CN114737392A - Lyocell-based activated carbon fiber and preparation method and application thereof - Google Patents
Lyocell-based activated carbon fiber and preparation method and application thereof Download PDFInfo
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- CN114737392A CN114737392A CN202210545375.0A CN202210545375A CN114737392A CN 114737392 A CN114737392 A CN 114737392A CN 202210545375 A CN202210545375 A CN 202210545375A CN 114737392 A CN114737392 A CN 114737392A
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- activated carbon
- carbon fiber
- lyocell
- nitrogen
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 229920000433 Lyocell Polymers 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 96
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 52
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 26
- 238000002791 soaking Methods 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 16
- 239000011148 porous material Substances 0.000 claims abstract description 16
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 14
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 12
- 230000004913 activation Effects 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000007598 dipping method Methods 0.000 claims abstract description 7
- 150000001412 amines Chemical class 0.000 claims abstract description 6
- -1 ammonium ions Chemical class 0.000 claims abstract description 5
- 230000009471 action Effects 0.000 claims abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract 8
- 238000001994 activation Methods 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 6
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 6
- 238000004887 air purification Methods 0.000 claims description 6
- 238000003763 carbonization Methods 0.000 claims description 6
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 4
- 230000007420 reactivation Effects 0.000 claims description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 3
- 235000019270 ammonium chloride Nutrition 0.000 claims description 3
- 238000010000 carbonizing Methods 0.000 claims description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 3
- 239000013043 chemical agent Substances 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 claims 4
- 229910052709 silver Inorganic materials 0.000 claims 4
- 239000004332 silver Substances 0.000 claims 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 4
- 125000003277 amino group Chemical group 0.000 abstract description 4
- 239000001569 carbon dioxide Substances 0.000 abstract description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 abstract description 2
- 230000008030 elimination Effects 0.000 abstract 1
- 238000003379 elimination reaction Methods 0.000 abstract 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 abstract 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 16
- 238000000746 purification Methods 0.000 description 15
- 239000000243 solution Substances 0.000 description 15
- 239000007789 gas Substances 0.000 description 12
- 241000894006 Bacteria Species 0.000 description 8
- 238000001179 sorption measurement Methods 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 241000588724 Escherichia coli Species 0.000 description 5
- 241000191967 Staphylococcus aureus Species 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000003242 anti bacterial agent Substances 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000003385 bacteriostatic effect Effects 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 238000012356 Product development Methods 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001588 bifunctional effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000005360 mashing Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/325—Amines
- D06M13/338—Organic hydrazines; Hydrazinium compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
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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
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
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- D01F9/16—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate
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- 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
- D06M11/07—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
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Abstract
The invention belongs to the field of activated carbon fiber preparation, and particularly relates to a lyocell-based activated carbon fiber and a preparation method and application thereof, wherein the lyocell fiber is carbonized and activated at high temperature under the action of vapor containing phosphoric acid in a nitrogen atmosphere, and after the activation is finished, the lyocell-based activated carbon fiber is cooled under the protection of nitrogen to prepare the activated carbon fiber; soaking the activated carbon fiber in a potassium hydroxide solution, heating to 650-850 ℃ under the protection of nitrogen, and reactivating to obtain the microporous activated carbon fiber with the pore diameter of 0.5-1.2 nm; dipping the microporous activated carbon fiber with the pore diameter of 0.5-1.2nm by using a chemical reagent containing organic amine or ammonium ions to obtain the amino-enriched activated carbon fiber; and (3) soaking the amino-rich activated carbon fiber in the nano silver solution, and drying to obtain the target product. The lyocell activated carbon fiber can utilize the micropores with specific aperture range and surface amino groups to adsorb and enrich low-concentration formaldehyde, and can also utilize the catalytic action of nano silver to degrade the formaldehyde into carbon dioxide and water, thereby realizing the complete elimination of formaldehyde molecules.
Description
Technical Field
The invention belongs to the field of activated carbon fiber preparation, and particularly relates to a lyocell-based activated carbon fiber and a preparation method and application thereof.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
The activated carbon fiber is a new generation of high-efficiency adsorption material developed on the basis of combining a carbon fiber technology and an activated carbon technology, and has the characteristics of large adsorption capacity, high adsorption rate, mild desorption conditions, easiness in regeneration and the like.
Although the large-scale production and market application of the activated carbon fiber are realized in domestic and foreign markets, the activated carbon fiber faces a plurality of problems such as lack of functional product development and the like. In addition, the raw materials for preparing the activated carbon fiber mainly comprise viscose fiber and polyacrylonitrile fiber, and especially lack the preparation technology based on the biomass-based precursor.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a lyocell activated carbon fiber and a preparation method and application thereof.
In order to realize the purpose, the invention is realized by the following technical scheme:
in a first aspect, the present invention provides a method for preparing lyocell activated carbon fibers, comprising the steps of:
carbonizing and activating the lyocell fiber at high temperature under the action of vapor containing phosphoric acid in a nitrogen atmosphere, and cooling under the protection of nitrogen after the activation is finished to prepare the activated carbon fiber;
soaking the activated carbon fiber in a potassium hydroxide solution, heating to 650-850 ℃ under the protection of nitrogen, and reactivating to obtain the microporous activated carbon fiber with the pore diameter of 0.5-1.2 nm;
dipping the microporous activated carbon fiber with the pore diameter of 0.5-1.2nm by using a chemical reagent containing organic amine or ammonium ions to obtain the amino-enriched activated carbon fiber;
and (3) soaking the amino-rich activated carbon fiber in the nano silver solution, and drying to obtain the target product.
In a second aspect, the invention provides a lyocell activated carbon fiber prepared by the preparation method.
In a third aspect, the invention provides the use of the lyocell activated carbon fiber in air purification, particularly in air purification rich in formaldehyde.
In a fourth aspect, an air purifier is prepared from the lyocell activated carbon fiber.
The beneficial effects achieved by one or more of the embodiments of the invention are as follows:
(1) the method utilizes the lyocell fiber biomass raw material as the carbon source, and has the advantages of low cost, low energy consumption and environmental protection. The method not only provides a preparation technology for developing the activated carbon fiber by using the lyocell fiber, the performance of the prepared activated carbon fiber reaches or is superior to the level of the activated carbon fiber produced in the prior industry, but also provides a method for regulating and controlling the aperture of the lyocell-based activated carbon fiber by a reactivation technology.
(2) The lyocell activated carbon fiber provided by the invention can be used for adsorbing and enriching low-concentration formaldehyde by utilizing micropores with specific aperture ranges and surface amino groups, and can also be used for degrading formaldehyde into carbon dioxide and water by utilizing the catalytic action of nano silver, so that the formaldehyde molecules are thoroughly eliminated. In addition, the antibacterial agent also has excellent bacteriostatic action against common bacteria.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
Fig. 1 is a flow chart of a preparation method of the bifunctional lyocell-based activated carbon fiber with formaldehyde purification and bacteriostasis functions according to one or more embodiments of the present invention.
FIG. 2 is a graph showing the formaldehyde purification in example 1.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
A preparation method of a lyocell activated carbon fiber comprises the following steps:
carbonizing and activating the lyocell fiber at high temperature under the action of vapor containing phosphoric acid in a nitrogen atmosphere, and cooling under the protection of nitrogen after the activation is finished to prepare the activated carbon fiber;
soaking the activated carbon fiber in a potassium hydroxide solution, heating to 650-850 ℃ under the protection of nitrogen, and reactivating to obtain the microporous activated carbon fiber with the pore diameter of 0.5-1.2 nm;
dipping the microporous activated carbon fiber with the pore diameter of 0.5-1.2nm by using a chemical reagent containing organic amine or ammonium ions to obtain the amino-enriched activated carbon fiber;
and (3) soaking the amino-rich activated carbon fiber in the nano silver solution, and drying to obtain the target product.
The lyocell fiber is prepared by taking pulp which is formed by mashing reproducible bamboo, wood and the like as a raw material, so that the development of the lyocell-based activated carbon fiber has the advantages of wide raw material source, greenness, no pollution, low cost and the like. The inventor finds that the lyocell-based activated carbon fiber has higher specific surface area and abundant surface chemical structures, and the microporous structure is directly opened on the surface of the fiber, so that the lyocell-based activated carbon fiber has higher adsorption rate and adsorption capacity for low-concentration formaldehyde gas.
In some embodiments, the activation temperature is 650-.
In some embodiments, the concentration of the phosphoric acid solution used to generate the phosphoric acid-containing water vapor is between 5 wt% and 25 wt%, and the phosphoric acid and water vapor components provided by the dilute phosphoric acid solution function as both activators in the present invention.
Preferably, nitrogen or argon is used for providing inert gas protection during the carbonization and activation processes, and the volume ratio of the water vapor to the nitrogen or argon is 0.5-2: 1.
In some embodiments, the activated carbon fiber is ultrasonically immersed in a potassium hydroxide solution for 2 to 6 hours, wherein the mass fraction of the potassium hydroxide solution is 5 to 25 weight percent.
Preferably, the temperature for reactivation is 650-. The concentration of the potassium hydroxide solution and the reactivation temperature are limited to adjust the pore diameter of the micropores of the microporous activated carbon fibers and enrich the micropores with the pore diameter of 0.5-1.2 nm.
In some embodiments, the chemical agent containing an organic amine or ammonium ion is ethylenediamine, hydrazine hydrate, or ammonium chloride.
In some embodiments, the nanosilver solution has a concentration of 10 to 100 ppm.
Preferably, the temperature for drying after the nano silver solution is dipped is 60-100 ℃.
In a second aspect, the invention provides a lyocell activated carbon fiber prepared by the preparation method, the surface of the lyocell activated carbon fiber is rich in micropores with the aperture of 0.5-1.2nm, the amino content of the surface of the lyocell activated carbon fiber is 5% -20%, and the mass percentage of silver nanoparticles is 5% -15%.
The activated carbon fiber has high pore volume in a specific pore diameter range, abundant surface nitrogen-containing groups and a nano-silver catalyst structure, wherein a 0.5-1.2nm microporous structure and a surface amino structure form a nano-confinement system, and the activated carbon fiber has the coupling effect of physical adsorption and chemical adsorption on formaldehyde gas and can realize the quick adsorption of low-concentration formaldehyde. The formaldehyde molecules are enriched on the surface of the activated carbon fibers and near the structure of the nano-silver catalyst under the synergistic action of micropores and amino groups, so that the cycle effect of adsorption-degradation-reabsorption is formed, and the degradation effect of the nano-silver catalyst on low-concentration formaldehyde gas is improved. In addition, the nano-silver catalyst structure can realize the bacteriostatic action of the activated carbon fiber material while realizing effective formaldehyde purification through contact reaction with bacteria.
In a third aspect, the invention provides the use of the lyocell activated carbon fiber in air purification, particularly in air purification rich in formaldehyde.
In a fourth aspect, an air purifier is prepared from the lyocell activated carbon fiber.
Example 1
A preparation method of Lyocell-based activated carbon fiber with formaldehyde purification and bacteriostasis functions comprises the following steps:
(1) heating the lyocell fiber to 700 ℃ at a speed of 15 ℃/min under the protection of nitrogen, introducing water vapor containing phosphoric acid for carbonization and activation, wherein the concentration of the used phosphoric acid solution is 15 wt%, the volume ratio of the water vapor to the nitrogen is 1, and cooling to 25 ℃ under the protection of nitrogen after the activation is finished, thereby completing the preparation of the activated carbon fiber.
(2) Placing the activated carbon fiber in a potassium hydroxide solution with the mass fraction of 20 wt%, soaking for 6h under an ultrasonic environment, heating to 850 ℃ at 15 ℃/min under the protection of nitrogen, cooling to 25 ℃ under the protection of nitrogen, taking out, and washing to be neutral by using deionized water to obtain the activated carbon fiber with the microporous structure enriched with the pore size range of 0.5-1.2 nm.
(3) Preparing 45 wt% of hydrazine hydrate aqueous solution, putting the activated carbon fiber prepared in the step (2) into the aqueous solution for dipping for 3 hours, and washing and drying the carbon fiber after dipping to obtain the amino-enriched activated carbon fiber.
(4) And (3) soaking the activated carbon fiber prepared in the step (3) in a nano-silver solution for 3 hours, wherein the concentration of the nano-silver solution is 60ppm, and drying at the temperature of 80 ℃ after soaking is finished, so that the preparation of the lyocell-based activated carbon fiber with the functions of formaldehyde purification and bacteriostasis is completed.
The specific surface area of the prepared functional activated carbon fiber is 1060m2/g。
1g of functional lyocell-based activated carbon fiber is placed at 2m3Adsorbing in the space at 3mg/m when the ambient temperature is 23 + -2 deg.C and the relative humidity is 30% + -2% RH3The purification rate of the low-concentration formaldehyde gas can reach 100 percent, and the formaldehyde purification curve is shown as an attached figure 2.
When the concentration of the bacteria test solution is 1 x 105-3*105The bacteriostasis rate of the antibacterial agent to bacteria such as escherichia coli, staphylococcus aureus and the like is more than 99 percent under the condition of 37 +/-2 ℃ when the antibacterial agent is CFU/mL.
Example 2
A preparation method of a Lyocell-based activated carbon fiber with formaldehyde purification and bacteriostasis functions comprises the following steps:
(1) heating the lyocell fiber to 750 ℃ at a speed of 10 ℃/min under the protection of nitrogen, introducing water vapor containing phosphoric acid for carbonization and activation, wherein the concentration of the used phosphoric acid solution is 20 wt%, the volume ratio of the water vapor to the nitrogen is 1.5, and cooling to 25 ℃ under the protection of nitrogen after the activation is finished, thus finishing the preparation of the activated carbon fiber.
(2) Placing the activated carbon fiber in a potassium hydroxide solution with the mass fraction of 25 wt%, soaking for 6h under an ultrasonic environment, heating to 850 ℃ at 10 ℃/min under the protection of nitrogen, cooling to 25 ℃ under the protection of nitrogen, taking out, and washing to be neutral by using deionized water to obtain the activated carbon fiber with the microporous structure enriched with the pore size range of 0.5-1.2 nm.
(3) Preparing an ammonium chloride aqueous solution with the mass fraction of 55 wt%, putting the activated carbon fiber prepared in the step (2) into the aqueous solution for soaking for 4 hours, and after the soaking is finished, washing with water and drying to obtain the amino-enriched activated carbon fiber.
(4) And (3) soaking the activated carbon fiber prepared in the step (3) in a nano-silver solution for 4 hours, wherein the concentration of the nano-silver solution is 80ppm, and drying at the temperature of 80 ℃ after soaking is finished, so that the preparation of the lyocell-based activated carbon fiber with the functions of formaldehyde purification and bacteriostasis is completed.
The specific surface area of the prepared functional activated carbon fiber is 820m2Per g, for 3mg/m3The purification rate of the low-concentration formaldehyde gas is 97%, and the bacteriostasis rate of the low-concentration formaldehyde gas to bacteria such as escherichia coli, staphylococcus aureus and the like is more than 99%.
Example 3
A preparation method of Lyocell-based activated carbon fiber with formaldehyde purification and bacteriostasis functions comprises the following steps:
(1) heating the lyocell fiber to 650 ℃ at the speed of 8 ℃/min under the protection of nitrogen, introducing water vapor containing phosphoric acid for carbonization and activation, wherein the concentration of the used phosphoric acid solution is 25 wt%, the volume ratio of the water vapor to the nitrogen is 1.5, and cooling to 30 ℃ under the protection of nitrogen after the activation is finished, thus finishing the preparation of the activated carbon fiber.
(2) Placing the activated carbon fiber in a potassium hydroxide solution with the mass fraction of 10 wt%, soaking for 6h under an ultrasonic environment, heating to 800 ℃ at the speed of 8 ℃/min under the protection of nitrogen, cooling to 30 ℃ under the protection of nitrogen, taking out, and washing to be neutral by using deionized water to obtain the activated carbon fiber with the microporous structure enriched with the pore size range of 0.5-1.2 nm.
(3) Preparing an ethylenediamine aqueous solution with the mass fraction of 30 wt%, putting the activated carbon fiber prepared in the step (2) into the ethylenediamine aqueous solution for soaking for 4 hours, and after the soaking is finished, washing with water and drying to obtain the amino-enriched activated carbon fiber.
(4) And (3) soaking the activated carbon fiber prepared in the step (3) in a nano-silver solution for 4 hours, wherein the concentration of the nano-silver solution is 15ppm, and drying at the temperature of 80 ℃ after soaking is finished, so that the preparation of the lyocell-based activated carbon fiber with the functions of formaldehyde purification and bacteriostasis is completed.
The specific surface area of the prepared functional activated carbon fiber is 1290m2Per g, for 6mg/m3The purification rate of the low-concentration formaldehyde gas can reach 100 percent, and the bacteriostasis rate of the low-concentration formaldehyde gas to bacteria such as escherichia coli, staphylococcus aureus and the like is more than 99 percent.
Comparative example 1
The difference from example 3 is that: and (3) omitting the step (2), namely not adjusting the aperture range of the activated carbon fiber. The specific surface area of the prepared functional activated carbon fiber is 1240m2Per g, for 6mg/m3The purification rate of the low-concentration formaldehyde gas is 85 percent, and the bacteriostasis rate of the low-concentration formaldehyde gas to bacteria such as escherichia coli, staphylococcus aureus and the like is 92 percent.
Comparative example 2
The difference from example 3 is that: step (3) is omitted, namely amino groups are not enriched on the surface of the activated carbon fiber. The specific surface area of the prepared functional activated carbon fiber is 1390m2Per g, for 6mg/m3The purification rate of the low-concentration formaldehyde gas can reach 75 percent, and the bacteriostasis rate of the low-concentration formaldehyde gas to bacteria such as escherichia coli, staphylococcus aureus and the like is 92 percent.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a lyocell activated carbon fiber is characterized by comprising the following steps: the method comprises the following steps:
carbonizing and activating the lyocell fiber at high temperature under the action of vapor containing phosphoric acid in a nitrogen atmosphere, and cooling under the protection of nitrogen after the activation is finished to prepare the activated carbon fiber;
soaking the activated carbon fiber in a potassium hydroxide solution, heating to 650-850 ℃ under the protection of nitrogen, and reactivating to obtain the microporous activated carbon fiber with the pore diameter of 0.5-1.2 nm;
dipping the microporous activated carbon fiber with the pore diameter of 0.5-1.2nm by using a chemical reagent containing organic amine or ammonium ions to obtain the amino-enriched activated carbon fiber;
and (3) soaking the amino-rich activated carbon fiber in the nano silver solution, and drying to obtain the target product.
2. The method for preparing a lyocell activated carbon fiber according to claim 1, wherein: the carbonization temperature is 650-850 ℃;
the temperature for reactivation was 650-850 ℃.
3. The method for preparing a lyocell activated carbon fiber according to claim 1, wherein: the concentration of the phosphoric acid solution used to form the phosphoric acid-containing water vapor is 5 wt% to 25 wt%.
4. The method for preparing a lyocell activated carbon fiber according to claim 1, wherein: the volume ratio of the water vapor to the nitrogen is 0.5-2:1 in the carbonization and activation processes.
5. The method for preparing a lyocell activated carbon fiber according to claim 1, wherein: ultrasonically dipping the activated carbon fiber in a potassium hydroxide solution for 2-6h, wherein the mass fraction of the potassium hydroxide solution is 5-25 wt%.
6. The method for preparing a lyocell activated carbon fiber according to claim 1, wherein: the chemical agent containing organic amine or ammonium ions is ethylenediamine, hydrazine hydrate or ammonium chloride.
7. The method for preparing a lyocell activated carbon fiber according to claim 1, wherein: the concentration of the nano silver solution is 10-100 ppm.
8. A lyocell activated carbon fiber characterized in that: the silver nanoparticle is prepared by the preparation method of any one of claims 1 to 7, the surface of the silver nanoparticle is rich in micropores with the pore diameter of 0.5 to 1.2nm, the amino content of the surface of the silver nanoparticle is 5 to 20 percent, and the mass percent of the silver nanoparticle is 5 to 15 percent.
9. Use of lyocell activated carbon fibers according to claim 8 for air purification, in particular for air purification rich in formaldehyde.
10. An air purifier, its characterized in that: prepared from the lyocell activated carbon fiber of claim 8.
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