CN113275014B - High-molecular surface modified gamma-Fe 2 O 3 Diatomite catalyst, preparation method and application thereof - Google Patents
High-molecular surface modified gamma-Fe 2 O 3 Diatomite catalyst, preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a high-molecular surface modified gamma-Fe 2O 3/diatomite catalyst and a preparation method and application thereof, wherein the preparation method takes a sol-gel roasting method as a basic process and takes ferric nitrate nonahydrate as Fe 3+ Ethylene glycol is used as a solvent. The high molecular surfactant is one or at least two of polyvinylpyrrolidone, carboxymethyl cellulose and cetyl trimethyl ammonium bromide. The preparation method has the advantages of simple process, strong operability, short preparation period, high yield and easy realization of industrial production. The catalyst prepared by the method realizes high-efficiency volatile organic compound degradation efficiency and O in cooperation with low-temperature plasma 3 High decomposition efficiency, high catalytic activity and high stability.
Description
Technical Field
The invention relates to a high-molecular surface modified gamma-Fe 2 O 3 A diatomite catalyst and a preparation method and application thereof belong to the technical field of magnetic diatomite preparation.
Technical Field
At present, china faces PM 2.5 And O 3 The dual pressure of pollution, volatile Organic Compounds (VOCs) are the major contributors to these two serious atmospheric pollution problemsFactors. Effective control of the emissions of VOCs is therefore a key to alleviating current atmospheric pollution problems. Compared with the traditional VOCs treatment technology, the low-temperature plasma technology has the advantages of short retention time, simple operation, small occupied area, wide selectivity, mild reaction conditions and the like when being applied to the VOCs treatment aspect, so that the low-temperature plasma technology has wide prospect in practical application. However, in terms of the present, the low temperature plasma technology still has the disadvantages of high energy consumption, incomplete degradation of pollutants, large influence of humidity and O 3 Secondary pollution problem.
Diatomaceous earth (SiO) 2 ·nH 2 O) is essentially a biogenic siliceous sedimentary rock formed by the death of ancient diatoms by long-term stacking and extrusion, the main component being SiO 2 . The diatomite is light in weight, stable in structure, high in porosity and large in specific surface area, and therefore the diatomite is widely applied to adsorption, such as fluoride removal, heavy metal removal and organic matter separation. Yu et al studied and prepared a load Fe 3 O 4 The SN-based modified composite diatomite adsorbent of the nano particles realizes excellent phenol adsorption and removal effects. Zurayk et al studied to prepare an organic modified natural diatomaceous earth adsorbent for Pb (II), cr (VI), and Cr (III) removal. The research result shows that the adsorption performance of the material is influenced by various factors including time, temperature, ionic strength and the like. Chen et al prepared an illite-doped Fe 3 O 4 The magnetic diatomite adsorbent has good phenol adsorption performance and strong magnetism, and can be quickly separated from a water body through strong magnetism after the adsorption process is finished.
The above working contents indicate that the diatomite is modified to improve the adsorption performance of the diatomite on organic matters and metal ions, but if the diatomite is used as a catalyst carrier, the problems of diatomite pore channel blockage, structural damage, poor catalytic activity improvement effect and the like caused by the massive agglomeration of metal oxides often occur in a metal oxide/diatomite catalyst prepared by a traditional impregnation method.
However, the diatomite has large reserve amount and low cost and the main component is SiO 2 Especially suitable for being used as a carrier of a low-temperature plasma catalyst,the diatomite-based catalyst with simple preparation process, low cost and highly dispersed active components is developed, the catalytic degradation efficiency of plasma is improved, and the tail gas O is reduced 3 The concentration has important significance for promoting the application of low-temperature plasma catalysis.
Disclosure of Invention
In view of the above problems, the present invention provides a polymer surface modified γ -Fe suitable for low temperature plasma 2 O 3 A diatomite catalyst and a preparation method thereof.
In one aspect, the invention provides a polymer surface modified gamma-Fe suitable for low temperature plasma 2 O 3 A diatomite catalyst. Another purpose of the invention is to provide a high molecular surface modified gamma-Fe suitable for low-temperature plasma 2 O 3 A preparation method of the diatomite catalyst.
The purpose of the invention can be realized by the following technical scheme:
high-molecular surface modified gamma-Fe suitable for low-temperature plasma 2 O 3 The preparation method of the diatomite catalyst comprises the following steps:
1) Dissolving a certain amount of ferric nitrate nonahydrate, a high molecular surfactant and diatomite in an ethylene glycol solution, carrying out ultrasonic treatment for 15-20 min, and then heating, stirring and refluxing at 75-85 ℃ for 9-12 h to generate sol A;
2) Drying the sol A in a vacuum drying oven at the temperature of 80-85 ℃ for 12-14 h to obtain dry gel;
3) And putting the crushed dry gel into a muffle furnace for calcining at the temperature of 280-400 ℃, after the calcining is finished, taking out a product after the muffle furnace is cooled to the temperature of 25-28 ℃, filtering and washing for a plurality of times after grinding, and then carrying out vacuum drying at the temperature of 55-60 ℃ for 12-14 h to obtain a target product.
Preferably, the diatomite in the step 1) is refined diatomite, the refining process is that ultrasonic treatment is carried out in 0.1M hydrochloric acid solution for 30min, then deionized water is used for washing to be neutral, then ultrasonic treatment is carried out in acetone solution for 30min, and then absolute ethyl alcohol and deionized water are used for washing for 3 times respectively, and then the obtained product is placed in a vacuum drying oven to be dried for 12h at the temperature of 60 ℃.
As a preferable example of the present invention, the polymeric surfactant in step 1) is one or at least two of PVP, CMC and CTAB.
As a preferable aspect of the present invention, the molar ratio of the ferric nitrate nonahydrate to the diatomaceous earth in the step 1) is 1 to 1.
As one preferable aspect of the present invention, the molar ratio of the iron nitrate nonahydrate to the ethylene glycol in the step 1) is 1.
As a preferable aspect of the present invention, the amount of the ferric nitrate nonahydrate and the polymeric surfactant used in step 1) is Fe 3+ And the molar ratio of the macromolecular surfactant = 1.
As a preferable mode of the invention, in the step 3), the muffle furnace calcination temperature is 300 ℃, the time is 120min, and the heating rate is 5 ℃/min.
As a preferable selection of the invention, the solution used in the filtration washing in the step 3) is deionized water and absolute ethyl alcohol, and the filtration washing times are 3-5.
The polymer surface modified gamma-Fe prepared by the method of the invention 2 O 3 A diatomite catalyst.
The general formula of the composition structure of the catalyst is alpha-gamma-Fe 2 O 3 -X b The X is one or at least two of polyvinylpyrrolidone (PVP), carboxymethyl cellulose (CMC), and Hexadecyl trimethyl ammonium bromide (CTAB), and the a is gamma-Fe 2 O 3 B is a polymer modified compound and Fe 3+ In a molar ratio of (a). Effectively avoids the agglomeration of active components after the modification of macromolecular compounds, namely gamma-Fe 2 O 3 The particles are uniformly dispersed on the surface of the diatomite shell to form the magnetic diatomite.
The high molecular surface modified gamma-Fe suitable for low-temperature plasma prepared by the method 2 O 3 The application of the diatomite catalyst and the low-temperature plasma in degrading volatile organic compounds and reducing the concentration of by-product ozone.
In a preferred embodiment of the present invention, the volatile organic compound is styrene or toluene.
Preferably, the concentration of the volatile organic compounds is 100-400mg/m 3 。
By adopting the technology, compared with the prior art, the invention has the following beneficial effects:
the invention is based on a sol-gel-roasting preparation process, and takes ferric nitrate nonahydrate as Fe 3+ The source is that different kinds of high molecular compounds with different weights are introduced in the sol-gel forming process to prepare the gamma-Fe with small particle size and uniform size 2 O 3 And highly dispersing active components on the surface of diatomite to improve gamma-Fe 2 O 3 The electron utilization rate of the diatomite catalyst in a plasma catalytic system improves the catalytic activity and stability of the catalyst, so that the catalyst is not easy to deposit carbon and deactivate; high dispersity gamma-Fe 2 O 3 The ozone decomposition efficiency is improved, and the problem of secondary ozone pollution in the plasma operation process is effectively avoided; and the catalyst is made magnetic, thereby increasing the recovery amount of the catalyst.
Drawings
FIG. 1% gamma-Fe 2 O 3 -PVP 2 SEM-EDS-mapping diagram of/Diatomite
a:10％-γ-Fe 2 O 3 -PVP 2 EDS-mapping plot of/diatemite; b, an element distribution diagram of Fe; c, an element distribution diagram of Si; elemental distribution diagram of d: O
FIG. 2% -gamma-Fe 2 O 3 -PVP 2 Styrene conversion and CO2 selectivity of the Diatomite catalyst at different oxygen contents (catalyst loading: 0.1g, styrene concentration 100 mg/m) 3 Flow 0.1L/min, temperature 25 ℃ C.)
a, toluene conversion rate; b is CO 2 Selectivity is
FIG. 3 GC-MS diagram of styrene degradation
FIG. 4 is a schematic diagram of a low-temperature plasma catalytic evaluation system
Detailed Description
The present invention is further illustrated with reference to specific examples, but the scope of protection of the invention is not limited thereto.
Example 1
4.04g of ferric nitrate nonahydrate, 2.22g of PVP and 6g of refined diatomite are dissolved in 9.4g of glycol solution, ultrasonic treatment is carried out for 20min, then heating stirring reflux is carried out for 10h at 80 ℃ to generate sol A, and then the sol A is placed in a vacuum drying oven to be dried for 12h at 80 ℃ to obtain dry gel. And (4) crushing the dried gel, placing the crushed dried gel in a muffle furnace, heating to 300 ℃ at a speed of 5 ℃/min, and calcining for 120min. And after the calcining and sintering are finished, taking out the product after the muffle furnace is cooled to room temperature, alternately washing the product for 4 times by using absolute ethyl alcohol and deionized water after grinding, and then carrying out vacuum drying for 12 hours at 60 ℃ to obtain the target product.
10% -gamma-Fe prepared by the method 2 O 3 -PVP 2 the/Diatomite catalyst is used for catalyzing and degrading styrene by low-temperature plasma, and the reaction conditions are as follows: the catalyst is filled in the medium barrier reactor, the filling amount of the catalyst is 0.1g, and the concentration of the styrene is 100mg/m 3 The flow rate is 0.1L/min, the temperature is 25 ℃, and the energy density is 1000J/L. The tail gas concentration is measured after the degradation reaction is stable for 1h, and the result is that the conversion rate of the styrene reaches 85.13 percent, and the CO content is measured 2 The selectivity reaches 77.23%, the ozone concentration of the tail gas is 22.14ppm, and compared with single low-temperature plasma (the concentration of generated ozone is 418 ppm), the ozone decomposition efficiency of 94.7% is realized.
Example 2
4.04g of iron nitrate nonahydrate, 3.33g of PVP and 3g of refined diatomite are dissolved in 9.4g of ethylene glycol solution, ultrasonic treatment is carried out for 20min, then heating, stirring and refluxing are carried out at 82 ℃ for 9.5h to generate sol A, and then the sol A is placed in a vacuum drying oven to be dried for 12h at 80 ℃ to obtain dry gel. The dried gel is crushed and then placed in a muffle furnace, the temperature is raised to 330 ℃ at the speed of 5 ℃/min, and the calcination is carried out for 110min. After calcining and sintering, taking out the product after the muffle furnace is cooled to room temperature, alternately washing the product for 4 times by using absolute ethyl alcohol and deionized water after grinding, and then carrying out vacuum drying for 12h at 60 ℃ to obtain the target product.
20% -gamma-Fe prepared by the above steps 2 O 3 -PVP 3 The/dialimite catalyst is used for catalyzing and degrading styrene by low-temperature plasma, and the reaction conditions are as follows: catalyst is filled inIn the medium barrier reactor, the loading of the catalyst is 0.1g, and the concentration of the styrene is 100mg/m 3 The flow rate is 0.1L/min, the temperature is 25 ℃, and the energy density is 877J/L. The concentration of tail gas is measured after the degradation reaction is stable for 1h, and the result shows that the conversion rate of styrene reaches 95.24 percent, and CO is 2 The selectivity reaches 85.19 percent, the ozone concentration of the tail gas is 11.35ppm, and compared with single low-temperature plasma (the concentration of generated ozone is 469 ppm), the ozone decomposition efficiency of 97.58 percent is realized.
Example 3
4.04g of ferric nitrate nonahydrate, 4.84g of CMC and 3g of refined diatomite are dissolved in 12.41g of glycol solution, ultrasonic treatment is carried out for 20min, then heating stirring reflux is carried out for 10h at 80 ℃ to generate sol A, and then the sol A is placed in a vacuum drying oven to be dried for 12h at 80 ℃ to obtain dry gel. And (4) crushing the dried gel, placing the crushed dried gel in a muffle furnace, heating to 300 ℃ at a speed of 5 ℃/min, and calcining for 120min. After calcining and sintering, taking out the product after the muffle furnace is cooled to room temperature, alternately washing the product for 4 times by using absolute ethyl alcohol and deionized water after grinding, and then carrying out vacuum drying for 12h at 60 ℃ to obtain the target product.
20% -gamma-Fe prepared by the above steps 2 O 3 -CMC 2 the/Diatomite catalyst is used for catalyzing and degrading styrene by low-temperature plasma, and the reaction conditions are as follows: the catalyst is filled in the medium barrier reactor, the filling amount of the catalyst is 0.1g, and the concentration of the styrene is 100mg/m 3 The flow rate is 0.1L/min, the temperature is 25 ℃, and the energy density is 562J/L. The tail gas concentration is measured after the degradation reaction is stable for 1h, and the result is that the conversion rate of the styrene reaches 90.17 percent, and the CO content is measured 2 The selectivity reaches 80.68 percent, and the ozone concentration of the tail gas is 15.35ppm.
Example 4
4.04g of ferric nitrate nonahydrate, 7.28g of CTAB and 2g of refined diatomite are dissolved in 15.51g of glycol solution, ultrasonic treatment is carried out for 20min, then heating stirring reflux is carried out at 80 ℃ for 10h to generate sol A, and then the sol A is placed in a vacuum drying oven to be dried for 12h at 80 ℃ to obtain dry gel. And (4) crushing the dried gel, placing the crushed dried gel in a muffle furnace, heating to 300 ℃ at a speed of 5 ℃/min, and calcining for 120min. After calcining and sintering, taking out the product after the muffle furnace is cooled to room temperature, alternately washing for 5 times by deionized water after grinding, and then carrying out vacuum drying for 12h at 60 ℃ to obtain the target product.
30% -gamma-Fe prepared by the above steps 2 O 3 -CTAB 2 the/Diatomite catalyst is used for catalyzing and degrading methylbenzene by using low-temperature plasma, and the reaction conditions are as follows: the catalyst is filled in a medium barrier reactor, the filling amount of the catalyst is 0.1g, and the concentration of the toluene is 100mg/m 3 The flow rate is 0.1L/min, the temperature is 25 ℃, and the energy density is 556J/L. The concentration of tail gas is measured after the degradation reaction is stable for 1h, and the result shows that the conversion rate of toluene reaches 92.36 percent, and CO 2 The selectivity reaches 81.32%, the ozone concentration of the tail gas is 13.18ppm, and compared with single low-temperature plasma (the concentration of generated ozone is 399 ppm), the ozone decomposition efficiency of 96.7% is realized.
Example 5
4.04g of ferric nitrate nonahydrate, 1.11g of PVP,3.64g of CTAB and 2g of refined diatomite are dissolved in 15.51g of glycol solution, ultrasonic treatment is carried out for 20min, then the solution is heated and stirred at 80 ℃ for 10h under reflux to generate sol A, and then the sol A is placed in a vacuum drying oven to be dried for 12h at 80 ℃ to obtain dry gel. And (4) crushing the dried gel, placing the crushed dried gel in a muffle furnace, heating to 300 ℃ at a speed of 5 ℃/min, and calcining for 120min. After calcining and sintering, taking out the product after the muffle furnace is cooled to room temperature, alternately washing for 5 times by deionized water after grinding, and then carrying out vacuum drying for 12h at 60 ℃ to obtain the target product.
30% -gamma-Fe prepared by the above steps 2 O 3 -PVP 1 -CTAB 1 the/Diatomite catalyst is used for catalyzing and degrading methylbenzene by using low-temperature plasma, and the reaction conditions are as follows: the catalyst is filled in a medium barrier reactor, the filling amount of the catalyst is 0.1g, and the concentration of the toluene is 100mg/m 3 The flow rate is 0.1L/min, the temperature is 25 ℃, and the energy density is 485J/L. The concentration of tail gas is measured after the degradation reaction is stable for 1h, and the result shows that the conversion rate of toluene reaches 97.84 percent, and CO 2 The selectivity reaches 87.92 percent, the ozone concentration of the tail gas is 4.76ppm, and compared with single low-temperature plasma (the concentration of the generated ozone is 352 ppm), the ozone decomposition efficiency of 98.65 percent is realized.
Example 6
The target pollutants in the simulated exhaust gas are configured through a micro-injection pump and a customized small-sized tube furnace. In the research process, the target pollutant is toluene or styrene, the temperature of the tubular furnace is controlled to be about 80 ℃, and the simulated preparation of the target pollutants with different concentrations is realized by adjusting the push rod speed of the micro-injection pump (in the actual test process, the push rod speed is corrected through respective standard curves of the toluene or the styrene to realize stable intake concentration).
10% -Gamma-Fe prepared in example 1 2 O 3 -PVP 2 the/Diatomite catalyst is used for catalyzing and degrading styrene by low-temperature plasma, and the influence of oxygen content change on the degradation effect is examined. The reaction conditions are as follows: the catalyst is filled in the medium barrier reactor, the filling amount of the catalyst is 0.1g, and the concentration of the styrene is 100mg/m 3 The flow rate is 0.1L/min, the temperature is 25 ℃, and the energy density is 1000J/L. Background gas in the simulated exhaust gas was formulated by high purity nitrogen and high purity oxygen at 78 (V/V). Specifically, the flow rates of high-purity oxygen and high-purity nitrogen are respectively regulated by a mass flow meter so as to realize the configuration of background gases with different oxygen contents (N) 2 、 5％O 2 +95％N 2 、10％O 2 +90％N 2 、20％O 2 +80％N 2 ，30％O 2 +70％N 2 V/V). And (5) measuring the concentration of the tail gas after the degradation reaction is stable for 1 h.
The results show that with O in the background atmosphere 2 Increased styrene conversion and CO content 2 The selectivity is increased therewith, at 20% 2 +80％N 2 At an energy density of 995J/L under a (V/V) atmosphere, the highest styrene conversion of 85.13% and CO were achieved 2 The selectivity was 77.23%. O is 2 The increase in the content contributes to the generation of.O and OH in the system, and these active radicals are more active than nitrogen radicals, thereby enabling higher degradation efficiency. However, when the oxygen concentration is too high and the oxygen-rich state is exhibited, the conversion of styrene and CO 2 But the selectivity is reduced. At 30% of 2 +70％N 2 At an energy density of 995J/L under a (V/V) atmosphere, the highest styrene conversion of 63.17% and CO were achieved 2 Selectivity 54.41%, and 20% 2 +80％N 2 Comparison of results in (V/V) atmosphere, styrene conversion and CO 2 The selectivity decreased by 25.8% and 29.86%, respectively. The reason for this may be thatAt an excessive O content 2 The molecules consume a large amount of high-energy electrons, and the electronegativity of the O atom is 3.44, which indicates that the O atom has higher capability of attracting electrons, so that the collision probability of pollutant molecules and the high-energy electrons is reduced, and the degradation efficiency of the styrene is reduced.
The description set out herein is merely illustrative of implementations of the inventive concept and the scope of the invention should not be construed as being limited to the specific forms set forth in the examples.
Claims (7)
1. High-molecular surface modified gamma-Fe suitable for low-temperature plasma 2 O 3 A diatomite catalyst is characterized by being prepared by the following steps:
1) Dissolving a certain amount of ferric nitrate nonahydrate, a high molecular surfactant and diatomite in an ethylene glycol solution, carrying out ultrasonic treatment for 15 to 20min, and then heating, stirring and refluxing at 75 to 85 ℃ for 9 to 12h to generate sol A; the polymer surfactant is one or two selected from PVP, CMC and CTAB; the dosage of the ferric nitrate nonahydrate and the high molecular surfactant is Fe 3+ The molar ratio of the high molecular surfactant is 1;
2) Putting the sol A into a vacuum drying oven, and drying for 12-14 h at the temperature of 80-85 ℃ to obtain dry gel;
3) And (3) calcining the crushed dry gel in a muffle furnace at the temperature of 280-400 ℃, after the calcination is finished, taking out the product after the muffle furnace is cooled to the temperature of 25-28 ℃, grinding, filtering, washing for several times, and performing vacuum drying at the temperature of 55-60 ℃ for 12-14 h to obtain the target product.
2. The polymer surface modified γ -Fe of claim 1 2 O 3 The diatomite catalyst is characterized in that the diatomite in the step 1) is refined diatomite, and the refining method comprises the steps of carrying out ultrasonic treatment in a 0.1M hydrochloric acid solution for 30min, washing the diatomite with deionized water to be neutral, carrying out ultrasonic treatment in an acetone solution for 30min, washing the diatomite with absolute ethyl alcohol and deionized water for 2 to 3 times respectively, and drying the diatomite in a vacuum drying oven at the temperature of 60 to 65 ℃ for 11 to 12 hours.
3. The boom of claim 2Molecular surface modified gamma-Fe 2 O 3 A diatomite catalyst, characterized in that the molar ratio of ferric nitrate nonahydrate to refined diatomite in 1) is 1 to 1.
4. The polymer surface modified γ -Fe of claim 1 2 O 3 A diatomite catalyst, characterized in that the molar ratio of ferric nitrate nonahydrate to ethylene glycol in step 1) is 1.
5. The polymer surface modified γ -Fe of claim 1 2 O 3 The diatomite catalyst is characterized in that in the step 3), the muffle furnace calcination temperature is 300 ℃, the time is 110-120 min, and the heating rate is 5 ℃/min.
6. The polymer surface modified γ -Fe of claim 1 2 O 3 The diatomite catalyst is characterized in that the solution used for filtering and washing in the step 3) is deionized water and absolute ethyl alcohol, and the filtering and washing times are 3 to 5.
7. Polymer surface modified γ -Fe of any one of claims 1 to 6 2 O 3 The diatomite catalyst can degrade volatile organic compounds in cooperation with low-temperature plasma and reduce the concentration of by-product ozone.
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