CN114950433A - Fe 0 @Fe 3 O 4 Preparation method and application of volcanic catalyst - Google Patents
Fe 0 @Fe 3 O 4 Preparation method and application of volcanic catalyst Download PDFInfo
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- CN114950433A CN114950433A CN202210726151.XA CN202210726151A CN114950433A CN 114950433 A CN114950433 A CN 114950433A CN 202210726151 A CN202210726151 A CN 202210726151A CN 114950433 A CN114950433 A CN 114950433A
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- 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
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention discloses Fe 0 @Fe 3 O 4 Preparation method and application of volcanic catalyst, belonging to the technical field of metal or metal oxide catalyst. The method comprises the following steps of (1) carrying out high-temperature heat treatment on volcanic rock: crushing, screening, washing, drying and roasting; (2) FeSO (ferric oxide) is added 4 And Fe 2 O 3 Preparation of Fe from volcanic rock and ammonia water 3 O 4 Volcanic catalyst; (3) will dissolve FeSO 4 Distilled water of (2) is added to the solution containing Fe 3 O 4 Introducing nitrogen into a container of the volcanic catalyst, adding a sodium borohydride solution, stirring for reaction, cleaning and drying to obtain Fe 0 @Fe 3 O 4 Volcanic catalyst. The invention utilizes the iron element of the volcanic rock to modify the volcanic rockPreparation of Fe 0 @Fe 3 O 4 The prepared catalyst can effectively catalyze methylene blue in wastewater to decolor, the cost is low, and the decoloration rate in 3 hours can reach 98%.
Description
Technical Field
The invention relates to the technical field of metal or metal oxide catalysts, in particular to Fe 0 @Fe 3 O 4 Volcanic rock modified catalyst.
Background
The volcanic rock has rough and porous surface, good stability, corrosion resistance and hydrophilicity, can replace quartz sand, active carbon, anthracite and the like to be used as a filter medium in the aspects of treating municipal sewage, biochemical organic industrial wastewater, slightly polluted water and the like, has complex surface components and contains dozens of mineral substances and trace elements, namely silicon, aluminum, calcium, manganese, iron, molybdenum and the like. Volcanic rock is researched and applied by more and more people due to the characteristics of low price, stable property, composition of more than ten kinds of minerals and trace elements, and the like, for example, volcanic rock is used as a carrier to prepare a novel efficient catalyst.
Yan, etc. with volcanic rock as carrier, by isovolumetric impregnation x Volcanic catalyst, and evaluating the activity of the catalyst by simulating methylene blue wastewater. At a roasting temperature of 200 ℃ and an ozone flux of 1.0 mg/min -1 Under the condition, the decoloring rate of the catalyst to methylene blue reaches 100 percent when the catalyst is used for 12 min. (Yan, Houyongjiang, Liu, etc., volcanic rock loaded manganese-containing oxides catalyzed ozonization degradation of methylene blue in water, Industrial catalysis, 2016, 24 (09): 23-28).
Magnetic Fe 3 O 4 The nanometer material has wide application in biology, chemistry, medicine, spaceflight and other aspects. The ferroferric oxide has larger specific surface area and can adsorb pollutants in sewage. And Fe 3 O 4 The preparation method is simple and low in price. Liuyiqing and the like through preparing magnetic Fe 3 O 4 The activated persulfate degrades sulfamethoxazole in water, and the degradation rate can reach 93.3 percent (Liuyiqing, Subingqin, taoyuan and the like, magnetic nano Fe) in 180 min 3 O 4 Activated persulfate is used for degrading sulfamethoxazole in water, and the environmental engineering report 2020 and 14(9) comprise: 2515-2526). Utilization of nano Fe for aged seedling 3 O 4 /H 2 O 2 The Fenton-like system can almost completely degrade sulfamethoxazole (aged seedling, Huchunhua, Guocheng, etc.) with the concentration of 20mg/L and magnetic Fe 3 O 4 Preparation of nano particles and research on catalytic degradation of sulfamethoxazole in water, water resource and water engineering report, 2018, 29 (5): 46-52). The nanometer zero-valent iron (nZVI) can be used for removing methylene blue and organic dye pollution in sewage due to strong adsorption capacity, reduction capacity and antibacterial capacityAnd the like. Through preparing the biochar loaded nano zero-valent iron, danjunmin is used as a catalyst of a Fenton system to degrade sulfadimethomozine in water, and the removal rate can reach 74.04% (danmin, research on removal of pollutants by biochar loaded nano zero-valent iron in a reduction and oxidation system, Changsha, university of Hunan, 2018).
The printing and dyeing as a water pollution household has the wastewater discharge amount and the total pollutant amount at the forefront of national industrial departments, and occupies about seven components of the wastewater of textile industry. And the organic dye in the printing and dyeing wastewater has high chroma, a plurality of components, poor biodegradability and difficult degradation, and is a relatively difficult category in industrial wastewater. Among them, Methylene Blue (MB) is one of typical contaminants, and has a molecular formula of C 16 H 18 N 3 SCl is soluble in water, ethanol and the like, and the water body is alkaline and is a heterocyclic aromatic organic matter. Most of the molecules in the dye are ionizable molecules, and have different auxochromes and chromophores, and different forms and properties. The dye components are stable, benzene rings, naphthalene, quinone and the like in the molecular structure are difficult to degrade, when aromatic rings are replaced by sulfonic acid, a mixed system is formed in the environment and is difficult to naturally decompose when entering the environment, and serious harm is caused to the environment and human bodies when the MB concentration is high.
Disclosure of Invention
The technical problem to be solved by the invention is to provide Fe 0 @Fe 3 O 4 The prepared catalyst has better catalytic performance, can effectively catalyze the decolorization of methylene blue in hydrogen peroxide oxidation wastewater, is simple and easy to operate, has low cost, and realizes the recycling of the volcanic. The catalyst prepared by the invention catalyzes the oxidative decolorization of methylene blue of 100ml and 20mg/L, and the decolorization rate reaches 98% in 3 hours.
Fe 0 @Fe 3 O 4 The preparation method of the volcanic catalyst comprises the following steps of (1) carrying out high-temperature heat treatment on volcanic: crushing, screening, washing and drying the volcanic rock, putting the volcanic rock into a crucible and roasting in a muffle furnace after drying, and separating Fe out of the surface of the volcanic rock 2 O 3 To obtain Fe 2 O 3 Volcanic rock;
after being crushed, the mixture is sieved, and the particle size is controlled to be 200-300 meshes.
Naturally heating the volcanic rock from room temperature to 950 ℃ after drying, roasting for 3h, cooling to room temperature, and taking out.
(2) FeSO (ferric oxide) is added 4 And Fe 2 O 3 Adding volcanic rock into a container containing distilled water, continuously stirring until the mixture is uniformly mixed, slowly adding ammonia water into the mixture in the container, continuously stirring at 50-70 ℃ until the reaction is complete, cooling, filtering, washing and drying to obtain Fe 3 O 4 Volcanic catalyst.
The reaction process is as follows: fe 2+ +2Fe 3+ +8OH − →Fe 3 O 4 +4H 2 O。
(3) Taking FeSO 4 Dissolving in distilled water to dissolve FeSO 4 To the solution containing Fe 3 O 4 Introducing nitrogen into a container of the volcanic catalyst to exhaust air, dropwise adding excessive sodium borohydride solution to fully reduce ferrous iron to zero-valent iron, respectively washing with oxygen-free water and deoxidized anhydrous ethanol for several times after complete stirring reaction, and vacuumizing and drying to obtain Fe 0 @Fe 3 O 4 Volcanic catalyst.
The reaction process is as follows: fe 2+ + 2BH 4 − + 6H 2 O →Fe 0 ↓+ 2B(OH) 3 + 7H 2 ↑。
Drying for 24 hours in a forced air drying oven at the temperature of 50-70 ℃ in the step (1); preferably, the drying is carried out in a forced air drying oven at 60 ℃ for 24 hours.
Roasting in a muffle furnace at 900-1000 ℃ for 3 hours in the step (1); preferably a muffle furnace at 950 ℃ for 3 hours.
The mass concentration of the ammonia water in the step (2) is 25 percent, and the dropping speed of the separating funnel is controlled to be 1-2 drops/s for slow dropping.
In the step (3), the sodium borohydride solution is formed by dissolving solid sodium borohydride in a sodium hydroxide solution, every 0.855g of sodium borohydride is dissolved in 50ml of the sodium hydroxide solution, and the pH value of the sodium hydroxide solution is 13.
FeSO in step (2) 4 And Fe 2 O 3 The mass ratio of volcanic rock to volcanic rock is 1: 1-3; preferred FeSO 4 And Fe 2 O 3 The mass ratio of the raw materials to the volcanic rock is 1: 2.
FeSO in step (3) 4 With Fe 3 O 4 The mass ratio of the volcanic catalyst to the volcanic catalyst is 1: 1-3.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
(1) the invention utilizes the iron element of the volcanic rock to modify the volcanic rock under the condition of reducing the additional iron source to prepare Fe 0 @Fe 3 O 4 The prepared catalyst has good catalytic performance, can effectively catalyze the decolorization of methylene blue in hydrogen peroxide oxidation wastewater, is simple and easy to operate, has low cost, and realizes the recycling of the volcanic.
(2) Under the conditions of 0.5g of the catalyst prepared in example 1 and 2ml of 30% hydrogen peroxide, the catalyst prepared by the invention catalyzes 100ml of methylene blue with the oxidation and decolorization of 20mg/L, and the decolorization rate at 3 hours reaches 98%.
Drawings
FIG. 1 shows Fe obtained in example 1 of the present invention 3 O 4 XRD pattern (X-ray diffraction pattern) of volcanic rock.
FIG. 2 shows Fe obtained in example 1 of the present invention 0 @Fe 3 O 4 XRD pattern (X-ray diffraction pattern) of volcanic catalyst.
FIG. 3 shows Fe obtained in example 1 of the present invention 0 @Fe 3 O 4 TEM image (transmission electron micrograph) at 100nm scale of the/volcanic catalyst.
FIG. 4 shows Fe obtained in example 1 of the present invention 0 @Fe 3 O 4 TEM image (transmission electron micrograph) of volcanic catalyst at 50nm scale
FIG. 5 is H 2 O 2 In amounts corresponding to the amounts of Fe prepared in example 1 of the present invention 0 @Fe 3 O 4 Influence diagram of removing methylene blue by catalysis of volcanic catalyst.
FIG. 6 shows the pH value versus the present inventionFe prepared in example 1 0 @Fe 3 O 4 Influence diagram of removing methylene blue by catalysis of volcanic catalyst.
FIG. 7 is a graph of reaction temperature versus Fe prepared in example 1 of the present invention 0 @Fe 3 O 4 Influence diagram of removing methylene blue by catalysis of volcanic catalyst.
Detailed Description
Example 1
(1) Pretreatment of volcanic rock: selecting clean and regular volcanic rock, crushing in a crusher, sieving with 200-mesh and 300-mesh standard sieves, washing the sieved volcanic rock with water for several times, and drying in a blast drying oven at 60 deg.C for 24 hr to obtain clean volcanic rock.
(2) Preparation of oxygen-free water and oxygen-free absolute ethyl alcohol: and respectively pouring deionized water and absolute ethyl alcohol into a washing bottle, filling nitrogen, and evacuating air for later use.
(3) Thermal treatment of volcanic rock at 950 ℃: putting 5g of clean volcanic rock into a crucible, putting the crucible into a muffle furnace, heating to 950 ℃, roasting for 3h, and separating Fe on the surface of the volcanic rock 2 O 3 To obtain Fe 2 O 3 Volcanic rock.
(4) 2.5g of FeSO are taken 4 Same as 5g Fe 2 O 3 Volcanic rock was added together into a clean glass beaker with 25 mL deionized water and stirred continuously at 25 ℃ for 45 min. Then, 15 mL of aqueous ammonia (25%) was slowly added to the mixture as a precipitant. Stirring at 60 deg.C under alkaline condition for 2 hr, naturally cooling to room temperature, vacuum filtering, centrifugal washing with deionized water and anhydrous ethanol, and drying to obtain Fe 3 O 4 Volcanic rock.
(5) 2.5g of FeSO are taken 4 Dissolving in 50mL of distilled water, transferring the solution to a solution containing Fe 3 O 4 A three-neck flask of volcanic rock is filled with N 2 0.855g of sodium borohydride is dissolved in 50mL of sodium hydroxide solution and added dropwise, and the reaction is continuously stirred for 1 h to generate Fe 0 @Fe 3 O 4 Volcanic catalyst is prepared by alternately cleaning with oxygen-free water and oxygen-free anhydrous ethanol for several times, placing in a vacuum drying oven, vacuumizing, and drying in vacuumDrying for 24 h at 60 ℃ to obtain a sample.
Example 2
(1) Pretreatment of volcanic rock: selecting clean and regular volcanic rock, crushing in a crusher, sieving with 200-mesh and 300-mesh standard sieves, washing the sieved volcanic rock with water for several times, and drying in a blast drying oven at 50 deg.C for 24 hr to obtain clean volcanic rock.
(2) Preparation of oxygen-free water and oxygen-free absolute ethyl alcohol: and respectively pouring deionized water and absolute ethyl alcohol into a washing bottle, filling nitrogen, and evacuating air for later use.
(3) Carrying out 900 ℃ heat treatment on volcanic rock: placing 2.5g clean volcanic rock into a crucible, placing into a muffle furnace, heating to 900 deg.C, calcining for 3 hr to separate out Fe on the surface of volcanic rock 2 O 3 To obtain Fe 2 O 3 Volcanic rock.
(4) 2.5g of FeSO are taken 4 Same 2.5g Fe 2 O 3 Volcanic rock was added together into a clean glass beaker with 25 mL deionized water and stirred continuously at 25 ℃ for 45 min. Then, 10mL of aqueous ammonia (25%) was slowly added to the mixture as a precipitant. Stirring at 60 deg.C under alkaline condition for 2 hr, naturally cooling to room temperature, vacuum filtering, centrifugal washing with deionized water and anhydrous ethanol, and drying to obtain Fe 3 O 4 Volcanic rock.
(5) 2.5g of FeSO were taken 4 Dissolved in 50mL of distilled water, and the solution was transferred to a solution containing 2.5g of Fe 3 O 4 A three-neck flask of volcanic rock is filled with N 2 0.855g of sodium borohydride is dissolved in 50mL of sodium hydroxide solution and added dropwise, and the reaction is continuously stirred for 1 h to generate Fe 0 @Fe 3 O 4 The volcanic catalyst is alternately cleaned by using oxygen-free water and oxygen-free absolute ethyl alcohol for a plurality of times, put into a vacuum drying oven, vacuumized and dried for 24 hours at the temperature of 60 ℃ to obtain a sample.
Example 3
(1) Pretreatment of volcanic rock: selecting clean and regular volcanic rock, crushing in a crusher, sieving with 200-mesh and 300-mesh standard sieves, washing the sieved volcanic rock with water for several times, and drying in a blast drying oven at 70 deg.C for 24 hr to obtain clean volcanic rock.
(2) Preparation of oxygen-free water and oxygen-free absolute ethyl alcohol: and respectively pouring deionized water and absolute ethyl alcohol into a washing bottle, filling nitrogen, and evacuating air for later use.
(3) Carrying out heat treatment on volcanic rock at 1000 ℃: putting 7.5g of clean volcanic rock into a crucible, putting the crucible into a muffle furnace, heating to 1000 ℃, roasting for 3h, and separating Fe out of the surface of the volcanic rock 2 O 3 To obtain Fe 2 O 3 Volcanic rock.
(4) 2.5g of FeSO are taken 4 Same as 7.5g Fe 2 O 3 Volcanic rock was added together into a clean glass beaker with 25 mL deionized water and stirred continuously at 25 ℃ for 45 min. Then, 20mL of aqueous ammonia (25%) was slowly added to the mixture as a precipitant. Stirring at 60 deg.C under alkaline condition for 2 hr, naturally cooling to room temperature, vacuum filtering, centrifugal washing with deionized water and anhydrous ethanol, and drying to obtain Fe 3 O 4 Volcanic rock.
(5) 2.5g of FeSO are taken 4 Dissolved in 50mL of distilled water, and the solution was transferred to a solution containing 7.5g of Fe 3 O 4 A three-neck flask of volcanic rock is filled with N 2 0.855g of sodium borohydride is dissolved in 50mL of sodium hydroxide solution and added dropwise, and the reaction is continuously stirred for 1 h to generate Fe 0 @Fe 3 O 4 The volcanic catalyst is alternately washed by oxygen-free water and oxygen-free absolute ethyl alcohol for a plurality of times respectively, and then is put into a vacuum drying oven for vacuumizing and drying for 24 hours at the temperature of 60 ℃ to obtain a sample.
Examples of specific applications
Under the conditions of 0.5g of the catalyst prepared in example 1 and 1ml, 2ml and 3ml of 30% hydrogen peroxide, the catalyst prepared by the invention catalyzes 100ml and 20mg/L of methylene blue to be oxidized and decolored, the decoloration rate is shown in figure 3, and the decoloration rate reaches 98% under the condition of 2ml of hydrogen peroxide for 3 hours.
Under the conditions that 0.5g of the catalyst prepared in example 1 is adopted and the pH is respectively 5, 7 and 9, the catalyst prepared by the invention catalyzes 100ml of methylene blue and 20mg/L of the methylene blue to be subjected to oxidative decolorization, the decolorization rate is shown in the attached figure 4, and the decolorization rate reaches 98% under the condition of pH =7 for 3 h.
The catalyst prepared by the invention can catalyze the oxidative decoloration of methylene blue of 100ml and 20mg/L under the conditions of 0.5g of the catalyst prepared by the embodiment 1, 15 ℃, 25 ℃, 35 ℃ and 45 ℃, the decoloration rate is shown in a figure 5, and the decoloration rate reaches 98% under the condition of 25 ℃ for 3 hours.
Claims (7)
1.Fe 0 @Fe 3 O 4 A preparation method of the volcanic catalyst is characterized by comprising the following steps: the method comprises the following steps of (1) carrying out high-temperature heat treatment on the volcanic rock: crushing, screening, washing and drying the volcanic rock, putting the volcanic rock into a crucible and roasting in a muffle furnace after drying, and separating Fe out of the surface of the volcanic rock 2 O 3 To obtain Fe 2 O 3 Volcanic rock; (2) FeSO (ferric oxide) is added 4 And Fe 2 O 3 Adding volcanic rock into a container containing distilled water, continuously stirring until the mixture is uniformly mixed, slowly adding ammonia water into the mixture in the container, continuously stirring at 50-70 ℃ until the reaction is complete, cooling, filtering, washing and drying to obtain Fe 3 O 4 Volcanic catalyst; (3) taking FeSO 4 Dissolving in distilled water to dissolve FeSO 4 Distilled water of (2) is added to the solution containing Fe 3 O 4 Introducing nitrogen into a container of the volcanic catalyst to exhaust air, dropwise adding excessive sodium borohydride solution to fully reduce ferrous iron into zero-valent iron, respectively alternately cleaning with oxygen-free water and deoxidized anhydrous ethanol for several times after complete stirring reaction, and vacuumizing and drying to obtain Fe 0 @Fe 3 O 4 Volcanic catalyst.
2. The method for preparing a volcanic catalyst as claimed in claim 1, wherein: and (2) drying for 24 hours in a forced air drying oven at the temperature of between 50 and 70 ℃ in the step (1).
3. A method for preparing a volcanic catalyst as defined in claim 1, wherein: in the step (1), the material is roasted in a muffle furnace at 900-1000 ℃ for 3 hours.
4. The method for preparing a volcanic catalyst as claimed in claim 1, wherein: the mass concentration of the ammonia water in the step (2) is 25 percent.
5. The method for preparing a volcanic catalyst as claimed in claim 1, wherein: in the step (3), the sodium borohydride solution is formed by dissolving solid sodium borohydride in a sodium hydroxide solution, every 0.855g of sodium borohydride is dissolved in 50ml of the sodium hydroxide solution, and the pH value of the sodium hydroxide solution is 13.
6. The method for preparing a volcanic catalyst as claimed in claim 1, wherein: FeSO in step (2) 4 And Fe 2 O 3 The mass ratio of the raw materials to the volcanic rock is 1: 1-3.
7. The method for preparing a volcanic catalyst as claimed in claim 1, wherein: FeSO in step (3) 4 With Fe 3 O 4 The mass ratio of the volcanic catalyst to the volcanic catalyst is 1: 1-3.
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Citations (4)
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| CN1235868A (en) * | 1998-04-30 | 1999-11-24 | 科地亚泰乐股份有限公司 | Arsenic adsorbent and fluorine adsorbent using soil as raw material and its producing method |
| JP2004255376A (en) * | 2003-02-05 | 2004-09-16 | Ishihara Sangyo Kaisha Ltd | Environmental purification material and environmental purification method using the same |
| CN106040244A (en) * | 2016-06-01 | 2016-10-26 | 中国科学院过程工程研究所 | Supported solid catalyst for Fenton reaction and preparing method thereof |
| CN112169727A (en) * | 2020-10-21 | 2021-01-05 | 哈尔滨理工大学 | Preparation method of halloysite-based micro-nano reactor for advanced catalytic oxidation |
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- 2022-06-24 CN CN202210726151.XA patent/CN114950433A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1235868A (en) * | 1998-04-30 | 1999-11-24 | 科地亚泰乐股份有限公司 | Arsenic adsorbent and fluorine adsorbent using soil as raw material and its producing method |
| JP2004255376A (en) * | 2003-02-05 | 2004-09-16 | Ishihara Sangyo Kaisha Ltd | Environmental purification material and environmental purification method using the same |
| CN106040244A (en) * | 2016-06-01 | 2016-10-26 | 中国科学院过程工程研究所 | Supported solid catalyst for Fenton reaction and preparing method thereof |
| CN112169727A (en) * | 2020-10-21 | 2021-01-05 | 哈尔滨理工大学 | Preparation method of halloysite-based micro-nano reactor for advanced catalytic oxidation |
Non-Patent Citations (2)
| Title |
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| AHMED S.A.A. ABU SHARIB ET AL.: "Utilizing modifed weathered basalt as a novel approach in the preparation of Fe3O4 nanoparticles: Experimental and theoretical studies for crystal violet adsorption", JOURNAL OF ENVIRONMENTAL CHEMICAL ENGINEERING, pages 1 * |
| 杨博: "金属氧化物/石墨烯复合材料催化降解亚甲基蓝研究", 中国优秀硕士学位论文全文数据库 工程科技I辑, pages 17 - 18 * |
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