below in conjunction with accompanying drawing embodiments of the invention are described in further detail.
Fig. 1 is the structural representation of the building mortion of doughnut blood filtering membrane of the present invention.
Wherein: the 1-air inlet pipeline, the 2-Pressure gauge, the 3-control valve, 4-fills pipe, 5-feed tube, 6-container, 7-distributing pipe, 8-diplopore spinning head, 9-pressure sensor, 10-digital display manometer, 11-controller.
The specific embodiment
See as shown in Figure 1, the building mortion of doughnut blood filtering membrane of the present invention comprises airtight container 6, feed tube 5 and fills pipe 4, distributing pipe 7, concentric diplopore spinning head 8 and pressure sensor 9, filling pipe 4 communicates with the endoporus of diplopore spinning head 8, fill in the pipe 4 filling liquid is housed, make the filter membrane of making keep hollow.Container of the present invention 6 outsides have horizontally disposed distributing pipe 7, to keep identical fluid pressure, container 6 bottoms communicate with distributing pipe 7, concentric diplopore spinning head 8 more than six is installed on the distributing pipe 7, this diplopore spinning head 8 can 8~20 be installed on the distributing pipe 7, pressure sensor 9 is contained in the distributing pipe 7, and digital display manometer 10 also is housed on the distributing pipe 7, can be observed the fluid pressure value at distributing pipe 7 places.The air inlet pipeline 1 on container 6 tops communicates with clean compressed gas source, the control valve 3 of regulator solution surface pressure and the Pressure gauge 2 of the gas pressure value in the demonstration air inlet pipeline 1 are housed on the air inlet pipeline 1, by the liquid level pressure in the control valve 3 control containers, and reach the stability of distributing pipe 7 place's fluid pressures, the input of the output termination controller 11 of pressure sensor 8 of the present invention, and the output termination pressure-regulating valve 3 of controller 11, this controller 11 can adopt single-chip microcomputer or Programmable Logic Controller, and pressure-regulating valve 3 can be magnetic valve, when controller 11 with detected fluid pressure value and setup pressure value relatively after, the aperture of output signal of telecommunication control and regulation valve 3, make container 6 internal pressure values keep stable, keep diplopore spinning head 8 stable go out flow quantity.
Embodiment 1
By weight percentage, polyether sulfone with 23%, 5% polyvinylpyrrolidone, 72% dimethylacetylamide under 80 ℃ of conditions, was dried 1 hour in the adding container 6, raw material and other components of oven dry are put into container 6, through under constant temperature, carrying out deaeration after swelling, stirring, the insulation then, make the spinning solution of rotary viscosity at 600cp~9000cp (40 ℃), spinning solution is delivered in the building mortion of the present invention.In container 6, feed the clean gas of 0.02MPa~0.06MPa, this clean gas is clean air or inert gas, as nitrogen, argon gas etc., under the pressure of clean gas, spinning solution is through being horizontally set on the distributing pipe 7 of container 6 outsides, spray from the outer hole of concentric diplopore spinning head 8 more than six on the distributing pipe 7 with 0.1~10ml/min flow, filling liquid is under the pressure of 0.01MPa~0.10MPa simultaneously, with the endoporus ejection of the flow of 0.05~5ml/min from diplopore spinning head 8, as-spun fibre is through the air section distance, solidification forming in the aqueous solution about 40 ℃ is reeled with 30~50m/min speed, forms the doughnut blood filtering membrane.Simultaneously, 9 fluid pressures to distributing pipe 7 places of pressure sensor detect in real time, and fluid pressure signal fed back to controller 11, controller 11 with detected force value and setup pressure value relatively after, controller 11 output signals control to adjust valve 3 actions at any time by controller 11, control container 6 admission pressures, keep diplopore spinning head 8 stable go out flow quantity, 10 fluid pressure signals of the digital display manometer on the distributing pipe 7 show.With the be shaped membrane area of the doughnut blood filtering membrane make of the inventive method is 1.2m 2, wall thickness 40~60um, fiber aperture 210~215um, ultrafiltrate coefficient 50~100ml/mmHg.h, urea clearance 150~200ml/min, CCr rate 150~200ml/min, middle molecule VB 12Clearance rate 40~150ml/min, the doughnut of spinning is made finished product after the processing of subsequent handling, make housing with polycarbonate, and the centrifugal envelope of polyamine fat glue both-end is irritated, and makes haemodialyser.
Embodiment 2
By weight percentage, polyether sulfone with 18%, 6% polyvinylpyrrolidone, 76% dimethylacetylamide under 80 ℃ of conditions, was dried 1 hour in the adding container, raw material and other components of oven dry are put into container, through under constant temperature, carrying out deaeration after swelling, stirring, the insulation then, make the spinning solution of rotary viscosity at 1000cp~6000cp (40 ℃), spinning solution is delivered in the building mortion of the present invention.In container 6, lead under the pressure of 0.01MPa~0.1Mpa, spinning solution is through being horizontally set on the distributing pipe 7 of container 6 outsides, spray from the outer hole of concentric diplopore spinning head 8 more than six on the distributing pipe 7 with 0.1~10ml/min flow, filling liquid is under the pressure of 0.01MPa~0.03MPa simultaneously, with the endoporus ejection of the flow of 0.05~5ml/min from diplopore spinning head 8, as-spun fibre is through the air section distance, solidification forming in the aqueous solution about 40 ℃, reel with 10~30m/min speed, form the doughnut blood filtering membrane.9 fluid pressures to distributing pipe 7 places of pressure sensor detect in real time simultaneously, and fluid pressure signal fed back to controller, controller with the force value of detected force value and setting relatively after, controller output signal, at any time control to adjust valve 3 actions by controller 11, control container 6 admission pressures, keep diplopore spinning head 8 stable go out flow quantity.Membrane area with the obtained doughnut filter membrane of the inventive method is 1.40m 2, wall thickness 45~55um, fiber aperture 220um, ultrafiltrate coefficient 200~300ml/mmHg.h, urea clearance 180~200ml/min, CCr rate 160~200ml/min, middle molecule VB 12Clearance rate 150~180ml/min, inulin clearance 100~150ml/min, the doughnut that shaping makes is made finished product after the processing of subsequent handling, make housing with polycarbonate, and the centrifugal envelope of polyamine fat glue both-end is irritated, and makes blood filter.
Embodiment 3
By weight percentage, polysulfones with 13%, 5% polyvinylpyrrolidone, 82% dimethylacetylamide under 80 ℃ of conditions, was dried 1 hour in the adding container, raw material and other components of oven dry are put into container, through under constant temperature, carrying out deaeration after swelling, stirring, the insulation then, make the spinning solution of rotary viscosity at 1000cp~2500cp (40 ℃), spinning solution is delivered in the building mortion of the present invention.Logical 0.01MPa~0.06Mpa's in container 6 at clean gas, under the pressure of clean gas, spinning solution is through being horizontally set on the distributing pipe 7 of container 6 outsides, spray from the outer hole of concentric diplopore spinning head 8 more than six on the distributing pipe 7 with 0.2~8ml/min flow, filling liquid is under the pressure of 0.01MPa~0.04MPa simultaneously, with the endoporus ejection of the flow of 0.01~4ml/min from diplopore spinning head 8, as-spun fibre is through the air section distance of 17cm, solidification forming in the aqueous solution about 40 ℃, reel with 10~20m/min speed, form the doughnut blood filtering membrane.9 fluid pressures to distributing pipe 7 places of pressure sensor detect in real time simultaneously, and fluid pressure signal fed back to controller 11, controller 11 with the force value of detected force value and setting relatively after, controller 11 output signals, at any time control to adjust valve 3 actions by controller 11, the admission pressure of control container 6, keep diplopore spinning head 8 stable go out flow quantity.With the prepared doughnut blood filtering membrane of the inventive method, membrane area is 0.8m 2, wall thickness 60~80um, fiber aperture 250~280um, ultrafiltrate coefficient 200~300ml/mmHg.h, urea clearance 200ml/min, CCr rate 200ml/min, middle molecule VB 12Clearance rate 200ml/min, inulin clearance 200ml/min, the doughnut of albumin screening efficiency 80%~95% spinning is made finished product after the processing of subsequent handling, make housing with polycarbonate, and the centrifugal envelope of polyamine fat glue both-end is irritated, and makes plasma separator.
Table 1 is 1.2m for measuring pump spinning membrane area 2Haemodialyser product performance index, table 2 are that adopt method of the present invention to be shaped to make membrane area be 1.2m 2The performance indications of haemodialyser product; Table 3 is that adopt method of the present invention to be shaped to make membrane area be 1.4m 2The performance indications of blood filter product;
Table 4 is that adopt method of the present invention to be shaped to make membrane area be 0.8m 2The performance indications of plasma separator product.
Table 1
Figure S2008101239090D00061
Table 2
Figure S2008101239090D00062
Table 3
Figure S2008101239090D00063
Table 4
As can be seen, the fiber blood filtering membrane that the present invention makes is compared with the fiber blood filtering membrane that the conventional metered dose pump is made from table 1 and table 2, and the product wall thickness is even, and urea clearance and CCr rate improve, and especially obviously improve at ultrafiltrate coefficient.From table 3 and table 4 as can be seen, the method according to this invention can make the blood filtering membrane that the material of small-molecular weight, middle molecular weight and macromolecule in the blood is removed.

Claims (6)

1. the manufacturing process of a doughnut blood filtering membrane, it is characterized in that: the spinning solution that 40 ℃ of rotary viscosity 600cp~9000cp is contained polysulfones is delivered in the airtight container; In container, feed the clean gas of 0.01MPa~0.10MPa; Under the pressure of clean gas, spinning solution is through being horizontally set on the distributing pipe of external container, flow with 0.1~10ml/min sprays from the outer hole of concentric diplopore spinning head more than six on the distributing pipe, filling liquid is under the pressure of 0.01MPa~0.10MPa simultaneously, with the endoporus ejection of the flow of 0.05~5ml/min from the diplopore spinning head, as-spun fibre enters water-bath solidification forming, coiling again behind air setting, form the doughnut blood filtering membrane; Simultaneously, pressure sensor feeds back to controller with the fluid pressure signal at distributing pipe place, controller with detected force value and setup pressure value relatively after, controller output signal control container admission pressure, keep the diplopore spinning head stable go out flow quantity.
2. the manufacturing process of doughnut blood filtering membrane according to claim 1 is characterized in that: the pressure in the described container is at 0.02MPa~0.06Mpa, and the pressure of filling liquid is at 0.01MPa~0.03MPa.
3. the manufacturing process of doughnut blood filtering membrane according to claim 1 is characterized in that: 40 ℃ of the rotary viscosity 1000cp~6000cp of described spinning solution.
4. the manufacturing process of doughnut blood filtering membrane according to claim 1 is characterized in that: described clean gas is clean air or inert gas.
5. the building mortion of a doughnut blood filtering membrane, comprise airtight container (6), feed tube (5) and filling pipe (4) and concentric diplopore spinning head (8), filling pipe (4) communicates with the endoporus of diplopore spinning head (8), it is characterized in that: described container (6) outside has horizontally disposed distributing pipe (7), and container (6) bottom distributing pipe (7) communicates, adorn six above diplopore spinning heads (8) on the distributing pipe (7), pressure sensor (9) is housed on the distributing pipe (7), the air inlet pipeline (1) on container (6) top communicates with clean compressed gas source, and the control valve (3) of regulator solution surface pressure is housed on the air inlet pipeline (1), the output of pressure sensor (9) is connected with the input of controller (11), the output termination control valve (3) of controller (11).
6. the building mortion of doughnut blood filtering membrane according to claim 5 is characterized in that: (8) 8~20 at described diplopore spinning head is installed on the distributing pipe (7).
CN2008101239090A 2008-06-12 2008-06-12 Forming method and device of hollow fiber blood filtering membrane Expired - Fee Related CN101288831B (en)

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CN102085458A (en) * 2011-01-12 2011-06-08 常州市美纤膜技术有限公司 Bidirectional forming device of hollow fiber blood filtering membrane
CN102580558A (en) * 2012-02-15 2012-07-18 常州市美纤膜技术有限公司 Non-pressure type hollow fiber filter membrane and preparation method thereof
CN102698609B (en) * 2012-05-31 2014-06-25 南京工业大学 Device for semi-continuously preparing composite membrane and composite membrane preparation process thereof
WO2020133313A1 (en) * 2018-12-29 2020-07-02 中芳特纤股份有限公司 Flow control system and control method for para-aramid spinning

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