Polysaccharide-based hemostatic sponge material for rapid hemostasis of deep wound cavity and preparation method of polysaccharide-based hemostatic sponge material

Abstract

The invention provides a polysaccharide-based hemostatic sponge material for rapid hemostasis of a deep wound cavity and a preparation method of the polysaccharide-based hemostatic sponge material. The problems that a hemostatic porous material prepared in the prior art is difficult to expand rapidly, poor in hydrophilicity, low in shape recovery rate, large in pores, uneven in pores, low in elastic modulus, poor in compression cycle performance and the like are solved. According to the preparation method, natural polysaccharide is adopted as a raw material, and the porous material which can absorb liquid and expand quickly, and is high in hydrophilicity, good in biocompatibility, high in shape recovery rate, small and uniform in pores, high in elasticity modulus and good in compression cycle performance is prepared through the aging salting-out method and the processes of alkalization, esterification, mixing, aging and forming.

Description

Technical Field

[0001] This invention belongs to the field of hemostatic material research and development technology, specifically relating to a polysaccharide-based hemostatic sponge material for rapid hemostasis in deep wound cavities and its preparation method. This material can cope with bleeding in deep wound cavities and can expand ultra-rapidly to stop bleeding. Background Technology

[0002] In traumatic injuries, bleeding is one of the leading causes of death, with bleeding from deep wound cavities being particularly dangerous. This type of bleeding often occurs in the trunk, major blood vessels, or internal organs. Due to the unique anatomical structure and vascular distribution, traditional tourniquets and other hemostatic methods are often ineffective. Timely bleeding control is crucial in emergency care and trauma treatment. Statistics show that most traumatic deaths occur within the first hour after injury, making the development of rapid and effective hemostatic materials a key research focus in emergency medicine.

[0003] Currently, commonly used hemostatic materials in clinical practice mainly include powders, gauze, hydrogels, and sponges. However, these traditional materials have significant limitations when dealing with deep wound bleeding: ordinary sponges and gauze are difficult to adapt to irregular features and cannot effectively reach deep bleeding sites; hemostatic powders often fail to form stable clots and easily dissolve in the blood under blood flushing, resulting in poor hemostatic effects on arterial and venous bleeding; while viscous hydrogels can form a physical barrier, they generally suffer from low biocompatibility, slow adhesion formation, and poor mechanical compatibility with tissues, especially in the blood environment, where their adhesion strength to the tissue surface is significantly reduced.

[0004] In contrast, expandable hemostatic materials exhibit unique advantages. These materials can rapidly expand at the wound site, adaptively filling wounds of various shapes and depths, promoting coagulation through physical pressure, and achieving rapid hemostasis. Currently, the raw materials used to prepare expandable hemostatic materials mainly include chitosan, sodium carboxymethyl polysaccharide, gelatin, and starch. Among them, chitosan has attracted much attention due to its excellent hemostatic properties and good biocompatibility, and is widely used in the preparation of porous hemostatic materials. However, existing chitosan-based hemostatic materials still have significant shortcomings: slow water absorption and expansion rates, poor hydrophilicity, and low shape recovery rates limit their hemostatic effects. In terms of preparation processes, current methods mainly employ phase separation, foaming, freeze-drying, and template methods to prepare porous hemostatic materials. Although these methods each have their own characteristics, the prepared porous hemostatic materials generally suffer from uneven pore size, large pore size, low elastic modulus, and poor compression cycle performance, making it difficult to achieve precise control of the pore structure, affecting the hemostatic and mechanical properties of the material, and limiting its application in deep wound cavity bleeding.

[0005] In view of the above problems, it is necessary to explore a new hemostatic porous material and its preparation method, which can be used for rapid hemostasis in deep wound cavities. Summary of the Invention

[0006] The purpose of this invention is to solve the problems of existing hemostatic porous materials, such as difficulty in achieving rapid expansion, poor hydrophilicity, low shape recovery rate, large pore size, uneven pore size, low elastic modulus, and poor compression cycle performance. The invention provides a polysaccharide-based hemostatic sponge material for rapid hemostasis of deep wound cavities and its preparation method.

[0007] To achieve the above objectives, the technical solution provided by this invention is:

[0008] A method for preparing a polysaccharide-based hemostatic sponge material, characterized by the following steps:

[0009] 1) Alkalization

[0010] The polysaccharide was soaked in an excess of alkaline solution and hydrolyzed to obtain alkalized polysaccharide;

[0011] 2) Esterification

[0012] The alkalized polysaccharide obtained in step 1) is mixed with carbon disulfide to undergo xanthation reaction, resulting in a mixture containing xanthated polysaccharide. This reaction is very easy and can be carried out in a vacuum, air or inert gas atmosphere. The reaction temperature can be any temperature between 0-50 ℃, and the entire reaction process can be stirred or not.

[0013] 3) Mixing

[0014] An inorganic salt hydrate with a salting-out effect is added to the mixture obtained in step 2) and mixed evenly to obtain a free-flowing precursor.

[0015] 4) Aging

[0016] The precursor obtained in step 3) is left to stand and age (i.e., undergo aging and salting out) until the fluidity of the precursor decreases and a gel-like substance is formed.

[0017] 5) Molding

[0018] After heating and molding the gel obtained in step 4), the polysaccharide-based hemostatic sponge material is obtained by soaking, washing, compressing and shaping, and drying.

[0019] Further, in step 1), the polysaccharide is one or more of the following: wood fiber, bamboo fiber, cotton fiber, sugarcane bagasse pulp, grass pulp, lignin, and starch.

[0020] The alkaline solution is a sodium hydroxide, potassium hydroxide, barium hydroxide, calcium hydroxide, sodium bicarbonate, or sodium carbonate solution with a mass fraction of 5%-20%.

[0021] The amount of alkaline solution used is 10-50 times the mass of the polysaccharide;

[0022] The soaking time is 0.1-24 hours.

[0023] Further, in step 1), after hydrolysis is completed, excess alkaline solution is removed by filtration to obtain alkalized polysaccharide.

[0024] Furthermore, in step 2), the amount of alkalized polysaccharide used is 2-8 times the mass of polysaccharide used in step 1);

[0025] The amount of carbon disulfide used is 0.5-10 times the mass of the alkalized polysaccharide. Excess carbon disulfide has no effect on the reaction, and excess carbon disulfide does not participate in the reaction. However, in order to reduce the amount of carbon disulfide entering subsequent steps, it is best to control its amount within this range.

[0026] The xanthan acidification reaction takes 5-72 hours.

[0027] Further, in step 3), the inorganic salt hydrate with salting-out effect is sodium sulfate hydrate, sodium citrate hydrate, potassium sulfate hydrate, cesium sulfate hydrate, cesium carbonate hydrate, sodium carbonate hydrate, or potassium carbonate hydrate.

[0028] The amount of the inorganic salt hydrate used is 2-15 times the mass of the mixture containing xanthan acidified polysaccharide.

[0029] Furthermore, in step 4), the settling and aging time is 10-80 minutes.

[0030] Furthermore, in step 5), the heating temperature is 40-98℃; the heating time is 0.5-72 hours.

[0031] The material was first soaked and cleaned with deionized water and then with ethanol. Deionized water was used first, which filled the pores of the material with water. Ethanol was then used to replace the water in the pores in order to facilitate compression and shaping and to better restore the shape after liquid absorption.

[0032] Furthermore, this invention also provides a polysaccharide-based hemostatic sponge material prepared by the above-described method, and its application in the preparation of hemostatic materials for deep wound cavity bleeding. This material has the advantages of high hydrophilicity, good cyclic compression performance, and rapid expansion after absorbing liquid (e.g., water, blood) after being compressed and fixed in shape by external force.

[0033] Based on the above applications, the present invention also provides a hemostatic medical material made of the aforementioned polysaccharide-based hemostatic sponge material, which can address deep wound cavity bleeding.

[0034] The concept and principle of this invention:

[0035] To address the technical problems existing in the prior art, this invention explores ultra-rapid expansion materials that can cope with deep wound cavity bleeding by focusing on both raw material selection and preparation process.

[0036] Natural polysaccharides possess excellent biocompatibility and environmental friendliness. As one of the most abundant organic macromolecules in nature, they are not only widely available but also exhibit excellent biodegradability, reducing the burden on the ecological environment. Furthermore, the bioinertness of polysaccharides means they do not elicit a significant immune response upon contact with human tissues, making them ideal for preparing medical materials and contributing to improved patient safety and comfort. On the other hand, polysaccharides, represented by cellulose, have the potential to undergo xanthation reactions with carbon disulfide. The resulting products are unstable and will precipitate under certain temperatures (i.e., molding heating temperatures) and the influence of inorganic salt hydrates with a salting-out effect, regenerating polysaccharides, as shown in the following formula. Therefore, this invention proposes to use natural polysaccharides as the base material for ultra-rapid expansion materials.

[0037]

[0038] Porosity is a key characteristic for ensuring the rapid liquid absorption and hemostasis capabilities of ultra-rapid expansion materials. The porous structure provides a large surface area, allowing the material to absorb large amounts of liquid in a short time and rapidly expand to fill the wound. The uniform distribution of pores is also crucial for the material's performance, ensuring consistent absorption rates and preventing uneven expansion during absorption, thus improving the reliability and effectiveness of hemostasis. A uniform pore structure also provides more stable physical support, preventing material breakage or failure during use. Therefore, in the process of converting natural polysaccharides into ultra-rapid expansion materials, the porosity and uniformity of the pore structure of the target product should be ensured through the manufacturing process.

[0039] Good mechanical properties are fundamental to ensuring the effective performance of ultra-rapid expansion materials in practical applications. After absorbing liquid and expanding, the material needs to maintain sufficient mechanical strength to resist internal and external pressures and tearing, ensuring a stable hemostatic barrier at critical moments. If the material is prone to deformation or fracture under stress, its hemostatic effect may be reduced. Therefore, optimizing the material's fiber structure and porosity characteristics can effectively improve its mechanical properties, ensuring effectiveness in various environments.

[0040] In summary, the development of ultra-rapid expansion materials for deep wound cavity bleeding should combine the superior biocompatibility and environmental friendliness of natural polysaccharides with the material's rich and uniform porous morphology, excellent mechanical properties, and liquid absorption capacity, providing a new, efficient, safe, and environmentally friendly option for controlling deep wound cavity bleeding.

[0041] Therefore, this invention proposes a liquid-absorbing, rapidly expanding porous material (i.e., polysaccharide-based hemostatic sponge material) and its preparation method for addressing deep wound bleeding. Using an aging salting-out method, polysaccharides are used as the raw material for preparing the hemostatic porous material. First, the polysaccharides are hydrolyzed and extracted in an alkaline solution to obtain alkalized polysaccharides. Next, the alkalized polysaccharides are reacted with carbon disulfide to obtain a mixture containing xanthate-modified polysaccharides. Then, the mixture containing xanthate-modified polysaccharides is mixed with an inorganic salt solution exhibiting a salting-out effect to obtain a fluid precursor. The precursor is then aged to obtain a gel. Subsequently, heating is used to form a porous material, which is then soaked, washed, compressed, shaped, and dried to finally become the liquid-absorbing, rapidly expanding porous material—the polysaccharide-based hemostatic sponge material.

[0042] The aforementioned preparation process primarily utilizes the aging salting-out method, where a polymer solution is blended with salt hydrates. The Hofmeister effect is used to regulate the aggregation of hydrophilic polymer chains at the molecular level, thereby producing porous materials with excellent mechanical properties to meet the urgent needs of this field. This is entirely different from previous research findings on the ion-specific effects of hydrophilic polymers. Different salts exhibit varying abilities to precipitate proteins from aqueous solutions; this is known as the Hofmeister effect or ion-specific effect. Previous studies have shown that the ion-specific effect arises from the influence of different ions on the hydration of water surrounding hydrophilic functional groups on hydrophobic chains. For natural macromolecules, numerous researchers have investigated the effects of different ions on polymer solubility and swelling under this effect. A few studies have reported methods to improve the mechanical properties of hydrogels by immersing them in salt solutions after synthesis. However, no research has yet demonstrated the influence of ions on the mechanical properties of porous materials prepared from hydrogels or on the molding process of porous materials.

[0043] The beneficial effects of this invention are as follows:

[0044] 1. This invention relates to a method for preparing high-performance polysaccharide-based hemostatic sponge materials based on the aging and salting-out method. This method, through alkalization, esterification, mixing, aging, and molding processes, successfully prepares polysaccharide-based hemostatic sponge materials with rapid liquid absorption and expansion, high hydrophilicity, excellent biocompatibility, high shape recovery rate, small and uniform pores, high elastic modulus, and good compression cycle performance.

[0045] 2. This invention achieves precise control over the microstructure of the material by introducing a room-temperature aging salting-out process to regulate the flowability and molecular aggregation behavior of the precursor. During the aging salting-out process, the high-concentration salt solution disrupts the hydration layer on the surface of the polar molecular chains, promoting molecular chain aggregation and crystallization to form a stable gel network structure. This process not only significantly improves the mechanical properties of the material but also effectively avoids large-sized pores caused by rapid water evaporation during the heating and molding process by reducing the flowability of the precursor. The final product is a hemostatic porous material with advantages such as uniform and fine pore structure, high elastic modulus, excellent compression cycle performance, fast liquid absorption expansion rate, and high shape recovery rate. These characteristics enable the material to better adapt to irregular wound morphologies, quickly fill deep wound cavities, and achieve effective hemostasis.

[0046] 3. The material prepared by this invention also exhibits good biocompatibility and degradation performance, which can meet the safety requirements for clinical use; by adjusting the aging and salting-out process parameters, the pore structure and mechanical properties of the material can be controlled; this method has the advantages of simple process, low cost and easy large-scale production, providing a new technical approach for the development of a new generation of high-efficiency hemostatic materials. Attached Figure Description

[0047] Figure 1 The images show SEM images of cross-sections of the polysaccharide-based hemostatic sponge materials prepared in Example 1 with aging and salting-out times of 0 minutes and 20 minutes, respectively; a and b are SEM images of the material with an aging and salting-out time of 0 minutes, and c and d are SEM images of the material with an aging and salting-out time of 20 minutes.

[0048] Figure 2 The compressive stress-strain relationship diagram (a) and compressive modulus diagram (b) of polysaccharide-based hemostatic sponge materials prepared for salting out at times of 0, 10, 20, 40 and 80 minutes are shown.

[0049] Figure 3 Images of cross-sections of polysaccharide-based hemostatic sponge materials prepared with salting-out times of 0 and 20 minutes.

[0050] Figure 4 The diagram and digital photograph show the cyclic compression stress-strain relationship of the polysaccharide-based hemostatic sponge material prepared in Example 3.

[0051] Figure 5 The diagram shows the cyclic compression modulus of the polysaccharide-based hemostatic sponge material prepared in Example 3.

[0052] Figure 6 The graph shows the relationship between the deformation recovery rate and water absorption rate of the polysaccharide-based hemostatic sponge material prepared in Example 4 and the change with compressive strain.

[0053] Figure 7This is a graph showing the relationship between the deformation recovery rate of the polysaccharide-based hemostatic sponge material prepared in Example 4 and the number of cycles.

[0054] Figure 8 The results of hemolysis and cytotoxicity experiments of the polysaccharide-based hemostatic sponge material prepared in Example 6 are shown. Detailed Implementation

[0055] The present invention will be further described below with reference to specific embodiments. Unless otherwise specified, the experimental methods used in the following embodiments are conventional methods. Unless otherwise specified, the materials, reagents, methods, and instruments used are all conventional materials, reagents, methods, and instruments in the art, and can be obtained commercially by those skilled in the art.

[0056] Example 1:

[0057] A method for preparing a polysaccharide-based hemostatic sponge material is as follows:

[0058] 1) Weigh 3g of lignin into a 250 mL glass beaker, add 90 mL of 20% sodium hydroxide solution, mix well and soak for 2 hours to obtain an alkalized polysaccharide mixture containing excess alkali solution. Filter the mixture to remove excess sodium hydroxide solution to obtain 12g of alkalized polysaccharide.

[0059] 2) Add 16 g of carbon disulfide to the alkalized polysaccharide and react at 25°C for 36 hours to obtain a mixture containing xanthate-modified polysaccharide.

[0060] 3) Mix the mixture containing xanthan acidified polysaccharide with sodium sulfate decahydrate at a mass ratio of 1:10 and let it stand at room temperature for 20 minutes to obtain a gel.

[0061] 4) After heating the gel at 90°C for 24 hours to form it, soak it in deionized water for 24 hours to wash away excess sodium sulfate and byproducts. Then soak it in ethanol for a period of time to displace the water. Finally, compress and dry it at 60°C to obtain polysaccharide-based hemostatic sponge material.

[0062] Comparative Example 1

[0063] The difference from Example 1 is as follows:

[0064] Step 3) After mixing the mixture containing xanthan acidified polysaccharide with sodium sulfate decahydrate at a mass ratio of 1:10, proceed directly to Step 4), i.e., the aging and salting-out time is 0 minutes.

[0065] The present invention compares the products obtained in Example 1 and Comparative Example 1:

[0066] Figure 1SEM images of cross-sections of polysaccharide-based hemostatic sponge materials (also known as porous materials) prepared with aging and salting-out times of 0 minutes (a, b) and 20 minutes (c, d). Figure 1 It can be seen that the SEM cross-section of the porous material with an aging salting-out time of 0 minutes (a, b) shows a porous morphology, and the fibers that make up the pores are arranged in a uniform and non-oriented manner. However, the SEM cross-section of the porous material with an aging salting-out time of 20 minutes (c, d) shows an oriented arrangement. This may be because during the salting-out process, the high concentration of sodium sulfate, under the Hofmeister effect, causes the bound water on the surface of the hydrophilic polysaccharide to become free water, and the hydrophilic polysaccharide further aggregates and becomes oriented.

[0067] Meanwhile, the present invention also conducted the same examples as Example 1, except that the settling time (i.e., aging and salting-out time) in step 3) was 10, 40 and 80 minutes respectively, and was compared with Example 1 and Comparative Example 1. Figure 2 The figures (a) and (b) show the compressive stress-strain relationship and compressive modulus of the polysaccharide-based hemostatic sponge materials prepared with salting-out times of 0, 10, 20, 40, and 80 minutes, respectively. It can be seen that the compressive modulus of the polysaccharide-based hemostatic sponge materials first increases and then decreases with increasing salting-out time. The maximum compressive modulus is 14.07 kPa for the porous material prepared with a salting-out time of 20 minutes, which is 3.27 times that of the material prepared with a salting-out time of 0 minutes (4.3 kPa). This is mainly attributed to the aggregation of fibers during the salting-out process, resulting in orientation. With further extension of the salting-out time, the compressive modulus of the polysaccharide-based hemostatic sponge materials decreases, which may be due to premature precipitation of xanthate esters caused by excessively long salting-out times.

[0068] Figure 3 Images of the cross-sections of porous materials prepared with salting-out times of 0 and 20 minutes are shown. The left side is the cross-section image of the product of Comparative Example 1, and the right side is the cross-section image of the product of Example 1. It can be seen that the internal pores of the porous material with an aging salting-out time of 20 minutes are significantly smaller than those of the porous material with an aging salting-out time of 0 minutes.

[0069] Example 2:

[0070] A method for preparing a polysaccharide-based hemostatic sponge material is as follows:

[0071] 1) Weigh 3g of bamboo fiber into a 250 mL glass beaker, add 30 mL of 20% sodium bicarbonate solution, mix well and soak for 10 hours to obtain an alkalized polysaccharide mixture containing excess alkali solution. Filter the mixture to remove excess sodium hydroxide solution to obtain 12g of alkalized polysaccharide.

[0072] 2) Add 6g of carbon disulfide to the alkalized polysaccharide and react at 25°C for 36 hours to obtain a mixture containing xanthate-modified polysaccharide.

[0073] 3) Mix the mixture containing xanthan acidified polysaccharide with sodium sulfate decahydrate at a mass ratio of 1:5 and let it stand at room temperature for 20 minutes to obtain a gel.

[0074] 4) After heating the gel at 40°C for 72 hours to form it, it was soaked in deionized water for 24 hours to remove excess sodium sulfate and byproducts. Then it was soaked in ethanol for a period of time to displace the water. Finally, it was compressed and dried at 60°C to obtain polysaccharide-based hemostatic sponge material.

[0075] Example 3:

[0076] A method for preparing a polysaccharide-based hemostatic sponge material is as follows:

[0077] 1) Weigh 3g of wood fiber into a 250 mL glass beaker, add 150 mL of 10% sodium hydroxide solution, mix well and soak for 24 hours to obtain an alkalized polysaccharide mixture containing excess alkali solution. Filter the mixture to remove excess sodium hydroxide solution to obtain 48g of alkalized polysaccharide.

[0078] 2) Add 48g of carbon disulfide to the alkalized polysaccharide and react at 25°C for 36 hours to obtain a mixture containing xanthan acidified polysaccharide.

[0079] 3) Mix the mixture containing xanthan acidified polysaccharide with sodium sulfate decahydrate at a mass ratio of 1:8 and let it stand at room temperature for 20 minutes to obtain a gel.

[0080] 4) The gel was heated at 98°C for 0.5 hours to form a gel, then soaked in deionized water for 48 hours to remove excess sodium sulfate and byproducts. Afterward, it was soaked in ethanol for a period of time to displace the water. Finally, it was compressed and dried at 60°C to obtain the polysaccharide-based hemostatic sponge material.

[0081] Figure 4These are cyclic compression stress-strain diagrams and digital photographs of the polysaccharide-based hemostatic sponge material prepared in Example 3. It can be seen that the stress-strain curve of the porous material during compression after liquid absorption can be roughly divided into two stages. The first stage is the strain range of 0-70%. In this stage, the stress of the porous material during compression exhibits a roughly linear change with strain. This is due to the relatively uniform pores within the porous material during compression and folding. As the compression deformation further deepens to over 80%, the stress of the porous material still exhibits a linear change with strain, but the modulus significantly increases. This may be because, in addition to the larger pores, there are also smaller pores and capillaries within the porous material. Furthermore, after 10 cycles, the stress-strain curves of the porous material essentially overlap, indicating that the porous material prepared in this invention has good compressive cyclic properties. Figure 5 The graph shows the cyclic compression modulus of the polysaccharide-based hemostatic sponge material prepared in Example 3. It can be seen that the compression modulus of the porous material does not decrease significantly during the cyclic process, which further proves the good compression cyclic performance of the porous material.

[0082] Example 4:

[0083] A method for preparing a polysaccharide-based hemostatic sponge material is as follows:

[0084] 1) Weigh 3g of starch into a 250 mL glass beaker, add 60 mL of 20% sodium hydroxide solution, mix well and soak for 0.1 hours to obtain an alkalized polysaccharide mixture containing excess alkali solution. Filter the mixture to remove excess sodium hydroxide solution to obtain 12g of alkalized polysaccharide.

[0085] 2) Add 12g of carbon disulfide to the alkalized polysaccharide and react at 25°C for 5 hours to obtain a mixture containing xanthan acidified polysaccharide.

[0086] 3) Mix the mixture containing xanthan acidified polysaccharide with sodium sulfate decahydrate at a mass ratio of 1:15 and let it stand at room temperature for 20 minutes to obtain a gel.

[0087] 4) After heating the gel at 60°C for 48 hours to form it, it was soaked in deionized water for 24 hours to remove excess sodium sulfate and byproducts. Then it was soaked in ethanol for a period of time to displace the water. Finally, it was compressed and dried at 60°C to obtain polysaccharide-based hemostatic sponge material.

[0088] The water absorption content of polysaccharide-based hemostatic sponge material upon swelling in deionized water was tested. Compressed polysaccharide-based hemostatic sponge material (m0) was placed in deionized water at room temperature for 20 minutes. The polysaccharide-based hemostatic sponge material was then held with tweezers and left in the air for 1 minute to remove excess liquid adhering to its surface, and then weighed (m0).w The water absorption rate (WR) is calculated using the following formula, and the results are shown in [the table below]. Figure 6 .

[0089]

[0090] The shape recovery properties of porous materials were measured to evaluate their shape memory ability. The original length of the prepared cylindrical porous material (approximately 10 mm in diameter) was L1, and the height after compression was set as L2. After immersing it in deionized water for 30 seconds, the height of the porous material was measured as L3. The expansion rate of the porous material was calculated using the following formula, and the results are shown in [Figure number missing]. Figure 6 .

[0091]

[0092] It can be seen that below 80% compressive strain, porous materials exhibit extremely high strain recovery rates (approaching 100%). However, when the strain exceeds 80%, the strain recovery rate decreases rapidly. This may be because under higher strains, the microporous structure of the porous material is compressed or even destroyed, resulting in plastic deformation. Furthermore, below 80% compressive strain, porous materials exhibit extremely high water absorption rates (all exceeding 1650%), due to their porous structure and high hydrophilicity.

[0093] Figure 7 The graph shows the relationship between the deformation recovery rate of the polysaccharide-based hemostatic sponge material prepared in Example 4 and the number of compression cycles. It can be seen that the deformation recovery rate of the porous material did not decrease significantly under multiple compression cycles, indicating that the prepared porous material has extremely strong shape recovery performance under compression cycles.

[0094] Example 5:

[0095] A method for preparing a polysaccharide-based hemostatic sponge material is as follows:

[0096] 1) Weigh 3g of sugarcane bagasse pulp into a 250 mL glass beaker, add 120 mL of 20% sodium hydroxide solution, mix well and soak for 12 hours to obtain an alkalized polysaccharide mixture containing excess alkali solution. Filter the mixture to remove excess sodium hydroxide solution to obtain 12g of alkalized polysaccharide.

[0097] 2) Add 20g of carbon disulfide to the alkalized polysaccharide and react at 25°C for 36 hours to obtain a mixture containing xanthan acidified polysaccharide.

[0098] 3) Mix the mixture containing xanthan acidified polysaccharide with sodium sulfate decahydrate at a mass ratio of 1:20 and let it stand at room temperature for 20 mins to obtain a gel.

[0099] 4) After heating the gel at 72°C for 36 hours to form it, it was soaked in deionized water for 24 hours to remove excess sodium sulfate and byproducts. Then it was soaked in ethanol for a period of time to displace the water. Finally, it was compressed and dried at 60°C to obtain polysaccharide-based hemostatic sponge material.

[0100] Example 6:

[0101] A method for preparing a polysaccharide-based hemostatic sponge material is as follows:

[0102] 1) Weigh 3g of cotton fiber into a 250 mL glass beaker, add 90 mL of 20% sodium hydroxide solution, mix well and soak for 24 hours to obtain an alkalized polysaccharide mixture containing excess alkali solution. Filter the mixture to remove excess sodium hydroxide solution to obtain 12g of alkalized polysaccharide.

[0103] 2) Add 48 g of carbon disulfide to the alkalized polysaccharide and react at 25°C for 72 hours to obtain a mixture containing xanthan acidified polysaccharide.

[0104] 3) In order to obtain porous materials with different densities, the mixture containing xanthan acidified polysaccharide was mixed with sodium sulfate decahydrate at mass ratios of 1:3, 1:5, 1:7 and 1:10 respectively, and allowed to stand at room temperature for 20 minutes to obtain gels.

[0105] 4) After heating each gel at 90°C for 3 hours to form, soak it in deionized water for 24 hours to remove excess sodium sulfate and byproducts. Then soak it in ethanol for a period of time to replace the water. Finally, compress and dry it at 60°C to obtain polysaccharide-based hemostatic sponge materials of different densities.

[0106] Figure 8 The results of blood compatibility (a) and cytotoxicity experiments (b, c) of porous materials prepared by mixing xanthate-containing polysaccharides with sodium sulfate decahydrate in different ratios show that the prepared materials have a hemolysis rate of less than 5% and no cytotoxicity, indicating high safety for use.

[0107] In summary, the polysaccharide-based hemostatic sponge material prepared by this invention has high hydrophilicity, high shape recovery rate, adaptability to various wound shapes and depths, can fill irregular wounds, has the performance to deal with deep wound cavity bleeding, and can be used as a hemostatic material for deep wound cavity bleeding.

[0108] The above description is merely a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any person skilled in the art can easily conceive of various equivalent modifications or substitutions within the scope of the technology disclosed in the present invention, and such modifications or substitutions should all be covered within the scope of protection of the present invention.

Claims

1. A method for preparing a polysaccharide-based hemostatic sponge material, characterized in that, Includes the following steps: 1) Alkalization The polysaccharide was soaked in an excess of alkaline solution and hydrolyzed to obtain alkalized polysaccharide; 2) Esterification The alkalized polysaccharide obtained in step 1) is mixed with carbon disulfide to undergo xanthation reaction, resulting in a mixture containing xanthated polysaccharide; 3) Mixing An inorganic salt hydrate with a salting-out effect is added to the mixture obtained in step 2) and mixed evenly to obtain a free-flowing precursor. 4) Aging The precursor obtained in step 3) is left to stand and age until a gel is formed; 5) Molding and Compression After heating and molding the gel obtained in step 4), the polysaccharide-based hemostatic sponge material is obtained by soaking, washing, compressing and shaping, and drying.

2. The preparation method according to claim 1, characterized in that: In step 1), the polysaccharide is one or more of the following: wood fiber, bamboo fiber, cotton fiber, sugarcane bagasse pulp, grass pulp, lignin, and starch. The alkaline solution is a sodium hydroxide, potassium hydroxide, barium hydroxide, calcium hydroxide, sodium bicarbonate, or sodium carbonate solution with a mass fraction of 5%-20%. The amount of alkaline solution used is 10-50 times the mass of the polysaccharide; The soaking time is 0.1-24 hours.

3. The preparation method according to claim 1 or 2, characterized in that: In step 1), after hydrolysis is completed, excess alkali solution is removed by filtration to obtain alkalized polysaccharide.

4. The preparation method according to claim 3, characterized in that: In step 2), the amount of carbon disulfide used is 0.5-10 times the mass of the alkalized polysaccharide; The xanthan acidification reaction takes 5-72 hours.

5. The preparation method according to claim 4, characterized in that: In step 3), the inorganic salt hydrate with salting-out effect is sodium sulfate hydrate, sodium citrate hydrate, potassium sulfate hydrate, cesium sulfate hydrate, cesium carbonate hydrate, sodium carbonate hydrate, or potassium carbonate hydrate. The amount of the inorganic salt hydrate used is 2-15 times the mass of the mixture containing xanthan acidified polysaccharide.

6. The preparation method according to claim 5, characterized in that: In step 4), the settling and aging time is 10-80 minutes.

7. The preparation method according to claim 6, characterized in that: In step 5), the heating temperature is 40-98℃; the heating time is 0.5-72 hours. The samples were then soaked and cleaned in deionized water and ethanol in sequence.

8. A polysaccharide-based hemostatic sponge material, characterized in that: It is prepared by any of the preparation methods described in claims 1-7.

9. The application of the polysaccharide-based hemostatic sponge material according to claim 8 in the preparation of hemostatic materials for deep wound cavity bleeding.

10. A material for rapid hemostasis in deep wound cavities, characterized in that: Its material is the polysaccharide-based hemostatic sponge material as described in claim 8.

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