CN113941332A - Heterogeneous CoFe/Mg-LDO catalyst, preparation method and dimethylamine wastewater treatment method - Google Patents
Heterogeneous CoFe/Mg-LDO catalyst, preparation method and dimethylamine wastewater treatment method Download PDFInfo
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Abstract
The invention provides a preparation method of a heterogeneous CoFe/Mg-LDO catalyst, which comprises the following steps: firstly, synthesizing a CoFe/Mg-LDH precursor by adopting a coprecipitation method; and secondly, calcining the product obtained in the first step in a muffle furnace to obtain the heterogeneous CoFe/Mg-LDO catalyst. The catalyst prepared by the method can efficiently degrade dimethylamine in water, greatly reduce the leaching rate of toxic metals, improve the reusability of the catalyst, and show higher DMA removal rate (> 90%) in 80 minutes by adopting a CoFe/Mg-LDO catalyst and PMS oxidant system.
Description
Technical Field
The invention relates to the technical field of organic wastewater treatment, in particular to a heterogeneous CoFe/Mg-LDO catalyst applied to degradation of organic pollutant dimethylamine in water and a preparation method thereof.
Background
N, N-Dimethylformamide (DMF) is widely used as a solvent in the production process of Polyurethane (PU) synthetic leather, and is generally sent to a distillation process for recycling. However, it causes Dimethylamine (DMA) waste water to be produced at the top of the distillation column in an amount of up to several hundred or several thousand mg/l. Besides, DMA is present in wastewater from agricultural chemicals, pharmaceuticals and rubber industries, which have DMA as an important raw material. Because the boiling point of DMA is low (only 6.9 ℃ at normal temperature and normal pressure), dimethylamine in the wastewater has the problem of serious volatilization and re-release, the DMA-containing wastewater can generate pungent odor, and serious secondary pollution to air and water resources can be caused if the DMA-containing wastewater is not treated. The efficient and economical removal of DMA from wastewater is an important research topic.
At present, the method for processing Dimethylamine (DMA) at home and abroad mainly comprises the recovery and degradation. The medium and high concentration DMA waste water is suitable for adopting a recovery method, the medium and low concentration (less than or equal to 400mg/L) DMA waste water is suitable for adopting a degradation method, but the DMA has stable chemical property, is not easy to decompose and has biological toxicity.
The advanced oxidation technology leads DMA to be degraded thoroughly through the adsorption and oxidative decomposition, can be carried out at normal temperature and normal pressure, and has simple operation and lower secondary pollution. The oxidation method can change the structure of the organic matter, improve the biodegradability of the treated wastewater or directly oxidize and degrade the organic matter. Currently, among various oxidation methods, advanced oxidation methods are widely considered to have a promising prospect because they can generate a large amount of strongly oxidizing radicals, second only to fluorine, and can directly oxidize various organic compounds.
In recent years, based on sulfate radicals (SO)4 -Advanced oxidation technologies (AOPs) are considered to be a promising method for degrading refractory organic pollutants due to their strong oxidizing power and high efficiency. PMS (KHSO)5·0.5KHSO4·0.5K2SO4) Is a multifunctional, stable and environmentally friendly oxidant widely used for generating highly reactive SO4 -Free radical. In general, SO can be achieved by activating PMS by ultraviolet, thermal, ultrasonic or transition metal4 -Production of free radicals. Among various methods, heterogeneous transition metal catalysts are widely used due to their advantages of high efficiency, low energy consumption, easy separation, etc. In particular, Co and Fe based catalysts show high efficiency for PMS activation. However, the adverse effects of dissolving metal ions remain unresolved. The cobalt-based and iron-based catalysts may haveThe PMS is effectively activated, and the leaching potential to metal ions is low. Layered Double Hydroxide (LDH) is an anionic clay mineral comprising divalent and trivalent metal cations. Due to significant dispersibility, tunability of ionic composition, and unique structure, LDHs are considered acceptable precursors for the preparation of mixed metal oxides. Mixed oxides, also known as Layered Double Oxides (LDO), can be obtained by calcining LDHs. LDOs have a large number of active sites and well-dispersed metals that can act as heterogeneous catalysts in AOPs.
Based on the method, the CoFe/Mg-LDO catalyst which is low in cost and easy to operate is prepared, and the DMA is deeply oxidized under mild conditions (normal temperature, normal pressure and natural pH) to be thoroughly degraded into micromolecular inorganic substances. The method can directly treat the wastewater containing DMA at low concentration, and can also be used as a pretreatment procedure of a biological method and the like.
Disclosure of Invention
The invention aims to provide a heterogeneous CoFe/Mg-LDO catalyst which has the advantages of a stable layered structure, wherein the stable layered structure can fix active metals and reduce metal leaching, a Co-Fe bimetal heterogeneous catalyst loaded by the LDO can efficiently degrade dimethylamine in water, greatly reduce the leaching rate of toxic metals and improve the reusability of the catalyst, and a CoFe/Mg-LDO catalyst and PMS oxidant system is adopted to show higher DMA removal rate (> 90%) in 80 minutes.
In order to solve the technical problem, the invention provides a preparation method of a heterogeneous CoFe/Mg-LDO catalyst, which comprises the following steps:
firstly, synthesizing a CoFe/Mg-LDH precursor by adopting a coprecipitation method;
and secondly, calcining the product obtained in the first step in a muffle furnace to obtain the heterogeneous CoFe/Mg-LDO catalyst.
Wherein, in the first step, the ratio of Co: mg: the molar ratio of Fe is 1: 11: 4.
wherein the raw material used in the first step comprises Co (NO)3)2·6H2O, anhydrous Mg (SO)4)2And Fe (NO)3)3·9H2O。
Wherein the first step is to mix Co (NO)3)2·6H2O, anhydrous Mg (SO)4)2And Fe (NO)3)3·9H2O is continuously stirred evenly according to molar ratio under the condition of water bath and is added dropwise to Na2CO3Keeping pH constant in the solution, aging, centrifuging to obtain precipitate, washing the precipitate with deionized water, centrifuging, washing the precipitate with anhydrous ethanol, centrifuging again, and drying.
Wherein the calcining temperature in the second step is between 500 and 600 ℃, and the calcining time is between 3 and 7 hours.
The invention also provides a method for degrading organic wastewater by adopting the heterogeneous CoFe/Mg-LDO catalyst, which adopts the CoFe/Mg-LDO catalyst and PMS oxidant.
Wherein the mass ratio of the two is 0.3: 2.
the dimethylamine in the organic wastewater is treated.
The invention has the advantages of
The heterogeneous CoFe/Mg-LDO catalyst provided by the invention can efficiently degrade dimethylamine in a water body, greatly reduce the leaching rate of toxic metals, and improve the reusability of the catalyst, and a CoFe/Mg-LDO catalyst and PMS oxidant system is adopted, so that the catalyst shows higher DMA removal rate (> 90%) within 80 minutes.
Drawings
FIG. 1 (a-b): scanning Electron Microscope (SEM) images of CoFe/Mg-LDO; (c-d): high Resolution Transmission Electron Microscope (HRTEM) images of CoFe/Mg-LDO;
FIG. 2(a) X-ray diffraction pattern (XRD); (b) fourier transform infrared spectroscopy (FT-IR); (c) - (f) X-ray photoelectron spectroscopy (XPS);
FIG. 3 dimethylamine degradation analysis at different PMS dosages;
FIG. 4 dimethylamine degradation analysis with different catalysts.
Detailed Description
The invention provides a preparation method of a heterogeneous CoFe/Mg-LDO catalyst, which comprises the following steps:
firstly, synthesizing a CoFe/Mg-LDH precursor by adopting a coprecipitation method;
and secondly, calcining the product obtained in the first step in a muffle furnace to obtain the heterogeneous CoFe/Mg-LDO catalyst.
In the first step, the ratio of Co: mg: the molar ratio of Fe is preferably 1: 11: 4.
the raw material used in the first step includes Co (NO)3)2·6H2O, anhydrous Mg (SO)4)2And Fe (NO)3)3·9H2O。
The first further embodiment is Co (NO)3)2·6H2O, anhydrous Mg (SO)4)2And Fe (NO)3)3·9H2O is continuously stirred and evenly added into Na dropwise according to molar ratio under the condition of water bath2CO3Keeping pH constant in the solution, aging, centrifuging to obtain precipitate, washing the precipitate with deionized water, centrifuging, washing the precipitate with anhydrous ethanol, centrifuging again, and drying.
In the first step Na2CO3The concentration of the solution is preferably 0.05. mu. mol/L.
The pH is preferably 9 to 11, more preferably 10.
The aging time is preferably 8 to 24 hours, preferably 12 hours.
The number of washing with deionized water and anhydrous ethanol is preferably 1 to 5, and more preferably 2.
The drying time in the first step is preferably 8 to 24 hours, and more preferably 12 hours.
NaOH solution is used for adjusting the pH value.
The calcination temperature in the second step is between 500 ℃ and 600 ℃, preferably 500 ℃, and the calcination time is between 3h and 7h, preferably 5 h.
The heterogeneous catalyst CoFe/Mg-LDO provided by the invention is obtained by calcining layered double hydroxide (CoFe/Mg-LDH), and the reason for the high catalytic degradation performance of the catalyst on dimethylamine is that bimetallic Co and Fe are doped during the preparation of the catalyst, active Co is uniformly dispersed in the catalyst, and the Co and Fe in the catalyst generate a synergistic effect.
Layered Double Hydroxides (LDHs) are a typical 2d ion layered material with a host layer formed of metal hydroxides and interlayer regions composed of charge compensating exchange anions. Including divalent and trivalent metal cations, divalent metal cations (M)2+) May be Co2+、Fe2+、Ni2+、 Cu2+、Zn2+Or Mg2+. Trivalent metal cation (M)3+) May be Al3+，Fe3+，In3+， Mn3+Or Cr3+The anion may be CO3 2-，NO3 -，SO4 2-Or Cl-. The Layered Double Oxide (LDO) is obtained by calcining LD H in air, and not only has the advantages of LDH such as layered structure, but also has higher stability. The stable layered structure can fix the active metal and reduce Co2+Leaching.
The catalyst can activate PMS to generate active free radical (SO)4 -Free radical and OH free radical) to degrade DMA, transform DMA structure, and completely degrade into inorganic ions (NH)4 +，NO3 -And NO2 -Etc.), nitrogen is predominantly present as NH in the final product4 +The form exists.
The invention also provides a method for activating PMS to degrade DMA by adopting the heterogeneous CoFe/Mg-LDO catalyst, which adopts the CoFe/Mg-LDO catalyst and PMS oxidant in a mass ratio of 0.3: 2.
embodiments of the present invention will be described in detail below with reference to examples, so that how to apply technical means to solve technical problems and achieve technical effects can be fully understood and implemented.
Co(NO3)2·6H2O and Fe (NO)3)3·9H2O from Mecanna Mediterranean, Anhydrous Mg (SO)4)2Anhydrous Na available from chemical reagents GmbH of Miou, Tianjin2CO3From Fuchen chemical reagents GmbH, NaOH and absolute ethanol from Tianjin CityFuke technology development Co., Ltd.
EXAMPLE 1 heterogeneous CoFe/Mg-LDO catalyst
Will contain 0.00625mol Co (NO)3)2·6H2O, 0.06875mol of anhydrous Mg (SO)4)2And 0.025mol Fe (NO)3)3·9H2O100 mL mixed metal salt solution is continuously stirred and evenly added to 0.05mol/L Na in water bath at the temperature of 30 DEG C2CO3In solution (100 mL). During the synthesis, the pH was kept constant at 10 by adding 4mol/L NaOH solution. After aging for 12 hours, the precipitate was centrifuged, washed with deionized water 2 times and centrifuged, and then washed with absolute ethanol 2 times and centrifuged. Finally, CoFe/Mg-LDH was obtained by drying at 60 ℃ for 12 hours. After calcining the mixture for 5 hours at 500 ℃ in a muffle furnace, the CoFe/Mg-LDO is obtained.
Scanning Electron Microscopy (SEM), High Resolution Transmission Electron Microscopy (HRTEM) characterization of the CoFe/Mg-LDO is shown in FIG. 1. In FIG. 1a, CoFe/Mg-LDO exhibits a "flower-like" morphology, which is a typical characteristic of LDO morphology. FIG. 1b shows the "petal" structure of CoFe/Mg-LDO. The petals have a diameter of about 500 nanometers. In FIG. 1d, the lattice distance of the Mg species in the CoFe/Mg-LDO is 0.21nm, which is attributed to the (200) crystal plane of MgO (JCPDS PDF # 45-0946). The lattice distances of 0.209nm and 0.24nm are attributed to the (400) plane of MgFe2O4 (JCPDS PDF #36-0398) and Co3O4(311) (JCPDS PDF # 42-1467). This indicates well dispersed Co3O4Successfully loaded on CoFe/Mg-LDO, the effective contact area of Co3O4 is increased, and a plurality of effective Co active sites are generated. In addition, this successful loading facilitates contact of the CoFe/Mg-LDO with PMS, thereby increasing the efficiency of the active site and reducing Co usage. EDS analysis was used for further chemical analysis of CoFe/Mg-LDO nanoparticles, as shown in Table 1. The metal composition is in good agreement with the predetermined molar ratio (nCo: nFe). Furthermore, EDS analysis of CoFe/Mg-LDO after reaction (Table 2) did not occur
TABLE 1 EDS of CoFe/Mg-LDO with different Co/Fe molar ratios
TABLE 2 EDS of CoFe/Mg-LDO before and after use
FIG. 2a shows XRD spectra of fresh and used CoFe/Mg-LDO. Characteristic peaks of CoFe/Mg-LDO are clearly observed at 2 θ ═ 36.94 °, 42.92 °, 62.30 °, 74.69 ° and 78.63 °, which can be classified as MgO (111), (200), (220), (311) and (222) planes (JCPDS PDF # 45-0946). In addition, diffraction peaks at 35.47 °, 43.12 °, 62.59 °, 75.06 °, and 79.01 ° were attributed to MgFe2O4The (311), (400), (440), (622) and (444) crystal planes (JCPDS PDF # 36-0398). However, no separate peak of cobalt was observed in the mixed metal oxide due to the small amount of added cobalt. FIG. 2b shows Fourier transform infrared spectroscopy (FT-IR) of Co/Mg-LDO, Fe/Mg-LDO, CoFe/Mg-LDO and CoFe/Mg-LDO used, corresponding functional groups having been indicated in the figure. FIG. 2C is a full spectrum analysis of X-ray photoelectron spectroscopy (XPS) characterization, showing the presence of C1s, O1s, Fe 2p, Co 2p, Mg 1s spectra. FIG. 2d shows a spacing between Co 2p3/2 and 2p l/2 of 15.7eV, which can be attributed to spin-orbit splitting. The Co 2p3/2 peak can be fit to two subbands, 780.18-780.2 and 782.1-782.32 eV. The chemical state of the Co species is Co2+And Co3+. For used CoFe/Mg-LDO, the characteristic peak position was slightly shifted to lower binding energy, indicating the occurrence of oxidation and Co2 +–Co3+–Co2+Participation of the redox cycle. No significant change was observed in the spectra of the used CoFe/Mg-LDO, indicating the stability of the active cobalt species. As can be seen from fig. 2e, the Fe 2p spectrum was fitted to six peaks. In the case of the Fe 2p3/2 spectrum, three peaks near 709.6eV, 711.1eV, and 712.96eV can be assigned to the octahedral Fe2+, Fe3+And tetrahedral Fe3+. In FIG. 2f, high resolution of CoMgFe-LDO before and after reactionThe ratio O1s spectrum was fitted to two peaks with binding energies of 529.58eV and 531.54eV, respectively, corresponding to lattice Oxygen (OA) and adsorbed oxygen or surface hydroxyl species (OB), respectively.
Dimethylamine (DMA) degradation experiments
In a 400mL beaker at room temperature. In each experiment, 100mL of 100mg/L dimethylamine solution was previously poured into a beaker. 0.3g of catalyst CoFe/Mg-LDO and a certain amount of PMS (KHSO)5·0.5KHSO4·0.5K2SO4) Added simultaneously to the reactor and mixed under continuous magnetic stirring (300 rpm). At the indicated time intervals, 1mL of sample was drawn off by syringe and immediately filtered through a 0.45 μm PTFE syringe filter tip into a 50mL cuvette. The concentration of dimethylamine in water is determined by spectrophotometry using sodium hypochlorite-potassium iodide as a color developing agent.
The experimental conditions are as follows: [ DMA ]]0＝100mg/L，V＝100mL，CoFe/Mg-LDO＝0.3 g，T＝25℃。
The amounts of PMS were 0g, 0.5g, 1g, 1.5g, 2g, 2.5g, 3g, 3.5g, 4g, respectively, and the results are shown in FIG. 3.
The results in FIG. 3 show that CoFe/Mg-LDO/PMS shows higher DMA removal rate in 80 minutes, with PMS dosage of 2g being optimal (removal rate > 90%).
Different LDO catalysts are used for DMA degradation, a catalytic oxidation system is constructed by CoFe/Mg-LDO, Co/Mg-LDO, Fe/Mg-LDO, CoAl/Mg-LDO and PMS, and the catalytic activity of the heterogeneous catalyst is evaluated by adopting the self-adsorption of the CoFe/Mg-LDO catalyst and the self-oxidation of the PMS. The boiling point of DMA is low, only 6 and 7 degrees, and strong ammonia smell is volatilized after the cover is opened.
Reaction conditions are as follows: [ DMA ]]0＝100mg/L，V＝100mL，CoFe/Mg-LDO＝0.3 g，PMS＝2g，T＝25℃。
Figure 4 shows the effect of DMA degradation under different catalyst conditions, with the volatilization of the DMA solution alone resulting in a decrease in DMA concentration. When PMS is added alone, it dissolves in the aqueous solution and produces a small amount of S2O8 2-Organic contaminants can be degraded, but S2O8 2-Is relatively weak in oxidizing power. When added separatelyWith the addition of CoFe/Mg-LDO, DMA removal may be due primarily to adsorption. The experimental data show that the activity of PMS alone and CoFe/Mg-LDO alone can be neglected. Obviously, in the catalyst obtained in the above, after PMS is added, CoFe/Mg-LDO has the highest catalytic activity and can degrade DMA (A), (B), (C), (D) and D in 80 minutes>90%). These results indicate that CoFe/Mg-LDO is an effective activator for PMS to degrade DMA, and the superior catalytic activity is attributed to the synergistic effect of Co and Fe active sites.
All of the above mentioned intellectual property rights are not intended to be restrictive to other forms of implementing the new and/or new products. Those skilled in the art will take advantage of this important information, and the foregoing will be modified to achieve similar performance. However, all modifications or alterations are based on the new products of the invention and belong to the reserved rights.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention. However, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention still belong to the protection scope of the technical solution of the present invention.
Claims (9)
1. A preparation method of a heterogeneous CoFe/Mg-LDO catalyst is characterized by comprising the following steps:
firstly, synthesizing a CoFe/Mg-LDH precursor by adopting a coprecipitation method;
and secondly, calcining the product obtained in the first step in a muffle furnace to obtain the heterogeneous CoFe/Mg-LDO catalyst.
2. The method of preparing a heterogeneous CoFe/Mg-LDO catalyst according to claim 1, wherein: in the first step, the ratio of Co: mg: the molar ratio of Fe is 1: 11: 4.
3. the method of claim 1 or 2, wherein the catalyst is selected from the group consisting of heterogeneous CoFe/Mg-LDO catalystsThe method is characterized in that: the raw material used in the first step includes Co (NO)3)2·6H2O, anhydrous Mg (SO)4)2And Fe (NO)3)3·9H2O。
4. The method of preparing a heterogeneous CoFe/Mg-LDO catalyst according to claim 1 or 2, wherein: the first further embodiment is Co (NO)3)2·6H2O, anhydrous Mg (SO)4)2And Fe (NO)3)3·9H2O is continuously stirred and evenly added into Na dropwise according to molar ratio under the condition of water bath2CO3Keeping pH constant in the solution, aging, centrifuging to obtain precipitate, washing the precipitate with deionized water, centrifuging, washing the precipitate with anhydrous ethanol, centrifuging again, and drying.
5. The method of preparing a heterogeneous CoFe/Mg-LDO catalyst according to claim 1 or 2, wherein: the calcination temperature in the second step is between 500 and 600 ℃, and the calcination time is between 3 and 7 hours.
6. A heterogeneous CoFe/Mg-LDO catalyst prepared by the process of any of claims 1 to 5.
7. A method for degrading organic wastewater by using the heterogeneous CoFe/Mg-LDO catalyst according to claim 6, wherein the method comprises the following steps: CoFe/Mg-LDO catalyst and PMS oxidant are adopted.
8. The method of claim 6 wherein the heterogeneous CoFe/Mg-LDO catalyst is used for degrading organic wastewater, wherein: the mass ratio of the CoFe/Mg-LDO catalyst to the PMS oxidant is 0.3: 2.
9. the method for degrading organic wastewater by using the heterogeneous CoFe/Mg-LDO catalyst according to claim 6 or 7, wherein the organic wastewater is treated by the following steps: the dimethylamine in the organic wastewater is treated.
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