CN101519488B - Device and method for medical macromolecular material continuous precipitation and fractionation - Google Patents
Device and method for medical macromolecular material continuous precipitation and fractionation Download PDFInfo
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- CN101519488B CN101519488B CN2009100682512A CN200910068251A CN101519488B CN 101519488 B CN101519488 B CN 101519488B CN 2009100682512 A CN2009100682512 A CN 2009100682512A CN 200910068251 A CN200910068251 A CN 200910068251A CN 101519488 B CN101519488 B CN 101519488B
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Abstract
The invention discloses a device and a method for medical macromolecular material continuous precipitation fractionation. The device comprises a separation column. The lower part of the separation column is provided with a precipitator feed pipe connected with a first distributor, the upper part of the separation column is provided with a low molecular weight polymer solution discharge hole, and the bottom end of the separation column is provided with a high molecular weight polymer solution discharge hole. A long polymer solution feed pipe is movably connected with the top end of the separation column, thereby a discharge hole of the long polymer solution feed pipe is made to move in the separation column from top to bottom. A short polymer solution feed pipe is movably connected with the top end of the separation column, the lower end part of the short polymer solution feed pipe is connected with a second distributor positioned at the middle upper part in the separation column, and the open pore of the second distributor is downward. The device and the method enhance the fractionation efficiency, reach the fractionation standard of the technical scale, are applicable to the continuous precipitation fractionation of common polymers, and have good effect on polymers which are prone to larger precipitation lumps, particles, precipitation threads, or the like.
Description
Technical field
The present invention relates to a kind of polymer grading plant and method, particularly relate to a kind of polymer precipitation grading plant and method.
Background technology
Polymer all has certain molecular weight distribution, and in order to satisfy specific user demand, the polymer after must will synthesizing carries out grading purification.When especially using as biomaterial, part that must molecular weight is low is separated, so that polymer has good mechanical performance and anti-degradation property etc.For example, polyurethane is to use biomaterial very widely, yet the condensation polymerization reaction principle has determined synthesis of polyurethane in the ordinary course of things, and molecular weight distribution is very wide, more than 2.Low molecular weight part in the synthesis of polyurethane causes the Material Physics mechanical performance relatively poor, especially uses the heart material or the vascular grafts of polyurethane preparation, in the body planted agent time spent, degraded and damage takes place easily.In order to obtain the artificial heart material of HMW and narrow molecular weight distribution, must carry out classification to synthesis of polyurethane and purify.
The classification of polymer generally is to realize from the solution of high dilution, and this traditional separating technology was described in detail in a lot of documents.It is with according to the principle that balances each other that traditional polymer separates, by molecular weight vary in size and (or) structure of chemical composition of polymer is different, cause different solubility in solvent and precipitating reagent, and realization.Under the usual condition, can pass through repeatedly repeated isolation, obtain the separating effect of a satisfaction.Yet this separating technology is unreasonable economically, and for example the disengaging time of this arts demand is very long and the consumption quantity of solvent is very big, also can pollute environment.This technology is not green chemical industry technology.
The device and the technology of the industrial polymer classification that Wolf B.A. and his colleagues mention in patent DE3242130A1 and US 5242594.
This device comprises a splitter, a polymer solution feed is set in the middle and upper part of splitter, the opening of polymer solution feed is positioned at the center of splitter, a precipitating reagent charging aperture is set in the bottom of splitter, a low-molecular weight polymer solution discharging opening is set on the top of splitter, a heavy polymer solution discharging opening is set in the bottom of splitter, utilize this equipment, by the continuous countercurrent extraction method, big or the little polymer solution of molecular weight is separated, and obtains the polymer of narrow distribution.This technology is that polymer is dissolved in the suitable solvent of one or more components, realizes mutually as transmission with this mixed solution.This technology is used for the classification of polymer such as polyvinyl chloride, polyisobutene, but is not suitable for the classification of the bigger polymer of adhesive force such as polyurethane.
At said apparatus, the feed of polymer solution mouth is fixed, separate needs in order to guarantee commercial scale, the diameter of this mouthful is very big, when polymer solution contacts with precipitating reagent, the polymer solution of different molecular weight can not in time be disperseed, and causes the solution that is rich in polymer too big mutually, and separating effect is not good.At said apparatus, the precipitating reagent charging aperture is fixed on the splitter bottom, and after precipitating reagent entered splitter, inhomogeneous easily flowing reduced separative efficiency.During the operation beginning, pump into precipitating reagent to splitter, and separate the starting stage, polymer solution and precipitating reagent be along with carry out running time, progressively from unstable state to the stable state transition, the composition of gained heavy polymer is changing like this, molecular weight is also gradually changing from low to high, after stable state reached, the gained heavy polymer was just stable, so the classification loss is serious.So this method is not suitable for the classification of expensive medical macromolecular materials and small lot polymer.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of medical macromolecular materials continuous precipitation grading plant is provided.
Second purpose of the present invention provides a kind of medical macromolecular materials continuous precipitation stage division.
Technical scheme of the present invention is summarized as follows:
A kind of medical macromolecular materials continuous precipitation grading plant, comprise splitter, the bottom of described splitter is provided with the precipitating reagent feed pipe, described precipitating reagent feed pipe is connected with first distributor, the top of described splitter is provided with low-molecular weight polymer solution discharging opening, the bottom of described splitter is provided with heavy polymer solution discharging opening, the top of feed of polymer solution long tube and described splitter flexibly connects, the discharging opening of described feed of polymer solution long tube is moved up and down in described splitter, the top of feed of polymer solution short tube and described splitter flexibly connects, the bottom of described feed of polymer solution short tube is connected with second distributor, described second distributor is positioned at the middle and upper part of described splitter, and the described second distributor perforate is directed downwards.
The upper end of feed of polymer solution short tube can also be connected with and can produce reciprocating device, and the feed of polymer solution short tube can be pumped.
The material of described feed of polymer solution long tube can be polytetrafluoroethylene (PTFE), polyethylene, ethylene-tetrafluoroethylene copolymer, engineering plastics, ABS resin or polyvinyl chloride, and the material of described feed of polymer solution short tube can be polytetrafluoroethylene (PTFE), polyethylene, ethylene-tetrafluoroethylene copolymer, engineering plastics, ABS resin or polyvinyl chloride.
A kind of medical macromolecular materials continuous precipitation stage division comprises the steps:
(1) splitter is installed, the bottom of described splitter is provided with the precipitating reagent feed pipe, described precipitating reagent feed pipe is connected with first distributor, the top of described splitter is provided with low-molecular weight polymer solution discharging opening, the bottom of described splitter is provided with heavy polymer solution discharging opening, the top of feed of polymer solution long tube and described splitter flexibly connects, the discharging opening of described feed of polymer solution long tube is moved up and down in described splitter, the top of feed of polymer solution short tube and described splitter flexibly connects, the bottom of described feed of polymer solution short tube is connected with second distributor, described second distributor is positioned at the middle and upper part of described splitter, and the described second distributor perforate is directed downwards;
(2) open precipitating reagent feed pipe valve and feed of polymer solution long tube valve, promote the feed of polymer solution long tube, the lower end charging aperture and the interior liquid level of splitter of feed of polymer solution long tube are risen synchronously, rise to described low-molecular weight polymer solution discharging opening place, close feed of polymer solution long tube valve, open the valve on the feed of polymer solution short tube, open low-molecular weight polymer solution discharging opening valve, low-molecular weight polymer solution flows out automatically, open heavy polymer solution discharging opening valve, heavy polymer solution flows out automatically.
The upper end of feed of polymer solution short tube preferably is connected with and can produces reciprocating device, open and to produce reciprocating device, described feed of polymer solution short tube is pumped, and described reciprocating frequency is 10-120 time/minute, amplitude 40-100 millimeter.
The material of described feed of polymer solution long tube can be polytetrafluoroethylene (PTFE), polyethylene, ethylene-tetrafluoroethylene copolymer, engineering plastics, ABS resin or polyvinyl chloride, and the material of described feed of polymer solution short tube can be polytetrafluoroethylene (PTFE), polyethylene, ethylene-tetrafluoroethylene copolymer, engineering plastics, ABS resin or polyvinyl chloride.
Advantage of the present invention: improve separative efficiency and reach commercial scale and separate; be applicable to the continuous precipitation classification of general polymer; and to polymer such as easy formation bigger precipitation group or particle or precipitation silks, as: the classification of polyurethane, polyester etc. is effective especially.In addition, classification is in stable state from start to end substantially in the splitter, and the composition of gained heavy polymer does not change in time like this, and molecular weight does not also change in time, and the gained heavy polymer is formed and molecular weight is stablized.
Description of drawings
Fig. 1 is the structural representation of a kind of polymer continuous precipitation grading plant of the present invention.
Fig. 2 is the upward view of second distributor.
The specific embodiment
The present invention is further illustrated below in conjunction with accompanying drawing.
The specific embodiment
The present invention is further illustrated below in conjunction with the drawings and specific embodiments.
A kind of medical macromolecular materials continuous precipitation grading plant, comprise splitter 1, the bottom of splitter is provided with precipitating reagent feed pipe 6, the precipitating reagent feed pipe is connected with first distributor 7, first distributor is provided with aperture, the opening direction of aperture upwards, the top of splitter is provided with low-molecular weight polymer solution discharging opening 3, the bottom of splitter is provided with heavy polymer solution discharging opening 8, feed of polymer solution long tube 5 flexibly connects with the top of described splitter, the discharging opening of feed of polymer solution long tube is moved up and down in splitter, feed of polymer solution short tube 2 flexibly connects with the top of splitter, the bottom of feed of polymer solution short tube is connected with the middle and upper part that second distributor, 4, the second distributors are positioned at splitter, and the second distributor perforate 9 is directed downwards.(see Fig. 1, Fig. 2)
The upper end of feed of polymer solution short tube can also be connected with and can produce reciprocating device, and the feed of polymer solution short tube can be pumped.
The material of feed of polymer solution long tube can be polytetrafluoroethylene (PTFE), polyethylene, ethylene-tetrafluoroethylene copolymer, engineering plastics, ABS resin or polyvinyl chloride, and the material of feed of polymer solution short tube can be polytetrafluoroethylene (PTFE), polyethylene, ethylene-tetrafluoroethylene copolymer, engineering plastics, ABS resin or polyvinyl chloride.
A kind of medical macromolecular materials continuous precipitation stage division comprises the steps:
(1) splitter 1 is installed, the bottom of splitter is provided with precipitating reagent feed pipe 6, the precipitating reagent feed pipe is connected with first distributor 7, first distributor is provided with aperture, the opening direction of aperture upwards, the top of splitter is provided with low-molecular weight polymer solution discharging opening, the bottom of splitter is provided with heavy polymer solution discharging opening 8, feed of polymer solution long tube 5 flexibly connects with the top of splitter, the discharging opening of feed of polymer solution long tube is moved up and down in splitter, feed of polymer solution short tube 2 flexibly connects with the top of splitter, the bottom of feed of polymer solution short tube is connected with second distributor 4, second distributor is positioned at the middle and upper part of splitter, and the second distributor perforate is directed downwards;
(2) open precipitating reagent feed pipe valve and feed of polymer solution long tube valve, control by calculating proportioning through the control flow pump, promote the feed of polymer solution long tube, the lower end charging aperture and the interior liquid level of splitter of feed of polymer solution long tube are risen synchronously, rise to described low-molecular weight polymer solution discharging opening place, close feed of polymer solution long tube valve, open the valve on the feed of polymer solution short tube, open low-molecular weight polymer solution discharging opening valve, low-molecular weight polymer solution flows out automatically, open heavy polymer solution discharging opening valve, heavy polymer solution flows out automatically.
The upper end of feed of polymer solution short tube preferably is connected with and can produces reciprocating device, and adjustable speed motor is for example controlled the Oscillation Amplitude and the reciprocating frequency of this pipe by motor, open motor, described feed of polymer solution short tube is pumped, reciprocating frequency is for can be adjusted to 10 times/minute, 20 times/minute, 30 times/minute, 40 times/minute, 50 times/minute, 60 times/minute, 70 times/minute, 80 times/minute, 90 times/minute, 100 times/minute, 110 times/minute or 120 times/minute, amplitude can be adjusted to 5 millimeters, 10 millimeters, 20 millimeters, 30 millimeters, 40 millimeters, 50 millimeters, 60 millimeters, 70 millimeters, 80 millimeters, 90 millimeters or 100 millimeters.
The material of described feed of polymer solution long tube can be polytetrafluoroethylene (PTFE), polyethylene, ethylene-tetrafluoroethylene copolymer, engineering plastics, ABS resin or polyvinyl chloride, and the material of described feed of polymer solution short tube can be polytetrafluoroethylene (PTFE), polyethylene, ethylene-tetrafluoroethylene copolymer, engineering plastics, ABS resin or polyvinyl chloride.
The present invention can be so that the polymer separating effect be more complete by countercurrent action.And the concentrated phase of heavy polymer is moved to the splitter bottom under the self gravitation effect because proportion is bigger, and discharges by the heavy polymer solution discharging opening in the bottom.And upper end low-molecular weight polymer solution discharging opening is used for the solution discharge that contains most of low-molecular-weight polymer of light specific gravity.
Medical macromolecular materials polycarbonate polyurethane (PCU) continuous precipitation stage division comprises the steps:
Number-average molecular weight is 53000 before the classification, and molecular weight distribution is 1.84, and polymer solution consists of: PCU-111% (w/w), dimethylacetylamide 47% (w/w), isopropyl alcohol 42% (w/w); Precipitant solution consists of dimethylacetylamide 36% (w/w), isopropyl alcohol 64% (w/w).
Polymer precipitation grading plant splitter parameter is:
Post height: 350cm, the splitter temperature is controlled at 25 degree constant temperature.The precipitating reagent feed pipe is apart from splitter bottom 30cm, the top that the feed of polymer solution short tube passes splitter extend into the inside of splitter, second distributor is apart from 300cm place, splitter bottom, feed of polymer solution short tube reciprocating frequency is controlled at 10 millimeters of 60 times/minute and amplitudes, material flow is controlled between the 0-1000mL/min, preferably be controlled between the 5-500mL/min, the velocity ratio of polymer solution and precipitating reagent is controlled at 1/2.
Before series classification begins, open precipitating reagent feed pipe valve, press the calculating proportioning through the control flow pump, promote the feed of polymer solution long tube, the lower end charging aperture and the interior liquid level of splitter of feed of polymer solution long tube are risen synchronously, rise to described low-molecular weight polymer solution discharging opening place, make in splitter solvent and precipitating reagent ratio according to highly different and different, solution forms a gradient and distributes in the splitter.Close feed of polymer solution long tube valve, and the feed of polymer solution long tube is promoted to more than the low-molecular weight polymer solution discharging opening.Open the valve on the feed of polymer solution short tube simultaneously, open low-molecular weight polymer solution discharging opening valve, low-molecular weight polymer solution flows out automatically, opens heavy polymer solution discharging opening valve, and heavy polymer solution flows out automatically.Heavy polymer by the time collects through processes such as washing of precipitate dryings, obtains polycarbonate polyurethane.Their molecular weight and distribution thereof are listed in the table 1.
From table 1, can learn, gained biomaterial polycarbonate polyurethane molecular weight is apparently higher than raw material PCU-1, and molecular weight distribution obviously narrows down, and they are with changing running time, this illustrates a kind of polymer precipitation stage division grading effect of the present invention clearly, and very stable from start to finish.In classification process, the phenomenon that polymer or heavy polymer stick to equipment such as splitter and pipeline does not appear simultaneously.Polymer solution forms small HMW concentrated phase after being micropore that snail is provided with and flowing out from the bottom of polymer solution feed immediately, and low-molecular-weight polymer is dissolved or be scattered in the mixed solution.Wherein in small HMW concentrated phase the embedded portion low-molecular weight polymer in concentrated phase from high-end infall process, further mixed solution dissolving reaches the purpose of high score from effect like this.
Table 1. polycarbonate polyurethane is through series classification gained high molecular polymer molecular weight and distribution (gel permeation chromatography) thereof
| Material | The running time/hour | Number-average molecular weight | Weight average molecular weight | Molecular weight distribution |
| PCU-1 | 0 | 53000 | 97500 | 1.84 |
| PCU-2 | 1 | 85000 | 115000 | 1.35 |
| PCU-3 | 2 | 86000 | 117000 | 1.36 |
| PCU-4 | 3 | 85000 | 117000 | 1.37 |
| PCU-5 | 4 | 86000 | 115000 | 1.35 |
| PCU-6 | 5 | 85000 | 116000 | 1.35 |
| PCU-7 | 10 | 85000 | 115000 | 1.35 |
Claims (6)
1. medical macromolecular materials continuous precipitation grading plant, comprise splitter, the bottom of described splitter is provided with the precipitating reagent feed pipe, described precipitating reagent feed pipe is connected with first distributor, the top of described splitter is provided with low-molecular weight polymer solution discharging opening, the bottom of described splitter is provided with heavy polymer solution discharging opening, the top that it is characterized in that feed of polymer solution long tube and described splitter flexibly connects, the discharging opening of described feed of polymer solution long tube is moved up and down in described splitter, the top of feed of polymer solution short tube and described splitter flexibly connects, the bottom of described feed of polymer solution short tube is connected with second distributor, described second distributor is positioned at the middle and upper part of described splitter, and the described second distributor perforate is directed downwards.
2. a kind of medical macromolecular materials continuous precipitation grading plant according to claim 1 is characterized in that being connected with in the upper end of described feed of polymer solution short tube and can produce reciprocating device.
3. a kind of medical macromolecular materials continuous precipitation grading plant according to claim 1, the material that it is characterized in that described feed of polymer solution long tube is polytetrafluoroethylene (PTFE), polyethylene, ethylene-tetrafluoroethylene copolymer, ABS resin or polyvinyl chloride, and the material of described feed of polymer solution short tube is polytetrafluoroethylene (PTFE), polyethylene, ethylene-tetrafluoroethylene copolymer, ABS resin or polyvinyl chloride.
4. a medical macromolecular materials continuous precipitation stage division is characterized in that comprising the steps:
(1) splitter is installed, the bottom of described splitter is provided with the precipitating reagent feed pipe, described precipitating reagent feed pipe is connected with first distributor, the top of described splitter is provided with low-molecular weight polymer solution discharging opening, the bottom of described splitter is provided with heavy polymer solution discharging opening, the top of feed of polymer solution long tube and described splitter flexibly connects, the discharging opening of described feed of polymer solution long tube is moved up and down in described splitter, the top of feed of polymer solution short tube and described splitter flexibly connects, the bottom of described feed of polymer solution short tube is connected with second distributor, described second distributor is positioned at the middle and upper part of described splitter, and the described second distributor perforate is directed downwards;
(2) open precipitating reagent feed pipe valve and feed of polymer solution long tube valve, promote the feed of polymer solution long tube, the lower end charging aperture and the interior liquid level of splitter of feed of polymer solution long tube are risen synchronously, rise to described low-molecular weight polymer solution discharging opening place, close feed of polymer solution long tube valve, open the valve on the feed of polymer solution short tube, open low-molecular weight polymer solution discharging opening valve, low-molecular weight polymer solution flows out automatically, open heavy polymer solution discharging opening valve, heavy polymer solution flows out automatically.
5. a kind of medical macromolecular materials continuous precipitation stage division according to claim 4, the upper end that it is characterized in that described feed of polymer solution short tube is connected with and can produces reciprocating device, open and to produce reciprocating device, described feed of polymer solution short tube is pumped, described reciprocating frequency is 10-120 time/minute, amplitude 40-100 millimeter.
6. a kind of medical macromolecular materials continuous precipitation stage division according to claim 4, the material that it is characterized in that described feed of polymer solution long tube is polytetrafluoroethylene (PTFE), polyethylene, ethylene-tetrafluoroethylene copolymer, ABS resin or polyvinyl chloride, and the material of described feed of polymer solution short tube is polytetrafluoroethylene (PTFE), polyethylene, ethylene-tetrafluoroethylene copolymer, ABS resin or polyvinyl chloride.
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| CN101519488B true CN101519488B (en) | 2011-03-30 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5242594A (en) * | 1991-02-14 | 1993-09-07 | Pluess-Staufer Ag | Process and apparatus for industrial fractionation of polymers |
| CN1622960A (en) * | 2002-01-24 | 2005-06-01 | 伯恩哈德·A·沃尔夫 | Process and apparatus for the technical fractionation of oligomers and polymers |
| CN1918199A (en) * | 2004-01-09 | 2007-02-21 | 切弗朗菲利浦化学公司 | Ultra high molecular weight polyethylene fractions having narrow molecular weight distributions and methods of making and using the same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5242594A (en) * | 1991-02-14 | 1993-09-07 | Pluess-Staufer Ag | Process and apparatus for industrial fractionation of polymers |
| CN1622960A (en) * | 2002-01-24 | 2005-06-01 | 伯恩哈德·A·沃尔夫 | Process and apparatus for the technical fractionation of oligomers and polymers |
| CN1918199A (en) * | 2004-01-09 | 2007-02-21 | 切弗朗菲利浦化学公司 | Ultra high molecular weight polyethylene fractions having narrow molecular weight distributions and methods of making and using the same |
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