CN113499471A - Self-degradable medical aerogel particles and preparation process thereof - Google Patents
Self-degradable medical aerogel particles and preparation process thereof Download PDFInfo
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- 239000004964 aerogel Substances 0.000 title claims abstract description 84
- 239000002245 particle Substances 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000654 additive Substances 0.000 claims abstract description 30
- 230000000996 additive effect Effects 0.000 claims abstract description 30
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 25
- 229920000642 polymer Polymers 0.000 claims abstract description 25
- 239000002904 solvent Substances 0.000 claims abstract description 23
- 238000007710 freezing Methods 0.000 claims abstract description 20
- 230000008014 freezing Effects 0.000 claims abstract description 20
- 239000011148 porous material Substances 0.000 claims abstract description 20
- -1 organic acid compound Chemical class 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 11
- 239000000661 sodium alginate Substances 0.000 claims abstract description 11
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims description 37
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 35
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 32
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid group Chemical group C(CC(O)(C(=O)O)CC(=O)O)(=O)O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 27
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 21
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 20
- ABBQHOQBGMUPJH-UHFFFAOYSA-M Sodium salicylate Chemical compound [Na+].OC1=CC=CC=C1C([O-])=O ABBQHOQBGMUPJH-UHFFFAOYSA-M 0.000 claims description 16
- 229960004025 sodium salicylate Drugs 0.000 claims description 16
- 238000011049 filling Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000012046 mixed solvent Substances 0.000 claims description 15
- 238000004806 packaging method and process Methods 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 15
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 14
- 239000011159 matrix material Substances 0.000 claims description 13
- 239000000499 gel Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000005469 granulation Methods 0.000 claims description 10
- 230000003179 granulation Effects 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 10
- 239000011240 wet gel Substances 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 238000009413 insulation Methods 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- 239000011888 foil Substances 0.000 claims description 8
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 230000002439 hemostatic effect Effects 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000013526 supercooled liquid Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims description 3
- 230000023597 hemostasis Effects 0.000 claims description 3
- 239000003349 gelling agent Substances 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 6
- 238000004132 cross linking Methods 0.000 abstract description 4
- 230000018044 dehydration Effects 0.000 abstract description 2
- 238000006297 dehydration reaction Methods 0.000 abstract description 2
- 238000012377 drug delivery Methods 0.000 abstract description 2
- 231100000956 nontoxicity Toxicity 0.000 abstract description 2
- 238000000859 sublimation Methods 0.000 abstract description 2
- 230000008022 sublimation Effects 0.000 abstract description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract 1
- 229910052708 sodium Inorganic materials 0.000 abstract 1
- 239000011734 sodium Substances 0.000 abstract 1
- 238000007789 sealing Methods 0.000 description 8
- 125000004122 cyclic group Chemical group 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 239000004642 Polyimide Substances 0.000 description 3
- 229920001721 polyimide Polymers 0.000 description 3
- 159000000000 sodium salts Chemical class 0.000 description 3
- 238000005886 esterification reaction Methods 0.000 description 2
- 150000002989 phenols Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 239000004965 Silica aerogel Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/001—Use of materials characterised by their function or physical properties
- A61L24/0036—Porous materials, e.g. foams or sponges
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/24—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/28—Polysaccharides or their derivatives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/425—Porous materials, e.g. foams or sponges
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/001—Use of materials characterised by their function or physical properties
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/04—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials
- A61L24/06—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/04—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials
- A61L24/08—Polysaccharides
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/04—Materials for stopping bleeding
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- Health & Medical Sciences (AREA)
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- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
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- Veterinary Medicine (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Hematology (AREA)
- Surgery (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Preparation (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses self-degradable medical aerogel particles and a preparation process thereof, belongs to the technical field of aerogels, and comprises aerogel particles, wherein the aerogel particles are polymer matrixes prepared from polyacrylamide, and the polymer matrixes comprise the following components in parts by weight: polyacrylamide, organic acid compound, additive, accelerant and solvent. According to the invention, during production, the moisture in the pores is subjected to sublimation drying through low-temperature freezing, so that the collapse of a pore structure due to rapid dehydration is avoided, the aerogel is integrally crushed and granulated in a frozen state through ultrasonic waves after being processed, the collapse of the aerogel structure is avoided from influencing the mixed use of the load, the application range of organic crosslinking in the medical aspect is improved through the non-toxicity of the water sample sodium, the wound can be coated through the mixed material with sodium alginate, and the use of the load in the aspects of drug delivery and controllable release is realized through multiple micropores.
Description
Technical Field
The invention belongs to the technical field of aerogel, and particularly relates to self-degradable medical aerogel particles and a preparation process thereof.
Background
Aerogel is a kind of nano-porous solid material with three-dimensional network structure, and the pores and network structure of the solid matrix are filled with gas (usually air). Because of the excellent characteristics of large specific surface area, high porosity, low volume density, heat conductivity coefficient and the like, the aerogel has huge potential application in various fields such as heat insulation, catalysis, energy, adsorption, aerospace and the like. The aerogel is divided into inorganic aerogel and organic aerogel, compares in breakable inorganic aerogel, and organic aerogel has the better advantage of mechanical properties, the pliability.
Chinese patent document CN107531493B discloses an aerogel having as high and permanent hydrophobicity as possible and reduced flammability, and chinese patent document CN110903511A discloses a flexible flame retardant polyimide aerogel and a preparation method thereof, the polyimide aerogel preparation method is simple and convenient, the cost is low, the prepared aerogel has low density and high porosity, but the porous interface of the polyimide aerogel is not applicable to medical treatment, and the toxicity of the raw material phenols limits the applicable range of organic crosslinking, so that the effects of fine pore size and light weight of the aerogel are not applicable to medical treatment.
Disclosure of Invention
The invention aims to: the self-degradable medical aerogel particles and the preparation process are provided for solving the problems that the porous interface of the medical aerogel particles cannot be applied to the medical direction, the application range of organic crosslinking is limited by the toxicity of raw materials of phenols, and the fine pore size and light weight of the aerogel cannot be applied to the medical aspect.
In order to achieve the purpose, the invention adopts the following technical scheme:
self-degrading medical aerogel particles comprising aerogel particles, said aerogel particles being a polymer matrix prepared by polyacrylamide, said polymer matrix consisting of, by weight: polyacrylamide, organic acid compound, additive, accelerant and solvent.
As a further description of the above technical solution:
the organic acid compound is sodium salicylate, and the accelerant is citric acid gel.
As a further description of the above technical solution:
the additive is one or more of ethylene glycol, glycerol, polydactylene glycol, formamide and dimethylformamide.
As a further description of the above technical solution:
the solvent is ethanol, and the concentration of the ethanol is 80-95.
As a further description of the above technical solution:
the aerogel particles also comprise medical dressing mixed with the loaded filling particles, the loaded filling particles are sodium alginate, and the volume ratio of the loaded particles is 0.3.
As a further description of the above technical solution:
the preparation method of the medical dressing specifically comprises the following steps: s1, adding medical ethanol into the prepared aerogel particles and sodium alginate fibers, and placing the mixture into a mixer for centrifugal mixing to obtain the hemostatic dressing;
s2, after fully mixing, coating the mixed hemostatic dressing on the surface of the medical bandage, and then performing bandage dressing hemostasis.
A preparation process of self-degradable medical aerogel particles specifically comprises the following steps:
s1, preparing a precursor mixed solvent, namely adding polyacrylamide with a formula amount into deionized water with a required amount, adding sodium salicylate after fully dissolving and mixing, fully stirring and mixing to obtain the mixed solvent, and taking the sodium salicylate and the polyacrylamide as precursors;
s2, adding an additive into the mixed solvent after stirring and mixing, heating to a temperature of 45-60 ℃ which is convenient to control, performing magnetic stirring and mixing, after the additive is fully mixed and the surface of the additive does not flocculate, adding a gel accelerator with a formula amount into a mixing kettle through an additive pump, fully stirring and mixing the mixture in a stirring kettle to obtain a polymer aqueous solution, adding the polymer aqueous solution into a low-temperature sealing mould, adjusting the temperature of the sealing mould to be 45-60 ℃, and performing cyclic heating for 36-48h to obtain wet gel;
s3, replacing the solvent, namely, wholly adding the obtained wet gel and the mold into an autoclave, adding an exchange solvent into the mold, pressurizing and heating the autoclave for replacement, and partially replacing deionized water in pores after replacing for a certain time;
s4, cooling and drying in the environment, introducing a super-cooled liquid nitrogen solution into the high-pressure kettle, pressurizing at the same time, freezing and sublimating the residual refrigerating fluid in the pores, and freeze-drying for 3-15 hours;
and S5, granulating and packaging, taking out the prepared aerogel from the die, performing ultrasonic crushing granulation under the unfrozen state, filling the obtained aerogel into a packaging bag after granulation, and freezing for later use.
As a further description of the above technical solution:
the freezing temperature in the S4 is controlled to be-110 to-80 ℃.
As a further description of the above technical solution:
and the pressure of the high-pressure kettle in the S4 is 6.5-13 Mpa.
As a further description of the above technical solution:
and the packaging bag in the S5 is an aluminum foil heat insulation bag.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
in the invention, by adopting polyacrylamide and water-like sodium salt for mixing and using citric acid as a gel promoter, meanwhile, by adding alcohols or amide compounds, acid and alcohol are subjected to esterification reaction to form a high molecular polymer, expansion foaming is generated along with volatilization of ethanol, the process is favorable for forming porous and loose multiple holes, and simultaneously, the water in the pore space is sublimated and dried by low-temperature freezing during production, so that the collapse of the pore structure due to rapid dehydration is avoided, and the aerogel is integrally crushed and granulated in a frozen state by ultrasonic after being processed, so that the phenomenon that the collapse of the aerogel structure influences the load mixing use is avoided, the non-toxicity of the water-like sodium salt improves the application range of organic crosslinking in the aspect of medical treatment, and the wound can be coated by the mixed material of the water-like sodium salt and the sodium alginate, meanwhile, the microporous loading method can be used for drug delivery and controllable release.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides a technical scheme: self-degrading medical aerogel particles comprising aerogel particles, said aerogel particles being a polymer matrix prepared by polyacrylamide, said polymer matrix consisting of, by weight: the preparation method comprises the following steps of preparing a medical dressing, wherein the medical dressing comprises polyacrylamide, an organic acid compound, an additive, an accelerant and a solvent, the organic acid compound is sodium salicylate, the accelerant is a citric acid gel, the additive is one or a composition of ethylene glycol, glycerol, polydactylene glycol, formamide and dimethylformamide, the solvent is ethanol, the concentration of the ethanol is 80-95, the aerogel particles further comprise the medical dressing mixed with loaded filling particles, the loaded filling particles are sodium alginate, and the volume ratio of the loaded particles is 0.3, and the preparation method of the medical dressing specifically comprises the following steps: adding medical ethanol into prepared aerogel particles and sodium alginate fibers, then placing the mixed materials into a mixer to centrifugally mix the materials to prepare the hemostatic dressing, S2, fully mixing the materials, coating the hemostatic dressing on the surface of a medical bandage with the mixed materials to perform bandage dressing hemostasis, and forming a high polymer through esterification reaction of citric acid, glycol, glycerol, polyvidone, formamide and dimethylformamide by using a citric acid gel, wherein the gel expands and foams along with volatilization of ethanol, so that a porous and loose porous aerogel is formed.
Example 2
Self-degrading medical aerogel particles comprising aerogel particles, said aerogel particles being a polymer matrix prepared by polyacrylamide, said polymer matrix consisting of, by weight: polyacrylamide, an organic acid compound, an additive, an accelerant and a solvent, wherein the organic acid compound is sodium salicylate, the accelerant is a citric acid gel, the additive is one or a composition of ethylene glycol, glycerol, polydactylene glycol, formamide and dimethylformamide, the solvent is ethanol, the concentration of the ethanol is 80-95, the aerogel particles further comprise a medical dressing mixed with loaded filling particles, the loaded filling particles are sodium alginate, the volume ratio of the loaded particles is 0.3, and the preparation process of the self-degradable medical aerogel particles specifically comprises the following steps: s1, preparing a precursor mixed solvent, namely adding polyacrylamide with a formula amount into deionized water with a required amount, adding sodium salicylate after fully dissolving and mixing, fully stirring and mixing to obtain the mixed solvent, and taking the sodium salicylate and the polyacrylamide as precursors; s2, adding an additive into the mixed solvent after stirring and mixing, heating to a temperature of 45-60 ℃ which is convenient to control, performing magnetic stirring and mixing, after the additive is fully mixed and the surface of the additive does not flocculate, adding a gel accelerator with a formula amount into a mixing kettle through an additive pump, fully stirring and mixing the mixture in a stirring kettle to obtain a polymer aqueous solution, adding the polymer aqueous solution into a low-temperature sealing mould, adjusting the temperature of the sealing mould to be 45-60 ℃, and performing cyclic heating for 36-48h to obtain wet gel; s3, replacing the solvent, namely, wholly adding the obtained wet gel and the mold into an autoclave, adding an exchange solvent into the mold, pressurizing and heating the autoclave for replacement, and partially replacing deionized water in pores after replacing for a certain time; s4, cooling and drying in the environment, introducing a super-cooled liquid nitrogen solution into the high-pressure kettle, pressurizing at the same time, freezing and sublimating the residual refrigerating fluid in the pores, and freeze-drying for 3-15 hours; s5, granulating and packaging, performing ultrasonic crushing and granulation on the prepared aerogel taken out of the die in an unfrozen packaged state, filling the obtained aerogel into a packaging bag after granulation, and freezing for later use, wherein the pressurization of the high-pressure kettle in the S4 is 6.5-13Mpa, the packaging bag in the S5 is an aluminum foil heat insulation bag, the influence of external temperature change on the shape of aerogel particles is avoided by selecting the aluminum foil heat insulation bag, and the preferred embodiment is to control the freezing temperature in the S4 to be-110 ℃.
Example 3
Self-degrading medical aerogel particles comprising aerogel particles, said aerogel particles being a polymer matrix prepared by polyacrylamide, said polymer matrix consisting of, by weight: polyacrylamide, an organic acid compound, an additive, an accelerant and a solvent, wherein the organic acid compound is sodium salicylate, the accelerant is a citric acid gel, the additive is one or a composition of ethylene glycol, glycerol, polydactylene glycol, formamide and dimethylformamide, the solvent is ethanol, the concentration of the ethanol is 80-95, the aerogel particles further comprise a medical dressing mixed with loaded filling particles, the loaded filling particles are sodium alginate, the volume ratio of the loaded particles is 0.3, and the preparation process of the self-degradable medical aerogel particles specifically comprises the following steps: s1, preparing a precursor mixed solvent, namely adding polyacrylamide with a formula amount into deionized water with a required amount, adding sodium salicylate after fully dissolving and mixing, fully stirring and mixing to obtain the mixed solvent, and taking the sodium salicylate and the polyacrylamide as precursors; s2, adding an additive into the mixed solvent after stirring and mixing, heating to a temperature of 45-60 ℃ which is convenient to control, performing magnetic stirring and mixing, after the additive is fully mixed and the surface of the additive does not flocculate, adding a gel accelerator with a formula amount into a mixing kettle through an additive pump, fully stirring and mixing the mixture in a stirring kettle to obtain a polymer aqueous solution, adding the polymer aqueous solution into a low-temperature sealing mould, adjusting the temperature of the sealing mould to be 45-60 ℃, and performing cyclic heating for 36-48h to obtain wet gel; s3, replacing the solvent, namely, wholly adding the obtained wet gel and the mold into an autoclave, adding an exchange solvent into the mold, pressurizing and heating the autoclave for replacement, and partially replacing deionized water in pores after replacing for a certain time; s4, cooling and drying in the environment, introducing a super-cooled liquid nitrogen solution into the high-pressure kettle, pressurizing at the same time, freezing and sublimating the residual refrigerating fluid in the pores, and freeze-drying for 3-15 hours; s5, granulating and packaging, performing ultrasonic crushing and granulation on the prepared aerogel taken out of the die in an unfrozen packaged state, filling the obtained aerogel into a packaging bag after granulation, and freezing for later use, wherein the pressurization of the high-pressure kettle in the S4 is 6.5-13Mpa, the packaging bag in the S5 is an aluminum foil heat insulation bag, the influence of external temperature change on the shape of aerogel particles is avoided by selecting the aluminum foil heat insulation bag, and the preferred embodiment is to control the freezing temperature in the S4 to be-80 ℃.
Example 4
Self-degrading medical aerogel particles comprising aerogel particles, said aerogel particles being a polymer matrix prepared by polyacrylamide, said polymer matrix consisting of, by weight: polyacrylamide, an organic acid compound, an additive, an accelerant and a solvent, wherein the organic acid compound is sodium salicylate, the accelerant is a citric acid gel, the additive is one or a composition of ethylene glycol, glycerol, polydactylene glycol, formamide and dimethylformamide, the solvent is ethanol, the concentration of the ethanol is 80-95, the aerogel particles further comprise a medical dressing mixed with loaded filling particles, the loaded filling particles are sodium alginate, the volume ratio of the loaded particles is 0.3, and the preparation process of the self-degradable medical aerogel particles specifically comprises the following steps: s1, preparing a precursor mixed solvent, namely adding polyacrylamide with a formula amount into deionized water with a required amount, adding sodium salicylate after fully dissolving and mixing, fully stirring and mixing to obtain the mixed solvent, and taking the sodium salicylate and the polyacrylamide as precursors; s2, adding an additive into the mixed solvent after stirring and mixing, heating to a temperature of 45-60 ℃ which is convenient to control, performing magnetic stirring and mixing, after the additive is fully mixed and the surface of the additive does not flocculate, adding a gel accelerator with a formula amount into a mixing kettle through an additive pump, fully stirring and mixing the mixture in a stirring kettle to obtain a polymer aqueous solution, adding the polymer aqueous solution into a low-temperature sealing mould, adjusting the temperature of the sealing mould to be 45-60 ℃, and performing cyclic heating for 36-48h to obtain wet gel; s3, replacing the solvent, namely, wholly adding the obtained wet gel and the mold into an autoclave, adding an exchange solvent into the mold, pressurizing and heating the autoclave for replacement, and partially replacing deionized water in pores after replacing for a certain time; s4, cooling and drying in the environment, introducing a super-cooled liquid nitrogen solution into the high-pressure kettle, pressurizing at the same time, freezing and sublimating the residual refrigerating fluid in the pores, and freeze-drying for 3-15 hours; s5, granulating and packaging, performing ultrasonic crushing and granulation on the prepared aerogel taken out of the die in an unfrozen packaged state, filling the obtained aerogel into a packaging bag after granulation, and freezing for later use, wherein the pressurization of the high-pressure kettle in the S4 is 6.5-13Mpa, the packaging bag in the S5 is an aluminum foil heat insulation bag, the influence of external temperature change on the shape of aerogel particles is avoided by selecting the aluminum foil heat insulation bag, and the preferred embodiment is to control the freezing temperature in the S4 to be-90 ℃.
Under the same process conditions, by controlling the freezing temperature during cooling and drying, the samples prepared in examples 2-4 were subjected to performance inspection by observing the surface pore size, and the data of commercially available silica aerogel was used as a comparative example, to obtain the data shown in Table 1,
as can be seen from the above table, in example 4, the freezing temperature is-90 ℃, and the collapse of the aerogel pores can be avoided during the freezing sublimation treatment, so as to ensure the uniform pore size of the whole aerogel, which is a preferred embodiment of the present invention.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. Self-degrading medical aerogel particles, comprising aerogel particles, wherein said aerogel particles are a polymer matrix prepared from polyacrylamide, and wherein said polymer matrix consists of the following components in parts by weight: polyacrylamide, organic acid compound, additive, accelerant and solvent.
2. The self-degrading medical aerogel particles of claim 2, wherein the organic acid compound is sodium salicylate and the accelerator is citric acid gelling agent.
3. The self-degrading medical aerogel particles of claim 1, wherein the additive is one or more of ethylene glycol, glycerol, polydactylene glycol, formamide, and dimethylformamide.
4. The self-degrading medical aerogel particles of claim 1, wherein the solvent is ethanol, and the concentration of ethanol is 80-95.
5. The self-degrading medical aerogel particles of any of claims 1-4, wherein the aerogel particles further comprise a medical dressing mixed with loaded packing particles, and the loaded packing particles are sodium alginate, and the loaded particle volume ratio is 0.3.
6. The self-degrading medical aerogel particles according to claim 5, wherein the method for preparing the medical dressing specifically comprises the following steps: s1, adding medical ethanol into the prepared aerogel particles and sodium alginate fibers, and placing the mixture into a mixer for centrifugal mixing to obtain the hemostatic dressing;
s2, after fully mixing, coating the mixed hemostatic dressing on the surface of the medical bandage, and then performing bandage dressing hemostasis.
7. The process for the preparation of self-degrading medical aerogel particles according to any of claims 1 to 4, comprising in particular the following steps:
s1, preparing a precursor mixed solvent, namely adding polyacrylamide with a formula amount into deionized water with a required amount, adding sodium salicylate after fully dissolving and mixing, fully stirring and mixing to obtain the mixed solvent, and taking the sodium salicylate and the polyacrylamide as precursors;
s2, adding an additive into the mixed solvent after stirring and mixing, heating to a controlled temperature, mixing, adding a gel accelerator after uniformly mixing, placing into a stirring kettle, fully stirring and mixing to obtain a polymer aqueous solution, adding into a low-temperature sealed mold, adjusting the temperature of the sealed mold to be 45-60 ℃, and circularly heating for 36-48h to obtain wet gel;
s3, replacing the solvent, namely, wholly adding the obtained wet gel and the mold into an autoclave, adding an exchange solvent into the mold, pressurizing and heating the autoclave for replacement, and partially replacing deionized water in pores after replacing for a certain time;
s4, cooling and drying in the environment, introducing a super-cooled liquid nitrogen solution into the high-pressure kettle, pressurizing at the same time, freezing and sublimating the residual refrigerating fluid in the pores, and freeze-drying for 3-15 hours;
and S5, granulating and packaging, taking out the prepared aerogel from the die, performing ultrasonic crushing granulation under the unfrozen state, filling the obtained aerogel into a packaging bag after granulation, and freezing for later use.
8. The process for preparing self-degradable medical aerogel particles according to claim 7, wherein the freezing temperature in S4 is controlled to be-110 to-80 ℃.
9. The process for preparing self-degradable medical aerogel particles according to claim 7, wherein the autoclave pressure in S4 is 6.5-13 MPa.
10. The process for preparing self-degradable medical aerogel particles according to claim 7, wherein the packaging bag in S5 is an aluminum foil heat insulation bag.
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