CN113493941A - Biological friendly slow-release nano fiber and preparation method thereof - Google Patents
Biological friendly slow-release nano fiber and preparation method thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
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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
- 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
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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
- 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
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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
- 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
- A61L15/32—Proteins, polypeptides; Degradation products or derivatives thereof, e.g. albumin, collagen, fibrin, gelatin
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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
- 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
- A61L15/32—Proteins, polypeptides; Degradation products or derivatives thereof, e.g. albumin, collagen, fibrin, gelatin
- A61L15/325—Collagen
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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
- 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
- A61L15/44—Medicaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/06—Washing or drying
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/04—Dry spinning methods
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
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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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/412—Tissue-regenerating or healing or proliferative agents
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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
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/418—Agents promoting blood coagulation, blood-clotting agents, embolising agents
Abstract
The invention provides a bio-friendly nano cellulose fiber and a preparation method thereof, wherein the nano fiber spinning solution comprises 10-30 wt% of cellulose ionic liquid solution, 20-60 wt% of other natural macromolecules, 10-30 wt% of organic solvent, 5-15 wt% of filler, 0.5-5 wt% of medicinal preparation, 0.5-5 wt% of catalyst and 5-10 wt% of dispersing agent. The invention adopts the cellulose ionic liquid solution and other natural polymer aqueous solutions, utilizes the jet spinning technology to organically combine cellulose and polymer materials, fully utilizes the advantageous properties of the cellulose ionic liquid solution and other natural polymer aqueous solutions, adopts the natural polymer with excellent hemostatic property, and has more excellent stability on the premise of good biocompatibility of the cellulose fiber, thereby prolonging the degradation time of the material in a human body and playing a role of slow release. The obtained cellulose fiber has a diameter of less than 400nm and excellent physical properties, and the fiber with the diameter is easy to contact and interact with the body.
Description
Technical Field
The invention belongs to the field of bio-friendly slow-release nano fibers, and particularly relates to a biodegradable cellulose and cellulose-based nano fiber material, a preparation method thereof, and industrial and medical applications thereof.
Background
Cellulose (cellulose) is a macromolecular polysaccharide composed of glucose, is insoluble in water and common organic solvents, and is the main component of plant cell walls. Cellulose is the most abundant natural organic matter in the world and accounts for more than 50% of the carbon content in the plant world. The cellulose content of cotton is close to 100%; in general, the cellulose accounts for 40-50% of the wood. Cellulose (i.e., dietary fiber) in foods has an important role in the health of the human body. Cellulose is one of the most abundant renewable organic resources in the plant kingdom, and thus it has good biocompatibility, and is a natural biodegradable and bioabsorbable resource. The cellulose is insoluble in water, dilute acid or dilute alkali and common organic solvents due to strong hydrogen bond action in and among molecules, so that the cellulose has excellent acid and alkali resistance, corrosion resistance and organic solvent resistance; meanwhile, compared with other natural polymers, the cellulose has better thermal and mechanical properties, so that the cellulose has stronger stability as an application material and is convenient for processing, forming and application. The study of cellulose spinning has been on the past for over 100 years. For most of the past, cellulose spinning has been carried out using viscose, which is both wasteful and an environmental problem, so that in recent decades, much work has been focused on the development of pollution-free spinning techniques for cellulose to produce high-performance fibers.
The subsequent electrostatic spinning process is one simple and effective process for preparing superfine polymer fiber, and the polymer fluid is charged with high voltage static electricity of thousands to ten thousand volts, and when the electric field strength is great enough, the polymer liquid drops overcome the surface tension to form jet stream, which forms several forms of unstable flow in the air and finally falls onto the grounded receiver to form polymer fiber similar to non-woven fabric or ordered superfine fiber.
However, it is difficult to spin cellulose fibers having a diameter of less than 400nm by the above spinning method.
The jet spinning technology is a novel nano fiber preparation technology, a polymer solution is taken as an object, high-speed airflow is taken as a driving force, the spinning solution forms polymer jet flow under the action of the high-speed airflow after being extruded through a spinneret orifice, the jet flow is further drawn and refined in a receiving device, the jet spinning has higher spinning efficiency than electrostatic spinning, and the diameter of the obtained fiber is thinner due to the driving action of the high-speed airflow, so that the jet spinning technology is a spinning fiber technology with great industrial prospects.
Disclosure of Invention
The technical problem actually solved by the invention is to provide a bio-friendly nano cellulose fiber and a preparation method thereof, the diameter of the obtained cellulose fiber is less than 400nm, the physical property is excellent, and the fiber with the diameter is easy to contact and interact with the organism. The invention adopts the cellulose ionic liquid solution and other natural polymer aqueous solutions, utilizes the jet spinning technology to organically combine cellulose and polymer materials, fully utilizes the advantages of the two, adopts the natural polymer with excellent hemostatic performance, and the cellulose fiber has more excellent stability on the premise of good biocompatibility, can prolong the degradation time of the material in a human body, plays a role in slow release, and obtains the novel hemostatic material with more excellent slow release performance.
The raw materials of the bio-friendly slow-release nano fiber comprise cellulose ionic liquid solution, other natural polymers, medicinal preparations, catalysts, fillers and dispersing agents. Wherein, the cellulose ionic liquid solution accounts for 10 to 30 weight percent, the other natural macromolecules account for 20 to 60 weight percent, the organic solvent accounts for 10 to 30 weight percent, the filler accounts for 5 to 15 weight percent, the pharmaceutical preparation accounts for 0.5 to 5 weight percent, the catalyst accounts for 0.5 to 5 weight percent, and the dispersant accounts for 5 to 10 weight percent.
Wherein the cellulose is selected from one or more of methyl cellulose, ethyl cellulose, microcrystalline cellulose, carboxymethyl cellulose, and hydroxyethyl cellulose. Especially preferred is carboxymethyl cellulose. The ionic liquid is one or more of pyridine cationic liquid, quaternary ammonium salt cationic liquid, quaternary phosphine cationic liquid, thiazole cationic liquid and guanidine salt cationic liquid.
Wherein the other natural polymers are selected from: one or more of polyvinyl alcohol, chitosan, gelatin, hyaluronic acid and collagen. Chitosan is particularly preferred.
The organic solvent is selected from: one or more of ethanol, acetone, ethyl acetate and dimethylformamide.
The pharmaceutical formulation is selected from: one or more of anti-inflammatory drugs, antibiotics, anti-infective drugs, traditional Chinese medicine extracts and nano-silver.
The catalyst is noble metal catalyst or metallocene catalyst such as Pt, Rh, Pd, etc.
The filler is selected from: one or more of nano titanium dioxide, gas-phase silicon dioxide, nano montmorillonite and potassium titanate whisker.
The dispersant is selected from: one or more of sodium dodecyl benzene sulfonate, alkyl glycoside, fatty alcohol-polyoxyethylene ether, polyvinyl alcohol 400 and dendritic polymer.
The preparation method of the bio-friendly slow-release nano fiber is carried out according to the following steps:
(1) preparing a spinning solution: adding cellulose into the ionic liquid, and stirring until the cellulose is completely dissolved. Adding natural polymer into organic solvent, stirring to dissolve completely. Adding the natural polymer/organic solvent system into the cellulose ionic liquid solution under the condition of stirring. Controlling the rotating speed at 400-600r/min and the temperature at 40 ℃, and sequentially adding a dispersing agent, a catalyst, a pharmaceutical preparation and a filler into the system, wherein the stirring time is 15-30 min;
(2) preparing the nano-fiber by jet spinning: and (2) feeding the spinning solution obtained in the step (1) into a spinning box body through a metering pump at the speed of 7-10mL/h by using an injection pump, forming a trickle when the spinning solution is extruded from a spinning nozzle, introducing compressed gas into the spinning box body at the same time, wherein the pressure of the compressed gas is 0.08MPa, enabling the obtained spinning trickle to enter the spinning box body, volatilizing the solvent to form fibers under the combined action of high-pressure air flow and the spinning box body, and collecting the fibers on a receiving plate by using the air suction action generated by a fan to obtain the cellulose/natural polymer nano fibers.
(3) And (3) repeatedly washing the cellulose/natural polymer nano-fiber obtained in the step (2) with ethanol/water solution for three times, and then drying in an oven to obtain a finished product.
The mass concentration of the cellulose ionic liquid solution is 50-70 wt%, the temperature of a spinning manifold is 60-90 ℃, the receiving distance is 40-60cm, the mass concentration of the ethanol/water solution is 60 wt%, the drying temperature is 60-80 ℃, and the drying time is 0.5-4 h.
The cellulose fibers obtained have a diameter of less than 400 nm.
Advantageous effects
The invention adds cellulose and other natural polymers into the spinning solution, so that the obtained nano-fiber has excellent functions of stopping bleeding and healing wounds, and the fiber can exist in a human body for a long time due to the action of the cellulose, thereby achieving the slow-release effect. The cellulose fiber has a diameter of less than 400nm, and can be contacted with affected part sufficiently to exert effective effect. The ionic liquid is adopted to dissolve the cellulose in the spinning solution, the high-concentration cellulose exists in a low-viscosity state under the action of the ionic liquid, the content of the cellulose in the spinning solution is greatly improved, and the breaking strength and the breaking elongation of the obtained fiber are greatly improved compared with the prior art.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1:
a bio-friendly slow-release carboxymethyl cellulose/chitosan nano fiber comprises 30 wt% of carboxymethyl cellulose/1-butyl-3-methyl-imidazole chloride ionic liquid solution, 30 wt% of chitosan, 10 wt% of ethanol, 5 wt% of fumed silica, 10 wt% of nano silver and honeysuckle flower extract, 5 wt% of metallocene catalyst and 10 wt% of fatty alcohol-polyoxyethylene ether.
The biological friendly slow-release carboxymethyl cellulose/chitosan nano fiber is prepared by the following method:
(1) preparing a spinning solution: adding carboxymethyl cellulose into the 1-butyl-3-methyl-imidazole chloride ionic liquid, and stirring until the carboxymethyl cellulose is completely dissolved. Adding chitosan into ethanol, and stirring to dissolve completely. Adding the chitosan/ethanol system into the cellulose ionic liquid solution under the stirring condition. Controlling the rotating speed at 500r/min and the temperature at 40 ℃, and adding a dispersing agent, a catalyst, a medicinal preparation and a filler into the system in sequence, and stirring for 15 min;
(2) preparing the nano-fiber by jet spinning: and (2) feeding the spinning solution obtained in the step (1) into a spinning box body through a metering pump at the speed of 8mL/h by using an injection pump, forming a trickle when the spinning solution is extruded from a spinning nozzle, introducing compressed gas into the spinning box body at the same time, wherein the pressure of the compressed gas is 0.08MPa, enabling the obtained spinning trickle to enter the spinning box body, volatilizing the solvent to form fibers under the combined action of high-pressure gas flow and the spinning box body, and collecting the fibers on a receiving plate by using the air suction action generated by a fan to obtain the carboxymethyl cellulose/chitosan nano-fibers.
(3) And (3) repeatedly washing the carboxymethyl cellulose/chitosan nano-fiber obtained in the step (2) with ethanol/water solution for three times, and then drying in an oven to obtain a finished product.
The mass concentration of the cellulose ionic liquid solution is 50 wt%, the temperature of a spinning manifold is 75 ℃, the receiving distance is 50cm, the mass concentration of ethanol/water solution is 60 wt%, the drying temperature is 70 ℃, and the drying time is 2 h.
The average diameter of the obtained cellulose fiber is 380nm, the breaking strength of the fiber is 2.05cn/dtex, and the elongation at break reaches 11.15%. Through testing the absorbance, the release time of the carboxymethyl cellulose/chitosan nano fiber in water is nearly 90 times longer than that of a pure drug preparation.
Example 2:
a bio-friendly slow-release carboxymethyl cellulose/polyvinyl alcohol nano fiber comprises 30 wt% of carboxymethyl cellulose/1-butyl-3-methyl-imidazole bromide ionic liquid solution, 30 wt% of polyvinyl alcohol, 10 wt% of ethanol, 5 wt% of fumed silica, 10 wt% of nano silver and honeysuckle extracts, 5 wt% of metallocene catalyst and 10 wt% of fatty alcohol-polyoxyethylene ether.
The bio-friendly slow-release carboxymethyl cellulose/polyvinyl alcohol nano fiber is prepared by the following method:
(1) preparing a spinning solution: adding carboxymethyl cellulose into the ionic liquid of the 1-butyl-3-methyl-imidazole bromide salt, and stirring until the carboxymethyl cellulose is completely dissolved. Adding polyvinyl alcohol into ethanol, and stirring until the polyvinyl alcohol is completely dissolved. Adding the polyvinyl alcohol/ethanol system into the cellulose ionic liquid solution under the stirring condition. Controlling the rotating speed at 600r/min and the temperature at 40 ℃, and adding a dispersing agent, a catalyst, a medicinal preparation and a filler into the system in sequence, and stirring for 15 min;
(2) preparing the nano-fiber by jet spinning: and (2) feeding the spinning solution obtained in the step (1) into a spinning box body through a metering pump at the speed of 10mL/h by using an injection pump, forming a trickle when the spinning solution is extruded from a spinning nozzle, introducing compressed gas into the spinning box body at the same time, wherein the pressure of the compressed gas is 0.08MPa, enabling the obtained spinning trickle to enter the spinning box body, volatilizing the solvent to form fibers under the combined action of high-pressure air flow and the spinning box body, and collecting the fibers on a receiving plate by using the air suction action generated by a fan to obtain the carboxymethyl cellulose/polyvinyl alcohol nano fibers.
(3) And (3) repeatedly washing the carboxymethyl cellulose/polyvinyl alcohol nano-fiber obtained in the step (2) with ethanol/water solution for three times, and then drying in an oven to obtain a finished product.
The mass concentration of the cellulose ionic liquid solution is 50 wt%, the temperature of a spinning manifold is 75 ℃, the receiving distance is 50cm, the mass concentration of ethanol/water solution is 60 wt%, the drying temperature is 70 ℃, and the drying time is 2 h.
The average diameter of the obtained cellulose fiber is 390nm, the breaking strength of the fiber is 2.55cn/dtex, and the breaking elongation reaches 12.44%. Through testing the absorbance, the release time of the carboxymethyl cellulose/polyvinyl alcohol nano-fiber in water is nearly 100 times longer than that of a pure drug preparation.
Example 3:
a bio-friendly slow-release hydroxyethyl cellulose/chitosan nano fiber comprises 30 wt% of hydroxyethyl cellulose/1-butyl-3-methyl-imidazole bromide ionic liquid solution, 30 wt% of chitosan, 10 wt% of ethanol, 5 wt% of fumed silica, 10 wt% of nano silver and honeysuckle flower extract, 5 wt% of metallocene catalyst and 10 wt% of fatty alcohol-polyoxyethylene ether.
The bio-friendly slow-release hydroxyethyl cellulose/chitosan nano fiber is prepared by the following method:
(1) preparing a spinning solution: adding hydroxyethyl cellulose into the ionic liquid of the 1-butyl-3-methyl-imidazole bromide salt, and stirring until the hydroxyethyl cellulose is completely dissolved. Adding chitosan into ethanol, and stirring to dissolve completely. Adding the chitosan/ethanol system into the cellulose ionic liquid solution under the stirring condition. Controlling the rotating speed at 500r/min and the temperature at 40 ℃, and adding a dispersing agent, a catalyst, a medicinal preparation and a filler into the system in sequence, and stirring for 15 min;
(2) preparing the nano-fiber by jet spinning: and (2) feeding the spinning solution obtained in the step (1) into a spinning box body through a metering pump at the speed of 8mL/h by using an injection pump, forming a trickle when the spinning solution is extruded from a spinning nozzle, introducing compressed gas into the spinning box body at the same time, wherein the pressure of the compressed gas is 0.08MPa, enabling the obtained spinning trickle to enter the spinning box body, volatilizing the solvent to form fibers under the combined action of high-pressure gas flow and the spinning box body, and collecting the fibers on a receiving plate by using the air suction action generated by a fan to obtain the hydroxyethyl cellulose/chitosan nano fibers.
(3) And (3) repeatedly washing the hydroxyethyl cellulose/chitosan nano-fiber obtained in the step (2) with ethanol/water solution for three times, and then drying in an oven to obtain a finished product.
The mass concentration of the cellulose ionic liquid solution is 50 wt%, the temperature of a spinning manifold is 75 ℃, the receiving distance is 50cm, the mass concentration of ethanol/water solution is 60 wt%, the drying temperature is 70 ℃, and the drying time is 2 h.
The average diameter of the obtained cellulose fiber is 390nm, the breaking strength of the fiber is 1.97cn/dtex, and the elongation at break reaches 10.74%. Through testing the absorbance, the release time of the hydroxyethyl cellulose/chitosan nano-fiber in water is nearly 80 times longer than that of a pure drug preparation.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A bio-friendly slow release nano fiber comprises a cellulose ionic liquid solution, other natural polymers, a medicinal preparation, a catalyst, a filler and a dispersing agent; wherein, the cellulose ionic liquid solution accounts for 10 to 30 weight percent, the other natural macromolecules account for 20 to 60 weight percent, the organic solvent accounts for 10 to 30 weight percent, the filler accounts for 5 to 15 weight percent, the pharmaceutical preparation accounts for 0.5 to 5 weight percent, the catalyst accounts for 0.5 to 5 weight percent, and the dispersant accounts for 5 to 10 weight percent.
2. The bio-friendly slow-release nano fiber as claimed in claim 1, wherein the cellulose is selected from one or more of methyl cellulose, ethyl cellulose, microcrystalline cellulose, carboxymethyl cellulose and hydroxyethyl cellulose, and the ionic liquid is one or more of pyridine cationic liquid, quaternary ammonium cationic liquid, quaternary phosphine cationic liquid, thiazole cationic liquid and guanidine cationic liquid.
3. The bio-friendly sustained-release nanofiber as claimed in claim 1, wherein the other natural polymers are selected from the group consisting of: one or more of polyvinyl alcohol, chitosan, gelatin, hyaluronic acid and collagen.
4. The bio-friendly sustained-release nanofiber as claimed in claim 1, wherein the organic solvent is selected from the group consisting of: one or more of ethanol, acetone, ethyl acetate and dimethylformamide.
5. The bio-friendly sustained-release nanofiber as claimed in claim 1, wherein the pharmaceutical preparation is selected from the group consisting of: one or more of anti-inflammatory drugs, antibiotics, anti-infective drugs, traditional Chinese medicine extracts and nano-silver.
6. The bio-friendly slow-release nano fiber as claimed in claim 1, wherein the catalyst is noble metal catalyst such as Pt, Rh, Pd, etc. or metallocene catalyst.
7. The bio-friendly sustained-release nanofiber as claimed in claim 1, wherein the filler is selected from the group consisting of: one or more of nano titanium dioxide, gas-phase silicon dioxide, nano montmorillonite and potassium titanate whisker.
8. The bio-friendly sustained-release nanofiber as claimed in claim 1, wherein the dispersing agent is selected from the group consisting of: one or more of sodium dodecyl benzene sulfonate, alkyl glycoside, fatty alcohol-polyoxyethylene ether, polyvinyl alcohol 400 and dendritic polymer.
9. A method for preparing the bio-friendly sustained-release nanofiber as claimed in claim 1, which comprises the following process steps:
(1) preparing a spinning solution: adding cellulose into the ionic liquid, and stirring until the cellulose is completely dissolved; adding natural polymer into organic solvent, stirring to dissolve completely; adding a natural polymer/organic solvent system into the cellulose ionic liquid solution under the stirring condition; controlling the rotating speed at 400-600r/min and the temperature at 40 ℃, and sequentially adding a dispersing agent, a catalyst, a pharmaceutical preparation and a filler into the system, wherein the stirring time is 15-30 min;
(2) preparing the nano-fiber by jet spinning: feeding the spinning solution obtained in the step (1) into a spinning box body through a metering pump at the speed of 7-10mL/h by using an injection pump, forming a trickle when the spinning solution is extruded from a spinning nozzle, simultaneously introducing compressed gas into the spinning box body, wherein the pressure of the compressed gas is 0.08MPa, enabling the obtained spinning trickle to enter the spinning box body, volatilizing the solvent to form fibers under the combined action of high-pressure gas flow and the spinning box body, and collecting the fibers on a receiving plate by using the air suction action generated by a fan to obtain the cellulose/natural polymer nano fibers;
(3) and (3) repeatedly washing the cellulose/natural polymer nano-fiber obtained in the step (2) with ethanol/water solution for three times, and then drying in an oven to obtain a finished product.
10. The preparation method according to claim 9, wherein the mass concentration of the cellulose ionic liquid solution is 50-70 wt%, the temperature of the spinning beam is 60-90 ℃, the receiving distance is 40-60cm, the mass concentration of the ethanol/water solution is 60 wt%, the drying temperature is 60-80 ℃, and the drying time is 0.5-4 h.
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| CN202010252014.8A CN113493941A (en) | 2020-04-01 | 2020-04-01 | Biological friendly slow-release nano fiber and preparation method thereof |
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| CN115804373A (en) * | 2022-12-08 | 2023-03-17 | 上海师范大学 | Nano cellulose based ultraviolet-resistant pesticide microcapsule and preparation method thereof |
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