First aid fixation material capable of releasing antibacterial gas in a directional manner and method for manufacturing the same
Patent Information
- Application Number
- CN202410106593.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-01-25
- Publication Date
- 2026-09-08
- Estimated Expiration
- 2044-01-25
AI Technical Summary
[0004]本发明的目的是提供可定向释放抗菌气体的急救固定材料制备方法,解决了现有技术中存在的抗菌气体无法定向释放导致抗菌效果不足的问题
[0027] The beneficial effects of this invention are as follows: This invention provides an emergency fixation material capable of directionally releasing antibacterial gas. It generates NO gas in response to near-infrared light, producing a broad-spectrum antibacterial effect upon release at the wound site. The composite positively charged ferroelectric material allows for the spontaneous formation of an endogenous electric field between the fixation material and the negatively charged contaminated wound. Because NO possesses a dipole moment aligned with the field lines, the gas experiences force in the same direction as the electric field, enabling the directional release of NO onto the wound surface. This avoids insufficient effective antibacterial concentration due to random diffusion of NO in three-dimensional space, thus improving the antibacterial effect. Controlling the content and polarization degree of the ferroelectric material controls the intensity of the endogenous electric field, thereby controlling the gas-targeted release cycle and maintaining the NO gas-targeted release time during the emergency transport period (24-72 hours), ensuring the fixation material has a sustained broad-spectrum antibacterial effect. The preparation method of this invention's emergency fixation material involves calcination and polarization to prepare sodium niobate ceramic powder with ferroelectric properties. Furthermore, polydopamine is modified onto the surface of sodium niobate using alkaline self-polymerization technology to enhance the ferroelectric properties of sodium niobate.
Abstract
Description
Technical Field
[0001] This invention belongs to the field of pharmaceutical technology, and relates to a method for preparing an emergency fixation material that can release antibacterial gas in a targeted manner, as well as the material obtained by the above preparation method. Background Technology
[0002] Immobilization is an essential first aid measure after trauma. Ideal immobilization materials should not only stabilize the limb but also provide broad-spectrum antibacterial protection for open wounds, preventing irreversible damage such as wound contamination, infection, tissue suppuration, and organ failure caused by various bacteria. Therefore, endowing immobilization materials with broad-spectrum antibacterial properties is particularly important. Gas antibacterial therapy is a novel antibacterial method that has emerged in recent years as an alternative to antibiotics and metal ions. Gas molecules can disperse biofilms, kill bacteria, avoid the development of drug resistance, and do not cause toxicity to wound tissue. Introducing gas into immobilization materials can achieve broad-spectrum antibacterial protection at the wound site. However, uncontrolled and random diffusion of gas will result in insufficient gas concentration reaching the wound surface, thus limiting the antibacterial effect. Therefore, forcing the gas to be released in a targeted manner is a key means and a technical challenge to improve the antibacterial effect of immobilization materials.
[0003] Chinese invention patent "A Nanoparticle Based on Multi-Component Dynamic Covalent Chemical Assembly and Its Preparation Method and Application" (Announcement No.: CN115252791B, Announcement Date: 2023.08.11) discloses a nanoparticle that uses nitric oxide gas for antibacterial purposes, capable of treating bacterial infections. However, this nanoparticle still cannot achieve directional release of gas molecules. Chinese invention patent "A Nanofiber Antibacterial Dressing and Its Preparation Method" (Announcement No.: CN114177342B, Announcement Date: 2023.09.20) designs and synthesizes a nanocomposite film with photodynamic therapy and synergistic antibacterial effects of nitric oxide. Under blue light irradiation, it can release ROS-NO, producing a highly efficient killing effect on fungi and bacteria. However, it still suffers from the drawback of the inability to directionally release the antibacterial gas. Summary of the Invention
[0004] The purpose of this invention is to provide a method for preparing an emergency fixation material that can release antibacterial gas in a directional manner, thereby solving the problem of insufficient antibacterial effect caused by the inability to release antibacterial gas in a directional manner in the prior art.
[0005] The technical solution adopted in this invention is a method for preparing an emergency fixation material capable of directionally releasing antibacterial gas, comprising the following steps:
[0006] Step 1: Prepare L-Arg@Microsphere (microspheres loaded with L-arginine);
[0007] Step 2: Mix L-Arg@Microsphere, initiator, sodium bicarbonate, and CA (citric acid) to obtain component 1 of the emergency external fixation material;
[0008] Step 3: Mix MMA (methyl methacrylate monomer), N,N-dimethyl-p-toluidine, and hydroquinone to obtain emergency external fixation material composition 2;
[0009] Step 4: Mix component 1 and component 2 of the emergency external fixation material to obtain the emergency fixation material.
[0010] The invention is further characterized by:
[0011] Step 1 specifically includes the following steps:
[0012] Step 1.1: Disperse KNN (sodium niobate ferroelectric ceramic powder) and DA (dopamine) in buffer solution and polymerize to obtain PDA@KNN (polydopamine-modified KNN particles);
[0013] Step 1.2: After mixing HEMA (hydroxyethyl methacrylate) and MMA (methyl methacrylate) monomers, MBA (methylene bisacrylamide), PVP (polyvinylpyrrolidone), PDA@KNN, and AIBN (azobisisobutyronitrile) are added to the mixture. Then, a water-ethanol mixture is added, filtered, and dried to obtain PDA@KNN composite hydroxyethyl methacrylate-methyl methacrylate copolymer microspheres.
[0014] Step 1.3: Immerse the PDA@KNN composite hydroxyethyl methacrylate-methyl methacrylate copolymer microspheres in L-Arg (L-arginine) and let them stand. Then, after centrifugation and drying, L-Arg@Microsphere is obtained.
[0015] The preparation method of KNN is as follows: potassium carbonate, sodium carbonate and niobium oxide powder are ball-milled and mixed, then calcined, ground and sieved to obtain KNN;
[0016] By polarizing the KNN, a KNN with a positive surface potential is obtained.
[0017] The mass ratio of potassium carbonate, sodium carbonate, and niobium oxide is 0.5:0.5:1 according to the atomic molar ratio of K, Na, and Nb. The calcination temperature is 750-1000℃ and the calcination time is 2-5h. The polarization voltage is 3-5kV and the polarization time is 15-30min.
[0018] In step 1.1, the weight ratio of KNN to DA is 10–15:0.5–1, and the pH of the buffer solution is 10–11.
[0019] Step 1.2 is as follows: After mixing HEMA and MMA monomers, MBA, PVP, and PDA@KNN are added to the mixture. The mixture is stirred under an inert atmosphere. After stirring, AIBN is added, and a water-ethanol mixture is added and heated and stirred. After stirring, the mixture is vacuum filtered and freeze-dried to obtain PDA@KNN composite hydroxyethyl methacrylate-methyl methacrylate copolymer microspheres.
[0020] In step 1.2, the molar ratio of HEMA and MMA monomers is 0.1–0.5, MBA is 1–5% of the total monomer mass, PVP is 2–8% of the total monomer mass, and the mass of PDA@KNN is 0.01–0.1 g. The first stirring temperature is 30–40℃, and the stirring time is 30–60 min. In step 1.2, AIBN is 1–5% of the total monomer mass, the volume ratio of water to ethanol is 20–50:1, the second stirring temperature is 70–80℃, and the stirring time is 3–5 h.
[0021] The L-Arg solution concentration is 0.5–1.5 mg / ml, the mass of PDA@KNN composite hydroxyethyl methacrylate-methyl methacrylate copolymer microspheres soaked in L-Arg is 5–10 g, and the standing time is 1–5 h.
[0022] In step 2, the mass percentages of L-Arg@Microsphere, initiator, sodium bicarbonate, and CA are: 77.75–89.9% L-Arg@Microsphere, 5–10% CA, 5–10% NaHCO3, and 0.1–0.25% initiator. In step 3, the mass ratio of MMA, N,N-dimethyl-p-toluidine, and hydroquinone is 96.5–99.5:0.4–3:0.1–0.5. In step 4, the solid-liquid ratio of component 1 and component 2 of the emergency external fixation material is 1–2 g / ml.
[0023] Another object of the present invention is to provide an emergency fixation material that can release antibacterial gas in a targeted manner.
[0024] Another technical solution adopted in this invention is an emergency fixation material that can release antibacterial gas in a directional manner, comprising emergency external fixation material component 1 and emergency external fixation material component 2, wherein the solid-liquid ratio of emergency external fixation material component 1 and emergency external fixation material component 2 is 1-2 g / ml;
[0025] The emergency external fixation material consists of the following components by mass percentage: 77.75–89.9% L-Arg@Microsphere, 5–10% CA, 5–10% NaHCO3, and 0.1–0.25% initiator, with the total mass percentage of the above components being 100%.
[0026] The emergency external fixation material consists of MMA, N,N-dimethyl-p-toluidine, and hydroquinone, with a mass ratio of 96.5–99.5:0.4–3:0.1–0.5.
[0027] The beneficial effects of this invention are as follows: This invention provides an emergency fixation material capable of directionally releasing antibacterial gas. It generates NO gas in response to near-infrared light, producing a broad-spectrum antibacterial effect upon release at the wound site. The composite positively charged ferroelectric material allows for the spontaneous formation of an endogenous electric field between the fixation material and the negatively charged contaminated wound. Because NO possesses a dipole moment aligned with the field lines, the gas experiences force in the same direction as the electric field, enabling the directional release of NO onto the wound surface. This avoids insufficient effective antibacterial concentration due to random diffusion of NO in three-dimensional space, thus improving the antibacterial effect. Controlling the content and polarization degree of the ferroelectric material controls the intensity of the endogenous electric field, thereby controlling the gas-targeted release cycle and maintaining the NO gas-targeted release time during the emergency transport period (24-72 hours), ensuring the fixation material has a sustained broad-spectrum antibacterial effect. The preparation method of this invention's emergency fixation material involves calcination and polarization to prepare sodium niobate ceramic powder with ferroelectric properties. Furthermore, polydopamine is modified onto the surface of sodium niobate using alkaline self-polymerization technology to enhance the ferroelectric properties of sodium niobate. Detailed Implementation
[0028] The present invention will now be described in detail with reference to specific embodiments.
[0029] A method for preparing an emergency fixation material capable of directional release of antibacterial gas includes the following steps:
[0030] Step 1: Prepare L-Arg@Microsphere;
[0031] Step 1.1: Potassium carbonate, sodium carbonate, and niobium oxide powders are ball-milled and mixed according to the atomic molar ratio of K, Na, and Nb of 0.5:0.5:1, then dried. After calcination at 750-1000℃ for 2-5 hours, the mixture is cooled, ground, and sieved to obtain KNN. The KNN is then polarized at a voltage of 3-5kV for 15-30 minutes to obtain KNN with a positive surface potential.
[0032] KNN and DA with positive surface potential were dispersed in an alkaline buffer solution with pH 10-11 at a weight ratio of 10-15:0.5-1 and reacted at room temperature with stirring for a period of time. In the alkaline environment, DA was allowed to self-polymerize on the surface of KNN. After centrifugation and drying, PDA@KNN was obtained.
[0033] Step 1.2: Mix HEMA and MMA monomers at a molar ratio of 0.1-0.5 in a three-necked flask, add 1-5% MBA, 2-8% PVP, and 0.01-0.1g PDA@KNN by mass of total monomers, and stir at 30-40℃ for 30-60 minutes under an inert atmosphere. Then add 1-5% AIBN by mass of total monomers and a water-ethanol mixture with a volume ratio of 20-50:1. Stir at 70-80℃ for 3-5 hours. After stirring, vacuum filter and freeze dry to obtain PDA@KNN composite hydroxyethyl methacrylate-methyl methacrylate copolymer microspheres (hereinafter referred to as microspheres).
[0034] Step 1.3: Soak 5-10g of microspheres in L-Arg at a concentration of 0.5-1.5mg / ml and let stand for 1-5 hours. Then, centrifuge and dry to obtain L-Arg@Microsphere.
[0035] Step 2: Mix L-Arg@Microsphere, initiator, sodium bicarbonate, and CA in the following mass percentages: 77.75-89.9% L-Arg@Microsphere, 5-10% CA, 5-10% NaHCO3, and 0.1-0.25% initiator to obtain component 1 of the emergency external fixation material.
[0036] Step 3: Mix MMA, N,N-dimethyl-p-toluidine, and hydroquinone in a mass ratio of 96.5–99.5:0.4–3:0.1–0.5 to obtain emergency external fixation material composition 2;
[0037] Step 4: Mix and stir the components 1 and 2 of the emergency external fixation material at a solid-liquid ratio of 1-2 g / ml to obtain the emergency fixation material. When using, apply the mixture to the open wound site. After the reaction between components 1 and 2 is complete, further fixation of the wound site can be achieved.
[0038] An emergency fixation material capable of releasing antibacterial gas in a targeted manner, comprising emergency external fixation material component 1 and emergency external fixation material component 2, wherein the solid-liquid ratio of emergency external fixation material component 1 and emergency external fixation material component 2 is 1-2 g / ml;
[0039] The emergency external fixation material consists of the following components by mass percentage: 77.75–89.9% L-Arg@Microsphere, 5–10% CA, 5–10% NaHCO3, and 0.1–0.25% initiator, with the total mass percentage of the above components being 100%.
[0040] The emergency external fixation material consists of MMA, N,N-dimethyl-p-toluidine, and hydroquinone, with a mass ratio of 96.5–99.5:0.4–3:0.1–0.5.
[0041] Through the above methods, this invention provides an emergency fixation material capable of directionally releasing antibacterial gas. It generates NO gas in response to near-infrared light, producing a broad-spectrum antibacterial effect upon release at the wound site. The composite positively charged ferroelectric material allows for the spontaneous formation of an endogenous electric field between the fixation material and the negatively charged contaminated wound. Because NO possesses a dipole moment aligned with the field lines, the gas experiences force in the same direction as the electric field, enabling the directional release of NO onto the wound surface. This avoids insufficient effective antibacterial concentration due to irregular diffusion of NO in three-dimensional space, thus improving the antibacterial effect. By controlling the content and polarization of the ferroelectric material, the strength of the endogenous electric field is controlled, thereby controlling the gas's targeted release cycle. This maintains the NO gas's targeted release time within the emergency transport period (24-72 hours), ensuring the fixation material has a sustained broad-spectrum antibacterial effect. This invention solves the technical problem of insufficient antibacterial effect caused by the inability to directionally release antibacterial gas, and the prepared fixation material has promising application prospects in trauma emergency fixation. This invention discloses a method for preparing an emergency fixation material capable of directional release of antibacterial gas. The method employs calcination and polarization to prepare sodium niobate ceramic powder with ferroelectric properties, and then modifies the surface of sodium niobate with polydopamine using alkaline environment self-polymerization technology to improve the ferroelectric properties of sodium niobate. This method yields an emergency fixation material capable of directional release of antibacterial gas.
[0042] Example 1
[0043] A method for preparing an emergency fixation material capable of directional release of antibacterial gas includes the following steps:
[0044] Step 1: Potassium carbonate, sodium carbonate and niobium oxide powders were ball-milled and mixed according to the atomic molar ratio of K, Na and Nb of 0.5:0.5:1, and then dried. After calcination at 750℃ for 2 hours, the mixture was cooled, ground and sieved to obtain KNN. KNN was then polarized at 5kV for 15 minutes to obtain KNN with a positive surface potential.
[0045] KNN and DA with positive surface potential were dispersed in 100 ml of Tris at pH 10 at a weight ratio of 10:0.5. The mixture was reacted at room temperature with stirring for 1 h. After centrifugation and drying, PDA@KNN was obtained.
[0046] HEMA and MMA monomers were mixed in a three-necked flask at a molar ratio of 0.5. 1% MBA, 2% PVP, and 0.1g PDA@KNN were added to the mixture. The mixture was stirred at 30°C for 30 min under an inert atmosphere. Then, 1% AIBN and a water-ethanol mixture with a volume ratio of 20:1 were added. The mixture was stirred at 70°C for 3 h. After stirring, the mixture was vacuum filtered and freeze-dried to obtain microspheres.
[0047] 5g of microspheres were soaked in L-Arg at a concentration of 0.5mg / ml and allowed to stand for 1 hour. After centrifugation and drying, L-Arg@Microsphere was obtained.
[0048] Step 2: Mix 77.75% L-Arg@Microsphere, 10% CA, 10% NaHCO3, and 0.25% BPO (benzoyl peroxide) according to the mass percentage to obtain component 1 of the emergency external fixation material;
[0049] Step 3: Mix MMA, N,N-dimethyl-p-toluidine, and hydroquinone in a mass ratio of 96.5:3:0.5 to obtain the emergency external fixation material composition 2;
[0050] Step 4: Mix and stir the components 1 and 2 of the emergency external fixation material at a solid-liquid ratio of 1g / ml to obtain the emergency fixation material. When using, apply the mixture to the open wound site. After the reaction between components 1 and 2 is complete, further fixation of the wound site can be achieved.
[0051] Example 2
[0052] A method for preparing an emergency fixation material capable of directional release of antibacterial gas includes the following steps:
[0053] Step 1: Potassium carbonate, sodium carbonate and niobium oxide powders were ball-milled and mixed according to the atomic molar ratio of K, Na and Nb of 0.5:0.5:1, and then dried. After calcination at 800℃ for 2 hours, the mixture was cooled, ground and sieved to obtain KNN. KNN was then polarized at 4kV for 20 minutes to obtain KNN with a positive surface potential.
[0054] KNN and DA with positive surface potential were dispersed in 100 ml of Tris at pH 10 at a weight ratio of 15:0.5. The mixture was reacted at room temperature with stirring for 2 h. After centrifugation and drying, PDA@KNN was obtained.
[0055] HEMA and MMA monomers were mixed in a three-necked flask at a molar ratio of 0.5. 3% MBA, 5% PVP, and 0.1 g PDA@KNN were added to the mixture. The mixture was stirred at 40°C for 60 min under an inert atmosphere. Then, 5% AIBN and a water-ethanol mixture with a volume ratio of 30:1 were added. The mixture was stirred at 80°C for 5 h. After stirring, the mixture was vacuum filtered and freeze-dried to obtain microspheres.
[0056] 10g of microspheres were soaked in L-Arg at a concentration of 1mg / ml and allowed to stand for 3 hours. After centrifugation and drying, L-Arg@Microsphere was obtained.
[0057] Step 2: Mix 79.8% L-Arg@Microsphere, 10% CA, 10% NaHCO3 and 0.2% BPO according to the mass percentage to obtain the composition 1 of the emergency external fixation material;
[0058] Step 3: Mix MMA, N,N-dimethyl-p-toluidine, and hydroquinone in a mass ratio of 97.5:3:0.5 to obtain emergency external fixation material composition 2;
[0059] Step 4: Mix and stir the components 1 and 2 of the emergency external fixation material at a solid-liquid ratio of 1.5 g / ml to obtain the emergency fixation material. When using, apply the mixture to the open wound site. After the reaction between components 1 and 2 is complete, further fixation of the wound site can be achieved.
[0060] Example 3
[0061] A method for preparing an emergency fixation material capable of directional release of antibacterial gas includes the following steps:
[0062] Step 1: Prepare L-Arg@Microsphere;
[0063] Step 1.1: Potassium carbonate, sodium carbonate and niobium oxide powders were ball-milled and mixed according to the atomic molar ratio of K, Na and Nb of 0.5:0.5:1, and then dried. After calcination at 850℃ for 2 hours, the mixture was cooled, ground and sieved to obtain KNN. KNN was then polarized at 3kV for 25 minutes to obtain KNN with a positive surface potential.
[0064] KNN and DA with positive surface potential were dispersed in 100 ml of Tris at pH 10 at a weight ratio of 10:0.5. The mixture was reacted at room temperature with stirring for 1 h. After centrifugation and drying, PDA@KNN was obtained.
[0065] Step 1.2: Mix HEMA and MMA monomers at a molar ratio of 0.5 in a three-necked flask, add 3% MBA, 6% PVP, and 0.1g PDA@KNN by mass of total monomers, and stir at 30℃ for 30min under an inert atmosphere. Then add 2% AIBN by mass of total monomers and a water-ethanol mixture with a volume ratio of 40:1. Stir at 70℃ for 3h. After stirring, vacuum filter and freeze dry to obtain microspheres.
[0066] Step 1.3: Soak 10g of microspheres in L-Arg at a concentration of 1.5mg / ml and let stand for 5h. After centrifugation and drying, L-Arg@Microsphere is obtained.
[0067] Step 2: Mix 79.85% L-Arg@Microsphere, 10% CA, 10% NaHCO3 and 0.15% BPO according to the mass percentage to obtain the composition 1 of the emergency external fixation material;
[0068] Step 3: Mix MMA, N,N-dimethyl-p-toluidine, and hydroquinone in a mass ratio of 96.5:3:0.5 to obtain the emergency external fixation material composition 2;
[0069] Step 4: Mix and stir the components 1 and 2 of the emergency external fixation material at a solid-liquid ratio of 2g / ml to obtain the emergency fixation material. When using, apply the mixture to the open wound site. After the reaction between components 1 and 2 is complete, further fixation of the wound site can be achieved.
[0070] Example 4
[0071] A method for preparing an emergency fixation material capable of directional release of antibacterial gas includes the following steps:
[0072] Step 1: Prepare L-Arg@Microsphere;
[0073] Step 1.1: Potassium carbonate, sodium carbonate and niobium oxide powders were ball-milled and mixed according to the atomic molar ratio of K, Na and Nb of 0.5:0.5:1, dried, calcined at 950℃ for 4 hours, cooled, ground and sieved to obtain KNN; KNN was polarized at 5kV for 25 minutes to obtain KNN with a positive surface potential.
[0074] KNN and DA with positive surface potential were dispersed in 100 ml of Tris at pH 11 at a weight ratio of 10:0.8. The mixture was reacted at room temperature with stirring for 1 h. After centrifugation and drying, PDA@KNN was obtained.
[0075] Step 1.2: Mix HEMA and MMA monomers at a molar ratio of 0.5 in a three-necked flask, add 4% MBA, 4% PVP, and 0.1g PDA@KNN by mass of total monomers, stir at 40℃ for 60min under an inert atmosphere, then add 4% AIBN by mass of total monomers, and add a water-ethanol mixture with a volume ratio of 50:1. Stir at 75℃ for 5h. After stirring, vacuum filter and freeze dry to obtain microspheres.
[0076] Step 1.3: Soak 10g of microspheres in L-Arg at a concentration of 1.2mg / ml and let stand for 4h. After centrifugation and drying, L-Arg@Microsphere is obtained.
[0077] Step 2: Mix 87.75% L-Arg@Microsphere, 6% CA, 6% NaHCO3, and 0.25% BPO according to the mass percentage to obtain the composition 1 of the emergency external fixation material;
[0078] Step 3: Mix MMA, N,N-dimethyl-p-toluidine, and hydroquinone in a mass ratio of 97.5:2:0.5 to obtain the emergency external fixation material composition 2;
[0079] Step 4: Mix and stir the components 1 and 2 of the emergency external fixation material at a solid-liquid ratio of 2g / ml to obtain the emergency fixation material. When using, apply the mixture to the open wound site. After the reaction between components 1 and 2 is complete, further fixation of the wound site can be achieved.
[0080] Example 5
[0081] A method for preparing an emergency fixation material capable of directional release of antibacterial gas includes the following steps:
[0082] Step 1: Prepare L-Arg@Microsphere;
[0083] Step 1.1: Potassium carbonate, sodium carbonate and niobium oxide powders were ball-milled and mixed according to the atomic molar ratio of K, Na and Nb of 0.5:0.5:1, dried, calcined at 1000℃ for 5 hours, cooled, ground and sieved to obtain KNN; KNN was polarized at 5kV for 30 minutes to obtain KNN with a positive surface potential.
[0084] KNN and DA with positive surface potential were dispersed in 100 ml of Tris at pH 10 at a weight ratio of 12:0.6. The mixture was reacted at room temperature with stirring for 1 h. After centrifugation and drying, PDA@KNN was obtained.
[0085] Step 1.2: Mix HEMA and MMA monomers at a molar ratio of 0.5 in a three-necked flask, add 5% MBA, 8% PVP, and 0.1g PDA@KNN by mass of total monomers, and stir at 30℃ for 60min under an inert atmosphere. Then add 5% AIBN by mass of total monomers and stir the mixture of water and ethanol (volume ratio 50:1) at 80℃ for 5h. After stirring, vacuum filter and freeze dry to obtain microspheres.
[0086] Step 1.3: Soak 10g of microspheres in L-Arg at a concentration of 1.5mg / ml and let stand for 5h. After centrifugation and drying, L-Arg@Microsphere is obtained.
[0087] Step 2: Mix 89.9% L-Arg@Microsphere, 5% CA, 5% NaHCO3, and 0.1% BPO according to the mass percentage to obtain the composition 1 of the emergency external fixation material;
[0088] Step 3: Mix MMA, N,N-dimethyl-p-toluidine, and hydroquinone in a mass ratio of 99.5:0.4:0.1 to obtain the emergency external fixation material composition 2;
[0089] Step 4: Mix and stir the components 1 and 2 of the emergency external fixation material at a solid-liquid ratio of 2g / ml to obtain the emergency fixation material. When using, apply the mixture to the open wound site. After the reaction between components 1 and 2 is complete, further fixation of the wound site can be achieved.
Claims
1. A method for preparing an emergency fixation material capable of directionally releasing antibacterial gas, characterized in that, Includes the following steps: Step 1: Prepare L-Arg@Microsphere; Step 2: Mix L-Arg@Microsphere, initiator, sodium bicarbonate, and CA to obtain component 1 of the emergency external fixation material; Step 3: Mix MMA, N,N-dimethyl-p-toluidine, and hydroquinone to obtain emergency external fixation material composition 2; Step 4: Mix the emergency external fixation material component 1 and emergency external fixation material component 2 to obtain the emergency fixation material; Step 1 specifically includes the following steps: Step 1.1: Disperse KNN and DA in buffer solution and polymerize to obtain PDA@KNN; Step 1.2: After mixing HEMA and MMA monomers, add MBA, PVP, PDA@KNN and AIBN to the mixture, then add a water-ethanol mixture solution, filter and dry to obtain PDA@KNN composite hydroxyethyl methacrylate-methyl methacrylate copolymer microspheres. Step 1.3: Immerse the PDA@KNN composite hydroxyethyl methacrylate-methyl methacrylate copolymer microspheres in L-Arg and let them stand. Then, centrifuge and dry them to obtain L-Arg@Microsphere. The preparation method of KNN is as follows: potassium carbonate, sodium carbonate and niobium oxide powder are ball-milled and mixed, then calcined, ground and sieved to obtain KNN; The KNN is polarized to obtain a KNN with a positive surface potential; Step 1.2 is as follows: After mixing HEMA and MMA monomers, MBA, PVP, and PDA@KNN are added to the mixture. The mixture is stirred under an inert atmosphere. After stirring, AIBN is added, and a water-ethanol mixture is added and heated and stirred. After stirring, the mixture is vacuum filtered and freeze-dried to obtain PDA@KNN composite hydroxyethyl methacrylate-methyl methacrylate copolymer microspheres.
2. The method for preparing the emergency fixation material capable of directional release of antibacterial gas as described in claim 1, characterized in that, The mass ratio of potassium carbonate, sodium carbonate, and niobium oxide is 0.5:0.5:1 (K, Na, Nb atomic molar ratio), the calcination temperature is 750-1000℃, and the calcination time is 2-5h; the polarization voltage is 3-5kV, and the polarization time is 15-30min.
3. The method for preparing the emergency fixation material capable of directional release of antibacterial gas as described in claim 1, characterized in that, The weight ratio of KNN to DA in step 1.1 is 10~15:0.5~1, and the pH of the buffer solution is 10~11.
4. The method for preparing the emergency fixation material capable of directionally releasing antibacterial gas as described in claim 1, characterized in that, In step 1.2, the molar ratio of HEMA and MMA monomers is 0.1~0.5, the MBA is 1~5% of the total monomer mass, the PVP is 2~8% of the total monomer mass, and the PDA@KNN is 0.01~0.1g. The first stirring temperature is 30~40℃, and the stirring time is 30~60min. The AIBN is 1~5% of the total monomer mass, the volume ratio of water to ethanol is 20~50:1ml, the second stirring temperature is 70~80℃, and the stirring time is 3~5h.
5. The method for preparing the emergency fixation material capable of directional release of antibacterial gas as described in claim 1, characterized in that, The L-Arg solution concentration is 0.5~1.5mg / ml, the mass of PDA@KNN composite hydroxyethyl methacrylate-methyl methacrylate copolymer microspheres soaked in L-Arg is 5~10g, and the standing time is 1-5h.
6. The method for preparing the emergency fixation material capable of directional release of antibacterial gas as described in claim 1, characterized in that, In step 2, the L-Arg@Microsphere, initiator, sodium bicarbonate, and CA are present in the following mass percentages: 77.75-89.9% L-Arg@Microsphere, 5-10% CA, 5-10% NaHCO3, and 0.1-0.25% initiator. In step 3, the mass ratio of MMA, N,N-dimethyl-p-toluidine, and hydroquinone is 96.5-99.5:0.4-3:0.1-0.
5. In step 4, the solid-liquid ratio of component 1 and component 2 of the emergency external fixation material is 1-2 g / ml.
7. The emergency immobilization material capable of directional release of antibacterial gas as described in claim 1, characterized in that, It includes emergency external fixation material component 1 and emergency external fixation material component 2, wherein the solid-liquid ratio of emergency external fixation material component 1 and emergency external fixation material component 2 is 1~2g / ml; The emergency external fixation material composition 1 comprises the following components by mass percentage: 77.75~89.9% L-Arg@Microsphere, 5~10% CA, 5~10% NaHCO3, and 0.1~0.25% initiator, with the total mass percentage of the above components being 100%. The emergency external fixation material 2 comprises MMA, N,N-dimethyl-p-toluidine, and hydroquinone, with a mass ratio of 96.5~99.5:0.4~3:0.1~0.5.
Citation Information
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