CN111498846A - Active carbon filter material and preparation method thereof - Google Patents
Active carbon filter material and preparation method thereof Download PDFInfo
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- CN111498846A CN111498846A CN202010366356.2A CN202010366356A CN111498846A CN 111498846 A CN111498846 A CN 111498846A CN 202010366356 A CN202010366356 A CN 202010366356A CN 111498846 A CN111498846 A CN 111498846A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 180
- 239000000463 material Substances 0.000 title claims abstract description 66
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 229910000314 transition metal oxide Inorganic materials 0.000 claims abstract description 57
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 43
- 150000003624 transition metals Chemical class 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 26
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 238000001354 calcination Methods 0.000 claims abstract description 22
- 239000002243 precursor Substances 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 16
- -1 transition metal salt Chemical class 0.000 claims abstract description 15
- 239000012716 precipitator Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000011259 mixed solution Substances 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 18
- 239000012153 distilled water Substances 0.000 claims description 13
- 239000002244 precipitate Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 7
- 150000000703 Cerium Chemical class 0.000 claims description 4
- 150000001868 cobalt Chemical class 0.000 claims description 4
- 150000002505 iron Chemical class 0.000 claims description 4
- 150000002696 manganese Chemical class 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract description 133
- 230000003197 catalytic effect Effects 0.000 abstract description 12
- 238000001556 precipitation Methods 0.000 abstract description 11
- 230000003647 oxidation Effects 0.000 abstract description 9
- 238000007254 oxidation reaction Methods 0.000 abstract description 9
- 238000011068 loading method Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 7
- 239000011148 porous material Substances 0.000 abstract description 6
- 230000009467 reduction Effects 0.000 abstract description 2
- 239000013049 sediment Substances 0.000 abstract 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 27
- 239000003054 catalyst Substances 0.000 description 16
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 13
- 239000002245 particle Substances 0.000 description 12
- 238000001179 sorption measurement Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 5
- 239000004202 carbamide Substances 0.000 description 5
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 5
- 229940011182 cobalt acetate Drugs 0.000 description 5
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical group [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 230000002035 prolonged effect Effects 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 231100000252 nontoxic Toxicity 0.000 description 3
- 230000003000 nontoxic effect Effects 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009298 carbon filtering Methods 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000027756 respiratory electron transport chain Effects 0.000 description 2
- 239000003440 toxic substance Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 1
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 1
- 229910016978 MnOx Inorganic materials 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 description 1
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- 229910000361 cobalt sulfate Inorganic materials 0.000 description 1
- 229940044175 cobalt sulfate Drugs 0.000 description 1
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 1
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 1
- 235000002867 manganese chloride Nutrition 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 229940099607 manganese chloride Drugs 0.000 description 1
- 229940099596 manganese sulfate Drugs 0.000 description 1
- 235000007079 manganese sulphate Nutrition 0.000 description 1
- 239000011702 manganese sulphate Substances 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
- C01B32/372—Coating; Grafting; Microencapsulation
-
- 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
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/615—100-500 m2/g
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/617—500-1000 m2/g
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/618—Surface area more than 1000 m2/g
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
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Abstract
The invention provides an activated carbon filter material and a preparation method thereof. The preparation method comprises the following steps: s1, heating the raw materials including the transition metal salt, the precipitator and the first solvent by a microwave hydrothermal method to obtain a transition metal precursor; s2, calcining the transition metal precursor to obtain a nanometer transition metal oxide; and S3, mixing the nano transition metal oxide and the activated carbon in a second solvent so that the nano transition metal oxide is loaded on the activated carbon. In the method, a microwave hydrothermal method is adopted to firstly prepare the nanometer transition metal oxide with uniform appearance, so that the appearance is more uniform; and, through the direct mixing stirring with self-made transition metal oxide load to the active carbon on, the inhomogeneous sediment of having avoided when loading through the mode of precipitation causes the active carbon carrier pore canal to block up to the whole formaldehyde of filter material that leads to gets rid of the reduction of activity, makes the active carbon filter material have better formaldehyde catalytic oxidation performance.
Description
Technical Field
The invention relates to the technical field of filter materials, and particularly relates to an activated carbon filter material and a preparation method thereof.
Background
Formaldehyde (HCHO) is a common volatile organic compound in indoor air and seriously harms human health, so that the method has very important research significance on removal and treatment of formaldehyde pollution in the indoor air.
The main component of the filter screen for the air purifier at present is activated carbon, formaldehyde is removed mainly by adsorption to a pure activated carbon filter material, the service life is limited by adsorption saturation amount, and once the activated carbon reaches the adsorption saturation, toxic substances can be generated to harm human health.
Research shows that the formaldehyde can be completely converted into nontoxic and harmless CO by catalytic oxidation technology2And H2And O, the process can be realized at normal temperature without additional energy input, and has important significance for prolonging the service life of the filter screen, so that the formaldehyde catalytic oxidation technology is widely concerned by various social circles. At present, noble metals are better normal-temperature formaldehyde catalysts, but the noble metals are limited to be widely applied due to high price.
Disclosure of Invention
The invention mainly aims to provide an active carbon filter material and a preparation method thereof, and aims to solve the problem that the service life of the active carbon filter material in the prior art is limited by adsorption saturation.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for preparing an activated carbon filter material, comprising the steps of: s1, heating the raw materials including the transition metal salt, the precipitator and the first solvent by a microwave hydrothermal method to obtain a transition metal precursor; s2, calcining the transition metal precursor to obtain a nanometer transition metal oxide; and S3, mixing the nano transition metal oxide and the activated carbon in a second solvent so that the nano transition metal oxide is loaded on the activated carbon.
Further, in step S1, the transition metal salt is independently selected from any one of a cobalt salt, a manganese salt, a cerium salt and an iron salt, and preferably, the first solvent contains distilled water and an alcohol, and the volume ratio of the distilled water to the alcohol is (1-10): 1.
furthermore, the temperature of the microwave hydrothermal method is 150-200 ℃, and the heating time is 20-60 min.
Further, step S1 includes the steps of: s11, mixing and stirring the transition metal salt, the precipitator and the first solvent to obtain a first mixed solution; s12, heating the first mixed solution by a microwave hydrothermal method to obtain a second mixed solution containing the transition metal precipitate; and S13, separating the transition metal precipitate from the second mixed solution to obtain a transition metal precursor.
Further, the step S13 further includes a step of drying the separated transition metal precursor, preferably at a drying temperature of 80-120 ℃ for 1-24 hours.
Furthermore, the calcination temperature is 300-600 ℃, the calcination time is 1-4 h, and the preferred heating rate is 1-10 ℃/min.
Further, after the step of calcining the transition metal precursor, a rod-shaped transition metal oxide is obtained, and the step S2 further includes: carrying out tabletting treatment and grinding on the rod-shaped transition metal oxide to obtain granular transition metal oxide; and screening the granular transition metal oxide to obtain the nano transition metal oxide, preferably screening by using a screen of 40-60 meshes.
Further, in step S3, the mass ratio of the nano transition metal oxide to the activated carbon is 1:100 to 1: 10.
Further, in step S3, the stirring speed is 300 to 800 r/min.
According to another aspect of the invention, the active carbon filter material is provided, and the specific surface area of the active carbon filter material is 300-1300 m2/g。
Further, the active carbon filter material is prepared by the preparation method.
By applying the technical scheme of the invention, the preparation method of the active carbon filter material is provided, and the microwave hydrothermal method is adopted to firstly prepare the nanometer transition metal oxide with uniform appearance, so that the appearance is more uniform; then, transition metal oxide is loaded on the activated carbon in a mixing and stirring mode to obtain a catalyst-loaded activated carbon filter material, and in the method, self-made transition metal oxide is loaded on the activated carbon through direct mixing and stirring, so that the blockage of pore channels of the activated carbon carrier due to uneven precipitation during loading in a precipitation mode is avoided, the reduction of activity of the whole formaldehyde removal of the filter material is reduced, and the activated carbon filter material has better formaldehyde catalytic oxidation performance.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It is noted that the terms first, second and the like in the description and in the claims of the present invention are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged under appropriate circumstances in order to facilitate the description of the embodiments of the invention herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
As described in the background art, the main component of the filter screen of the air purifier is activated carbon, formaldehyde is removed from a pure activated carbon filter material mainly by adsorption, the service life is limited by the adsorption saturation amount, and once the activated carbon reaches the adsorption saturation, toxic substances may be generated to harm human health.
In order to solve the above technical problems, the applicant of the present invention provides a method for preparing an activated carbon filter material, comprising the following steps: s1, heating the raw materials including the transition metal salt, the precipitator and the first solvent by a microwave hydrothermal method to obtain a transition metal precursor; s2, calcining the transition metal precursor to obtain a nanometer transition metal oxide; and S3, mixing the nano transition metal oxide and the activated carbon in a second solvent so that the nano transition metal oxide is loaded on the activated carbon.
According to the preparation method, the microwave hydrothermal method is adopted to prepare the nanometer transition metal oxide with uniform appearance, so that the appearance is more uniform; then loading transition metal oxide on the active carbon by mixing and stirring to obtain the catalyst-loaded active carbon filter material, transition metal oxide (Co)3O4、MnOx、CeO2Etc.) has the characteristics of low price, multiple valence states, rapid electron transfer capability, wide sources and the like, and Co3O4The transition metal oxide has a large number of surface oxygen cavities on the surface, and is enabled to show excellent formaldehyde catalytic oxidation performance due to the beneficial factors such as abundant active oxygen species and multi-valence ions.
In addition, in the method, the self-made transition metal oxide is loaded on the activated carbon through direct mixing and stirring, so that the problem that pore channels of the activated carbon carrier are blocked due to uneven precipitation during loading in a precipitation mode is avoided, the activity of the whole formaldehyde in the filter material is reduced, and the activated carbon filter material has better formaldehyde catalytic oxidation performance.
When formaldehyde passes through the activated carbon filter material, the formaldehyde is adsorbed and concentrated on the surface of the activated carbon and Co around the activated carbon by the activated carbon3O4When the transition metal oxides are contacted with each other, the transition metal oxides are converted into nontoxic and harmless CO under the catalytic oxidation action of the transition metal oxides2And H2And O, thereby achieving the purpose of purifying formaldehyde. Through the process, on one hand, the contact time of formaldehyde and the catalyst is prolonged, the catalytic effect of the catalyst on formaldehyde is improved, on the other hand, formaldehyde adsorbed on the activated carbon is continuously consumed under the action of the catalyst, so that the time for the activated carbon to reach adsorption saturation is prolonged, and the method has very important significance for prolonging the service life of the filter material.
An exemplary embodiment of a method of preparing an activated carbon filter material provided according to the present invention will be described in more detail below. These exemplary embodiments may, however, be embodied in many different forms and should not be construed as limited to only the embodiments set forth herein. It should be understood that these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of these exemplary embodiments to those skilled in the art.
First, step S1 is executed: and heating the raw materials comprising the transition metal salt, the precipitator and the first solvent by adopting a microwave hydrothermal method to obtain a transition metal precursor. Specifically, a proper amount of transition metal salt and a precipitator are weighed according to calculation and dissolved in a certain amount of first solvent, the mixed solution is transferred to a high-pressure reaction kettle with a proper volume after being uniformly stirred, and the high-pressure reaction kettle is placed in a microwave heating furnace with a program temperature control for heating treatment.
In the step S1, the transition metal salt may be independently selected from any one of a cobalt salt, a manganese salt, a cerium salt, and an iron salt, and the cobalt salt may be selected from any one of cobalt acetate, cobalt nitrate, cobalt chloride, and cobalt sulfate; the manganese salt may be selected from manganese sulfate, manganese chloride, manganese nitrate, etc.; the cerium salt may be selected from cerium acetate, cerium sulfate, cerium nitrate, etc.; the iron salt may be selected from iron nitrate, iron chloride, iron sulfate, etc.
In step S1, a person skilled in the art can select the kind of the precipitant and the first solvent according to the specific kind of the transition metal salt, for example, when the transition metal salt is a cobalt salt, the precipitant may be urea, and the first solvent may be ethylene glycol or a mixture of ethylene glycol and distilled water.
In order to better improve the synthesis performance of the catalyst, preferably, the first solvent contains distilled water and alcohol, and the volume ratio of the distilled water to the alcohol is controlled to be (1-10): 1, more preferably, the alcohol is ethylene glycol; and, preferably, the temperature of the microwave hydrothermal method is 150-200 ℃, and the heating time is 20-60 min.
In a preferred embodiment, the step S1 includes the following steps: s11, mixing and stirring the transition metal salt, the precipitator and the first solvent to obtain a first mixed solution; s12, heating the first mixed solution by a microwave hydrothermal method to obtain a second mixed solution containing the transition metal precipitate; and S13, separating the transition metal precipitate from the second mixed solution to obtain a transition metal precursor.
In the above preferred embodiment, step S13 may further include a process of drying the separated transition metal precursor; in order to improve the drying efficiency, the drying temperature is preferably 80-120 ℃, and the drying time is preferably 1-24 h.
After the above step S1 is completed, a transition metal precursor is obtained, and then step S2 is performed: and calcining the transition metal precursor to obtain the nano transition metal oxide. The nanometer transition metal oxide can be used as a catalyst to catalyze and oxidize formaldehyde and convert the formaldehyde into nontoxic and harmless CO2And H2And O. For example, the transition metal salt is a cobalt salt, and the obtained nano transition metal oxide is Co3O4，Co3O4The oxide comprising Co at the same time2+、Co3+Cobalt ions in two valence states.
In the step S2, the transition metal precursor may be calcined in a muffle furnace, and in order to improve the conversion efficiency of the metal precursor, the calcination temperature is preferably 300 to 600 ℃, and the calcination time is preferably 1 to 4 hours; more preferably, the temperature is raised from room temperature to the above-mentioned calcination temperature at a temperature raising rate of 1 to 10 ℃/min.
After the step of calcining the transition metal precursor, a rod-shaped transition metal oxide is obtained, and in order to subsequently enrich the rod-shaped transition metal oxide on the activated carbon more by mixing and stirring, preferably, the above step S2 further includes: carrying out tabletting treatment and grinding on the rod-shaped transition metal oxide to obtain granular transition metal oxide; and screening the granular transition metal oxide to obtain the nano transition metal oxide. More preferably, the particulate transition metal oxide is sieved with a 40-60 mesh sieve.
The nano transition metal oxide is obtained through the above step S2, and then the step S3 is performed: mixing the nano transition metal oxide and the activated carbon in a second solvent to load the nano transition metal oxide onto the activated carbon. The nanometer transition metal oxide is loaded on the active carbon by adopting a mixing and stirring mode, so that the problem that pore channels of the active carbon carrier are blocked due to uneven precipitation when the active carbon carrier is loaded by adopting a precipitation mode in the prior art, and the integral activity of the filter material is reduced. The second solvent may be deionized water.
In the step S3, in order to simultaneously increase the loading amount and the loading efficiency of the catalyst, the mass ratio of the nano transition metal oxide to the activated carbon is preferably 1:100 to 1: 10; and, preferably, the stirring speed of the nano transition metal oxide and the activated carbon in the second solvent is 300 to 800 r/min.
After step S3, a second mixed solution containing an activated carbon filter is obtained, in which case, the above preparation method of the present invention may further include the steps of: and separating and drying the activated carbon filter material from the second mixed solution. In order to improve the drying efficiency, the drying temperature is preferably 60-100 ℃, and the drying time is preferably 1-24 h.
According to another aspect of the invention, the invention also provides an activated carbon filter material, and the specific surface area of the activated carbon filter material is 300-1300 m2(ii) in terms of/g. The active carbon filter material can be prepared by the preparation method of the invention, and the preparation method can be adopted to prepare the active carbon filter materialThe method can avoid the catalyst from blocking the active carbon pore canal, so compared with the active carbon filter material obtained by the preparation method in the prior art, the active carbon filter material in the scheme has larger specific surface area, thereby leading the active carbon filter material to have higher activity.
The above-mentioned activated carbon filter material and the preparation method thereof according to the present invention will be further described with reference to examples and comparative examples.
Example 1
The embodiment provides a preparation method of an activated carbon filter material, which comprises the following steps:
1) nano Co3O4The preparation of (1):
preparation of nano Co by microwave hydrothermal method3O4Selecting cobalt acetate as a cobalt source, weighing cobalt acetate and urea according to a mass ratio of 1:4, dissolving the cobalt acetate and urea in a certain amount of mixed solution of ethylene glycol and distilled water (the volume ratio of the distilled water to the ethylene glycol is 12: 1), uniformly stirring, transferring the mixed solution into a high-pressure reaction kettle with a proper volume, and placing the high-pressure reaction kettle in a microwave heating furnace with a programmed temperature control function for heating treatment, wherein the temperature is controlled at 150 ℃, and the heating time is set to be 10 min. And after cooling, separating by adopting a centrifugal mode to obtain a precipitate, washing the precipitate for multiple times by using water and ethanol, and drying the precipitate in a drying oven at the temperature of 100 ℃ for 2 hours. Then calcining the dried solid substance in a muffle furnace at the temperature rise rate of 0.5 ℃/min at 300 ℃ for 0.5h, and cooling to obtain the nano Co with uniform appearance3O4。
For the above obtained nano Co3O4Tabletting on a tabletting machine, grinding in a mortar, sieving the obtained particles with different particle sizes by using a screen, and repeatedly grinding and sieving for multiple times to finally obtain the nano Co with uniform particle size3O4A material.
2)Co3O4Preparation of activated carbon:
selecting proper particle size distribution (the particle size is larger than Co)3O4Particle diameter of) as a carrier, with (Co)3O4: 1:1 of activated carbon50, mass ratio) of Co3O4Dissolving the activated carbon in deionized water, fully stirring at the stirring speed of 200r/min, then carrying out suction filtration, and drying the obtained mixture in a 60 ℃ oven for 1h to obtain the final Co3O4Active carbon filtering material.
Example 2
The difference between the preparation method of the activated carbon filter material provided in this embodiment and embodiment 1 is that:
the mass ratio of the distilled water to the ethylene glycol is 1: 1.
example 3
The difference between the preparation method of the activated carbon filter material provided in this embodiment and embodiment 1 is that:
the mass ratio of the distilled water to the ethylene glycol is 10: 1.
example 4
The difference between the preparation method of the activated carbon filter material provided in this embodiment and embodiment 3 is that:
heating in a microwave oven at 150 deg.C for 20 min.
Example 5
The difference between the preparation method of the activated carbon filter material provided in this embodiment and embodiment 3 is that:
heating in a microwave oven at 200 deg.C for 60 min.
Example 6
The difference between the preparation method of the activated carbon filter material provided in this embodiment and embodiment 5 is that:
and calcining the dried solid substance in a muffle furnace, wherein the heating rate is controlled to be 1 ℃/min, the temperature is 300 ℃, and the calcining time is 1 h.
Example 7
The difference between the preparation method of the activated carbon filter material provided in this embodiment and embodiment 5 is that:
and calcining the dried solid substance in a muffle furnace, wherein the heating rate is controlled to be 10 ℃/min, the temperature is 600 ℃, and the calcining time is 4 h.
Example 8
The difference between the preparation method of the activated carbon filter material provided in this embodiment and embodiment 7 is that:
Co3O4the mass ratio of the active carbon to the active carbon is 1: 100.
Example 9
The difference between the preparation method of the activated carbon filter material provided in this embodiment and embodiment 7 is that:
Co3O4the mass ratio of the active carbon to the active carbon is 1: 10.
Example 10
The difference between the preparation method of the activated carbon filter material provided in this embodiment and embodiment 9 is that:
taking Co3O4And dissolving the activated carbon in deionized water, and fully stirring at the stirring speed of 300 r/min.
Example 11
The difference between the preparation method of the activated carbon filter material provided in this embodiment and embodiment 9 is that:
taking Co3O4And dissolving the activated carbon in deionized water, and fully stirring at the stirring speed of 800 r/min.
Example 12
The embodiment provides a preparation method of an activated carbon filter material, which comprises the following steps:
1) nano CeO2The preparation of (1):
preparation of nano CeO by microwave hydrothermal method2Selecting cobalt acetate as a cobalt source, weighing cerium nitrate and urea according to a mass ratio of 1:4, dissolving the cerium nitrate and the urea in a certain amount of mixed solution of ethylene glycol and distilled water (the volume ratio of the distilled water to the ethylene glycol is 5: 1), uniformly stirring, transferring the mixed solution into a high-pressure reaction kettle with a proper volume, and placing the high-pressure reaction kettle in a microwave heating furnace with a programmed temperature control function for heating treatment, wherein the temperature is controlled at 160 ℃, and the heating time is set to be 30 min. And after cooling, separating by adopting a centrifugal mode to obtain a precipitate, washing the precipitate for multiple times by using water and ethanol, and drying the precipitate in a drying oven at the temperature of 100 ℃ for 2 hours. Then calcining the dried solid substance in a muffle furnace, and controlling the temperature rise rate to be5 ℃/min, the temperature is 500 ℃, the calcination time is 2h, and the nano CeO with uniform appearance is obtained after cooling2。
To the above obtained nano CeO2Tabletting on a tabletting machine, grinding in a mortar, sieving the obtained particles with different particle sizes by using a screen, repeatedly grinding and sieving for multiple times to finally obtain the nano CeO with uniform particle size2A material.
2)CeO2Preparation of activated carbon:
selecting proper particle size distribution (the particle size is larger than CeO)2Particle diameter of (b) as a carrier with (CeO)2: activated carbon 1:20, mass ratio) CeO was weighed out2Dissolving the active carbon in deionized water, fully stirring at the stirring speed of 500r/min, then carrying out suction filtration, and drying the obtained mixture in a 60 ℃ oven for 1h to obtain the final CeO2Active carbon filtering material.
Comparative example 1
This comparative example used activated carbon without a catalyst.
Comparative example 2
This comparative example provides a Co/C process prepared by a common precipitation process, comprising the steps of:
firstly, 0.5 mol/L mol of Na is prepared2CO3The solution is used as a precipitant for standby, and then CoCl is weighed according to calculation2·6H2And adding pure water to dissolve O, adding the dissolved O and active carbon to stir, continuously dropwise adding a precipitator solution under the stirring condition after a period of time till the pH value of the solution is 9, standing and aging for 3h, obtaining an active carbon precipitate through suction filtration and washing, and drying in an oven at 80 ℃ overnight to obtain the final filter material product Co/C.
The formaldehyde catalytic performance of each sample in the above examples and comparative examples was tested, and the formaldehyde performance testing process included: putting a sample to be tested into a fixed bed reactor, introducing air to confirm the tightness of a pipeline, introducing formaldehyde gas, controlling the concentration of formaldehyde within 10ppm by regulating the flow ratio of the formaldehyde gas to the air, measuring the formaldehyde test performance of the catalyst after the gas is stabilized, monitoring the formaldehyde concentration on line by using an infrared spectrum detector, taking the time T for keeping the formaldehyde removal rate above 90% as a parameter for judging the formaldehyde removal performance of the catalyst, and monitoring data on line from the moment of introducing the formaldehyde gas, wherein the test result shows that the T value of the activated carbon material in the comparative example 1 without load is about 15min, the T value of the Co/C prepared by a simple precipitation method in the comparative example 2 is less than 10min, and the performance is even worse than that of a pure activated material, and the sample prepared by the methods in the examples 1-12, the formaldehyde removal rate can still be kept above 90% within about 60 min; the formaldehyde removal rate of the samples in the above examples was measured for about 60min, and the results are shown in table 1.
TABLE 1
| Examples | 1 | 2 | 3 | 4 | 5 | 6 |
| Removal rate of formaldehyde | 90.2％ | 91.1％ | 90.8％ | 91.3％ | 91.4％ | 91.7％ |
| Examples | 7 | 8 | 9 | 10 | 11 | 12 |
| Removal rate of formaldehyde | 91.9％ | 92.2％ | 92.5％ | 92.9％ | 93.1％ | 93.2％ |
From the test results, the activated carbon filter materials prepared in the above examples 1 to 12 can still reach a formaldehyde removal rate of more than 90% in about 60min, and compared with example 1, the activated carbon filter materials prepared in examples 2 to 12 can have a higher formaldehyde removal rate by respectively optimizing the use amount of the raw materials and the process conditions.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
1. firstly, preparing nanometer transition metal oxide with uniform appearance by adopting a microwave hydrothermal method, so that the appearance is more uniform; then loading transition metal oxide on the active carbon to obtain the active carbon filter material, wherein the transition metal oxide has the characteristics of low price, multiple valence states, rapid electron transfer capability, wide source and the like, and Co3O4The transition metal oxide has a large number of surface oxygen cavities on the surface, and the excellent formaldehyde catalytic oxidation performance can be shown due to the beneficial factors such as abundant active oxygen species and multi-valence ions;
2. according to the method, the self-made transition metal oxide is loaded on the activated carbon through direct mixing and stirring, so that the problem that pore channels of the activated carbon carrier are blocked due to uneven precipitation during loading in a precipitation mode, the activity of removing formaldehyde in the whole filter material is reduced, and the activated carbon filter material has better formaldehyde catalytic oxidation performance;
3. the active carbon filter material is used for purifying formaldehyde, so that on one hand, the contact time of the formaldehyde and the catalyst is prolonged, the catalytic effect of the catalyst on the formaldehyde is improved, on the other hand, the formaldehyde adsorbed on the active carbon is continuously consumed under the action of the catalyst, the time for the active carbon to reach adsorption saturation is prolonged, and the active carbon filter material has important significance for prolonging the service life of the filter material.
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 (11)
1. The preparation method of the activated carbon filter material is characterized by comprising the following steps:
s1, heating the raw materials including the transition metal salt, the precipitator and the first solvent by a microwave hydrothermal method to obtain a transition metal precursor;
s2, calcining the transition metal precursor to obtain a nano transition metal oxide;
s3, mixing the nano transition metal oxide and the activated carbon in a second solvent so as to load the nano transition metal oxide on the activated carbon.
2. The method according to claim 1, wherein in step S1, the transition metal salt is independently selected from any one of a cobalt salt, a manganese salt, a cerium salt and an iron salt, preferably the first solvent comprises distilled water and an alcohol, and the volume ratio of the distilled water to the alcohol is (1-10): 1.
3. the preparation method according to claim 1, wherein the temperature of the microwave hydrothermal method is 150-200 ℃ and the heating time is 20-60 min.
4. The production method according to any one of claims 1 to 3, wherein the step S1 includes the steps of:
s11, mixing and stirring the transition metal salt, the precipitant and the first solvent to obtain a first mixed solution;
s12, heating the first mixed solution by adopting a microwave hydrothermal method to obtain a second mixed solution containing the transition metal precipitate;
and S13, separating the transition metal precipitate from the second mixed solution to obtain the transition metal precursor.
5. The preparation method according to claim 4, wherein the step S13 further comprises a process of drying the separated transition metal precursor, preferably at a temperature of 80-120 ℃ for 1-24 h.
6. The preparation method according to claim 1, wherein in the step S2, the calcination temperature is 300-600 ℃, the calcination time is 1-4 h, and the temperature rise rate is preferably 1-10 ℃/min.
7. The production method according to claim 1 or 6, wherein a rod-shaped transition metal oxide is obtained after the step of calcining the transition metal precursor, and the step S2 further includes:
tabletting and grinding the rod-shaped transition metal oxide to obtain granular transition metal oxide;
and screening the granular transition metal oxide to obtain the nano transition metal oxide.
8. The preparation method according to claim 1, wherein in the step S3, the mass ratio of the nano transition metal oxide to the activated carbon is 1:100 to 1: 10.
9. The method according to claim 1 or 8, wherein in the step S3, the stirring speed is 300 to 800 r/min.
10. The active carbon filter material is characterized in that the specific surface area of the active carbon filter material is 300-1300 m2/g。
11. The activated carbon filter material according to claim 10, which is produced by the production method according to any one of claims 1 to 9.
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