CN108815590A - A kind of preparation method of the compound anticoagulant biomaterial of polysaccharide-fibroin albumen - Google Patents
A kind of preparation method of the compound anticoagulant biomaterial of polysaccharide-fibroin albumen Download PDFInfo
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- A61L33/00—Antithrombogenic treatment of surgical articles, e.g. sutures, catheters, prostheses, or of articles for the manipulation or conditioning of blood; Materials for such treatment
- A61L33/06—Use of macromolecular materials
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- A61L33/00—Antithrombogenic treatment of surgical articles, e.g. sutures, catheters, prostheses, or of articles for the manipulation or conditioning of blood; Materials for such treatment
- A61L33/0005—Use of materials characterised by their function or physical properties
- A61L33/0011—Anticoagulant, e.g. heparin, platelet aggregation inhibitor, fibrinolytic agent, other than enzymes, attached to the substrate
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- A61L33/00—Antithrombogenic treatment of surgical articles, e.g. sutures, catheters, prostheses, or of articles for the manipulation or conditioning of blood; Materials for such treatment
- A61L33/04—Use of organic materials, e.g. acetylsalicylic acid
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- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L33/00—Antithrombogenic treatment of surgical articles, e.g. sutures, catheters, prostheses, or of articles for the manipulation or conditioning of blood; Materials for such treatment
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- A61L33/00—Antithrombogenic treatment of surgical articles, e.g. sutures, catheters, prostheses, or of articles for the manipulation or conditioning of blood; Materials for such treatment
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/42—Anti-thrombotic agents, anticoagulants, anti-platelet agents
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Abstract
The invention discloses a kind of preparation methods of compound anticoagulant biomaterial of polysaccharide-fibroin albumen, the technique is by cornstarch, Arabic gum, mannosan, polyethylene carbonic ester, polycarbonate, fibroin albumen, polydimethylsiloxane, triethyl phosphate, ethambutol, the raw materials such as methane sulfonic acid pass through sonic oscillation dispersion respectively, sieving sorting, heating in vacuum reaction, it is molded pressing mold, it is cooling to fix, ultrasonic cleaning, just, negative polyelectrolyte adsorption from aqueous solution balance, washing is dried, nitrogen protection solidification and etc. the compound anticoagulant biomaterial of polysaccharide-fibroin albumen is prepared.The compound anticoagulant biomaterial of polysaccharide-fibroin albumen being prepared, cost of material is low, has significant anticoagulation, antithrombotic acitivity, is suitable for the application in terms of a variety of medicinal blood tubing, auxiliary material.
Description
Technical field
The present invention relates to this technical fields of biomaterial, are related specifically to a kind of compound anticoagulation of polysaccharide-fibroin albumen
The preparation method of biomaterial.
Background technique
Blood environment is one of most important environment of human body, and good blood compatibility material can be widely used in all kinds of
With the medical intervention device of contacting blood, blood purification and dialysis apparatus are extracorporeal circulation apparatus and artificial lung, artificial liver, artificial
The various artificial organs such as heart.With huge clinical meaning.But it can be non-specific when the synthetic material and contacting blood of majority
Property induce the absorption of multiple proteins (including coagulation factor), it is living to pass through endogenous and exogenous cruor pathway inductive formation blood coagulation
Enzyme activates blood platelet, eventually leads to blood coagulation.People pass through synthesizing new anticoagulant material and the surface modification system to current material
The standby biomaterial with good anticoagulant property.Since existing various biomaterials usually have good physical mechanical property
With lower price, and it has been widely used in different kind organism medical apparatus, therefore repaired by the surface to current material
Decorations improve the anticoagulant property of material on maintaining material good physical mechanical performance ground foundation, are a kind of economically and efficiently sides
Formula.In current research application, it includes a variety of sufacings and the paintings such as chemical grafting treated, surface Graft copolymerization that people, which use,
Layer technology modifies material surface, by the surface charge, hydrophilic and hydrophobic, the various drugs of load and the biology that adjust material
Molecule improves anticoagulation, the anti-infection property of material, achieves preferable achievement.However, since these surface modification means are universal
There is the weakness such as solvent toxicity, complex technical process, controllable ability difference, not only greatly limit designing for material surface
Property, and cannot achieve the modification to the medical apparatus with complex geometry shape, it is not able to satisfy medical apparatus rapid development
It needs.Fibroin albumen is a kind of protein extracted from silk, have good biocompatibility, can prepare film forming, gel,
The material of the variforms such as microcapsules, due to its unique physicochemical property, fibroin material is in field of biomedical materials quilt
Extensive research, such as immobilised enzymes material, cell culture substrate, medicinal slow release agent, artificial organs.In order to improve fibroin egg
White performance, makes it be preferably applied for technical field of biological material, and domestic and foreign scholars carry out fibroin albumen by distinct methods
Chemical modification achieves some new research achievements.Also there is document report modified to fibroin material to improve fibroin egg
The physicochemical properties such as mechanical property, the thermal stability of white material;Change fibroin material to the rate of release of drug;Assign fibroin
The performance of protein material blood-clot resistance, the control that cell is grown etc..
Summary of the invention
In order to solve the above-mentioned technical problem, the invention discloses a kind of compound anticoagulant biomaterials of polysaccharide-fibroin albumen
Preparation method, the technique by cornstarch, Arabic gum, mannosan, polyethylene carbonic ester, polycarbonate, fibroin albumen,
The raw materials such as polydimethylsiloxane, triethyl phosphate, ethambutol, methane sulfonic acid pass through sonic oscillation dispersion respectively, sieving sorts,
Heating in vacuum is reacted, injection molding pressing mold, cooling fixed, ultrasonic cleaning, positive and negative polyelectrolyte adsorption from aqueous solution balances, washing is dried,
Nitrogen protection solidification and etc. the compound anticoagulant biomaterial of polysaccharide-fibroin albumen is prepared.Polysaccharide-the fibroin being prepared
The compound anticoagulant biomaterial of albumen, cost of material is low, has significant anticoagulation, antithrombotic acitivity, is suitable for a variety of doctors
With the application in terms of blood tubing, auxiliary material.
Technical solution：To solve the above-mentioned problems, the invention discloses a kind of compound anticoagulation biologies of polysaccharide-fibroin albumen
The preparation method of material, includes the following steps：
（1）By 20-25 parts of cornstarch, 10-16 parts of Arabic gum, 2-8 parts of mannosan, 10-18 parts of polyethylene carbonic ester, gather
2-8 parts of carbonic ester, 8-10 parts of fibroin albumen, 2-5 parts of coupling agent are added in ultrasonator and are dispersed, are coupled, and what is obtained is molten
Liquid sieving sorting, it is spare；
（2）By step（1）Solution be added in vacuum reaction kettle, polydimethylsiloxane 2- is sequentially added after being heated to 50 DEG C
6 parts, 2-5 parts of triethyl phosphate, 1-2 parts of ethambutol, 3-6 parts of methane sulfonic acid, then temperature rises to 180-185 DEG C again, takes out
Vacuum, sustained response 2-5h, air pressure returns back to normal pressure in furnace after reaction, and reactant heat preservation is spare；
（3）By step（2）Reaction solution injection injection molding machine in carry out injection molding pressing mold, then cooling, fixed, demoulding；
（4）By step（3）Moulding be put into sterile distilled water and be cleaned by ultrasonic, removal surface organic impurities residual is dried in the air
It is dry；
（5）By step（4）Moulding be put into positive polyelectrolyte aqueous solution and carry out, adsorption equilibrium 30-50min, with sterile steaming
Distilled water washing, naturally dry；
（6）By step（5）Moulding be put into negative polyelectrolyte aqueous solution and carry out, adsorption equilibrium 30-50min, with sterile steaming
Distilled water washing, naturally dry；
（7）With ethyl alcohol cleaning step（6）Moulding material is carried out under 75-80 DEG C of nitrogen protection atmosphere then with being dried with nitrogen
Material solidification 90-150min, is then packed to get finished product.
Preferably, the step（1）In ultrasonic power be 250KW, sonic oscillation 30-50min.
Preferably, the step（1）In cross mesh size be 2000 mesh.
Preferably, the step（1）In coupling agent be selected from tetra isopropyl two（Phosphorous acid dilauryl）Titanate esters, two
（Dioctyl pyrophosphoryl base）Oxygen-containing acetic acid esters titanium, isopropyl three（Isostearoyl base）Titanate esters, two（Dioctyl pyrophosphoryl base）Second
Support one or more of titanate esters.
Preferably, the step（2）In vacuum pressure be 5*10-8Pa。
Preferably, the step（3）In injecting condition be nozzle temperature be 150-180 DEG C, the temperature in an area and 2nd area
It is 150-180 DEG C, the temperature in 3rd area and 4th area is 130-150 DEG C, and the temperature in 5th area and 6th area is 130-150 DEG C, injection mold
Mould temperature be 90-95 DEG C, injection pressure 100-150MPa, injection speed 220-300mm/s.
Preferably, the step（5）In positive polyelectrolyte aqueous solution composition be w/v：Collagen 10%,
Lactalbumin 3%, legumelin 8%, chitin 4%, glucan 1%, magnesium sulfate 1%, potassium chloride 1%, water.
Preferably, the step（6）In negative polyelectrolyte aqueous solution composition be w/v：Hyaluronic acid 6%,
Kayexalate 8%, sodium alginate 10%, mannitol 1%, heparin 1%, ethyl alcohol 1%, water.
Preferably, the step（7）In nitrogen pressure be 2Mpa.
Compared with prior art, the present invention its advantages are：
（1）A kind of preparation method of compound anticoagulant biomaterial of polysaccharide-fibroin albumen of the invention is by cornstarch, Arab
Glue, mannosan, polyethylene carbonic ester, polycarbonate, fibroin albumen, polydimethylsiloxane, triethyl phosphate, ethambutol,
The raw materials such as methane sulfonic acid pass through sonic oscillation dispersion respectively, sieving sorting, heating in vacuum reaction, are molded pressing mold, are cooling fixed, super
Sound cleaning, positive and negative polyelectrolyte adsorption from aqueous solution balance, washing dry, nitrogen protection solidification and etc. polysaccharide-silk is prepared
The compound anticoagulant biomaterial of fibroin.The compound anticoagulant biomaterial of polysaccharide-fibroin albumen being prepared, cost of material
It is low, have significant anticoagulation, antithrombotic acitivity, be suitable for the application in terms of a variety of medicinal blood tubing, auxiliary material.
（2）The compound anticoagulant biomaterial raw material of polysaccharide-fibroin albumen of the invention is easy to get, simple process, is suitable for big rule
Mould industrialization is used, practical.
Specific embodiment
Embodiment 1
（1）By 20 parts of cornstarch, 10 parts of Arabic gum, 2 parts of mannosan, 10 parts of polyethylene carbonic ester, 2 parts of polycarbonate,
8 parts of fibroin albumen, tetra isopropyl two（Phosphorous acid dilauryl）It 2 parts of titanate esters, is added in ultrasonator and is dispersed, is even
Connection, obtained solution sieving sorting, spare, wherein ultrasonic power is 250KW, sonic oscillation 30min, and crossing mesh size is 2000
Mesh；
（2）By step（1）Solution be added in vacuum reaction kettle, polydimethylsiloxane 2 is sequentially added after being heated to 50 DEG C
Part, 2 parts of triethyl phosphate, 1 part of ethambutol, 3 parts of methane sulfonic acid, then temperature rises to 180-185 DEG C again, vacuumizes, very
Pneumatics is 5*10 by force-8Pa, sustained response 2h, air pressure returns back to normal pressure in furnace after reaction, and reactant heat preservation is spare；
（3）By step（2）Reaction solution injection injection molding machine in carry out injection molding pressing mold, then cooling, fixed, demoulding, wherein infusing
Modeling condition is that nozzle temperature is 150-180 DEG C, and the temperature in an area and 2nd area is 150-180 DEG C, and the temperature in 3rd area and 4th area is
130-150 DEG C, the temperature in 5th area and 6th area is 130-150 DEG C, and the mould temperature of injection mold is 90-95 DEG C, injection pressure 100-
150MPa, injection speed 220-300mm/s；
（4）By step（3）Moulding be put into sterile distilled water and be cleaned by ultrasonic, removal surface organic impurities residual is dried in the air
It is dry；
（5）By step（4）Moulding be put into positive polyelectrolyte aqueous solution and carry out, adsorption equilibrium 30min uses sterile distilled water
Washing, naturally dry, the composition of positive polyelectrolyte aqueous solution are w/v：Collagen 10%, lactalbumin 3%, beans are clear
Albumen 8%, chitin 4%, glucan 1%, magnesium sulfate 1%, potassium chloride 1%, water；
（6）By step（5）Moulding be put into negative polyelectrolyte aqueous solution and carry out, adsorption equilibrium 30min uses sterile distilled water
Washing, naturally dry, the composition of negative polyelectrolyte aqueous solution are w/v：Hyaluronic acid 6%, kayexalate 8%,
Sodium alginate 10%, mannitol 1%, heparin 1%, ethyl alcohol 1%, water；
（7）With ethyl alcohol cleaning step（6）Moulding, then with being dried with nitrogen, at 75-80 DEG C, the nitrogen that pressure is 2MPa is protected
It protects and carries out material solidification 90min under atmosphere, then pack to get finished product.
Embodiment 2
（1）By 22 parts of cornstarch, 13 parts of Arabic gum, 4 parts of mannosan, 12 parts of polyethylene carbonic ester, 3 parts of polycarbonate,
9 parts of fibroin albumen, two（Dioctyl pyrophosphoryl base）3 parts of oxygen-containing acetic acid esters titanium is added in ultrasonator and is dispersed, is coupled,
Obtained solution sieving sorting, spare, wherein ultrasonic power is 250KW, sonic oscillation 30min, and crossing mesh size is 2000 mesh；
（2）By step（1）Solution be added in vacuum reaction kettle, polydimethylsiloxane 3 is sequentially added after being heated to 50 DEG C
Part, 3 parts of triethyl phosphate, 1 part of ethambutol, 4 parts of methane sulfonic acid, then temperature rises to 180-185 DEG C again, vacuumizes, very
Pneumatics is 5*10 by force-8Pa, sustained response 3h, air pressure returns back to normal pressure in furnace after reaction, and reactant heat preservation is spare；
（3）By step（2）Reaction solution injection injection molding machine in carry out injection molding pressing mold, then cooling, fixed, demoulding, wherein infusing
Modeling condition is that nozzle temperature is 150-180 DEG C, and the temperature in an area and 2nd area is 150-180 DEG C, and the temperature in 3rd area and 4th area is
130-150 DEG C, the temperature in 5th area and 6th area is 130-150 DEG C, and the mould temperature of injection mold is 90-95 DEG C, injection pressure 100-
150MPa, injection speed 220-300mm/s；
（4）By step（3）Moulding be put into sterile distilled water and be cleaned by ultrasonic, removal surface organic impurities residual is dried in the air
It is dry；
（5）By step（4）Moulding be put into positive polyelectrolyte aqueous solution and carry out, adsorption equilibrium 35min uses sterile distilled water
Washing, naturally dry, the composition of positive polyelectrolyte aqueous solution are w/v：Collagen 10%, lactalbumin 3%, beans are clear
Albumen 8%, chitin 4%, glucan 1%, magnesium sulfate 1%, potassium chloride 1%, water；
（6）By step（5）Moulding be put into negative polyelectrolyte aqueous solution and carry out, adsorption equilibrium 35min uses sterile distilled water
Washing, naturally dry, the composition of negative polyelectrolyte aqueous solution are w/v：Hyaluronic acid 6%, kayexalate 8%,
Sodium alginate 10%, mannitol 1%, heparin 1%, ethyl alcohol 1%, water；
（7）With ethyl alcohol cleaning step（6）Moulding, then with being dried with nitrogen, at 75-80 DEG C, the nitrogen that pressure is 2MPa is protected
It protects and carries out material solidification 100min under atmosphere, then pack to get finished product.
Embodiment 3
（1）By 24 parts of cornstarch, 14 parts of Arabic gum, 7 parts of mannosan, 16 parts of polyethylene carbonic ester, 6 parts of polycarbonate,
9 parts of fibroin albumen, isopropyl three（Isostearoyl base）It 4 parts of titanate esters, is added in ultrasonator and is dispersed, is coupled, obtain
Solution be sieved sorting, it is spare, wherein ultrasonic power be 250KW, sonic oscillation 30min, cross mesh size be 2000 mesh；
（2）By step（1）Solution be added in vacuum reaction kettle, polydimethylsiloxane 5 is sequentially added after being heated to 50 DEG C
Part, 4 parts of triethyl phosphate, 2 parts of ethambutol, 5 parts of methane sulfonic acid, then temperature rises to 180-185 DEG C again, vacuumizes, very
Pneumatics is 5*10 by force-8Pa, sustained response 4h, air pressure returns back to normal pressure in furnace after reaction, and reactant heat preservation is spare；
（3）By step（2）Reaction solution injection injection molding machine in carry out injection molding pressing mold, then cooling, fixed, demoulding, wherein infusing
Modeling condition is that nozzle temperature is 150-180 DEG C, and the temperature in an area and 2nd area is 150-180 DEG C, and the temperature in 3rd area and 4th area is
130-150 DEG C, the temperature in 5th area and 6th area is 130-150 DEG C, and the mould temperature of injection mold is 90-95 DEG C, injection pressure 100-
150MPa, injection speed 220-300mm/s；
（4）By step（3）Moulding be put into sterile distilled water and be cleaned by ultrasonic, removal surface organic impurities residual is dried in the air
It is dry；
（5）By step（4）Moulding be put into positive polyelectrolyte aqueous solution and carry out, adsorption equilibrium 45min uses sterile distilled water
Washing, naturally dry, the composition of positive polyelectrolyte aqueous solution are w/v：Collagen 10%, lactalbumin 3%, beans are clear
Albumen 8%, chitin 4%, glucan 1%, magnesium sulfate 1%, potassium chloride 1%, water；
（6）By step（5）Moulding be put into negative polyelectrolyte aqueous solution and carry out, adsorption equilibrium 45min uses sterile distilled water
Washing, naturally dry, the composition of negative polyelectrolyte aqueous solution are w/v：Hyaluronic acid 6%, kayexalate 8%,
Sodium alginate 10%, mannitol 1%, heparin 1%, ethyl alcohol 1%, water；
（7）With ethyl alcohol cleaning step（6）Moulding, then with being dried with nitrogen, at 75-80 DEG C, the nitrogen that pressure is 2MPa is protected
It protects and carries out material solidification 120min under atmosphere, then pack to get finished product.
Embodiment 4
（1）By 25 parts of cornstarch, 16 parts of Arabic gum, 8 parts of mannosan, 18 parts of polyethylene carbonic ester, 8 parts of polycarbonate,
10 parts of fibroin albumen, two（Dioctyl pyrophosphoryl base）It 5 parts of ethylene titanate esters, is added in ultrasonator and is dispersed, is coupled, obtain
The solution sieving sorting arrived, spare, wherein ultrasonic power is 250KW, sonic oscillation 30min, and crossing mesh size is 2000 mesh；
（2）By step（1）Solution be added in vacuum reaction kettle, polydimethylsiloxane 6 is sequentially added after being heated to 50 DEG C
Part, 5 parts of triethyl phosphate, 2 parts of ethambutol, 6 parts of methane sulfonic acid, then temperature rises to 180-185 DEG C again, vacuumizes, very
Pneumatics is 5*10 by force-8Pa, sustained response 5h, air pressure returns back to normal pressure in furnace after reaction, and reactant heat preservation is spare；
（3）By step（2）Reaction solution injection injection molding machine in carry out injection molding pressing mold, then cooling, fixed, demoulding, wherein infusing
Modeling condition is that nozzle temperature is 150-180 DEG C, and the temperature in an area and 2nd area is 150-180 DEG C, and the temperature in 3rd area and 4th area is
130-150 DEG C, the temperature in 5th area and 6th area is 130-150 DEG C, and the mould temperature of injection mold is 90-95 DEG C, injection pressure 100-
150MPa, injection speed 220-300mm/s；
（4）By step（3）Moulding be put into sterile distilled water and be cleaned by ultrasonic, removal surface organic impurities residual is dried in the air
It is dry；
（5）By step（4）Moulding be put into positive polyelectrolyte aqueous solution and carry out, adsorption equilibrium 50min uses sterile distilled water
Washing, naturally dry, the composition of positive polyelectrolyte aqueous solution are w/v：Collagen 10%, lactalbumin 3%, beans are clear
Albumen 8%, chitin 4%, glucan 1%, magnesium sulfate 1%, potassium chloride 1%, water；
（6）By step（5）Moulding be put into negative polyelectrolyte aqueous solution and carry out, adsorption equilibrium 50min uses sterile distilled water
Washing, naturally dry, the composition of negative polyelectrolyte aqueous solution are w/v：Hyaluronic acid 6%, kayexalate 8%,
Sodium alginate 10%, mannitol 1%, heparin 1%, ethyl alcohol 1%, water；
（7）With ethyl alcohol cleaning step（6）Moulding, then with being dried with nitrogen, at 75-80 DEG C, the nitrogen that pressure is 2MPa is protected
It protects and carries out material solidification 150min under atmosphere, then pack to get finished product.
Comparative example 1
（1）By 20 parts of cornstarch, 10 parts of Arabic gum, 10 parts of polyethylene carbonic ester, 2 parts of polycarbonate, tetra isopropyl two（It is sub-
Didodecyl phosphate）It 2 parts of titanate esters, being added in ultrasonator and is dispersed, is coupled, obtained solution sieving sorting is spare,
Wherein ultrasonic power is 250KW, sonic oscillation 30min, and crossing mesh size is 2000 mesh；
（2）By step（1）Solution be added in vacuum reaction kettle, polydimethylsiloxane 2 is sequentially added after being heated to 50 DEG C
Part, 2 parts of triethyl phosphate, 1 part of ethambutol, 3 parts of methane sulfonic acid, then temperature rises to 180-185 DEG C again, vacuumizes, very
Pneumatics is 5*10 by force-8Pa, sustained response 2h, air pressure returns back to normal pressure in furnace after reaction, and reactant heat preservation is spare；
（3）By step（2）Reaction solution injection injection molding machine in carry out injection molding pressing mold, then cooling, fixed, demoulding, wherein infusing
Modeling condition is that nozzle temperature is 150-180 DEG C, and the temperature in an area and 2nd area is 150-180 DEG C, and the temperature in 3rd area and 4th area is
130-150 DEG C, the temperature in 5th area and 6th area is 130-150 DEG C, and the mould temperature of injection mold is 90-95 DEG C, injection pressure 100-
150MPa, injection speed 220-300mm/s；
（4）By step（3）Moulding be put into sterile distilled water and be cleaned by ultrasonic, removal surface organic impurities residual is dried in the air
It is dry；
（5）By step（4）Moulding be put into positive polyelectrolyte aqueous solution and carry out, adsorption equilibrium 30min uses sterile distilled water
Washing, naturally dry, the composition of positive polyelectrolyte aqueous solution are w/v：Collagen 10%, lactalbumin 3%, beans are clear
Albumen 8%, chitin 4%, glucan 1%, magnesium sulfate 1%, potassium chloride 1%, water；
（6）By step（5）Moulding be put into negative polyelectrolyte aqueous solution and carry out, adsorption equilibrium 30min uses sterile distilled water
Washing, naturally dry, the composition of negative polyelectrolyte aqueous solution are w/v：Hyaluronic acid 6%, kayexalate 8%,
Sodium alginate 10%, mannitol 1%, heparin 1%, ethyl alcohol 1%, water；
（7）With ethyl alcohol cleaning step（6）Moulding, then with being dried with nitrogen, at 75-80 DEG C, the nitrogen that pressure is 2MPa is protected
It protects and carries out material solidification 90min under atmosphere, then pack to get finished product.
Comparative example 2
（1）By 25 parts of cornstarch, 16 parts of Arabic gum, 8 parts of mannosan, 18 parts of polyethylene carbonic ester, 8 parts of polycarbonate,
10 parts of fibroin albumen, two（Dioctyl pyrophosphoryl base）It 5 parts of ethylene titanate esters, is added in ultrasonator and is dispersed, is coupled, obtain
The solution sieving sorting arrived, spare, wherein ultrasonic power is 250KW, sonic oscillation 30min, and crossing mesh size is 2000 mesh；
（2）By step（1）Solution be added in vacuum reaction kettle, polydimethylsiloxane 6 is sequentially added after being heated to 50 DEG C
Part, 5 parts of triethyl phosphate, 2 parts of ethambutol, 6 parts of methane sulfonic acid, then temperature rises to 180-185 DEG C again, vacuumizes, very
Pneumatics is 5*10 by force-8Pa, sustained response 5h, air pressure returns back to normal pressure in furnace after reaction, and reactant heat preservation is spare；
（3）By step（2）Reaction solution injection injection molding machine in carry out injection molding pressing mold, then cooling, fixed, demoulding, wherein infusing
Modeling condition is that nozzle temperature is 150-180 DEG C, and the temperature in an area and 2nd area is 150-180 DEG C, and the temperature in 3rd area and 4th area is
130-150 DEG C, the temperature in 5th area and 6th area is 130-150 DEG C, and the mould temperature of injection mold is 90-95 DEG C, injection pressure 100-
150MPa, injection speed 220-300mm/s；
（4）By step（3）Moulding be put into sterile distilled water and be cleaned by ultrasonic, removal surface organic impurities residual is dried in the air
It is dry；
（5）By step（4）Moulding be put into positive polyelectrolyte aqueous solution and carry out, adsorption equilibrium 50min uses sterile distilled water
Washing, naturally dry, the composition of positive polyelectrolyte aqueous solution are w/v：Collagen 10%, lactalbumin 3%, beans are clear
Albumen 8%, chitin 4%, glucan 1%, magnesium sulfate 1%, potassium chloride 1%, water；
（6）By step（5）Moulding be put into negative polyelectrolyte aqueous solution and carry out, adsorption equilibrium 50min uses sterile distilled water
Washing, naturally dry, the composition of negative polyelectrolyte aqueous solution are w/v：Hyaluronic acid 6%, kayexalate 8%,
Sodium alginate 10%, mannitol 1%, heparin 1%, ethyl alcohol 1%, water；
（7）With ethyl alcohol cleaning step（6）Moulding, naturally dry solidification, then pack to get finished product.
The compound anticoagulant biomaterial of polysaccharide-fibroin albumen obtained of embodiment 1-4 and comparative example 1-2 is carried out respectively
This several Whole blood experiments, blood coagulation test, antioxygenic property performance tests, test result are shown in Table 1.
Table 1
| Whole blood experiments | 30min is tested in blood coagulation | Antioxygenic property | |
| Embodiment 1 | Without thrombus | Without blood coagulation | Well |
| Embodiment 2 | Without thrombus | Without blood coagulation | Well |
| Embodiment 3 | Without thrombus | Without blood coagulation | Well |
| Embodiment 4 | Without thrombus | Without blood coagulation | Well |
| Comparative example 1 | Slight thrombus | Without blood coagulation | Generally |
| Comparative example 2 | Without thrombus | Without blood coagulation | Generally |
A kind of preparation method of compound anticoagulant biomaterial of polysaccharide-fibroin albumen of the invention by cornstarch, Arabic gum,
Mannosan, polyethylene carbonic ester, polycarbonate, fibroin albumen, polydimethylsiloxane, triethyl phosphate, ethambutol, methyl
The raw materials such as sulfonic acid pass through sonic oscillation dispersion respectively, sieving sorts, heating in vacuum reaction, are molded pressing mold, are cooling fixed, ultrasonic clear
Wash, positive and negative polyelectrolyte adsorption from aqueous solution balance, washing dry, nitrogen protection solidification and etc. polysaccharide-fibroin egg is prepared
Bai Fuhe anticoagulant biomaterial.The compound anticoagulant biomaterial of polysaccharide-fibroin albumen being prepared, cost of material is low,
With significant anticoagulation, antithrombotic acitivity, it is suitable for the application in terms of a variety of medicinal blood tubing, auxiliary material.Of the invention is more
The compound anticoagulant biomaterial raw material of sugar-fibroin albumen is easy to get, simple process, is suitable for heavy industrialization and uses, practical.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (9)
1. a kind of preparation method of the compound anticoagulant biomaterial of polysaccharide-fibroin albumen, which is characterized in that include the following steps：
（1）By 20-25 parts of cornstarch, 10-16 parts of Arabic gum, 2-8 parts of mannosan, 10-18 parts of polyethylene carbonic ester, gather
2-8 parts of carbonic ester, 8-10 parts of fibroin albumen, 2-5 parts of coupling agent are added in ultrasonator and are dispersed, are coupled, and what is obtained is molten
Liquid sieving sorting, it is spare；
（2）By step（1）Solution be added in vacuum reaction kettle, polydimethylsiloxane 2- is sequentially added after being heated to 50 DEG C
6 parts, 2-5 parts of triethyl phosphate, 1-2 parts of ethambutol, 3-6 parts of methane sulfonic acid, then temperature rises to 180-185 DEG C again, takes out
Vacuum, sustained response 2-5h, air pressure returns back to normal pressure in furnace after reaction, and reactant heat preservation is spare；
（3）By step（2）Reaction solution injection injection molding machine in carry out injection molding pressing mold, then cooling, fixed, demoulding；
（4）By step（3）Moulding be put into sterile distilled water and be cleaned by ultrasonic, removal surface organic impurities residual is dried in the air
It is dry；
（5）By step（4）Moulding be put into positive polyelectrolyte aqueous solution and carry out, adsorption equilibrium 30-50min, with sterile steaming
Distilled water washing, naturally dry；
（6）By step（5）Moulding be put into negative polyelectrolyte aqueous solution and carry out, adsorption equilibrium 30-50min, with sterile steaming
Distilled water washing, naturally dry；
（7）With ethyl alcohol cleaning step（6）Moulding material is carried out under 75-80 DEG C of nitrogen protection atmosphere then with being dried with nitrogen
Material solidification 90-150min, is then packed to get finished product.
2. the preparation method of the compound anticoagulant biomaterial of polysaccharide-fibroin albumen according to claim 1, feature exist
In the step（1）In ultrasonic power be 250KW, sonic oscillation 30-50min.
3. the preparation method of the compound anticoagulant biomaterial of polysaccharide-fibroin albumen according to claim 1, feature exist
In the step（1）In cross mesh size be 2000 mesh.
4. the preparation method of the compound anticoagulant biomaterial of polysaccharide-fibroin albumen according to claim 1, feature exist
In the step（1）In coupling agent be selected from tetra isopropyl two（Phosphorous acid dilauryl）Titanate esters, two（Dioctyl pyrophosphoryl
Base）Oxygen-containing acetic acid esters titanium, isopropyl three（Isostearoyl base）Titanate esters, two（Dioctyl pyrophosphoryl base）One in ethylene titanate esters
Kind is several.
5. the preparation method of the compound anticoagulant biomaterial of polysaccharide-fibroin albumen according to claim 1, feature exist
In the step（2）In vacuum pressure be 5*10-8Pa。
6. the preparation method of the compound anticoagulant biomaterial of polysaccharide-fibroin albumen according to claim 1, feature exist
In the step（3）In injecting condition be nozzle temperature be 150-180 DEG C, the temperature in an area and 2nd area is 150-180 DEG C,
The temperature in 3rd area and 4th area is 130-150 DEG C, and the temperature in 5th area and 6th area is 130-150 DEG C, and the mould temperature of injection mold is 90-95
DEG C, injection pressure 100-150MPa, injection speed 220-300mm/s.
7. the preparation method of the compound anticoagulant biomaterial of polysaccharide-fibroin albumen according to claim 1, feature exist
In the step（5）In positive polyelectrolyte aqueous solution composition be w/v：Collagen 10%, lactalbumin 3%,
Legumelin 8%, chitin 4%, glucan 1%, magnesium sulfate 1%, potassium chloride 1%, water.
8. the preparation method of the compound anticoagulant biomaterial of polysaccharide-fibroin albumen according to claim 1, feature exist
In the step（6）In negative polyelectrolyte aqueous solution composition be w/v：Hyaluronic acid 6%, polystyrolsulfon acid
Sodium 8%, sodium alginate 10%, mannitol 1%, heparin 1%, ethyl alcohol 1%, water.
9. the preparation method of the compound anticoagulant biomaterial of polysaccharide-fibroin albumen according to claim 1, feature exist
In the step（7）In nitrogen pressure be 2MPa.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109893684A (en) * | 2019-02-11 | 2019-06-18 | 赵延延 | A kind of preparation method of the compound anticoagulant biomaterial of carboxymethyl chitosan |
| CN109942903A (en) * | 2019-02-11 | 2019-06-28 | 赵延延 | A kind of preparation method of antibacterial type blood compatibility biological material |
| CN114681685A (en) * | 2022-04-08 | 2022-07-01 | 东莞市人民医院 | Preparation method of hybrid protein coating, hybrid protein coating material and application |
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| CN1897986A (en) * | 2003-09-29 | 2007-01-17 | 莱萨克集团股份有限公司 | Polysaccharide phyllosilicate absorbent or superabsorbent nanocomposite materials |
| CN103736157A (en) * | 2013-12-20 | 2014-04-23 | 江苏科技大学 | Composite anticoagulation material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1897986A (en) * | 2003-09-29 | 2007-01-17 | 莱萨克集团股份有限公司 | Polysaccharide phyllosilicate absorbent or superabsorbent nanocomposite materials |
| CN103736157A (en) * | 2013-12-20 | 2014-04-23 | 江苏科技大学 | Composite anticoagulation material and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109893684A (en) * | 2019-02-11 | 2019-06-18 | 赵延延 | A kind of preparation method of the compound anticoagulant biomaterial of carboxymethyl chitosan |
| CN109942903A (en) * | 2019-02-11 | 2019-06-28 | 赵延延 | A kind of preparation method of antibacterial type blood compatibility biological material |
| CN114681685A (en) * | 2022-04-08 | 2022-07-01 | 东莞市人民医院 | Preparation method of hybrid protein coating, hybrid protein coating material and application |
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