CN113398953A - Plasma-assisted catalyst desulfurization and storage bit thermal regeneration method and application - Google Patents

Plasma-assisted catalyst desulfurization and storage bit thermal regeneration method and application Download PDF

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CN113398953A
CN113398953A CN202110636561.0A CN202110636561A CN113398953A CN 113398953 A CN113398953 A CN 113398953A CN 202110636561 A CN202110636561 A CN 202110636561A CN 113398953 A CN113398953 A CN 113398953A
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desulfurization
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石川
王芷卉
陈冰冰
赵琦
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Dalian University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01J23/90—Regeneration or reactivation
    • B01J23/96—Regeneration or reactivation of catalysts comprising metals, oxides or hydroxides of the noble metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B01J38/02—Heat treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
    • B01J38/10—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst using elemental hydrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
    • F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
    • F01N3/18—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control
    • F01N3/20—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control specially adapted for catalytic conversion ; Methods of operation or control of catalytic converters
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
    • F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
    • F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
    • F01N3/28—Construction of catalytic reactors
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N2370/00—Selection of materials for exhaust purification
    • F01N2370/02—Selection of materials for exhaust purification used in catalytic reactors

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Abstract

The invention discloses a plasma-assisted catalyst desulfurization and storage bit thermal regeneration method and application, and belongs to the technical field of nitrogen oxide control in environmental protection. Putting the sulfur poisoning catalyst into a non-thermal equilibrium plasma catalytic reactor, introducing mixed gas containing reducing gas into the reactor, and completely decomposing and desorbing sulfate species adsorbed on the surface of the sulfur poisoning catalyst by utilizing the non-thermal equilibrium plasma discharging process to complete the desulfurization treatment of the sulfur poisoning catalyst; and then the thermal regeneration of the catalyst storage bit and the reconstruction of oxygen species are completed in a thermal roasting mode, so that the catalytic performance is recovered and regenerated. The non-thermal equilibrium plasma technology can realize the desulfurization of the PNA material under the room temperature condition without adding an additional heat source, compared with high-temperature thermal regeneration, the desulfurization amount is higher, the desulfurization temperature is lower, and the sintering of the active center noble metal in the high-temperature desulfurization process is avoided.

Description

Plasma-assisted catalyst desulfurization and storage bit thermal regeneration method and application
Technical Field
The invention belongs to the technical field of nitrogen oxide control in environmental protection, and particularly relates to a plasma-assisted noble metal-loaded catalyst desulfurization and storage bit thermal regeneration method and application.
Background
In recent years, environmental protection is more and more strongly demanded, and industrially developed countries such as the united states, the japanese, the korean, and the europe have recently made and executed new emission standards, and the emission limit of NO is becoming strict. Therefore, how to control nitrogen oxides has become a research hotspot at home and abroad. Commercial NOxThe emission reduction technology is NH3Selective catalytic reduction of NOx(NH3-SCR) and NOxStorage Reduction (NSR), however, the catalyst operating temperature of these methods is generally 250-400 ℃ and the denitration system has not been raised to its operating temperature below 200 ℃, so most of the NO isxThe emissions are generated during the cold start phase. Since environmental regulations increasingly limit regulated nitrogen oxide emission concentrations, PNA (Passive NO) was introduced during the cold start phase of automobilesxAdsorber, low temperature nox storage catalyst) technology to control NO during cold start phase of lean burn enginesxAnd (4) discharging. The goal of PNA technology is to store nitrogen oxides during cold start of a vehicle when NO is presentxReleasing NO when the reduction catalyst reaches its operating temperaturexPNA technology with NH3Selective Catalytic Reduction (SCR) technology is used in combination.
The core catalyst of the PNA technology is mainly Pd ion exchange zeolite molecular sieve or ceria-based oxide, however, in practical application, it is found that the combustion of sulfur-containing fuel and vehicle lubricating oil inevitably leads to the generation of low-concentration sulfur oxides in automobile exhaust, and the sulfur oxides lead to the deactivation of storage materials due to sulfur poisoning, thereby greatly reducing the storage capacity of nitrogen oxides. Sulfur oxide and NOxProduces competitive adsorption and preferentially occupies NO on the catalystxStorage bit of (2), reduction of catalyst NOxThe adsorption amount of (c); in NOxThe sulfates formed on the storage sites are more thermally stable than nitrates and nitrites and, therefore, have a higher decomposition index (typically above 700 ℃).
At present, the domestic aims at low-temperature storage of NO in lean burn engine tail gas in cold start stage by oxide catalystxThe technical research is just started, and the deactivation of the catalyst caused by sulfur poisoning is a key problem to be solved in the practical application of the catalyst. At present, the heating mode is mainly used for the regeneration of the sulfur poisoning catalyst at home and abroad, but the thermal regeneration desulfurization process not only needs higher energy consumption, but also can cause the problems of catalyst structure deactivation, precious metal sintering and the like, and further influences the nitrogen oxide storage capacity of the catalyst (Catalysis Today 2015,258, 378-385; Catalysis Communications,2013, 5-9), so that the development of a novel low-energy-consumption sulfur poisoning catalyst regeneration method is urgently needed.
Disclosure of Invention
The invention aims to provide a method and application for desulfurizing a plasma-assisted catalyst and thermally regenerating a storage bit, and the method is applied to a cold start reaction, so that the problem that the storage performance of the existing PNA material is seriously reduced after sulfur poisoning can be effectively solved, and the PNA material can keep higher nitrogen oxide storage capacity for a long time in practical application.
The invention is realized by the following technical scheme:
a plasma-assisted method for desulfurizing a catalyst and thermally regenerating a storage bit comprises the steps of placing a noble metal-loaded catalyst stored in a sulfur poisoning nitrogen oxide to be treated in a non-thermal equilibrium plasma catalytic reactor, introducing mixed gas containing reducing gas into the non-thermal equilibrium plasma catalytic reactor, and completely decomposing and desorbing sulfate species adsorbed on the surface of the sulfur poisoning catalyst to be treated by using non-thermal equilibrium plasma in the non-thermal equilibrium plasma catalytic reactor, namely completing desulfurization treatment on the sulfur poisoning catalyst; and then, filling the reduced surface and lattice oxygen species of the catalyst in the desulfurization process by a mode of hot roasting in the air, completing the structural recombination of the oxygen species in the catalyst, and recovering and regenerating the catalytic performance.
The non-thermal equilibrium plasma catalytic reactor (fig. 1) is: use of non-thermal equilibrium plasma reactor for adsorption and desorption of SO2And NOx. The non-thermal equilibrium plasma catalytic reactor comprises a hollow quartz tube (the inner diameter is 6mm, the outer diameter is 8mm), a discharge area is arranged in the quartz tube, certain spaces are reserved between the discharge area and two ends of the quartz tube, a catalyst to be treated is placed in the discharge area, the outer side wall of the quartz tube at the position of the discharge area is wrapped by a ground electrode (a copper mesh), sealing heads are arranged at two ends of the quartz tube, a sealing head at one end is provided with an air outlet, a sealing head at the other end is penetrated by a stainless steel electrode (the diameter is 2mm), the stainless steel electrode reserved outside the quartz tube is connected with a plasma generator, the stainless steel electrode reserved inside the quartz tube penetrates through the catalyst to be treated in the discharge area, and an air inlet is further formed in the sealing head connected with one side of the stainless steel electrode.
Further, the noble metal includes Pt, Pd, or Ag.
Further, the mixed gas containing the reducing gas comprises the reducing gas and H2O、CO2And a mixed gas of an inert gas; the reducing gas comprises hydrogen.
Further, the mixed gas contains reducing gas H2O、CO2The volume ratio of the inert gas to the inert gas is 0.01-0.2: 0.02: 0.05: 0.92-0.73; the total flow rate of the mixed gas is 50-200 mL/min.
Further, the treatment time of the non-thermal equilibrium plasma discharge process is 20-40min, and the temperature is room temperature.
Further, the discharge mode of the non-thermal equilibrium plasma discharge process is dielectric barrier discharge, the discharge voltage is 30-35V, and the input power is 30-50W.
Furthermore, the atmosphere of the hot roasting is air, the roasting temperature is 500-800 ℃, and the time is 3-25 h.
A method for desulfurizing a catalyst assisted by plasma and thermally regenerating a storage bit is applied to the desulfurization and regeneration of a noble metal-loaded catalyst stored in sulfur-poisoned low-temperature nitrogen oxides in an automobile cold start reaction. The low temperature is 80-200 ℃.
(1) The desulfurization process of the plasma treatment catalyst comprises the following steps:
with Pd/CeO2Taking the catalyst as an example, the sulfur poisoned catalyst is subjected to room temperature non-thermal equilibrium plasma discharge treatment, the discharge mode is dielectric barrier discharge, the center frequency of a discharge power supply is 30kHZ, the discharge voltage is 30V, the input power is 48W, and the discharge atmosphere is H2/H2O/CO2The total flow of discharge atmosphere is 100mL/min, and 2Pd/CeO is obtained after discharge is finished after 40min2-nH2A catalyst.
(2) The storage position process of the catalyst regenerated by roasting treatment comprises the following steps:
further, after the above technical scheme of plasma desulfurization, the process of regenerating the catalyst storage bit is as follows: for 2Pd/CeO2-nH2Roasting the catalyst, and roasting the catalyst in a muffle furnace at 500 ℃ for 3-25h to obtain 2Pd/CeO2-nH2-nh catalysis catalyst.
Advantageous effects of the invention
1. The invention organically combines the two processes of plasma desulfurization and catalyst calcination regeneration and is used for the regeneration of sulfur-poisoned PNA material of automobile cold start reaction.
2. The non-thermal equilibrium plasma technology can realize the desulfurization of the PNA material under the room temperature condition without adding an additional heat source, compared with high-temperature thermal regeneration, the desulfurization amount is higher, the desulfurization temperature is lower, and the sintering of the active center noble metal in the high-temperature desulfurization process is avoided.
3. The invention can obtain the best desulfurization effect by adjusting the regeneration atmosphere and proportion, and utilizes high-energy electrons generated in the non-thermal equilibrium plasma discharge process to remove reducing gas such as H2The sulfate species adsorbed on the surface of the catalyst is completely converted into H by isodissociation into atoms with higher reduction capability or other excited state species2S and SO2And ensures the dispersibility of the noble metal.
4. The invention mixes H in the regeneration atmosphere2O and CO2Improving the speed of sulfur on the surface of the catalystDesorption, and better desulfurization treatment effect on the catalyst.
5. The storage position process of the roasting regeneration catalyst is realized by roasting in the air at high temperature, filling reduced surface and lattice oxygen species in the desulfurization process and restructuring the catalyst structure. The proper roasting temperature and the prolonged roasting time are more favorable for completing the regeneration of the storage position of the catalyst and the reconstruction of oxygen species.
Drawings
FIG. 1 is a schematic diagram of a non-thermal equilibrium plasma catalytic reactor according to the present invention.
In the figure, 1, a quartz tube; 2. a ground electrode; 3. a stainless steel electrode; 4. a discharge region; 5. an air inlet; 6. an air outlet; 7. a plasma generator.
Detailed Description
The following non-limiting examples will allow one of ordinary skill in the art to more fully understand the present invention, but are not intended to limit the invention in any way.
Example 1 plasma reducing atmosphere desulfurization experiment
(1) Taking 130mg of Pd/CeO2Loading the catalyst into a fixed bed reactor, introducing Ar gas into a reaction tube, heating to 300 ℃ by using a non-standard open-type tubular furnace, and introducing 20ppm SO after the temperature is raised to 300 DEG C2A mixed atmosphere with Ar for a period of 95min, followed by lowering the temperature to room temperature, whereby the vulcanization step was completed, and the amount of sulfur added was calculated to be 0.017gSO2/gcat. The storage capacity of the catalyst after sulfur poisoning is greatly reduced, from 193. mu. mol/g of fresh catalystcatThe concentration is reduced to 133 mu mol/gcat。
(2) Performing room temperature non-thermal equilibrium plasma discharge treatment on sulfur-poisoned catalyst, wherein the discharge mode is dielectric barrier discharge, the discharge power frequency is 10-30kHZ, the discharge voltage is 30V, the discharge power is 48W, and the discharge atmosphere is 1-20% H2/2％H2O/5％CO292% -73% of Ar, and the total flow of the discharge atmosphere is 100 mL/min; and SO is used in the discharge process2Gas analyzer (S710) real-time monitoring desorption SO2Concentration (ppm), end of discharge after 40 minutes2Pd/CeO is obtained2-nH2The catalyst is further characterized by organic element analysis to calculate the desulfurization ratio of the catalyst. The experimental result shows that the desulfurization proportion reaches 62.3 percent under the conditions that the frequency of a discharge power supply is 30kHZ, the discharge voltage is 30V and the discharge power is 48W.
TABLE 1 Pd/CeO after Sulfur poisoning2Deactivation catalyst NOxStorage capacity and fresh Pd/CeO2Catalyst NOxComparison of memory
Figure BDA0003105975880000041
Table 2 shows comparison of desulfurization amounts in a reducing atmosphere under non-thermal equilibrium plasma conditions at room temperature
Figure BDA0003105975880000042
Comparative example 1 reducing atmosphere heat regeneration reaction experiment
(1) Taking 130mg of Pd/CeO2Loading the catalyst into a fixed bed reactor, introducing Ar gas into a reaction tube, heating to 300 ℃ by using a non-standard open-type tubular furnace, and introducing 20ppm SO after the temperature is raised to 300 DEG C2A mixed atmosphere with Ar for a period of 95min, followed by lowering the temperature to room temperature, whereby the vulcanization step was completed, and the amount of sulfur added was calculated to be 0.017gSO2/gcat。
(2) And carrying out thermal regeneration on the sulfur poisoning catalyst according to the designed temperature programming reaction. The experiment is carried out in a fixed bed reactor, the reaction atmosphere is Ar, the total gas flow is 100mL/min, the temperature is increased to 800 ℃ at the heating rate of 15 ℃/min and is kept for 2h, the outlet gas in the desulfurization process is monitored by adopting S710, and the desulfurization proportion of the catalyst is calculated through the analysis and characterization of organic elements. The experimental result shows that the desulfurization proportion reaches 52.1 percent and is lower than the room temperature plasma desulfurization proportion (62.3 percent) under the conditions that the thermal regeneration temperature is 800 ℃ and the desulfurization is carried out for 2 hours.
TABLE 3 SO in Ar atmosphere under thermal regeneration conditions of comparative example 12Amount of desorption
Figure BDA0003105975880000051
EXAMPLE 2 calcination treatment of catalyst experiment
(1) The catalyst activity was regenerated by adding 2Pd/CeO obtained in example 12-nH2The catalyst is roasted for a long time and is roasted for 3 to 25 hours at the temperature of 500 ℃ and 900 ℃ in a muffle furnace to obtain the regenerated catalyst.
(2) Research on 2 wt% Pd/CeO after regeneration by using fixed bed microreactor2NO of catalystxAnd (4) storing the performance. The total flow rate of the atmosphere is 400mL/min, and the space velocity (GHSV) is 200,000h-1And the desorbed NO concentration (ppm) is monitored with an NO gas analyzer (S710). First at 500 ℃ with 20% O2And Ar is balance gas to pretreat the catalyst for 1h, and then the temperature is reduced to 100 ℃ in Ar atmosphere to carry out NO treatmentxStorage Performance test with a storage atmosphere of 200ppm NO/500ppm CO/2% H2O/5％CO2/10％O2Ar, reaction time is 20 min. NOxStorage (NSC) normalized to catalyst mass, given in μmol/gcat。
Figure BDA0003105975880000052
The experimental result shows that the frequency of a discharge power supply is 30kHZ, the discharge voltage is 30V, the discharge power is 48W, and the discharge atmosphere is 20% H2/5％CO2/2％H2After desulfurization under O/Ar (100mL/min), NSC of the regenerated catalyst is restored to 171 mu mol/g after roasting in a muffle furnace at 500 ℃ for 20hcat。
Table 4 shows Pd/CeO after regeneration in example 22Catalyst NOxMemory comparison
Figure BDA0003105975880000061

Claims (9)

1. A method for desulfurizing a catalyst and thermally regenerating a storage bit by plasma assistance is characterized by comprising the following steps: placing a noble metal-loaded catalyst stored in sulfur poisoning nitrogen oxides to be treated in a non-thermal equilibrium plasma catalytic reactor, introducing mixed gas containing reducing gas into the non-thermal equilibrium plasma catalytic reactor, and completely decomposing and desorbing sulfate species adsorbed on the surface of the sulfur poisoning catalyst to be treated by using non-thermal equilibrium plasma in the non-thermal equilibrium plasma catalytic reactor, namely completing desulfurization treatment on the sulfur poisoning catalyst; and then, filling the reduced surface and lattice oxygen species of the catalyst in the desulfurization process by a mode of hot roasting in the air, completing the structural recombination of the oxygen species in the catalyst, and recovering and regenerating the catalytic performance.
2. The method of claim 1 for plasma-assisted desulfurization of catalysts and thermal regeneration of stored bits, wherein: the noble metal includes Pt, Pd, or Ag.
3. The method of claim 1 for plasma-assisted desulfurization of catalysts and thermal regeneration of stored bits, wherein: the mixed gas containing reducing gas comprises reducing gas and H2O、CO2And a mixed gas of an inert gas; the reducing gas comprises hydrogen.
4. A method of plasma-assisted catalyst desulfurization and storage bit thermal regeneration in accordance with claim 3, wherein: reducing gas and H in the mixed gas2O、CO2The volume ratio of the inert gas to the inert gas is 0.01-0.2: 0.02: 0.05: 0.92-0.73; the total flow rate of the mixed gas is 50-200 mL/min.
5. The method of claim 1 for plasma-assisted desulfurization of catalysts and thermal regeneration of stored bits, wherein: the treatment time of the non-thermal equilibrium plasma discharge process is 20-40min, and the temperature is room temperature.
6. The method of claim 1 for plasma-assisted desulfurization of catalysts and thermal regeneration of stored bits, wherein: the discharge mode of the non-thermal equilibrium plasma discharge process is dielectric barrier discharge, the discharge frequency is 2-30kHz, the discharge voltage is 20-60V, and the input power is 15-80W.
7. The method of claim 1 for plasma-assisted desulfurization of catalysts and thermal regeneration of stored bits, wherein: the atmosphere of the hot roasting is air, the roasting temperature is 500-800 ℃, and the time is 3-25 h.
8. Use of the method according to any one of claims 1 to 7, characterized in that: the catalyst is applied to the desulfurization and regeneration of the noble metal-loaded catalyst stored in sulfur-poisoned low-temperature nitrogen oxides in the cold start reaction of automobiles.
9. Use according to claim 8, wherein the low temperature is 80-200 ℃.
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Publication number Priority date Publication date Assignee Title
CN115957826A (en) * 2023-01-18 2023-04-14 常熟理工学院 Low-temperature plasma irradiation regeneration method of waste denitration catalyst and regenerated denitration catalyst
CN115957826B (en) * 2023-01-18 2023-08-04 常熟理工学院 Low-temperature plasma irradiation regeneration method of waste denitration catalyst and regenerated denitration catalyst

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