CN117531298A - Preparation method of hollow activated carbon fiber and filter screen material containing hollow activated carbon fiber - Google Patents
Preparation method of hollow activated carbon fiber and filter screen material containing hollow activated carbon fiber Download PDFInfo
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 239000000463 material Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000004745 nonwoven fabric Substances 0.000 claims abstract description 84
- 239000002131 composite material Substances 0.000 claims abstract description 56
- 229920002239 polyacrylonitrile Polymers 0.000 claims abstract description 32
- 238000009987 spinning Methods 0.000 claims abstract description 25
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000005576 amination reaction Methods 0.000 claims abstract description 18
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 13
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 13
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 12
- 239000002121 nanofiber Substances 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 7
- 230000003647 oxidation Effects 0.000 claims abstract description 6
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 6
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 5
- 238000003763 carbonization Methods 0.000 claims abstract description 4
- 230000004913 activation Effects 0.000 claims abstract description 3
- 238000001994 activation Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 31
- 238000010438 heat treatment Methods 0.000 claims description 22
- 239000004814 polyurethane Substances 0.000 claims description 18
- 229920002635 polyurethane Polymers 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- 230000003213 activating effect Effects 0.000 claims description 10
- 238000010000 carbonizing Methods 0.000 claims description 9
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 claims description 2
- 230000001070 adhesive effect Effects 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 abstract description 36
- 239000012855 volatile organic compound Substances 0.000 abstract description 27
- 238000001179 sorption measurement Methods 0.000 abstract description 23
- 230000003197 catalytic effect Effects 0.000 abstract description 17
- 238000006731 degradation reaction Methods 0.000 abstract description 17
- 230000000694 effects Effects 0.000 abstract description 6
- 238000000746 purification Methods 0.000 abstract description 5
- 238000004887 air purification Methods 0.000 abstract description 3
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 34
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 24
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 18
- 239000004917 carbon fiber Substances 0.000 description 16
- 230000015556 catabolic process Effects 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 14
- 238000001816 cooling Methods 0.000 description 10
- 239000001273 butane Substances 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 9
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 9
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 239000000843 powder Substances 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 239000011888 foil Substances 0.000 description 6
- 230000001105 regulatory effect Effects 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 5
- 239000000835 fiber Substances 0.000 description 5
- 230000001590 oxidative effect Effects 0.000 description 5
- 229920002523 polyethylene Glycol 1000 Polymers 0.000 description 5
- 229920006395 saturated elastomer Polymers 0.000 description 5
- 238000009849 vacuum degassing Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 229910052593 corundum Inorganic materials 0.000 description 4
- 239000010431 corundum Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000000643 oven drying Methods 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- 239000004753 textile Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000001523 electrospinning Methods 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
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- 238000005034 decoration Methods 0.000 description 2
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- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
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- 150000008282 halocarbons Chemical class 0.000 description 1
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- 210000000777 hematopoietic system Anatomy 0.000 description 1
- 208000026278 immune system disease Diseases 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
- B01D39/2055—Carbonaceous material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/30—Particle separators, e.g. dust precipitators, using loose filtering material
-
- 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Inorganic Chemistry (AREA)
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention belongs to the technical field of air purification materials, and discloses a preparation method of hollow activated carbon fibers and a filter screen material containing the hollow activated carbon fibers. The preparation method comprises the following steps: dissolving polyacrylonitrile, ethylenediamine, melamine and polyethylene glycol in a solvent to prepare spinning solution; carrying out electrostatic spinning on the spinning solution to obtain PAN amination nanofiber; and then the hollow activated carbon fiber is prepared through pre-oxidation, carbonization and activation. The filter screen material comprises a hollow activated carbon fiber layer and a composite non-woven fabric layer. The hollow activated carbon fiber provided by the invention has the advantages of abundant holes, large specific surface area, strong adsorption capacity and extremely slow release speed after adsorption saturation, and provides sufficient time for the catalytic degradation process of the composite non-woven fabric. The filter screen material provided by the invention can efficiently adsorb, catalyze and degrade various VOCs gases, has a long-acting adsorption and purification effect, and can be widely applied to various in-vehicle and indoor air purifiers.
Description
Technical Field
The invention belongs to the technical field of air purification materials, and particularly relates to a preparation method of hollow activated carbon fibers and a filter screen material containing the hollow activated carbon fibers.
Background
Volatile organic compounds (Volatile Organic Compounds, VOCs) are organic compounds with saturated vapor pressure at normal temperature greater than 70.91Pa and boiling point below 50-260 ℃ at standard atmospheric pressure. VOCs can be divided into eight classes according to the difference in chemical structure: alkanes, aromatic hydrocarbons, alkenes, halogenated hydrocarbons, esters, aldehydes, ketones, and others. The discharge of VOCs has a very serious damaging effect on human health, and the special odor of VOCs can damage the cardiovascular system of human body, induce diseases of immune system, endocrine system and hematopoietic system, and cause metabolic defects. In recent years, with rapid development of industry and improvement of life quality of people, the problem of VOCs pollution is increasingly serious. When house decoration and decoration are carried out, materials such as decorative board wallpaper, furniture paint coating, household appliances and the like can continuously release VOCs to the closed indoor environment, and the physical and mental health of a human body is endangered.
At present, the methods for purifying VOCs are more, such as recovery adsorption technologies mainly comprising an adsorption method, a membrane separation method and a condensation method, and non-recovery degradation technologies comprising a thermal oxidation (combustion) method, a biodegradation method, a low-temperature plasma method, a photocatalysis method and the like. Among them, the adsorption method is attracting attention because of its advantages of low energy consumption, low cost, good effect, easy operation, etc. The most widely used adsorbent material in the market at present is activated carbon. The active carbon material has various pore structures and high specific surface area, but has limited adsorption capacity, and water in the air is easy to produce competitive adsorption with VOCs to cause the active carbon to be easily adsorbed and saturated, and moreover, the improper treatment of the active carbon is easy to cause adsorbed pollutants to return to the air again, so that the problem of secondary pollution is caused. This is also a cause of short life cycle and increased cost of the activated carbon adsorbent material. In addition, the existing activated carbon adsorption purification device has the defects of short service life, low purification efficiency, few acting objects and the like, so that the purification of VOCs is short in time effect and low in efficiency. Therefore, the active carbon material and the purifying device for efficiently and effectively adsorbing and purifying VOCs are prepared, and have important significance for air purification.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the prior art described above. Therefore, the invention provides a preparation method of hollow activated carbon fiber and a filter screen material containing the same. The hollow activated carbon fiber provided by the invention has strong adsorption capacity, the filter screen material prepared by the hollow activated carbon fiber can efficiently adsorb and purify various VOCs gases for a long time, and the adsorbed VOCs gases are not easy to return to the air again to generate secondary pollution.
The invention provides a preparation method of hollow activated carbon fiber.
Specifically, the preparation method of the hollow activated carbon fiber comprises the following steps:
(1) Dissolving polyacrylonitrile, ethylenediamine, melamine and polyethylene glycol in a solvent to prepare spinning solution;
(2) Carrying out electrostatic spinning on the spinning solution prepared in the step (1) to prepare PAN amination nanofiber;
(3) Pre-oxidizing the PAN amination nanofiber prepared in the step (2), carbonizing in a protective atmosphere, and finally performing CO (carbon monoxide) treatment 2 Activating to obtain the hollow activated carbon fiber.
Preferably, in step (1), the solvent is selected from at least one of N, N-Dimethylformamide (DMF), dimethylacetamide (DMA), dimethylsulfoxide (DMSO).
Preferably, in the step (1), 10-25 parts by weight of polyacrylonitrile, 10-20 parts by weight of polyethylene glycol, 5-20 parts by weight of ethylenediamine, 2-8 parts by weight of melamine and 55-75 parts by weight of solvent are calculated; it is further preferred that in step (1), 15-20 parts by weight of polyacrylonitrile, 10-15 parts by weight of polyethylene glycol, 10-15 parts by weight of ethylenediamine, 3-5 parts by weight of melamine and 60-70 parts by weight of solvent are used.
Preferably, in step (2), the method of electrospinning is as follows: after the spinning solution is sucked, the spinning solution is propelled at a speed of 0.01-0.02mL/min, and the voltage of the electrostatic spinning is controlled to be 30-40kV, and the receiving distance is 15-20cm. More specifically, the method of electrospinning is as follows: sucking 10-20mL of spinning solution by adopting a syringe, and adjusting the propulsion rate to be 0.01-0.02mL/min; the positive electrode of the high-voltage power generator is connected with the needle point of the injector, the negative electrode is connected with the aluminum foil paper of the receiving screen, the voltage is regulated to be 30-40kV, and the receiving distance is 15-20cm.
Preferably, in step (2), a degassing treatment is performed before the process of electrospinning is performed.
Preferably, in step (3), the pre-oxidation process is: air or oxygen is used as a medium, the temperature is raised to 200-350 ℃ at a heating rate of 1-10 ℃/min, and then the temperature is kept for 1-10h; further preferably, in step (3), the pre-oxidation process is: air is used as a medium, the temperature is raised to 250-300 ℃ at a temperature rising rate of 5-10 ℃/min, and then the heat is preserved for 1-5h.
Preferably, in step (3), the carbonization process is: heating to 600-1000 ℃ at a heating rate of 20-120 ℃/min under a protective atmosphere, and carbonizing for 50-120min.
Preferably, the protective atmosphere is N 2 。
Preferably, in step (3), the activating process is: introducing CO at a rate of 400-600mL/min 2 Activating at 800-1000deg.C for 40-90min, and then at CO 2 Cooled to room temperature (e.g., 5-40 ℃ C.) under the protection of (C.).
The invention also provides a filter screen material.
Specifically, the filter screen material comprises a hollow activated carbon fiber layer and a composite non-woven fabric layer, wherein the hollow activated carbon fiber layer contains the hollow activated carbon fibers, and the composite non-woven fabric layer comprises a non-woven fabric middle layer and MnO attached to two sides of the non-woven fabric middle layer 2 A layer.
Preferably, the preparation method of the composite non-woven fabric layer comprises the following steps: mnO is added to 2 Mixing polyurethane gel with water to obtain polyurethane gel solution, and coating on the front and back surfaces of the non-woven fabric to obtain the composite non-woven fabric layer.
PreferablyThe MnO 2 The mass ratio of the polyurethane adhesive to the water is 1: (2-4): (0.5-3).
Preferably, the MnO 2 The preparation method of (2) is as follows: mnCO is processed by 3 Placing in a tube furnace, heating to 500-600deg.C at a heating rate of 1-3deg.C/min, heating for 3-6 hr, cooling, washing, and oven drying to obtain MnO 2 。
Preferably, in the filter screen material, the composite non-woven fabric layer has at least two layers, and the two layers of the composite non-woven fabric layers are respectively positioned on the outer sides of the hollow activated carbon fiber layers. If the filter screen material is three layers, the filter screen material is a composite non-woven fabric layer, a hollow activated carbon fiber layer and a composite non-woven fabric layer in sequence; the filter screen material is composed of four layers, namely a composite non-woven fabric layer, a hollow activated carbon fiber layer and a composite non-woven fabric layer in sequence; the filter screen material is five layers, namely a composite non-woven fabric layer, a hollow activated carbon fiber layer, a composite non-woven fabric layer, a hollow activated carbon fiber layer and a composite non-woven fabric layer in sequence.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention prepares spinning solution by taking polyacrylonitrile, ethylenediamine, melamine and polyethylene glycol as raw materials, performs electrostatic spinning to aminate PAN, and prepares PAN aminated hollow activated carbon fiber (hollow activated carbon fiber) through the processes of pre-oxidation, carbonization, activation and the like. The PAN amination hollow active carbon fiber provided by the invention has a hollow structure, the total specific surface area of the inner wall and the outer wall is far larger than that of a common active carbon fiber, and the adsorption performance of the PAN amination hollow active carbon fiber is greatly improved due to a large number of porous structures, and the PAN amination hollow active carbon fiber is not easy to release after the adsorption is saturated.
(2) The filter screen material provided by the invention consists of a hollow active carbon fiber layer formed by hollow active carbon fibers and a composite non-woven fabric, wherein the composite non-woven fabric comprises a non-woven fabric intermediate layer and MnCO attached to two sides of the non-woven fabric intermediate layer 3 MnO generated in situ 2 A layer. Wherein the hollow activated carbon fiber layer can rapidly and efficiently adsorb VOCs gas, and the composite non-woven fabric is positioned at the outer side of the hollow activated carbon fiber layer, so that MnO is not only realized when the VOCs gas passes through the composite non-woven fabric in the adsorption process 2 Can enterPrimary catalytic degradation is carried out once, and after the hollow activated carbon fiber layer is adsorbed and saturated, VOCs gas is returned to the air, and then the VOCs gas is subjected to catalytic degradation again through the composite non-woven fabric, and after the VOCs gas is degraded twice, the VOCs gas is basically not released to the air, so that secondary pollution is not caused. The hollow activated carbon fiber provided by the invention has the advantages of abundant holes, large specific surface area, strong adsorption capacity and extremely slow release speed after adsorption saturation, and provides sufficient time for the catalytic degradation process of the composite non-woven fabric. Therefore, the filter screen material provided by the invention can efficiently adsorb, catalyze and degrade various VOCs gases, has a long-acting adsorption and purification effect, and can be widely applied to various in-vehicle and indoor air purifiers.
(3) The invention provides a composite non-woven fabric in a filter screen material, mnO thereof 2 The layer has high specific surface area and high porosity, so that the layer has high low-temperature catalytic oxidation activity, and can catalyze and degrade VOCs at room temperature. And the preparation process is simple, and other chemical reagents are not needed.
(4) The filter screen material provided by the invention firstly adsorbs VOCs in the environment on the hollow active carbon fiber layer, and then carries out MnO through the composite non-woven fabric 2 The catalyst layer is used for catalyzing and degrading VOCs, so that VOCs adsorbed by the filter screen material can not be released into the environment again to cause secondary pollution, and the effect of purifying the VOCs efficiently and for a long time can be realized.
(5) The filter screen material provided by the invention has the advantages of abundant and easily available raw materials and low price and cost.
Drawings
FIG. 1 is a graph of catalytic degradation of the screen material of example 1 to remove styrene;
FIG. 2 is a graph of the catalytic degradation of the filter material of example 2 to remove toluene;
FIG. 3 is a graph of catalytic degradation of the screen material of example 3 to remove methyl mercaptan;
FIG. 4 is a graph of the catalytic degradation of the screen material of example 4 to remove butane.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples will be presented. It should be noted that the following examples do not limit the scope of the invention.
The starting materials, reagents or apparatus used in the following examples are all available from conventional commercial sources or may be obtained by methods known in the art unless otherwise specified.
Example 1
The preparation method of the hollow activated carbon fiber comprises the following steps:
(1) 20g of polyacrylonitrile, 15g of PEG (PEG 1000) and 5g of melamine are weighed and dissolved in 70mL (66.36 g) of DMF solution, 10mL (8.99 g) of ethylenediamine solution is added, and the mixture is fully stirred and mixed to prepare spinning solution;
(2) After the spinning solution is subjected to vacuum degassing, 20mL of spinning solution is sucked into a syringe, and the propulsion rate is regulated to be 0.02mL/min. Connecting the positive electrode of a high-voltage power generator with the needle point of the injector, connecting the negative electrode of the high-voltage power generator with aluminum foil paper of a receiving screen, adjusting the voltage to 40kV, and obtaining PAN amination fiber with the receiving distance of 20 cm;
(3) Placing PAN aminated nano fibers in an oven, heating the temperature to 250 ℃ at a speed of 5 ℃/min, and pre-oxidizing for 2 hours; placing the product into a tube furnace, heating to 900 ℃ at a speed of 30 ℃/min, carbonizing for 1h, and introducing N during the reaction process 2 The method comprises the steps of carrying out a first treatment on the surface of the Activating the product at 800 deg.C for 40min, introducing 500mL/min CO during the reaction 2 Product at CO 2 Cooling to room temperature under protection to obtain PAN amination hollow carbon fiber, and storing in a dryer.
A filter screen material comprises 2 hollow activated carbon fiber layers and 2 composite non-woven fabric layers, wherein the hollow activated carbon fiber layers are positioned between the 2 composite non-woven fabric layers, and the hollow activated carbon fiber layers are fixedly assembled with the composite non-woven fabric layers. The hollow activated carbon fiber layer is made into a sheet shape by the hollow activated carbon fiber, and the composite non-woven fabric layer comprises a non-woven fabric middle layer and MnO attached to two sides of the non-woven fabric middle layer 2 The specific manufacturing method of the layer and the composite non-woven fabric layer is as follows:
(1) Weigh 20g MnCO 3 Adding the corundum reaction boat into a tube furnace, heating to 550 ℃ at a speed of 2 ℃/min, and reactingNaturally cooling to room temperature after 4h to obtain black powder, repeatedly washing the obtained powder with deionized water for 3 times, and drying at 60 ℃ to obtain MnO 2 A catalyst;
(2) According to MnO 2 The mass ratio of the catalyst to the water to the polyurethane gel is 1 to 3 to 4, and the uniform polyurethane gel solution is prepared by ultrasonic treatment for 30 minutes. And uniformly spraying the polyurethane colloidal solution on the front side and the back side of the non-woven fabric provided by the textile industry to obtain the composite non-woven fabric.
The screen material provided in example 1 was applied to a treated styrene gas. A 36L organic glass glove box is selected, styrene gas is uniformly input into the glove box, the initial concentration is 3.53ppm, and a hollow carbon fiber/non-woven fabric filter screen material is placed into the glove box for adsorption catalytic degradation experiments. The concentration of styrene gas in the glove box was measured by a gas chromatograph. The catalytic degradation diagram of the filter screen material to styrene is shown in figure 1. In fig. 1, the abscissa indicates the treatment time, the left ordinate indicates the styrene removal rate, and the right ordinate indicates the styrene tail gas concentration. As can be seen from FIG. 1, after the filter screen material provided in example 1 is used for 25min, the removal rate of styrene reaches 94%, and the high removal rate can be continuously maintained within 200 min, the concentration of styrene is below 0.5ppm, and the phenomenon that the adsorbed styrene gas returns to the air again can not occur.
Example 2
The preparation method of the hollow activated carbon fiber comprises the following steps:
(1) 20g of polyacrylonitrile and 10g of PEG (PEG 1000) are weighed, 3g of melamine is dissolved in 65mL (61.62 g) of DMF solution, 15mL (13.49 g) of ethylenediamine solution is added, and the mixture is fully stirred and mixed to prepare spinning solution;
(2) After the spinning solution is subjected to vacuum degassing, 20mL of spinning solution is sucked into a syringe, and the propulsion rate is regulated to be 0.015mL/min. Connecting the positive electrode of a high-voltage power generator with the needle point of the injector, connecting the negative electrode of the high-voltage power generator with aluminum foil paper of a receiving screen, adjusting the voltage to 40kV, and obtaining PAN amination fiber with the receiving distance of 20 cm;
(3) Placing PAN aminated nano fibers in an oven, heating the temperature to 250 ℃ at a speed of 10 ℃/min, and pre-oxidizing for 2 hours; placing the productHeating the temperature to 1000 ℃ at a speed of 20 ℃/min in a tube furnace, carbonizing for 1h, and introducing N in the reaction process 2 The method comprises the steps of carrying out a first treatment on the surface of the Activating the product at 1000deg.C for 40min, introducing 500mL/min CO during the reaction 2 Product at CO 2 Cooling to room temperature under protection to obtain PAN amination hollow carbon fiber, and storing in a dryer.
A filter screen material comprises 2 hollow activated carbon fiber layers and 2 composite non-woven fabric layers, wherein the hollow activated carbon fiber layers are positioned between the 2 composite non-woven fabric layers, and the hollow activated carbon fiber layers are fixedly assembled with the composite non-woven fabric layers. The hollow activated carbon fiber layer is made into a sheet shape by the hollow activated carbon fiber, and the composite non-woven fabric layer comprises a non-woven fabric middle layer and MnO attached to two sides of the non-woven fabric middle layer 2 The specific manufacturing method of the layer and the composite non-woven fabric layer is as follows:
(1) Weigh 25g MnCO 3 Adding into corundum reaction boat, placing into tubular furnace, heating to 550deg.C at a rate of 2deg.C/min, reacting for 4 hr, naturally cooling to room temperature to obtain black powder, repeatedly washing the powder with deionized water for 3 times, oven drying at 60deg.C to obtain MnO 2 A catalyst;
(2) According to MnO 2 The mass ratio of the catalyst to the water to the polyurethane gel is 1 to 2 to 4, and the uniform polyurethane gel solution is prepared by ultrasonic treatment for 30 min. And uniformly spraying the polyurethane colloidal solution on the front side and the back side of the non-woven fabric provided by the textile industry to obtain the composite non-woven fabric.
The screen material provided in example 2 was applied to process toluene gas. A 36L organic glass glove box is selected, toluene gas is uniformly input into the glove box, the initial concentration is 5.93ppm, and a hollow carbon fiber/non-woven fabric filter screen material is placed into the glove box to perform an adsorption catalytic degradation experiment. Toluene gas concentration in the glove box was measured by a gas chromatograph. The catalytic degradation diagram of toluene as a filter screen material is shown in fig. 2. As can be seen from FIG. 2, after 10min of treatment with the filter screen material of example 2, the toluene removal rate reached 97.5%, and the high removal rate could be maintained continuously within 2 hours, the toluene concentration was below 0.5ppm, and the phenomenon that the adsorbed toluene gas was returned to the air again was avoided.
Example 3
The preparation method of the hollow activated carbon fiber comprises the following steps:
(1) 15g of polyacrylonitrile, 10g of PEG (PEG 1000) and 5g of melamine are weighed and dissolved in 60mL (56.88 g) of DMF solution, 15mL (13.49 g) of ethylenediamine solution is added, and the mixture is fully stirred and mixed to prepare spinning solution;
(2) After the spinning solution is subjected to vacuum degassing, 15mL of the spinning solution is sucked into a syringe, and the propulsion rate is regulated to be 0.02mL/min. Connecting the positive electrode of a high-voltage power generator with the needle point of the injector, connecting the negative electrode of the high-voltage power generator with aluminum foil paper of a receiving screen, adjusting the voltage to 40kV, and obtaining PAN amination fiber with the receiving distance of 20 cm;
(3) Placing PAN aminated nano fibers in an oven, heating the temperature to 300 ℃ at a speed of 10 ℃/min, and pre-oxidizing for 4 hours; placing the product into a tube furnace, heating the temperature to 1000 ℃ at a speed of 25 ℃/min, carbonizing for 2 hours, and introducing N in the reaction process 2 The method comprises the steps of carrying out a first treatment on the surface of the Activating the product at 1000deg.C for 40min, introducing 500mL/min CO during the reaction 2 Product at CO 2 Cooling to room temperature under protection to obtain PAN amination hollow carbon fiber, and storing in a dryer.
A filter screen material comprises 2 hollow activated carbon fiber layers and 2 composite non-woven fabric layers, wherein the hollow activated carbon fiber layers are positioned between the 2 composite non-woven fabric layers, and the hollow activated carbon fiber layers are fixedly assembled with the composite non-woven fabric layers. The hollow activated carbon fiber layer is made into a sheet shape by the hollow activated carbon fiber, and the composite non-woven fabric layer comprises a non-woven fabric middle layer and MnO attached to two sides of the non-woven fabric middle layer 2 The specific manufacturing method of the layer and the composite non-woven fabric layer is as follows:
(1) Weigh 25g MnCO 3 Adding into corundum reaction boat, placing into tubular furnace, heating to 600deg.C at a rate of 3deg.C/min, reacting for 4 hr, naturally cooling to room temperature to obtain black powder, repeatedly washing the powder with deionized water for 3 times, oven drying at 60deg.C to obtain MnO 2 A catalyst;
(2) According to MnO 2 Preparing polyurethane gel with catalyst, water and polyurethane gel at a mass ratio of 1:2:3, and ultrasonic treating for 30min to obtain uniform polyurethaneA colloidal solution. And uniformly spraying the polyurethane colloidal solution on the front side and the back side of the non-woven fabric provided by the textile industry to obtain the composite non-woven fabric.
The screen material provided in example 3 was applied to the treatment of methyl mercaptan gas. A 36L organic glass glove box is selected, methyl mercaptan gas is uniformly input into the glove box, the initial concentration is 20.06ppm, and a hollow carbon fiber/non-woven fabric filter screen material is placed into the glove box for adsorption catalytic degradation experiments. Methyl mercaptan gas concentration in the glove box was measured by gas chromatograph. The catalytic degradation diagram of methyl mercaptan by the filter screen material is shown in figure 3. As can be seen from fig. 3, when the high concentration methyl mercaptan gas is treated by the filter screen material provided in example 3, the methyl mercaptan removal rate reaches 72% after only 20min, and the high removal rate can be maintained continuously within 2 hours, and the methyl mercaptan concentration is less than 6ppm, so that the phenomenon that the adsorbed methyl mercaptan gas returns to the air again can not occur.
Example 4
The preparation method of the hollow activated carbon fiber comprises the following steps:
(1) 15g of polyacrylonitrile, 15g of PEG (PEG 1000) and 5g of melamine are weighed and dissolved in 60mL (56.88 g) of DMF solution, 10mL (8.99 g) of ethylenediamine solution is added, and the mixture is fully stirred and mixed to prepare spinning solution;
(2) After the spinning solution is subjected to vacuum degassing, 20mL of spinning solution is sucked into a syringe, and the propulsion rate is regulated to be 0.02mL/min. Connecting the positive electrode of a high-voltage power generator with the needle point of the injector, connecting the negative electrode of the high-voltage power generator with aluminum foil paper of a receiving screen, adjusting the voltage to 40kV, and obtaining PAN amination fiber with the receiving distance of 20 cm;
(3) Placing PAN aminated nano fibers in an oven, heating the temperature to 250 ℃ at a speed of 5 ℃/min, and pre-oxidizing for 2 hours; placing the product into a tube furnace, heating to 900 ℃ at a speed of 30 ℃/min, carbonizing for 1h, and introducing N during the reaction process 2 The method comprises the steps of carrying out a first treatment on the surface of the Activating the product at 800 deg.C for 40min, introducing 500mL/min CO during the reaction 2 Product at CO 2 Cooling to room temperature under protection to obtain PAN amination hollow carbon fiber, and storing in a dryer.
A filter screen material comprises 3 hollow activated carbon fiber layers and 3 composite layersThe non-woven fabric layer is composed of a composite non-woven fabric layer, a hollow activated carbon fiber layer, a composite non-woven fabric layer, a hollow activated carbon fiber layer and a composite non-woven fabric layer from top to bottom in sequence. The hollow activated carbon fiber layer and the composite non-woven fabric layer are fixedly assembled. The hollow activated carbon fiber layer is made into a sheet shape by the hollow activated carbon fiber, and the composite non-woven fabric layer comprises a non-woven fabric middle layer and MnO attached to two sides of the non-woven fabric middle layer 2 The specific manufacturing method of the layer and the composite non-woven fabric layer is as follows:
(1) 30g of MnCO is weighed 3 Adding into corundum reaction boat, placing into tubular furnace, heating to 600deg.C at a rate of 3deg.C/min, reacting for 4 hr, naturally cooling to room temperature to obtain black powder, repeatedly washing the powder with deionized water for 3 times, oven drying at 60deg.C to obtain MnO 2 A catalyst;
(2) According to MnO 2 The mass ratio of the catalyst to the water to the polyurethane gel is 1 to 2 to 3, and the uniform polyurethane gel solution is prepared by ultrasonic treatment for 30 min. And uniformly spraying the polyurethane colloidal solution on the front side and the back side of the non-woven fabric provided by the textile industry to obtain the composite non-woven fabric.
The screen material provided in example 4 was applied to the treatment of butane gas. A 36L organic glass glove box is selected, butane gas is uniformly input into the glove box, the initial concentration is 37ppm, and a hollow carbon fiber/non-woven fabric filter screen material is placed into the glove box to perform an adsorption catalytic degradation experiment. Butane gas concentration in the glove box was measured by gas chromatograph. The catalytic degradation of butane by the screen material is shown in figure 4. As can be seen from FIG. 4, the high-concentration butane gas was treated with the sieve material of example 4, and after only 18 minutes, the butane removal rate reached 99%, and the high removal rate could be maintained continuously for 2 hours, with the butane concentration below 1ppm, and the adsorbed butane gas could not be returned to the air again.
Comparative example 1
Comparative example 1 differs from example 1 in that a common nonwoven fabric was used instead of the composite nonwoven fabric layer in example 1.
Specifically, the filter screen material comprises 2 layers of the hollow activated carbon fiber layer prepared in the embodiment 1 and 2 layers of the common non-woven fabric layer, wherein the hollow activated carbon fiber layer is positioned between the 2 layers of the common non-woven fabric layer, and the hollow activated carbon fiber layer is fixedly assembled with the common non-woven fabric layer.
The same test experiment as in example 1 was conducted, and it was tested that the removal rate of styrene could reach 91% after 25 minutes of treatment with the filter screen material provided in comparative example 1, but the removal rate could be maintained for only 50 minutes, and the styrene gas adsorbed by the filter screen material was returned to the air again after 50 minutes, and the concentration of styrene was gradually increased to 2.2ppm.
Comparative example 2
Comparative example 2 is different from example 1 in that the hollow activated carbon fiber was prepared by the same method as example 1 without adding melamine. Specifically, the preparation method of the hollow activated carbon fiber comprises the following steps:
(1) 23g of polyacrylonitrile and 17g of PEG (PEG 1000) are weighed, dissolved in 70mL (66.36 g) of DMF solution, and 10mL (8.99 g) of ethylenediamine solution is added, and fully stirred and mixed to prepare spinning solution;
(2) After the spinning solution is subjected to vacuum degassing, 20mL of spinning solution is sucked into a syringe, and the propulsion rate is regulated to be 0.02mL/min. Connecting the positive electrode of a high-voltage power generator with the needle point of the injector, connecting the negative electrode of the high-voltage power generator with aluminum foil paper of a receiving screen, adjusting the voltage to 40kV, and obtaining PAN amination fiber with the receiving distance of 20 cm;
(3) Placing PAN aminated nano fibers in an oven, heating the temperature to 250 ℃ at a speed of 5 ℃/min, and pre-oxidizing for 2 hours; placing the product into a tube furnace, heating to 900 ℃ at a speed of 30 ℃/min, carbonizing for 1h, and introducing N during the reaction process 2 The method comprises the steps of carrying out a first treatment on the surface of the Activating the product at 800 deg.C for 40min, introducing 500mL/min CO during the reaction 2 Product at CO 2 Cooling to room temperature under protection to obtain PAN amination hollow carbon fiber, and storing in a dryer.
The same test experiment as in example 1 was conducted, and it was tested that the removal rate of styrene was only 78% after 25 minutes of treatment with the filter screen material of comparative example 2, and the removal rate was only 130 minutes, and after 130 minutes, the styrene gas adsorbed by the filter screen material was partially returned to the air again, and the concentration of styrene was gradually increased to 1.7ppm. According to analysis, when melamine is not added in the process of preparing the hollow activated carbon fiber, the adsorption effect of the finally prepared filter screen material on organic gases such as styrene is obviously affected, the early adsorption effect is poor, the release speed is high again after the adsorption is saturated, and the outer composite non-woven fabric layer is degraded less quickly and can return to the air again.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. The preparation method of the hollow activated carbon fiber is characterized by comprising the following steps:
(1) Dissolving polyacrylonitrile, ethylenediamine, melamine and polyethylene glycol in a solvent to prepare spinning solution;
(2) Carrying out electrostatic spinning on the spinning solution prepared in the step (1) to prepare PAN amination nanofiber;
(3) Pre-oxidizing the PAN amination nanofiber prepared in the step (2), carbonizing in a protective atmosphere, and finally performing CO (carbon monoxide) treatment 2 Activating to obtain the hollow activated carbon fiber.
2. The method according to claim 1, wherein in the step (1), the solvent is at least one selected from the group consisting of N, N-dimethylformamide, dimethylacetamide and dimethylsulfoxide.
3. The production method according to claim 1 or 2, wherein in step (1), the polyacrylonitrile is 10 to 25 parts by weight, the polyethylene glycol is 10 to 20 parts by weight, the ethylenediamine is 5 to 20 parts by weight, the melamine is 2 to 8 parts by weight, and the solvent is 55 to 75 parts by weight.
4. The method according to claim 1 or 2, wherein in step (3), the pre-oxidation is performed by: air or oxygen is used as a medium, the temperature is raised to 200-350 ℃ at a heating rate of 1-10 ℃/min, and then the temperature is kept for 1-10h.
5. The method according to claim 4, wherein in the step (3), the carbonization is performed by: heating to 600-1000 ℃ at a heating rate of 20-120 ℃/min under a protective atmosphere, and carbonizing for 50-120min.
6. The method according to claim 4, wherein in the step (3), the activation is performed by: introducing CO at a rate of 400-600mL/min 2 Activating at 800-1000deg.C for 40-90min, and then at CO 2 Cooled to room temperature under the protection of (2).
7. A filter screen material comprising a hollow activated carbon fiber layer comprising hollow activated carbon fibers prepared by the preparation method of any one of claims 1 to 6 and a composite nonwoven fabric layer comprising a nonwoven fabric intermediate layer and MnO attached to both sides of the nonwoven fabric intermediate layer 2 A layer.
8. The filter screen material of claim 7, wherein the composite nonwoven fabric layer is prepared by the following method: mnO is added to 2 Mixing polyurethane gel with water to obtain polyurethane gel solution, and coating on the front and back surfaces of the non-woven fabric to obtain the composite non-woven fabric layer.
9. The screen material of claim 8, wherein the MnO 2 The mass ratio of the polyurethane adhesive to the water is 1: (2-4): (0.5-3).
10. The filter screen material according to any one of claims 7 to 9, wherein the composite nonwoven fabric layer has at least two layers, and the two layers of the composite nonwoven fabric layer are respectively located outside the hollow activated carbon fiber layer.
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