CN111996792A - Preparation method of magnetic self-cleaning fiber - Google Patents
Preparation method of magnetic self-cleaning fiber Download PDFInfo
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- CN111996792A CN111996792A CN202010831831.9A CN202010831831A CN111996792A CN 111996792 A CN111996792 A CN 111996792A CN 202010831831 A CN202010831831 A CN 202010831831A CN 111996792 A CN111996792 A CN 111996792A
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- ferroferric oxide
- magnetic
- silicon dioxide
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- fiber
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- 239000000835 fiber Substances 0.000 title claims abstract description 76
- 238000004140 cleaning Methods 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 79
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 75
- 239000000243 solution Substances 0.000 claims abstract description 44
- 239000002244 precipitate Substances 0.000 claims abstract description 43
- 239000004005 microsphere Substances 0.000 claims abstract description 37
- 238000001035 drying Methods 0.000 claims abstract description 34
- 239000007864 aqueous solution Substances 0.000 claims abstract description 26
- 238000003756 stirring Methods 0.000 claims abstract description 25
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 19
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 18
- 239000011258 core-shell material Substances 0.000 claims abstract description 17
- QWMFKVNJIYNWII-UHFFFAOYSA-N 5-bromo-2-(2,5-dimethylpyrrol-1-yl)pyridine Chemical compound CC1=CC=C(C)N1C1=CC=C(Br)C=N1 QWMFKVNJIYNWII-UHFFFAOYSA-N 0.000 claims abstract description 12
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000004809 Teflon Substances 0.000 claims abstract description 9
- 229920006362 Teflon® Polymers 0.000 claims abstract description 9
- 238000007789 sealing Methods 0.000 claims abstract description 9
- 239000002002 slurry Substances 0.000 claims abstract description 9
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000002431 foraging effect Effects 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 33
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 30
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 30
- 239000000047 product Substances 0.000 claims description 26
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 16
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 11
- 230000005588 protonation Effects 0.000 claims description 9
- 229910002804 graphite Inorganic materials 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 239000010439 graphite Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 229910052797 bismuth Inorganic materials 0.000 description 13
- 239000005871 repellent Substances 0.000 description 11
- 238000005406 washing Methods 0.000 description 11
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000007885 magnetic separation Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 4
- 239000004744 fabric Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 239000004753 textile Substances 0.000 description 4
- 239000011941 photocatalyst Substances 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000006552 photochemical reaction Methods 0.000 description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000001453 impedance spectrum Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- FGHSTPNOXKDLKU-UHFFFAOYSA-N nitric acid;hydrate Chemical compound O.O[N+]([O-])=O FGHSTPNOXKDLKU-UHFFFAOYSA-N 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 210000002374 sebum Anatomy 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- -1 tungstate ions Chemical class 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/49—Oxides or hydroxides of elements of Groups 8, 9,10 or 18 of the Periodic Table; Ferrates; Cobaltates; Nickelates; Ruthenates; Osmates; Rhodates; Iridates; Palladates; Platinates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/48—Oxides or hydroxides of chromium, molybdenum or tungsten; Chromates; Dichromates; Molybdates; Tungstates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
- D06M11/64—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
- D06M11/65—Salts of oxyacids of nitrogen
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses a preparation method of magnetic self-cleaning performance fiber, which comprises the steps of preparing ferroferric oxide @ silicon dioxide composite microspheres with a core-shell structure, dispersing the composite microspheres in a nitric acid solution to generate ferroferric oxide @ silicon dioxide magnetic cores, adding a solution containing the magnetic cores into a sodium tungstate aqueous solution for aging, magnetically separating black precipitates in an aqueous solution, dispersing the black precipitates in the nitric acid aqueous solution, adding a mixture consisting of graphite phase carbon nitride, sodium tungstate dihydrate and bismuth nitrate pentahydrate into the solution, suspending the mixture in a liner of a Teflon high-pressure autoclave for sealing, putting the liner back into the high-pressure autoclave for heating, taking out, magnetically separating the precipitates, drying to obtain a magnetic composite material, adding the magnetic composite material into fiber slurry, uniformly stirring to ensure that the magnetic composite material is uniformly attached to the fiber, and drying the fiber to obtain the magnetic self-cleaning fiber.
Description
Technical Field
The invention belongs to the technical field of textile engineering, and relates to a preparation method of a magnetic self-cleaning fiber.
Background
In daily life, a human body is stained with water and oil carelessly during wearing, and is stained with a lot of sweat, sebum and other various human body secretions, and the stains not only influence the use of people, but also are good environments for microbial propagation. In order to solve this problem, there is a constant effort to pursue self-cleaning textiles and their self-cleaning fibers.
At present, the self-cleaning fibers on the market are mainly divided into three types: firstly, the self-cleaning fiber containing water-repellent and oil-repellent finishing agent type; self-cleaning fiber of fluorine-containing water-repellent and oil-repellent finishing agent; and thirdly, the nano photocatalyst-containing fiber. A self-cleaning fiber containing a water-repellent and oil-repellent finishing agent is characterized in that functional after-finishing is carried out on textiles through various water-repellent and oil-repellent finishing agents, the surface performance of the fiber is changed, the surface tension of the fiber is lower than that of water and oil, water drops and oil stains cannot be spread on the surface of the fabric and can be easily shaken off, and original dust on the surface of the fabric can be taken away by the water drops in the process of slipping off, so that the purpose of self-cleaning the textiles is achieved. The fluorine-containing water-repellent and oil-repellent finishing agent self-cleaning fiber is used more at present. The photocatalyst fiber containing nano-photocatalyst adopts the principle of water repellency and self-cleaning of lotus leaves, and is mainly characterized in the microstructure rather than the chemical components. The nano-scale particles are added on the surface of the fabric, so that the roughness is improved to form nano-scale papilla bulges, and the water and oil repellent effect is achieved, so that the fabric has the self-cleaning capability. However, the preparation process of these self-cleaning fibers is complex, and the self-cleaning ability is poor, so that the actual requirements of people cannot be met.
Disclosure of Invention
The invention aims to provide a preparation method of a magnetic self-cleaning fiber, which solves the problems that the existing self-cleaning fiber is complex in preparation process and the prepared fiber is poor in self-cleaning capability.
The technical scheme adopted by the invention is that the preparation method of the magnetic self-cleaning fiber comprises the following steps:
step 3, dispersing the black precipitate in a nitric acid aqueous solution, adding a mixture consisting of graphite-phase carbon nitride, sodium tungstate dihydrate and bismuth nitrate pentahydrate into the solution, suspending the mixture in a liner of a Teflon high-pressure autoclave, sealing, putting the liner back into the high-pressure autoclave, heating to 150-240 ℃, keeping the temperature for a period of time, taking out, magnetically separating out the precipitate, and finally drying the precipitate to obtain the magnetic composite material;
and 4, adding the magnetic composite material into the fiber slurry, uniformly stirring to ensure that the magnetic composite material is uniformly attached to the fibers, and drying the fibers to obtain the magnetic self-cleaning fiber.
The present invention is also technically characterized in that,
the specific process of step 1 is as follows:
adding ferroferric oxide powder into an absolute ethyl alcohol and ammonia water mixed solution, stirring uniformly at room temperature, then adding tetraethoxysilane into the solution, magnetically separating a black product in the solution after stirring uniformly, cleaning the separated black product with absolute ethyl alcohol, and finally drying the black product to obtain the ferroferric oxide @ silicon dioxide composite microsphere with the core-shell structure.
In the step 1, finally, drying the black product at the temperature of 40-80 ℃ for 5-12 h.
In the step 1, the mass ratio of the ferroferric oxide powder to the tetraethoxysilane is 0.015-15: 0.045-4.5.
The mass ratio of the ferroferric oxide powder to the graphite-phase carbon nitride is 0.015-15: 0.0138-13.8, wherein the mass ratio of the ferroferric oxide powder to the sodium tungstate dihydrate is 0.015-15: 0.02475-2.475, wherein the mass ratio of the ferroferric oxide powder to the bismuth nitrate pentahydrate is (0.015-15): 0.07275-7.275.
The volume ratio of the absolute ethyl alcohol and ammonia water mixed solution is 12-1200: 0.35-35% of absolute ethyl alcohol and 28 wt% of ammonia water.
And step 3, putting the lining back into the high-pressure kettle, heating to 150-240 ℃, preserving heat for 15-96 h, and taking out.
And in the step 3, finally drying the precipitate at the drying temperature of 40-80 ℃ for 2-36 h.
The invention has the beneficial effects that ferroferric oxide @ silicon dioxide composite microspheres are prepared by adopting ferroferric oxide, absolute ethyl alcohol, ammonia water and ethyl orthosilicate, protonation and aging treatment are carried out on the ferroferric oxide @ silicon dioxide composite microspheres, the ferroferric oxide @ silicon dioxide composite microspheres are added into a mixture of graphite-phase carbon nitride, sodium tungstate dihydrate and bismuth nitrate pentahydrate, heating and drying are carried out to prepare a magnetic composite material, the magnetic composite material is attached to fibers, under the condition of illumination, a hole-electron pair formed by photochemical reaction of the magnetic composite material is generated, organic dirt on the surfaces of the fibers can be oxidized into water and other harmless substances, and then the harmless substances automatically fall off under the action of natural external forces such as gravity, wind power, rainwater and the like, so that the.
Drawings
FIG. 1 is an evaluation diagram of rhodamine B photocatalytic degradation of the magnetic composite material prepared in example 1 of the present invention;
FIG. 2 is a photocurrent measurement spectrum of a magnetic composite prepared in example 1 of the present invention;
fig. 3 is a graph of an electrochemical impedance plot of the magnetic composite material prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of a magnetic self-cleaning fiber, which comprises the following steps:
Adding 0.015-15 g of ferroferric oxide powder into 12-1200 mL of anhydrous ethanol and ammonia water mixed solution, stirring for 0.05-5 h at room temperature, adding 0.045-4.5 g of ethyl orthosilicate into the solution, continuously and mechanically stirring for 0.5-8.0 h, magnetically separating a black product in the solution, cleaning the separated black product with a large amount of anhydrous ethanol, and finally drying the black product at 40-80 ℃ for 5-12 h to obtain the ferroferric oxide @ silicon dioxide composite microsphere with the core-shell structure.
Wherein the volume ratio of the absolute ethyl alcohol and the ammonia water mixed solution is 12-1200: 0.35-35% of absolute ethyl alcohol and 28 wt% of ammonia water.
step 3, washing the black precipitate with deionized water, dispersing the black precipitate in 6.5-650 mL of nitric acid aqueous solution, adding a mixture consisting of 0.0138-13.8 g of graphite-phase carbon nitride, 0.02475-2.475 g of sodium tungstate dihydrate and 0.07275-7.275 g of bismuth nitrate pentahydrate into the solution, suspending the mixture in a liner of a Teflon high-pressure autoclave, sealing the liner, putting the liner back into the high-pressure autoclave, heating the liner to 150-240 ℃, keeping the temperature for 15-96 hours, taking out the liner, magnetically separating the precipitate, and finally drying the precipitate at 40-80 ℃ for 2-36 hours to obtain the magnetic composite material;
and 4, adding the magnetic composite material into the fiber slurry, uniformly stirring to ensure that the magnetic composite material is uniformly attached to the fibers, and drying the fibers to obtain the magnetic self-cleaning fiber.
Example 1
Preparing a magnetic self-cleaning fiber, comprising the following steps:
Adding 0.15g of ferroferric oxide powder into 123.5mL of anhydrous ethanol and ammonia water mixed solution, wherein the anhydrous ethanol and ammonia water mixed solution is formed by mixing 120mL of anhydrous ethanol and 3.5mL of ammonia water, the concentration of the used ammonia water is 28 wt%, stirring at room temperature for 0.5h, gradually adding 0.45g of ethyl orthosilicate into the solution, continuously and mechanically stirring for 8.0h, then magnetically separating a black product in the solution, washing the separated black product with a large amount of anhydrous ethanol, and finally drying the black product at 60 ℃ for 12h to obtain the ferroferric oxide @ silicon dioxide composite microspheres with the core-shell structure.
step 3, washing the black precipitate with deionized water, dispersing the black precipitate in 65mL of nitric acid aqueous solution, adding a mixture consisting of 0.138g of graphite-phase carbon nitride, 0.2475g of sodium tungstate dihydrate and 0.7275g of bismuth nitrate pentahydrate into the solution, suspending the mixture in a liner of a Teflon high-pressure kettle, sealing the liner, putting the liner back into the high-pressure kettle, heating to 180 ℃, keeping the temperature for 24 hours, taking out the liner, magnetically separating out the precipitate, and finally drying the precipitate at 80 ℃ for 12 hours to obtain the magnetic composite material;
FIG. 1 is an evaluation chart of rhodamine B photocatalytic degradation for the magnetic composite material prepared in example 1, from which it can be seen that3N4Compared with FSB (ferroferric oxide @ silicon dioxide @ bismuth tungstate), the magnetic composite material FSBG (ferroferric oxide @ silicon dioxide @ bismuth tungstate @ graphite phase carbon nitride) prepared by the method has higher photocatalytic activity.
Fig. 2 is a photocurrent test spectrum of the magnetic composite material prepared in example 1, wherein a to f represent ferroferric oxide, ferroferric oxide @ silica, bismuth tungstate, graphite-phase carbon nitride, ferroferric oxide @ silica @ bismuth tungstate @ graphite-phase carbon nitride, respectively, and it can be seen from the graph that the magnetic composite material (ferroferric oxide @ silica @ bismuth tungstate @ graphite-phase carbon nitride) prepared in the present application has the highest photocurrent intensity compared to the ferroferric oxide, ferroferric oxide @ silica, bismuth tungstate, ferroferric oxide @ silica @ bismuth tungstate @ graphite-phase carbon nitride, which indicates that the magnetic composite material (ferroferric oxide silica @ bismuth tungstate @ graphite-phase carbon nitride) prepared in the present application can effectively improve the separation efficiency of photo-generated carriers.
Fig. 3 is an electrochemical impedance spectrum of the magnetic composite material prepared in example 1, wherein a to f represent ferroferric oxide, ferroferric oxide @ silica, bismuth tungstate, graphite-phase carbon nitride, ferroferric oxide @ silica @ bismuth tungstate and graphite-phase carbon nitride, respectively, and it can be seen from the diagram that the magnetic composite material prepared in the present application (ferroferric oxide @ silica @ bismuth tungstate and graphite-phase carbon nitride) has the smallest impedance radius compared with the ferroferric oxide, ferroferric oxide @ silica, bismuth tungstate, ferroferric oxide @ silica @ bismuth tungstate and graphite-phase carbon nitride, which indicates that the transfer rate of the photo-generated carrier at the interface of the material is the fastest.
And 4, adding the magnetic composite material into the fiber slurry, uniformly stirring to ensure that the magnetic composite material is uniformly attached to the fibers, and drying the fibers to obtain the magnetic self-cleaning fiber. Under the condition of illumination, the magnetic composite material on the surface of the magnetic self-cleaning fiber generates a hole-electron pair formed by photochemical reaction, and the hole-electron pair is combined with organic dirt on the surface of the fiber to generate an oxidation-reduction reaction, so that the hole-electron pair can be thoroughly oxidized into water and other harmless substances; moreover, the hole-electron pair can also react with water on the surface of the fiber or in the surrounding air to generate active substances such as active oxygen, hydroxyl free radicals and the like, and the active substances have extremely strong oxidation action and can not only oxidize and destroy microorganisms, but also completely oxidize and destroy organic chemical pollutants on the fiber, thereby playing roles in cleaning the environment, deodorizing and the like. The filth on the surface of the fiber can easily fall off automatically or be removed by photocatalytic degradation under the action of gravity, wind power, rainwater and other natural external forces, and the aim of self-cleaning is effectively fulfilled.
Example 2
Preparing a magnetic self-cleaning fiber, comprising the following steps:
Adding 0.015g of ferroferric oxide powder into 12.35mL of anhydrous ethanol and ammonia water mixed solution, wherein the anhydrous ethanol and ammonia water mixed solution is formed by mixing 12mL of anhydrous ethanol and 0.35mL of ammonia water, the concentration of the used ammonia water is 28 wt%, stirring at room temperature for 0.05h, gradually adding 0.045g of ethyl orthosilicate into the solution, continuously and mechanically stirring for 2.0h, then magnetically separating a black product in the solution, washing the separated black product with a large amount of anhydrous ethanol, and finally drying the black product at 40 ℃ for 5h to obtain the ferroferric oxide @ silicon dioxide composite microsphere with the core-shell structure.
step 3, washing the black precipitate with deionized water, dispersing the black precipitate in 7mL of nitric acid aqueous solution, adding a mixture consisting of 0.05g of graphite-phase carbon nitride, 0.12g of sodium tungstate dihydrate and 0.355g of bismuth nitrate pentahydrate into the solution, suspending the mixture in a liner of a Teflon high-pressure kettle, sealing the liner, putting the liner back into the high-pressure kettle, heating to 150 ℃, keeping the temperature for 18 hours, taking out the liner, magnetically separating out the precipitate, and finally drying the precipitate at 50 ℃ for 5 hours to obtain the magnetic composite material;
and 4, adding the magnetic composite material into the fiber slurry, uniformly stirring to ensure that the magnetic composite material is uniformly attached to the fibers, and drying the fibers to obtain the magnetic self-cleaning fiber.
Example 3
Preparing a magnetic self-cleaning fiber, comprising the following steps:
Adding 1.5g of ferroferric oxide powder into 520mL of anhydrous ethanol and ammonia water mixed solution, wherein the anhydrous ethanol and ammonia water mixed solution is formed by mixing 500mL of anhydrous ethanol and 20mL of ammonia water, the concentration of the used ammonia water is 28 wt%, stirring at room temperature for 2h, gradually adding 1.5g of ethyl orthosilicate into the solution, continuously and mechanically stirring for 3h, magnetically separating a black product in the solution, washing the separated black product with a large amount of anhydrous ethanol, and finally drying the black product at 50 ℃ for 8h to obtain the ferroferric oxide @ silicon dioxide composite microspheres with the core-shell structures.
step 3, washing the black precipitate with deionized water, dispersing the black precipitate in 25mL of nitric acid water solution, adding a mixture consisting of 0.08g of graphite-phase carbon nitride, 0.163g of sodium tungstate dihydrate and 0.62g of bismuth nitrate pentahydrate into the solution, suspending the mixture in a liner of a Teflon high-pressure kettle, sealing the liner, putting the liner back into the high-pressure kettle, heating to 220 ℃, keeping the temperature for 50 hours, taking out the liner, magnetically separating out the precipitate, and finally drying the precipitate at 60 ℃ for 10 hours to obtain the magnetic composite material;
and 4, adding the magnetic composite material into the fiber slurry, uniformly stirring to ensure that the magnetic composite material is uniformly attached to the fibers, and drying the fibers to obtain the magnetic self-cleaning fiber.
Example 4
Preparing a magnetic self-cleaning fiber, comprising the following steps:
Adding 13g of ferroferric oxide powder into 800mL of anhydrous ethanol and ammonia water mixed solution, wherein the anhydrous ethanol and ammonia water mixed solution is formed by mixing 770mL of anhydrous ethanol and 30mL of ammonia water, the concentration of the used ammonia water is 28 wt%, stirring at room temperature for 3h, gradually adding 3.0g of ethyl orthosilicate into the solution, continuously and mechanically stirring for 6.0h, magnetically separating a black product in the solution, washing the separated black product with a large amount of anhydrous ethanol, and finally drying the black product at 70 ℃ for 10h to obtain the ferroferric oxide @ silicon dioxide composite microspheres with the core-shell structures.
step 3, washing the black precipitate with deionized water, dispersing the black precipitate in 400mL of nitric acid aqueous solution, adding a mixture consisting of 8.2g of graphite-phase carbon nitride, 1.75g of sodium tungstate dihydrate and 4.15g of bismuth nitrate pentahydrate into the solution, suspending the mixture in a liner of a Teflon high-pressure kettle, sealing the liner, putting the liner back into the high-pressure kettle, heating to 220 ℃, keeping the temperature for 74 hours, taking out the liner, magnetically separating out the precipitate, and finally drying the precipitate at 70 ℃ for 22 hours to obtain the magnetic composite material;
and 4, adding the magnetic composite material into the fiber slurry, uniformly stirring to ensure that the magnetic composite material is uniformly attached to the fibers, and drying the fibers to obtain the magnetic self-cleaning fiber.
Example 5
Preparing a magnetic self-cleaning fiber, comprising the following steps:
Adding 15g of ferroferric oxide powder into 1200mL of anhydrous ethanol and ammonia water mixed solution, wherein the anhydrous ethanol and ammonia water mixed solution is formed by mixing 1165mL of anhydrous ethanol and 35mL of ammonia water, the concentration of the used ammonia water is 28 wt%, stirring at room temperature for 5h, gradually adding 4.5g of ethyl orthosilicate into the solution, continuously mechanically stirring for 8.0h, magnetically separating a black product in the solution, washing the separated black product with a large amount of anhydrous ethanol, and finally drying the black product at 80 ℃ for 12h to obtain the ferroferric oxide @ silicon dioxide composite microspheres with the core-shell structures.
step 3, washing the black precipitate with deionized water, dispersing the black precipitate in 650mL of nitric acid aqueous solution, adding a mixture consisting of 13.8g of graphite-phase carbon nitride, 2.4g of sodium tungstate dihydrate and 7.275g of bismuth nitrate pentahydrate into the solution, suspending the mixture in a liner of a Teflon high-pressure kettle, sealing the liner, putting the liner back into the high-pressure kettle, heating to 240 ℃, keeping the temperature for 96 hours, taking out the liner, magnetically separating out the precipitate, and finally drying the precipitate at 80 ℃ for 36 hours to obtain the magnetic composite material;
and 4, adding the magnetic composite material into the fiber slurry, uniformly stirring to ensure that the magnetic composite material is uniformly attached to the fibers, and drying the fibers to obtain the magnetic self-cleaning fiber.
Claims (8)
1. A preparation method of magnetic self-cleaning fiber is characterized by comprising the following steps:
step 1, preparing ferroferric oxide @ silicon dioxide composite microspheres with core-shell structures;
step 2, dispersing the ferroferric oxide @ silicon dioxide composite microspheres in a diluted nitric acid solution to carry out a rapid protonation process, forming a layer of positive charges on the surfaces of the ferroferric oxide @ silicon dioxide composite microspheres to generate ferroferric oxide @ silicon dioxide magnetic cores, adding a solution containing the ferroferric oxide @ silicon dioxide magnetic cores into a sodium tungstate aqueous solution for aging, and then magnetically separating black precipitates in an aqueous solution;
step 3, dispersing the black precipitate in a nitric acid aqueous solution, adding a mixture consisting of graphite-phase carbon nitride, sodium tungstate dihydrate and bismuth nitrate pentahydrate into the solution, suspending the mixture in a liner of a Teflon high-pressure autoclave, sealing, putting the liner back into the high-pressure autoclave, heating to 150-240 ℃, keeping the temperature for a period of time, taking out, magnetically separating out the precipitate, and finally drying the precipitate to obtain the magnetic composite material;
and 4, adding the magnetic composite material into the fiber slurry, uniformly stirring to ensure that the magnetic composite material is uniformly attached to the fibers, and drying the fibers to obtain the magnetic self-cleaning fiber.
2. The method for preparing a magnetic self-cleaning fiber according to claim 1, wherein the specific process of step 1 is as follows:
adding ferroferric oxide powder into an absolute ethyl alcohol and ammonia water mixed solution, stirring uniformly at room temperature, then adding tetraethoxysilane into the solution, magnetically separating a black product in the solution after stirring uniformly, cleaning the separated black product with absolute ethyl alcohol, and finally drying the black product to obtain the ferroferric oxide @ silicon dioxide composite microsphere with the core-shell structure.
3. The method for preparing the magnetic self-cleaning fiber as claimed in claim 2, wherein in the step 1, the black product is finally dried, the drying temperature is 40-80 ℃, and the drying time is 5-12 h.
4. The preparation method of the magnetic self-cleaning fiber according to claim 2, wherein in the step 1, the mass ratio of the ferroferric oxide powder to the tetraethoxysilane is 0.015-15: 0.045-4.5.
5. The preparation method of the magnetic self-cleaning fiber according to claim 4, wherein the mass ratio of the ferroferric oxide powder to the graphite-phase carbon nitride is 0.015-15: 0.0138-13.8, wherein the mass ratio of the ferroferric oxide powder to the sodium tungstate dihydrate is 0.015-15: 0.02475-2.475, wherein the mass ratio of the ferroferric oxide powder to the bismuth nitrate pentahydrate is (0.015-15): 0.07275-7.275.
6. The preparation method of the magnetic self-cleaning fiber as claimed in claim 1, wherein the volume ratio of the absolute ethyl alcohol + ammonia water mixed solution is 12-1200: 0.35-35% of absolute ethyl alcohol and 28 wt% of ammonia water.
7. The method for preparing the magnetic self-cleaning fiber as claimed in claim 1, wherein in the step 3, the lining is placed back into the autoclave to be heated to 150-240 ℃ and kept warm for 15-96 h, and then taken out.
8. The method for preparing the magnetic self-cleaning fiber as claimed in claim 1, wherein in the step 3, the precipitate is finally dried, the drying temperature is 40-80 ℃, and the drying time is 2-36 h.
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