CN109967031B - Activated carbon fiber adsorbent for benzene series adsorption and preparation method thereof - Google Patents
Activated carbon fiber adsorbent for benzene series adsorption and preparation method thereof Download PDFInfo
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 239000003463 adsorbent Substances 0.000 title claims abstract description 51
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 125000001997 phenyl group Chemical class [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 title abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 111
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 56
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 57
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 45
- 239000002243 precursor Substances 0.000 claims description 36
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 23
- 239000011259 mixed solution Substances 0.000 claims description 23
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 22
- 229910052796 boron Inorganic materials 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 22
- 239000004094 surface-active agent Substances 0.000 claims description 17
- 239000003638 chemical reducing agent Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 15
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 12
- 159000000000 sodium salts Chemical class 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- 239000004202 carbamide Substances 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 9
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 9
- 239000004327 boric acid Substances 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 9
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 8
- FZQSLXQPHPOTHG-UHFFFAOYSA-N [K+].[K+].O1B([O-])OB2OB([O-])OB1O2 Chemical compound [K+].[K+].O1B([O-])OB2OB([O-])OB1O2 FZQSLXQPHPOTHG-UHFFFAOYSA-N 0.000 claims description 8
- 229910021538 borax Inorganic materials 0.000 claims description 8
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 8
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 claims description 8
- 239000004328 sodium tetraborate Substances 0.000 claims description 8
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 8
- 235000012000 cholesterol Nutrition 0.000 claims description 7
- 229920005610 lignin Polymers 0.000 claims description 7
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 claims description 6
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 claims description 6
- 235000010323 ascorbic acid Nutrition 0.000 claims description 6
- 239000011668 ascorbic acid Substances 0.000 claims description 6
- 229960005070 ascorbic acid Drugs 0.000 claims description 6
- 239000002502 liposome Substances 0.000 claims description 6
- HVCOBJNICQPDBP-UHFFFAOYSA-N 3-[3-[3,5-dihydroxy-6-methyl-4-(3,4,5-trihydroxy-6-methyloxan-2-yl)oxyoxan-2-yl]oxydecanoyloxy]decanoic acid;hydrate Chemical compound O.OC1C(OC(CC(=O)OC(CCCCCCC)CC(O)=O)CCCCCCC)OC(C)C(O)C1OC1C(O)C(O)C(O)C(C)O1 HVCOBJNICQPDBP-UHFFFAOYSA-N 0.000 claims description 5
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 5
- 229930186217 Glycolipid Natural products 0.000 claims description 5
- 239000010426 asphalt Substances 0.000 claims description 5
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 5
- 239000008103 glucose Substances 0.000 claims description 5
- -1 phenolic aldehyde Chemical class 0.000 claims description 5
- 150000003904 phospholipids Chemical class 0.000 claims description 5
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 abstract description 12
- 238000000576 coating method Methods 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 5
- 125000004122 cyclic group Chemical group 0.000 abstract description 4
- 238000003795 desorption Methods 0.000 abstract description 4
- 239000004917 carbon fiber Substances 0.000 description 30
- 150000001555 benzenes Chemical class 0.000 description 17
- 229920006395 saturated elastomer Polymers 0.000 description 13
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 12
- 229920002239 polyacrylonitrile Polymers 0.000 description 8
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 7
- 239000001509 sodium citrate Substances 0.000 description 7
- 238000011049 filling Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 229920000297 Rayon Polymers 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000011247 coating layer Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000012855 volatile organic compound Substances 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- SLGWESQGEUXWJQ-UHFFFAOYSA-N formaldehyde;phenol Chemical compound O=C.OC1=CC=CC=C1 SLGWESQGEUXWJQ-UHFFFAOYSA-N 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 235000010378 sodium ascorbate Nutrition 0.000 description 2
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 description 2
- 229960005055 sodium ascorbate Drugs 0.000 description 2
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- JIHQDMXYYFUGFV-UHFFFAOYSA-N 1,3,5-triazine Chemical compound C1=NC=NC=N1 JIHQDMXYYFUGFV-UHFFFAOYSA-N 0.000 description 1
- 208000005623 Carcinogenesis Diseases 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 230000036952 cancer formation Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 231100000504 carcinogenesis Toxicity 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000021615 conjugation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 230000035772 mutation Effects 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28023—Fibres or filaments
-
- 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
-
- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Inorganic Fibers (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides an activated carbon fiber adsorbent for benzene series adsorption, which comprises the following components in percentage by weight: 1-30% of boron-doped nitrogen carbide and 70-99% of activated carbon fiber. The invention further provides a preparation method of the activated carbon fiber adsorbent for benzene series adsorption. The activated carbon fiber adsorbent for benzene series adsorption and the preparation method thereof provided by the invention can be used for preparing a boron-doped nitrogen carbide coating with higher activity, improve the desorption efficiency of benzene series, and greatly improve the cyclic adsorption performance of the adsorbent.
Description
Technical Field
The invention belongs to the technical field of environmental pollution treatment, relates to an activated carbon fiber adsorbent for benzene series adsorption and a preparation method thereof, and particularly relates to a nitrogen carbide modified activated carbon fiber adsorbent for benzene series adsorption and a preparation method thereof.
Background
Volatile Organic Compounds (VOCs) are organic compounds having a saturated vapor pressure of more than 70Pa at normal temperature and a boiling point of 260 ℃ or less at normal pressure, such as many benzene series, hydrocarbons, alcohols, and the like, and are common pollutants in the atmospheric environment. In modern industries, enterprises such as chemical industry, petrochemical industry, pharmacy, electronics, chemical fiber, rubber, paint and the like, and technical processes such as printing, coating, painting and the like all relate to the generation and emission of VOCs waste gas, wherein benzene series has strong three-cause effects (mutation, carcinogenesis and teratogenesis), has great harm to ecological environment and human health, and needs to be monitored and treated.
Activated Carbon Fiber (ACF) is a novel carbonaceous adsorption material developed by combining carbon fiber technology and activated carbon technology, and compared with the traditional granular activated carbon (GRANULAR ACTIVATED CARBON), the Activated Carbon Fiber (ACF) has the characteristics of large specific surface area, developed micropores, narrow pore size distribution, high adsorption speed, strong adsorption capacity, easy regeneration and the like. In order to improve the adsorption capacity of the activated carbon fiber to atmospheric pollutants to the maximum extent, a series of modification work of the activated carbon fiber is carried out at home and abroad.
Wanghiffei (carbonization)Research and application of nitrogen chemiluminescence performance, 2015, academic thesis, page 16-24) reported that a graphite-phase nitrogen carbide (g-C) is prepared by reacting sodium citrate as a reducing agent and urea as a nitrogen source at 180 ℃ for 4 hours by a hydrothermal reduction method 3 N 4 ) The method of (1). Yan et al (Langmuir, 2016, vol.26, No. 6, pp.3894-3902) reported a method for preparing boron-doped graphite-phase nitrogen carbide by heating a mixture of melamine and boron oxide and indicated that its photocatalytic performance for rhodamine B was improved. From the literature, g-C 3 N 4 Is a graphite-like compound, which is superimposed by polymerized s-triazine to form a two-dimensional conjugated skeleton as a structural unit, SP 2 By presence of hybridized C, N atom in P z The lone pair of electrons on the orbit form a large pi bond, g-C, similar to the structure of a benzene ring 3 N 4 The layer is a large conjugated system composed of three benzene ring structures, and the introduction of the B element further enhances the delocalization of the conjugated system, so that pi bonds of benzene rings are easy to generate conjugation when the B element adsorbs benzene series substances, and the adsorption capacity is enhanced. However, there are still few reports on the research on the use of boron-doped nitrogen carbide-modified activated carbon fiber for adsorbing benzene compounds.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide an activated carbon fiber adsorbent which is economical, energy-saving, green and environment-friendly, and a preparation method thereof, so as to achieve extremely high adsorption and desorption efficiency and excellent cyclic adsorption performance for benzene series.
In order to achieve the above objects and other related objects, a first aspect of the present invention provides an activated carbon fiber adsorbent for benzene series adsorption, comprising the following components, by weight:
1 to 30 percent of boron-doped nitrogen carbide,
70-99% of activated carbon fiber.
Preferably, the activated carbon fiber adsorbent for benzene series adsorption comprises the following components in percentage by weight:
5 to 20 percent of boron-doped nitrogen carbide,
80-95% of activated carbon fiber.
Preferably, in the boron-doped nitrogen carbide, the doping amount of the boron element in the nitrogen carbide is 0.5-10 wt%. The boron-doped nitrogen carbide is obtained by reducing a boron precursor and a nitrogen precursor.
Preferably, the activated carbon fiber is selected from one of a glue-based activated carbon fiber, a Polyacrylonitrile (PAN) -based activated carbon fiber, a phenol-formaldehyde-based activated carbon fiber, a pitch-based activated carbon fiber, a polyvinyl alcohol (PVA) -based activated carbon fiber, and a lignin activated carbon fiber.
The second aspect of the invention provides a preparation method of an activated carbon fiber adsorbent for benzene series adsorption, which comprises the following steps:
1) dissolving boron precursor, nitrogen precursor and reducing agent in water, gradually dripping surfactant, stirring to dissolve completely,
obtaining a mixed solution;
2) soaking the activated carbon fiber in the mixed solution obtained in the step 1), uniformly stirring, heating, performing ultrasonic treatment, and drying to obtain the required activated carbon fiber adsorbent.
Preferably, in the step 1), the mass ratio of the boron precursor, the nitrogen precursor, the reducing agent and the water is (0.5-3) to 12 (12-15) to (70-75.5).
Preferably, in step 1), the boron precursor is selected from one of boric acid, sodium tetraborate or potassium tetraborate.
Preferably, in step 1), the nitrogen precursor is selected from one of urea, cyanamide or dicyandiamide.
Preferably, in step 1), the reducing agent is selected from one of glucose and sodium salt thereof, maltose and sodium salt thereof, ascorbic acid and sodium salt thereof, citric acid and sodium salt thereof.
Preferably, in step 1), the surfactant is a liposome selected from one of phospholipid, glycolipid or cholesterol.
Preferably, in the step 1), the addition amount of the surfactant is 1-2% of the total mass of the mixed solution.
Preferably, in the step 1), the stirring temperature is normal temperature. The normal temperature is 20-30 ℃.
Preferably, in the step 2), the activated carbon fiber is selected from one of a glue-based activated carbon fiber, a Polyacrylonitrile (PAN) -based activated carbon fiber, a phenol-formaldehyde-based activated carbon fiber, a pitch-based activated carbon fiber, a polyvinyl alcohol (PVA) -based activated carbon fiber, and a lignin activated carbon fiber.
Preferably, in the step 2), the ratio of the added mass g of the activated carbon fiber to the added volume mL of the mixed solution is 1: 1-5.
Preferably, in step 2), the heating conditions are as follows: heating temperature: 150-250 ℃; heating time: 4-48 h.
Preferably, in the step 2), the time of the ultrasonic treatment is 1-12 h.
Preferably, in step 2), the drying conditions are as follows: drying temperature: 100-120 ℃; heating time: 12-48 h.
By adjusting the ratio of boron precursor to nitrogen precursor [ (0.5-3): 12) and the proportion of the activated carbon fiber and the mixed solution [1 (1-5) ], thus obtaining the modified activated carbon fiber adsorbent with different boron-doped nitrogen carbide coating amounts.
The third aspect of the invention provides the use of the activated carbon fiber modified adsorbent in benzene series adsorption.
Preferably, the use is packing the adsorbent in a fixed bed reactor, and introducing a benzene-containing gas.
More preferably, the reaction temperature is 20-80 ℃.
More preferably, the benzene-containing gas can be operated under a pressure of 0.1 to 10 MPa.
More preferably, the space velocity of the benzene-containing substance is 500-20000 h -1 。
More preferably, the benzene-containing gas has a benzene concentration of 10 to 9000 ppm.
As described above, the activated carbon fiber adsorbent for benzene series adsorption and the preparation method thereof provided by the present invention are obtained by dispersing activated carbon fibers in an aqueous solution of a precursor such as boron, nitrogen, etc., sealing and heating to a certain temperature, and reacting for a period of time, and have the following beneficial effects:
(1) according to the boron-doped nitrogen carbide modified activated carbon fiber adsorbent prepared by the invention, the nano boron-doped nitrogen carbide coating layer can be prepared by reasonably controlling the concentration and hydrothermal time of each precursor solution, so that the nano boron-doped nitrogen carbide coating layer is uniformly distributed on the pore channel surface of the activated carbon fiber on a nano scale, and finally the boron-doped nitrogen carbide coating layer with uniformity, continuity and high bonding strength is generated by in-situ reduction on the surface of the activated carbon fiber.
(2) The invention takes the liposome with reducibility as the surfactant, so that the boron element is uniformly distributed in the nitrogen carbide coating, the mass fraction of the boron element is greatly higher, and the invention is favorable for further enhancing the large pi-bond conjugated system of the nitrogen carbide.
(3) Because the boron-doped nitrogen carbide coating with higher activity has an excellent electronic structure, the activated carbon fiber modified adsorbent has extremely high desorption efficiency on benzene series, and can greatly improve the cyclic adsorption performance of the adsorbent.
Detailed Description
The present invention is further illustrated below with reference to specific examples, which are only intended to illustrate the invention and are not intended to limit the scope of the invention.
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Example 1
Boric acid is used as a boron precursor, urea is used as a nitrogen precursor, sodium citrate is used as a reducing agent, the mass ratio of the boric acid to the urea to the sodium citrate to water is 0.5:12:12:75.5, and the total mass of the boric acid to the urea to the sodium citrate is 100 g. Then 1g of phospholipid is gradually dropped as a surfactant, and the mixture is stirred at room temperature until the dissolution is completed to prepare a mixed solution.
Weighing 465g of viscose-based active carbon fiber, soaking the viscose-based active carbon fiber in the prepared mixed solution, uniformly stirring, heating at the constant temperature of 150 ℃ for 4 hours, performing ultrasonic treatment for 1 hour, and drying at the temperature of 110 ℃ for 12 hours to obtain the boron-doped nitrogen carbide modified active carbon fiber adsorbent with the coating amount of 5%, namely the active carbon fiber adsorbent comprises the following components in percentage by weight: 5% of boron-doped nitrogen carbide and 95% of activated carbon fiber.
Respectively filling the original viscose-based activated carbon fiber and the modified activated carbon fiber adsorbent in a fixed bed reactor, controlling the reaction temperature at 20 ℃, introducing benzene-containing gas, controlling the pressure at 0.1MPa, controlling the concentration of benzene at 10ppm and the airspeed at 500h -1 The benzene adsorption efficiency of the original viscose-based activated carbon fiber is 80 percent, the saturated adsorption capacity is 215mg/g, the benzene adsorption efficiency of the modified activated carbon fiber is 90 percent, and the saturated adsorption capacity is 254 mg/g.
Example 2
The method comprises the following steps of taking sodium tetraborate as a boron precursor, taking cyanamide as a nitrogen precursor and taking glucose as a reducing agent, wherein the adding mass ratio of the sodium tetraborate to the cyanamide to the glucose to water is 3:12:15:70, and the total adding mass is 100 g. Then, 2g of glycolipid as a surfactant is gradually dropped, and the solution is stirred at room temperature until the dissolution is completed to prepare a mixed solution.
Weighing 120g of polyacrylonitrile-based active carbon fiber, soaking the polyacrylonitrile-based active carbon fiber in the prepared mixed solution, uniformly stirring, heating at the constant temperature of 250 ℃ for 48 hours, performing ultrasonic treatment for 12 hours, and drying at the temperature of 110 ℃ for 48 hours to obtain a boron-doped nitrogen carbide modified active carbon fiber adsorbent with the coating amount of 20%, wherein the boron-doped nitrogen carbide modified active carbon fiber adsorbent comprises the following components in percentage by weight: boron-doped nitrogen carbide 20% and active carbon fiber 80%.
Respectively filling original polyacrylonitrile-based active carbon fiber and the modified active carbon fiber adsorbent in a fixed bed reactor, controlling the reaction temperature at 80 ℃, introducing toluene-containing gas, controlling the pressure at 10MPa, controlling the concentration of toluene at 9000ppm and the airspeed at 20000h -1 The toluene adsorption efficiency of the original polyacrylonitrile-based active carbon fiber is 55 percent, the saturated adsorption capacity is 120mg/g, and the toluene adsorption efficiency of the modified active carbon fiber is79% and a saturated adsorption capacity of 209 mg/g.
Example 3
Potassium tetraborate is taken as a boron precursor, dicyanodiamide is taken as a nitrogen precursor, ascorbic acid is taken as a reducing agent, the mass ratio of the potassium tetraborate to the dicyanodiamide to the ascorbic acid to water is 1:12:13:74, and the total mass of the potassium tetraborate to the dicyanodiamide to the ascorbic acid is 100 g. Then gradually dripping 1g of cholesterol as a surfactant, stirring at room temperature until the cholesterol is dissolved, and preparing a mixed solution.
Weighing 234g of phenolic aldehyde-based activated carbon fiber, soaking the phenolic aldehyde-based activated carbon fiber in the prepared mixed solution, uniformly stirring, heating at the constant temperature of 200 ℃ for 12h, performing ultrasonic treatment for 6h, and drying at the temperature of 110 ℃ for 24h to obtain a boron-doped nitrogen carbide modified activated carbon fiber adsorbent with the coating amount of 10%, namely the activated carbon fiber adsorbent comprises the following components in percentage by weight: 10% of boron-doped nitrogen carbide and 90% of activated carbon fiber.
Respectively filling the original phenolic aldehyde based active carbon fiber and the modified active carbon fiber adsorbent in a fixed bed reactor, controlling the reaction temperature at 25 ℃, introducing styrene-containing gas, controlling the pressure at 1MPa, controlling the concentration of styrene at 200ppm and the airspeed at 1000h -1 The benzene adsorption efficiency of the original phenolic active carbon fiber is 83 percent, the saturated adsorption capacity is 412mg/g, the benzene adsorption efficiency of the modified active carbon fiber is 97 percent, and the saturated adsorption capacity is 598 mg/g.
Example 4
Sodium tetraborate is used as a boron precursor, urea is used as a nitrogen precursor, maltose is used as a reducing agent, the mass ratio of the sodium tetraborate to the urea to the maltose to water is 2:12:14:72, and the total mass of the sodium tetraborate to the urea to the maltose to water is 100 g. Then, 2g of phospholipid as a surfactant is gradually dropped, and the mixture is stirred at room temperature until the dissolution is completed to prepare a mixed solution.
Weighing 158g of asphalt-based active carbon fiber, soaking the asphalt-based active carbon fiber in the prepared mixed solution, uniformly stirring, heating at the constant temperature of 180 ℃ for 16h, performing ultrasonic treatment for 10h, and drying at the temperature of 110 ℃ for 36h to obtain the boron-doped nitrogen carbide modified active carbon fiber adsorbent with the coating amount of 15%, namely the active carbon fiber adsorbent comprises the following components in percentage by weight: 15% of boron-doped nitrogen carbide and 85% of activated carbon fiber.
Respectively filling the original asphalt-based active carbon fiber and the modified active carbon fiber adsorbent in a fixed bed reactor, controlling the reaction temperature at 40 ℃, introducing xylene-containing gas, controlling the pressure at 5MPa, controlling the concentration of xylene at 5000ppm and the space velocity at 3000h -1 The benzene adsorption efficiency of the original asphalt-based activated carbon fiber is 85 percent, the saturated adsorption capacity is 455mg/g, the benzene adsorption efficiency of the modified activated carbon fiber is 98 percent, and the saturated adsorption capacity is 623 mg/g.
Example 5
Boric acid is used as a boron precursor, cyanamide is used as a nitrogen precursor, sodium citrate is used as a reducing agent, the mass ratio of the boric acid to the cyanamide to the sodium citrate to water is 0.5:12:15:72.5, and the total mass of the boric acid to the cyanamide to the sodium citrate is 100 g. Then 1g of glycolipid is gradually dropped as a surfactant, and the mixture is stirred at room temperature until the dissolution is completed to prepare a mixed solution.
Weighing 102g of polyvinyl alcohol (PVA) -based active carbon fiber, soaking the active carbon fiber in the prepared mixed solution, uniformly stirring, heating at the constant temperature of 220 ℃ for 10h, performing ultrasonic treatment for 7h, and drying at the temperature of 110 ℃ for 28h to obtain the boron-doped nitrogen carbide modified active carbon fiber adsorbent with the coating amount of 18%, namely the active carbon fiber adsorbent comprises the following components in percentage by weight: 18 percent of boron-doped nitrogen carbide and 88 percent of activated carbon fiber.
Respectively filling original polyvinyl alcohol-based active carbon fiber and the modified active carbon fiber adsorbent in a fixed bed reactor, controlling the reaction temperature at 55 ℃, introducing styrene-containing gas, controlling the pressure at 0.2MPa, controlling the concentration of styrene at 650ppm and the airspeed at 10000h -1 The benzene adsorption efficiency of the original polyvinyl alcohol-based activated carbon fiber is 76%, and the saturated adsorption capacity is 305mg/g, and the benzene adsorption efficiency of the modified activated carbon fiber is 92%, and the saturated adsorption capacity is 497 mg/g.
Example 6
Potassium tetraborate is taken as a boron precursor, dicyanodiamide is taken as a nitrogen precursor, sodium ascorbate is taken as a reducing agent, the mass ratio of the potassium tetraborate to the dicyanodiamide to the sodium ascorbate to water is 2:12:13:73, and the total added mass is 100 g. Then gradually dripping 1g of cholesterol as a surfactant, stirring at room temperature until the cholesterol is dissolved, and preparing a mixed solution.
Weighing 358g of lignin activated carbon fiber, soaking the lignin activated carbon fiber in the prepared mixed solution, uniformly stirring, heating at the constant temperature of 170 ℃ for 8h, performing ultrasonic treatment for 8h, and drying at the temperature of 110 ℃ for 18h to obtain a boron-doped nitrogen carbide modified activated carbon fiber adsorbent with a coating amount of 7%, wherein the activated carbon fiber adsorbent comprises the following components in percentage by weight: 7% of boron-doped nitrogen carbide and 93% of activated carbon fiber.
Respectively filling the raw lignin activated carbon fiber and the modified activated carbon fiber adsorbent in a fixed bed reactor, controlling the reaction temperature at 65 ℃, introducing styrene-containing gas, controlling the pressure at 8MPa, controlling the concentration of styrene at 7000ppm and the airspeed at 15000h -1 The benzene adsorption efficiency of the original lignin activated carbon fiber is 73 percent, the saturated adsorption capacity is 324mg/g, the benzene adsorption efficiency of the modified activated carbon fiber is 94 percent, and the saturated adsorption capacity is 512 mg/g.
In conclusion, the activated carbon fiber adsorbent for benzene series adsorption and the preparation method thereof provided by the invention can be used for preparing the boron-doped nitrogen carbide coating with higher activity, improve the desorption efficiency of the benzene series, and greatly improve the cyclic adsorption performance of the adsorbent. Therefore, the invention effectively overcomes various defects in the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (8)
1. An activated carbon fiber adsorbent comprises the following components in percentage by weight:
5 to 20 percent of boron-doped nitrogen carbide,
80-95% of activated carbon fiber;
in the boron-doped nitrogen carbide, the doping amount of the boron element in the nitrogen carbide is 0.5-10 wt%;
the activated carbon fiber is selected from one of phenolic aldehyde-based activated carbon fiber, asphalt-based activated carbon fiber, polyvinyl alcohol-based activated carbon fiber and lignin activated carbon fiber;
the activated carbon fiber adsorbent is prepared by the following method, and the method comprises the following steps:
1) dissolving a boron precursor, a nitrogen precursor and a reducing agent in water, gradually dropwise adding a surfactant, and stirring until the surfactant is completely dissolved to obtain a mixed solution;
2) soaking activated carbon fibers in the mixed solution obtained in the step 1), uniformly stirring, heating, performing ultrasonic treatment, and drying to obtain the required activated carbon fiber adsorbent;
in step 1), any one or more of the following conditions are included:
A1) the boron precursor is selected from one of boric acid, sodium tetraborate or potassium tetraborate;
A2) the nitrogen precursor is selected from one of urea, cyanamide or dicyandiamide;
A3) the reducing agent is selected from one of glucose and sodium salt thereof, maltose and sodium salt thereof, ascorbic acid and sodium salt thereof, citric acid and sodium salt thereof;
A4) the surfactant is liposome, and the liposome is selected from one of phospholipid, glycolipid or cholesterol;
in the step 1), the mass ratio of the boron precursor, the nitrogen precursor, the reducing agent and the water is (0.5-3) to 12 (12-15) to (70-75.5);
in the step 2), the heating conditions are as follows: heating temperature: 150-250 ℃; heating time: 4-48 h.
2. The method for preparing an activated carbon fiber adsorbent according to claim 1, comprising the steps of:
1) dissolving a boron precursor, a nitrogen precursor and a reducing agent in water, gradually dropwise adding a surfactant, and stirring until the surfactant is completely dissolved to obtain a mixed solution;
2) soaking activated carbon fibers in the mixed solution obtained in the step 1), uniformly stirring, heating, performing ultrasonic treatment, and drying to obtain the required activated carbon fiber adsorbent;
in step 1), any one or more of the following conditions are included:
A1) the boron precursor is selected from one of boric acid, sodium tetraborate or potassium tetraborate;
A2) the nitrogen precursor is selected from one of urea, cyanamide or dicyandiamide;
A3) the reducing agent is selected from one of glucose and sodium salt thereof, maltose and sodium salt thereof, ascorbic acid and sodium salt thereof, citric acid and sodium salt thereof;
A4) the surfactant is liposome, and the liposome is selected from one of phospholipid, glycolipid or cholesterol.
3. The preparation method of the activated carbon fiber adsorbent according to claim 2, wherein in the step 1), the mass ratio of the boron precursor, the nitrogen precursor, the reducing agent and the water is (0.5-3): 12, (12-15): 70-75.5.
4. The preparation method of the activated carbon fiber adsorbent according to claim 2, wherein in the step 1), the addition amount of the surfactant is 1-2% of the total mass of the mixed solution.
5. The method for preparing the activated carbon fiber adsorbent according to claim 2, wherein in the step 2), the ratio of the added mass g of the activated carbon fiber to the added volume mL of the mixed solution is 1: 1-5.
6. The method for preparing the activated carbon fiber adsorbent according to claim 2, wherein the step 2) comprises any one or more of the following conditions:
B1) the heating conditions are as follows: heating temperature: 150-250 ℃; heating time: 4-48 h;
B2) the ultrasonic time is 1-12 h;
B3) the drying conditions are as follows: drying temperature: 100-120 ℃; heating time: 12-48 h.
7. Use of the activated carbon fiber adsorbent according to claim 1 in benzene-based adsorption.
8. The use of claim 7, wherein the adsorbent is packed in a fixed bed reactor and the benzene-containing gas is introduced.
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