CN112941662B - Preparation method of polysulfonamide/ferroferric oxide magnetic filament - Google Patents
Preparation method of polysulfonamide/ferroferric oxide magnetic filament Download PDFInfo
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- CN112941662B CN112941662B CN202110373657.2A CN202110373657A CN112941662B CN 112941662 B CN112941662 B CN 112941662B CN 202110373657 A CN202110373657 A CN 202110373657A CN 112941662 B CN112941662 B CN 112941662B
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- polysulfonamide
- ferroferric oxide
- oxide magnetic
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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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
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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
Abstract
The invention discloses a preparation method of polysulfonamide/ferroferric oxide magnetic filament, which comprises the following steps: preparing ferroferric oxide magnetic nano particles, preparing polysulfonamide/ferroferric oxide blended spinning solution, and performing wet spinning to obtain the magnetic filaments with different cross-sectional shapes. The invention can realize the continuous wet spinning of polysulfonamide, and the preparation process is mild and controllable; according to the invention, ferroferric oxide magnetic particles are combined into polysulfonamide fibers, so that the functionalization of the polysulfonamide fibers can be realized, and the polysulfonamide fibers have magnetism; according to the invention, the ferroferric oxide magnetic particles are prepared by adopting a protein template regulation method, so that the morphology and size regulation of the ferroferric oxide magnetic particles are realized, and the nano particles are uniformly dispersed in the spinning solution; the polysulfonamide/ferroferric oxide magnetic filament prepared by the method can be used in the fields of health care, filtration, intelligent textiles and the like.
Description
Technical Field
The invention relates to the technical field of textile fiber processing, in particular to a preparation method of polysulfonamide/ferroferric oxide magnetic filaments.
Background
The polysulfonamide belongs to aromatic polyamide high-temperature resistant fibers and has the characteristics of heat resistance, thermal stability, high-temperature dimensional stability, flame retardance, electrical insulation and the like. In the existing preparation research of polysulfonamide fibers, yang designs a novel polysulfone amide/polyacrylonitrile-boehmite composite nanofiber filtering membrane by means of an electrostatic spinning technology, improves the spinnability of polysulfone amide by adding a small amount of polyacrylonitrile, introduces boehmite to construct fiber surface roughness and improves the charge storage capacity of a fiber filtering material (Xue Yang, yi Pu, shuxia Li, xiaofang Liu, zhesha Wang, ding Yuan, xin Ning. Electrospun polymer composite membrane with super thermal stability and ex chemical resistance for high efficiency PM2.5 capture. ACS Applied Materials & Interfaces 2019, 11: 43188-43199.). Li adopts a dimethylacetamide/lithium chloride dissolving system to dissolve polysulfonamide, and obtains polysulfonamide fibers through wet spinning, wherein the strength, elongation and crystallinity of the polysulfonamide fibers are respectively 4.4 cN/dtex,15.9% and 33.53% (Humin Li, yin Zhu, bing Xu, chengxun Wu, jiongxin Zhuao, mingxin Dai. Preparation and catalysis of all para position polysufonamide fiber. Journal of Applied Polymer Science 2013, 127: 342-348.). However, few studies have been made on the functionalization of polysulfonamide fibers by the preparation technology, and no studies have been reported on polysulfonamide magnetic filaments. The invention successfully obtains the polysulfonamide/ferroferric oxide magnetic filament by taking wet spinning as a means, wherein the shape and the size of the magnetic particles are regulated and controlled by adopting a gel template method for preparing the ferroferric oxide magnetic particles, and the problem of poor dispersibility of the nano particles is solved.
Disclosure of Invention
The invention aims to provide a preparation method of polysulfonamide/ferroferric oxide magnetic filament to realize functionalization of polysulfonamide.
Therefore, the invention provides a preparation method of polysulfonamide/ferroferric oxide magnetic filaments, which comprises the following steps:
(1) Dissolving ferric trichloride hexahydrate in ethylene glycol, adding sodium acetate, and uniformly stirring to obtain a mixed solution;
(2) Putting the protein gel into the mixed solution, and then transferring the protein gel into a reaction kettle;
(3) Heating the reaction kettle for reaction, and cooling to room temperature after the reaction is finished; taking out a sample in the reaction kettle, centrifugally washing, and freeze-drying to obtain ferroferric oxide magnetic nanoparticles;
(4) Mixing polysulfonamide and magnetic nanoparticles, adding the mixture into a mixed solution of dimethylacetamide and dichloromethane, and uniformly stirring at room temperature to prepare a spinning solution;
(5) Transferring the spinning solution into a wet spinning device for spinning, and preparing polysulfonamide/ferroferric oxide magnetic filaments with different cross-sectional shapes by taking water as a coagulating bath; and drying the prepared filament to obtain the polysulfonamide/ferroferric oxide magnetic filament.
Compared with the prior art, the invention has the advantages and positive effects that: the invention provides a preparation method of polysulfonamide/ferroferric oxide magnetic filament, which can realize continuous wet spinning of polysulfonamide, and has mild and controllable preparation process; according to the invention, ferroferric oxide magnetic particles are combined into polysulfonamide fibers, so that the functionalization of the polysulfonamide fibers can be realized, and the polysulfonamide fibers have magnetism; according to the invention, the ferroferric oxide magnetic particles are prepared by adopting a protein template regulation method, so that the morphology and size regulation of the ferroferric oxide magnetic particles are realized, and the nano particles are uniformly dispersed in the spinning solution; the polysulfonamide/ferroferric oxide magnetic filament prepared by the method can be used in the fields of health care, filtration, intelligent textiles and the like.
Other features and advantages of the present invention will become apparent upon reading the detailed description of the invention.
Drawings
FIG. 1 is a TEM morphology of ferroferric oxide magnetic particles in example 1 of the present invention;
FIG. 2 is an X-ray diffraction pattern of ferroferric oxide magnetic particles according to example 1 of the present invention;
fig. 3 is an SEM image of polysulfonamide/ferroferric oxide magnetic filaments of example 1 of the present invention.
Fig. 4 is a hysteresis loop diagram of ferroferric oxide (a) and polysulfonamide/ferroferric oxide magnetic filaments (b) of example 1 of the present invention.
Detailed Description
The following detailed description of the present invention is provided to illustrate and explain the present invention and should not be taken as limiting the scope of the present invention.
The preparation method of the polysulfonamide/ferroferric oxide magnetic filament comprises the following steps:
(1) Dissolving ferric trichloride hexahydrate in ethylene glycol, adding sodium acetate, and uniformly stirring to obtain a mixed solution; the mass ratio of ferric trichloride hexahydrate to sodium acetate is 1-5, and the volume ratio of ferric trichloride hexahydrate to glycol is 1;
(2) Putting the protein gel into the mixed solution, and then transferring the protein gel into a reaction kettle; the protein gel is used as a template, and the three-dimensional space provided by the protein gel can provide Fe 3 O 4 The site of growth; meanwhile, the three-dimensional space of the protein gel limits Fe 3 O 4 Unlimited growth, induction of Fe 3 O 4 Growing with a specific shape.
(3) Heating the reaction kettle for reaction, and cooling to room temperature after the reaction is finished; taking out a sample in the reaction kettle, centrifugally washing, and freeze-drying to obtain ferroferric oxide magnetic nanoparticles; the centrifugal water washing step comprises: centrifuging and washing for 3 times at 8000rpm/min for 10 min; the temperature in the oven is 180-220 ℃, and the reaction time is 10-15h;
(4) Mixing polysulfonamide and magnetic nanoparticles, adding the mixture into a mixed solution of dimethylacetamide and dichloromethane, and uniformly stirring at room temperature to prepare a spinning solution; the protein gel structure is fibrous, preferably silk fibroin fiber gel, and the mass ratio of the protein gel to ferric trichloride hexahydrate is 1; the mass ratio of the polysulfonamide to the magnetic nanoparticles is 100; the mass ratio of the dimethylacetamide to the dichloromethane is 3.4; the mass fraction of the spinning solution is 8-15%, and the polysulfonamide/ferroferric oxide magnetic filament with excellent formation can be obtained within the concentration range, and the spinning formation is difficult when the concentration range is exceeded; the mixed solution of dimethylacetamide and dichloromethane is used as a solvent, so that polysulfonamide and magnetic nanoparticles can be uniformly mixed to obtain a uniformly mixed spinning solution, and the spinning process can be smoothly and effectively implemented;
(5) Transferring the spinning solution into a wet spinning device for spinning, and preparing polysulfonamide/ferroferric oxide magnetic filaments with different cross-sectional shapes by taking water as a coagulating bath; drying the prepared filament to obtain the polysulfonamide/ferroferric oxide magnetic filament; the section of the magnetic filament is of a solid circular structure, a skin-core structure, a porous structure, a hollow structure and a special-shaped structure.
The invention provides a preparation method of polysulfonamide/ferroferric oxide magnetic filament, which can realize continuous wet spinning of polysulfonamide, and has mild and controllable preparation process; according to the invention, ferroferric oxide magnetic particles are combined into polysulfonamide fibers, so that the functionalization of the polysulfonamide fibers can be realized, and the polysulfonamide fibers have magnetism; according to the invention, the ferroferric oxide magnetic particles are prepared by adopting a protein template regulation method, so that the morphology and size regulation of the ferroferric oxide magnetic particles are realized, and the nano particles are uniformly dispersed in the spinning solution; the polysulfonamide/ferroferric oxide magnetic filament prepared by the method can be used in the fields of health care, filtration, intelligent textiles and the like.
Example 1
(1) Adding 0.45g of ferric chloride hexahydrate into 20mL of glycol, and stirring to completely dissolve; then 1.99g of sodium acetate was added, and the solution was left to stand and mixed uniformly.
(2) Transferring 0.3g of the silk fibroin fiber gel and the mixed solution of the step (1) into a 50mL reaction kettle.
(3) Placing the reaction kettle in an oven at 200 ℃, reacting for 12h, cooling to room temperature after the reaction is finished, repeatedly washing with distilled water, and centrifugally washing for 3 times at the rotating speed of 8000rpm/min, wherein each time lasts for 10 minutes; and drying the product in a freeze dryer to obtain ferroferric oxide magnetic particles.
(4) Adding the polysulfonamide and the magnetic particles into a dimethylacetamide/dichloromethane mixed solution according to the proportion of 98.
(5) Transferring the spinning solution into a wet spinning device, wherein the coagulating bath is water, the cross section of a spinneret is circular, the diameter of a spinneret orifice is 0.7mm, the spinning speed is 1 mL/min, and the winding speed is 100 cm/min, and spinning is carried out; and drying the prepared filament to obtain the polysulfonamide/ferroferric oxide magnetic filament.
Fig. 1 is a TEM topography of the ferroferric oxide magnetic particles of example 1, and it can be seen from fig. 1 that the magnetic particles are nano-scale and round nanoparticles.
Fig. 2 is an X-ray diffraction pattern of the ferroferric oxide magnetic particles in example 1, and it can be seen from the figure that characteristic peaks (220), (311), (400), (511) and (440) are all characteristic peaks of ferroferric oxide, which indicates that the preparation of ferroferric oxide is successfully realized by the protein gel template method in the present invention.
Fig. 3 is an SEM image of the polysulfonamide/ferroferric oxide magnetic filament of example 1, and it can be seen from fig. 3 that the magnetic filament is in micron-sized and has a smooth surface.
Fig. 4 is a hysteresis chart of ferroferric oxide (a) and polysulfonamide/ferroferric oxide magnetic filaments (b) in example 1, and it is clear from fig. 4 that the magnetic filaments exhibit good magnetic properties.
Example 2
(1) Adding 0.45g of ferric chloride hexahydrate into 20mL of glycol, and stirring to completely dissolve; then 1.99g of sodium acetate was added, and the solution was left to stand and mixed well.
(2) 0.3g of the silk fibroin fiber gel and the mixed solution of step (1) were transferred to a 50mL reaction vessel.
(3) Placing the reaction kettle in an oven at 200 ℃, reacting for 12h, cooling to room temperature after the reaction is finished, repeatedly washing with distilled water, and centrifugally washing for 3 times at a rotating speed of 8000rpm/min, wherein each time lasts for 10 minutes; and drying the product in a freeze dryer to obtain ferroferric oxide magnetic particles.
(4) Adding polysulfonamide and magnetic particles into a dimethylacetamide/dichloromethane mixed solution according to the ratio of 95.
(5) Transferring the spinning solution into a wet spinning device, wherein the coagulating bath is water, a spinning nozzle is triangular, the diameter of a spinning hole is 0.7mm, the spinning speed is 5 mL/min, and the winding speed is 200 cm/min, and spinning is carried out; and drying the prepared filament to obtain the polysulfonamide/ferroferric oxide magnetic filament.
Example 3
(1) Adding 0.9g of ferric chloride hexahydrate into 35mL of glycol, and stirring to completely dissolve; then 3.98g of sodium acetate is added, and the solution is kept still and mixed evenly.
(2) Transferring 0.5g of the silk fibroin fiber gel and the mixed solution of the step (1) into a 50mL reaction kettle.
(3) Placing the reaction kettle in an oven at 200 ℃, reacting for 12h, cooling to room temperature after the reaction is finished, repeatedly washing with distilled water, and centrifugally washing for 3 times at the rotating speed of 6000rpm/min, wherein each time lasts for 10 minutes; and drying the product in a freeze dryer to obtain ferroferric oxide magnetic particles.
(4) Adding the polysulfonamide and the magnetic particles into a dimethylacetamide/dichloromethane mixed solution according to a ratio of 95.
(5) Transferring the spinning solution into a wet spinning device, wherein a coagulating bath is water, a spinning nozzle is of a coaxial circular structure, an inner hole of a spinning hole is 0.5mm, an outer hole of the spinning hole is 0.9mm, the spinning speed is 5 mL/min, and the winding speed is 150 cm/min, and spinning is carried out; and drying the prepared filaments to obtain the polysulfonamide/ferroferric oxide magnetic filaments with hollow section appearances.
The above examples are only intended to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described in the foregoing embodiments, or equivalents may be substituted for some of the features thereof; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions.
Claims (6)
1. A preparation method of polysulfonamide/ferroferric oxide magnetic filaments is characterized by comprising the following steps:
(1) Dissolving ferric trichloride hexahydrate in ethylene glycol, adding sodium acetate, and uniformly stirring to obtain a mixed solution;
(2) Putting the protein gel into the mixed solution, and then moving the protein gel into a reaction kettle;
(3) Heating the reaction kettle for reaction, and cooling to room temperature after the reaction is finished; taking out a sample in the reaction kettle, centrifugally washing, and freeze-drying to obtain ferroferric oxide magnetic nanoparticles;
(4) Mixing polysulfonamide and magnetic nanoparticles, adding the mixture into a mixed solution of dimethylacetamide and dichloromethane, and uniformly stirring at room temperature to prepare a spinning solution;
(5) Transferring the spinning solution into a wet spinning device for spinning, and preparing polysulfonamide/ferroferric oxide magnetic filaments with different cross-sectional shapes by taking water as a coagulating bath; drying the prepared filament to obtain the polysulfonamide/ferroferric oxide magnetic filament;
in the step (2), the protein gel structure is fibrous and is silk fibroin fiber gel, and the mass ratio of the protein gel to ferric trichloride hexahydrate is 1;
in the step (4), the mass ratio of the polysulfonamide to the magnetic nanoparticles is 95-90;
in the step (4), the mass ratio of dimethylacetamide to dichloromethane is 3-4.
2. The method for preparing polysulfonamide/ferroferric oxide magnetic filaments according to claim 1,
in the step (1), the mass ratio of ferric trichloride hexahydrate to sodium acetate is 1-5, and the volume ratio of ferric trichloride hexahydrate to glycol is 1.
3. The method for preparing polysulfonamide/ferroferric oxide magnetic filaments according to claim 1,
in the step (3), the centrifugal water washing comprises: the washing was carried out 3 times for 10 minutes each at 8000 rpm/min.
4. The method for preparing polysulfonamide/ferroferric oxide magnetic filaments as claimed in claim 1,
in the step (3), the temperature in the oven is 180-220 ℃, and the reaction time is 10-15h.
5. The method for preparing polysulfonamide/ferroferric oxide magnetic filaments according to claim 1,
in the step (4), the mass fraction of the spinning solution is 8-15%.
6. The method for preparing polysulfonamide/ferroferric oxide magnetic filaments as claimed in claim 1,
in the step (5), the cross section of the magnetic filament is of a solid circular structure, a skin-core structure, a porous structure, a hollow structure or a special-shaped structure.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101343083A (en) * | 2008-05-15 | 2009-01-14 | 复旦大学 | Magnetic carbon sphere of surface finished C8 alkyl chain, preparation and application thereof |
| CN101724919A (en) * | 2009-08-13 | 2010-06-09 | 上海大学 | Device and method for preparing oriented polysulfonamide superfine fiber by using magnetized electrostatic spinning method |
| CN102417208A (en) * | 2011-08-08 | 2012-04-18 | 江苏大学 | Mesoporous magnetic ferriferrous oxide, its preparation method and application |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101343083A (en) * | 2008-05-15 | 2009-01-14 | 复旦大学 | Magnetic carbon sphere of surface finished C8 alkyl chain, preparation and application thereof |
| CN101724919A (en) * | 2009-08-13 | 2010-06-09 | 上海大学 | Device and method for preparing oriented polysulfonamide superfine fiber by using magnetized electrostatic spinning method |
| CN102417208A (en) * | 2011-08-08 | 2012-04-18 | 江苏大学 | Mesoporous magnetic ferriferrous oxide, its preparation method and application |
Non-Patent Citations (1)
| Title |
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| 蛋白功能化磁性纳米颗粒的制备及应用;黄天天 等;《化学进展》;20120831;第24卷(第8期);第1610-1622页 * |
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