CN114404641A - Preparation method of medical antibacterial gauze and medical antibacterial gauze - Google Patents
Preparation method of medical antibacterial gauze and medical antibacterial gauze Download PDFInfo
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Abstract
The invention relates to a preparation method of medical antibacterial gauze and the medical antibacterial gauze, comprising the steps of S10 preparing antibacterial MOFs particles, S20 activating the gauze and S30 preparing the medical antibacterial gauze; the preparation method of the medical antibacterial gauze is simple, is green and environment-friendly, and is also suitable for industrial production; the medical antibacterial gauze consists of common non-oily medical gauze and an antibacterial coating adhered to the medical gauze, has obvious and lasting antibacterial effect, can effectively promote wound healing, can greatly shorten the time of a wound, and reduces the formation of scars; the problem of poor antibacterial property of the traditional medical gauze is solved, and the medical gauze can be effectively used for healing burn wounds.
Description
Technical Field
The invention relates to the technical field of medical gauze, in particular to a preparation method of medical antibacterial gauze and the medical antibacterial gauze.
Background
The skin is the first barrier to protect the body from damage. In daily life, people inevitably encounter various accidents to cause skin damage. Burn is the most common type, the degree of burn is often large-area skin injury, and the burn is very easily infected by pathogenic bacteria in the environment during the healing process, so that the wound is easily deteriorated, and systemic septicemia, phlebitis and even death can be caused seriously.
The medical gauze is the main medical gauze for treating mild burns at present due to low price and good air permeability. However, the traditional gauze usually needs to be added with antibiotics due to high permeability and poor antibacterial performance, so that the emergence of drug-resistant germs is easily caused, and the healing effect on the wounded surface is hardly promoted. In addition, most of the gauze used for treating burn in the literature has the disadvantages of complicated manufacturing method, high cost, simple and convenient method, unobvious treatment effect and easy scar generation after wound healing.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of medical antibacterial gauze and the medical antibacterial gauze aiming at the defects in the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of medical antibacterial gauze comprises the following steps:
s10 preparation of antibacterial MOFs particles: preparing MOFs precursor solution, pouring the MOFs precursor solution into a reaction kettle containing a polytetrafluoroethylene lining, fully reacting at the high temperature of 120-200 ℃, drying, taking out, and removing excessive reaction solvent to obtain antibacterial MOFs particles;
s20 gauze activation treatment: soaking medical gauze in a sodium hydroxide solution with the mass concentration of 10% -25%, taking out after full infiltration, drying, washing and drying the medical gauze to prepare carboxymethylated medical gauze;
s30, preparing medical antibacterial gauze, namely dissolving the antibacterial MOFs particles obtained in S10 in a DMF (dimethyl formamide) organic solvent with the mass concentration of 40-80% to obtain an MOFs solution, and soaking the carboxymethylated medical gauze obtained in S20 in the MOFs solution; taking out after full infiltration, washing with distilled water and drying; repeating the preparation process in the step S30 for multiple times to obtain the medical antibacterial gauze adhered with the antibacterial coating;
wherein the MOFs precursor solution consists of a metal source, an organic ligand and a solvent; the metal source is zinc nitrate hexahydrate and/or cerium nitrate hexahydrate; the organic ligand is one or a combination of more of 2-methylimidazole, 2-amino isophthalic acid, 2, 3-dihydroxy terephthalic acid and 2-aminobenzimidazole; the solvent is a combination of methanol, DMF, silver nitrate, citric acid and antibiotics; the mass ratio of the metal source, the organic ligand and the solvent in the precursor solution of the MOFs is 1 (1-60) to 20-100;
the preparation method of the medical antibacterial gauze comprises the following steps of preparing the MOFs precursor solution in the step S10 according to the following method: weighing the zinc nitrate hexahydrate and the cerium nitrate hexahydrate in a mass ratio of 1 (1-2); adding 2-methylimidazole into zinc nitrate hexahydrate, pouring into a methanol solution, and dissolving to obtain a solution A; the mass ratio of the zinc nitrate hexahydrate to the 2-methylimidazole is 20: 1; the mass ratio of the zinc nitrate hexahydrate to the methanol solution is 40: 1;
adding 2-amino isophthalic acid with equal mass into cerium nitrate hexahydrate, and pouring into a DMF solution for dissolving; the mass ratio of the cerous nitrate hexahydrate to the DMF solution is (25-50): 1, marking as solution B;
respectively and fully stirring the solution A and the solution B, and then mixing to obtain a solution C;
slowly dropwise adding a silver nitrate solution into the solution C, finally adding citric acid, and fully stirring to obtain the MOFs precursor solution; the mass ratio of the silver nitrate to the zinc nitrate hexahydrate is 1: 85 parts by weight; the mass ratio of the citric acid to the zinc nitrate hexahydrate is 1: 2;
the preparation method of the medical antibacterial gauze comprises the following steps of preparing the MOFs precursor solution in the step S10 according to the following method: weighing the zinc nitrate hexahydrate and the cerium nitrate hexahydrate in a mass ratio of 1: 1; adding 2-methylimidazole into zinc nitrate hexahydrate, pouring into a methanol solution, and dissolving to obtain a solution A'; the mass ratio of the zinc nitrate hexahydrate to the 2-methylimidazole is 20: 1; the mass ratio of the zinc nitrate hexahydrate to the methanol solution is 40: 1;
adding 2-amino isophthalic acid with equal mass into cerium nitrate hexahydrate, and pouring into a DMF solution for dissolving; the mass ratio of the cerous nitrate hexahydrate to the DMF solution is 50: 1, denoted as solution B';
fully stirring the solution A and the solution B respectively and then mixing to obtain a solution C';
slowly dripping antibiotics into the solution C', and fully stirring to obtain the MOFs precursor solution; the mass ratio of the antibiotic to the zinc nitrate hexahydrate is 1: (1-2);
the preparation method of the medical antibacterial gauze comprises the following steps of preparing the MOFs precursor solution in the step S10 according to the following method: weighing 1mmol of cerous nitrate hexahydrate; adding 2, 3-dihydroxyterephthalic acid with equal mass into the cerium nitrate hexahydrate, pouring into the DMF solution, dissolving and stirring, wherein the mass ratio of the cerium nitrate hexahydrate to the DMF solution is 25: 1; denoted as solution A ";
slowly dropwise adding a silver nitrate solution into the solution A', finally adding citric acid, and fully stirring to obtain the MOFs precursor solution; the mass ratio of the silver nitrate to the cerium nitrate hexahydrate is 1: 85 parts by weight; the mass ratio of the citric acid to the cerous nitrate hexahydrate is 1: 2;
the preparation method of the medical antibacterial gauze comprises the following steps of preparing the MOFs precursor solution in the step S10 according to the following method: weighing 1mmol of zinc nitrate hexahydrate; adding 2-aminobenzimidazole into the zinc nitrate hexahydrate, and then pouring into the DMF solution for dissolving and stirring; the mass ratio of the zinc nitrate hexahydrate to the 2-aminobenzimidazole is 20: 1; the mass ratio of the cerous nitrate hexahydrate to the DMF solution is 25: 1; denoted solution a' ″;
slowly dropwise adding a silver nitrate solution into the solution A', finally adding citric acid, and fully stirring to obtain the MOFs precursor solution; the mass ratio of the silver nitrate to the cerium nitrate hexahydrate is 1: 85 parts by weight; the mass ratio of the citric acid to the cerous nitrate hexahydrate is 1: 2;
in the step S20, the MOFs particles are washed with DMF and methanol for 3-5 times to remove excess reaction solvent on the MOFs;
the preparation method of the medical antibacterial gauze comprises the step S30, soaking the medical gauze in the sodium hydroxide solution for 1-2h, pre-drying at 60-90 ℃, washing for 5-10 times, and drying at 120-150 ℃ for 1-5min to obtain carboxymethylated medical gauze;
the preparation method of the medical antibacterial gauze comprises the step of preparing one or more of vancomycin, fusidic acid, clindamycin, benzathine, azithromycin and ciprofloxacin by using antibiotics.
The invention also discloses medical antibacterial gauze, wherein the medical antibacterial gauze comprises common non-oily medical gauze and an antibacterial coating adhered to the medical gauze; the antibacterial coating is prepared by soaking and washing MOFs solution; the MOFs solution comprises N, N-dimethylformamide, polyvinylpyrrolidone and MOFs particles; the MOFs solution comprises the following components in percentage by mass: polyvinylpyrrolidone: MOFs particles are (5-20), (10-15) and (5-15); the MOFs particles are prepared by mixing and stirring various solutions of antibiotics, silver nitrate solution, cerium nitrate hexahydrate, zinc nitrate hexahydrate, 2-methylimidazole, 2-amino isophthalic acid or 2, 3-dihydroxy terephthalic acid and citric acid, and drying, washing and drying again for multiple times;
the medical antibacterial gauze provided by the invention is characterized in that the quantity ratio of antibiotics, silver nitrate solution, cerium nitrate hexahydrate, zinc nitrate hexahydrate, 2-methylimidazole, 2-amino isophthalic acid and citric acid substances in MOFs particles is (1-3) to (1-5) to (3-10) to (25-100) to (1-3) to (3-5);
the medical antibacterial gauze provided by the invention is characterized in that the mass ratio of the medical gauze to the MOFs solution is 1 (4-10).
The invention has the following beneficial effects:
the preparation method of the medical antibacterial gauze is simple, is green and environment-friendly, and is also suitable for industrial production;
the medical antibacterial gauze consists of common non-oily medical gauze and an antibacterial coating adhered to the medical gauze, wherein the antibacterial coating is prepared by soaking and washing MOFs solution; the MOFs solution contains N, N-dimethylformamide, polyvinylpyrrolidone and MOFs particles; the MOFs can induce the generation of single oxygen (1O2) and active oxygen (ROS), has excellent nonspecific antibiosis, good biocompatibility and small influence on the environment, and the medical antibacterial gauze with the antibacterial coating can slowly release antibacterial effective substances in an acid environment, has obvious and lasting antibacterial effect, can effectively promote the healing of wounds, can greatly shorten the time of the wounds and reduce the formation of scars; the problem of poor antibacterial property of the traditional medical gauze is solved, and the medical gauze can be effectively used for healing burn wounds.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the present invention will be further described with reference to the accompanying drawings and embodiments, wherein the drawings in the following description are only part of the embodiments of the present invention, and for those skilled in the art, other drawings can be obtained without inventive efforts according to the accompanying drawings:
FIG. 1 is a flow chart of a method for preparing medical antibacterial gauze according to a preferred embodiment of the present invention;
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without inventive step, are within the scope of the present invention.
Reference herein to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the invention. The appearances of the phrase in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. It is explicitly and implicitly understood by one skilled in the art that the embodiments described herein can be combined with other embodiments.
"plurality" means two or more. "and/or" describes the association relationship of the associated objects, meaning that there may be three relationships, e.g., a and/or B, which may mean: a exists alone, A and B exist simultaneously, and B exists alone. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.
It should be noted that the MOFs are mainly formed by coordination bonds formed by metal ions and organic ligands, can induce the generation of singlet oxygen (1O2) and Reactive Oxygen Species (ROS), have excellent nonspecific antibacterial properties, have better biocompatibility, are less environmentally friendly compared with traditional metal antibacterial agents, have better stability and longer-lasting antibacterial efficacy compared with natural antibacterial agents, and are ideal antibacterial finishing agents.
Zinc is a trace element necessary for human body, and the zinc and oxide particles thereof have good ultraviolet protection function and antibacterial activity. Zn2+ has been studied in biomedical applications, and is commonly used in Photodynamic (PDT) or photothermal Power (PTT) therapies.
Cerium belongs to lanthanide rare earth elements, the storage capacity in the earth crust is equivalent to that of copper, and the price is lower. Ce3+ has good antibacterial activity and biocompatibility due to strong binding capacity with ATP (adenosine triphosphate) and enzyme-like activity, can promote cell growth, and has wide research and application in the fields of artificial implants, bone repair, tissue engineering and the like.
Example 1
A preparation method of medical antibacterial gauze comprises calculating and weighing zinc nitrate hexahydrate and cerium nitrate hexahydrate in a mass ratio of 1: 1. Adding 2-methylimidazole into zinc nitrate hexahydrate, wherein the mass ratio of the zinc nitrate hexahydrate to the 2-methylimidazole is 20: 1; and pouring zinc nitrate hexahydrate and 2-methylimidazole into a methanol solution for dissolving, wherein the mass ratio of the zinc nitrate hexahydrate to the methanol solution is 40: 1; denoted as solution a 1;
adding 2-amino isophthalic acid with equal mass into cerium nitrate hexahydrate, and pouring the cerium nitrate hexahydrate and the 2-amino isophthalic acid into a DMF solution for dissolving, wherein the mass ratio of the cerium nitrate hexahydrate to the DMF solution is 25: 1, noted as solution B1;
respectively stirring the solution A1 and the solution B1 for 20-40min by using a magnetic stirrer with the rotating speed of 800-;
slowly dropwise adding a silver nitrate solution into the solution C1, wherein the mass ratio of silver nitrate to zinc nitrate hexahydrate is 1: 85 parts by weight; and finally adding citric acid, wherein the mass ratio of the citric acid to the zinc nitrate hexahydrate is 1:2, and stirring and processing for 25-50min by using an ultrasonic cleaning device of 80-120W to obtain the MOFs precursor solution.
Pouring the MOFs precursor solution into a reaction kettle containing a polytetrafluoroethylene lining, and putting the reaction kettle into an oven at the temperature of 120-200 ℃ for reaction for 36-72 hours. After the reaction is finished, MOFs particles are obtained, washing is carried out for 3-5 times by using DMF and methanol solution, excessive reaction solvent is removed, and the MOFs particles are dried by using an oven to obtain the antibacterial MOFs particles.
Taking a piece of medical gauze, immersing the medical gauze into a sodium hydroxide solution with the mass concentration of 10-25% for treatment for 1-2h, then performing pre-drying treatment in the environment of 60-90 ℃, washing for 5-10 times, and finally drying for 1-5min in the environment of 120-150 ℃ to obtain the carboxymethylated medical gauze.
It is worth noting that the weight of sodium hydroxide corresponds to 5% to 10% of the weight of the medical gauze to be treated.
The prepared antibacterial MOFs particles are dissolved in DMF (organic solvent) solution with the mass concentration of 40-80%. Soaking the prepared carboxymethylated medical gauze into MOFs solution for 10-20min, washing the soaked gauze by using distilled water at room temperature for 5-10min by using magnetic stirring, and then drying the gauze for 20-50min at the temperature of 80 ℃; repeating the above process for 3-10 times to obtain the medical antibacterial gauze adhered with the antibacterial coating.
Example 2
A preparation method of medical antibacterial gauze comprises calculating and weighing zinc nitrate hexahydrate and cerium nitrate hexahydrate in a mass ratio of 1: 2. Adding 2-methylimidazole into zinc nitrate hexahydrate, wherein the mass ratio of the zinc nitrate hexahydrate to the 2-methylimidazole is 20: 1; and pouring zinc nitrate hexahydrate and 2-methylimidazole into a methanol solution for dissolving, wherein the mass ratio of the zinc nitrate hexahydrate to the methanol solution is 40: 1; denoted as solution a 2;
adding 2-amino isophthalic acid with equal mass into cerium nitrate hexahydrate, and pouring the cerium nitrate hexahydrate and the 2-amino isophthalic acid into a DMF solution for dissolving, wherein the mass ratio of the cerium nitrate hexahydrate to the DMF solution is 50: 1, noted as solution B2;
respectively stirring and treating the solution A2 and the solution B2 for 20-40min by using a magnetic stirrer with the rotation speed of 800-1200r/min, and then mixing the solution A2 and the solution B2 to obtain a solution C2.
Slowly dropwise adding a silver nitrate solution into the solution C2, wherein the mass ratio of silver nitrate to zinc nitrate hexahydrate is 1: 85 parts by weight; and finally adding citric acid, wherein the mass ratio of the citric acid to the zinc nitrate hexahydrate is 1:2, and stirring and processing for 25-50min by using an ultrasonic cleaning device of 80-120W to obtain the MOFs precursor solution.
Pouring the MOFs precursor solution into a reaction kettle containing a polytetrafluoroethylene lining, and putting the reaction kettle into an oven at the temperature of 120-200 ℃ for reaction for 36-72 hours. After the reaction is finished, MOFs particles are obtained, washing is carried out for 3-5 times by using DMF and methanol solution, excessive reaction solvent is removed, and the MOFs particles are dried by using an oven to obtain the antibacterial MOFs particles.
Taking a piece of medical gauze, immersing the medical gauze into a sodium hydroxide solution with the mass concentration of 10-25% for treatment for 1-2h, then performing pre-drying treatment in the environment of 60-90 ℃, washing for 5-10 times, and finally drying for 1-5min in the environment of 120-150 ℃ to obtain the carboxymethylated medical gauze.
It is worth noting that the weight of sodium hydroxide corresponds to 5% to 10% of the weight of the medical gauze to be treated.
The prepared antibacterial MOFs particles are dissolved in DMF (organic solvent) solution with the mass concentration of 40-80%. Soaking the prepared carboxymethylated medical gauze into MOFs solution for 10-20min, washing the soaked gauze by using distilled water at room temperature for 5-10min by using magnetic stirring, and then drying the gauze for 20-50min at the temperature of 80 ℃; repeating the above process for 3-10 times to obtain the medical antibacterial gauze adhered with the antibacterial coating.
Example 3
A preparation method of medical antibacterial gauze comprises calculating and weighing zinc nitrate hexahydrate and cerium nitrate hexahydrate in a mass ratio of 1: 1. Adding 2-methylimidazole into zinc nitrate hexahydrate, wherein the mass ratio of the zinc nitrate hexahydrate to the 2-methylimidazole is 20: 1; and pouring zinc nitrate hexahydrate and 2-methylimidazole into a methanol solution for dissolving, wherein the mass ratio of the zinc nitrate hexahydrate to the methanol solution is 40: 1; denoted as solution a 3;
adding 2-amino isophthalic acid with equal mass into cerium nitrate hexahydrate, and pouring the cerium nitrate hexahydrate and the 2-amino isophthalic acid into a DMF solution for dissolving, wherein the mass ratio of the cerium nitrate hexahydrate to the DMF solution is 50: 1, noted as solution B3;
respectively stirring the solution A3 and the solution B3 for 20-40min by using a magnetic stirrer with the rotating speed of 800-;
slowly and dropwise adding vancomycin into the solution C3, wherein the mass ratio of the vancomycin to zinc nitrate hexahydrate is 1:2, it is worth to say that vancomycin is one of antibiotics; stirring and processing for 25-50min by using an ultrasonic cleaning device of 80-120W to obtain MOFs precursor solution;
pouring the MOFs precursor solution into a reaction kettle containing a polytetrafluoroethylene lining, and putting the reaction kettle into an oven at the temperature of 120-200 ℃ for reaction for 36-72 hours. After the reaction is finished, MOFs particles are obtained, washing is carried out for 3-5 times by using DMF and methanol solution, excessive reaction solvent is removed, and the MOFs particles are dried by using an oven to obtain the antibacterial MOFs particles.
Taking a piece of medical gauze, immersing the medical gauze into a sodium hydroxide solution with the mass concentration of 10-25% for treatment for 1-2h, then performing pre-drying treatment in the environment of 60-90 ℃, washing for 5-10 times, and finally drying for 1-5min in the environment of 120-150 ℃ to obtain the carboxymethylated medical gauze.
It is worth noting that the weight of sodium hydroxide corresponds to 5% to 10% of the weight of the medical gauze to be treated.
The prepared antibacterial MOFs particles are dissolved in DMF (organic solvent) solution with the mass concentration of 40-80%. Soaking the prepared carboxymethylated medical gauze into MOFs solution for 10-20min, washing the soaked gauze by using distilled water at room temperature for 5-10min by using magnetic stirring, and then drying the gauze for 20-50min at the temperature of 80 ℃; repeating the above process for 3-10 times to obtain the medical antibacterial gauze adhered with the antibacterial coating.
Example 4
A preparation method of medical antibacterial gauze comprises calculating and weighing zinc nitrate hexahydrate and cerium nitrate hexahydrate in a mass ratio of 1: 1. Adding 2-methylimidazole into zinc nitrate hexahydrate, wherein the mass ratio of the zinc nitrate hexahydrate to the 2-methylimidazole is 20: 1; and pouring zinc nitrate hexahydrate and 2-methylimidazole into a methanol solution for dissolving, wherein the mass ratio of the zinc nitrate hexahydrate to the methanol solution is 40: 1; denoted as solution a 4;
adding 2-amino isophthalic acid with equal mass into cerium nitrate hexahydrate, and pouring the cerium nitrate hexahydrate and the 2-amino isophthalic acid into a DMF solution for dissolving, wherein the mass ratio of the cerium nitrate hexahydrate to the DMF solution is 50: 1, noted as solution B4.
Respectively stirring the solution A4 and the solution B4 for 20-40min by using a magnetic stirrer with the rotating speed of 800-;
slowly dropwise adding vancomycin and fusidic acid into the solution C3, wherein the mass ratio of the vancomycin to the fusidic acid to the zinc nitrate hexahydrate is 1: 1:1, it is worth mentioning that vancomycin and fusidic acid are both one of the antibiotics; stirring and processing for 25-50min by using an ultrasonic cleaning device of 80-120W to obtain MOFs precursor solution;
and adding vancomycin and fusidic acid with equal mass of zinc nitrate hexahydrate into the mixed solution, and treating for 25-50min by using an ultrasonic cleaning device (80-120W), wherein the solution is marked as solution C4.
Pouring the MOFs precursor solution into a reaction kettle containing a polytetrafluoroethylene lining, and putting the reaction kettle into an oven at the temperature of 120-200 ℃ for reaction for 36-72 hours. After the reaction is finished, MOFs particles are obtained, washing is carried out for 3-5 times by using DMF and methanol solution, excessive reaction solvent is removed, and the MOFs particles are dried by using an oven to obtain the antibacterial MOFs particles.
Taking a piece of medical gauze, immersing the medical gauze into a sodium hydroxide solution with the mass concentration of 10-25% for treatment for 1-2h, then performing pre-drying treatment in the environment of 60-90 ℃, washing for 5-10 times, and finally drying for 1-5min in the environment of 120-150 ℃ to obtain the carboxymethylated medical gauze.
It is worth noting that the weight of sodium hydroxide corresponds to 5% to 10% of the weight of the medical gauze to be treated.
The prepared antibacterial MOFs particles are dissolved in DMF (organic solvent) solution with the mass concentration of 40-80%. Soaking the prepared carboxymethylated medical gauze into MOFs solution for 10-20min, washing the soaked gauze by using distilled water at room temperature for 5-10min by using magnetic stirring, and then drying the gauze for 20-50min at the temperature of 80 ℃; repeating the above process for 3-10 times to obtain the medical antibacterial gauze adhered with the antibacterial coating.
Example 5
A preparation method of medical antibacterial gauze comprises calculating and weighing 1mmol of cerous nitrate hexahydrate; the difference from examples 1 to 4 is that the organic intermediate ligand is modified, in particular in that: adding 2, 3-dihydroxyterephthalic acid into cerium nitrate hexahydrate, wherein the mass ratio of the cerium nitrate hexahydrate to the 2, 3-dihydroxyterephthalic acid is 1: 1; and pouring the cerous nitrate hexahydrate and the 2, 3-dihydroxy terephthalic acid into a DMF solution for dissolving, wherein the mass ratio of the cerous nitrate hexahydrate to the DMF solution is 25: 1; denoted as solution a 5;
stirring the solution A5 for 20-40min by using a magnetic stirrer with the rotating speed of 800-.
Slowly dropwise adding a silver nitrate solution into the solution A5, wherein the mass ratio of silver nitrate to cerium nitrate hexahydrate is 1: 85 parts by weight; and finally adding citric acid, wherein the mass ratio of the citric acid to the cerous nitrate hexahydrate is 1:2, and stirring and treating for 25-50min by using an ultrasonic cleaning device of 80-120W to obtain the MOFs precursor solution.
Pouring the MOFs precursor solution into a reaction kettle containing a polytetrafluoroethylene lining, and putting the reaction kettle into an oven at the temperature of 120-200 ℃ for reaction for 36-72 hours. After the reaction is finished, MOFs particles are obtained, washing is carried out for 3-5 times by using DMF and methanol solution, excessive reaction solvent is removed, and the MOFs particles are dried by using an oven to obtain the antibacterial MOFs particles.
Taking a piece of medical gauze, immersing the medical gauze into a sodium hydroxide solution with the mass concentration of 10-25% for treatment for 1-2h, then performing pre-drying treatment in the environment of 60-90 ℃, washing for 5-10 times, and finally drying for 1-5min in the environment of 120-150 ℃ to obtain the carboxymethylated medical gauze.
It is worth noting that the weight of sodium hydroxide corresponds to 5% to 10% of the weight of the medical gauze to be treated.
The prepared antibacterial MOFs particles are dissolved in DMF (organic solvent) solution with the mass concentration of 40-80%. Soaking the prepared carboxymethylated medical gauze into MOFs solution for 10-20min, washing the soaked gauze by using distilled water at room temperature for 5-10min by using magnetic stirring, and then drying the gauze for 20-50min at the temperature of 80 ℃; repeating the above process for 3-10 times to obtain the medical antibacterial gauze adhered with the antibacterial coating.
Example 6
A preparation method of medical antibacterial gauze calculates and weighs 1mmol of zinc nitrate hexahydrate, which is different from the embodiment 1-4 in that an organic intermediate ligand is changed, and specifically comprises the following steps: adding 2-aminobenzimidazole into zinc nitrate hexahydrate, wherein the mass ratio of the zinc nitrate hexahydrate to the 2-aminobenzimidazole is 20: 1; and pouring zinc nitrate hexahydrate and 2-aminobenzimidazole into a DMF solution for dissolving, wherein the mass ratio of the cerous nitrate hexahydrate to the DMF solution is 25: 1; denoted as solution a 6;
stirring the solution A5 for 20-40min by using a magnetic stirrer with the rotating speed of 800-.
Slowly dropwise adding a silver nitrate solution into the solution A6, wherein the mass ratio of silver nitrate to zinc nitrate hexahydrate is 1: 85 parts by weight; finally adding citric acid, wherein the mass ratio of the citric acid to the cerous nitrate hexahydrate is 1:2, and stirring by using an ultrasonic cleaning device of 80-120W for 25-50min to obtain an MOFs precursor solution;
pouring the MOFs precursor solution into a reaction kettle containing a polytetrafluoroethylene lining, and putting the reaction kettle into an oven at the temperature of 120-200 ℃ for reaction for 36-72 hours. After the reaction is finished, MOFs particles are obtained, washing is carried out for 3-5 times by using DMF and methanol solution, excessive reaction solvent is removed, and the MOFs particles are dried by using an oven to obtain the antibacterial MOFs particles.
Taking a piece of medical gauze, immersing the medical gauze into a sodium hydroxide solution with the mass concentration of 10-25% for treatment for 1-2h, then performing pre-drying treatment in the environment of 60-90 ℃, washing for 5-10 times, and finally drying for 1-5min in the environment of 120-150 ℃ to obtain the carboxymethylated medical gauze.
It is worth noting that the weight of sodium hydroxide corresponds to 5% to 10% of the weight of the medical gauze to be treated.
The prepared antibacterial MOFs particles are dissolved in DMF (organic solvent) solution with the mass concentration of 40-80%. Soaking the prepared carboxymethylated medical gauze into MOFs solution for 10-20min, washing the soaked gauze by using distilled water at room temperature for 5-10min by using magnetic stirring, and then drying the gauze for 20-50min at the temperature of 80 ℃; repeating the above process for 3-10 times to obtain the medical antibacterial gauze adhered with the antibacterial coating.
Example 7
A medical antibacterial gauze, employ the preparation method of the above-mentioned medical antibacterial gauze, the medical antibacterial gauze includes ordinary non-oily medical gauze and antibacterial coating adhered to medical gauze; the antibacterial coating is prepared by soaking and washing MOFs solution; the MOFs solution comprises N, N-dimethylformamide, polyvinylpyrrolidone and MOFs particles; the mass ratio of each component in the MOFs solution is as follows: polyvinylpyrrolidone: MOFs particles are (5-20), (10-15) and (5-15); the MOFs particles are prepared by mixing and stirring a plurality of solutions of antibiotics, silver nitrate solution, cerium nitrate hexahydrate, zinc nitrate hexahydrate, 2-methylimidazole, 2-amino isophthalic acid or 2, 3-dihydroxy terephthalic acid and citric acid, and drying, washing and drying again for multiple times.
Specifically, the quantity ratio of antibiotics, silver nitrate solution, cerium nitrate hexahydrate, zinc nitrate hexahydrate, 2-methylimidazole, 2-amino isophthalic acid and citric acid substances in the MOFs particles is (1-3): 1-5): 3-10): 25-100): 1-3): 3-5.
Specifically, the mass ratio of the medical gauze to the MOFs solution is 1 (4-10)
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (10)
1. A preparation method of medical antibacterial gauze comprises the following steps:
s10 preparation of antibacterial MOFs particles: preparing MOFs precursor solution, pouring the MOFs precursor solution into a reaction kettle containing a polytetrafluoroethylene lining, fully reacting at the high temperature of 120-200 ℃, drying, taking out, and removing excessive reaction solvent to obtain antibacterial MOFs particles;
s20 gauze activation treatment: soaking medical gauze in a sodium hydroxide solution with the mass concentration of 10% -25%, taking out after full infiltration, drying, washing and drying the medical gauze to prepare carboxymethylated medical gauze;
s30, preparing medical antibacterial gauze, namely dissolving the antibacterial MOFs particles obtained in S10 in a DMF (dimethyl formamide) organic solvent with the mass concentration of 40-80% to obtain an MOFs solution, and soaking the carboxymethylated medical gauze obtained in S20 in the MOFs solution; taking out after full infiltration, washing with distilled water and drying; repeating the preparation process in the step S30 for multiple times to obtain the medical antibacterial gauze adhered with the antibacterial coating;
wherein the MOFs precursor solution consists of a metal source, an organic ligand and a solvent; the metal source is zinc nitrate hexahydrate and/or cerium nitrate hexahydrate; the organic ligand is one or a combination of more of 2-methylimidazole, 2-amino isophthalic acid, 2, 3-dihydroxy terephthalic acid and 2-aminobenzimidazole; the solvent is a combination of methanol, DMF, silver nitrate, citric acid and antibiotics; the mass ratio of the metal source, the organic ligand and the solvent in the precursor solution of the MOFs is 1 (1-60) to 20-100.
2. The method for preparing medical antibacterial gauze according to claim 1, wherein the MOFs precursor solution in step S10 is prepared according to the following method: weighing the zinc nitrate hexahydrate and the cerium nitrate hexahydrate in a mass ratio of 1 (1-2); adding 2-methylimidazole into zinc nitrate hexahydrate, pouring into a methanol solution, and dissolving to obtain a solution A; the mass ratio of the zinc nitrate hexahydrate to the 2-methylimidazole is 20: 1; the mass ratio of the zinc nitrate hexahydrate to the methanol solution is 40: 1;
adding 2-amino isophthalic acid with equal mass into cerium nitrate hexahydrate, and pouring into a DMF solution for dissolving; the mass ratio of the cerous nitrate hexahydrate to the DMF solution is (25-50): 1, marking as solution B;
respectively and fully stirring the solution A and the solution B, and then mixing to obtain a solution C;
slowly dropwise adding a silver nitrate solution into the solution C, finally adding citric acid, and fully stirring to obtain the MOFs precursor solution; the mass ratio of the silver nitrate to the zinc nitrate hexahydrate is 1: 85 parts by weight; the mass ratio of the citric acid to the zinc nitrate hexahydrate is 1: 2.
3. The method for preparing medical antibacterial gauze according to claim 1, wherein the MOFs precursor solution in step S10 is prepared according to the following method: weighing the zinc nitrate hexahydrate and the cerium nitrate hexahydrate in a mass ratio of 1: 1; adding 2-methylimidazole into zinc nitrate hexahydrate, pouring into a methanol solution, and dissolving to obtain a solution A'; the mass ratio of the zinc nitrate hexahydrate to the 2-methylimidazole is 20: 1; the mass ratio of the zinc nitrate hexahydrate to the methanol solution is 40: 1;
adding 2-amino isophthalic acid with equal mass into cerium nitrate hexahydrate, and pouring into a DMF solution for dissolving; the mass ratio of the cerous nitrate hexahydrate to the DMF solution is 50: 1, denoted as solution B';
fully stirring the solution A and the solution B respectively and then mixing to obtain a solution C';
slowly dripping antibiotics into the solution C', and fully stirring to obtain the MOFs precursor solution; the mass ratio of the antibiotic to the zinc nitrate hexahydrate is 1: (1-2).
4. The method for preparing medical antibacterial gauze according to claim 1, wherein the MOFs precursor solution in step S10 is prepared according to the following method: weighing 1mmol of cerous nitrate hexahydrate; adding 2, 3-dihydroxyterephthalic acid with equal mass into the cerium nitrate hexahydrate, pouring into the DMF solution, dissolving and stirring, wherein the mass ratio of the cerium nitrate hexahydrate to the DMF solution is 25: 1; denoted as solution A ";
slowly dropwise adding a silver nitrate solution into the solution A', finally adding citric acid, and fully stirring to obtain the MOFs precursor solution; the mass ratio of the silver nitrate to the cerium nitrate hexahydrate is 1: 85 parts by weight; the mass ratio of the citric acid to the cerous nitrate hexahydrate is 1: 2.
5. The method for preparing medical antibacterial gauze according to claim 1, wherein the MOFs precursor solution in step S10 is prepared according to the following method: weighing 1mmol of zinc nitrate hexahydrate; adding 2-aminobenzimidazole into the zinc nitrate hexahydrate, and then pouring into the DMF solution for dissolving and stirring; the mass ratio of the zinc nitrate hexahydrate to the 2-aminobenzimidazole is 20: 1; the mass ratio of the cerous nitrate hexahydrate to the DMF solution is 25: 1; denoted solution a' ″;
slowly dropwise adding a silver nitrate solution into the solution A', finally adding citric acid, and fully stirring to obtain the MOFs precursor solution; the mass ratio of the silver nitrate to the cerium nitrate hexahydrate is 1: 85 parts by weight; the mass ratio of the citric acid to the cerous nitrate hexahydrate is 1: 2.
6. The method for preparing medical antibacterial gauze according to any one of claims 1 to 5, wherein in the step S20, the MOFs particles are washed 3-5 times with DMF and methanol to remove excess reaction solvent on the MOFs.
7. The method for preparing medical antibacterial gauze according to claim 6, wherein in the step S30, the medical gauze is soaked in the sodium hydroxide solution for 1-2h, pre-dried at 60-90 ℃, washed for 5-10 times, and then dried at 120-150 ℃ for 1-5min to obtain the carboxymethylated medical gauze.
8. The method for preparing medical antibacterial gauze according to claim 6, wherein the antibiotic comprises one or more of vancomycin, fusidic acid, clindamycin, benzathine, azithromycin and ciprofloxacin.
9. The medical antibacterial gauze prepared by the method for preparing the medical antibacterial gauze according to claim 1, wherein the medical antibacterial gauze comprises common non-oily medical gauze and an antibacterial coating adhered to the medical gauze; the antibacterial coating is prepared by soaking and washing MOFs solution; the MOFs solution comprises N, N-dimethylformamide, polyvinylpyrrolidone and MOFs particles; the MOFs solution comprises the following components in percentage by mass: polyvinylpyrrolidone: MOFs particles are (5-20), (10-15) and (5-15); the MOFs particles are prepared by mixing and stirring various solutions of antibiotics, silver nitrate solution, cerium nitrate hexahydrate, zinc nitrate hexahydrate, 2-methylimidazole, 2-amino isophthalic acid or 2, 3-dihydroxy terephthalic acid and citric acid, and drying, washing and drying again for multiple times.
10. The medical antibacterial gauze according to claim 9, wherein the amount ratio of the antibiotic, silver nitrate solution, cerium nitrate hexahydrate, zinc nitrate hexahydrate, 2-methylimidazole, 2-aminoisophthalic acid and citric acid in the MOFs particles is (1-3): 1-5): 3-10): 25-100): 1-3): 3-5.
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