CN115873299A - Porous cellulose/gelatin composite hemostatic aerogel and preparation method and application thereof - Google Patents
Porous cellulose/gelatin composite hemostatic aerogel and preparation method and application thereof Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Materials For Medical Uses (AREA)
Abstract
The invention discloses a porous cellulose/gelatin composite hemostatic aerogel and a preparation method and application thereof, and belongs to the technical field of biological medicines. The porous cellulose/gelatin composite hemostatic aerogel prepared by the invention is compounded by I-type gelatin, microcrystalline cellulose and diatomite, firstly, quantitative microcrystalline cellulose, gelatin and diatomite are added into an ionic liquid solvent and are uniformly stirred, then, the mixed solution is placed in an oil bath pot for heating treatment,dropping the obtained solution into deionized water by using an injector, and replacing the solution with the deionized water for multiple times until AgNO is dropped 3 The solution has no white precipitate, and is finally freeze-dried without pre-freezing. The aerogel material disclosed by the invention has a relatively abundant internal pore structure, can quickly absorb water in blood, can be directly used for bleeding wounds, is quick in hemostasis and good in effect, and has a certain adhesive plugging effect. The preparation method is simple, low in process requirement, low in energy consumption and easy for large-scale industrial production.
Description
Technical Field
The invention belongs to the technical field of biological medicines, particularly relates to a cellulose-based hemostatic material, and more particularly relates to a porous cellulose/gelatin composite hemostatic aerogel and a preparation method and application thereof.
Background
In daily life, medical surgery, and the like, unexpected bleeding sometimes occurs, and uncontrolled bleeding may lead to serious consequences. In an emergency, when acute hemorrhage exceeds 800-1000mL, hemorrhagic shock, microbial infection, multi-organ failure and even life-threatening serious conditions can be caused. Therefore, timely use of safe and effective hemostatic materials to control bleeding is critical to avoid serious complications, reduce mortality, and the like. After bleeding occurs due to wound generation, the body's own repair mechanism is mediated by blood vessels, platelets, the fibrinolytic equilibrium system and the blood coagulation system. The blood flowing speed is slowed down by the contraction of the blood vessel wall, the blood platelets are adhered to the surface of foreign matters to deform, coagulation factors are released to activate thromboplastin in the blood, generated thrombin acts on dissolved fibrinogen in the blood, the dissolved fibrinogen is converted into solid fibrin to be connected into a net structure to adsorb red blood cells, and finally, thrombus is formed on the surface of a wound under the combined action of the fibrin net and the blood platelets to inhibit the bleeding condition.
At present, the hemostatic materials used clinically mainly include inorganic hemostatic materials and natural organic high molecular polymer hemostatic materials, and the inorganic components used for preparing the hemostatic materials mainly include zeolite, clay, kaolin, mesoporous silicon and the like, but in view of the problems of poor biocompatibility and degradability of the inorganic materials, the organic hemostatic materials of natural components are more popular and mainly comprise chitosan, cellulose, gelatin, starch, sodium alginate and the like. The hemostatic materials commonly used in the market at present are common cotton gauze, hemostatic bandages, gelatin sponges, regenerated oxidized cellulose sponges, celox hemostatic powder and the like.
As a clinical commonly used local hemostatic material, the solid collagen material has good hemostatic performance, promotes platelet aggregation by combining with platelets, directly activates an endogenous coagulation pathway to generate a coagulation effect, and simultaneously blood cells are adhered to form a thrombus clot so as to effectively prevent blood from washing away wounds. In addition, the collagen can promote granulation tissue generation and accelerate wound healing. A large number of researches show that the hemostatic activity of the collagen material is obviously superior to that of other polysaccharide hemostatic materials, and the collagen material can also have strong affinity with cells and growth factors in the wound healing process, so that wound repair and tissue regeneration are promoted.
In recent years, gelatin sponges have been widely used in the fields of drug release, medical dressings, cell culture, tissue engineering, and the like. The medical sponge used for a biological system needs to meet the following requirements, such as good biocompatibility, cell compatibility and histocompatibility. Biocompatibility is the first problem in the application of biological materials in the human body, and is also the key to the clinical application. The ideal hemostatic sponge has the characteristics of good porosity and hydrophilicity, higher air permeability and water absorption, moderate mechanical strength, high hemostatic efficiency, good biocompatibility and degradable absorbability, easy tissue absorption, rich raw materials and the like. At present, the common medical sponge can not meet the requirement.
At present, cotton gauze and bandages on the market can only temporarily compress for hemostasis, gelatin sponge can only locally absorb a small amount of blood, regenerated oxidized cellulose sponge is expensive and can only control small-flow bleeding, celox hemostatic powder can effectively control large-flow bleeding, but the material is difficult to degrade, and the residual material in a wound must be removed before an operation. The research and development of the ideal hemostatic material with multiple functions is the work which is concerned and paid attention by scientific researchers at home and abroad. In view of the above, there is a need to design a porous fiber composite hemostatic material.
Disclosure of Invention
In view of the above-mentioned reasons, the present invention aims to provide a porous cellulose/gelatin composite hemostatic aerogel, a preparation method and an application thereof, which solve or at least partially solve the above-mentioned technical drawbacks in the prior art.
In order to achieve one of the above objects of the present invention, the present invention adopts the following technical solutions:
a preparation method of a porous cellulose/gelatin composite hemostatic aerogel specifically comprises the following steps:
(1) Pretreatment: drying microcrystalline cellulose and diatomite; crushing gelatin to obtain gelatin powder;
(2) Mixing treatment: taking ionic liquid (chloridized-1-butyl-3-methylimidazole) as a solvent, adding the dried microcrystalline cellulose prepared in the step (1), diatomite and gelatin powder, and uniformly mixing to obtain a mixed solution a;
(3) And (3) heat treatment: stirring and heating the mixed solution a in the step (2) to obtain a cellulose composite solution b;
(4) And (3) regeneration reaction: dripping the cellulose composite solution b prepared in the step (3) into water by a falling ball method to prepare a composite cellulose hydrogel ball c;
(5) Cleaning: washing residual solvent in the composite cellulose hydrogel ball c prepared in the step (4) by using deionized water to obtain a composite cellulose hydrogel ball d;
(6) And (3) freeze drying: and (4) freeze-drying the composite cellulose hydrogel spheres d prepared in the step (5) to obtain the porous cellulose/gelatin composite hemostatic aerogel.
Further, in the above technical solution, the drying treatment in the step (1) may be hot air drying or vacuum drying. For example, in a preferred embodiment of the present invention, the drying process specifically includes the following steps: the drying temperature is 45-120 deg.C, and the drying time is 6-24h.
Further, in the above technical solution, the gelatin in step (1) is a biotechnological grade gelatin, and may be, for example, commercially available type I gelatin.
Further, in the technical scheme, the size of the gelatin powder in the step (1) is preferably 60-100 meshes.
Further, in the above technical scheme, the mass fraction of the chlorinated 1-butyl-3-methylimidazole in the solvent in the step (2) is 99%.
Further, according to the technical scheme, the total mass fraction of the microcrystalline cellulose, the gelatin and the diatomite added in the step (2) in the mixed solution a is 3-8%.
Further, according to the technical scheme, the mass ratio of the microcrystalline cellulose, the gelatin and the diatomite added in the step (2) is (3-7): (1-2): 1. for example, in a preferred embodiment of the present invention, the mass ratio of the added microcrystalline cellulose, gelatin and diatomaceous earth may be 4:1:1,7:2:1,3:1:1.
further, according to the technical scheme, in the step (3), the heating temperature is 80-120 ℃, the stirring speed is 300-800rpm, and the stirring and heating time is 20-120min.
Further, in the above technical scheme, the washing step in the step (5) is specifically: replacing 4-8 times with deionized water, i.e. replacing 4-8 times with deionized water until AgNO is dropped 3 The solution has no white precipitate, each time for 1-3h.
Preferably, in the above technical scheme, the number of the substitutions is 6, and the time for each substitution is 2h.
Further, in the technical scheme, the freeze drying in the step (6) is preferably vacuum freeze drying, and the temperature of the vacuum freeze drying is-65 ℃ to-35 ℃ for 24-48h.
Further, according to the technical scheme, the preparation method further comprises the step of recovering the ionic liquid, and the specific operation is as follows: and filtering the residual solvent to remove impurities, and performing rotary evaporation to recover the ionic liquid.
Preferably, in the technical scheme, the temperature of the rotary evaporation is 80 ℃, and the rotating speed is 120-240rpm.
Further, in the above technical solution, the ionic liquid or a part of the ionic liquid in the step (2) is the ionic liquid recovered as described above.
The second purpose of the invention is to provide the porous cellulose/gelatin composite hemostatic aerogel prepared by the method. The aerogel has the aperture of 6-20 mu m and a richer internal pore structure.
The third purpose of the invention is to provide the application of the porous cellulose/gelatin composite hemostatic aerogel prepared by the method as a rapid hemostatic material.
The invention relates to a rapid hemostatic material, which comprises porous cellulose/gelatin composite hemostatic aerogel prepared by the method.
Compared with the prior art, the invention has the advantages and positive effects that:
1. the cellulose-based composite hydrogel spheres prepared by the invention are prepared by slowly replacing a composite solution in an anti-solvent system, regenerating cellulose and gelatin molecules in the anti-solvent system to obtain a highly abundant space network structure, and removing moisture in the gel system through freeze drying to obtain the aerogel material with abundant pore diameters. Firstly, cellulose is dissolved and regenerated, the crystallinity of the cellulose is reduced, a large amount of free hydroxyl is released, and the liquid absorption capacity of the cellulose is further improved; secondly, by physical blending, the gelatin and the diatomite are introduced into a cellulose system, imino and siloxy can be introduced into the gel system, and the hemostatic performance of the aerogel is further improved. Finally, the cellulose and the gelatin are renewable and degradable natural polymer materials, have excellent biocompatibility and degradability, and are real high-quality environment-friendly hemostatic materials.
2. The invention uses the chloridized-1-butyl-3-methylimidazole ionic liquid as a dissolving system, and uses cellulose as a raw material to prepare the porous cellulose/gelatin composite hemostatic aerogel material, thereby simplifying the preparation process of the cellulose-based hemostatic material, and the obtained product has excellent performance and does not need the investment of special equipment, and the ionic liquid can be recycled and treated for repeated use, thereby having the advantages of environmental protection and no pollution.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) picture of a porous cellulose/gelatin composite hemostatic aerogel material prepared according to example 1 of the present invention;
FIG. 2 is a diagram illustrating rapid coagulation of blood under the effect of the porous cellulose/gelatin composite hemostatic aerogel material prepared in example 1 of the present invention;
FIG. 3 is a graph showing the adhesion and coagulation of erythrocytes in the gaps of the porous cellulose/gelatin composite hemostatic aerogel material prepared in example 1 of the present invention.
Detailed Description
The porous cellulose/gelatin composite hemostatic aerogel prepared by the invention is prepared by compounding I-type gelatin, microcrystalline cellulose and diatomite; firstly, adding quantitative microcrystalline cellulose, gelatin and diatomite into an ionic liquid solvent, uniformly stirring, then placing the mixed solution into an oil bath pot for heating treatment, dripping the obtained solution into deionized water by using an injector, and replacing the solution with the deionized water for multiple times until AgNO is dripped 3 The solution generates no white precipitate, and finally, the porous cellulose/gelatin composite hemostatic aerogel can be obtained by freeze drying without pre-freezing. The aerogel material has the aperture of 6-20 mu m, has abundant internal pore structures, can quickly absorb water in blood, concentrates the blood, quickly activates a blood coagulation mechanism, and thus obviously improves the hemostasis speed. The introduction of amino, imino and siloxy can quickly adsorb charged components in blood, so that platelets in the blood at a bleeding part can be quickly adhered and aggregated to form thrombus, red blood cells are aggregated to play a role in stabilizing blood clots, and the effect of quickly stopping bleeding is finally achieved. The hemostatic material prepared by the method can be directly used for bleeding wounds, has quick hemostasis and good effect, and has a certain adhesive plugging effect. The preparation method is simple, low in process requirement, low in energy consumption and easy for large-scale industrial production.
In order that the above objects, features and advantages of the present invention may be more clearly understood, the present invention will be further described with reference to specific embodiments. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflict.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced otherwise than as specifically described herein and, therefore, the present invention is not limited to the specific embodiments disclosed in the following description.
The equipment and raw materials used in the present invention are commercially available or commonly used in the art. The methods in the following examples are conventional in the art unless otherwise specified.
Type I gelatin used in the following examples of the invention was purchased from mcelin, CAS number: 9000-70-8, biotech grade; the microcrystalline cellulose is obtained from Anhui mountain river pharmaceutic adjuvant corporation, product model SH-102; the diatomite is purchased from Zhengzhou Mingzhu Uzhu Utility and marketing department and is food grade.
Example 1
The embodiment provides a preparation method of a porous cellulose/gelatin composite hemostatic aerogel material, which comprises the following specific steps:
(1) Pretreatment: vacuum drying microcrystalline cellulose and diatomaceous earth at 45 deg.C for 24 hr; crushing the type I gelatin to obtain gelatin powder with the size of 60-200 meshes;
(2) Mixing treatment: carrying out dehydration and melting treatment on 1-butyl-3-methylimidazole chloride, and then adding vacuum-dried microcrystalline cellulose, kieselguhr and gelatin (the mass ratio of the microcrystalline cellulose to the gelatin to the kieselguhr is =4: 1) into a solvent to obtain a mixed solution, wherein the total mass fraction of the microcrystalline cellulose, the gelatin and the kieselguhr in the mixed solution is 5%;
(3) And (3) heat treatment: placing the mixed solution obtained by mixing treatment in the step (2) in a heat preservation device at 80 ℃, and carrying out water isolation treatment for 120min at the stirring speed of 300 rpm;
(4) And (3) regeneration reaction: dropping the mixed solution obtained after the heat treatment in the step (3) into deionized water by using an injector, wherein the water temperature is 25 ℃, the temperature of the mixed solution is 80 ℃, the dropping height is 10cm, the dropping speed is 10mL/min, and washing out the ionic liquid in the mixed solution by using the principle of an anti-solvent to obtain a cellulose composite hydrogel sphere;
(5) Fully cleaning: replacing with purified water for 6 times, each time for 2h, to obtain pure cellulose composite hydrogel spheres;
(6) And (3) freeze drying: carrying out vacuum freeze drying on the pure cellulose hydrogel at the temperature of-55 ℃ for 24 hours to obtain a final product, namely the porous cellulose/gelatin composite hemostatic aerogel material;
(7) And (3) recovering the ionic liquid: filtering and removing impurities from a mixed solution of ionic liquid and water, putting the mixed solution into a rotary evaporator, setting the temperature at 80 ℃ and the rotating speed at 120rpm until no liquid drops drop in a condensation reflux device, taking out the obtained ionic liquid, cooling to room temperature, and transferring the ionic liquid into a conical flask for recycling.
The porous cellulose/gelatin composite hemostatic aerogel material prepared in this embodiment utilizes an anti-solvent method to perform a regeneration reaction on dissolved cellulose and gelatin molecules, so that the dissolved cellulose and gelatin molecules have rich pore structures and are uniformly distributed, and a three-dimensional network structure (as shown in fig. 1) is formed. The three-dimensional network pore structure can absorb a large amount of liquid, and the maximum adsorption capacity can reach 24 times of the self weight. Finally, the ionic liquid used in the embodiment can be recycled, and the used hemostatic aerogel material can be completely and naturally degraded in the natural environment and cannot generate any pollutant after being sterilized.
Example 2
The embodiment provides a preparation method of a porous cellulose/gelatin composite hemostatic aerogel material, which comprises the following specific steps:
(1) Pretreatment: drying microcrystalline cellulose and diatomite at 120 deg.C for 6 hr; crushing the type I gelatin to obtain gelatin powder with the size of 60-200 meshes;
(2) Mixing treatment: drying the chlorinated-1-butyl-3-methylimidazole, and then adding the microcrystalline cellulose, the kieselguhr and the gelatin (the mass ratio of the microcrystalline cellulose to the gelatin to the kieselguhr is 7: 1) which are subjected to vacuum drying into a solvent to obtain a mixed solution, wherein the total mass fraction of the microcrystalline cellulose, the gelatin and the kieselguhr in the mixed solution is 8%;
(3) And (3) heat treatment: placing the mixed solution obtained by mixing treatment in the step (2) in a heat preservation device at 120 ℃, insulating water for treatment for 20min, and stirring at 480rpm;
(4) And (3) regeneration reaction: dripping the cellulose solution obtained after the heat treatment in the step (3) into deionized water by using a falling ball method, wherein the water temperature is 25 ℃, the temperature of the cellulose solution is 120 ℃, the dripping height is 10cm, the dripping speed is 5mL/min, and washing out the ionic liquid in the mixed solution by using the principle of an anti-solvent to obtain cellulose composite hydrogel balls;
(5) And (3) fully cleaning: replacing with purified water for 6 times, each time for 2 hr, to obtain pure cellulose composite hydrogel spheres;
(6) And (3) freeze drying: carrying out vacuum freeze-drying on the fully substituted cellulose hydrogel spheres at the temperature of minus 40 ℃ for 24 hours to obtain a final product, namely the porous cellulose/gelatin composite hemostatic aerogel material;
(7) And (3) recovering the ionic liquid: filtering and removing impurities from a mixed solution of ionic liquid and water, transferring the mixed solution into a rotary evaporator, setting the temperature at 85 ℃ and the rotating speed at 120rpm until no liquid drops drop in a condensation reflux device, taking out the obtained ionic liquid, cooling to room temperature, and transferring the ionic liquid into a conical flask for recycling.
The porous cellulose/gelatin composite hemostatic aerogel material prepared by the embodiment can be dissolved in ionic liquid only in a short time at a high temperature, and the obtained porous cellulose/gelatin composite hemostatic aerogel material has rich pore structures and uniform pore structure distribution, forms a three-dimensional network pore structure, can quickly absorb liquid, and has a maximum adsorption capacity of 16.5 times. The ionic liquid used in the embodiment can be recycled, and the hemostatic aerogel material can be completely and naturally degraded in the natural environment and cannot generate any pollutant after being sterilized.
Example 3
The embodiment provides a preparation method of a porous cellulose/gelatin composite hemostatic aerogel material, which comprises the following specific steps:
(1) Pretreatment: drying microcrystalline cellulose and diatomite at 80 deg.C for 12 hr; crushing the type I gelatin to obtain gelatin powder with the size of 60-200 meshes;
(2) Mixing treatment: carrying out dehydration and melting treatment on 1-butyl-3-methylimidazole chloride, and then adding dried microcrystalline cellulose, kieselguhr and gelatin (the mass ratio of the microcrystalline cellulose to the gelatin to the kieselguhr is 4: 1) into a solvent to obtain a mixed solution, wherein the total mass fraction of the microcrystalline cellulose, the gelatin and the kieselguhr in the mixed solution is 7%;
(3) And (3) heat treatment: placing the mixed solution obtained by mixing treatment in the step (2) in a heat preservation device at 100 ℃, insulating water for treatment for 60min, and stirring at 600rpm;
(4) And (3) regeneration reaction: dripping the cellulose solution obtained after the heat treatment in the step (3) into deionized water by using a falling ball method, wherein the water temperature is 25 ℃, the temperature of the cellulose solution is 100 ℃, the dripping height is 10cm, the dripping speed is 8mL/min, and the ionic liquid in the mixed solution is washed out by using the principle of an anti-solvent to obtain cellulose composite hydrogel balls;
(5) Fully cleaning: replacing with purified water for 6 times, each time for 2 hr, to obtain pure cellulose composite hydrogel spheres;
(6) And (3) freeze drying: carrying out vacuum freeze-drying on the pure cellulose composite hydrogel spheres at the temperature of minus 45 ℃ for 24 hours to obtain a final product, namely a porous cellulose/gelatin composite hemostatic aerogel material;
(7) And (3) recovering the ionic liquid: filtering and removing impurities from a mixed solution of ionic liquid and water, transferring the mixed solution into a rotary evaporator, setting the temperature at 85 ℃ and the rotating speed at 120rpm until no liquid drops drop in a condensation reflux device, taking out the obtained ionic liquid, cooling to room temperature, and transferring the ionic liquid into a conical flask for recycling.
According to the porous cellulose/gelatin composite hemostatic aerogel material prepared by the embodiment, the heat treatment time is increased along with the increase of the content of cellulose, the size of the pore structure of the prepared porous cellulose/gelatin composite hemostatic aerogel material is slightly reduced compared with that of 5%, but the pore structure distribution is still uniform, a three-dimensional network pore structure is formed, liquid can be well absorbed, and the maximum equilibrium adsorption capacity reaches 19.4 times. The ionic liquid used in the embodiment can be recycled, and the hemostatic aerogel material after being used can be completely and naturally degraded in the natural environment without generating any pollutant after being sterilized.
Example 4
The embodiment provides a preparation method of a porous cellulose/gelatin composite hemostatic aerogel material, which comprises the following specific steps:
(1) Pretreatment: drying microcrystalline cellulose and diatomite at 45 deg.C for 18 hr; crushing the type I gelatin to obtain gelatin powder with the size of 60-200 meshes;
(2) Mixing treatment: drying the 1-butyl-3-methylimidazole chloride, adding dried microcrystalline cellulose, kieselguhr and gelatin (the mass ratio of the microcrystalline cellulose to the gelatin to the kieselguhr is 3;
(3) And (3) heat treatment: placing the mixed solution obtained after the mixing treatment in the step (2) in a heat preservation device at 90 ℃, insulating water for treatment for 80min, and stirring at 480rpm;
(4) And (3) regeneration reaction: dripping the cellulose solution obtained after the heat treatment in the step (3) into deionized water by using a falling ball method, wherein the water temperature is 20 ℃, the temperature of the cellulose solution is 90 ℃, the dripping height is 15cm, the dripping speed is 4mL/min, and eluting ionic liquid in the mixed solution by using the principle of an anti-solvent to obtain cellulose composite hydrogel balls;
(5) Fully cleaning: replacing with purified water for 6 times, each time for 2h, to obtain pure cellulose composite hydrogel spheres;
(6) And (3) freeze drying: carrying out vacuum freeze-drying on the fully substituted cellulose hydrogel spheres at the temperature of minus 50 ℃ for 24 hours to obtain a final product, namely the porous cellulose/gelatin composite hemostatic aerogel material;
(7) And (3) recovering the ionic liquid: filtering and removing impurities from a mixed solution of ionic liquid and water, transferring the mixed solution into a rotary evaporator, setting the temperature at 80 ℃ and the rotating speed at 120rpm until no liquid drops drop in a condensation reflux device, taking out the obtained ionic liquid, cooling to room temperature, and transferring the ionic liquid into a conical flask for recycling.
The porous cellulose/gelatin composite hemostatic aerogel material prepared by the embodiment has the advantages that the heat treatment time is prolonged along with the reduction of the heat treatment temperature, the internal pores of the prepared porous cellulose/gelatin composite hemostatic aerogel material are improved, the pore structure is uniformly distributed, a three-dimensional network pore structure is formed, and the liquid absorption capacity is improved to a certain extent and reaches 22.5 times. The ionic liquid used in the embodiment can be recycled, and the hemostatic aerogel material can be completely and naturally degraded in the natural environment and cannot generate any pollutant after being sterilized.
Example 5
The embodiment provides a preparation method of a porous cellulose/gelatin composite hemostatic aerogel material, which comprises the following specific steps:
(1) Pretreatment: drying microcrystalline cellulose and diatomite at 60 deg.C for 24 hr; crushing the type I gelatin to obtain gelatin powder with the size of 60-200 meshes;
(2) And (3) recovering and reusing the solution: taking the ionic liquid recovered in the examples 1-4 as a solvent;
(3) Mixing treatment: drying the recycled 1-butyl-3-methylimidazole chloride, and then adding the dried microcrystalline cellulose, kieselguhr and gelatin (the mass ratio of the cellulose to the gelatin to the kieselguhr is 3;
(4) And (3) heat treatment: placing the mixed solution obtained after the mixing treatment in the step (2) in a heat preservation device at 100 ℃, insulating water for treatment for 80min, and stirring at 480rpm;
(5) And (3) regeneration reaction: dropping the cellulose composite solution obtained after the heat treatment in the step (4) into purified water by using a ball dropping method, wherein the water temperature is 25 ℃, the temperature of the cellulose solution is 100 ℃, the dropping height is 15cm, the dropping speed is 5mL/min, and eluting ionic liquid in the mixed solution by using the principle of an anti-solvent to obtain cellulose composite hydrogel balls;
(6) And (3) fully cleaning: replacing with purified water for 6 times, each time for 2h, to obtain pure cellulose composite hydrogel spheres;
(7) And (3) freeze drying: carrying out vacuum freeze-drying on the fully substituted cellulose composite hydrogel at the temperature of minus 65 ℃ for 24 hours to obtain a final product, namely a porous cellulose/gelatin composite hemostatic aerogel material;
(8) And (3) recovering the ionic liquid: filtering and removing impurities from a mixed solution of ionic liquid and water, transferring the mixed solution into a rotary evaporator, setting the temperature at 80 ℃ and the rotating speed at 120rpm until no liquid drops drop in a condensation reflux device, taking out the obtained ionic liquid, cooling to room temperature, and transferring the ionic liquid into a conical flask for recycling.
The porous cellulose/gelatin composite hemostatic aerogel material prepared by using the recovered ionic liquid can be obtained according to experimental results, and the recovered ionic liquid has no influence on cellulose dissolution, and can dissolve cellulose in a short time. And the prepared porous cellulose/gelatin composite hemostatic aerogel material still has rich pore structures formed inside, uniform structural distribution and rich pore diameter structures, and has various pore diameter structures of 6-20 mu m, wherein the large pores are favorable for absorbing plasma, and the small pores can realize the blocking and grading of blood cells, are favorable for forming thrombus clot and improve the hemostatic effect. In addition, the liquid absorption capacity of the three-dimensional network pore structure formed by the aerogel material is consistent with the quality of a product prepared by common ionic liquid, reaches 18.7 times, and can absorb moisture in blood in time to achieve the purposes of concentrating blood and stopping bleeding quickly.
Claims (10)
1. A preparation method of porous cellulose/gelatin composite hemostatic aerogel is characterized by comprising the following steps: the method specifically comprises the following steps:
(1) Pretreatment: drying microcrystalline cellulose and diatomite; crushing gelatin to obtain gelatin powder;
(2) Mixing treatment: adding the dried microcrystalline cellulose prepared in the step (1), diatomite and gelatin powder into ionic liquid serving as a solvent, and uniformly mixing to obtain a mixed solution a;
(3) And (3) heat treatment: stirring and heating the mixed solution a in the step (2) to obtain a cellulose composite solution b;
(4) And (3) regeneration reaction: dripping the cellulose composite solution b prepared in the step (3) into water by a ball dropping method to prepare a composite cellulose hydrogel ball c;
(5) Cleaning: washing residual solvent in the composite cellulose hydrogel ball c prepared in the step (4) by using deionized water to obtain a composite cellulose hydrogel ball d;
(6) And (3) freeze drying: and (4) freezing and drying the composite cellulose hydrogel spheres d prepared in the step (5) to obtain the porous cellulose/gelatin composite hemostatic aerogel.
2. The method of claim 1, wherein: the total mass fraction of the microcrystalline cellulose, the gelatin and the diatomite added in the step (2) in the mixed solution a is 3-8%.
3. The method of claim 1, wherein: the mass ratio of the microcrystalline cellulose, the gelatin and the diatomite added in the step (2) is (3-7): (1-2): 1.
4. the method of claim 1, wherein: in the step (3), the heating temperature is 80-120 ℃, the stirring speed is 300-800rpm, and the stirring and heating time is 20-120min.
5. The method of claim 1, wherein: the washing step in the step (5) is specifically as follows: deionized water is used for replacing for 4-8 times, and each time lasts for 1-3 hours.
6. The method of claim 1, wherein: the method also comprises a step of recovering the ionic liquid, and the specific operations are as follows: and filtering the residual solvent to remove impurities, and performing rotary evaporation to recover the ionic liquid.
7. The method of claim 1, wherein: the ionic liquid or a part of the ionic liquid in the step (2) is the ionic liquid recovered by the method of claim 6.
8. A porous cellulose/gelatin composite hemostatic aerogel prepared by the method of any one of claims 1-7.
9. Use of the porous cellulose/gelatin composite hemostatic aerogel prepared by the method of any one of claims 1-7 as a rapid hemostatic material.
10. A rapid hemostatic material, comprising: the porous cellulose/gelatin composite hemostatic aerogel prepared by the method of any one of claims 1-7.
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