CN114917880A - Reusable nitrogen oxide adsorbent, preparation method and application - Google Patents
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- 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 belongs to the technical field of advanced materials, relates to a nitrogen oxide adsorbent, and particularly relates to a reusable nitrogen oxide adsorbent, and a preparation method and application thereof. The preparation method comprises the following steps: manganese acetate, potassium ferricyanide and polyvinylpyrrolidone are reacted to obtain ferromanganese cyanide, and the ferromanganese cyanide is calcined to obtain the manganese ferricyanide. The adsorbent provided by the invention has good nitrogen oxide adsorption performance and can be repeatedly used.
Description
Technical Field
The invention belongs to the technical field of advanced materials, relates to a nitrogen oxide adsorbent, and particularly relates to a reusable nitrogen oxide adsorbent, and a preparation method and application thereof.
Background
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
NH with V-W/Mo-Ti as commercial catalyst 3 SCR is the most efficient NOx removal technology. However, the SCR catalyst activation temperature is higher than 250 ℃, and the catalytic performance during a cold start of the vehicle is insufficient. To treat cold start emissions, it is a potential strategy to combine a passive nitrogen oxide adsorber (PNA) unit with an SCR unit. PNA materials adsorb NOx at temperatures below 200 deg.C, and stored NOx can be converted to N by downstream SCR units at high temperatures 2 . Noble metal (Pd, Pt) supported zeolites and metal oxides are the most advanced PNA materials and many studies have been carried out to improve their NOx adsorption capacity. Noble metal adsorbents have two major drawbacks: the high cost of the precious metals and the tendency of the dispersed precious metals to aggregate during the NOx adsorption/desorption cycle. Therefore, the search for new efficient and inexpensive adsorption materials to cope with NOx abatement is urgently needed.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide a reusable nitrogen oxide adsorbent, a preparation method and application thereof.
In order to achieve the purpose, the technical scheme of the invention is as follows:
on the one hand, the preparation method of the reusable nitrogen oxide adsorbent comprises the steps of reacting manganese acetate, potassium ferricyanide and polyvinylpyrrolidone to obtain ferromanganese cyanide, and then calcining the ferromanganese cyanide to obtain the reusable nitrogen oxide adsorbent.
The manganese ferricyanide precursor with special morphology is generated in polyvinylpyrrolidone (PVP) through manganese salt and potassium ferricyanide, and then the manganese ferricyanide composite metal material with adsorption activity to nitrogen oxides is obtained through calcination. Experiments show that the adsorbing efficiency of the adsorbent prepared by using the inorganic manganese salts such as manganese nitrate and manganese sulfate as raw materials is sharply reduced when the adsorbent is used for 30-45 min, the removal rate of nitrogen oxides in gas is as low as 5%, and the adsorbing performance is poor. Experiments show that when manganese acetate is used for replacing inorganic manganese salt to be used as a manganese salt raw material for preparation, the obtained adsorbent can last for 4 hours, and the removal rate of nitrogen oxides in gas is still higher than 70%. The main reason is that manganese acetate is an organic salt, when PVP is used as a template to control the morphology of ferromanganese cyanide, acetate is easy to hydrolyze in water to generate acetic acid molecules, the acetic acid molecules can interact with the PVP to adjust the microstructure of a ferromanganese cyanide precursor, the microstructure of a ferromanganese metal composite material can be further adjusted through calcination, and the adjusted microstructure of the ferromanganese metal composite material is more favorable for adsorbing nitrogen oxides in gas, so that the adsorption performance of the adsorbent on the nitrogen oxides is improved.
In another aspect, a reusable nitrogen oxide adsorbent is obtained by the above-described method of preparation.
In a third aspect, use of a reusable nitrogen oxide adsorbent as described above for adsorbing nitrogen oxides in exhaust gas in a motor vehicle.
The invention has the beneficial effects that:
1. in the preparation method, manganese ions and potassium ferricyanide form a ferromanganese cyanide precursor with special morphology under the action of PVP (polyvinyl pyrrolidone) as a template, the ferromanganese metal composite material with adsorption activity on nitrogen oxides is obtained by calcining, and meanwhile, manganese acetate is used as a raw material, wherein the addition of acetate can cooperate with PVP to further adjust the microscopic morphology of the adsorbent, improve the adsorption activity of the adsorbent on nitrogen oxides, and further improve the adsorption performance of the adsorbent.
2. The low-temperature NOx adsorbent effectively adsorbs and stores NOx at low temperature, releases the stored NOx after temperature rise, and is suitable for NOx emission control in the cold start stage of a motor vehicle. The raw material composition elements of the adsorbent are low in price and low in cost, and the adsorbent is an efficient and low-cost NOx adsorbent.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a NOx adsorption removal curve at different temperatures for the adsorbent prepared in example 1 of the present invention;
FIG. 2 is a NOx adsorption removal curve of synthetic adsorbents prepared in examples 1 to 3 according to different metal ratios of the present invention;
FIG. 3 is a NOx adsorption removal curve of synthetic adsorbents prepared in examples 1 and 4 to 5 of the present invention at different calcination temperatures;
FIG. 4 is a NOx adsorption removal curve of different precursor synthetic adsorbents prepared in embodiments 1, 6 to 7 of the present invention.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
In view of the problem of high cost of the adsorbent in the prior art, the invention provides a reusable nitrogen oxide adsorbent, and a preparation method and application thereof.
The invention provides a preparation method of a reusable nitrogen oxide adsorbent, which comprises the steps of reacting manganese acetate, potassium ferricyanide and polyvinylpyrrolidone to obtain ferromanganese cyanide, and calcining the ferromanganese cyanide to obtain the reusable nitrogen oxide adsorbent.
Manganese acetate is used as a raw material, wherein manganese ions and potassium ferricyanide form a ferromanganese cyanide precursor with a special shape under the template action of PVP, and then the ferromanganese composite metal material with the adsorption activity on nitrogen oxides is obtained through calcination; acetate ions can be hydrolyzed to form acetic acid molecules, the morphology of the adsorbent can be further improved by cooperating with PVP, and the adsorption activity of the adsorbent on nitrogen oxides can be improved.
In some examples of this embodiment, manganese acetate, potassium ferricyanide, and polyvinylpyrrolidone are reacted in an aqueous ethanol solution. Is beneficial to the uniform mixing and reaction efficiency of manganese acetate, potassium ferricyanide and polyvinylpyrrolidone. The ethanol and the water are mixed in any ratio, and the preferred volume ratio is 2-5: 1.
In some examples of this embodiment, the manganese acetate and the polyvinylpyrrolidone are dissolved to obtain a mixed solution, and the potassium ferricyanide solution is added dropwise to the mixed solution to perform the reaction.
In some examples of this embodiment, the molar ratio of manganese acetate to potassium ferricyanide is 1:0.3 to 2.2. Research shows that the molar ratio of manganese acetate to potassium ferricyanide also influences the adsorption efficiency of the adsorbent, and under the condition, the obtained adsorbent can be ensured to have higher adsorption efficiency within 2 hours, and the removal rate of nitrogen oxides is higher than 60%. When the molar ratio of manganese acetate to potassium ferricyanide is 1: 1.8-2.2, the obtained adsorbent has higher adsorption activity.
In some embodiments of this embodiment, the temperature of the calcining is 450 to 550 ℃. Research shows that the calcination condition can ensure that the adsorbent has higher adsorption activity, and when the calcination temperature is 450-500 ℃, the adsorbent has higher adsorption activity.
In some examples of this embodiment, the temperature increase rate of the calcination is 1 to 3 ℃ for min -1 . The phenomenon that the microscopic morphology of the adsorbent is influenced by too fast temperature rise is avoided.
In some examples of this embodiment, the calcination time is 1 to 3 hours.
In another embodiment of the present invention, there is provided a reusable nitrogen oxide adsorbent obtained by the above-described production method.
In a third embodiment of the invention, there is provided a use of the above-described reusable nitrogen oxide adsorbent for adsorbing nitrogen oxides in exhaust gas of a motor vehicle.
Specifically, the exhaust gas is adsorbed by the nitrogen oxide adsorbent.
More specifically, the adsorption temperature is 180-220 ℃.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
Example 1
Certain amount of manganese acetate and PVP are dissolved in ethanol water (the volume ratio of ethanol to water is 2: 1), potassium ferricyanide is dissolved in the water solution, and the obtained solution is kept for 1h under stirring at room temperature. The molar ratio of manganese acetate to potassium ferricyanide is 1: 2. Dripping potassium ferricyanide solution into mixed solution of manganese acetate and PVP, standing at room temperature for 24h, centrifuging, washing, drying, calcining at 450 deg.C for 2h, and heating at 1 deg.C for min -1 Cooling to room temperature to obtain Mn 1 Fe 2 -450 adsorbents.
Example 2
Certain amount of manganese acetate and PVP are dissolved in ethanol water (the volume ratio of ethanol to water is 2: 1), potassium ferricyanide is dissolved in the water solution, and the obtained solution is kept for 1h under stirring at room temperature. The molar ratio of manganese acetate to potassium ferricyanide is 1:1. Dripping potassium ferricyanide solution into mixed solution of manganese acetate and PVP, standing at room temperature for 24h, centrifuging, washing, drying, calcining at 450 deg.C for 2h, and heating at 1 deg.C for min -1 Cooling to room temperature to obtain the product Mn 1 Fe 1 -450 adsorbents.
Example 3
Certain amount of manganese acetate and PVP are dissolved in ethanol water (the volume ratio of ethanol to water is 2: 1), potassium ferricyanide is dissolved in the water solution, and the obtained solution is kept for 1h under stirring at room temperature. The molar ratio of manganese acetate to potassium ferricyanide is 2: 1. Dripping the mixed solution of manganese acetate and PVP into potassium ferricyanide solution, and standing at room temperatureStanding for 24h, centrifuging, washing, drying, calcining at 450 deg.C for 2h, and heating at 1 deg.C for min -1 Cooling to room temperature to obtain the product Mn 2 Fe 1 -450 adsorbents.
Example 4
Certain amount of manganese acetate and PVP are dissolved in ethanol water (the volume ratio of ethanol to water is 2: 1), potassium ferricyanide is dissolved in the water solution, and the obtained solution is kept for 1h under stirring at room temperature. The molar ratio of manganese acetate to potassium ferricyanide is 1: 2. Dripping potassium ferricyanide solution into mixed solution of manganese acetate and PVP, standing at room temperature for 24h, centrifuging, washing, drying, calcining at 500 deg.C for 2h, and heating at 1 deg.C for min -1 Cooling to room temperature to obtain Mn 1 Fe 2 -500 adsorbents.
Example 5
Certain amount of manganese acetate and PVP are dissolved in ethanol water (the volume ratio of ethanol to water is 2: 1), potassium ferricyanide is dissolved in the water solution, and the obtained solution is kept for 1h under stirring at room temperature. The molar ratio of manganese acetate to potassium ferricyanide is 1: 2. Dripping potassium ferricyanide solution into mixed solution of manganese acetate and PVP, standing at room temperature for 24h, centrifuging, washing, drying, calcining at 550 deg.C for 2h, and heating at 1 deg.C for min -1 Cooling to room temperature to obtain Mn 1 Fe 2 -550 adsorbent.
Example 6
Certain amount of manganese nitrate and PVP are dissolved in aqueous ethanol (the volume ratio of ethanol to water is 2: 1), potassium ferricyanide is dissolved in the aqueous solution, and the obtained solution is kept for 1h under stirring at room temperature. The molar ratio of manganese nitrate to potassium ferricyanide is 1: 2. Dripping potassium ferricyanide solution into mixed solution of manganese nitrate and PVP, standing at room temperature for 24h, centrifuging, washing, drying, calcining at 450 deg.C for 2h, and heating at 1 deg.C for min -1 Cooling to room temperature to obtain Mn 1 Fe 2 -450 adsorbents.
Example 7
Certain amount of manganese sulfate and PVP are dissolved in ethanol water solution (the volume ratio of ethanol to water is 2: 1), potassium ferricyanide is dissolved in the water solution, and the obtained solution is kept for 1h under stirring at room temperature. Mole of manganese sulfate and potassium ferricyanideThe molar ratio is 1: 2. Dripping potassium ferricyanide solution into manganese sulfate and PVP mixed solution, standing at room temperature for 24h, centrifuging, washing, drying, calcining at 450 deg.C for 2h, and heating at 1 deg.C for min -1 Cooling to room temperature to obtain the product Mn 1 Fe 2 -450 adsorbents.
NOx adsorption Performance detection
The synthesized adsorbent was subjected to NOx adsorption performance test under the following conditions: the mixed gas contains 500ppm NO and 5% O 2 、N 2 As balance gas, the relative space velocity is 15000h -1 。
The results of the adsorption performance at different temperatures are shown in FIG. 1, and under the test conditions, Mn prepared in example 1 of the present invention 1 Fe 2 The-450 adsorbent shows good low-temperature adsorption performance, and the NOx removal rate is maintained to be more than 70% within 240min when the adsorption temperature is 200 ℃.
The results of the adsorption performance of the adsorbents synthesized at different metal ratios are shown in FIG. 2, and under the test conditions, at an adsorption temperature of 200 ℃, the adsorbents Mn prepared in examples 1, 2 and 3 of the present invention 1 Fe 2 -450、Mn 1 Fe 1 -450 and Mn 2 Fe 1 450 comparison found that example 1 produced Mn with a ferromanganese ratio of 1:2 1 Fe 2 450 shows good low-temperature adsorption performance, and the NOx removal rate is maintained to be more than 70% within 240 min.
The results of the adsorption performance of the adsorbents obtained at different calcination temperatures are shown in FIG. 3, and under the test conditions, at an adsorption temperature of 200 ℃, the adsorbents Mn obtained at different calcination temperatures according to the present invention prepared in examples 1, 4 and 5 were obtained 1 Fe 2 -450、Mn 1 Fe 2 -500 and Mn 1 Fe 2 Comparison of-550 shows Mn prepared at a calcination temperature of 450 ℃ in example 1 1 Fe 2 450 shows good low-temperature adsorption performance, and the NOx removal rate is maintained to be more than 70% in 240 min.
The results of the adsorption performance of the adsorbents prepared from different manganese precursors are shown in FIG. 4, under the test conditions, when the adsorption temperature is 200 ℃, the adsorbents are obtained by using manganese acetate, manganese nitrate and manganese sulfate as precursorsAdsorbents Mn prepared in examples 1, 6 and 7 1 Fe 2 -AC、Mn 1 Fe 2 -SO 4 And Mn 1 Fe 2 -NO 3 By comparison, the Mn prepared in example 1 by using manganese acetate as a manganese precursor at the calcination temperature of 450 DEG C 1 Fe 2 -450(Mn 1 Fe 2 -NO 3 ) The catalyst shows good low-temperature adsorption performance, and the NOx removal rate is maintained to be more than 70% within 240 min.
For the adsorbent Mn prepared in example 1 1 Fe 2 -450 performing a NOx adsorption-desorption 3 cycle test, the desorption test being performed with N 2 The purged NOx adsorbing material is used for adsorbing NOx at the temperature of 5 ℃ for min -1 The temperature was raised to 500 ℃ for 2 hours. The amount of adsorption and desorption of NOx were calculated, and as shown in table 1, it was found that the adsorbent had good reusability.
TABLE 1 NOx adsorption-desorption 3 cycles test results
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a reusable nitrogen oxide adsorbent is characterized in that manganese acetate, potassium ferricyanide and polyvinylpyrrolidone are reacted to obtain ferromanganese cyanide, and the ferromanganese cyanide is calcined to obtain the reusable nitrogen oxide adsorbent.
2. The method of claim 1, wherein the manganese acetate, potassium ferricyanide and polyvinylpyrrolidone are reacted in an aqueous ethanol solution.
3. The method of preparing the reusable nitrogen oxide adsorbent as set forth in claim 1, wherein the manganese acetate is dissolved in the polyvinylpyrrolidone to obtain a mixed solution, and the potassium ferricyanide solution is added dropwise to the mixed solution to carry out the reaction.
4. The method for preparing the reusable nitrogen oxide adsorbent as claimed in claim 1, wherein the molar ratio of manganese acetate to potassium ferricyanide is 1: 0.3-2.2; preferably, the molar ratio of manganese acetate to potassium ferricyanide is 1: 1.8-2.2.
5. The method of claim 1, wherein the calcining temperature is 450-550 ℃; preferably, the calcination temperature is 450-500 ℃.
6. The method for preparing the reusable nitrogen oxide adsorbent as claimed in claim 1, wherein the temperature rise rate of the calcination is 1 to 3 ℃ for min -1 。
7. The method according to claim 1, wherein the calcination time is 1 to 3 hours.
8. A reusable nitrogen oxide adsorbent obtainable by the production method according to any one of claims 1 to 7.
9. Use of the reusable nitrogen oxide adsorbent of claim 8 in the adsorption of nitrogen oxides in exhaust gas emissions in a motor vehicle.
10. Use according to claim 9, wherein the exhaust gas is subjected to adsorption by said nitrogen oxide adsorbent;
preferably, the adsorption temperature is 180-220 ℃.
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| JPH09313883A (en) * | 1996-05-24 | 1997-12-09 | Sakai Chem Ind Co Ltd | Method for removing nitrogen oxide |
| CN102068994A (en) * | 2010-12-14 | 2011-05-25 | 昆明理工大学 | Catalyst and preparation method thereof |
| CN103055799A (en) * | 2013-01-28 | 2013-04-24 | 中国科学院上海硅酸盐研究所 | Mesoporous manganese-based composite metal oxide as well as preparation method and application thereof |
| CN103752321A (en) * | 2014-01-02 | 2014-04-30 | 上海大学 | Method for preparing hierarchical bimetallic composite oxide denitrification catalyst |
| CN105776249A (en) * | 2016-05-09 | 2016-07-20 | 上海第二工业大学 | Manganese hexacyanoferrate nano cube and preparation method thereof |
| CN107233895A (en) * | 2017-07-31 | 2017-10-10 | 清华大学 | A kind of motor vehicle tail-gas purifying oxidation catalyst and preparation method thereof |
| CN109653848A (en) * | 2018-12-27 | 2019-04-19 | 天津大学 | A method of nitric oxide adsorption and/or hydrocarbon compound during motor vehicle cold start |
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2022
- 2022-05-17 CN CN202210535497.1A patent/CN114917880B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH09313883A (en) * | 1996-05-24 | 1997-12-09 | Sakai Chem Ind Co Ltd | Method for removing nitrogen oxide |
| CN102068994A (en) * | 2010-12-14 | 2011-05-25 | 昆明理工大学 | Catalyst and preparation method thereof |
| CN103055799A (en) * | 2013-01-28 | 2013-04-24 | 中国科学院上海硅酸盐研究所 | Mesoporous manganese-based composite metal oxide as well as preparation method and application thereof |
| CN103752321A (en) * | 2014-01-02 | 2014-04-30 | 上海大学 | Method for preparing hierarchical bimetallic composite oxide denitrification catalyst |
| CN105776249A (en) * | 2016-05-09 | 2016-07-20 | 上海第二工业大学 | Manganese hexacyanoferrate nano cube and preparation method thereof |
| CN107233895A (en) * | 2017-07-31 | 2017-10-10 | 清华大学 | A kind of motor vehicle tail-gas purifying oxidation catalyst and preparation method thereof |
| CN109653848A (en) * | 2018-12-27 | 2019-04-19 | 天津大学 | A method of nitric oxide adsorption and/or hydrocarbon compound during motor vehicle cold start |
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