CN111005082A - Whole-body porous polycaprolactone fiber and preparation method thereof - Google Patents
Whole-body porous polycaprolactone fiber and preparation method thereof Download PDFInfo
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- CN111005082A CN111005082A CN201911297857.3A CN201911297857A CN111005082A CN 111005082 A CN111005082 A CN 111005082A CN 201911297857 A CN201911297857 A CN 201911297857A CN 111005082 A CN111005082 A CN 111005082A
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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
- D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
- D01D5/247—Discontinuous hollow structure or microporous structure
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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
- D01D5/18—Formation of filaments, threads, or the like by means of rotating spinnerets
Abstract
The invention discloses a full-body porous polycaprolactone fiber and a preparation method thereof. The polycaprolactone fiber is of a porous structure. The preparation method comprises the following steps: adding polycaprolactone into dichloromethane, and stirring uniformly at room temperature; and injecting the obtained solution into a centrifugal spinning device for centrifugal spinning to obtain the porous polycaprolactone fiber. The invention does not need pore-forming agent or post-treatment, and uses the air flow generated by the high-speed rotation of the fan blade to accelerate the volatilization of the solvent and induce the phase separation to form pores. The obtained polycaprolactone fiber is porous in whole body, has ultrahigh porosity and specific surface area, has excellent mechanical property and good biocompatibility, and is expected to be applied to the field of tissue engineering. The method has clear thought, simple operation and high preparation efficiency.
Description
Technical Field
The invention relates to a full-body porous polycaprolactone fiber and a preparation method thereof, belonging to the technical field of porous fiber material preparation.
Background
With the continuous development and progress of science and technology, the human eyes are gradually shifted from the macroscopic world to the microscopic world. Micro-nano materials are widely concerned due to unique physical properties and chemical properties, micro-nano fibers are common micro-nano materials, and micro-nano fiber membranes are widely applied to the fields of high-efficiency filtration barrier materials, biological tissue engineering, ultra-high sensitivity sensors and the like due to the ultra-high specific surface area and controllable pore size.
With the progress of research, scientific researchers find that the application potential of the micro-nanofiber membrane is closely related to the specific surface area of the micro-nanofiber membrane, and the application performance of the micro-nanofiber membrane is improved along with the increase of the specific surface area of the micro-nanofiber membrane. Therefore, the preparation of the micro-nano fiber membrane with higher specific surface area is very important. Compared with the fiber with a smooth surface, the porous micro-nano fiber has a higher specific surface area due to the porous structure, and the application of the micro-nano fiber in the field is certainly promoted.
At present, the porous micro-nano fiber is mainly prepared by an electrostatic spinning method. One-step and multi-step methods can be classified according to the major factors affecting the formation of the pore structure.
The one-step method is also called liquid phase separation porogenic, and means that in the spinning process, the concentration of jet flow is rapidly increased and the temperature is rapidly reduced due to rapid volatilization of a solvent in the jet flow. The concentration rise and the temperature drop of the jet flow act together, so that the jet flow enters a metastable state or an unstable state and then is subjected to phase separation to form a polymer gathering area and a solvent gathering area, finally, the polymer gathering area is solidified to form a framework of the fiber, and the solvent gathering area is volatilized to form holes of the fiber. Regarding the pore-forming principle, there is also explanation of "breathing effect", that is, after the temperature of the jet flow is reduced to below 0 ℃, water molecules in the air are gathered on the surface of the fiber to form small water drops, the small water drops accelerate the solidification of the polymer, and then the polymer is coated, and finally the small water drops are evaporated to form pores after the fiber is formed. Therefore, the volatilization rate of the solvent in the jet flow can be controlled by controlling the concentration of the spinning solution and the spinning environment conditions (temperature and humidity) so as to obtain the porous fibers with different appearances, but the size and the shape of the obtained pore structure cannot be accurately controlled, and the spinning conditions and the pore structure are not in simple linear corresponding relation.
The multi-step method is also called solid phase separation pore-forming, and means that solid substances (including other polymers or inorganic salts and the like) are added into spinning solution, and after spinning, the solid substances are removed through certain post-treatment to leave pores. The method can regulate and control the size and the shape of holes in the fiber by controlling the particle shape and the size of the solid substances, but additives can remain in the fiber, so that the purity of the fiber is influenced, the structure and the performance of the fiber are also influenced, and the fiber is easily damaged in the post-treatment process.
Generally speaking, the liquid phase separation and pore-forming of the one-step method need to control more severe experimental environment and conditions; the solid phase separation pore-forming operation of the multi-step method is complex, impurities cannot be completely removed, and the fibers may be damaged. Although the electrostatic spinning can be used for quickly and conveniently preparing the porous micro-nano fiber, the following problems also exist: (1) high voltage over kilovolt is needed, and potential safety hazards exist; (2) the polarity of the spinning solution is required; (3) and the production efficiency is lower.
Centrifugal spinning is another method for preparing micro-nano fibers by gradually heating in recent years, the defects of electrostatic spinning are overcome perfectly, firstly, the centrifugal spinning does not need high voltage of over kilovolt, and the potential safety hazard of electric leakage and electric shock does not exist; secondly, the centrifugal spinning utilizes the force generated by the high-speed rotation of a spinneret to stretch the fiber, and has no requirement on the polarity of the spinning solution; finally, compared with electrostatic spinning, the centrifugal spinning production efficiency is greatly improved. Needless to say, centrifugal spinning will play an increasingly important role in the future way of preparing micro-nano fibers.
At present, the research on preparing porous micro-nano fibers by centrifugal spinning is few and less. Chinese patent CN105714388B discloses a method for rapidly preparing superfine full-body porous fiber, which comprises the steps of adding ethyl cellulose into a mixed solvent of ethanol and water, uniformly stirring, adding polyvinylpyrrolidone, uniformly stirring again, and carrying out centrifugal spinning to obtain the full-body porous fiber. According to the method, the difference between the volatility of ethanol and the volatility of water is utilized, so that the ethanol in the jet flow of the spinning solution is quickly volatilized, the water is slowly volatilized and is gathered in the fiber solidification process, a polymer enrichment area and a water enrichment area are formed, and finally, a porous structure is formed through the volatilization of the water. Chinese patent CN108823790A discloses a centrifugal spinning porous micro/nano fiber membrane and a preparation method thereof, wherein a polymer, a solvent and inorganic nano particles are mixed according to a certain proportion, centrifugal spinning is carried out after uniform stirring, a light source with the power more than or equal to 800W is adopted for irradiation in the spinning process, and the fiber membrane can be further subjected to acid treatment after the spinning is finished. The method increases the temperature of the spinning environment through the irradiation of a high-power light source, accelerates the volatilization of the solvent on the fiber after the fiber is formed, is beneficial to constructing a porous structure of the fiber, and simultaneously verifies the influence of inorganic particles and acid treatment on the hollow structure.
In addition to the preparation of the centrifugal spinning porous micro-nano fiber by configuring the spinning solutions with different polymer ratios and different solvent ratios mentioned in the chinese patent CN105714388B and the introduction of the high-power light source, the inorganic particles and the acid treatment mentioned in the chinese patent CN108823790A, the preparation of the centrifugal spinning porous micro-nano fiber can also be realized by improving the device of the centrifugal spinning itself. A plurality of fan blades are added below the spinneret orifice, and the spinneret drives the fan blades to rotate simultaneously when rotating for spinning to form upward high-speed airflow, so that the volatilization of the solvent on the fiber is accelerated, and a porous structure is obtained through phase separation. The method does not need to prepare spinning solutions of various polymers and various solvents, does not need to introduce a high-power light source and inorganic particles, and does not need to carry out acid treatment. The method only introduces the fan blades on the original basis of the centrifugal spinning device, generates high-speed airflow by utilizing the rotation of the spinning nozzle, and has the advantages of simple principle, convenient operation, energy conservation and environmental protection.
Polycaprolactone is a degradable high molecular material with good biocompatibility, and is widely applied to tissue engineering scaffolds because it is non-toxic to human bodies and degradation products do not cause inflammatory reactions. The polycaprolactone tissue engineering scaffold has unique advantages, good biocompatibility of the polycaprolactone tissue engineering scaffold is favorable for cell climbing adhesion and proliferation, and the polycaprolactone tissue engineering scaffold can be matched with different tissues due to controllable appearance, pore structure and stable mechanical property, so that the polycaprolactone tissue engineering scaffold has bright development prospects in the fields of bone repair, blood vessel repair, nerve repair and the like.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the prepared porous polycaprolactone fiber has ultrahigh specific surface area and porosity, and has good biocompatibility and mechanical property.
In order to solve the problems, the invention adopts the technical scheme that:
the full-body porous polycaprolactone fiber is characterized in that the polycaprolactone fiber is of a porous structure. The porous tissue has the advantages of porosity, ultrahigh specific surface area, high porosity, excellent mechanical property, good biocompatibility and great potential in the field of tissue engineering.
Preferably, the diameter of the polycaprolactone fiber is 0.5-30 μm.
The invention also provides a preparation method of the whole porous polycaprolactone fiber, which is characterized by comprising the following steps:
step 1): adding polycaprolactone into dichloromethane, and stirring uniformly at room temperature;
step 2): injecting the solution obtained in the step 1) into a centrifugal spinning device for centrifugal spinning to obtain the porous polycaprolactone fiber.
Preferably, the concentration of polycaprolactone in the solution obtained in the step 1) is 0.10-0.25 g/mL.
Preferably, the centrifugal spinning device in the step 2) comprises a rotating body provided with a spinneret orifice, fan blades are arranged on the outer edge of the rotating body, the rotating body is fixed on a rotating motor, and collecting rods are uniformly distributed around the rotating body.
More preferably, the fan blade is arranged below the spinneret orifice, and the vertical distance between the fan blade and the spinneret orifice is 3-10 cm; the number of flabellum is 2 ~ 8, evenly distributed at the rotator outer fringe. The spinning jet drives the fan blades to rotate to generate high-speed airflow to accelerate the volatilization of the solvent in the jet flow, and the solvent is induced to separate from the fan blades to form holes.
More preferably, the spinneret orifices are uniformly distributed around the rotating body, the diameter of the spinneret orifices is 0.1-0.8 mm, and the number of the spinneret orifices is 2-8.
Preferably, the process parameters of the centrifugal spinning device in the step 2) are as follows: the rotating speed is 500-5000 rpm/min, and the receiving distance is 8-15 cm.
The principle of the preparation method is that polycaprolactone is dissolved in dichloromethane to prepare spinning solution, then spinning is carried out on a centrifugal spinning device provided with fan blades, and the solvent is quickly volatilized to enable the fibers to be separated in the solidification process, so that the porous polycaprolactone fibers are obtained. In the centrifugal spinning process, the fan blades rotate along with the spinneret to generate upward high-speed airflow, and the solvent is quickly volatilized by jet flow sprayed from the spinneret orifices under the action of the high-speed airflow, so that the jet flow temperature is quickly reduced, and the jet flow concentration is quickly increased. Under the combined action of the jet temperature and the jet concentration, the jet enters a metastable state or an unstable state, so that phase separation occurs to form a polymer accumulation zone and a solvent accumulation zone. Finally, the polymer aggregation zone is solidified into a skeleton of the fiber, and the solvent aggregation zone forms a porous structure along with the further volatilization of the solvent. The invention skillfully improves the traditional centrifugal spinning device, and the introduction of the fan blades enables the spinning jet to automatically generate high-speed airflow in the rotating process, so that the volatilization of the solvent in the jet flow is accelerated, and the porous micro-nano fiber is obtained.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention develops a full-body porous polycaprolactone fiber which has ultrahigh specific surface area and porosity, good biocompatibility and mechanical property and great potential in the field of biological tissue engineering;
(2) the invention generates high-speed airflow by introducing fan blades, induces jet flow to generate phase separation to form pores, does not need pore-forming agent or post-treatment, reduces the introduction of impurities, ensures the quality of fibers, does not need to prepare spinning solution of various polymers and solvents, does not need to introduce a high-power light source, and has simple and effective principle, energy-saving process and environmental protection.
(3) The invention adopts the centrifugal spinning technology to prepare the porous micro-nano fiber, does not need high voltage of over kilovolt, has high safety factor, has no requirement on the polarity of the spinning solution, and has simple centrifugal spinning production process and high production efficiency.
Drawings
FIG. 1 is a schematic structural view of a centrifugal spinning apparatus;
FIG. 2 is a 2000-fold SEM image of the whole body porous polycaprolactone fiber prepared in example 1;
FIG. 3 is a SEM image of the whole body porous polycaprolactone fiber prepared in example 1, magnified 5000 times;
FIG. 4 is a 2000-fold SEM image of the whole body porous polycaprolactone fiber prepared in example 2;
FIG. 5 is a SEM image of the whole body porous polycaprolactone fiber prepared in example 2, magnified 5000 times;
FIG. 6 is a 2000-fold SEM image of the whole body porous polycaprolactone fiber prepared in example 3;
FIG. 7 is a SEM image of the whole body porous polycaprolactone fiber prepared in example 3, magnified 5000 times.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
The centrifugal spinning device used in embodiments 1 to 3 is shown in fig. 1, and comprises a rotating body 1 provided with a spinneret orifice 2, fan blades 3 are arranged on the outer edge of the rotating body 1, the rotating body 1 is fixed on a rotating motor 4, and collecting rods 5 are uniformly distributed around the rotating body 1. The fan blade 3 is arranged below the spinneret orifice 2, and the vertical distance between the fan blade and the spinneret orifice 2 is 3-10 cm; the number of the fan blades 3 is 2-8, and the fan blades are uniformly distributed on the outer edge of the rotating body 1. The spinneret orifices 2 are uniformly distributed around the rotating body (1), the diameter is 0.1-0.8 mm, and the number is 2-8.
Example 1
The preparation method of the full-body porous polycaprolactone fiber comprises the following steps:
(1) building a centrifugal spinning device: carrying 3 fan blades below a spinneret orifice of a traditional solution centrifugal spinning device;
(2) preparing a spinning solution: adding 1.5g of polycaprolactone into 10mL of dichloromethane, and uniformly stirring at room temperature to prepare polycaprolactone spinning solution with the concentration of 0.15 g/mL;
(3) carrying out centrifugal spinning: injecting the solution obtained in the step (2) into a spinneret, and carrying out centrifugal spinning under the parameters of the rotation number of 1500rpm/min and the receiving distance of 8cm to obtain the polycaprolactone porous fiber (shown in figures 2 and 3).
Example 2
The preparation method of the full-body porous polycaprolactone fiber comprises the following steps:
(1) building a centrifugal spinning device: carrying 3 fan blades below a spinneret orifice of a traditional solution centrifugal spinning device;
(2) preparing a spinning solution: adding 1.7g of polycaprolactone into 10mL of dichloromethane, and uniformly stirring at room temperature to prepare polycaprolactone spinning solution with the concentration of 0.17 g/mL;
(3) carrying out centrifugal spinning: injecting the solution obtained in the step (2) into a spinneret, and carrying out centrifugal spinning under the parameters of 2000rpm/min of rotation number and 10cm of receiving distance to obtain the polycaprolactone porous fiber (shown in figures 4 and 5).
Example 3
The preparation method of the full-body porous polycaprolactone fiber comprises the following steps:
(1) building a centrifugal spinning device: carrying 3 fan blades below a spinneret orifice of a traditional solution centrifugal spinning device;
(2) preparing a spinning solution: adding 1.9g of polycaprolactone into 10mL of dichloromethane, and uniformly stirring at room temperature to prepare polycaprolactone spinning solution with the concentration of 0.19 g/mL;
(3) carrying out centrifugal spinning: injecting the solution obtained in the step (2) into a spinneret, and carrying out centrifugal spinning under the parameters of the rotation speed of 2500rpm/min and the receiving distance of 12cm to obtain the polycaprolactone porous fiber (shown in figures 6 and 7).
Claims (8)
1. The full-body porous polycaprolactone fiber is characterized in that the polycaprolactone fiber is of a porous structure.
2. The full-body porous polycaprolactone fiber of claim 1, wherein the diameter of the polycaprolactone fiber is 0.5-30 μm.
3. The method for preparing the full-body porous polycaprolactone fiber according to claim 1 or 2, characterized by comprising the following steps:
step 1): adding polycaprolactone into dichloromethane, and stirring uniformly at room temperature;
step 2): injecting the solution obtained in the step 1) into a centrifugal spinning device for centrifugal spinning to obtain the porous polycaprolactone fiber.
4. The preparation method of the full-body porous polycaprolactone fiber according to claim 3, wherein the concentration of polycaprolactone in the solution obtained in the step 1) is 0.10-0.25 g/mL.
5. The preparation method of the full body porous polycaprolactone fiber according to claim 3, wherein the centrifugal spinning device in the step 2) comprises a rotating body (1) provided with a spinneret orifice (2), the outer edge of the rotating body (1) is provided with fan blades (3), the rotating body (1) is fixed on a rotating motor (4), and collecting rods (5) are uniformly distributed around the rotating body (1).
6. The preparation method of the full-body porous polycaprolactone fiber according to claim 5, wherein the fan blade (3) is arranged below the spinneret orifice (2) and has a vertical distance of 3-10 cm from the spinneret orifice (2); the number of the fan blades (3) is 2-8, and the fan blades are uniformly distributed on the outer edge of the rotating body (1).
7. The preparation method of the full-body porous polycaprolactone fiber according to claim 5, wherein the spinneret holes (2) are uniformly distributed around the rotating body (1), the diameter is 0.1-0.8 mm, and the number is 2-8.
8. The preparation method of the full-body porous polycaprolactone fiber according to claim 3, wherein the process parameters of the centrifugal spinning device in the step 2) are as follows: the rotating speed is 500-5000 rpm/min, and the receiving distance is 8-15 cm.
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| CN113882036A (en) * | 2021-11-15 | 2022-01-04 | 罗莱生活科技股份有限公司 | Polyester composite elastic fiber and production method thereof |
| CN115467107A (en) * | 2022-08-26 | 2022-12-13 | 东华大学 | Solvent vapor control system for porous yarn surface pore structure phase separation forming and porous yarn preparation method |
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Application publication date: 20200414 |