Rapid hemostatic cotton with good antibacterial property and adhesion as well as preparation method and application of rapid hemostatic cotton

Abstract

The invention relates to the technical field of hemostatic cotton, in particular to rapid hemostatic cotton with good antibacterial property and adhesion as well as a preparation method and application of the rapid hemostatic cotton. The invention discloses rapid hemostatic cotton with good antibacterial property and adhesion. The rapid hemostatic cotton is obtained by sequentially carrying out carboxymethyl treatment, tannic acid treatment and silver ion chelating treatment on cotton fabric. The rapid hemostatic cotton provided by the invention has a very high liquid absorption rate, can be rapidly gelatinized when being in contact with blood, and can be adhered to a wound, seal the wound and prevent bacteria from invading the wound, so that the purposes of rapidly stopping bleeding and promoting healing are achieved.

Description

Technical Field

[0001] The invention relates to the technical field of hemostatic cotton, and in particular to a quick hemostatic cotton with good antibacterial and adhesive properties, and a preparation method and application thereof. Background Art

[0002] Death caused by bleeding is a major global problem. According to statistics from the National Health and Family Planning Commission, about 250 million injuries occur in my country each year, and about 500,000 to 550,000 people are injured in traffic accidents, major natural disasters, etc. Excessive blood loss is the main factor leading to traumatic death. In daily life, first aid knowledge recommends pressing the wound or cut directly with a clean cloth, paper towel or gauze until the bleeding stops. However, these materials cannot quickly stop the threat of bleeding due to the lack of rapid hemostasis. According to statistics, if the heavy bleeding caused by various injury accidents can be stopped within 5 minutes, more than 60% of lives can be saved. Therefore, in pre-hospital care, rapid and thorough hemostasis is crucial to ensure the survival of patients with heavy bleeding. The ideal hemostatic material should have the properties of rapid hemostasis, ease of use, and prevention of microbial infection, but most hemostatic agents or dressings cannot achieve these parameters.

[0003] Cotton is a widely used natural wound dressing material, but pure cotton has limited hemostatic properties and generally does not have antibacterial properties and tissue adhesion. In recent years, a lot of research has been done on how to further improve the hemostatic properties of cotton, such as by compounding cotton fabrics with zeolite, chitosan and other substances to improve the hemostatic properties of cotton. The prepared cotton composite hemostatic material has significantly improved hemostatic properties, but there are also a lot of problems, such as zeolite easily generates heat and burns tissues when it comes into contact with water, and zeolite has a certain shedding rate, which can easily cause thrombosis when it falls into blood vessels; there are a large number of cationic groups in the chitosan molecular chain, which can agglutinate blood cells in the blood, activate platelet aggregation, and activate thrombin. After compounding with cotton fabrics, the purpose of rapid hemostasis can be achieved, but a certain proportion of patients are prone to allergic reactions to chitosan, thereby causing some adverse events. This situation is difficult to avoid, limiting the widespread use of chitosan in clinical practice, and the existing methods focus on improving the hemostatic effect of cotton, and the improvement of the antibacterial and adhesion properties of cotton fabrics is limited.

[0004] To this end, the present application provides a quick hemostatic cotton with good antibacterial and adhesive properties, and a preparation method and application thereof. Summary of the invention

[0005] The present application provides a rapid hemostatic cotton with good antibacterial and adhesive properties, and a preparation method and application thereof. The rapid hemostatic cotton is obtained by sequentially subjecting cotton fabric to carboxymethyl treatment, tannic acid treatment, and silver ion chelation treatment. The rapid hemostatic cotton has a high liquid absorption rate, can quickly gel when in contact with blood, and adhere to the wound, seal the wound, and prevent bacteria from invading the wound, thereby achieving the purpose of rapid hemostasis and promoting healing.

[0006] The technical solution adopted by this application to solve its technical problem is:

[0007] In the first aspect, the present application provides a quick hemostatic cotton with good antibacterial and adhesive properties, wherein the quick hemostatic cotton is a cotton fabric that has been sequentially treated with carboxymethyl, tannic acid, and silver ion chelation;

[0008] The carboxymethyl treatment process comprises the following steps: immersing the cotton fabric in an alkaline ethanol solution, reacting at 10-40° C. for 0.5-12 hours; then adding a sodium chloroacetate solution, reacting at 20-70° C. for 0.5-12 hours, to obtain a carboxymethyl cotton fabric;

[0009] The tannic acid treatment process comprises the following steps: immersing the carboxymethyl cotton fabric in a tannic acid ethanol solution to react, and obtaining a tannic acid modified cotton fabric after the reaction is completed;

[0010] The silver ion chelation treatment process comprises the following steps: immersing the tannic acid modified cotton fabric in a silver nitrate ethanol solution to react, and obtaining a quick hemostatic cotton after the reaction is completed.

[0011] In some embodiments, the alkaline ethanol solution is prepared by mixing an aqueous alkaline solution having a mass concentration of 20 to 50% and anhydrous ethanol in a volume ratio of 1:1 to 19.

[0012] In some embodiments, the mass content of sodium chloroacetate in the sodium chloroacetate solution is 5-45%.

[0013] In some embodiments, during the carboxymethyl treatment, a sodium chloroacetate solution is added, and the reaction is carried out at 20-70° C. for 0.5 to 12 hours. After the reaction is completed, a crude cotton fabric is obtained; the crude cotton fabric is immersed in an ethanol solution, and lactic acid is added for neutralization; the crude cotton fabric is taken out, and then washed three times with an ethanol solution, and after washing, it is centrifuged and dried to obtain a carboxymethyl cotton fabric.

[0014] In some embodiments, the tannic acid concentration in the tannic acid ethanol solution is 1 to 20 mg / mL.

[0015] In some embodiments, the tannic acid treatment process is to react at 15-30° C. for 0.5 to 12 hours.

[0016] In some embodiments, the silver ion chelation treatment process is to react at 15-30° C. for 0.5 to 24 hours.

[0017] In some embodiments, the concentration of silver nitrate in the silver nitrate ethanol solution is 10 to 1000 mmol / L.

[0018] In a second aspect, the present application provides a method for preparing hemostatic cotton, comprising the following steps:

[0019] 1) Carboxymethyl treatment

[0020] The cotton fabric is immersed in an alkaline ethanol solution and reacted at 10-40°C for 0.5-12 hours; then a sodium chloroacetate solution is added and reacted at 20-70°C for 0.5-12 hours to obtain a carboxymethyl cotton fabric;

[0021] 2) Tannic acid treatment

[0022] The carboxymethyl cotton fabric is immersed in a tannic acid ethanol solution to react, and after the reaction is completed, a tannic acid-modified cotton fabric is obtained;

[0023] 3) Silver ion chelation treatment

[0024] The tannic acid modified cotton fabric is immersed in a silver nitrate ethanol solution to react, and after the reaction is completed, a quick hemostatic cotton is obtained.

[0025] On the third aspect, the present application provides an application of hemostatic cotton, which is used as a hemostatic material for hemostasis.

[0026] The beneficial effects of this application are:

[0027] 1. The hemostatic cotton described in the present application is treated with carboxymethyl to improve the liquid absorption capacity of cotton fabric, and then treated with tannic acid. The tannic acid is grafted onto the cotton fabric by utilizing the hydrogen bonding between tannic acid and cotton hydroxyl groups to form a hemostatic cotton with excellent performance; tannic acid can not only promote coagulation by activating FXII coagulation factor to achieve rapid hemostasis, but also has antioxidant, antibacterial and anti-inflammatory effects, and can effectively solve the problems of infection and oxidation in the process of wound healing;

[0028] 2. In order to optimize the antibacterial ability, the present application also uses silver ion chelation treatment to form metal coordination bonds between the phenolic hydroxyl groups on the tannic acid and the silver ions, and chelate the silver ions to the cotton fabric. The silver ions can be slowly released when they come into contact with the wound surface, thereby continuously killing or inhibiting the growth of bacteria and improving the antibacterial properties of the wound;

[0029] 3. The hemostatic cotton prepared in this application solves the deficiencies of traditional hemostatic materials in hemostatic effect, antibacterial performance and adhesion performance, and provides a fast, effective and safe hemostatic solution. As a hemostatic material, the hemostatic cotton has broad application prospects in emergency medical assistance and surgical operations, and is expected to significantly reduce the mortality and complication rate caused by bleeding. DETAILED DESCRIPTION

[0030] In order to facilitate the understanding of those skilled in the art, the present invention is further described below in conjunction with embodiments, and the contents mentioned in the implementation modes are not intended to limit the present invention.

[0031] As used herein, "and / or" includes the term of any and all combinations of one or more associated listed items. The terms used herein are only used to describe specific embodiments and are not intended to limit the present invention. As used herein, the singular forms "a", "an", "an" and "the" are also intended to include the plural forms, unless the context clearly indicates otherwise. It is further understood that "including", when used in this specification, specifies the stated features, integers, steps, operations, elements and / or compositions, but does not exclude the existence or addition of one or more other features, integers, steps, operations, elements, compositions and / or combinations thereof.

[0032] Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the invention belongs. It is further understood that terms, such as defined in commonly used dictionaries, are interpreted in accordance with their meanings in the context of the relevant art and are not in an idealized or overly formal sense unless explicitly so defined herein.

[0033] The exemplary invention described herein may appropriately lack any one or more element limitations that are not specifically disclosed herein. Therefore, the terms "comprise", "include", "contain", etc. should be understood broadly and non-restrictively. In addition, the terminology used herein is used as a description, not a limitation, and it is unintentional to use these terminology expressions that do not include any equivalent characteristics, but only describe some of their characteristics, but various modifications are possible within the scope of the present invention according to the rights. Therefore, although the present invention has been specifically disclosed by preferred embodiments and optional features, the modifications disclosed herein to embody the changes of the present invention may be recorded by those skilled in the art, and such modifications and changes will be considered to be within the scope of the present invention.

[0034] In order to solve the deficiencies of traditional hemostatic materials in hemostatic effect, antibacterial performance and adhesion performance, the present application provides a rapid hemostatic cotton with good antibacterial and adhesion properties, wherein the rapid hemostatic cotton is obtained by sequentially treating cotton fabric with carboxymethyl, tannic acid and silver ion chelation;

[0035] The process of the carboxymethyl treatment is as follows: immersing the cotton fabric in an alkaline ethanol solution, reacting at 10-40° C. for 0.5-12 hours; then adding a sodium chloroacetate solution, reacting at 20-70° C. for 0.5-12 hours, to obtain a carboxymethyl cotton fabric;

[0036] The tannic acid treatment process is as follows: immersing the carboxymethyl cotton fabric in a tannic acid ethanol solution to react, and obtaining the tannic acid modified cotton fabric after the reaction is completed;

[0037] The process of the silver ion chelation treatment is to immerse the tannic acid modified cotton fabric in a silver nitrate ethanol solution to react, and obtain the rapid hemostatic cotton after the reaction is completed.

[0038] It can be understood that cotton fabric is the starting material of the quick hemostatic cotton and is made of pure cotton. For example, the cotton fabric can be any one or more of pure cotton gauze, medical absorbent cotton, and high-count cotton fabric.

[0039] Understandably, pure cotton gauze is the most common cotton fabric for medical use, with good moisture absorption and air permeability, but its hemostatic and antibacterial properties are limited in its original state; medical absorbent cotton is cotton fiber that has been degreased and is used in the medical field. It has better water absorption, but it also needs to be modified to improve its hemostatic and antibacterial properties. High-count cotton fabrics usually have a more delicate feel and better durability, and are suitable for medical products with higher material requirements.

[0040] In some embodiments, during the carboxymethyl treatment, the cotton fabric is immersed in an alkaline ethanol solution and reacted at 10-40°C for 0.5 to 12 hours; then a sodium chloroacetate solution is added and reacted at 20-70°C for 0.5 to 12 hours. After the reaction is completed, a crude cotton fabric is obtained; the crude cotton fabric is immersed in an ethanol solution, and then lactic acid is added for neutralization; the crude cotton fabric is taken out and washed three times with an ethanol solution, and after washing, it is centrifuged and dried to obtain a carboxymethyl cotton fabric.

[0041] In the present application, when the carboxymethyl treatment is carried out, the cotton fabric is first immersed in an alkaline ethanol solution for reaction, and the alkaline substance (such as sodium hydroxide and potassium hydroxide) plays a role in activating the cellulose hydroxyl groups on the cotton fabric, making it easier to react with sodium chloroacetate; the cotton fabric reacts with the sodium chloroacetate, and the chloroethyl group in the sodium chloroacetate reacts with the hydroxyl groups on the cotton fiber to form carboxymethyl cellulose; after the reaction is completed, the excess alkali is neutralized with a neutralizing agent such as lactic acid, and then the unreacted chemical substances are removed by multiple washings to obtain the carboxymethyl cotton fabric;

[0042] Through carboxymethyl treatment, the hydrophilicity of the carboxymethyl group enables the modified cotton fabric to quickly absorb and retain a large amount of liquid, thereby improving the liquid absorption capacity of the cotton fabric; the introduction of the carboxymethyl group improves the adhesion of the cotton fabric, allowing it to adhere more tightly to the wound surface and not fall off easily; this adhesion helps the hemostatic material to form a stable protective layer at the wound, further promoting hemostasis and wound healing. As an active group, the carboxymethyl group can react with other functional molecules (such as tannic acid), thereby introducing more functional groups on the cotton fabric.

[0043] Therefore, the present application uses carboxymethyl treatment to form a transparent gel after the cotton absorbs the liquid and adheres to the bleeding wound surface, blocking the ends of small blood vessels and capillaries, while increasing the adhesion of platelets and accelerating the aggregation of red blood cells, thereby achieving the purpose of rapid hemostasis.

[0044] Specifically, the alkaline ethanol solution is formed by mixing an alkaline aqueous solution with a mass concentration of 20-50% and anhydrous ethanol in a volume ratio of 1:1-19, the alkaline substance is sodium hydroxide or potassium hydroxide, for example, the mass content of the alkaline substance in the aqueous solution is 20%, and the volume ratio of the alkaline aqueous solution to the anhydrous ethanol is 1:1; or the mass content of the alkaline substance in the aqueous solution is 50%, and the volume ratio of the alkaline aqueous solution to the anhydrous ethanol is 1:19; or the mass content of the alkaline substance in the aqueous solution is 30%, and the volume ratio of the alkaline aqueous solution to the anhydrous ethanol is 1:10;

[0045] More specifically, sodium hydroxide\potassium hydroxide plays a role in activating the hydroxyl groups of cellulose during the carboxymethyl modification process, making it easier to react with sodium chloroacetate. If the content of sodium hydroxide\potassium hydroxide is low, the hydroxyl groups cannot be fully activated, resulting in poor modification effect; if the content of sodium hydroxide\potassium hydroxide is too high, the fiber structure of the cotton fabric may be destroyed and its mechanical strength may be reduced. Therefore, in the present application, by controlling the mass ratio of cotton fabric to alkaline substance to 1:0.3~3, the hydroxyl groups of cellulose can be activated.

[0046] Sodium hydroxide and potassium hydroxide are prepared into alkaline ethanol solution, and ethanol plays the role of solvent and stabilizer in the carboxymethyl modification process. The ethanol aqueous solution can dissolve the alkaline substance and make the reaction proceed in a homogeneous system.

[0047] Specifically, the mass content of sodium chloroacetate in the sodium chloroacetate solution is 5-45%, and the balance is water; the mass ratio of cotton fabric to sodium chloroacetate is 1:0.5-5.

[0048] In the present application, sodium chloroacetate is the main reagent of the carboxymethylation reaction, and its concentration directly affects the efficiency of the modification reaction and the performance of the product. When the concentration of the sodium chloroacetate solution is too low and the dosage is small, the reaction rate is slow and the modification effect is not significant; when the concentration of the sodium chloroacetate solution is too high and the dosage is too much, it may cause the reaction to be too violent, produce by-products, and even destroy the structure of the cotton fabric. Therefore, in the present application, the mass content of sodium chloroacetate in the sodium chloroacetate solution is 5-45%, and the balance is water; the mass ratio of cotton fabric to sodium chloroacetate is 1:0.5-5; for example, the mass content of sodium chloroacetate in the sodium chloroacetate solution is 5%, and the mass ratio of cotton fabric to sodium chloroacetate is 1:5; the mass content of sodium chloroacetate in the sodium chloroacetate solution is 45%, and the mass ratio of cotton fabric to sodium chloroacetate is 1:0.5.

[0049] In some embodiments, during the tannic acid treatment, the tannic acid concentration in the tannic acid ethanol solution is 1-20 mg / mL, and the tannic acid treatment process is reacted at 15-30° C. for 0.5-12 hours. The tannic acid ethanol solution is specifically prepared by using a tannic acid aqueous solution with a concentration of 100 mg / mL and anhydrous ethanol solution to prepare a tannic acid ethanol solution of corresponding concentration.

[0050] Tannic acid, as a natural dendritic water-soluble polyphenol, contains abundant phenolic hydroxyl groups in its molecular structure, which makes it highly reactive and can react with a variety of substances such as proteins, alkaloids, enzymes and metal ions. In this application, in the modification process of hemostatic cotton, the main purpose of tannic acid treatment is to significantly enhance the hemostatic performance, antibacterial performance and adhesion performance of hemostatic cotton, specifically:

[0051] ① Enhanced hemostatic properties

[0052] When tannic acid comes into contact with blood, its negatively charged properties can activate the FXII coagulation factor in the body, promote the initiation of the endogenous coagulation pathway, and thus accelerate the coagulation process. In addition, tannic acid can also promote the adhesion and aggregation of platelets, further accelerating the hemostatic effect.

[0053] ②Improve antibacterial properties

[0054] Tannic acid itself has antioxidant, antibacterial and anti-inflammatory effects, which can effectively inhibit the growth of a variety of bacteria and prevent wound infection. When tannic acid is combined with cotton fabric, these antibacterial properties will be imparted to hemostatic cotton, allowing it to stop bleeding while also providing antibacterial protection.

[0055] ③ Improve adhesion performance

[0056] The adhesion of tannic acid mainly comes from its abundant phenolic hydroxyl groups, which can form strong hydrogen bonds with wound tissue, allowing the hemostatic cotton to adhere tightly to the wound to prevent blood from flowing out. It also helps to seal the wound and reduce the risk of infection.

[0057] Specifically, in the present application, tannic acid is prepared into a tannic acid ethanol solution, which helps to improve the reaction rate and grafting effect of the reaction system.

[0058] Specifically, the concentration of tannic acid is a key factor affecting its grafting density and modification effect on cotton fabrics. In the tannic acid ethanol solution, if the concentration of tannic acid is too low, the amount of tannic acid grafted on the cotton fabric may be insufficient, and its performance cannot be fully exerted; if the concentration of tannic acid in the tannic acid ethanol solution is too high, it may cause excessive grafting or precipitation of tannic acid, which is also not conducive to the modification effect. Therefore, in the tannic acid ethanol solution, the tannic acid concentration is 1-20 mg / mL, which is beneficial to the grafting density and modification effect.

[0059] In some embodiments, the silver ion chelation treatment process is a reaction at 15-30°C for 0.5 to 24 hours, and the silver nitrate concentration in the silver nitrate ethanol solution is 10 to 1000 mmol / L; the silver nitrate ethanol solution is specifically prepared by using a silver nitrate aqueous solution and anhydrous ethanol solution with a concentration of 1000 mmol / L to prepare a silver nitrate ethanol solution of corresponding concentration.

[0060] In the present application, the silver ion chelation treatment is mainly based on the strong coordination effect between the abundant phenolic hydroxyl groups in the molecular structure of tannic acid and silver ions. Tannic acid is first grafted onto cotton fabric through a carboxymethyl modification process, and then the phenolic hydroxyl groups on the tannic acid are used to form stable metal coordination bonds with silver ions, thereby firmly chelating the silver ions to the cotton fabric.

[0061] Therefore, through the silver ion chelation treatment, the hemostatic cotton in the present application can continuously release silver ions when it contacts the wound, effectively killing or inhibiting bacteria around the wound, thereby significantly reducing the risk of infection. In addition, since the release of silver ions is slow and lasting, it can ensure that the effective antibacterial effect is maintained throughout the wound healing process.

[0062] Specifically, in the present application, by controlling the concentration of silver nitrate in the silver nitrate ethanol solution to be 10 to 1000 mmol / L, the silver ion chelation treatment is facilitated; when the concentration of silver nitrate in the silver nitrate ethanol solution is too high, although the silver ion loading can be increased, it may also cause uneven distribution of silver ions on the cotton fabric, forming agglomeration. In addition, too high a silver ion concentration may also damage the structure of the cotton fabric, affecting its physical properties and biocompatibility; if the silver nitrate concentration is too low, it may not be possible to obtain a sufficient silver ion loading, resulting in insufficient antibacterial performance.

[0063] Example 1

[0064] The preparation method of hemostatic cotton comprises the following steps:

[0065] 1) Carboxymethyl treatment

[0066] The cotton fabric is immersed in an alkaline ethanol solution and reacted at 10°C for 0.5h; then a sodium chloroacetate solution is added and reacted at 20°C for 0.5h. After the reaction is completed, a crude cotton fabric is obtained;

[0067] The crude cotton fabric is immersed in an ethanol solution with a volume concentration of 50%, and then lactic acid is added for neutralization; the crude cotton fabric is taken out and then washed three times with an ethanol solution with a volume concentration of 50%, and after washing, centrifugation is performed and drying is performed to obtain a carboxymethyl cotton fabric.

[0068] The mass content of sodium hydroxide in the alkaline ethanol solution is 1%, and the mass ratio of cotton fabric to alkaline substance is 1:0.3; the alkaline ethanol solution is prepared by mixing a sodium hydroxide aqueous solution with a mass concentration of 20% and anhydrous ethanol in a volume ratio of 1:1, and the mass ratio of cotton fabric to alkaline substance (sodium hydroxide) is 1:0.3;

[0069] The sodium chloroacetate solution is a sodium chloroacetate aqueous solution, the mass content of sodium chloroacetate in the sodium chloroacetate aqueous solution is 5%, and the sodium chloroacetate aqueous solution is added according to a mass ratio of cotton fabric to sodium chloroacetate of 1:5.

[0070] 2) Tannic acid treatment

[0071] The carboxymethyl cotton fabric is immersed in a tannic acid ethanol solution, and reacted at 15° C. for 0.5 h, and after the reaction is completed, a tannic acid-modified cotton fabric is obtained;

[0072] The concentration of tannic acid in the tannic acid ethanol solution is 1 mg / mL.

[0073] 3) Silver ion chelation treatment

[0074] The carboxymethyl cotton fabric modified by tannic acid is taken out, immersed in a silver nitrate ethanol solution, and reacted at 15°C for 0.5h. After the reaction, the obtained cotton fabric is taken out, repeatedly washed three times with a 50% ethanol solution, centrifuged and dried, and then dried to obtain a quick hemostatic cotton.

[0075] The concentration of silver nitrate in the silver nitrate ethanol solution is 10 mmol / L.

[0076] Example 2

[0077] The preparation method of hemostatic cotton comprises the following steps:

[0078] 1) Carboxymethyl treatment

[0079] The cotton fabric is immersed in an alkaline ethanol solution and reacted at 40°C for 12 hours; then a sodium chloroacetate solution is added and reacted at 70°C for 12 hours. After the reaction is completed, a crude cotton fabric is obtained;

[0080] The crude cotton fabric is immersed in an ethanol solution with a volume concentration of 50%, and then lactic acid is added for neutralization; the crude cotton fabric is taken out and then washed three times with an ethanol solution with a volume concentration of 50%, and after washing, centrifugation is performed and drying is performed to obtain a carboxymethyl cotton fabric.

[0081] The alkaline ethanol solution is prepared by mixing a sodium hydroxide aqueous solution with a mass concentration of 50% and anhydrous ethanol in a volume ratio of 1:19, and the mass ratio of cotton fabric to alkaline substance (sodium hydroxide) is 1:3;

[0082] The sodium chloroacetate solution is a sodium chloroacetate aqueous solution, the mass content of sodium chloroacetate in the sodium chloroacetate aqueous solution is 45%, and the sodium chloroacetate aqueous solution is added according to a mass ratio of cotton fabric to sodium chloroacetate of 1:0.5.

[0083] 2) Tannic acid treatment

[0084] The carboxymethyl cotton fabric is immersed in a tannic acid ethanol solution, and reacted at 30° C. for 12 hours, and after the reaction is completed, a tannic acid-modified cotton fabric is obtained;

[0085] The concentration of tannic acid in the tannic acid ethanol solution is 20 mg / mL.

[0086] 3) Silver ion chelation treatment

[0087] The carboxymethyl cotton fabric modified by tannic acid is taken out, immersed in a silver nitrate ethanol solution, and reacted at 30°C for 24 hours. After the reaction, the obtained cotton fabric is taken out, repeatedly washed three times with a 50% ethanol solution, centrifuged and dried, and then dried to obtain a quick hemostatic cotton.

[0088] The concentration of silver nitrate in the silver nitrate ethanol solution is 1000mmol / L.

[0089] Example 3

[0090] The preparation method of hemostatic cotton comprises the following steps:

[0091] 1) Carboxymethyl treatment

[0092] The cotton fabric is immersed in an alkaline ethanol solution and reacted at 20°C for 6 hours; then a sodium chloroacetate solution is added and reacted at 50°C for 6 hours. After the reaction is completed, a crude cotton fabric is obtained;

[0093] The crude cotton fabric is immersed in an ethanol solution with a volume concentration of 60%, and then lactic acid is added for neutralization; the crude cotton fabric is taken out, and then washed three times with an ethanol solution with a volume concentration of 60%, and after washing, centrifugation is performed and drying is performed to obtain carboxymethyl cotton fabric.

[0094] The alkaline ethanol solution is prepared by mixing a sodium hydroxide aqueous solution with a mass concentration of 30% and anhydrous ethanol in a volume ratio of 1:10, and the mass ratio of cotton fabric to alkaline substance (sodium hydroxide) is 1:2;

[0095] The sodium chloroacetate solution is a sodium chloroacetate aqueous solution, the mass content of sodium chloroacetate in the sodium chloroacetate aqueous solution is 20%, and the sodium chloroacetate aqueous solution is added according to a mass ratio of cotton fabric to sodium chloroacetate of 1:2.

[0096] 2) Tannic acid treatment

[0097] The carboxymethyl cotton fabric is immersed in a tannic acid ethanol solution, and reacted at 20° C. for 6 hours, and after the reaction is completed, a tannic acid-modified cotton fabric is obtained;

[0098] The concentration of tannic acid in the tannic acid ethanol solution is 10 mg / mL.

[0099] 3) Silver ion chelation treatment

[0100] The carboxymethyl cotton fabric modified by tannic acid is taken out, immersed in a silver nitrate ethanol solution, and reacted at 20°C for 12 hours. After the reaction, the obtained cotton fabric is taken out, repeatedly washed three times with a 60% ethanol solution, centrifuged and dried, and then dried to obtain a quick hemostatic cotton.

[0101] The concentration of silver nitrate in the silver nitrate ethanol solution is 800mmol / L.

[0102] Example 4

[0103] The preparation method of hemostatic cotton comprises the following steps:

[0104] 1) Carboxymethyl treatment

[0105] The cotton fabric is immersed in an alkaline ethanol solution and reacted at 10°C for 12 hours; then a sodium chloroacetate solution is added and reacted at 20°C for 12 hours. After the reaction is completed, a crude cotton fabric is obtained;

[0106] The crude cotton fabric is immersed in an ethanol solution with a volume concentration of 95%, and then lactic acid is added for neutralization; the crude cotton fabric is taken out, and then washed three times with an ethanol solution with a volume concentration of 95%, and after washing, centrifugation is performed and drying is performed to obtain a carboxymethyl cotton fabric.

[0107] The alkaline ethanol solution is prepared by mixing a potassium hydroxide aqueous solution with a mass concentration of 20% and anhydrous ethanol in a volume ratio of 1:5, and the mass ratio of the cotton fabric to the alkaline substance (potassium hydroxide) is 1:1;

[0108] The sodium chloroacetate solution is a sodium chloroacetate aqueous solution, the mass content of sodium chloroacetate in the sodium chloroacetate aqueous solution is 30%, and the sodium chloroacetate aqueous solution is added according to a mass ratio of cotton fabric to sodium chloroacetate of 1:3.

[0109] 2) Tannic acid treatment

[0110] The carboxymethyl cotton fabric is immersed in a tannic acid ethanol solution, and reacted at 15° C. for 12 hours, and after the reaction is completed, a tannic acid-modified cotton fabric is obtained;

[0111] The concentration of tannic acid in the tannic acid ethanol solution is 1 mg / mL.

[0112] 3) Silver ion chelation treatment

[0113] The carboxymethyl cotton fabric modified by tannic acid is taken out, immersed in a silver nitrate ethanol solution, and reacted at 15°C for 24 hours. After the reaction, the obtained cotton fabric is taken out, repeatedly washed three times with a 95% ethanol solution, centrifuged and dried, and then dried to obtain a quick hemostatic cotton.

[0114] The concentration of silver nitrate in the silver nitrate ethanol solution is 10 mmol / L.

[0115] Example 5

[0116] The preparation method of hemostatic cotton comprises the following steps:

[0117] 1) Carboxymethyl treatment

[0118] The cotton fabric is immersed in an alkaline ethanol solution and reacted at 40°C for 0.5h; then a sodium chloroacetate solution is added and reacted at 70°C for 0.5h. After the reaction is completed, a crude cotton fabric is obtained;

[0119] The crude cotton fabric is immersed in an ethanol solution with a volume concentration of 50%, and then lactic acid is added for neutralization; the crude cotton fabric is taken out and then washed three times with an ethanol solution with a volume concentration of 50%, and after washing, centrifugation is performed and drying is performed to obtain a carboxymethyl cotton fabric.

[0120] The alkaline ethanol solution is prepared by mixing a potassium hydroxide aqueous solution with a mass concentration of 40% and anhydrous ethanol in a volume ratio of 1:10, and the mass ratio of cotton fabric to potassium hydroxide is 1:2;

[0121] The sodium chloroacetate solution is a sodium chloroacetate aqueous solution, the mass content of sodium chloroacetate in the sodium chloroacetate aqueous solution is 10%, and the sodium chloroacetate aqueous solution is added according to a mass ratio of cotton fabric to sodium chloroacetate of 1:1.

[0122] 2) Tannic acid treatment

[0123] The carboxymethyl cotton fabric is immersed in a tannic acid ethanol solution, and reacted at 30° C. for 0.5 h, and after the reaction is completed, a tannic acid-modified cotton fabric is obtained;

[0124] The concentration of tannic acid in the tannic acid ethanol solution is 20 mg / mL.

[0125] 3) Silver ion chelation treatment

[0126] The carboxymethyl cotton fabric modified by tannic acid is taken out, immersed in a silver nitrate ethanol solution, and reacted at 30°C for 0.5h. After the reaction, the obtained cotton fabric is taken out, repeatedly washed three times with a 50% ethanol solution, centrifuged and dried, and then dried to obtain a quick hemostatic cotton.

[0127] The concentration of silver nitrate in the silver nitrate ethanol solution is 1000mmol / L.

[0128] Comparative Example 1

[0129] The method for preparing hemostatic cotton does not include step 1) carboxymethyl treatment, and the other conditions are consistent with those in Example 1.

[0130] Comparative Example 2

[0131] The method for preparing hemostatic cotton does not include step 2) tannic acid treatment, and the other conditions are the same as those in Example 1.

[0132] Comparative Example 3

[0133] The method for preparing hemostatic cotton does not include step 3) silver ion chelation treatment, and the other conditions are consistent with those in Example 1.

[0134] The hemostatic cotton prepared in Examples 1-5 and Comparative Examples 1-3 was subjected to hemostatic effect, adhesion test, AATCC-100 standard test and in vitro release method, and the test process was as follows:

[0135] 1. Using a rabbit liver bleeding animal model to evaluate the hemostatic effect of the hemostatic cotton prepared in Examples 1-5 and Comparative Examples 1-3

[0136] The specific method is: weigh the rabbit and use 1% sodium pentobarbital 30 mg kg -1Weight Anesthesia was performed through the ear vein of the rabbit, the skin was prepared, disinfected, and the abdominal cavity was opened to fully expose the right lobe of the liver. A cross incision (depth of about 0.3 cm, length of about 0.5 cm) was made at the same position of the right liver with a scalpel. Gauze (1.5 cm×1.5 cm) of the sample group and the commercial group was applied to the wound surface respectively, and light pressure was applied for 10 seconds. At the same time, the timing was started, and the blood flowing out was absorbed with clean filter paper of the same quality until the blood stopped flowing out. At this time, the timing was stopped and the bleeding time was recorded; the total weight of the filter paper after blood absorption was immediately weighed, the number of filter paper pieces was recorded, and the amount of bleeding was calculated according to the formula: Bleeding amount = total weight of filter paper after blood absorption - (weight of a single filter paper × number of filter paper pieces), so as to evaluate its hemostatic effect, and the bleeding time and bleeding amount were recorded in a table.

[0137] Example 1 Example 2 Example 3 Example 4 Example 5 Comparative Example 1 Comparative Example 2 Comparative Example 3 Hemostasis time / s 85 79 81 83 89 92 183 86 Bleeding volume / g 0.15 0.13 0.14 0.14 0.16 0.48 0.52 0.15

[0138] The test results show that the hemostatic samples of Examples 1-5 have a hemostatic time of 79-89 seconds and a bleeding volume of 0.13-0.16 g; while the hemostatic time of the cotton gauze of Comparative Example 2 is 183 seconds and the bleeding volume is 0.52 g, which proves that the hemostatic effect of the modified samples is significantly improved, indicating that tannic acid modification can significantly improve the hemostatic performance of cotton.

[0139] 2. Use fresh pigskin to test the adhesion of the sample

[0140] Cut fresh pigskin into strips of 2cm*8cm, clean the surface of the pigskin to ensure that there is no grease and impurities on the surface, place the moistened modified sample and the unmodified sample on the pigskin, then align another piece of pigskin with the pigskin coated with the sample and apply appropriate pressure for 5 minutes to ensure adhesion. Place the bonded pigskin sample in the fixture of the universal material testing machine, perform a tensile test at a speed of 200mm / min, and record the maximum load.

[0141] Example 1 Example 2 Example 3 Example 4 Example 5 Comparative Example 1 Comparative Example 2 Comparative Example 3 Adhesion force / N 1.4 2.1 1.8 1.4 1.5 0.8 0.5 1.4

[0142] The results showed that the tensile force of the modified group was between 1.4-2.1N, significantly higher than that of the comparative example 1 group, and the tensile force of the comparative example 3 was significantly higher than that of the comparative example 2, proving that tannic acid modification can significantly improve the adhesion ability of cotton gauze, and the adhesion increases with the increase of tannic acid content.

[0143] 3. The antimicrobial properties of tannic acid-modified and unmodified samples were evaluated by quantitative methods according to the AATCC-100 standard.

[0144] Staphylococcus aureus and Escherichia coli suspensions were inoculated onto the surfaces of Example 3 and Comparative Example 2, respectively, and cultured at 37±2°C for 1 day. Neutralizing solution was added and vortexed to mix. After continuous dilution, the suspensions were cultured on culture plates and the number of colonies was observed to evaluate the antibacterial properties of the samples.

[0145] The results showed that no colonies were produced in the tannic acid modified group, while colonies were formed in the unmodified group, proving that the tannic acid modified group had good antibacterial properties.

[0146] 4. Referring to the in vitro release method of drug patches in the United States Pharmacopoeia, the reciprocating stent method was used to evaluate the release of silver ions in water.

[0147] The sample of Example 3 was cut into a size of 5*5 cm and placed in a reciprocating bracket. 200 ml of water was measured in a beaker and set to release time points of 1, 6, 12 and 24 hours. The release temperature was 32±2°C. After each release point was completed, each beaker was filled with deionized water and mixed, and 5 ml of release liquid was taken to measure the total silver content released by an atomic absorption spectrophotometer.

[0148] The results showed that silver ions were released rapidly in the first 6 hours, with a total amount of 74 μg. The release rate slowed down in 6-12 hours, and silver ions were still released in 12-24 hours, with a total release amount of 128 μg. This proves that tannic acid-modified hemostatic cotton can slowly release silver ions on the wound for up to 24 hours, achieving a long-lasting antibacterial effect.

[0149] The raw materials or reagents used in the examples and comparative examples of the present invention are all purchased from mainstream manufacturers in the market. Those without indicating the manufacturer or concentration are all analytically pure raw materials or reagents that can be routinely obtained. As long as they can play the expected role, there is no special limitation.

[0150] The instruments and equipment used in this embodiment are all purchased from major manufacturers in the market, and there is no particular limitation as long as they can play the expected role. In this embodiment, if no specific technology or conditions are specified, the technology or conditions described in the literature in this field or the product instructions are used. The above embodiments are preferred implementation schemes of the present invention. In addition, the present invention can also be implemented in other ways. Any obvious replacement without departing from the concept of the present invention is within the protection scope of the present invention.

Claims

1. A quick hemostatic cotton with good antibacterial and adhesive properties, characterized in that: The quick hemostatic cotton is obtained by sequentially treating cotton fabric with carboxymethyl, tannic acid and silver ion chelation. The carboxymethyl treatment process comprises the following steps: immersing the cotton fabric in an alkaline ethanol solution, reacting at 10-40° C. for 0.5-12 hours; then adding a sodium chloroacetate solution, reacting at 20-70° C. for 0.5-12 hours, to obtain a carboxymethyl cotton fabric; The tannic acid treatment process comprises the following steps: immersing the carboxymethyl cotton fabric in a tannic acid ethanol solution to react, and obtaining a tannic acid modified cotton fabric after the reaction is completed; The silver ion chelation treatment process comprises the following steps: immersing the tannic acid modified cotton fabric in a silver nitrate ethanol solution to react, and obtaining a quick hemostatic cotton after the reaction is completed.

2. The rapid hemostatic cotton according to claim 1, characterized in that: The mass content of the alkaline substance in the alkaline ethanol solution is 1-20%.

3. The rapid hemostatic cotton according to claim 1, characterized in that: The mass content of sodium chloroacetate in the sodium chloroacetate solution is 5-45%.

4. The rapid hemostatic cotton according to claim 1, characterized in that: During the carboxymethyl treatment, a sodium chloroacetate solution is added, and the reaction is carried out at 20-70° C. for 0.5-12 hours. After the reaction is completed, a crude cotton fabric is obtained; the crude cotton fabric is immersed in an ethanol solution, and lactic acid is added for neutralization; The crude cotton fabric is taken out, and then washed three times with an ethanol solution. After washing, it is centrifuged and dried to obtain a carboxymethyl cotton fabric.

5. The rapid hemostatic cotton according to claim 1, characterized in that: The tannic acid concentration in the tannic acid ethanol solution is 1-20 mg / mL.

6. The rapid hemostatic cotton according to claim 1, characterized in that: The tannic acid treatment process is to react at 15-30° C. for 0.5 to 12 hours.

7. The rapid hemostatic cotton according to claim 1, characterized in that: The silver ion chelation treatment process is to react at 15-30° C. for 0.5 to 24 hours.

8. The rapid hemostatic cotton according to claim 1, characterized in that: The concentration of silver nitrate in the silver nitrate ethanol solution is 10-1000 mmol / L.

9. The method for preparing the hemostatic cotton according to any one of claims 1 to 8, characterized in that: The following steps are involved: 1) Carboxymethyl treatment The cotton fabric is immersed in an alkaline ethanol solution and reacted at 10-40°C for 0.5-12 hours; then a sodium chloroacetate solution is added and reacted at 20-70°C for 0.5-12 hours to obtain a carboxymethyl cotton fabric; 2) Tannic acid treatment The carboxymethyl cotton fabric is immersed in a tannic acid ethanol solution to react, and after the reaction is completed, a tannic acid-modified cotton fabric is obtained; 3) Silver ion chelation treatment The tannic acid modified cotton fabric is immersed in a silver nitrate ethanol solution to react, and after the reaction is completed, a quick hemostatic cotton is obtained.

10. The application of hemostatic cotton is characterized by: The hemostatic cotton described in any one of claims 1 to 8 or the hemostatic cotton prepared by the preparation method described in claim 9 is used as a hemostatic material and applied to hemostasis.