AU2020100596A4 - A Magnetic Catalyst For Bentonite Fenton And Its Preparation Method - Google Patents
A Magnetic Catalyst For Bentonite Fenton And Its Preparation Method Download PDFInfo
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- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 229910000278 bentonite Inorganic materials 0.000 title claims abstract description 63
- 239000000440 bentonite Substances 0.000 title claims abstract description 62
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 56
- 239000003054 catalyst Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 239000002105 nanoparticle Substances 0.000 claims abstract description 25
- 239000011148 porous material Substances 0.000 claims abstract description 22
- 239000011159 matrix material Substances 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 39
- 239000000203 mixture Substances 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 13
- 239000012456 homogeneous solution Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims description 13
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 12
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 12
- 239000001632 sodium acetate Substances 0.000 claims description 12
- 235000017281 sodium acetate Nutrition 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 11
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 11
- 239000002244 precipitate Substances 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 5
- 230000009471 action Effects 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 5
- 230000005415 magnetization Effects 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 2
- 229960004249 sodium acetate Drugs 0.000 claims description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 abstract description 19
- 238000001179 sorption measurement Methods 0.000 abstract description 16
- 230000000694 effects Effects 0.000 abstract description 12
- 239000010410 layer Substances 0.000 abstract description 9
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 abstract description 7
- 229940012189 methyl orange Drugs 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 239000008204 material by function Substances 0.000 abstract description 2
- 239000002344 surface layer Substances 0.000 abstract description 2
- 238000004042 decolorization Methods 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 8
- 239000002114 nanocomposite Substances 0.000 description 8
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 8
- 230000003197 catalytic effect Effects 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid group Chemical group C(CC(O)(C(=O)O)CC(=O)O)(=O)O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 239000000975 dye Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 3
- 238000007885 magnetic separation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052901 montmorillonite Inorganic materials 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- -1 ion compound Chemical class 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000004043 responsiveness Effects 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229920000604 Polyethylene Glycol 200 Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000002068 genetic effect Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- 238000002595 magnetic resonance imaging Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 229940031182 nanoparticles iron oxide Drugs 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/16—Clays or other mineral silicates
-
- 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
- B01J23/745—Iron
-
- 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
- B01J35/63—Pore volume
- B01J35/635—0.5-1.0 ml/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
- B01J35/64—Pore diameter
- B01J35/647—2-50 nm
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0203—Impregnation the impregnation liquid containing organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/08—Nanoparticles or nanotubes
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- Life Sciences & Earth Sciences (AREA)
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- Environmental & Geological Engineering (AREA)
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Abstract
Abstract The invention discloses a magnetic catalyst for bentonite Fenton and its preparation method, which belong to the technical field of inorganic functional materials. The modified bentonite is used as a loaded matrix to load magnetic Fe304 nanoparticles. The Fe304 nanoparticles are loaded between the layers and pores of the modified bentonite. The present invention uses modified bentonite as the main body and loads magnetic Fe304 nanoparticles. At the same time, the preparation process parameters are studied. The prepared bentonite Fenton magnetic catalyst has a loose pore structure, the inner and outer surface layers are expanded, which improves the removal effect of methyl orange and is beneficial to the adsorption of methyl orange.
Description
Descriptions
A magnetic catalyst for bentonite Fenton and its preparation method
Technical Field
The invention relates to the technical field of inorganic functional materials, in particular to a magnetic catalyst for bentonite Fenton and its preparation method.
Background Technology
In recent years, China's textile printing and dyeing industry has developed rapidly, resulting in a large amount of dye wastewater that needs to be treated urgently. General chemical dyes often have the characteristics of acid resistance, alkali resistance, and refractory degradation, which affect the genetic inheritance of aquatic plants and animals, seriously threaten their survival, and may threaten human life.
As one of the rich clay mineral resources in China, Bentonite is cheap and has great value in exploitation and research. Bentonite is mainly composed of water-containing layered aluminosilicate, and its basic performance is determined by the special structure of montmorillonite. Bentonite is mainly composed of water-containing layered aluminosilicate, and its basic performance is determined by the special structure of montmorillonite. The structure of montmorillonite determines the decolorization, stability, ion exchange, adsorption, suspension, etc. of bentonite. The internal specific surface area of bentonite is 600-800m2/g, and the volume of bentonite after water absorption can be increased by 10-30 times , which has a certain adsorption for dyes; however, the unmodified natural bentonite (Raw Bentonite, RB) has poor adsorption properties for dyes, and its strong dispersibility in water also makes it difficult for the adsorbed bentonite to achieve effective solid-liquid separation. Therefore, it is necessary to carry out organic modification or loading Fe3O4 of magnetic substances such as bentonite to improve its adsorption performance and solid-liquid separation ability.
Magnetic carrier refers to covering or introducing a strong magnetic substance with good dispersion performance to the surface or inside of a non-magnetic or weak magnetic material to form a composite material with a certain magnetic saturation strength, which can be separated quickly by solid-liquid under the action of external magnetic field and then recovered and reused. Fe3O4 nanoparticles are one of the most common magnetic materials. Its synthesis process is simple, it has good magnetic separation performance, and the Fe3O4 nanoparticles themselves have a certain adsorption capacity. However, FeTL nanoparticles are easy to agglomerate, easy to oxidize, and their properties are unstable, while bentonite has good dispersion in water. Therefore, the combination of bentonite and Fe3O4 nanoparticles to prepare Magnetic bentonite (MB) can not only solve the problems of easy agglomeration, easy oxidation and unstable performance of Fe3O4 nanoparticles, but also improve the solid-liquid separation ability of bentonite, and at the same time improve its adsorption ability to dye to a certain extent: Wang Yingya and other scholars prepared Fe3O4 nanoparticles by precipitation method, and attached them to alkaline calcium-based bentonite, i
Descriptions and then modified with citric acid to prepare a composite of magnetic citric acid bentonite, which has a good magnetic separation effect and good adsorption effect on Cr (VI); Ren Shuang and other scholars added Fe2(SO4)3 and FeaCU to the bentonite suspension, and then added anion (cation) ion compound modifier to prepare anion (cation) ion compound modified amphoteric magnetic bentonite, the surface area of the composite and the pore diameter of the pore volume increased significantly, the adsorption effect of phenol also increased significantly, and the adsorption capacity reached 491.61 mg/g.
The prior art discloses a new type of ferric oxide-modified bentonite (FeaCU-BT) catalyst, and its 60min decolorization rate of methyl orange is about 96.72%. However, the nanoparticles of Fe3O4 are mainly present on the surface of the modified bentonite and the outermost pores, most of which are on the surface of bentonite. Although such a structure improves the separation ability of bentonite to some extent, the nano-iron trioxide particles on the surface are easily oxidized and lose part of magnetism. Therefore, the pure surface structure of FeaCU nanoparticles loaded modified bentonite not only has little effect on the adsorption of dyes, but also because its magnetic property is easily oxidized, the solid-liquid separation effect is also not good.
Invention Summary
The object of the present invention is to provide a magnetic catalyst for bentonite Fenton and its preparation method to solve the above-mentioned problems in the prior art.
To achieve the above objectives, the present invention provides the following solutions:
The invention provides a bentonite Fenton magnetic catalyst, which is used as a loaded matrix to load magnetic Fe3O4 nanoparticles. The FcaCfi nanoparticles are loaded between the layers and pores of the modified bentonite.
Further, the layer spacing of the bentonite Fenton magnetic catalyst is 1.35-1.58 nm, the pore diameter is 6.25-6.85 nm, the pore volume is 0.48-0.52cm3/g, and the thermal stability can be maintained at 300-700°C ; the saturation magnetization value is 25.34-34.28emu/g, and the solid-liquid separation can be achieved within 2-4 s under the action of an external magnetic field, and it is slightly soluble in strong acid and strong alkali.
The invention also provides a method for preparing bentonite Fenton magnetic catalyst, which uses hydrothermal reaction to synthesize FeaCU / modified bentonite.
Further, the method includes the following steps:
The mixture of ferric chloride hexahydrate, sodium acetate and polyethylene glycol 200 is stirred in ethylene glycol to form a homogeneous solution.
The modified bentonite and epichlorohydrin are added into homogeneous solution and continuously stirred;
Descriptions
After the mixture is heated and reacted, it is cooled to indoor temperature to form a black solution;
After filtration, the precipitate is washed with distilled water / ethanol, dried, and finally a bentonite Fenton magnetic catalyst is obtained.
Still further, the method includes the following steps:
(1) A mixture of 2.16 grams of ferric chloride hexahydrate, 5.76 grams of sodium acetate, and 1.6 grams of polyethylene glycol 200 was stirred in 60 milliliters of ethylene glycol for 18 minutes to form a uniform solution;
(2) 0.5 g of modified bentonite and 1 ml of epichlorohydrin are added to the homogeneous solution; tirred for 1.5 hours at 43 ° C ;
(3) The mixture is transferred to a 100 ml autoclave and heated to 200°C for 9 hours, after which it is cooled to indoor temperature to form a black solution;
4) After filtration, the precipitate is washed with distilled water/ethanol (V: V,1: 1) and dried under vacuum 73°C. Finally, bentonite fenton magnetic catalyst is obtained.
The present invention discloses the following technical effects:
The invention takes modified bentonite as the main body and loads magnetic FesCU nanoparticles. At the same time, the preparation process parameters are studied. The prepared bentonite Fenton magnetic catalyst has a loose pore structure, and the inner and outer surface layers are expanded, which improves the removal effect of methyl orange. The reason is that the modified bentonite surface has a large amount of OH-, and the surface of the magnetic FesCU nanoparticles contains NH3 +, NH2 +, and H + ions. These ions are combined with the modified bentonite through electrostatic attraction and loaded between the layers or pores of the modified bentonite; the specially selected preparation parameters make the magnetic iron trioxide nanoparticles insert into the layer edge of the modified bentonite, improve the surface pore structure of the modified bentonite, so that the pore size of the modified bentonite can be increased to a certain extent, forming mesoporous materials and improving the adsorption ability, which is beneficial to the adsorption of methyl orange.
The layer spacing of the bentonite Fenton magnetic catalyst prepared by the invention is 1.58 nm, the pore diameter is 6.85 nm, the pore volume is 0.52cm3/g, and the thermal stability can be maintained at 700°C; the saturation magnetization value is 34.28emu/g, and the solid-liquid separation can be achieved within 2s under the action of an external magnetic field, and it is slightly soluble in strong acid and strong alkali. FesCU nanoparticles enter the interlayer or pores of bentonite, and are not loaded on the surface of bentonite. This structure is beneficial to provide a stable iron source for Fenton reaction, improve the adsorption
Descriptions performance of bentonite, at the same time, improve its magnetic responsiveness and improve the solid-liquid separation effect.
FesCU nanoparticles, as a superparamagnetic oxide, have controllable shape and size, and electron transfer occurs between Fe2+ and Fe3+ at the octahedral sites within the crystal lattice to produce unique electrical and magnetic properties. The use of FesCU nanoparticles has great application prospects and is widely used in various fields such as ferromagnetic fluid, biomedicine, magnetic resonance imaging (MRI), magnetic separation and so on. But at the same time, the FesCU nanoparticles are extremely easy to aggregate, which greatly hinders their application,and the present invention avoids this problem by loading FesCU nanoparticles between the layers and pores of bentonite, and greatly improves the adsorption performance and solid-liquid separation effect of bentonite.
Detailed Description of the Presently Preferred Embodiments
Various exemplary embodiments of the present invention will now be described in detail. The detailed description should not be construed as limiting the invention, but should be understood as a more detailed description of certain aspects, features and embodiments of the invention.
It should be understood that the terms described in the present invention are only used to describe specific embodiments and are not intended to limit the present invention. In addition, for the numerical range in the present invention, it should be understood that each intermediate value between the upper limit and the lower limit of the range is also specifically disclosed. Each smaller range between any stated value or intermediate value in the stated range and any other stated value or intermediate value in the stated range is also included in the invention. The upper and lower limits of these smaller ranges can independently be included or excluded from the range.
Unless otherwise stated, all technical and scientific terms used herein have the same meaning as commonly understood by those of ordinary skill in the art described in the present invention. Although the present invention describes only preferred methods and materials, any methods and materials similar or equivalent to those described herein can also be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference to disclose and describe methods and / or materials related to the documents. In case of conflict with any incorporated documents, the content of this specification shall prevail.
Without departing from the scope or spirit of the present invention, various improvements and changes may be made to the specific mode of implementation of the specification of the present invention, which is obvious to technicians in the field. Other embodiments obtained by the specification of the invention are obvious to the technician. This application specification and embodiments are illustrative only.
All raw materials of the present invention are commercially purchased. The modified
Descriptions bentonite is purchased from Heishan Wancheng Bentonite Co., Ltd., Liaoning Province, China. Before use, the modified bentonite sample is ground and passed through a 120 mesh screen. Its cation exchange capacity (CEC) is 108.4 mmol per 100 g of modified bentonite.Ferric trichloride hexahydrate, sodium acetate, ethylene glycol (EG), polyethylene glycol 200 (PEG200) and epichlorohydrin (ECH) are analytical reagents obtained from Tianjin Kemiou Chemical Reagent Co.,Ltd. (Tianjin, China). The chemical agents used in the present invention are of analytical grade, without further purification.
Embodiment 1
A preparation method of bentonite Fenton magnetic catalyst includes the following steps:
(1) A mixture of 2.16 grams of ferric chloride hexahydrate, 5.76 grams of sodium acetate, and 1.6 grams of polyethylene glycol 200 is stirred in 60 milliliters of ethylene glycol for 18 minutes ;
(2) 0.5 g of modified bentonite and 1 ml of epichlorohydrin are added to the homogeneous solution; the new mixture is continuously stirred for up to 1.5 hours at 43 ° C ;
(3) The mixture is transferred to a 100 ml autoclave and heated to 200°C for 9 hours, after which it is cooled to indoor temperature to form a black solution;
(4) After filtration, the precipitate is washed with distilled water/ethanol (V: V,l: 1) and dried under vacuum 73°C. Finally, bentonite fenton magnetic catalyst is obtained.
After testing, the layer spacing layer spacing of the bentonite Fenton magnetic catalyst prepared by the invention is 1.58 nm, the pore diameter is 6.85 nm, the pore volume is 0.52 cm3/g, and the thermal stability can be maintained at 700°C; the saturation magnetization value is 34.28emu/g, and the solid-liquid separation can be achieved within 2s under the action of an external magnetic field, and it is slightly soluble in strong acid and strong alkali. FC3O4 nanoparticles enter the interlayer or pores of bentonite, and are not loaded on the surface of bentonite. This structure is beneficial to provide a stable iron source for Fenton reaction, improve the adsorption performance of bentonite, at the same time, improve its magnetic responsiveness and improve the solid-liquid separation effect.
Experiment of catalytic performance
Under continuous magnetic mechanical stirring, batch heterogeneous Fenton experiments are carried out in a 250ml glass flask reactor (75 ml actual reaction volume) to remove methyl orange, which represents wastewater pollutants. Usually, an appropriate amount of catalyst is suspended in water (0.5 g/L) and placed in a glass reactor. After the system is heated to an appropriate temperature, methyl orange (100 mg / L) and hydrogen peroxide (5.66 g/L) are added to the reactor. Samples of the solution (1.0 ml) are taken at
Descriptions regular intervals; after the solid particles are removed, 0.5 ml of methanol is added for cold immersion. Ultraviolet-visible spectrophotometry is used to analyze the concentration of organic pollutants in the supernatant with time. The experimental result shows that the decolorization rate of the methyl orange solution in 15 min is 99.85%.
Comparative Example 1
A mixture of 2.16 grams of ferric chloride hexahydrate, 5.76 grams of sodium acetate, and 1.6 grams of polyethylene glycol 200 is uniformly stirred in 60 milliliters of ethylene glycol for 30 minutes. Immediately, 0.5 g of modified bentonite and 1 ml of epichlorohydrin are added to the homogeneous solution; the new mixture is continuously stirred for up to 2 hours at 55 ° C ; next, the mixture is transferred to a 100 ml autoclave and heated to 200°C for 12 hours, after which it is cooled to indoor temperature to form a black solution; After filtration, the precipitate is washed with distilled water/ethanol (1:1) and dried under vacuum 80°C. Finally, the FesCfi / modified bentonite nanocomposite is obtained.
The test shows that most of the FesCU nanoparticles of the FesCU / modified bentonite nanocomposite are loaded on the surface of bentonite.
It is tested with the same catalytic performance experiment in Embodiment 1. The result shows that it reached equilibrium in 20 minutes, and the decolorization rate of the methyl orange solution is only 96.72%.
Comparative Example 2
A preparation method of bentonite Fenton magnetic catalyst includes the following steps:
(1) A mixture of 2.16 grams of ferric chloride hexahydrate, 5.76 grams of sodium acetate, and 1.6 grams of polyethylene glycol 200 is stirred in 60 milliliters of ethylene glycol for 30 minutes ;
(2) 0.5 g of modified bentonite and 1 ml of epichlorohydrin are added to the homogeneous solution; the new mixture is continuously stirred for up to 1.5 hours at 43 ° C ;
(3) The mixture is transferred to a 100 ml autoclave and heated to 200°C for 9 hours, after which it is cooled to indoor temperature to form a black solution;
(4) After filtration, the precipitate is washed with distilled water/ethanol (V: V, 1: 1) and dried under vacuum 73°C. Finally, the FesCU / modified bentonite nanocomposite is obtained.
The test shows that most of the iron oxide nanoparticles of the FesCU / modified bentonite nanocomposite are supported on the surface of bentonite.
Descriptions
It is tested with the same catalytic performance experiment in Example 1. The result shows that it reached equilibrium in 20 minutes, and the decolorization rate of the methyl orange solution is only 97.65%.
Comparative Example 3
A preparation method of bentonite Fenton magnetic catalyst includes the following steps:
(1) A mixture of 2.16 grams of ferric chloride hexahydrate, 5.76 grams of sodium acetate, and 1.6 grams of polyethylene glycol 200 is stirred in 60 milliliters of ethylene glycol for 18 minutes ;
(2) 0.5 g of modified bentonite and 1 ml of epichlorohydrin are added to the homogeneous solution; the new mixture is continuously stirred for up to 1.5 hours at 55 ° C ;
(3) The mixture is transferred to a 100 ml autoclave and heated to 200°C for 9 hours, after which it is cooled to indoor temperature to form a black solution;
(4) After filtration, the precipitate is washed with distilled water/ethanol (V: V, 1: 1) and dried under vacuum 73°C. Finally, the FesCU / modified bentonite nanocomposite is obtained.
It is tested with the same catalytic performance experiment in Example 1. The result shows that it reached equilibrium in 20 minutes, and the decolorization rate of the methyl orange solution is only 97.95%.
Comparative Example 4
A preparation method of bentonite Fenton magnetic catalyst includes the following steps:
(1) A mixture of 2.16 grams of ferric chloride hexahydrate, 5.76 grams of sodium acetate, and 1.6 grams of polyethylene glycol 200 is stirred in 60 milliliters of ethylene glycol for 18 minutes ;
(2) 0.5 g of modified bentonite and 1 ml of epichlorohydrin are added to the homogeneous solution; the new mixture is continuously stirred for up to 2 hours at 43 ° C ;
(3) The mixture is transferred to a 100 ml autoclave and heated to 200°C for 9 hours, after which it is cooled to indoor temperature to form a black solution;
(4) After filtration, the precipitate is washed with distilled water/ethanol (V: V, 1: 1)
Descriptions and dried under vacuum 73°C. Finally, the FesCU / modified bentonite nanocomposite is obtained.
It is tested with the same catalytic performance experiment in Embodiment 1. The result shows that it reached equilibrium in 20 minutes, and the decolorization rate of the methyl orange solution is only 97.23%.
Comparative Example 5
A preparation method of bentonite Fenton magnetic catalyst includes the following steps:
(1) A mixture of 2.16 grams of ferric chloride hexahydrate, 5.76 grams of sodium acetate, and 1.6 grams of polyethylene glycol 200 is stirred in 60 milliliters of ethylene glycol for 18 minutes ;
(2) 0.5 g of modified bentonite and 1 ml of epichlorohydrin are added to the homogeneous solution; the new mixture is continuously stirred for up to 1.5 hours at 43 ° C ;
(3) The mixture is transferred to a 100 ml autoclave and heated to 200°C for 12 hours, after which it is cooled to indoor temperature to form a black solution;
(4) After filtration, the precipitate is washed with distilled water/ethanol (V: V,l: 1) and dried under vacuum 73°C. Finally, the FesCU / modified bentonite nanocomposite is obtained.
It is tested with the same catalytic performance experiment in Embodiment 1. The result shows that it reached equilibrium in 20 minutes, and the decolorization rate of the methyl orange solution is only 94.55%.
Comparative Example 6
A preparation method of bentonite Fenton magnetic catalyst includes the following steps:
(1) A mixture of 2.16 grams of ferric chloride hexahydrate, 5.76 grams of sodium acetate, and 1.6 grams of polyethylene glycol 200 is stirred in 60 milliliters of ethylene glycol for 18 minutes ;
(2) 0.5 g of modified bentonite and 1 ml of epichlorohydrin are added to the homogeneous solution; the new mixture is continuously stirred for up to 1.5 hours at 43 ° C ;
(3) The mixture is transferred to a 100 ml autoclave and heated to 200°C for 9 hours, after which it is cooled to indoor temperature to form a black solution;
(4) After filtration, the precipitate is washed with distilled water/ethanol (V: V, 1: 1)
Descriptions
2020100596 17 Apr 2020 and dried under vacuum 80°C. Finally, the FC3O4 / modified bentonite nanocomposite is obtained.
It is tested with the same catalytic performance experiment in Embodiment 1. The result 5 shows that it reached equilibrium in 20 minutes, and the decolorization rate of the methyl orange solution is only 98.98%.
The present invention has studied the preparation conditions of bentonite Fenton magnetic catalyst. Comparative examples 2-6 show that the bentonite Fenton magnetic 10 catalyst prepared under the process parameters adopted by the present invention has the best decolorization rate of methyl orange solution, and changing any one of its process parameters will adversely affect its catalyst effect.
The above-mentioned embodiments are only for describing the preferred modes of the 15 present invention, and do not limit the scope of the present invention. Without departing from the design spirit of the present invention, various modifications and improvements made by those ordinary technicians in the field to the technical scheme of the present invention shall fall within the scope of protection determined by the claim of the invention.
Claims (4)
- Claims1. A bentonite Fenton magnetic catalyst is characterized in that the modified bentonite is used as a loading matrix to load magnetic FC3O4 nanoparticles, and the FC3O4 nanoparticles are supported between the layers and pores of the modified bentonite.2. The bentonite Fenton magnetic catalyst according to claim 1 is characterized in that the layer spacing of the bentonite Fenton magnetic catalyst is 1.35-1.58 nm, the pore diameter is 6.25-6.85 nm, the pore volume is 0.48-0.52cm3/g, and the thermal stability can be maintained at 300-700°C; the saturation magnetization value is 25.34-34.28emu/g, and the solid-liquid separation can be achieved within 2-4 s under the action of an external magnetic field, and it is slightly soluble in strong acid and strong alkali.3. A method for preparing bentonite Fenton magnetic catalyst according to claim 1 or 2, characterized in that hydrothermal reaction is used to synthesize FC3O4 / modified bentonite.4. The method for preparing a bentonite Fenton magnetic catalyst according to claim 3, characterized in that it comprises the following steps:The mixture of ferric chloride hexahydrate, sodium acetate and polyethylene glycol 200 is stirred in ethylene glycol to form a homogeneous solution.The modified bentonite and epichlorohydrin are added into homogeneous solution and continuously stirred;After the mixture is heated and reacted, it is cooled to indoor temperature to form a black solution;After filtration, the precipitate is washed with distilled water / ethanol, dried, and finally a bentonite Fenton magnetic catalyst is obtained.5. The method for preparing a bentonite Fenton magnetic catalyst according to claim 4, characterized in that it comprises the following steps:(1) A mixture of 2.16 grams of ferric chloride hexahydrate, 5.76 grams of sodium acetate, and 1.6 grams of polyethylene glycol 200 is stirred in 60 milliliters of ethylene glycol for 18 minutes to form a uniform solution;
- (2) 0.5 g of modified bentonite and 1 ml of epichlorohydrin are added to the homogeneous solution; tirred for 1.5 hours at 43 0 C ;
- (3) The mixture is transferred to a 100 ml autoclave and heated to 200°C for 9 hours, after which it is cooled to indoor temperature to form a black solution;
- 4) After filtration, the precipitate is washed with distilled water/ethanol (V: V,1: 1) and dried under vacuum 73°C. Finally, bentonite fenton magnetic catalyst is obtained.
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