CN108978046B - Preparation method of PET porous fiber membrane - Google Patents
Preparation method of PET porous fiber membrane Download PDFInfo
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- CN108978046B CN108978046B CN201810771709.XA CN201810771709A CN108978046B CN 108978046 B CN108978046 B CN 108978046B CN 201810771709 A CN201810771709 A CN 201810771709A CN 108978046 B CN108978046 B CN 108978046B
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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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
- D01D5/0007—Electro-spinning
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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
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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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
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The invention discloses a preparation method of a PET porous fiber membrane, which is sequentially carried out according to the following steps: the first step is drying the PET slices; the second step is to prepare mixed solute and mixed solvent; the third step is to prepare a mixed solution; the fourth step is magnetic stirring; the fifth step is that the PET/PEG composite fiber membrane is prepared by electrostatic spinning; the sixth step is that the PET porous fiber membrane is prepared by water boiling; the invention has simple steps, designs proper spinning solution by the combination of various process parameters, and prepares the porous fiber with smoothness and excellent tensile property.
Description
Technical Field
The invention relates to the technical field of electrostatic spinning, in particular to a preparation method of porous fibers.
Background
Electrospinning provides a simple and efficient method for processing solutions or melts to spin polymers into continuous fibers with diameters from a few nanometers to a few micrometers. This technique enables the efficient production of ultra-fine fibres with diameters in the range of tens to hundreds of nanometres. Electrostatic spinning is a spinning method that uses a high-voltage electric field to push polymer solution or melt to run to a spinning receiving roller in a strong electric field, and liquid drops form fibers in the running process. Because the development of the nano technology is vigorous, the electrostatic spinning technology capable of simply, conveniently and effectively producing the nano fibers can greatly brighten in many fields.
The properties of the solution have great influence on the appearance and performance of the fibers prepared by electrostatic spinning.
Influence of viscosity: when the concentration of the solution is low, the viscosity of the solution becomes lower, so that the entanglement of molecular chains is insufficient, the jet flow is unstable, the spinning uniformity is influenced, the continuous jet flow is difficult to maintain, and spun yarns are beaded and unstable jet flow can cause uneven diameters of fibers; on the contrary, when the solution concentration is higher and the solution viscosity is too high, the solution is easy to condense at the nozzle because of small solvent amount and too fast solvent volatilization, and is not sprayed any more, thereby hindering spinning and even interrupting the spinning process.
Influence of the conductivity of the spinning solution: too high or too low conductivity can lead to the production of fibers that are not smooth enough, and the smoothness of the fibers can only be ensured if the conductivity is kept in a suitable range.
The development of a spinning solution requires that the solution be adapted in all respects to the properties of electrospinning at the same time to be successful. Many development efforts have failed because the spinning solutions selected have not been able to adapt their properties to electrospinning at the same time, such as the appropriate viscosity, but not the appropriate conductivity.
PET, i.e. polyethylene terephthalate, of the formula COC6H4COOCH2CH2And O. (English: Polyethylene terephthalate, abbreviated as PET), belongs to crystalline saturated polyester, is milk white or light yellow, highly crystalline polymer, has smooth and glossy surface, and is the most important variety in thermoplastic polyester. Alias: polyethylene terephthalate; polyethylene terephthalate; the quality is ensured; polyester fiber; polyethylene terephthalate; dacron and the like, commonly known as polyester resin.
PEG, polyethylene glycol, also known as polyethylene oxide (PEO) or Polyethylene Oxide (POE), refers to an oligomer or polymer of ethylene oxide. Polyethylene glycol is soluble in water, methanol, benzene, dichloromethane, and insoluble in diethyl ether and n-hexane. The product of its binding to hydrophobic molecules can be used as a nonionic surfactant. Polyethylene glycol can be used to modify drug proteins to protect drug molecules and prolong their half-life.
At present, no method for preparing porous fiber by using PET/PEG material exists.
Disclosure of Invention
The invention aims to provide a preparation method of a PET porous fiber membrane, which can prepare porous fibers with good performance.
In order to achieve the purpose, the preparation method of the PET porous fiber membrane sequentially comprises the following steps:
the first step is drying the PET slices;
drying the PET slices in a vacuum drying oven at the temperature of 70 +/-1 ℃ for 16 +/-0.5 hours, taking out and bagging the PET slices, and storing the PET slices in a dryer for use in the second step;
the second step is to prepare mixed solute and mixed solvent;
weighing PEG and PET as mixed solutes, wherein the weight ratio of the PEG to the PET is 1: (6 ± 0.2); and simultaneously preparing a mixed solvent of trifluoroacetic acid and dichloromethane, wherein the volume ratio of the trifluoroacetic acid to the dichloromethane is 1: 1; putting the prepared mixed solvent into a clean and dry container;
the third step is to prepare a mixed solution;
weighing a mixed solute and a mixed solvent, and putting the mixed solute into the mixed solvent to prepare a mixed solution, wherein the weight concentration of the mixed solute is (16 +/-0.2)%;
the fourth step is magnetic stirring;
putting the magnetons of the magnetic stirrer into a container filled with the prepared mixed solution, sealing the container, and then putting the container into the magnetic stirrer to stir for 5 +/-0.2 hours;
the fifth step is that the PET/PEG composite fiber membrane is prepared by electrostatic spinning;
taking the mixed solution after magnetic stirring as a spinning solution, and preparing a PET/PEG composite fiber membrane by using an electrostatic spinning machine;
the sixth step is that the PET porous fiber membrane is prepared by water boiling;
putting the PET/PEG composite fiber membrane prepared in the fifth step into a glass container filled with distilled water, then putting the glass container into a constant-temperature water bath kettle at the temperature of 65 +/-0.5 ℃ to be heated for 48 +/-0.5 hours at constant temperature, and replacing the distilled water for 2-4 times in the middle to ensure that the PEG component in the PET/PEG composite fiber membrane is dissolved in the water to form a PET porous fiber membrane; and taking out the PET porous fiber film from the constant-temperature water bath kettle and drying to obtain a finished product.
In the fifth step, when the electrostatic spinning machine is used for preparing the PET/PEG composite fiber membrane, the parameters of the electrostatic spinning machine are as follows:
injecting the spinning solution into an injector of an electrostatic spinning machine, wherein the inner diameter of a needle head of the injector is 0.5 mm, a 20 mL injector is selected, the propelling speed is 0.001 mm/s, the spinning voltage is 25 kV, the rotating speed of a receiving roller of the electrostatic spinning machine is 100 r/min, the ambient temperature of the electrostatic spinning machine is 20 +/-2 ℃, and the relative humidity of ambient air is more than or equal to 45% and less than or equal to 50%; the spinning time is 4 hours to ensure that the thicknesses are similar; the thickness of the prepared PET/PEG composite fiber membrane is 150 +/-5 mu m.
In the sixth step, the PET/PEG composite fiber membrane is wrapped by plastic window screen, and then the PET/PEG composite fiber membrane is put into a glass container filled with distilled water for boiling.
The invention has simple steps, designs proper spinning solution by the combination of various process parameters, and prepares the porous fiber with smoothness and excellent tensile property.
PET and PEG are mixed and then used as solute, trifluoroacetic acid and dichloromethane are mixed in equal volume and then used as solvent, the solute is dissolved in the solvent and then mixed to form mixed solution, under the condition that the whole concentration of the solute is not changed, according to normal understanding, the higher the content of PET is, the larger the viscosity of the solution is. The inventors first determined the overall concentration of 16% and then worked into the development work because PET/PEG was 3.7: about 1, the viscosity of the solution is most suitable for electrostatic spinning, but the conductivity of the spinning solution is too high at the moment, and the prepared fiber is very unsmooth. The higher the content of PET, the lower the conductivity of the spinning solution, so the ratio of PET/PEG needs to be increased.
The inventor gradually increases the proportion of PET/PEG until the viscosity of the solution is increased to a degree which is not suitable for electrostatic spinning, and the conductivity of the spinning solution is not reduced to a degree which is suitable for electrostatic spinning, so that the quality of the prepared PET porous fiber membrane has defects all the time. Even after the total concentration was adjusted to around 16%. In this way, it was concluded that the properties of the spinning solution could not be simultaneously suitable for electrospinning.
The inventors should stop the test, but for careless inertia, the inventors continued to increase the PET/PEG ratio and tested it, surprisingly, to find that when the PET/PEG ratio exceeds 5: after 1, the viscosity of the spinning solution had decreased. The reasons for this have yet to be investigated. The inventors finally found that the ratio of PET/PEG was adjusted to 6: when the spinning solution is about 1, various parameters such as viscosity, conductivity and the like of the spinning solution are suitable for electrostatic spinning, and porous fibers with excellent performance can be prepared.
Drawings
FIG. 1 is a graph of conductivity curves for spinning solutions made in five sets of preparation processes; wherein the horizontal coordinate is the ratio of PET/PEG, the vertical coordinate is the conductivity, the unit is us/cm, namely microsiemens per centimeter;
FIG. 2 is a viscosity profile of a spinning solution made by five sets of preparation processes; wherein the horizontal coordinate is the ratio of PET/PEG, the vertical coordinate is the viscosity value, and the unit is cP, namely centipoise;
fig. 3 is a scanning electron micrograph of the PET porous fiber films prepared in the first, second, third and fifth groups.
Detailed Description
The invention discloses a preparation method of a PET porous fiber membrane, which is sequentially carried out according to the following steps:
the first step is drying the PET slices;
drying the PET slices in a vacuum drying oven at the temperature of 70 +/-1 ℃ (preferably 70 ℃) for 16 +/-0.5 hours (preferably 16 hours), taking out and bagging the PET slices, and storing the PET slices in a dryer for use in the second step;
the second step is to prepare mixed solute and mixed solvent;
weighing PEG and PET as mixed solutes, wherein the weight ratio of the PEG to the PET is 1: (6 ± 0.2); and simultaneously preparing a mixed solvent of trifluoroacetic acid and dichloromethane, wherein the volume ratio of the trifluoroacetic acid to the dichloromethane is 1: 1; putting the prepared mixed solvent into a clean and dry container (such as an iodine measuring flask);
the third step is to prepare a mixed solution;
weighing a mixed solute and a mixed solvent, and putting the mixed solute into the mixed solvent to prepare a mixed solution, wherein the weight concentration of the mixed solute is (16 +/-0.2)%, preferably 16%;
the fourth step is magnetic stirring;
putting the magnetons of the magnetic stirrer into a container filled with the prepared mixed solution, sealing the container, and then putting the container into the magnetic stirrer to stir for 5 +/-0.2 hours, preferably 5 hours;
the fifth step is that the PET/PEG composite fiber membrane is prepared by electrostatic spinning;
taking the mixed solution after magnetic stirring as a spinning solution, and preparing a PET/PEG composite fiber membrane by using an electrostatic spinning machine;
the sixth step is that the PET porous fiber membrane is prepared by water boiling;
putting the PET/PEG composite fiber membrane prepared in the fifth step into a glass container filled with distilled water, then putting the glass container into a constant-temperature water bath kettle with 65 +/-0.5 ℃ (preferably 65 ℃) to be heated for 48 +/-0.5 hours (preferably 48 hours) at constant temperature, and replacing the distilled water for 2-4 times in the middle to ensure that the PEG component in the PET/PEG composite fiber membrane is dissolved in the water to form a PET porous fiber membrane; and taking out the PET porous fiber film from the constant-temperature water bath kettle and drying to obtain a finished product.
In the fifth step, when the electrostatic spinning machine is used for preparing the PET/PEG composite fiber membrane, the parameters of the electrostatic spinning machine are as follows:
injecting the spinning solution into an injector of an electrostatic spinning machine, wherein the inner diameter of a needle head of the injector is 0.5 mm, a 20 mL injector is selected, the propelling speed is 0.001 mm/s, the spinning voltage is 25 kV, the rotating speed of a receiving roller of the electrostatic spinning machine is 100 r/min, the ambient temperature of the electrostatic spinning machine is 20 +/-2 ℃, and the relative humidity of ambient air is more than or equal to 45% and less than or equal to 50%; the spinning time is 4 hours; the thickness of the prepared PET/PEG composite fiber membrane is 150 +/-5 mu m.
In the sixth step, the PET/PEG composite fiber membrane is wrapped by plastic window screen, and then the PET/PEG composite fiber membrane is put into a glass container filled with distilled water for boiling.
Therefore, the severe shrinkage of the fiber membrane caused by water boiling in the process of dissolving and removing PEG in water can be prevented, and the quality of the prepared PET porous fiber membrane is ensured.
The inventors have conducted five groups of preparations to illustrate the effect of the weight ratio of PEG to PET on the quality of the PET porous fiber membrane.
In the first and second steps, the weight ratio of PEG to PET is 1: 2.
and in the second step, the weight ratio of PEG to PET is 1: 4.
and in the third group, in the second step, the weight ratio of PEG to PET is 1: 6.
and in the second step, the weight ratio of PEG to PET is 1: 8.
and a fifth group, wherein in the second step, the weight ratio of PEG to PET is 1: 10.
measuring the conductivity of the mixed solution prepared in the third step in the five preparation processes by using a DDS-11A type conductivity meter produced by Shanghai RimXinjing instruments Co., Ltd to obtain a graph 1; the viscosity was measured using a viscosity measuring instrument (preferably, an NDJ-8S rotary viscometer manufactured by Shanghai Farre instruments Co., Ltd.) to obtain FIG. 2.
As can be seen from fig. 1, as the PET content increases, the conductivity of the spinning solution gradually decreases; as can be seen from fig. 2, as the content of PET gradually increases from small to large, the viscosity of the spinning solution gradually increases, but the weight ratio of PET to PEG increases to 1: and when the weight ratio of the PET to the PEG is continuously increased, the viscosity of the spinning solution is reduced, so that the possibility of preparing the PET/PEG solution with various parameters suitable for electrostatic spinning is provided.
And (3) carrying out tensile test on the PET porous fiber membranes prepared in the five groups of preparation processes through an XQ-1A type fiber strength elongation instrument produced by Shanghai RieJing instruments Co., Ltd, and testing the breaking strength of the PET porous fiber membranes obtained in each group of preparation processes.
The test results are shown in table 1:
| PEG/PET | 1: 2 | 1:4 | 1:6 | 1:8 | 1:10 |
| breaking strength (cN) | 8.65 | 53.93 | 61.83 | 71.29 | 72.94 |
| Membrane area (mm)2) | 0.49 | 0.74 | 0.37 | 0.42 | 0.33 |
| Breaking Strength of fiber film (MPa) | 0.18 | 0.73 | 0.94 | 1.71 | 2.21 |
As can be seen from table 1, the rupture strength of the PET porous fiber membrane gradually increased with the increase of the content of PET, and the weight ratio of PEG to PET was 1: when 2 (first group), the rupture strength of the PET porous fiber membrane was too low, meaning that the strength of the PET porous fiber membrane was insufficient. The strength of the PET porous fiber membranes prepared by the other groups is obviously higher than that of the PET porous fiber membrane prepared by the first group, and the PET porous fiber membranes can meet the quality requirements of normal PET porous fiber membranes (such as the PET porous fiber membranes used in the membrane separation field and the filtration field).
Fig. 3 is a scanning electron microscope photograph of the PET porous fiber films prepared from the first, second, third and fifth groups using a FEI Quanta 250 type scanning electron microscope manufactured by czech FEI corporation. In the photograph, the numbers "2: the 1' part is the scanning electron microscope picture of the first group of prepared PET porous fiber film; labeled "4: the 1' part is the scanning electron microscope picture of the second group of prepared PET porous fiber film; labeled "6: the 1' part is a scanning electron microscope picture of the PET porous fiber film prepared by the third group; labeled "10: the 1 "part is the scanning electron micrograph of the PET porous fiber membrane prepared in the fifth group.
As can be seen from the comparison in fig. 3, irregular pores are formed on the fiber surfaces of the PET porous fiber films prepared in the first and second groups, and the quality of the PET porous fiber films is poor. This is because when the PEG content is too high, PEG plays a very important supporting role for the structure of the fiber. After being removed by boiling in water, the porous fiber forms too large holes due to the high content of PEG, and partial area of the porous fiber is not enough to support, so that collapse is formed.
As can be seen from the comparison in fig. 3, the porous PET fiber membranes prepared in the third and fifth groups had relatively few voids formed on the fiber surface, and the voids were much smaller. The third group of prepared PET porous fiber membranes have the most smooth fibers, the most uniform fiber diameters and the most regular fiber arrangement, and the best quality of the PET porous fiber membranes are expected to be used in the fields of membrane separation technology, filtration and the like.
Although the present invention has been described in detail with reference to the above embodiments, it should be understood by those skilled in the art that: modifications and equivalents may be made thereto without departing from the spirit and scope of the invention and it is intended to cover in the claims the invention as defined in the appended claims.
Claims (1)
- The preparation method of the PET porous fiber membrane is characterized by comprising the following steps in sequence:the first step is drying the PET slices;drying the PET slices in a vacuum drying oven at the temperature of 70 +/-1 ℃ for 16 +/-0.5 hours, taking out and bagging the PET slices, and storing the PET slices in a dryer for use in the second step;the second step is to prepare mixed solute and mixed solvent;weighing PEG and PET as mixed solutes, wherein the weight ratio of the PEG to the PET is 1: (6 ± 0.2); and simultaneously preparing a mixed solvent of trifluoroacetic acid and dichloromethane, wherein the volume ratio of the trifluoroacetic acid to the dichloromethane is 1: 1; putting the prepared mixed solvent into a clean and dry container;the third step is to prepare a mixed solution;weighing a mixed solute and a mixed solvent, and putting the mixed solute into the mixed solvent to prepare a mixed solution, wherein the weight concentration of the mixed solute is (16 +/-0.2)%;the fourth step is magnetic stirring;putting the magnetons of the magnetic stirrer into a container filled with the prepared mixed solution, sealing the container, and then putting the container into the magnetic stirrer to stir for 5 +/-0.2 hours;the fifth step is that the PET/PEG composite fiber membrane is prepared by electrostatic spinning;taking the mixed solution after magnetic stirring as a spinning solution, and preparing a PET/PEG composite fiber membrane by using an electrostatic spinning machine;the sixth step is that the PET porous fiber membrane is prepared by water boiling;putting the PET/PEG composite fiber membrane prepared in the fifth step into a glass container filled with distilled water, and then putting the glass container into a constant-temperature water bath kettle at the temperature of 65 +/-0.5 ℃ to be heated at the constant temperature for 48 +/-0.5 hours, so that the PEG component in the PET/PEG composite fiber membrane is dissolved in water to form a PET porous fiber membrane; taking out the PET porous fiber film from the constant-temperature water bath pot and drying to obtain a finished product;in the fifth step, when the electrostatic spinning machine is used for preparing the PET/PEG composite fiber membrane, the parameters of the electrostatic spinning machine are as follows:injecting the spinning solution into an injector of an electrostatic spinning machine, wherein the inner diameter of a needle head of the injector is 0.5 mm, the propelling speed is 0.001 mm/s, the spinning voltage is 25 kV, the rotating speed of a receiving roller of the electrostatic spinning machine is 100 r/min, the ambient temperature of the electrostatic spinning machine is 20 +/-2 ℃, and the relative humidity of ambient air is more than or equal to 45% and less than or equal to 50%; the spinning time is 4 hours; the thickness of the prepared PET/PEG composite fiber membrane is 150 +/-5 mu m;in the sixth step, the PET/PEG composite fiber membrane is wrapped by plastic window screen, and then the PET/PEG composite fiber membrane is put into a glass container filled with distilled water for boiling.
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