CN111229180B - Adsorbent for storing nitrogen oxides and preparation method and application thereof - Google Patents
Adsorbent for storing nitrogen oxides and preparation method and application thereof Download PDFInfo
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- CN111229180B CN111229180B CN202010152110.5A CN202010152110A CN111229180B CN 111229180 B CN111229180 B CN 111229180B CN 202010152110 A CN202010152110 A CN 202010152110A CN 111229180 B CN111229180 B CN 111229180B
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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Abstract
The invention discloses a method for nitrogen oxidationAn adsorbent for storing substance is prepared from Polydivinylbenzene (PDVB) as carrier and TiO carried on said polydivinylbenzene2. According to the invention, organic polydivinylbenzene and non-noble metal oxide are compounded to be used as the adsorbent, the preparation method is simple, no noble metal is contained, and the cost is greatly reduced. The adsorbing agent has large nitrogen oxide adsorbing amount, and the adsorbing amount is 538.38 mu mol g‑1Is obviously superior to other metal oxide adsorbents.
Description
Technical Field
The invention relates to an adsorbent for storing nitrogen oxides, a preparation method and application thereof, in particular to an adsorbent for removing nitrogen oxides in flue gas of an industrial boiler/furnace at normal temperature, and a preparation method and application thereof.
Background
NOx(NO and NO)2Etc.) as one of the pollutants harmful to the atmosphere, which is a significant cause of acid rain and photochemical smog, and even causes respiratory diseases in humans, the control method thereof has been receiving attention. The general station of Chinese environmental monitoring explicitly indicates in the environmental annual report issued in 2017 that the emission of nitrogen oxides in industrial sources is the first place in 2011-2015 years. China is the biggest world iron and steel producing country, and the iron and steel sintering flue gas NOxEmission reduction of NOxThe total discharge capacity is 10 percent, therefore, effective measures are taken to reduce NOxEmissions are a subject of concern in the current field of environmental protection.
Control of NOxThe main methods of (3) include SCR, SNCR and adsorption methods. The adsorption process can be used for NO at lower temperatures than other catalytic reactions that need to be carried out at higher temperaturesxPerforming separation and enrichment to obtain NOxThe purpose of the removal is. The adsorbent having a high adsorption capacity being for adsorbing NOxIs the key point of (1). Common adsorbents include activated carbon, zeolites, and other alkali metal compounds, among others. The organic polymer has the advantages of high strength, high toughness and the like, and is an excellent carrier for preparing the composite material. NO carried by organic polymerxAdsorbents have not been reported.
CN 108579368A discloses a method for purifying nitrogen oxides by solid-phase chemical absorption technology, in which nitrogen oxide waste gas to be treated is passed through a catalytic oxidation solid catalyst and a chemical absorption solid reagent in sequence to obtain purified waste gas. The solid adsorbent is a mixture of an inorganic solid absorbent and an organic polymer resin solid absorbent, the inorganic solid absorbent is sodium hydroxide, sodium carbonate, sodium bicarbonate, calcium carbonate, calcium hydroxide, potassium carbonate or potassium hydroxide, and the organic polymer resin solid absorbent can be a divinylbenzene polymer. The nitrogen oxide is removed by combining catalysis and absorption, the adsorbent is mainly used for removing a small amount of residual nitrogen oxide in catalytic oxidation in an auxiliary manner, the adsorbent is mainly removed by a chemical reaction with an alkaline substance after being adsorbed by a divinylbenzene polymer, and the adsorption capacity of the pure divinylbenzene polymer is limited.
Disclosure of Invention
The invention aims to provide an adsorbent for nitrogen oxide storage, which is prepared by mixing TiO with a carrier2The catalyst is loaded on polydivinylbenzene, so that the adsorption capacity of nitrogen oxides is remarkably improved.
The adsorbent for storing nitrogen oxides takes Polydivinylbenzene (PDVB) as a carrier, and TiO is loaded on the polydivinylbenzene2. In the invention, TiO is mixed with2The catalyst is loaded on an organic polydivinylbenzene carrier, does not use noble metal, and is economical and efficient. And from the experimental results, the supported TiO2The adsorption capacity of the polydivinylbenzene to the nitrogen oxide is obviously improved.
Further, among the above adsorbents, TiO2The smaller the particle diameter of (A) is, the better the effect is, and preferably, TiO2Is nano TiO2。
Further, in the above adsorbent, 0.04 to 0.2g of TiO is supported on polydivinylbenzene formed by polymerizing one ml of a divinylbenzene monomer2。
The invention also provides a preparation method of the adsorbent for storing the nitrogen oxides, which comprises the following steps:
(1) adding TiO into the mixture2Adding the mixture into an organic solvent, adding an initiator, uniformly mixing by ultrasonic, adding a divinylbenzene monomer, and carrying out polymerization reaction under ultrasonic;
(2) and after the polymerization reaction, filtering, washing and drying the obtained solid to obtain the adsorbent for storing the nitrogen oxide.
Further, in the above-mentioned production method, the polymerization of the monomer is carried out by a cationic polymerization method, and TiO is polymerized simultaneously with the polymerization2Carrying out a supporting, TiO2The dispersion is more uniform on the polymer. The initiator used for the polymerization is boron trifluoride ethyl ether, and the volume of the initiator is 8-15% of the volume of the divinylbenzene monomer.
Further, in the above preparation method, the organic solvent is n-hexane, the organic solvent provides an environment for the reaction, and the amount thereof can be adjusted as required. In certain embodiments of the invention, the volume ratio of organic solvent to divinylbenzene monomer is from 30 to 50: 1.
Further, in the preparation method, the polymerization reaction temperature is 20-30 ℃, the reaction time is 20-30min, and after the reaction time is up, the reaction is stopped by using absolute ethyl alcohol.
Further, in the above preparation method, the divinylbenzene monomer is reacted with basic Al2O3The leaching column filters out the polymerization inhibitor and then adds the polymerization inhibitor into the system to ensure the normal operation of polymerization.
Further, TiO used in the present invention2Can be purchased directly from the market or prepared by the user. In one embodiment of the present invention, the TiO is2The following treatments were carried out and then used: taking P25 type TiO2Calcining at 450-500 deg.c for 3-4 hr and grinding into powder.
The adsorbent for storing the nitrogen oxides has high nitrogen oxide adsorption capacity at the adsorption temperature of 30-35 ℃ proved by experiments, and can be used for adsorbing and purifying the nitrogen oxides in various flue gases. Aiming at the excellent adsorption performance of the adsorbent, the invention also provides a method for removing nitrogen oxides in flue gas of an industrial boiler or a furnace, which comprises the following steps: the adsorbent for storing the nitrogen oxides absorbs the nitrogen oxides in the flue gas, so that the nitrogen oxides in the flue gas are removed. The adsorbent of the invention has low use temperature, and can realize the removal of nitrogen oxides within the low temperature range of 30-35 ℃.
The adsorbent for storing nitrogen oxide of the invention takes organic polydivinylbenzene as a carrier, and TiO is loaded on the carrier2. Through the synergistic cooperation of the components, high adsorption capacity of nitrogen oxides is realized. Compared with the prior art, the invention has the following advantages:
1. according to the invention, organic polydivinylbenzene and non-noble metal oxide are compounded to be used as the adsorbent, the adsorbent has large nitrogen oxide adsorption capacity, the preparation method is simple, and no noble metal is contained, so that the cost is greatly reduced;
2. the adsorbent of the invention has the advantages of adsorption temperature of 30 ℃, gas inlet flow rate of 200mL/min, NO 500ppm and O2The adsorption amount of nitrogen oxide is up to 538.38 mu mol g under the condition of 5 percent of smoke gas-1Left and right.
3. The adsorbent of the invention has higher sulfur resistance and better water resistance. At the adsorption temperature of 30 ℃, the gas inlet flow rate of 200mL/min, NO 500ppm and SO2 300ppm、O2The adsorption quantity of nitrogen oxide is 459.15 mu mol g under the condition of 5 percent of flue gas-1On the left and right sides, the high adsorption activity can be still maintained after multiple cycles; introduction of H2After O, the amount of nitrogen oxides adsorbed was maintained at 338.22. mu. mol g-1On the other hand, the adsorption activity is higher than that of most single metal oxides.
Drawings
FIG. 1 is a bar graph of the adsorption amounts of different adsorbents.
FIG. 2 is a graph of the breakthrough of nitrogen oxides at an adsorption temperature of 30 ℃ for the adsorbent of example 2.
Detailed Description
The present invention is further illustrated by the following specific examples, which are intended to be purely exemplary and are not intended to be limiting.
In the following examples, unless otherwise specified, the experimental methods used were all conventional methods, and the materials, reagents and the like used were commercially available.
Example 1
Metal oxide CeO2Preparation of
Weighing 1.202g Ce (NO)3)3·6H2O in 50mL of deionized water, with stirring well to obtain (NH4)2CO3Dropwise adding the solution serving as a precipitator into a cerium nitrate solution, and adjusting the pH to 9 to obtain a suspension; magnetically stirring the suspension for 2h, precipitating, aging for 1h, centrifuging, washing to neutrality, drying at 110 deg.C for 12h, calcining at 500 deg.C in muffle furnace for 4h, and grinding for 30min to obtain CeO2。
Metal oxide ZrO2Preparation of
Weighing 1.198g Zr (NO)3)4·5H2O in 50mL of deionized water, with stirring well to obtain (NH4)2CO3Dropwise adding the solution serving as a precipitator into a zirconium nitrate solution, and adjusting the pH to 4 to obtain a suspension; magnetically stirring the suspension for 2h, precipitating and aging for 1h, centrifuging, washing to neutrality, drying at 110 deg.C for 12h, calcining at 500 deg.C in muffle furnace for 4h, and grinding for 30min to obtain ZrO2。
Metal oxide Sm2O3Preparation of
Weighing 1.2g Sm (NO)3)3·6H2O in 50mL deionized water, stirred well, with C2H2O4·2H2Dropwise adding the O solution which is used as a precipitator into the samarium nitrate solution drop by drop, and adjusting the pH to 5 to obtain a suspension; magnetically stirring the suspension for 2h, precipitating and aging for 1h, centrifuging, washing to neutrality, drying at 110 deg.C for 12h, calcining at 500 deg.C in muffle furnace for 4h, and grinding for 30min to obtain Sm2O3。
Metal oxide TiO2Of (2) a
Weighing 1.2g of the existing P25 type titanium dioxide in a laboratory, putting the titanium dioxide in a muffle furnace for calcining at 450 ℃ for 4h, and grinding for 30min to obtain metal oxide TiO2。
Example 2
A round bottom flask was charged with 0.101g of TiO treated as in example 12Then adding 80mL of normal hexane as a solvent, and ultrasonically stirring for 5min to uniformly mix the two; adding 240 mu L of boron trifluoride diethyl etherate as an initiator into the round-bottom flask, and ultrasonically stirring for 3 min; then add into2.4mL of filtered divinylbenzene, ultrasonically stirring at room temperature for 20min, finally adding about 5mL of absolute ethyl alcohol to stop reaction, filtering the obtained solid, washing for 3 times by using the absolute ethyl alcohol, and drying to obtain an adsorbent, which is marked as 0.1TiO2PDVB, 0.1 stands for supported TiO2The number of grams of (c). The specific surface area of the obtained adsorbent is 35.5m through the test of a nitrogen adsorption-desorption experiment2/g。
Example 3
A metal oxide supported PDVB was prepared as in example 2, except that: TiO 22The mass of (3) was 0.24 g. The resulting adsorbent was recorded as 0.24TiO2PDVB, 0.24 for supported TiO2The number of grams of (c).
Example 4
A metal oxide supported PDVB was prepared as in example 2, except that: TiO 22The mass of (2) was 0.48 g. The resulting adsorbent was recorded as 0.48TiO2PDVB, 0.48 for supported TiO2The number of grams of (c).
Comparative example 1
Preparation of 0.1CeO2PDVB adsorbent: 0.102g of ground CeO was added to a round bottom flask2Then adding 80mL of n-hexane organic reagent as a solvent, and ultrasonically stirring for 5min so as to uniformly mix the two; adding 240 mu L of boron trifluoride diethyl etherate as an initiator into the round-bottom flask, and ultrasonically stirring for 3 min; then adding 2.4mL of filtered divinylbenzene, ultrasonically stirring for 20min, finally adding about 5mL of absolute ethyl alcohol to stop reaction, filtering the obtained solid, washing the solid for 3 times by using the absolute ethyl alcohol, and drying to obtain 0.1CeO2/PDVB。
Comparative example 2
Preparation of 0.1ZrO2PDVB adsorbent: a round-bottomed flask was charged with 0.1g of ground ZrO2Then adding 80mL of n-hexane organic reagent as a solvent, and ultrasonically stirring for 5min so as to uniformly mix the two; adding 240 mu L of boron trifluoride diethyl etherate as an initiator into the round-bottom flask, and ultrasonically stirring for 3 min; then adding 2.4mL of filtered divinylbenzene, ultrasonically stirring for 20min, finally adding about 5mL of absolute ethyl alcohol to stop reaction, filtering the obtained solid, washing for 3 times by using the absolute ethyl alcohol, and drying to obtain 0.1ZrO2/PDVB。
Comparative example 3
Preparation of 0.1Sm2O3PDVB adsorbent, method same as comparative example 2, except that the zirconium oxide is replaced by Sm2O3。
Comparative example 4
Preparing a PtBa/Al adsorbent: first, 0.043g of platinum diammine dinitrate and 0.4362g of Ba (NO)3)2Dissolved in 30mL of deionized water, sufficiently stirred to dissolve, and then 1.7g of Al was added to the mixture2O3Stirring is continued to make Al2O3Mixing with the solution; then, setting the stirring temperature to 80 ℃, stirring to be viscous, stopping stirring, and drying at 110 ℃ overnight; and (3) fully grinding the dried adsorbent, then putting the ground adsorbent into a muffle furnace, calcining for 4h at 700 ℃, tabletting and sieving the calcined adsorbent to obtain the PtBa/Al adsorbent.
Application example 1
The samples prepared in the above examples and comparative examples are used as adsorbents to treat nitrogen oxides in simulated flue gas, and the adsorption effect of each adsorbent is examined:
1. experimental samples: the adsorbents of examples 2-4, comparative examples 1-4, and PDVB alone without loading.
2、NOxAdsorption experiment: with NO 500ppm, O25％、N2The simulated gas as balance gas is flue gas, and 0.1g of each adsorbent is used for adsorbing NO to be discharged at 30 ℃ according to the inlet flow of 200mL/minxSaturation of adsorption is achieved when the concentration is constant. With N2Purging adsorbent, heating for desorption, and plotting desorption temperature and NOxConcentration curve, calculating NO according to the following formulaxAdsorption amount of (1), in the formula, QadsRepresents NOxTotal amount of adsorption (. mu. mol g)-1)；AdesIs NO + O2-integrated area of the desorption peak of the TPD curve (ppm ℃ C.); qcIs the total flow rate (Lmin) of the purge gas-1)；RTIs the program temperature rate (. degree.C.min.)-1)，mcatIs the mass (g) of the adsorbent.
3. The experimental results are as follows: the adsorption amounts of NOx by the respective adsorbents are shown in table 1 below, and the adsorption amounts of the adsorbents of example 2 and comparative examples 1 to 4 are shown in fig. 1:
TABLE 1
As can be seen from the results, the adsorbents of examples 2 to 4 exhibited a remarkable adsorption effect in terms of the amount of adsorbed nitrogen oxides, which was significantly higher than those of comparative examples 1 to 4 and PDVB alone.
4. And (3) water interference resistance experiment: adsorption temperature of 100 ℃, inlet gas flow of 200mL/min, NO 500ppm, O25%, water vapor 5%, N20.1g of the adsorbent of example 2 was taken under the fume conditions as a balance gas and tested for its resistance to water interference. As shown in FIG. 1, NOxThe adsorption amount of (2) was 338.22. mu. mol g-1。
5. Sulfur interference resistance test: at an adsorption temperature of 30 ℃ and an inlet gas flow rate of 200mL/min, NO of 500ppm and O25％、SO2300ppm、N2The sorbent of example 2 was tested for sulfur interference resistance under flue gas conditions with a balance gas of 0.1 g. As shown in FIG. 1, NOxThe adsorption amount of (2) was 459.15. mu. mol g-1。
6. FIG. 2 shows NO at the outlet of the adsorbent of example 2 in the adsorption processxThe breakthrough curve of the concentration of (2) over time, it can be seen from the figure that it takes about 440s for the adsorbent to reach adsorption saturation and the adsorbent to NOxThe adsorption of (2) is rapid.
Claims (9)
1. Use of an adsorbent for nitrogen oxide storageThe nitrogen oxide storage adsorbent takes polydivinylbenzene as a carrier, and TiO is loaded on the polydivinylbenzene2The method is characterized in that: the adsorbent is used for storing nitrogen oxides, and the preparation method of the adsorbent for storing nitrogen oxides comprises the following steps:
(1) adding TiO into the mixture2Adding the mixture into an organic solvent, adding an initiator, uniformly mixing by ultrasonic, adding a divinylbenzene monomer, and carrying out polymerization reaction under ultrasonic;
(2) and after the polymerization reaction, filtering, washing and drying the obtained solid to obtain the adsorbent for storing the nitrogen oxide.
2. Use according to claim 1, characterized in that: 0.04-0.2g of TiO supported on polydivinylbenzene polymerized from 1ml of divinylbenzene monomer2。
3. Use according to claim 1 or 2, characterized in that: the TiO is2Is nano TiO2。
4. Use according to claim 1, characterized in that: the initiator is boron trifluoride ethyl ether.
5. Use according to claim 1 or 4, characterized in that: the volume of the initiator is 8-15% of the volume of the divinylbenzene monomer.
6. Use according to claim 1, characterized in that: the organic solvent is n-hexane.
7. Use according to claim 1, characterized in that: the polymerization temperature is 20-30 ℃, and the reaction time is 20-30 min.
8. Use according to claim 1, characterized in that: divinyl benzene monomer by alkaline Al2O3The leaching column filters out the polymerization inhibitor and then adds the polymerization inhibitor into the polymerization reaction system.
9. A method for removing nitrogen oxides in flue gas of an industrial boiler or a furnace kiln is characterized by comprising the following steps: the use of the adsorbent for nitrogen oxide storage according to claim 1, 2 or 3 for adsorbing nitrogen oxides in flue gas at an adsorption temperature of 30 to 35 ℃.
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| AU2003285121A1 (en) * | 2002-10-30 | 2004-06-07 | Waters Investments Limited | Porous inorganic/organic hybrid materials and preparation thereof |
| CN103263911B (en) * | 2013-05-14 | 2015-02-25 | 上海大学 | Preparation method of denitration catalyst with nanoscale ordered honeycomb structure |
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