CN111774095A - Preparation of FeNiY-MOF composite peroxymonosulfate activator with activated alumina as matrix, product and application - Google Patents
Preparation of FeNiY-MOF composite peroxymonosulfate activator with activated alumina as matrix, product and application Download PDFInfo
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Abstract
The invention relates to a preparation method of FeNiY-MOF composite peroxymonosulfate activator with active alumina as matrix and a product and application thereof2O3‑NiO‑Y2O3-MOF composite catalysisThe agent effectively promotes the activation of PMS by utilizing the interaction among the components and accelerates SO4 ·‑Generation of and decomposition of contaminants. In addition, the synergistic effect between the carrier and the active component promotes the improvement of the load rate of FeNiY-MOF particles, effectively avoids the dissolution of transition metal ions and improves the catalytic activation capability on PMS.
Description
Technical Field
The invention relates to a preparation method of FeNiY-MOF composite peroxymonosulfate activator with activated alumina as matrix, and a product and application thereof, which can solve the problems of water pollution such as high organic matter content, high COD concentration and the like and are used in the field of water pollution treatment.
Background
The advanced oxidation method can directly mineralize the pollutants or improve the biodegradability of the pollutants through oxidation, effectively solves the problems of low efficiency, high cost, secondary pollution and the like of high-stability nondegradable organic pollutants in the treated water in the traditional water treatment method, and has good application prospect.
The traditional advanced oxidation technology is to generate hydroxyl radicals as main active species to degrade pollutants. Advanced oxidation technologies based on sulfate radicals are new technologies developed in recent years for the oxidative treatment of refractory organic pollutants. Persulfate ions have strong oxidizability, can generate sulfate radicals after activation, have strong oxidation characteristics, can oxidize and degrade refractory organic matters in the environment, and are more stable than hydroxyl radicals and have longer half-life. Although the persulfate has strong oxidizing capability, is relatively stable and is not easy to degrade, the persulfate is mainly activated by using transition metal ions at present, the method does not need high-temperature heating or ultraviolet irradiation, the persulfate is activated under the normal temperature condition, and the method is easy to realize under the laboratory condition or in the engineering implementation process. The transition metal ions usually used mainly comprise Fe2+、Cu2+、Mn2+、Ce2+Etc. of Fe2+Because of low price, high efficiency and no toxicity, the compound is the persulfate transition metal ion activator which is most widely applied, but Fe2+With SO4-Formation of competitive, excess Fe2+Consumes the redundant SO4-In addition, Fe2+Is easily oxidized into Fe3+Thereby limiting the oxidation efficiency of the process. To overcome this problem, multiphase Fe-containing compounds have been used instead of Fe2+To form a multiphase persulfate system, the multiphase catalysts developed to date, although effective in activating sulfate to produce highly active SO4-The organic pollutants are degraded, but the outstanding problems of large elution amount of transition metal ions, poor stability and the like generally exist. How to develop an efficient and stable heterogeneous catalyst is to apply SO4 ·-The key to advanced oxidation technology.
Based on the method, the supported ternary FeNiY-MO composite peroxymonosulfate activator is synthesized by taking activated alumina as a carrier and adopting a solvothermal-roasting method, the specific surface area and the surface high-density adsorption sites of the porous carrier are fully utilized, and the synergistic effect between the carrier and active components is utilized, so that the loading rate of FeNiY-MOF particles is effectively improved, and the dissolution of transition metal ions is effectively avoided. Meanwhile, a metal organic framework structure can be utilized to provide more PMS activation sites, and the degradation rate of organic pollutants in water is greatly improved. The process is simple and convenient to operate, good in catalyst stability and high in pollutant degradation efficiency, is easy to separate and recycle after treatment, can be recycled for multiple times, and has a wide application prospect.
Disclosure of Invention
The invention aims to provide a preparation method of a FeNiY-MOF composite peroxymonosulfate activator taking activated alumina as a matrix, aiming at the steel wastewater with high organic matter content, high COD concentration and the like which is difficult to reach the national emission standard by adopting the existing treatment technology.
Yet another object of the present invention is to: provides a FeNiY-MOF composite peroxymonosulfate activator product which is prepared by the method and takes activated alumina as a matrix.
Yet another object of the present invention is to: provides an application of the product.
The purpose of the invention is realized by the following scheme: a FeNiY-MOF composite peroxymonosulfate activator with active alumina as matrix is prepared from zeolite imidazolate as frame structure, active alumina balls as carrier, and CTABControlling, adopting solvothermal-roasting method to synthesize ternary composite catalyst Fe with metal organic frame structure2O3-NiO-Y2O3The method comprises the following steps:
(1) fe (NO) was added under magnetic stirring3)3·9H2O、Ni(NO3)2·6H2O、Y(NO3)3·6H2O and CTAB in molar amounts of 1: 1: 1: (10-100) placing the mixture in a beaker, and stirring the mixture until the solution is clear and transparent; weighing 14-27 g of 2-methylimidazole, dissolving in absolute ethyl alcohol, mixing the two solutions, stirring for 1h, adding activated small activated alumina balls into the mixed solution after stirring is stopped, placing in a hydrothermal reaction kettle, and controlling the reaction temperature and time;
(2) after the reaction is finished, performing suction filtration and washing, and then placing in a vacuum drying oven for drying to obtain a load type FeNiY-MOF precursor regulated and controlled by a CTAB template;
(3) and (3) placing the FeNiY-MOF precursor in the step (2) in a tube furnace, introducing a hydrogen-argon mixed gas, roasting for 2h, and finally placing the roasted product in a muffle furnace at a certain temperature, roasting for 2h to obtain the supported FeNiY-MOF composite peroxymonosulfate activator with the metal-organic framework structure.
The invention prepares the Fe with a load type hollow structure by using active alumina as a carrier, CTAB as a morphology regulator and ZIFs material as a sacrificial precursor through a solvent-roasting method2O3-NiO-Y2O3The MOF composite catalyst effectively improves the activation capability of PMS and accelerates SO4 DEG-Generation of and decomposition of contaminants.
On the basis of the scheme, in the step (1), the hydrothermal reaction temperature is 110-150 ℃, and the reaction time is 4-24 hours.
On the basis of the scheme, in the step (2), the vacuum drying temperature is 60-80 ℃, and the drying time is 3-12 hours.
On the basis of the scheme, in the step (3), the hydrogen content of the hydrogen-argon mixed gas is 5%, and the roasting temperature is 300-800 ℃.
The invention provides a FeNiY-MOF composite peroxymonosulfate activator taking activated alumina as a matrix, which is prepared according to the method.
The invention also provides the application of the FeNiY-MOF composite peroxymonosulfate activator taking the activated alumina as the matrix according to claim 5 in the removal of TOC in steel wastewater.
The degradation experiment of the FeNiY-MOF composite peroxymonosulfate activator is carried out in a beaker, 50g of supported FeNiY-MOF composite activator is added into 70mL of steel wastewater and is fully stirred, after organic pollutants in the steel wastewater reach adsorption-desorption balance on the surface of the supported FeNiY-MOF composite activator, 1mL of PMS solution with certain concentration is added and is fully stirred for 30min, a total organic carbon/total nitrogen analyzer is used for measuring the TOC concentration of the solution, and the TOC removal rate of the steel wastewater is calculated.
The invention relates to a preparation method of FeNiY-MOF composite peroxymonosulfate activator with active alumina as matrix and a product and application thereof2O3-NiO-Y2O3The MOF composite catalyst effectively promotes the activation of PMS and accelerates SO4 DEG by utilizing the interaction among the components-Generation of and decomposition of contaminants. In addition, the synergistic effect between the carrier and the active component promotes the improvement of the load rate of FeNiY-MOF particles, effectively avoids the dissolution of transition metal ions and improves the catalytic activation capability on PMS. The FeNiY-MOF composite peroxymonosulfate activator with active alumina as a matrix prepared by the method has the advantages of simple and controllable preparation process, good capability of catalyzing and activating PMS, capability of effectively solving the problems of difficult recovery of a suspended catalyst, secondary pollution to water quality, poor degradation effect and the like, greatly shortened reaction time, improved removal efficiency of organic pollutants and great application prospect.
The invention has the following advantages:
(1) the active alumina prepared by the invention is used as a matrixThe FeNiY-MOF composite peroxymonosulfate activator adopts a solvothermal-roasting method to synthesize the unique supported hollow nano-structure Fe2O3-NiO-Y2O3The MOF composite catalyst has good stability, high loading amount, high activity and good organic matter degradation removal effect, and effectively prevents the problem of secondary pollution caused by incomplete separation in the catalytic degradation process.
(2) The supported FeNiY-MOF composite peroxymonosulfate activator prepared by the invention utilizes the unique framework structure of the zeolite imidazole ester framework to provide more PMS activation sites for the composite activator and promote SO4-The specific surface area and the surface high-density adsorption sites of the porous carrier are fully utilized, and the synergistic effect between the carrier and the active component is utilized, so that the loading rate of FeNiY-MOF particles is effectively improved, the dissolution of transition metal ions is effectively avoided, the stability of the PMS activator is improved, and the recycling of the activator is facilitated.
(3) The preparation process of the supported peroxymonosulfate activator provided by the invention is simple and controllable, and effectively promotes SO4 ·-The organic pollutants are generated and decomposed, the catalytic degradation effect of the organic pollutants is excellent, and the method has great popularization and application values.
Detailed Description
The present invention is further illustrated by examples.
Example 1:
a FeNiY-MOF composite peroxymonosulfate activator with active alumina as matrix is prepared through synthesizing three-element composite catalyst Fe with metal-organic framework structure by using zeolite imidazole ester as framework structure, using active alumina balls as carrier, combining with CTAB shape regulation and control, and adopting solvothermal-roasting method2O3-NiO-Y2O3The preparation method comprises the following steps:
(1) under magnetic stirring, mixing the components according to a molar weight of 1: 1: 1: 10 will Fe (NO)3)3·9H2O、Ni(NO3)2·6H2O、Y(NO3)3·6H2Placing O and CTAB in a beaker, and stirring until the solution is clearA clear solution; weighing 14g of 2-methylimidazole, dissolving in absolute ethyl alcohol, mixing the two solutions, stirring for 1h, adding the activated small activated alumina balls into the mixed solution after the stirring is stopped, placing the mixture in a hydrothermal reaction kettle, and controlling the reaction temperature and the reaction time to be 150 ℃ and 8h respectively;
(2) after the reaction is finished, performing suction filtration and washing, and then placing in a vacuum drying oven at 60 ℃ for drying for 12h to obtain a load type FeNiY-MOF precursor regulated by a CTAB template;
(3) and (3) placing the FeNiY-MOF precursor in the step (2) in a tube furnace, and introducing a hydrogen-argon mixed gas into the tube furnace for roasting for 2 hours. And finally, placing the roasted product in a muffle furnace at 350 ℃ for roasting for 2h to obtain the supported FeNiY-MOF composite peroxymonosulfate activator with the metal organic framework structure. The degradation rate of the prepared composite peroxymonosulfate activator to TOC of the steel wastewater is 65.3%.
Example 2:
a FeNiY-MOF composite peroxymonosulfate activator taking activated alumina as a matrix is prepared by the following steps:
(1) under magnetic stirring, mixing the components according to a molar weight of 1: 1: 1: 100 Fe (NO)3)3·9H2O、Ni(NO3)2·6H2O、Y(NO3)3·6H2Placing O and CTAB in a beaker, and stirring until the solution is clear and transparent; weighing 27g of 2-methylimidazole, dissolving in absolute ethyl alcohol, mixing the two solutions, stirring for 1h, adding the activated small activated alumina balls into the mixed solution after the stirring is stopped, placing the mixture in a hydrothermal reaction kettle, and controlling the reaction temperature and the reaction time to be 150 ℃ and 12h respectively;
(2) after the reaction is finished, performing suction filtration and washing, and then placing in a vacuum drying oven at 60 ℃ for drying for 12h to obtain a load type FeNiY-MOF precursor regulated by a CTAB template;
(3) and (3) placing the FeNiY-MOF precursor in the step (2) in a tube furnace, and introducing a hydrogen-argon mixed gas into the tube furnace for roasting for 2 hours. And finally, placing the roasted product in a 400 ℃ muffle furnace for roasting for 2h to obtain the supported FeNiY-MOF composite peroxymonosulfate activator with the metal organic framework structure. The degradation rate of the prepared composite peroxymonosulfate activator to TOC of the steel wastewater is 78.1%.
Example 3:
a FeNiY-MOF composite peroxymonosulfate activator taking activated alumina as a matrix is prepared by the following steps:
(1) under magnetic stirring, mixing the components according to a molar ratio of 1: 1: 1: 10 will Fe (NO)3)3·9H2O、Ni(NO3)2·6H2O、Y(NO3)3·6H2O and CTAB were placed in a beaker and stirred until the solution was clear and transparent. Weighing 14g of 2-methylimidazole, dissolving in absolute ethyl alcohol, mixing the two solutions, stirring for 1h, adding the activated small activated alumina balls into the mixed solution after the stirring is stopped, placing the mixture in a hydrothermal reaction kettle, and controlling the reaction temperature and the reaction time to be 110 ℃ and 12h respectively;
(2) after the reaction is finished, performing suction filtration and washing, and then placing in a vacuum drying oven at 80 ℃ for drying for 3h to obtain a load-type FeNiY-MOF precursor regulated by a CTAB template;
(3) and (3) placing the FeNiY-MOF precursor in the step (2) in a tube furnace, and introducing a hydrogen-argon mixed gas into the tube furnace for roasting for 2 hours. And finally, placing the roasted product in a muffle furnace at 350 ℃ for roasting for 2h to obtain the supported FeNiY-MOF composite peroxymonosulfate activator with the metal organic framework structure. The degradation rate of the prepared composite peroxymonosulfate activator to TOC of the steel wastewater is 61.5%.
Example 4:
a FeNiY-MOF composite peroxymonosulfate activator taking activated alumina as a matrix is prepared by the following steps:
(1) under magnetic stirring, mixing the components according to a molar ratio of 1: 1: 1: 10 will Fe (NO)3)3·9H2O、Ni(NO3)2·6H2O、Y(NO3)3·6H2O and CTAB were placed in a beaker and stirred until the solution was clear and transparent. Weighing 14g of 2-methylimidazole, dissolving in absolute ethyl alcohol, mixing the two solutions, stirring for 1h, adding activated small activated alumina balls into the mixed solution after stirring is stopped, placing the mixture in a hydrothermal reaction kettle, and controlling the reaction temperature and the reaction timeRespectively at 150 ℃ and 4 h;
(2) after the reaction is finished, performing suction filtration and washing, and then placing in a vacuum drying oven at 80 ℃ for drying for 6h to obtain a load type FeNiY-MOF precursor regulated by a CTAB template;
(3) and (3) placing the FeNiY-MOF precursor in the step (2) in a tube furnace, and introducing a hydrogen-argon mixed gas into the tube furnace for roasting for 2 hours. And finally, placing the roasted product in a muffle furnace at 800 ℃ for roasting for 2h to obtain the supported FeNiY-MOF composite peroxymonosulfate activator with the metal organic framework structure. The degradation rate of the prepared composite peroxymonosulfate activator to TOC of the steel wastewater is 57.6%.
Claims (6)
1. A preparation method of FeNiY-MOF composite peroxymonosulfate activator with active alumina as a matrix is characterized in that a ternary composite catalyst Fe with a metal organic framework structure is synthesized by using a framework structure of zeolite imidazole ester, using active alumina spheres as a carrier, combining morphology regulation and control of CTAB (cetyltrimethyl ammonium bromide) and adopting a solvothermal-roasting method2O3-NiO-Y2O3The method comprises the following steps:
(1) fe (NO) was added under magnetic stirring3)3·9H2O、Ni(NO3)2·6H2O、Y(NO3)3·6H2O and CTAB in molar amounts of 1: 1: 1: (10-100) placing the mixture in a beaker, and stirring the mixture until the solution is clear and transparent; weighing 14-27 g of 2-methylimidazole, dissolving in absolute ethyl alcohol, mixing the two solutions, stirring for 1h, adding activated small activated alumina balls into the mixed solution after stirring is stopped, placing in a hydrothermal reaction kettle, and controlling the reaction temperature and time;
(2) after the reaction is finished, performing suction filtration and washing, and then placing in a vacuum drying oven for drying to obtain a load type FeNiY-MOF precursor regulated and controlled by a CTAB template;
(3) and (3) placing the FeNiY-MOF precursor in the step (2) in a tube furnace, introducing a hydrogen-argon mixed gas, roasting for 2h, and finally placing the roasted product in a muffle furnace at a certain temperature, roasting for 2h to obtain the supported FeNiY-MOF composite peroxymonosulfate activator with the metal-organic framework structure.
2. The preparation method of the FeNiY-MOF composite peroxymonosulfate activator taking activated alumina as the matrix according to claim 1, characterized in that in the step (1), the hydrothermal reaction temperature is 110-150 ℃, and the reaction time is 4-24 h.
3. The preparation method of the FeNiY-MOF composite peroxymonosulfate activator taking activated alumina as the matrix according to claim 1, characterized in that in the step (2), the vacuum drying temperature is 60-80 ℃, and the drying time is 3-12 h.
4. The preparation method of the FeNiY-MOF composite peroxymonosulfate activator taking activated alumina as the matrix according to claim 1, characterized in that in the step (3), the hydrogen content of the mixed gas of hydrogen and argon is 5%, and the roasting temperature is 300-800 ℃.
5. A FeNiY-MOF composite peroxymonosulfate activator based on activated alumina, characterized in that it is prepared according to any one of the methods of claims 1 to 4.
6. Use of the FeNiY-MOF composite peroxymonosulfate activator in the form of activated alumina according to claim 5 for TOC removal from steel wastewater.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114314795A (en) * | 2021-12-24 | 2022-04-12 | 王晶晶 | Method for degrading organic pollutants by activating persulfate through supported alumina particles |
| CN114620920A (en) * | 2022-03-15 | 2022-06-14 | 中国科学院生态环境研究中心 | Preparation method of magnetic material for conditioning sludge by activated persulfate |
| CN115356305A (en) * | 2022-07-08 | 2022-11-18 | 徐州工程学院 | Preparation method of novel aluminum-based MOF material and application of novel aluminum-based MOF material in tetracycline detection |
| CN115069254B (en) * | 2022-07-18 | 2024-01-26 | 洛阳师范学院 | High-activity nickel-based catalyst, preparation method thereof and application thereof in furfural hydrogenation |
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| CN114314795A (en) * | 2021-12-24 | 2022-04-12 | 王晶晶 | Method for degrading organic pollutants by activating persulfate through supported alumina particles |
| CN114314795B (en) * | 2021-12-24 | 2023-10-31 | 王晶晶 | Method for degrading organic pollutants by activating persulfate through supported alumina particles |
| CN114620920A (en) * | 2022-03-15 | 2022-06-14 | 中国科学院生态环境研究中心 | Preparation method of magnetic material for conditioning sludge by activated persulfate |
| CN115356305A (en) * | 2022-07-08 | 2022-11-18 | 徐州工程学院 | Preparation method of novel aluminum-based MOF material and application of novel aluminum-based MOF material in tetracycline detection |
| CN115356305B (en) * | 2022-07-08 | 2023-06-16 | 徐州工程学院 | Preparation method of aluminum-based MOF material and application of aluminum-based MOF material in tetracycline detection |
| CN115069254B (en) * | 2022-07-18 | 2024-01-26 | 洛阳师范学院 | High-activity nickel-based catalyst, preparation method thereof and application thereof in furfural hydrogenation |
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