CN1064265C - Anticoagulation composite and its preparation method - Google Patents
Anticoagulation composite and its preparation method Download PDFInfo
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- CN1064265C CN1064265C CN96112801A CN96112801A CN1064265C CN 1064265 C CN1064265 C CN 1064265C CN 96112801 A CN96112801 A CN 96112801A CN 96112801 A CN96112801 A CN 96112801A CN 1064265 C CN1064265 C CN 1064265C
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- chitose
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Abstract
The present invention relates to an anticoagulation composite material and a preparation method thereof. Chitose and polysiloxane which have a good biocompatibility are chosen for the preparation of the anticoagulation composite material, and the anticoagulation composite material is prepared through blending and crosslinking of the chitose and the polysiloxane by utilizing the difference of the hydrophilicity and the hydrophobicity of the chitose and the polysiloxane. The anticoagulation composite material has the advantages of favorable blood compatibility, favorable mechanical property and microphase separation structure and stable the thermal property so that the anticoagulation composite material meets the requirement of the service temperature of biological materials; the anticoagulation composite material has no skin stimulation and no intracutaneous stimulation so that the anticoagulation composite material meets the requirement of a pyrogen test and is an anticoagulation material with good performance. The method of the present invention used for preparing the composite material has the advantages of convenient operation and simple manufacture, and is a simple and easy preparation method.
Description
The present invention is a kind of anticoagulant material and preparation method thereof, belongs to the renovation technique of anticoagulant material and preparation method thereof.
The blood compatibility of anticoagulant material is the emphasis and the difficult point of biomaterial research, and improving the biomaterial blood compatibility generally has two kinds of approach: the one, and the exploitation surface has the new material of desirable blood compatibility; The 2nd, the surface of current material is modified to improve the blood compatibility of material.At present, the exploitation to new blood compatibility biological material mainly concentrates in the research of polyurethane; The surface of current material modified with the blood compatibility that improves material focus mostly in the finishing of high polymer.These two kinds of approach respectively have its characteristics, the biomaterial of being developed has certain blood compatibility and physical and mechanical properties, but do not develop the biomaterial that really has good anticoagulation function so far yet, the blood compatibility of existing anticoagulant material is all not good enough, and preparation is complicated.
The objective of the invention is to overcome the existing existing shortcoming and defect of anticoagulant biomaterial, a kind of have good blood compatibility, good physical and mechanical properties and the anticoagulation composite with micro phase separation structure are provided.
The present invention also aims to provide a kind of method for preparing above-mentioned composite, it is easy to operate, makes simple.
Anticoagulation composite of the present invention includes chitose, polysiloxanes, and the ratio of chitose and polysiloxanes (mass ratio) is 1: 99～99: 1.
The optimal proportion of above-mentioned chitose and polysiloxanes (mass ratio) is 1: 9～9: 1.
The present invention prepares the method for above-mentioned composite, follows these steps to carry out:
(1), chitose solution and polysiloxane emulsion are carried out blend by the certain mass ratio;
(2), cross-linking agent is added in the blended liquid, stir under the room temperature, make cross-linking agent carry out crosslinked chitose;
(3), pour casting film-forming in the mould into behind the static froth breaking, air-dryly put into baking oven freeze-day with constant temperature film forming again to solidifying substantially;
(4), earlier soak above-mentioned film material with dilute alkaline soln, reuse distilled water immersion, flushing are taken out the film material and are dried to constant weight to neutral;
(5), above-mentioned film material carries out crosslinked with cross-linking agent to polysiloxanes under acid condition;
(6), soak above-mentioned film material, reuse distilled water immersion, flushing are to neutral, and freeze-day with constant temperature is to constant weight with diluted alkaline.
Above-mentioned chitose solution is that 40%～100% chitose is dissolved in diluted acid and makes by deacetylation.
The concentration of above-mentioned chitose solution (mass percent) is 1 ‰～10%.
Cross-linking agent in the above-mentioned steps (2) is the dialdehyde aqueous solution, and the ratio of dialdehyde crosslinking agent and chitose (mass ratio) is 0.00001: 1～1: 10.
The concentration of above-mentioned dialdehyde aqueous solution (mass percent is) 2.5PPm～2.5%.
The polysiloxanes number-average molecular weight of above-mentioned polysiloxane emulsion is 3 * 10
3～3 * 10
5
The present invention has selected chitose and two kinds of materials with good biocompatibility of polysiloxanes for use, utilize the difference of its hydrophilic, hydrophobic property, by blend, crosslinkedly prepared a kind of anticoagulation composite, understand that from the evaluation table of blood coagulation, erythrocyte and three aspects of platelet deformation extent this composite has good blood compatibility; Simultaneously, this composite also has the favorable mechanical performance, and its maximum anti-Zhang Chengdu can reach 13.3MPa under hygrometric state, and elongation at break is 98%; In addition, this composite also has micro phase separation structure, and the microcell size changes between 10A to 10um; This composite hot property between-40 ℃ to+190 ℃ is stable in addition, meets the requirement on the biomaterial serviceability temperature, and its no skin irritation and Intradermal stimulation, meets the pyrogen testing requirement; Composite of the present invention is a kind of anticoagulant material of function admirable.
The present invention prepares the method for above-mentioned composite, and it is easy to operate, make simply, and be a kind of simple preparation method.
Below by embodiment each components contents of composite of the present invention and preparation method thereof is described:
Embodiment one:
Preparation chitose and polysiloxanes mass ratio are 1: 1 composite.
The preparation method step is as follows:
(1) getting deacetylation is 89% chitose, 6 grams, is dissolved in 2% the acetum, is made into 6% chitose solution, and the peek average molecular weight is that 3-6 ten thousand, content are 30 ± 2% polysiloxane emulsion 20 grams, carries out blend with above-mentioned chitose solution;
(2), the glutaraldehyde water solution (mass percent is 1 ‰) of 5.8g is added in the above-mentioned blended liquid, stir under the room temperature, make glutaraldehyde carry out crosslinked chitose;
(3), pour casting film-forming in the mould into behind the static froth breaking, air-dryly put into 50 ℃ of freeze-day with constant temperature film forming of baking oven again to solidifying substantially;
(4) with the above-mentioned film material of 10%NaOH solution soaking, reuse distilled water immersion, flushing are taken out the film material and are dried to constant weight to neutral;
(5), above-mentioned film material under acid (example hydrochloric acid) condition, with esters of silicon acis polysiloxanes is carried out crosslinkedly, the amount of silicic acid fat enough gets final product;
(6), soaked above-mentioned film material 24 hours, NaOH is neutralized to above-mentioned acidity, reuse distilled water immersion, flushing are to neutral, and 50 ℃ of freeze-day with constant temperature are to constant weight with 10%NaOH.
Embodiment two:
Preparation chitose and polysiloxanes mass ratio are 4: 1 composite.
The preparation method step is as follows:
(1) getting deacetylation is 89% chitose, 6 grams, is dissolved in 2% the acetum, is made into 6% chitose solution, and the peek average molecular weight is that 3-6 ten thousand, content are 30 ± 2% polysiloxane emulsion 5 grams, carries out blend with above-mentioned chitose solution 100 grams;
(2), the glutaraldehyde water solutions (mass percent is 0.1%) of 4 grams are added in the above-mentioned blended liquids, stir under the room temperature, make glutaraldehyde carry out crosslinked chitose;
Following steps are with step (3), (4), (5), (6) of embodiment one.
Embodiment three:
Preparation chitose and polysiloxanes mass ratio are 1: 4 composite.
The preparation method step is identical with embodiment one, two, but chitose solution is 10 grams (mass percent is 6%) in the step (1), rapid silicone emulsion 80 grams (mass percent is 30%); Glutaraldehyde water solution is 5.8 grams in the step (2), and mass percent is 0.01%, and other step is identical with embodiment one, two.
Claims (9)
1, a kind of anticoagulation composite is characterized in that including chitose, polysiloxanes, and the mass ratio of chitose and polysiloxanes is 1: 99～99: 1.
2, composite according to claim 1, the mass ratio that it is characterized in that above-mentioned chitose and polysiloxanes is 1: 9～9: 1.
3, a kind of method for preparing the described composite of claim 1 is characterized in that following these steps to carrying out:
(1), chitose solution and polysiloxane emulsion are connect the certain mass ratio and carry out blend;
(2), cross-linking agent is added in the blended liquid, stir under the room temperature, make cross-linking agent carry out crosslinked chitose;
(3), pour casting film-forming in the mould into behind the static froth breaking, air-dryly put into baking oven freeze-day with constant temperature film forming again to solidifying substantially;
(4), earlier soak above-mentioned film material with dilute alkaline soln, reuse distilled water immersion, flushing are taken out the film material and are dried to constant weight to neutral;
(5), above-mentioned film material carries out crosslinked with cross-linking agent to polysiloxanes under acid condition;
(6), soak above-mentioned film material, reuse distilled water immersion, flushing are to neutral, and freeze-day with constant temperature is to constant weight with diluted alkaline.
4, preparation method according to claim 3 is characterized in that above-mentioned chitose solution is that 40%～100% chitose is dissolved in diluted acid and makes by deacetylation.
5, according to claim 3 or 4 described preparation methoies, the concentration that it is characterized in that above-mentioned chitose solution is 1 ‰～10%.
6, preparation method according to claim 3 is characterized in that the cross-linking agent in the above-mentioned steps (2) is the dialdehyde aqueous solution, and the mass ratio of dialdehyde crosslinking agent and chitose is 0.00001: 1～1: 10.
7, preparation method according to claim 6, the mass percent that it is characterized in that above-mentioned dialdehyde aqueous solution is 2.5PPm～2.5%.
8, preparation method according to claim 3, the polysiloxanes number-average molecular weight that it is characterized in that above-mentioned polysiloxane emulsion is 3 * 10
3～3 * 10
5
9, preparation method according to claim 3 is characterized in that the cross-linking agent in the above-mentioned steps (5) is a silicic acid fat.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96112801A CN1064265C (en) | 1996-08-29 | 1996-08-29 | Anticoagulation composite and its preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96112801A CN1064265C (en) | 1996-08-29 | 1996-08-29 | Anticoagulation composite and its preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1150913A CN1150913A (en) | 1997-06-04 |
| CN1064265C true CN1064265C (en) | 2001-04-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96112801A Expired - Fee Related CN1064265C (en) | 1996-08-29 | 1996-08-29 | Anticoagulation composite and its preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1064265C (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1112775A (en) * | 1993-07-21 | 1995-11-29 | 株式会社大塚制药工厂 | Medical material and process for producing the same |
| CN1128497A (en) * | 1994-05-17 | 1996-08-07 | 株式会社大塚制药工场 | Method of inhibiting blood coagulation during extracorporeal blood circulation and device for releasing antithrombotic drug used therein |
-
1996
- 1996-08-29 CN CN96112801A patent/CN1064265C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1112775A (en) * | 1993-07-21 | 1995-11-29 | 株式会社大塚制药工厂 | Medical material and process for producing the same |
| CN1128497A (en) * | 1994-05-17 | 1996-08-07 | 株式会社大塚制药工场 | Method of inhibiting blood coagulation during extracorporeal blood circulation and device for releasing antithrombotic drug used therein |
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| Publication number | Publication date |
|---|---|
| CN1150913A (en) | 1997-06-04 |
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