CN111013667B - Photocatalytic multifunctional graphene fiber material and preparation method thereof - Google Patents
Photocatalytic multifunctional graphene fiber material and preparation method thereof Download PDFInfo
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 46
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 41
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000002657 fibrous material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- -1 polypropylene Polymers 0.000 claims abstract description 54
- 239000004743 Polypropylene Substances 0.000 claims abstract description 50
- 229920001155 polypropylene Polymers 0.000 claims abstract description 44
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims description 39
- 239000000463 material Substances 0.000 claims description 19
- 239000002244 precipitate Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000011240 wet gel Substances 0.000 claims description 15
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 12
- 229910002651 NO3 Inorganic materials 0.000 claims description 10
- 239000000084 colloidal system Substances 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 238000004898 kneading Methods 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 8
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 8
- 239000002518 antifoaming agent Substances 0.000 claims description 8
- 239000007822 coupling agent Substances 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 8
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 7
- 229910001868 water Inorganic materials 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000000835 fiber Substances 0.000 claims description 5
- 238000002074 melt spinning Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- 229960000583 acetic acid Drugs 0.000 claims description 4
- 239000006184 cosolvent Substances 0.000 claims description 4
- 239000012362 glacial acetic acid Substances 0.000 claims description 4
- 239000011159 matrix material Substances 0.000 claims description 4
- 150000002910 rare earth metals Chemical class 0.000 claims description 4
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 4
- AAQNGTNRWPXMPB-UHFFFAOYSA-N dipotassium;dioxido(dioxo)tungsten Chemical compound [K+].[K+].[O-][W]([O-])(=O)=O AAQNGTNRWPXMPB-UHFFFAOYSA-N 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 238000000354 decomposition reaction Methods 0.000 abstract description 5
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 5
- 230000001954 sterilising effect Effects 0.000 abstract description 4
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 4
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 3
- 229910001410 inorganic ion Inorganic materials 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 10
- 229910052721 tungsten Inorganic materials 0.000 description 10
- 239000010937 tungsten Substances 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- 239000007777 multifunctional material Substances 0.000 description 6
- 230000036541 health Effects 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- 239000004575 stone Substances 0.000 description 4
- 229940070527 tourmaline Drugs 0.000 description 4
- 229910052613 tourmaline Inorganic materials 0.000 description 4
- 239000011032 tourmaline Substances 0.000 description 4
- 229910052693 Europium Inorganic materials 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 229910052772 Samarium Inorganic materials 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 229910052777 Praseodymium Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
- 229910001940 europium oxide Inorganic materials 0.000 description 2
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 229910001954 samarium oxide Inorganic materials 0.000 description 2
- 229940075630 samarium oxide Drugs 0.000 description 2
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 description 2
- 230000001502 supplementing effect Effects 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- QMABZEWAQYHYST-UHFFFAOYSA-N europium samarium Chemical compound [Sm][Eu] QMABZEWAQYHYST-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003845 household chemical Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229910003447 praseodymium oxide Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/34—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of chromium, molybdenum or tungsten
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
-
- B01J35/39—
-
- B01J35/61—
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a photocatalytic multifunctional graphene fiber material and a preparation method thereof, wherein the photocatalytic multifunctional graphene fiber material is a mixture prepared from the following raw materials in percentage by weight: 10-25% of polypropylene master batch and 75-90% of polypropylene slices; the polypropylene master batch is a mixture prepared from the following raw materials in percentage by weight: the photocatalytic multifunctional fiber material has the beneficial effects that the photocatalytic multifunctional fiber material has a larger specific surface area, can be fully contacted with organic pollutants in the air, can quickly and efficiently eliminate the organic pollutants in the air, reduces heavy metal inorganic ions, has high decomposition rate and good sterilization and bacteriostasis effects, and can be recycled.
Description
Technical Field
The invention relates to the technical field of environment purification materials, in particular to a photocatalytic multifunctional graphene fiber material and a preparation method thereof.
Background
Along with the progress of society and the improvement of living standard of people, people put forward higher requirements on living quality, people buy houses, decorate living rooms, and apply and popularize petroleum, coal, natural gas, chemical products, automobiles and the like, the living standard of people is improved, and meanwhile, the people pollute indoor and outdoor air to a certain degree, especially, the indoor decoration is increasingly luxurious in recent years, the problem of indoor and outdoor air pollution caused by artificial activities such as mass use of household chemicals, smoking, cooking and the like is not ignored, the environment quality directly influences the body health of people, for the body health of people, people develop a photocatalysis technology, and solar energy is utilized to oxidize and decompose organic pollutants into H20 at room temperature, so that inorganic ions of heavy metals are reduced, sterilization, deodorization and the like are applied to materials such as paint, floors, glass, ceramics and the like, the pollution to the environment can be reduced to a certain extent, but the fiber materials with the function are few at present, the existing fiber materials are low in organic matter decomposition rate, bacteria inhibition rate and the like, the environment pollution purification effect is poor, and the fiber materials cannot bring benefits to the health of people.
In view of the above, there is a need for improvements in existing fiber materials that can accommodate the current needs for air purification materials.
Disclosure of Invention
The invention aims to solve the technical problems of low organic matter decomposition rate, unobvious sterilization and bacteriostasis effects and the like of the conventional fiber material, and designs a photocatalytic multifunctional graphene fiber material and a preparation method thereof.
The technical scheme of the invention is that the photocatalytic multifunctional graphene fiber material is a mixture prepared from the following raw materials in percentage by weight: polypropylene master batch
Polypropylene chip
The polypropylene master batch is a mixture prepared from the following raw materials in percentage by weight:
nano tungsten,
Rare earth oxide,
A cocatalyst material,
A graphene material,
Polypropylene and the balance of auxiliary agents.
Further describing the scheme, the auxiliary agent comprises a dispersing agent, a coupling agent and a defoaming agent, wherein the auxiliary agent comprises the following components in percentage by weight in the polypropylene master batch:
a dispersant,
Coupling agents and
and (4) defoaming agent.
The scheme is further supplemented, and the rare earth oxide is formed by mixing one or more of Er3+, Pr3+, Nd3+, Gd3+, Eu3+ and Ce3 +.
The scheme is further supplemented, the cocatalyst material is one or two of six-ring stone powder and tourmaline powder, and the particle size of the six-ring stone powder and the tourmaline powder is 0.5-3 μm.
The scheme is further supplemented, and the dispersing agent is any one of PE-g-ST, PP-g-ST, ABS-g-MAH, PE-g-MAH, PP-g-MAH, polyethylene wax and liquid wax.
The scheme is further supplemented, the coupling agent is any one of titanate, phosphate and silane, and the defoaming agent is polysiloxane.
Preparation method of photocatalytic multifunctional graphene fiber material, namely, taking
Adding tungstate into container, dissolving with sufficient water, adding excessive dilute acid until yellow precipitate is formed, standing
After hours, the precipitate was washed with water and filtered
Adding ammonia water with the mass fraction of 15% into the precipitate until the yellow precipitate is completely converted into transparent colloid; II, taking
Adding rare earth oxide into container, adding sufficient dilute nitric acid to dissolve completely, and adding
Uniformly mixing the cosolvent, adding 200-1800 g of graphene material, and stirring at room temperature
Obtaining a rare earth graphene nitrate mixed solution in hours; thirdly, adding the transparent colloid obtained in the first step into the rare earth nitrate mixed solution obtained in the second step, and then adding
The water for dissolving the tungstate in the step one is stirred at room temperature
After hours, dilute acid is added dropwise to a solution pH of
Standing still
Forming sol in hours; fourthly, adding 500-2000 g of cocatalyst material into the sol, stirring at 1000-3000 r/min until the sol is uniformly mixed, standing
Obtaining wet gel after hours; fifthly, drying the wet gel at 100-110 ℃ and grinding the wet gel into powder, calcining the powder at 450-560 ℃ for 1.5-2.5 hours, and then grinding the powder uniformly again, thenThen obtaining photocatalytic multifunctional fiber material powder with the particle size of 0.5-5 microns and containing rare earth doped nano tungsten oxide through ultrasonic dispersion; sixthly, adding a dried polypropylene matrix with the mass of 3-4 times that of the powder, 15-200 g of dispersing agent, 20-280 g of coupling agent and 10-100 g of defoaming agent into the photocatalytic multifunctional fiber material powder, uniformly mixing, and melting, kneading, extruding and granulating the mixture by a screw extruder at 180-220 ℃ to prepare polypropylene master batches; and seventhly, adding polypropylene slices with the mass of 3-9 times that of the master batch into the prepared polypropylene master batch, uniformly mixing, melting, kneading, extruding and granulating by using a screw extruder to prepare photocatalytic multifunctional fiber slices, and then preparing the photocatalytic multifunctional fiber material by using a conventional melt spinning and deformation process.
And further supplementing the scheme, wherein the tungstate is any one of ammonium metatungstate, sodium tungstate and potassium tungstate.
The scheme is further supplemented, and the cosolvent is any one of methanol, a B-type solvent and glacial acetic acid.
Further supplementing the scheme, the polypropylene matrix is polypropylene PP with spinnability.
The scheme is further supplemented, and the dilute acid is any one of dilute nitric acid, dilute hydrochloric acid and dilute sulfuric acid.
The photocatalytic multifunctional fiber material has the advantages that the photocatalytic multifunctional fiber material has larger specific surface area, can be fully contacted with organic pollutants in the air, can quickly and efficiently eliminate the organic pollutants in the air, reduces heavy metal inorganic ions, has high decomposition rate and good sterilization and bacteriostasis effects, and can be recycled.
Detailed Description
Firstly, the design of the invention is designed primarily because the existing fiber material with the function is less, the existing fiber material has low organic matter decomposition rate, bacteria inhibition rate and the like, has poor environment pollution purification effect and cannot bring benefits to human health, and therefore, the invention provides the photocatalytic multifunctional graphene fiber material and the preparation method thereof.
A photocatalytic multifunctional graphene fiber material is a mixture prepared from the following raw materials in percentage by weight: 25% of polypropylene master batch and 75% of polypropylene slices; the polypropylene master batch is composed of 3% of nano tungsten, 2% of rare earth oxide, 12% of cocatalyst material, 8% of graphene material, 74.1% of polypropylene, 0.3% of dispersing agent, 0.4% of coupling agent and 0.2% of defoaming agent.
The preparation method comprises the following steps:
firstly, adding 3400mL of deionized water into 180 g of sodium tungstate in a beaker, completely dissolving, then adding 1200mL of dilute hydrochloric acid until all yellow precipitates are generated, standing for 24 hours, washing with deionized water, filtering and precipitating for 3 times, and then adding 15% by mass of dilute ammonia water into the precipitates until all the yellow precipitates are converted into transparent nano tungsten colloids;
secondly, placing 40 g of samarium oxide and 80g of europium oxide in a beaker, adding sufficient dilute nitric acid to completely dissolve the samarium oxide and the europium oxide, adding 50 g of ethanol, uniformly mixing, adding 80g of graphene material, and stirring at room temperature for 0.4 hour to obtain a rare earth-graphene nitrate mixed solution;
thirdly, adding the transparent nano tungsten colloid obtained in the first step into the rare earth-graphene nitrate mixed solution obtained in the second step, adding 850mL of deionized water, stirring at room temperature for 0.8 hour, dropwise adding dilute hydrochloric acid until the pH value is 3, and standing for 4 hours to form samarium-europium-containing and graphene-doped nano tungsten oxide sol;
adding 800g of mixed powder of hexacyclic ring stone powder with the grain diameter of 0.5 micron and 400 g of tourmaline powder with the grain diameter of 1 micron into the sol, stirring at 1000 revolutions per minute until the sol is uniformly mixed, and standing for 2 hours to obtain wet gel;
fifthly, drying the wet gel at 100 ℃, grinding the wet gel into powder in an agate mortar, putting the powder into a muffle furnace, calcining the powder for 1.5 hours at 450 ℃, grinding the powder uniformly again, and performing ultrasonic dispersion to obtain 2-micron photocatalytic multifunctional material powder containing samarium, europium and graphene doped nano tungsten oxide;
sixthly, adding 3 times of polypropylene PP, 15 grams of polyethylene wax, 20 grams of titanate and 10 grams of polysiloxane into the photocatalytic multifunctional material powder containing samarium, europium and graphene doped nano tungsten oxide, uniformly mixing, and melting, kneading and extruding the mixture by a screw rod extruder at 180 ℃ to prepare polypropylene master batch;
and seventhly, adding polypropylene slices with the mass 3 times that of the master batch into the prepared polypropylene master batch, uniformly mixing, melting, kneading, extruding and granulating by using a screw extruder to prepare photocatalytic multifunctional graphene fiber slices, and then preparing the photocatalytic multifunctional graphene fiber material by using a conventional melt spinning and deformation process.
Example 2:
a photocatalytic multifunctional graphene fiber material is a mixture prepared from the following raw materials in percentage by weight: 16.7% of polypropylene master batch and 83.3% of polypropylene slices; the polypropylene master batch is composed of 4.8% of nano tungsten, 3% of rare earth oxide, 10% of cocatalyst material, 2% of graphene material, 71.7% of polypropylene, 3% of dispersing agent, 4.6% of coupling agent and 0.9% of defoaming agent.
The preparation method comprises the following steps:
firstly, 240 g of sodium tungstate is put into a beaker, 4500mL of deionized water is added to be completely dissolved, 1500mL of dilute hydrochloric acid is added until all yellow precipitates are generated, the solution is kept stand for 30 hours, deionized water is used for cleaning, filtering and precipitating for 5 times, and then diluted ammonia water with the mass fraction of 15% is added into the precipitates until all the yellow precipitates are converted into transparent nano tungsten colloids;
secondly, 160 g of praseodymium oxide is taken and put in a beaker, sufficient dilute nitric acid is added to be completely dissolved, 80g of glacial acetic acid is added and uniformly mixed, 40 g of graphene material is added, and the mixture is stirred and discharged at room temperature for 0.6 hour to obtain a rare earth-graphene nitrate mixed solution;
adding transparent nano tungsten colloid into the rare earth-graphene nitrate mixed solution, adding 1500mL of deionized water, stirring at room temperature for 1 hour, dropwise adding dilute hydrochloric acid until the pH value is 5, and standing for 5 hours to form praseodymium and graphene-doped nano tungsten oxide sol;
adding 600 g of hexacyclic ring stone powder with the particle size of 1.5 microns into the sol, stirring at 3000 r/min until the sol is uniformly mixed, and standing for 4 hours to obtain wet gel;
fifthly, drying the wet gel at 120 ℃, grinding the wet gel into powder in an agate mortar, putting the powder into a muffle furnace, calcining the powder for 2 hours at 500 ℃, grinding the powder uniformly again, and performing ultrasonic dispersion to obtain 2-micron photocatalytic multifunctional material powder containing praseodymium and graphene doped nano tungsten oxide;
sixthly, adding polypropylene PP (polypropylene), 210 g of liquid wax, 260 g of phosphate and 80g of polysiloxane which are 4 times of the mass of the powder into the photocatalytic multifunctional material powder containing samarium, europium and graphene doped nano tungsten oxide, uniformly mixing, and melting, kneading and extruding the mixture by a screw rod extruder at 190 ℃ to prepare polypropylene master batch;
and seventhly, adding polypropylene slices with the mass 4 times that of the master batch into the prepared polypropylene master batch, uniformly mixing, melting, kneading, extruding and granulating by using a screw extruder to prepare photocatalytic multifunctional graphene fiber slices, and then preparing the photocatalytic multifunctional graphene fiber material by using a conventional melt spinning and deformation process.
Example 3:
a photocatalytic multifunctional graphene fiber material is a mixture prepared from the following raw materials in percentage by weight: 20% of polypropylene master batch and 80% of polypropylene slices; the polypropylene master batch is composed of 3% of nano tungsten, 2.5% of rare earth oxide, 12% of cocatalyst material, 6% of graphene material, 74% of polypropylene, 1% of dispersing agent, 1% of coupling agent and 0.5% of defoaming agent.
The preparation method comprises the following steps:
firstly, 210 g of potassium tungstate is put into a beaker, 4300mL of deionized water is added to be completely dissolved, then 1300mL of dilute hydrochloric acid is added until all yellow precipitates are generated, the mixture is kept stand for 28 hours, then the precipitates are washed by deionized water, filtered and precipitated for 5 times, and then diluted ammonia water with the mass fraction of 15% is added into the precipitates until all the yellow precipitates are converted into transparent nano tungsten colloids;
secondly, rolling 80g of cerium oxide and 80g of oxidation into a beaker, adding sufficient dilute nitric acid to dissolve completely, adding 30 g of glacial acetic acid and 30 g of PE-g-ST, uniformly mixing, adding 80g of graphene material, and stirring at room temperature for 2 hours to obtain a rare earth-graphene nitrate mixed solution;
adding the transparent nano tungsten colloid into the rare earth-graphene nitrate mixed solution, adding 1800mL of deionized water, stirring at room temperature for 1.5 hours, dropwise adding dilute hydrochloric acid until the pH value is 5, and standing for 6 hours to form a cerium-doped nano tungsten oxide sol containing the rolled nano tungsten oxide and the graphene;
adding 2000g of tourmaline powder with the particle size of 3 microns into the sol, stirring at 2000 rpm until the sol is uniformly mixed, and standing for 4.5 hours to obtain wet gel;
fifthly, drying the wet gel at 110 ℃, grinding the wet gel into powder in an agate mortar, putting the powder into a muffle furnace, calcining the powder for 3 hours at 400 ℃, grinding the powder uniformly again, and performing ultrasonic dispersion to obtain the photocatalytic multifunctional material powder with the particle size of 5 microns and containing cerium, rolled and graphene doped nano tungsten oxide;
sixthly, adding 3.5 times of polypropylene PP, 220 g of liquid wax, 250 g of phosphate and 80g of polysiloxane into the cerium, rolled and graphene doped nano tungsten oxide-containing photocatalytic multifunctional material powder, uniformly mixing, and melting, kneading and extruding the mixture by a screw extruder at the temperature of 200 ℃ to prepare polypropylene master batches;
and seventhly, adding polypropylene slices with the mass 5 times that of the master batch into the prepared polypropylene master batch, uniformly mixing, melting, kneading, extruding and granulating by using a screw extruder to prepare photocatalytic multifunctional graphene fiber slices, and then preparing the photocatalytic multifunctional graphene fiber material by using a conventional melt spinning and deformation process.
The technical solutions described above only represent the preferred technical solutions of the present invention, and some possible modifications to some parts of the technical solutions by those skilled in the art all represent the principles of the present invention, and fall within the protection scope of the present invention.
Claims (4)
1. The preparation method of the photocatalytic multifunctional graphene fiber material is characterized by comprising the steps of firstly, taking
Adding tungstate into container, dissolving with sufficient water, adding excessive dilute acid until yellow precipitate is formed, standing
After hours, the precipitate was washed with water and filtered
Adding ammonia water with the mass fraction of 15% into the precipitate until the yellow precipitate is completely converted into transparent colloid; II, taking
Adding rare earth oxide into container, adding sufficient dilute nitric acid to dissolve completely, and adding
Uniformly mixing the cosolvent, adding 200-1800 g of graphene material, and stirring at room temperature
Obtaining a rare earth graphene nitrate mixed solution in hours; thirdly, adding the transparent colloid obtained in the first step into the rare earth nitrate mixed solution obtained in the second step, and then adding
The water for dissolving the tungstate in the step one is stirred at room temperature
After hours, dilute acid is added dropwise to a solution pH of
Standing still
Forming sol in hours; fourthly, adding 500-2000 g of cocatalyst material into the sol, stirring at 1000-3000 r/min until the sol is uniformly mixed, standing
Obtaining wet gel after hours; fifthly, drying the wet gel at 100-110 ℃ and grinding the wet gel into powder, calcining the powder at 450-560 ℃ for 1.5-2.5 hours, grinding the powder uniformly, and performing ultrasonic dispersion to obtain photocatalytic multifunctional fiber material powder with the particle size of 0.5-5 microns and containing rare earth doped nano tungsten oxide; sixthly, adding a dried polypropylene matrix with the mass of 3-4 times that of the powder, 15-200 g of dispersing agent, 20-280 g of coupling agent and 10-100 g of defoaming agent into the photocatalytic multifunctional fiber material powder, uniformly mixing, and melting, kneading, extruding and granulating the mixture by a screw extruder at 180-220 ℃ to prepare polypropylene master batches; and seventhly, adding polypropylene slices with the mass of 3-9 times that of the master batch into the prepared polypropylene master batch, uniformly mixing, melting, kneading, extruding and granulating by using a screw extruder to prepare photocatalytic multifunctional fiber slices, and then preparing the photocatalytic multifunctional fiber material by using a conventional melt spinning and deformation process.
2. The preparation method of the photocatalytic multifunctional graphene fiber material according to claim 1, wherein the tungstate is any one of ammonium metatungstate, sodium tungstate and potassium tungstate.
3. The preparation method of the photocatalytic multifunctional graphene fiber material according to claim 1, wherein the cosolvent is any one of methanol, a B-type solvent and glacial acetic acid.
4. The method for preparing the photocatalytic multifunctional graphene fiber material as claimed in claim 1, wherein the polypropylene matrix is polypropylene PP with spinnability.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101851805A (en) * | 2010-05-18 | 2010-10-06 | 田小兵 | Photocatalytic multifunctional fiber material and preparation method thereof |
| CN107286473A (en) * | 2017-08-01 | 2017-10-24 | 山东圣泉新材料股份有限公司 | A kind of modified polypropylene agglomerate, fusion spray cloth and its preparation method and application |
| CN108176360A (en) * | 2018-02-06 | 2018-06-19 | 温州包鹿新材料有限公司 | A kind of graphene Modified air scavenging material and its application |
| CN108503804A (en) * | 2018-04-27 | 2018-09-07 | 济南圣泉集团股份有限公司 | A kind of method of grapheme material modified poly ester master batch and grapheme material modified poly ester master batch therefrom and application |
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-
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101851805A (en) * | 2010-05-18 | 2010-10-06 | 田小兵 | Photocatalytic multifunctional fiber material and preparation method thereof |
| CN107286473A (en) * | 2017-08-01 | 2017-10-24 | 山东圣泉新材料股份有限公司 | A kind of modified polypropylene agglomerate, fusion spray cloth and its preparation method and application |
| CN108176360A (en) * | 2018-02-06 | 2018-06-19 | 温州包鹿新材料有限公司 | A kind of graphene Modified air scavenging material and its application |
| CN108503804A (en) * | 2018-04-27 | 2018-09-07 | 济南圣泉集团股份有限公司 | A kind of method of grapheme material modified poly ester master batch and grapheme material modified poly ester master batch therefrom and application |
Non-Patent Citations (1)
| Title |
|---|
| 王芳芳等.石墨烯/镧共掺杂TiO2纳米纤维的制备及光催化性能研究.《上海纺织科技》.2019,(第12期),全文. * |
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