CN117138092A - Preparation method of temperature-control moisturizing medical dressing loaded with biocompatible phase-change microcapsules - Google Patents
Preparation method of temperature-control moisturizing medical dressing loaded with biocompatible phase-change microcapsules Download PDFInfo
- Publication number
- CN117138092A CN117138092A CN202311158850.XA CN202311158850A CN117138092A CN 117138092 A CN117138092 A CN 117138092A CN 202311158850 A CN202311158850 A CN 202311158850A CN 117138092 A CN117138092 A CN 117138092A
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- Prior art keywords
- phase
- change
- temperature
- green
- biocompatible
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- 230000003020 moisturizing effect Effects 0.000 title claims abstract description 33
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- 239000000725 suspension Substances 0.000 claims abstract description 61
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000006185 dispersion Substances 0.000 claims abstract description 44
- 239000008367 deionised water Substances 0.000 claims abstract description 42
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- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims abstract description 21
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims abstract description 21
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- LJKMCTWPOSTJHB-UHFFFAOYSA-N [Na].C(=CC1=CC=CC=C1)/C/1=C/C(=O)OC1=O Chemical compound [Na].C(=CC1=CC=CC=C1)/C/1=C/C(=O)OC1=O LJKMCTWPOSTJHB-UHFFFAOYSA-N 0.000 claims description 7
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- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
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- FZWBNHMXJMCXLU-BLAUPYHCSA-N isomaltotriose Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@@H](OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O)O1 FZWBNHMXJMCXLU-BLAUPYHCSA-N 0.000 claims description 2
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Classifications
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Public Health (AREA)
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Abstract
The invention discloses a preparation method of a temperature-controlled moisturizing medical dressing loaded with biocompatible phase-change microcapsules, which comprises the steps of preparing a phase-change microcapsule suspension by using the biocompatible phase-change microcapsules and a surfactant solution; the dextran-based gel is prepared from dextran and sodium polyacrylate which are composite framework materials, sodium carboxymethyl cellulose which is a thickener, dihydroxyaluminum which is a cross-linking agent, glycerin which is a humectant, propylene glycol and deionized water; preparing a green compress powder solution from green compress powder, tartaric acid and deionized water; and three-dimensionally printing the phase-change microcapsule suspension, the glucan-based gel and the green application dispersion solution through a microfluidic device to form the temperature-control moisturizing medical dressing loaded with the biocompatible phase-change microcapsule and having a three-layer structure of a drug release layer, a temperature control layer and a moisturizing layer. The dressing prepared by the invention has good biocompatibility, chemical property stability, better thermodynamic property and mechanical property and low production cost.
Description
Technical Field
The invention belongs to the technical field of medical dressing materials, and particularly relates to a preparation method of a temperature-control and moisture-preservation medical dressing loaded with biocompatible phase-change microcapsules.
Background
The medical wound dressing plays a vital role in the field of promoting chronic wound recovery, and can effectively promote the growth of wound fibroblasts and accelerate the wound healing speed by closely attaching to local wound positions, absorbing exudates, resisting inflammation and avoiding external environmental stimulation. At the same time, the local temperature of the wound is also an important factor affecting its recovery, and neutrophil, fibrinogen and human keratinocyte activities are reduced when the temperature is lower than 33 ℃, thereby causing delayed healing, and the local temperature is diffused to the peripheral part when the temperature is higher than 38 ℃ to stimulate inflammation. Therefore, it is necessary to study a medical multifunctional wound dressing capable of simultaneously performing body temperature regulation. At present, adding phase change microcapsules into dressing is a main method for realizing temperature control effect, but related researches are still less.
Phase change microcapsules are a product of application of encapsulated microencapsulation technology to phase change materials. When the phase change material is directly added into the dressing, the phase change material can leak and run off in the phase change process, so that the temperature regulating capability is greatly weakened. The phase-change microcapsule can better solve the problem, the microcapsule has a complete shell-core structure, the phase-change material is used as a core material, and the core material is coated by an organic high-molecular polymer or an inorganic material and the like as a wall material to prevent the leakage of the core material and ensure that the microcapsule has certain mechanical strength. However, in the process of adding the phase-change microcapsule to a medical dressing, leakage of a small amount of core material still cannot be avoided, so that both the capsule wall material and the core material can be in direct contact with a wound. Therefore, in order to ensure safety, the added phase-change microcapsule should have biocompatibility while the medical wound dressing matrix meets the biocompatibility.
Patent publication No. CN 106400199B discloses a phase-change temperature-regulating microcapsule material, a preparation method thereof and dressing prepared by the same, wherein the phase-change temperature-regulating microcapsule material is prepared from phase-change microcapsules and chitosan; the phase-change microcapsule has the effects of phase-change temperature adjustment, and the chitosan has the antibacterial effect. The patent with publication number CN 115192763A discloses a multifunctional temperature-regulating wound dressing, a preparation method and application thereof, which consists of a phase-change heat-preserving layer and a long-acting antibacterial layer, wherein the phase-change temperature-regulating layer of the temperature-regulating wound dressing is prepared by chitosan, phase-change microcapsules and enzyme-soluble collagen; the long-acting antibacterial layer is prepared by utilizing polycaprolactone and ceftazidime and adopting an electrostatic spinning technology. According to the scheme, temperature control and antibacterial of wound auxiliary materials are achieved by adding the phase-change microcapsules, but the wall materials and the core materials of the phase-change microcapsules cannot meet biocompatibility, the phase-change enthalpy value is low, the phase-change temperature region cannot be accurately controlled to a body temperature region (33-38 ℃) suitable for wound recovery, and the preparation process of the dressing is complex. .
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a temperature-control moisturizing medical dressing loaded with biocompatible phase-change microcapsules, wherein three-dimensional printing is carried out on phase-change microcapsule suspension, glucan-based gel and green application dispersion solution through a microfluidic device to form a dressing with a three-layer structure of a drug release layer, a temperature control layer and a moisturizing layer; the phase-change microcapsule suspension is prepared from phase-change microcapsules and a surfactant solution, and core materials and wall materials of the phase-change microcapsules have good biocompatibility; the glucan-based gel is prepared from composite framework material glucan, sodium polyacrylate, thickener sodium carboxymethyl cellulose, crosslinking agent dihydroxyaluminum, humectant glycerin, propylene glycol and deionized water; the green compress powder solution is prepared from green compress powder, tartaric acid and deionized water. Finally, the multi-layer temperature-control moisturizing medical dressing loaded with the biocompatible phase-change microcapsules is prepared by asynchronously controlling and printing through a microfluidic device.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a preparation method of a temperature-controlled moisturizing medical dressing loaded with biocompatible phase-change microcapsules comprises the following steps:
step 1: preparing phase-change microcapsule suspension by biocompatible phase-change microcapsule and surfactant solution;
step 2: the dextran-based gel is prepared from dextran and sodium polyacrylate which are composite framework materials, sodium carboxymethyl cellulose which is a thickener, dihydroxyaluminum which is a cross-linking agent, glycerin which is a humectant, propylene glycol and deionized water;
step 3: preparing a green compress powder solution from green compress powder, tartaric acid and deionized water;
step 4: and three-dimensionally printing the phase-change microcapsule suspension, the glucan-based gel and the green application dispersion solution through a microfluidic device to form the temperature-control moisturizing medical dressing loaded with the biocompatible phase-change microcapsule and having a three-layer structure of a drug release layer, a temperature control layer and a moisturizing layer.
In order to optimize the technical scheme, the specific measures adopted further comprise:
the step 1 is to stir and mix the equal mass phase-change microcapsule and the surfactant solution to form a phase-change microcapsule suspension, wherein the preparation method of the biocompatible phase-change microcapsule comprises the following steps:
mixing a cross-linking agent, an initiator, wall material monomer methyl methacrylate and a composite phase change core material, and obtaining an oil phase mixture through ultrasonic oscillation; preparing a surfactant solution as an aqueous phase; mixing the oil phase and the water phase, and emulsifying by a high-speed homogenizer to form an oil-in-water microemulsion; stirring the microemulsion in a water bath environment to initiate polymerization reaction, and finally filtering, washing and drying to obtain the biocompatible phase-change microcapsule.
In the step 1, the mass ratio of the phase-change microcapsules in the phase-change microcapsule suspension is 30% -60%; the mass ratio of the cross-linking agent to the initiator to the wall material monomer methyl methacrylate to the composite phase change core material is 1-2:0.3:7-8:10; wherein the cross-linking agent is one or more of pentaerythritol tetraacrylate, pentaerythritol triacrylate, ethylene glycol dimethacrylate and divinylbenzene; the initiator is one or more of azodiisobutyronitrile, potassium persulfate, ammonium persulfate and benzoyl peroxide; the composite phase-change core material is formed by mixing lauric acid and stearic acid, the mass ratio of the lauric acid to the stearic acid is 7.6-8:2-2.4, and the phase-change temperature area of the mixture is close to the body temperature.
The temperature and duration of the ultrasonic vibration are respectively 45-50 ℃ and 15-25min. The concentration of the surfactant solution is 0.625% -1.000%, and the surfactant is one or more of styrene-maleic anhydride sodium salt, polyvinyl alcohol, polyvinylpyrrolidone, gelatin and sodium dodecyl sulfate. When the oil phase and the water phase are emulsified by a high-speed homogenizer to form the oil-in-water microemulsion, the temperature, the rotating speed and the duration of the emulsification are respectively 45-55 ℃, 3000-6000r/min and 10-15min; when the microemulsion is stirred in a water bath environment to initiate polymerization, the temperature, the rotating speed and the duration of the stirring reaction are respectively 70-80 ℃, 300-500r/min and 5-7h.
Step 2, stirring and mixing glucan, sodium polyacrylate, sodium carboxymethyl cellulose, glycerol, propylene glycol, aluminum glycollate and deionized water, and then centrifugally dispersing to obtain glucan-based gel, wherein the mass ratio of glucan, sodium polyacrylate, sodium carboxymethyl cellulose, glycerol, propylene glycol, aluminum glycollate and deionized water is 1:0.1:0.15:1.25:0.5:0.05:5; the rotational speed and duration of centrifugal dispersion are 6000-8000r/min and 3-5min respectively.
And 3, mixing the green compress powder, the tartaric acid and the deionized water to obtain a green compress powder solution, wherein the mass ratio of the green compress powder to the tartaric acid to the deionized water is 1:0.4:6.
Step 4, taking the phase-change microcapsule suspension, the glucan-based gel and the green dressing dispersion solution prepared in step 1-3 into an injector A, B, C, respectively controlling the flow ratio of the phase-change microcapsule suspension to the glucan-based gel and the green dressing dispersion solution and the jet nozzle to move quickly through a microfluidic device for three-dimensional printing, sequentially forming a medicine release layer, a temperature control layer and a moisture preservation layer, and finally drying in a forced air drying box to obtain the temperature control and moisture preservation medical dressing loaded with the biocompatible phase-change microcapsule; the material of the drug release layer is green compress dispersion solution, microcapsule suspension and dextran-based gel, the material of the temperature control layer is microcapsule suspension and dextran-based gel, and the material of the moisture preservation layer is dextran-based gel.
The microfluidic device comprises a syringe, a syringe pump, a micro-channel, a mixing device and a nozzle; the flow range controlled by the microfluidic device is 30-100 mu L/min; the moving speed of the nozzle of the micro-fluidic device is 2-10mm/s. When the drug release layer is printed, the flow ratio of the phase change microcapsule suspension to the dextran-based gel to the green application dispersion solution is 2-4:3:3; when the temperature control layer is printed, the flow ratio of the phase change microcapsule suspension to the dextran-based gel is 6-8:4, and the flow of the green application dispersion solution is 0; when the moisturizing layer is printed, the needed material is glucan-based gel, and the flow of the phase-change microcapsule suspension and the green application dispersion solution is 0.
The dressing comprises three-dimensional printing of phase-change microcapsule suspension, glucan-based gel and green application dispersion solution through a microfluidic device to form a three-layer structure with a drug release layer, a temperature control layer and a moisture preservation layer; wherein the phase-change microcapsule suspension is prepared from biocompatible phase-change microcapsules and a surfactant solution; the glucan-based gel is prepared from composite framework material glucan, sodium polyacrylate, thickener sodium carboxymethyl cellulose, crosslinking agent dihydroxyaluminum, humectant glycerin, propylene glycol and deionized water; the green compress powder solution is prepared from green compress powder, tartaric acid and deionized water.
The invention has the following beneficial effects:
(1) According to the invention, an organic high polymer material polymethyl methacrylate is coated on the outer side of a composite fatty acid phase change material to obtain a phase change microcapsule with biocompatibility, then a phase change microcapsule suspension is prepared, dextran-based gel and a green application dispersion solution are obtained through pretreatment, finally, flow is regulated and controlled through a microfluidic device, and a three-layer structure medical multifunctional wound dressing containing a drug release layer, a temperature control layer and a moisture preservation layer is prepared, and the prepared dressing has the advantages of good biocompatibility, chemical property stability, no toxicity and harmlessness, and safer use, and is used as a composite phase change material applied to the medical and biological fields, and the biocompatibility of the phase change microcapsule is higher than the phase change heat preservation performance of the phase change microcapsule.
(2) The biocompatible phase change microcapsule prepared by the invention has better thermodynamic property and mechanical property. The solidification and melting temperatures are controlled between 33-38 ℃ of the human body temperature, the phase transition temperature area is close to the body temperature, the low supercooling degree and the high enthalpy value of 124.7J/g are achieved, the rapid response of the low temperature difference is facilitated, and the healing of wounds can be effectively promoted. The biocompatible phase-change microcapsule can also be applied to the fields of food, environment, chemical industry, construction and the like.
(3) The three-layer structure medical wound multifunctional dressing with different performances is prepared by one-step three-dimensional printing, the operation is simple, the production cost is low, the drug release layer has the effects of resisting bacteria, diminishing inflammation, relieving pain and promoting fibroblast growth, the temperature control layer focuses on absorbing heat and realizing accurate temperature regulation, and the moisture preservation layer can provide a continuous moist environment for the wound. The three-dimensional printing method enables the shape of the dressing to be unlimited, components, thickness and the like of each layer can be accurately regulated and controlled through printing flow and moving speed, so that the dressing with an irregular shape is prepared, wounds are tightly attached, and the comfort level of wound attachment is improved.
Drawings
FIG. 1 is a diagram showing the construction of the external appearance of a temperature-controlled moisturizing medical dressing which is a biocompatible phase-change microcapsule;
FIG. 2 is a schematic diagram of a microfluidic device;
FIG. 3 is a SEM (scanning electron microscope) morphology diagram of the biocompatible phase-change microcapsule;
FIG. 4 is a physical diagram of a temperature-controlled moisturizing medical dressing loaded with biocompatible phase-change microcapsules;
fig. 5 is a chart of a DSC differential scanning calorimeter test for biocompatible phase change microcapsules.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Although the steps of the present invention are arranged by reference numerals, the order of the steps is not limited, and the relative order of the steps may be adjusted unless the order of the steps is explicitly stated or the execution of a step requires other steps as a basis. It is to be understood that the term "and/or" as used herein relates to and encompasses any and all possible combinations of one or more of the associated listed items.
As shown in fig. 1, the temperature-controlled moisturizing medical dressing loaded with the biocompatible phase-change microcapsule is formed by three-dimensionally printing a phase-change microcapsule suspension, a glucan-based gel and a green-dressing dispersion solution by a microfluidic device shown in fig. 2, and has a three-layer structure of a medicine release layer, a temperature-controlled layer and a moisturizing layer, and the preparation method comprises the following four steps:
step 1: preparing phase-change microcapsule suspension by biocompatible phase-change microcapsule and surfactant solution;
step 2: the dextran-based gel is prepared from dextran and sodium polyacrylate which are composite framework materials, sodium carboxymethyl cellulose which is a thickener, dihydroxyaluminum which is a cross-linking agent, glycerin which is a humectant, propylene glycol and deionized water;
step 3: preparing a green compress powder solution from green compress powder, tartaric acid and deionized water;
step 4: and three-dimensionally printing the phase-change microcapsule suspension, the glucan-based gel and the green application dispersion solution through a microfluidic device to form the temperature-control moisturizing medical dressing loaded with the biocompatible phase-change microcapsule and having a three-layer structure of a drug release layer, a temperature control layer and a moisturizing layer.
In specific implementation, the step 1 is to stir and mix the equal mass phase-change microcapsule and the surfactant solution to form a phase-change microcapsule suspension, wherein the preparation method of the biocompatible phase-change microcapsule comprises the following steps:
mixing a cross-linking agent, an initiator, wall material monomer methyl methacrylate and a composite phase change core material, and obtaining an oil phase mixture through ultrasonic oscillation; preparing a surfactant solution as an aqueous phase; mixing the oil phase and the water phase, and emulsifying by a high-speed homogenizer to form an oil-in-water (O/W) microemulsion; stirring the microemulsion in a water bath environment to initiate polymerization reaction, and finally filtering, washing and drying to obtain the biocompatible phase-change microcapsule. Fig. 3 shows a SEM scanning electron microscope topography of biocompatible phase-change microcapsules.
The mass ratio of the phase-change microcapsule in the phase-change microcapsule suspension is 30% -60%. The mass ratio of the cross-linking agent to the initiator to the wall material monomer methyl methacrylate to the composite phase change core material is 1-2:0.3:7-8:10; wherein the cross-linking agent is one or more of pentaerythritol tetraacrylate, pentaerythritol triacrylate, ethylene glycol dimethacrylate and divinylbenzene; the initiator is one or more of azodiisobutyronitrile, potassium persulfate, ammonium persulfate and benzoyl peroxide; the composite phase-change core material is formed by mixing lauric acid and stearic acid, the mass ratio of the lauric acid to the stearic acid is 7.6-8:2-2.4, and the phase-change temperature area of the mixture is close to the body temperature. The temperature and duration of the ultrasonic vibration are 45-50 ℃ and 15-25min respectively. The concentration of the surfactant solution is 0.625% -1.000%, and the surfactant is one or more of styrene-maleic anhydride sodium salt, polyvinyl alcohol, polyvinylpyrrolidone, gelatin and sodium dodecyl sulfate. When the oil phase and the water phase are emulsified by a high-speed homogenizer to form an oil-in-water (O/W) microemulsion, the temperature, the rotating speed and the duration of emulsification are respectively 45-55 ℃, 3000-6000r/min and 10-15min; when the microemulsion is stirred in a water bath environment to initiate polymerization, the temperature, the rotating speed and the duration of the stirring reaction are respectively 70-80 ℃, 300-500r/min and 5-7h. The wall material polymethyl methacrylate of the biocompatible microcapsule and the composite phase change core material have good biocompatibility.
In the specific implementation, the step 2 is to stir and mix dextran, sodium polyacrylate, sodium carboxymethylcellulose, glycerol, propylene glycol, aluminum glycollate and deionized water, and then to centrifugally disperse to obtain the dextran-based gel. Wherein the mass ratio of the glucan to the sodium polyacrylate to the sodium carboxymethylcellulose to the glycerol to the propylene glycol to the aluminum glycinate to the deionized water is 1:0.1:0.15:1.25:0.5:0.05:5; the rotational speed and duration of centrifugal dispersion are 6000-8000r/min and 3-5min respectively.
In the specific implementation, the step 3 is to mix the green compress powder, the tartaric acid and the deionized water to obtain a green compress powder solution, wherein the mass ratio of the green compress powder to the tartaric acid to the deionized water is 1:0.4:6.
In specific implementation, the step 4 is to take a certain amount of the phase-change microcapsule suspension liquid, the glucan-based gel and the green application dispersion solution prepared in the step 1-3 into an injector A, B, C, respectively control the flow ratio of the three components and the moving speed of a nozzle through a microfluidic device to perform three-dimensional printing, sequentially form a medicine release layer, a temperature control layer and a moisture preservation layer, and finally dry in a blast drying box to obtain the temperature control and moisture preservation medical dressing loaded with the biocompatible phase-change microcapsule; the material of the drug release layer is green compress dispersion solution, microcapsule suspension and dextran-based gel, the material of the temperature control layer is microcapsule suspension and dextran-based gel, and the material of the moisture preservation layer is dextran-based gel.
As shown in fig. 2, the microfluidic device includes a syringe, a syringe pump, a microchannel, a mixing device, and a nozzle; the flow range controlled by the microfluidic device is 30-100 mu L/min; the moving speed of the nozzle of the micro-fluidic device is 2-10mm/s. When the drug release layer is printed, the flow ratio of the phase change microcapsule suspension to the dextran-based gel to the green application dispersion solution is 2-4:3:3; when the temperature control layer is printed, the flow ratio of the phase change microcapsule suspension to the dextran-based gel is 6-8:4, and the flow of the green application dispersion solution is 0; when the moisturizing layer is printed, the needed material is glucan-based gel, and the flow of the phase-change microcapsule suspension and the green application dispersion solution is 0. The temperature and duration of drying in the forced air drying oven were 40-60℃and 3-5 hours, respectively. Single-layer or multi-layer dressings of any shape can be printed by means of a microfluidic device. Fig. 4 shows a temperature-controlled moisturizing medical dressing physical diagram loaded with biocompatible phase-change microcapsules. Fig. 5 shows a test chart of a DSC differential scanning calorimeter of the biocompatible phase-change microcapsule, and as can be seen from fig. 5, the solidification and melting temperatures are respectively 33 ℃ and 35 ℃, the temperatures are controlled between 33 ℃ and 38 ℃ of the human body, the phase-change temperature zone is close to the body temperature, the temperature has smaller supercooling degree and a high enthalpy value of 124.7J/g, the rapid response of the low temperature difference is facilitated, and the healing of wounds can be effectively promoted.
Example 1
Mixing 1g of pentaerythritol tetraacrylate, 0.3g of azodiisobutyronitrile, 8g of methyl methacrylate, 7.6g of lauric acid and 2.4g of stearic acid, then dispersing for 25 minutes at 45 ℃ in an ultrasonic vibration mode to prepare 150ml of polyvinyl alcohol solution with the mass fraction of 0.66% as a water phase, then mixing the oil phase and the water phase, heating to 50 ℃ and emulsifying for 10-15 minutes at the rate of 6000r/min to form microemulsion, stirring and reacting for 5-7 hours at the rate of 300r/min in a 75-80 ℃ water bath environment, and finally filtering, drying and washing to obtain the biocompatible phase change microcapsule.
9g of phase-change microcapsule and 6g of polyvinyl alcohol solution are stirred and mixed to form phase-change microcapsule suspension, 2g of dextran, 0.2g of sodium polyacrylate, 0.3g of sodium carboxymethyl cellulose, 2.5g of glycerol, 1g of propylene glycol, 0.1 g of aluminum glycollate and 10g of deionized water are stirred and mixed, and then centrifugal dispersion is carried out for 3-5min at the speed of 8000r/min to obtain dextran-based gel, and 1.5g of green compress powder, 0.6g of tartaric acid and 9g of deionized water are uniformly dispersed to obtain green compress powder solution.
Respectively taking 10ml of microcapsule suspension prepared by experiments, dextran-based gel and green application dispersion solution into an injector A, B, C, pushing the microcapsule suspension, the dextran-based gel and the green application dispersion solution simultaneously at a flow rate of 30 mu L/min through a microfluidic device, stopping pushing C after 100min, adjusting the flow rate of A to 70 mu L/min, adjusting the flow rate of B to 40 mu L/min, pushing A and B until A is finished, adjusting the flow rate of B to 100 mu L/min, pushing B until finishing, and finally drying the microcapsule in a blast drying box at 60 ℃ for 3-5h to obtain the temperature-controlled moisturizing medical dressing loaded with the biocompatible phase-change microcapsules.
Example 2
Mixing 2g of pentaerythritol tetraacrylate, 0.3g of azodiisobutyronitrile, 8g of methyl methacrylate, 7.6g of lauric acid and 2.4g of stearic acid, then dispersing for 25 minutes at 45 ℃ in an ultrasonic vibration mode to prepare 150ml of polyvinyl alcohol solution with the mass fraction of 0.66% as a water phase, then mixing the oil phase and the water phase, heating to 50 ℃ and emulsifying for 10-15 minutes at the rate of 6000r/min to form microemulsion, stirring and reacting for 5-7 hours at the rate of 300r/min in a 75-80 ℃ water bath environment, and finally filtering, drying and washing to obtain the biocompatible phase change microcapsule.
Stirring and mixing 12g of phase-change microcapsule and 8g of polyvinyl alcohol solution to form phase-change microcapsule suspension, stirring and mixing 2g of dextran, 0.2g of sodium polyacrylate, 0.3g of sodium carboxymethyl cellulose, 2.5g of glycerol, 1g of propylene glycol, 0.1 g of aluminum glycollate and 10g of deionized water, and then centrifugally dispersing for 3-5min at the speed of 8000r/min to obtain dextran-based gel, and uniformly dispersing 2g of green compress powder, 0.8g of tartaric acid and 12g of deionized water to obtain a green compress powder solution.
Respectively taking 10ml of microcapsule suspension prepared by experiments, dextran-based gel and green application dispersion solution into an injector A, B, C, pushing the microcapsule suspension, the dextran-based gel and the green application dispersion solution simultaneously at a flow rate of 30 mu L/min through a microfluidic device, stopping pushing C after 100min, adjusting the flow rate of A to 70 mu L/min, adjusting the flow rate of B to 40 mu L/min, pushing A and B until A is finished, adjusting the flow rate of B to 100 mu L/min, pushing B until finishing, and finally drying the microcapsule in a blast drying box at 60 ℃ for 3-5h to obtain the temperature-controlled moisturizing medical dressing loaded with the biocompatible phase-change microcapsules.
Example 3
Mixing 1.5g of pentaerythritol tetraacrylate, 0.3g of azodiisobutyronitrile, 8g of methyl methacrylate, 7.6g of lauric acid and 2.4g of stearic acid, then dispersing by ultrasonic vibration at 45 ℃ for 25min to prepare 150ml of styrene-maleic anhydride sodium salt solution with mass fraction of 0.66% as an aqueous phase, then mixing the aqueous phase with the oil phase, heating to 50 ℃ and emulsifying for 10-15min at the rate of 6000r/min to form microemulsion, stirring and reacting for 5-7h at the rate of 300r/min in a water bath environment at 75-80 ℃, and finally filtering, drying and washing to obtain the biocompatible phase change microcapsule.
9g of phase-change microcapsule and 6ml of styrene-maleic anhydride sodium salt solution are stirred and mixed to form phase-change microcapsule suspension, 2g of dextran, 0.2g of sodium polyacrylate, 0.3g of sodium carboxymethyl cellulose, 2.5g of glycerol, 1g of propylene glycol, 0.1 g of dihydroxyaluminum and 10g of deionized water are stirred and mixed, and then centrifugal dispersion is carried out for 3-5min at the speed of 8000r/min to obtain dextran-based gel, and 1.5g of green compress powder, 0.6g of tartaric acid and 9g of deionized water are uniformly dispersed to obtain a green compress powder solution.
Respectively taking 10ml of microcapsule suspension prepared by experiments, dextran-based gel and green application dispersion solution into an injector A, B, C, pushing the microcapsule suspension, the dextran-based gel and the green application dispersion solution simultaneously at a flow rate of 30 mu L/min through a microfluidic device, stopping pushing C after 100min, adjusting the flow rate of A to 70 mu L/min, adjusting the flow rate of B to 40 mu L/min, pushing A and B until A is finished, adjusting the flow rate of B to 100 mu L/min, pushing B until finishing, and finally drying the microcapsule in a blast drying box at 60 ℃ for 3-5h to obtain the temperature-controlled moisturizing medical dressing loaded with the biocompatible phase-change microcapsules.
Example 4
Mixing 1.5g of pentaerythritol tetraacrylate, 0.3g of azodiisobutyronitrile, 7g of methyl methacrylate, 7.6g of lauric acid and 2.4g of stearic acid, then dispersing by ultrasonic vibration at 45 ℃ for 25min to obtain oil phases, respectively preparing 150ml of sodium dodecyl sulfate/gelatin solution (each accounting for 50%) with the mass fraction of 0.66% as water phases, then mixing the oil phases with the water phases, heating to 50 ℃ and emulsifying at the rate of 6000r/min for 10-15min to form microemulsion, stirring at the rate of 300r/min in a water bath environment at 75-80 ℃ for reacting for 5-7h, and finally filtering, drying and washing to obtain the biocompatible phase-change microcapsule.
Stirring and mixing 12g of phase-change microcapsule with 8g of sodium dodecyl sulfate/gelatin solution to form phase-change microcapsule suspension, stirring and mixing 2g of dextran, 0.2g of sodium polyacrylate, 0.3g of sodium carboxymethyl cellulose, 2.5g of glycerol, 1g of propylene glycol, 0.1 g of dihydroxyaluminum and 10g of deionized water, and then centrifugally dispersing for 3-5min at the speed of 8000r/min to obtain dextran-based gel, and uniformly dispersing 2g of green compress powder, 0.8g of tartaric acid and 12g of deionized water to obtain a green compress powder solution.
Respectively taking 10ml of microcapsule suspension prepared by experiments, dextran-based gel and green application dispersion solution into an injector A, B, C, pushing the microcapsule suspension, the dextran-based gel and the green application dispersion solution simultaneously at a flow rate of 30 mu L/min through a microfluidic device, stopping pushing C after 100min, adjusting the flow rate of A to 70 mu L/min, simultaneously pushing A and B until A is finished, adjusting the flow rate of B to 100 mu L/min, pushing B until finishing, and finally drying the microcapsule-loaded temperature-controlled moisturizing medical dressing at 60 ℃ in a blast drying box for 3-5h.
Example 5
Mixing 1g of pentaerythritol tetraacrylate, 0.3g of azodiisobutyronitrile, 8g of methyl methacrylate, 7.6g of lauric acid and 2.4g of stearic acid, then dispersing for 25 minutes at 45 ℃ in an ultrasonic vibration mode to prepare 150ml of polyvinyl alcohol solution with the mass fraction of 0.66% as a water phase, then mixing the oil phase and the water phase, heating to 50 ℃ and emulsifying for 10-15 minutes at the rate of 6000r/min to form microemulsion, stirring and reacting for 5-7 hours at the rate of 300r/min in a 75-80 ℃ water bath environment, and finally filtering, drying and washing to obtain the biocompatible phase change microcapsule.
9g of phase-change microcapsule and 6g of polyvinyl alcohol solution are stirred and mixed to form phase-change microcapsule suspension, 2g of dextran, 0.2g of sodium polyacrylate, 0.3g of sodium carboxymethyl cellulose, 2.5g of glycerol, 1g of propylene glycol, 0.1 g of aluminum glycollate and 10g of deionized water are stirred and mixed, and then centrifugal dispersion is carried out for 3-5min at the speed of 8000r/min to obtain dextran-based gel, and 1.5g of green compress powder, 0.6g of tartaric acid and 9g of deionized water are uniformly dispersed to obtain green compress powder solution.
Respectively taking 10ml of microcapsule suspension prepared by experiments, dextran-based gel and green application dispersion solution into an injector A, B, C, pushing A at a flow rate of 20 mu L/min and B, C mu L/min by a microfluidic device, stopping pushing C after 100min, adjusting the flow rate of A to 80 mu L/min, adjusting the flow rate of B to 40 mu L/min, simultaneously pushing A and B until A is finished, adjusting the flow rate of B to 100 mu L/min, pushing B until finishing, enabling the moving speed of a nozzle in the process to be 6mm/s, and finally drying in a blast drying box at 60 ℃ for 3-5h to obtain the temperature-controlled and moisture-preserving medical dressing loaded with the biocompatible phase change microcapsules.
Example 6
Mixing 2g of pentaerythritol tetraacrylate, 0.3g of azodiisobutyronitrile, 8g of methyl methacrylate, 7.6g of lauric acid and 2.4g of stearic acid, then dispersing for 25 minutes at 45 ℃ in an ultrasonic vibration mode to prepare 150ml of polyvinyl alcohol solution with the mass fraction of 0.66% as a water phase, then mixing the oil phase and the water phase, heating to 50 ℃ and emulsifying for 10-15 minutes at the rate of 6000r/min to form microemulsion, stirring and reacting for 5-7 hours at the rate of 300r/min in a 75-80 ℃ water bath environment, and finally filtering, drying and washing to obtain the biocompatible phase change microcapsule.
Stirring and mixing 12g of phase-change microcapsule and 8g of polyvinyl alcohol solution to form phase-change microcapsule suspension, stirring and mixing 2g of dextran, 0.2g of sodium polyacrylate, 0.3g of sodium carboxymethyl cellulose, 2.5g of glycerol, 1g of propylene glycol, 0.1 g of aluminum glycollate and 10g of deionized water, and then centrifugally dispersing for 3-5min at the speed of 8000r/min to obtain dextran-based gel, and uniformly dispersing 2g of green compress powder, 0.8g of tartaric acid and 12g of deionized water to obtain a green compress powder solution.
Respectively taking 10ml of microcapsule suspension prepared by experiments, dextran-based gel and green application dispersion solution into an injector A, B, C, pushing A at a flow rate of 20 mu L/min and B, C mu L/min by a microfluidic device, stopping pushing C after 100min, adjusting the flow rate of A to 80 mu L/min, adjusting the flow rate of B to 40 mu L/min, simultaneously pushing A and B until A is finished, adjusting the flow rate of B to 100 mu L/min, pushing B until finishing, enabling the moving speed of a nozzle in the process to be 6mm/s, and finally drying in a blast drying box at 60 ℃ for 3-5h to obtain the temperature-controlled and moisture-preserving medical dressing loaded with the biocompatible phase change microcapsules.
Example 7
Mixing 1.5g of pentaerythritol tetraacrylate, 0.3g of azodiisobutyronitrile, 8g of methyl methacrylate, 7.6g of lauric acid and 2.4g of stearic acid, then dispersing by ultrasonic vibration at 45 ℃ for 25min to prepare 150ml of styrene-maleic anhydride sodium salt solution with mass fraction of 0.66% as an aqueous phase, then mixing the aqueous phase with the oil phase, heating to 50 ℃ and emulsifying for 10-15min at the rate of 6000r/min to form microemulsion, stirring and reacting for 5-7h at the rate of 300r/min in a water bath environment at 75-80 ℃, and finally filtering, drying and washing to obtain the biocompatible phase change microcapsule.
9g of phase-change microcapsule and 6ml of styrene-maleic anhydride sodium salt solution are stirred and mixed to form phase-change microcapsule suspension, 2g of dextran, 0.2g of sodium polyacrylate, 0.3g of sodium carboxymethyl cellulose, 2.5g of glycerol, 1g of propylene glycol, 0.1 g of dihydroxyaluminum and 10g of deionized water are stirred and mixed, and then centrifugal dispersion is carried out for 3-5min at the speed of 8000r/min to obtain dextran-based gel, and 1.5g of green compress powder, 0.6g of tartaric acid and 9g of deionized water are uniformly dispersed to obtain a green compress powder solution.
Respectively taking 10ml of microcapsule suspension prepared by experiments, dextran-based gel and green application dispersion solution into an injector A, B, C, pushing A at a flow rate of 20 mu L/min and B, C mu L/min by a microfluidic device, stopping pushing C after 100min, adjusting the flow rate of A to 80 mu L/min, adjusting the flow rate of B to 40 mu L/min, simultaneously pushing A and B until A is finished, adjusting the flow rate of B to 100 mu L/min, pushing B until finishing, enabling the moving speed of a nozzle in the process to be 6mm/s, and finally drying in a blast drying box at 60 ℃ for 3-5h to obtain the temperature-controlled and moisture-preserving medical dressing loaded with the biocompatible phase change microcapsules.
Example 8
Mixing 1.5g of pentaerythritol tetraacrylate, 0.3g of azodiisobutyronitrile, 7g of methyl methacrylate, 7.6g of lauric acid and 2.4g of stearic acid, then dispersing by ultrasonic vibration at 45 ℃ for 25min to obtain oil phases, respectively preparing 150ml of sodium dodecyl sulfate/gelatin solution (each accounting for 50%) with the mass fraction of 0.66% as water phases, then mixing the oil phases with the water phases, heating to 50 ℃ and emulsifying at the rate of 6000r/min for 10-15min to form microemulsion, stirring at the rate of 300r/min in a water bath environment at 75-80 ℃ for reacting for 5-7h, and finally filtering, drying and washing to obtain the biocompatible phase-change microcapsule.
Stirring and mixing 12g of phase-change microcapsule with 8g of sodium dodecyl sulfate/gelatin solution to form phase-change microcapsule suspension, stirring and mixing 2g of dextran, 0.2g of sodium polyacrylate, 0.3g of sodium carboxymethyl cellulose, 2.5g of glycerol, 1g of propylene glycol, 0.1 g of dihydroxyaluminum and 10g of deionized water, and then centrifugally dispersing for 3-5min at the speed of 8000r/min to obtain dextran-based gel, and uniformly dispersing 2g of green compress powder, 0.8g of tartaric acid and 12g of deionized water to obtain a green compress powder solution.
Respectively taking 10ml of microcapsule suspension prepared by experiments, dextran-based gel and green application dispersion solution into an injector A, B, C, pushing A at a flow rate of 20 mu L/min and B, C mu L/min through a microfluidic device, stopping pushing C after 100min, adjusting the flow rate of A to 80 mu L/min, adjusting the flow rate of B to 40 mu L/min, simultaneously pushing A and B until A is finished, adjusting the flow rate of B to 100 mu L/min, pushing B until finishing, enabling the moving speed of a nozzle in the process to be 6mm/s, and finally drying in a blast drying box at 60 ℃ for 3-5h to obtain the temperature-controlled and moisture-preserving medical dressing loaded with the biocompatible phase change microcapsules;
as can be seen from table 1: the temperature-controlled moisturizing medical dressing loaded with the biocompatible phase-change microcapsule has good thermodynamic performance, the phase-change temperature is controlled between 33 ℃ and 38 ℃ of human body temperature, the supercooling degree is small, the high enthalpy value of 49.88J/g is achieved, the rapid response of temperature regulation with low temperature difference is facilitated, and the healing of wounds can be effectively promoted.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (10)
1. The preparation method of the temperature-controlled moisturizing medical dressing loaded with the biocompatible phase-change microcapsules is characterized by comprising the following steps of:
step 1: preparing phase-change microcapsule suspension by biocompatible phase-change microcapsule and surfactant solution;
step 2: the dextran-based gel is prepared from dextran and sodium polyacrylate which are composite framework materials, sodium carboxymethyl cellulose which is a thickener, dihydroxyaluminum which is a cross-linking agent, glycerin which is a humectant, propylene glycol and deionized water;
step 3: preparing a green compress powder solution from green compress powder, tartaric acid and deionized water;
step 4: and three-dimensionally printing the phase-change microcapsule suspension, the glucan-based gel and the green application dispersion solution through a microfluidic device to form the temperature-control moisturizing medical dressing loaded with the biocompatible phase-change microcapsule and having a three-layer structure of a drug release layer, a temperature control layer and a moisturizing layer.
2. The method for preparing the temperature-controlled and moisture-preserving medical dressing loaded with the biocompatible phase-change microcapsules according to claim 1, wherein the step 1 is characterized in that the equal-mass phase-change microcapsules and the surfactant solution are stirred and mixed to form a phase-change microcapsule suspension, and the preparation method of the biocompatible phase-change microcapsules is as follows:
mixing a cross-linking agent, an initiator, wall material monomer methyl methacrylate and a composite phase change core material, and obtaining an oil phase mixture through ultrasonic oscillation; preparing a surfactant solution as an aqueous phase; mixing the oil phase and the water phase, and emulsifying by a high-speed homogenizer to form an oil-in-water microemulsion; stirring the microemulsion in a water bath environment to initiate polymerization reaction, and finally filtering, washing and drying to obtain the biocompatible phase-change microcapsule.
3. The method for preparing the temperature-controlled and moisture-preserving medical dressing loaded with the biocompatible phase-change microcapsules according to claim 2, wherein in the step 1, the mass ratio of the phase-change microcapsules in the phase-change microcapsule suspension is 30% -60%; the mass ratio of the cross-linking agent to the initiator to the wall material monomer methyl methacrylate to the composite phase change core material is 1-2:0.3:7-8:10; wherein the cross-linking agent is one or more of pentaerythritol tetraacrylate, pentaerythritol triacrylate, ethylene glycol dimethacrylate and divinylbenzene; the initiator is one or more of azodiisobutyronitrile, potassium persulfate, ammonium persulfate and benzoyl peroxide; the composite phase-change core material is formed by mixing lauric acid and stearic acid, the mass ratio of the lauric acid to the stearic acid is 7.6-8:2-2.4, and the phase-change temperature area of the mixture is close to the body temperature.
4. The method for preparing the temperature-controlled and moisture-preserving medical dressing loaded with the biocompatible phase-change microcapsules according to claim 2, wherein the temperature and the duration of the ultrasonic vibration are 45-50 ℃ and 15-25min respectively; the concentration of the surfactant solution is 0.625% -1.000%, and the surfactant is one or more of styrene-maleic anhydride sodium salt, polyvinyl alcohol, polyvinylpyrrolidone, gelatin and sodium dodecyl sulfate; when the oil phase and the water phase are emulsified by a high-speed homogenizer to form the oil-in-water microemulsion, the temperature, the rotating speed and the duration of the emulsification are respectively 45-55 ℃, 3000-6000r/min and 10-15min; when the microemulsion is stirred in a water bath environment to initiate polymerization, the temperature, the rotating speed and the duration of the stirring reaction are respectively 70-80 ℃, 300-500r/min and 5-7h.
5. The method for preparing the temperature-controlled moisturizing medical dressing loaded with the biocompatible phase-change microcapsules according to claim 1, wherein in the step 2, dextran, sodium polyacrylate, sodium carboxymethyl cellulose, glycerol, propylene glycol, aluminum glycollate and deionized water are stirred and mixed, and then are centrifugally dispersed to obtain a dextran-based gel, wherein the mass ratio of the dextran, the sodium polyacrylate, the sodium carboxymethyl cellulose, the glycerol, the propylene glycol, the aluminum glycollate and the deionized water is 1:0.1:0.15:1.25:0.5:0.05:5;
the rotational speed and duration of centrifugal dispersion are 6000-8000r/min and 3-5min respectively.
6. The method for preparing the temperature-controlled moisturizing medical dressing loaded with the biocompatible phase-change microcapsules according to claim 1, wherein the step 3 is characterized in that the green compress powder, the tartaric acid and the deionized water are mixed to obtain a green compress powder solution, and the mass ratio of the green compress powder to the tartaric acid to the deionized water is 1:0.4:6.
7. The method for preparing the temperature-controlled and moisture-preserving medical dressing loaded with the biocompatible phase-change microcapsules according to claim 1, wherein the phase-change microcapsule suspension prepared in the step 4, glucan-based gel and green application dispersion solution prepared in the step 1-3 are taken to be filled into an injector A, B, C, three-dimensional printing is carried out by respectively controlling the flow ratio of the three and the moving speed of a nozzle through a microfluidic device, a medicine release layer, a temperature control layer and a moisture-preserving layer are sequentially formed, and finally the temperature-controlled and moisture-preserving medical dressing loaded with the biocompatible phase-change microcapsules is obtained by drying in a blast drying box; the material of the drug release layer is green compress dispersion solution, microcapsule suspension and dextran-based gel, the material of the temperature control layer is microcapsule suspension and dextran-based gel, and the material of the moisture preservation layer is dextran-based gel.
8. The method for preparing a temperature-controlled and moisture-preserving medical dressing loaded with biocompatible phase-change microcapsules according to claim 7, wherein the microfluidic device comprises a syringe, a syringe pump, a microchannel, a mixing device and a nozzle; the flow range controlled by the microfluidic device is 30-100 mu L/min; the moving speed of the nozzle of the micro-fluidic device is 2-10mm/s.
9. The method for preparing the temperature-controlled and moisture-preserving medical dressing loaded with the biocompatible phase-change microcapsules according to claim 7, wherein the flow ratio of the phase-change microcapsule suspension to the dextran-based gel to the green dressing dispersion solution is 2-4:3:3 when the drug release layer is printed; when the temperature control layer is printed, the flow ratio of the phase change microcapsule suspension to the dextran-based gel is 6-8:4, and the flow of the green application dispersion solution is 0; when the moisturizing layer is printed, the needed material is glucan-based gel, and the flow of the phase-change microcapsule suspension and the green application dispersion solution is 0.
10. The biocompatible phase-change microcapsule-loaded temperature-controlled moisturizing medical dressing obtained by the method according to any one of claims 1 to 9, wherein the dressing comprises three-layer structures comprising a drug release layer, a temperature control layer and a moisturizing layer formed by three-dimensionally printing a phase-change microcapsule suspension, a dextran-based gel and a green dressing dispersion solution through a microfluidic device; wherein the phase-change microcapsule suspension is prepared from biocompatible phase-change microcapsules and a surfactant solution; the glucan-based gel is prepared from composite framework material glucan, sodium polyacrylate, thickener sodium carboxymethyl cellulose, crosslinking agent dihydroxyaluminum, humectant glycerin, propylene glycol and deionized water; the green compress powder solution is prepared from green compress powder, tartaric acid and deionized water.
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