CN1887368A - Prepn process of surface heparinized anticoagulant polyether-urethane material - Google Patents
Prepn process of surface heparinized anticoagulant polyether-urethane material Download PDFInfo
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- CN1887368A CN1887368A CN 200610054433 CN200610054433A CN1887368A CN 1887368 A CN1887368 A CN 1887368A CN 200610054433 CN200610054433 CN 200610054433 CN 200610054433 A CN200610054433 A CN 200610054433A CN 1887368 A CN1887368 A CN 1887368A
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Abstract
The present invention relates to anticoagulant material, and is especially preparation process of surface heparinized anticoagulant material on polyether urethane. The surface heparinized anticoagulant material is prepared with polyether urethane as base material and heparin as grafting monomer, and through a simple saponification process. The material has excellent anticoagulant performance and good mechanical performance, and the preparation process is simple and has mild reaction condition. The anticoagulant material of the present invention may be used widely in making medical implant, especially implant contacting directly to blood.
Description
One technical field
The invention belongs to the anticoagulant material technical field, particularly the preparation method of anticoagulant material.
Two background technologies
The blood compatibility of anticoagulant material is the emphasis and the difficult point of medical material research.Because poly(ether-urethane) is the wider macromolecular material of a class change in physical, and at room temperature be easy to by liquid monomer binary or multicomponent isocyanate and binary or progressively polymerization of polyhydric alcohol, obtain from softer elastomer to multiple products such as inflexible foam plasticss, so poly(ether-urethane) is widely used in the biomedical sector.Wherein, Biomer (linear segment polyether urethaneureas) and Avcothane-51 (polydimethylsiloxane-segment polyether urethaneureas block copolymer) are owing to have the soft tissue compatibility preferably and blood compatibility, therefore medical material implanted, particularly be used widely with the material implanted field that blood directly contacts.
Present method of modifying to poly(ether-urethane), it as application number " being used to improve the composition of blood compatibility of polyurethane surface coating liquid " patented technology of 00101714, adopt vulcabond to connect polyoxyethylene, be coated on the poly(ether-urethane) surface then, can improve the anticoagulation function of composite, the realization of its anticoagulation function mainly is the coating by means of particular components.Its main weak point is that coating liquid that this method is prepared can not effectively solve the reunification of anticoagulation function and mechanical property, and processing conditions is relatively harsh; And for example the technology of poly(ether-urethane) group compound film preparation is to prepare high molecule liquid crystal earlier, obtains composite membrane with the poly(ether-urethane) blended cross linking, and its main weak point is the process route complexity, and the consumption of raw materials amount is big, and the response time is long, the manufacturing cost height.
Three summary of the invention
The objective of the invention is weak point at existing poly(ether-urethane) method of modifying, a kind of preparation process of surface heparinized anticoagulant polyether-urethane material is provided, make poly(ether-urethane) have good anticoagulation function and good mechanical mechanics property, this method process route is simple, the consumption of raw materials amount is little, response time is short, and low cost of manufacture is easy to operate.
The object of the present invention is achieved like this: a kind of preparation process of surface heparinized anticoagulant polyether-urethane material, be to select for use EU (Polyurethane) to be base material, heparin (Heparin) is a grafted monomers, adopt simple saponification process, just prepare poly(ether-urethane) surface heparinization anticoagulant material.Its concrete method step is as follows.
(1) poly(ether-urethane) saponification modification
1. at first poly(ether-urethane) is dissolved in the oxolane, is configured to mass percent and is 1%～99% poly(ether-urethane) solution, this solution is fallen on clean glass plate again, to make thickness be the poly(ether-urethane) thin film of 0.1～1mm and take off.
2. under 0～100 ℃ of temperature, the poly(ether-urethane) thin film that (1)-1. step was made places saponification liquor, be that mass percent is 1～50% the sodium hydrate aqueous solution and the mixed solution of methanol, the volume ratio of sodium hydroxide and methanol is 1: 1～99, leave standstill after 1～60 minute and take out, clean standby with deionized water.
(2) poly(ether-urethane) heparinization
1. under 0～100 ℃ of temperature, it is the mixed solution of 1～50% citric acid solution and methanol that (1)-2. poly(ether-urethane) thin film that makes of step is placed mass percent, the volume ratio of citric acid and methanol is 1: 1～99, leaves standstill after 1～24 hour to take out, and cleans with deionized water;
2. with (2)-1. poly(ether-urethane) thin film that makes of step, immersing mass percent earlier is 1～50% carbodiimide solution, and is 3～7 with the pH of ethane sulfonic acid buffer agent regulator solution, leaves standstill after 1～60 minute and takes out, clean with deionized water.It is 0.1～5% heparin sodium aqua that mass percent is immersed in the back, and is 3～7 with the pH of ethane sulfonic acid buffer agent regulator solution, takes out after leaving standstill 1～24 hour under 0～80 ℃ the temperature again, clean with deionized water.Preparing surface combination heparin density at last is 10～40 μ g/cm
2Poly(ether-urethane) surface heparinization anticoagulant material finished film, and finished film is dried to constant weight under constant temperature, its thermostat temperature is 30～60 ℃.
The present invention carries out saponification to the poly(ether-urethane) surface earlier to handle, and carries out heparinization again, and just preparing surface combination heparin density is 10～40 μ g/cm
2Poly(ether-urethane) surface heparinization anticoagulant material, method is very simple, and the material of preparing be aqueous favoring with hydrophobic with the equally distributed surface microstructure of nano-scale, has good anticoagulation function, and kept good mechanical mechanics property, solved the reunification of the anticoagulation function and the mechanical mechanics property of composite effectively.The inventive method process route is simple, and the consumption of raw materials amount is little, and the response time is short, and low cost of manufacture is easy to operate, is a kind of effective ways of simple, convenient, practical preparation anticoagulant material.The anticoagulant material that adopts the inventive method to prepare can be widely used in make medical material implanted, particularly with blood directly contact material implanted.
Four specific embodiment
Below in conjunction with instantiation, further specify the present invention:
Embodiment 1: a kind of surface combination heparin density is 10 μ g/cm
2The concrete steps of preparation process of surface heparinized anticoagulant polyether-urethane material as follows:
(1) poly(ether-urethane) saponification modification
1. at first poly(ether-urethane) is dissolved in the oxolane, is configured to mass percent and is 10% poly(ether-urethane) solution, this solution is fallen on clean glass plate again, to make thickness be the poly(ether-urethane) thin film of 0.2mm and take off.
2. under 25 ℃ of temperature, (1)-1. poly(ether-urethane) thin film that makes of step is placed saponification liquor, and promptly mass percent is 13.4% the sodium hydrate aqueous solution and the mixed solution of methanol, and the volume ratio of sodium hydroxide and methanol is 1: 3, leave standstill after 1 minute and take out, clean standby with deionized water.
(2) poly(ether-urethane) heparinization
1. under 25 ℃ of temperature, it is the mixed solution of 10% citric acid solution and methanol that the poly(ether-urethane) thin film that (1)-2. step was made places mass percent, and the volume ratio of citric acid and methanol is 1: 3, leaves standstill taking-up after 3 hours, and is clean with deionized water.
2. with (2)-1. poly(ether-urethane) thin film that makes of step, immersing mass percent earlier is 10% carbodiimide solution, and is 6.5 with the pH of ethane sulfonic acid buffer agent regulator solution, leaves standstill after 30 minutes and takes out, clean with deionized water.It is 0.1% heparin sodium aqua that mass percent is immersed in the back, and the pH that regulates with the ethane sulfonic acid buffer agent is 6.5, takes out after leaving standstill 5 hours under 0 ℃ of temperature again, clean with deionized water.Preparing surface combination heparin density at last is 10 μ g/cm
2Poly(ether-urethane) surface heparinization anticoagulant material finished film, and finished film is dried to constant weight under constant temperature, its thermostat temperature is 40 ℃.
Embodiment 2: a kind of surface combination heparin density is 25 μ g/cm
2The concrete steps of preparation process of surface heparinized anticoagulant polyether-urethane material as follows:
(1) poly(ether-urethane) saponification modification
1. at first poly(ether-urethane) is dissolved in the oxolane, is configured to mass percent and is 10% poly(ether-urethane) solution, this solution is fallen on clean glass plate again, to make thickness be the poly(ether-urethane) thin film of 0.2mm and take off.
2. under 25 ℃ of temperature, (1)-1. poly(ether-urethane) thin film that makes of step is placed saponification liquor, and promptly mass percent is 13.4% the sodium hydrate aqueous solution and the mixed solution of methanol, and the volume ratio of sodium hydroxide and methanol is 1: 3, leave standstill after 1 minute and take out, clean standby with deionized water.
(2) poly(ether-urethane) heparinization
1. under 25 ℃ of temperature, it is the mixed solution of 10% citric acid solution and methanol that the poly(ether-urethane) thin film that (1)-2. step was made places mass percent, and the volume ratio of citric acid and methanol is 1: 3, leaves standstill taking-up after 3 hours, and is clean with deionized water.
2. with (2)-1. poly(ether-urethane) thin film that makes of step, immersing mass percent earlier is 10% carbodiimide solution, and is 5.5 with the pH of ethane sulfonic acid buffer agent regulator solution, leaves standstill after 30 minutes and takes out, clean with deionized water.It is 0.5% heparin sodium aqua that mass percent is immersed in the back, is 5.5 with the pH of ethane sulfonic acid buffer agent regulator solution, takes out after leaving standstill 12 hours under 0 ℃ the temperature again, clean with deionized water.Preparing surface combination heparin density at last is 25 μ g/cm
2Poly(ether-urethane) surface heparinization anticoagulant material finished film, and finished film is dried to constant weight under constant temperature, its thermostat temperature is 40 ℃.
Embodiment 3: a kind of surface combination heparin density is 40 μ g/cm
2The concrete steps of preparation process of surface heparinized anticoagulant polyether-urethane material as follows:
(1) poly(ether-urethane) saponification modification
1. at first poly(ether-urethane) is dissolved in the oxolane, is configured to mass percent and is 10% poly(ether-urethane) solution, this solution is fallen on clean glass plate again, to make thickness be the poly(ether-urethane) thin film of 0.2mm and take off.
2. under 25 ℃ of temperature, (1)-1. poly(ether-urethane) thin film that makes of step is placed saponification liquor, and promptly mass percent is 13.4% the sodium hydrate aqueous solution and the mixed solution of methanol, and the volume ratio of sodium hydroxide and methanol is 1: 3, leave standstill after 1 minute and take out, clean standby with deionized water.
(2) poly(ether-urethane) heparinization
1. under 25 ℃ of temperature, it is the mixed solution of 10% citric acid solution and methanol that the poly(ether-urethane) thin film that (1)-2. step was made places mass percent, and the volume ratio of citric acid and methanol is 1: 3, leaves standstill taking-up after 3 hours, and is clean with deionized water.
2. with (2)-1. poly(ether-urethane) thin film that makes of step, immersing mass percent earlier is 10% carbodiimide solution, and is 4.5 with the pH of ethane sulfonic acid buffer agent regulator solution, leaves standstill after 30 minutes and takes out, clean with deionized water.It is 1% heparin sodium aqua that mass percent is immersed in the back, and is 4.5 with the pH of ethane sulfonic acid buffer agent regulator solution, takes out after leaving standstill 24 hours under 0 ℃ the temperature again, clean with deionized water.Preparing surface combination heparin density at last is 40 μ g/cm
2Poly(ether-urethane) surface heparinization anticoagulant material finished film, and finished film is dried to constant weight under constant temperature, its thermostat temperature is 40 ℃.
Claims (4)
1. preparation process of surface heparinized anticoagulant polyether-urethane material is characterized in that its method step is as follows:
(1) poly(ether-urethane) saponification modification
1. at first poly(ether-urethane) is dissolved in the oxolane, is configured to mass percent and is 1%～99% poly(ether-urethane) solution, this solution is fallen on clean glass plate again, to make thickness be the poly(ether-urethane) thin film of 0.1～1mm and take off;
2. under 0～100 ℃ of temperature, the poly(ether-urethane) thin film that (1)-1. step was made places saponification liquor, be that mass percent is 1～50% the sodium hydrate aqueous solution and the mixed solution of methanol, the volume ratio of sodium hydroxide and methanol is 1: 1～99, leave standstill after 1～60 minute and take out, clean with deionized water;
(2) poly(ether-urethane) heparinization
1. under 0～100 ℃ of temperature, it is the mixed solution of 1～50% citric acid solution and methanol that (1)-2. poly(ether-urethane) thin film that makes of step is placed mass percent, the volume ratio of citric acid and methanol is 1: 1～99, leaves standstill after 1～24 hour to take out, and cleans with deionized water;
2. go on foot the poly(ether-urethane) thin film that makes with (2)-1., immersing mass percent earlier is 1～50% carbodiimide solution, and be 3～7 with the pH of ethane sulfonic acid buffer agent regulator solution, leave standstill after 1～60 minute and take out, clean with deionized water, back immersion mass percent is 0.1～5% heparin sodium aqua, and be 3～7 with the pH of ethane sulfonic acid buffer agent regulator solution, after leaving standstill 1～24 hour under 0～80 ℃ the temperature, take out again, clean with deionized water, preparing surface combination heparin density at last is 10～40 μ g/cm
2Poly(ether-urethane) surface heparinization anticoagulant material finished film, and finished film is dried to constant weight under constant temperature, its thermostat temperature is 30～60 ℃.
2. according to the described preparation process of surface heparinized anticoagulant polyether-urethane material of claim 1, it is characterized in that a kind of surface combination heparin density is 10 μ g/cm
2The concrete steps of preparation process of surface heparinized anticoagulant polyether-urethane material as follows:
(1) poly(ether-urethane) saponification modification
1. at first poly(ether-urethane) is dissolved in the oxolane, is configured to mass percent and is 10% poly(ether-urethane) solution, this solution is fallen on clean glass plate again, to make thickness be the poly(ether-urethane) thin film of 0.2mm and take off;
2. under 25 ℃ of temperature, (1)-1. poly(ether-urethane) thin film that makes of step is placed saponification liquor, and promptly mass percent is 13.4% the sodium hydrate aqueous solution and the mixed solution of methanol, and the volume ratio of sodium hydroxide and methanol is 1: 3, leave standstill after 1 minute and take out, clean with deionized water;
(2) poly(ether-urethane) heparinization
1. under 25 ℃ of temperature, it is the mixed solution of 10% citric acid solution and methanol that the poly(ether-urethane) thin film that (1)-2. step was made places mass percent, and the volume ratio of citric acid and methanol is 1: 3, leaves standstill taking-up after 3 hours, and is clean with deionized water;
2. go on foot the poly(ether-urethane) thin film that makes with (2)-1., immersing mass percent earlier is 10% carbodiimide solution, and be 6.5 with the pH of ethane sulfonic acid buffer agent regulator solution, leave standstill after 30 minutes and take out, clean with deionized water, back immersion mass percent is 0.1% heparin sodium aqua, and the pH that regulates with the ethane sulfonic acid buffer agent is 6.5, take out after leaving standstill 5 hours under 0 ℃ of temperature, clean with deionized water, preparing surface combination heparin density at last is 10 μ g/cm
2Poly(ether-urethane) surface heparinization anticoagulant material finished film, and finished film is dried to constant weight under constant temperature, its thermostat temperature is 40 ℃.
3. according to the described preparation process of surface heparinized anticoagulant polyether-urethane material of claim 1, it is characterized in that a kind of surface combination heparin density is 25 μ g/cm
2The concrete steps of preparation process of surface heparinized anticoagulant polyether-urethane material as follows:
(1) poly(ether-urethane) saponification modification
1. at first poly(ether-urethane) is dissolved in the oxolane, is configured to mass percent and is 10% poly(ether-urethane) solution, this solution is fallen on clean glass plate again, to make thickness be the poly(ether-urethane) thin film of 0.2mm and take off;
2. under 25 ℃ of temperature, (1)-1. poly(ether-urethane) thin film that makes of step is placed saponification liquor, and promptly mass percent is 13.4% the sodium hydrate aqueous solution and the mixed solution of methanol, and the volume ratio of sodium hydroxide and methanol is 1: 3, leave standstill after 1 minute and take out, clean with deionized water;
(2) poly(ether-urethane) heparinization
1. under 25 ℃ of temperature, it is the mixed solution of 10% citric acid solution and methanol that the poly(ether-urethane) thin film that (1)-2. step was made places mass percent, and the volume ratio of citric acid and methanol is 1: 3, leaves standstill taking-up after 3 hours, and is clean with deionized water;
2. go on foot the poly(ether-urethane) thin film that makes with (2)-1., immersing mass percent earlier is 10% carbodiimide solution, and be 5.5 with the pH of ethane sulfonic acid buffer agent regulator solution, leave standstill after 30 minutes and take out, clean with deionized water, back immersion mass percent is 0.5% heparin sodium aqua, pH with ethane sulfonic acid buffer agent regulator solution is 5.5, take out after leaving standstill 12 hours under 0 ℃ the temperature, clean with deionized water, preparing surface combination heparin density at last is 25 μ g/cm
2Poly(ether-urethane) surface heparinization anticoagulant material finished film, and finished film is dried to constant weight under constant temperature, its thermostat temperature is 40 ℃.
4. according to the described preparation process of surface heparinized anticoagulant polyether-urethane material of claim 1, it is characterized in that a kind of surface combination heparin density is 40 μ g/cm
2The concrete steps of preparation process of surface heparinized anticoagulant polyether-urethane material as follows:
(1) poly(ether-urethane) saponification modification
1. at first poly(ether-urethane) is dissolved in the oxolane, is configured to mass percent and is 10% poly(ether-urethane) solution, this solution is fallen on clean glass plate again, to make thickness be the poly(ether-urethane) thin film of 0.2mm and take off;
2. under 25 ℃ of temperature, (1)-1. poly(ether-urethane) thin film that makes of step is placed saponification liquor, and promptly mass percent is 13.4% the sodium hydrate aqueous solution and the mixed solution of methanol, and the volume ratio of sodium hydroxide and methanol is 1: 3, leave standstill after 1 minute and take out, clean with deionized water;
(2) poly(ether-urethane) heparinization
1. under 25 ℃ of temperature, it is the mixed solution of 10% citric acid solution and methanol that the poly(ether-urethane) thin film that (1)-2. step was made places mass percent, and the volume ratio of citric acid and methanol is 1: 3, leaves standstill taking-up after 3 hours, and is clean with deionized water;
2. go on foot the poly(ether-urethane) thin film that makes with (2)-1., immersing mass percent earlier is 10% carbodiimide solution, and be 4.5 with the pH of ethane sulfonic acid buffer agent regulator solution, leave standstill after 30 minutes and take out, clean with deionized water, back immersion mass percent is 1% heparin sodium aqua, and be 4.5 with the pH of ethane sulfonic acid buffer agent regulator solution, take out after leaving standstill 24 hours under 0 ℃ the temperature, clean with deionized water, preparing surface combination heparin density at last is 40 μ g/cm
2Poly(ether-urethane) surface heparinization anticoagulant material finished film, and finished film is dried to constant weight under constant temperature, its thermostat temperature is 40 ℃.
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| CN 200610054433 CN1887368A (en) | 2006-07-12 | 2006-07-12 | Prepn process of surface heparinized anticoagulant polyether-urethane material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127204A (en) * | 2011-01-28 | 2011-07-20 | 苏州大学 | Preparation method of novel antibiotic anticoagulant polyurethane material |
| CN102718977A (en) * | 2012-07-04 | 2012-10-10 | 南京师范大学 | Heparin sodium-loaded polyurethane micro nanometer particle solution and preparation method and application thereof |
| CN107903610A (en) * | 2017-11-14 | 2018-04-13 | 安徽省健源医疗器械设备有限公司 | A kind of medical polyurethane film and preparation method thereof |
| CN110947056A (en) * | 2019-11-29 | 2020-04-03 | 河南驼人贝斯特医疗器械有限公司 | Inner and outer wall anti-infection anticoagulant remaining needle hose and preparation method thereof |
-
2006
- 2006-07-12 CN CN 200610054433 patent/CN1887368A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127204A (en) * | 2011-01-28 | 2011-07-20 | 苏州大学 | Preparation method of novel antibiotic anticoagulant polyurethane material |
| CN102718977A (en) * | 2012-07-04 | 2012-10-10 | 南京师范大学 | Heparin sodium-loaded polyurethane micro nanometer particle solution and preparation method and application thereof |
| CN107903610A (en) * | 2017-11-14 | 2018-04-13 | 安徽省健源医疗器械设备有限公司 | A kind of medical polyurethane film and preparation method thereof |
| CN110947056A (en) * | 2019-11-29 | 2020-04-03 | 河南驼人贝斯特医疗器械有限公司 | Inner and outer wall anti-infection anticoagulant remaining needle hose and preparation method thereof |
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