CN113680352A - Low-load Pt-Mn bimetallic catalyst for CO oxidation and preparation method and application thereof - Google Patents

Low-load Pt-Mn bimetallic catalyst for CO oxidation and preparation method and application thereof Download PDF

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CN113680352A
CN113680352A CN202111066870.5A CN202111066870A CN113680352A CN 113680352 A CN113680352 A CN 113680352A CN 202111066870 A CN202111066870 A CN 202111066870A CN 113680352 A CN113680352 A CN 113680352A
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bimetallic catalyst
flue gas
manganese
roasting
catalyst
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CN113680352B (en
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朱廷钰
刘霄龙
刘法高
徐铁堯
邹洋
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Institute of Process Engineering of CAS
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Abstract

The invention provides a low-load Pt-Mn bimetallic catalyst for CO oxidation and a preparation method and application thereof, wherein the preparation method comprises the following steps: adding TiO into the mixture2Soaking the carrier in a Mn source solution, and roasting to obtain a manganese-titanium agent; dipping a manganese-titanium agent in a Pt source solution, and roasting to obtain a Pt-Mn bimetallic catalyst; the content of Mn element in the Pt-Mn bimetallic catalyst is 0.10-0.80 wt% based on 100 wt% of the Pt-Mn bimetallic catalyst. The Pt-Mn bimetallic catalyst of the invention uses TiO2The carrier is Pt simple substance and/or oxide of Pt as a first active component, and manganese oxide as a second active component; the synergistic effect between the first active component and the second active component obviously reduces the dosage of the noble metals Pt and Mn. Compared with the traditional catalyst, the catalyst has high water resistance and sulfur resistanceThe load capacity of the active component is low, and the CO oxidation efficiency is high.

Description

Low-load Pt-Mn bimetallic catalyst for CO oxidation and preparation method and application thereof
Technical Field
The invention belongs to the field of environmental catalysis, and relates to a low-load Pt-Mn bimetallic catalyst for CO oxidation, and a preparation method and application thereof.
Background
CO is greatly harmful to human health and the natural environment, and becomes one of six standard atmospheric pollutants. In many aspects of daily life and industrial production, CO removal is required, and one of the most effective ways to remove CO is to oxidize CO to CO using a catalyst2At present, the catalyst is widely applied to the fields of automobile exhaust treatment, industrial flue gas treatment, fuel cells (PEMFC) and the like.
The catalyst is not only widely applied to the research of important catalysis problems such as catalyst structure-activity relationship and the like, but also widely applied to the fields of environment and the like, and the catalyst for CO oxidation mainly comprises two types of noble metal catalysts and non-noble metal catalysts. Noble metals mainly comprise Pt, Au, Pd, Ru and the like, and research on non-noble metal catalysts mainly focuses on CuO in a mixed valence statex、MnOx、FeOx、CoOxAnd CeOxThe above.
CN110013858B discloses a cobaltosic oxide monolithic catalyst for CO purification, which is characterized in that a rodlike cobaltosic oxide nano catalyst is prepared by a hydrothermal method and used as an active component for carbon monoxide oxidation, and an iron-chromium-nickel metal honeycomb subjected to heat treatment and chemical treatment is used as a carrier, so that the prepared monolithic catalyst has a remarkable CO purification effect. CN112058288A discloses a Pt/CuO/SiC catalyst applied to CO oxidation, which is prepared by mixing a certain amount of carbon source, silicon source, nickel catalyst and oxalic acid, roasting and impregnating, wherein the prepared catalyst has high catalytic efficiency. CN105473221A discloses a catalyst in which a large amount of reduced noble metal is dispersed in CeO2、TiO2、ZrO2、Al2O3Or SiO2The carrier is used for catalyzing and oxidizing gases such as formaldehyde, methanol, carbon monoxide and the like.
In practice, even after the industrial flue gas is desulfurized by using a desulfurization facility, the flue gas still contains certain concentrationSO2. Although the catalysts can generate a certain purification effect on CO, the sulfur resistance and water resistance of the non-noble metal catalyst are poor, and the toxicity resistance and stability of the catalyst are difficult to guarantee when the catalyst is applied to CO purification of industrial flue gas; noble metal catalysts generally require higher loading, which increases production costs and limits the wide application of catalysts.
Therefore, the development of a catalyst for CO oxidation, which has better water resistance and sulfur resistance and lower loading capacity, is of great significance.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a low-load Pt-Mn bimetallic catalyst for CO oxidation and a preparation method and application thereof. The Pt-Mn bimetallic catalyst provided by the invention is TiO2The carrier is Pt simple substance and/or oxide of Pt as a first active component, and manganese oxide as a second active component; wherein, the synergistic effect between the first active component and the second active component obviously reduces the dosage of the noble metals Pt and Mn. Compared with the traditional catalyst, the Pt-Mn bimetallic catalyst provided by the invention has the characteristics of obviously improved water-resistant and sulfur-resistant performance, low active component loading capacity, low cost, strong universality and good stability, and has high CO oxidation efficiency and better application prospect.
In the present invention, the "low loading" means that in the Pt-Mn bimetallic catalyst, the content of Mn element is 0.10 to 0.80 wt% and the content of Pt element is 0.02 to 0.20 wt% based on 100 wt% of the mass of the Pt-Mn bimetallic catalyst.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing a low-loading Pt-Mn bimetallic catalyst for CO oxidation, the method comprising the steps of:
(1) adding TiO into the mixture2Soaking the carrier in a Mn source solution, and roasting to obtain a manganese-titanium agent;
(2) dipping the manganese-titanium agent obtained in the step (1) in a Pt source solution, and roasting to obtain a Pt-Mn bimetallic catalyst;
wherein the content of the Mn element in the Pt-Mn bimetallic catalyst is 0.10-0.80 wt%, for example, 0.10 wt%, 0.20 wt%, 0.30 wt%, 0.40 wt%, 0.50 wt%, 0.60 wt%, 0.70 wt%, 0.80 wt%, etc., based on 100 wt% of the mass of the Pt-Mn bimetallic catalyst.
The manganese-titanium agent obtained in the step (1) comprises manganese oxide and TiO2，TiO2As the support, a manganese oxide is supported on the surface thereof. The oxides of manganese may be oxides of manganese in a single valence state, or may be a mixture of oxides of manganese in multiple valence states, which is not limited in the present invention.
The invention adopts a step-by-step impregnation method, firstly TiO2The carrier is soaked in a solution containing a small amount of Mn source and roasted to disperse the manganese oxide in TiO2And forming a manganese-titanium agent on the surface of the carrier, and then soaking the manganese-titanium agent in a Pt source solution for roasting to obtain the Pt-Mn bimetallic catalyst.
In the invention, TiO is firstly added2The carrier is soaked in a small amount of Mn source solution and then roasted, compared with the traditional catalyst, because the content of Mn element is less, the carrier can be uniformly distributed on the premise of TiO2Reserving a space on the surface of the carrier to ensure that a Pt elementary substance and/or Pt oxide and TiO obtained after the subsequent Pt source impregnation and roasting are ensured2Contact of the support, favouring TiO2The Pt and Mn on the surface of the carrier are alternately arranged, so that the synergistic effect of the Pt and the Mn is better exerted, and better water-resistant and sulfur-resistant performance is obtained.
If the content of Mn element is too high, it is liable to be in TiO2A manganese oxide coating layer is formed on the surface of the carrier, so that the Pt component can not be reacted with TiO2The carriers are in full contact with each other to block TiO2Combined with Pt to exert sulfur resistance and TiO2The strong oxidizing property of the active-OH groups on the surface influences the catalytic performance of the Pt-Mn bimetallic catalyst.
The preparation method is simple, and the prepared Pt-Mn bimetallic catalyst has high CO oxidation efficiency, good water resistance and sulfur resistance, high stability and low active component content.
Preferably, the content of the Mn element in the Pt-Mn bimetallic catalyst is 0.40-0.60 wt% based on 100 wt% of the mass of the Pt-Mn bimetallic catalyst.
Preferably, the content of the Pt element in the Pt-Mn bimetallic catalyst is 0.02 to 0.20 wt%, for example, may be 0.02 wt%, 0.04 wt%, 0.06 wt%, 0.08 wt%, 0.10 wt%, 0.12 wt%, 0.14 wt%, 0.16 wt%, 0.18 wt%, or 0.20 wt%, etc., preferably 0.08 to 0.12 wt%, based on 100 wt% of the mass of the Pt-Mn bimetallic catalyst.
Preferably, said TiO of step (1)2The carrier is anatase type TiO2。
Preferably, the Mn source in step (1) comprises any one of manganese nitrate, manganese sulfate or manganese chloride or a combination of at least two of them, and may be, for example, a combination of manganese nitrate and manganese sulfate, a combination of manganese sulfate and manganese chloride, a combination of manganese nitrate and manganese chloride, or a combination of manganese nitrate, manganese sulfate and manganese chloride.
Preferably, the time for the impregnation in step (1) is 2-24h, and may be, for example, 2h, 3h, 5h, 7h, 10h, 12h, 14h, 16h, 18h, 20h, 22h, 24h, or the like.
Preferably, after the impregnation and before the calcination in step (1), the preparation method further comprises drying, wherein the drying temperature is 80-120 ℃, for example, 80 ℃, 85 ℃, 90 ℃, 95 ℃, 100 ℃, 105 ℃, 110 ℃, 105 ℃ or 120 ℃, and the drying time is 2-5h, for example, 2h, 2.5h, 3h, 3.5h, 4h, 4.5h or 5 h.
Preferably, the temperature of the calcination in step (1) is 450-.
Preferably, the roasting time in the step (1) is 2-10h, for example, 2h, 3h, 4h, 5h, 6h, 7h, 8h, 9h or 10h, etc.
In one embodiment, the atmosphere for the calcination in step (1) is air.
Preferably, the Pt source in step (2) includes any one of platinum nitrate, platinum chloride or chloroplatinic acid or a combination of at least two thereof, and may be, for example, a combination of platinum nitrate and platinum chloride, a combination of platinum chloride and chloroplatinic acid, a combination of platinum nitrate and chloroplatinic acid, or a combination of platinum nitrate, platinum chloride and chloroplatinic acid.
Preferably, the time for the impregnation in step (2) is 2-24h, and may be, for example, 2h, 3h, 5h, 7h, 10h, 12h, 14h, 16h, 18h, 20h, 22h, 24h, or the like.
Preferably, after the impregnation and before the calcination in the step (2), the preparation method further comprises drying, wherein the drying temperature is 80-120 ℃, for example, 80 ℃, 85 ℃, 90 ℃, 95 ℃, 100 ℃, 105 ℃, 110 ℃, 105 ℃ or 120 ℃, and the drying time is 2-5h, for example, 2h, 2.5h, 3h, 3.5h, 4h, 4.5h or 5 h.
Preferably, the temperature of the calcination in step (2) is 450-.
Preferably, the roasting time in the step (2) is 2-10h, for example, 2h, 3h, 4h, 5h, 6h, 7h, 8h, 9h or 10h, etc.
In one embodiment, the atmosphere for the calcination in step (2) is air.
As a preferable technical scheme of the preparation method of the invention, the preparation method comprises the following steps:
(1) preparing Mn source solution, adding anatase TiO2Dipping for 2-24h, drying for 2-5h at 80-120 ℃, and then roasting for 2-10h at 450-600 ℃ to obtain a manganese-titanium agent;
(2) preparing a Pt source solution, adding the manganese-titanium agent in the step (1) to dip for 2-24h, drying at 80-120 ℃ for 2-5h, and then roasting at 450-600 ℃ for 2-10h to obtain the Pt-Mn bimetallic catalyst.
In a second aspect, the present invention provides a low-loading Pt-Mn bimetallic catalyst for CO oxidation, the Pt-Mn bimetallic catalyst obtained by the preparation method of the first aspect, the bimetallic catalyst comprising TiO2A carrier, a first active component and a second active component;
the first active component is a Pt simple substance and/or an oxide of Pt, and the second active component is a manganese oxide.
SO resistance of Pt-based catalysts among noble and transition metal oxide catalysts2The capability is far superior to other metal catalysts because part of SO is generated in the oxidation process of Pt to CO in industrial flue gas2Will be oxidized simultaneously to form SO3And with H in the flue gas2Formation of H by O-binding2SO4And then transferred to the surface of the carrier in a flowing liquid form, thereby releasing the active sites. Even so, it is still difficult for Pt-based catalysts to achieve long-term stable operation of industrial flue gas CO oxidation on an industrial time scale due to the constant sulfur deposition on the catalyst surface.
The Pt-Mn bimetallic catalyst of the invention uses TiO2As a carrier, manganese oxide is introduced as a second active component, and the second active component and Pt simple substance and/or Pt oxide generate a synergistic effect, so that the sulfation phenomenon of the catalyst in the catalytic process is inhibited, the problems of poor stability, easy agglomeration and inactivation of noble metal Pt and sulfur poisoning of the traditional Pt-based catalyst in a high-temperature environment are solved, and meanwhile, the first active component is used as a main active component which plays a synergistic catalytic effect, and the catalytic efficiency and the sulfur resistance of the catalyst are obviously improved by the synergistic effect of the first active component added with the carrier and the second active component.
In the invention, the first active component and the second active component are alternately arranged on the surface of the carrier, so that the consumption of the noble metal Pt is reduced, the obvious economic benefit is achieved, the obtained Pt-Mn bimetallic catalyst has good water and sulfur resistance, high CO catalytic oxidation performance and high CO product resistance2High selectivity is shown.
In a third aspect, the invention provides an application of the Pt-Mn bimetallic catalyst in the second aspect in the field of CO oxidation treatment of industrial flue gas.
Preferably, the concentration of CO in the industrial flue gas is 7000-9000ppm, which may be 7000ppm, 7100ppm, 7500ppm, 8000ppm, 8500ppm or 9000ppm, SO, based on the total volume of the industrial flue gas2The concentration of (B) is 0 to 500ppm, and may be, for example, 0, 50ppm, 100ppm, 200ppm, 300ppm or 500ppm, preferably 50 to 500 ppm;
with industrial fumesTotal volume 100%, H2The O content is 5 to 20%, and may be, for example, 5%, 6%, 10%, 15% or 20%.
The Pt-Mn bimetallic catalyst provided by the invention has a good catalytic oxidation effect on CO in industrial flue gas, and when the industrial flue gas contains 10% of H2O and no SO2In the process, the CO removal rate can reach more than 90 percent; when the industrial flue gas contains 10 percent of H2O and 500ppm SO2When the catalyst is used, the CO removal rate is over 78 percent, and the catalyst has good water resistance and sulfur resistance.
Compared with the prior art, the invention has the following beneficial effects:
(1) in the invention, TiO is firstly added2The carrier is soaked in a small amount of Mn source solution and then roasted, compared with the traditional catalyst, because the content of Mn element is less, the carrier can be uniformly distributed on the premise of TiO2Reserving a space on the surface of the carrier to ensure that a Pt elementary substance and/or Pt oxide and TiO obtained after the subsequent Pt source impregnation and roasting are ensured2Contact of the support, favouring TiO2The Pt and Mn on the surface of the carrier are alternately arranged, so that the synergistic effect of the Pt and the Mn is better exerted, and better water-resistant and sulfur-resistant performance is obtained.
(2) The Pt-Mn bimetallic catalyst of the invention uses TiO2The carrier is a Pt simple substance and/or oxide of Pt as a first active component, the manganese oxide as a second active component, and the synergistic effect of the two active components obviously improves the sulfur resistance of the Pt-Mn bimetallic catalyst, reduces the contents of the two active components and has higher CO oxidation efficiency.
(3) The preparation method of the Pt-Mn bimetallic catalyst is simple and easy to operate, and has good repeatability.
Drawings
FIG. 1 is a schematic diagram of a Pt-Mn bimetallic catalyst according to one embodiment of the present invention.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
The embodiment of the invention provides a preparation method of a low-load Pt-Mn bimetallic catalyst for CO oxidation, the preparation process is schematically shown in figure 1, and the preparation method comprises the following steps:
(1) adding TiO into the mixture2Soaking the carrier in a Mn source solution, and roasting to obtain a manganese-titanium agent;
(2) dipping the manganese-titanium agent obtained in the step (1) in a Pt source solution, and roasting to obtain a Pt-Mn bimetallic catalyst;
wherein the content of Mn element in the Pt-Mn bimetallic catalyst is 0.10-0.80 wt% based on 100 wt% of the Pt-Mn bimetallic catalyst.
In some embodiments, the content of the Mn element in the Pt-Mn bimetallic catalyst is 0.40 to 0.60 wt% based on 100 wt% of the mass of the Pt-Mn bimetallic catalyst.
In some embodiments, the content of the Pt element in the Pt-Mn bimetallic catalyst is 0.02 to 0.20 wt%, preferably 0.08 to 0.12 wt%, based on 100 wt% of the mass of the Pt-Mn bimetallic catalyst.
In some embodiments, the TiO of step (1)2The carrier is anatase type TiO2。
In some embodiments, the Mn source of step (1) comprises any one of manganese nitrate, manganese sulfate, or manganese chloride, or a combination of at least two thereof.
In some embodiments, the time for said impregnating in step (1) is 2 to 24 hours.
In some embodiments, after the impregnating and before the roasting in the step (1), the preparation method further comprises drying, wherein the drying temperature is 80-120 ℃, and the drying time is 2-5 h.
In some embodiments, the temperature of the calcination in step (1) is 450-600 ℃.
In some embodiments, the calcination in step (1) is for a time period of 2 to 10 hours.
In some embodiments, the Pt source of step (2) comprises any one of platinum nitrate, platinum chloride, or chloroplatinic acid, or a combination of at least two thereof.
In some embodiments, the time for said impregnating in step (2) is from 2 to 24 hours.
In some embodiments, after the impregnating and before the roasting in the step (2), the preparation method further comprises drying, wherein the drying temperature is 80-120 ℃, and the drying time is 2-5 h.
In some embodiments, the temperature of the calcination in step (2) is 450-600 ℃.
In some embodiments, the calcination time in step (2) is from 2 to 10 hours.
In some embodiments, there is provided a Pt-Mn bimetallic catalyst prepared as described, including TiO2A carrier, a first active component and a second active component;
the first active component is a Pt simple substance and/or an oxide of Pt, and the second active component is a manganese oxide.
The following are typical but non-limiting examples of the invention:
example 1
This example provides a low loading Pt-Mn bimetallic catalyst for CO oxidation in the anatase TiO form2The carrier is a first active component, the first active component is Pt and oxides of Pt, and the second active component is manganese oxide; the content of Mn element in the Pt-Mn bimetallic catalyst is 0.80 wt% and the content of Pt element in the Pt-Mn bimetallic catalyst is 0.08 wt% based on 100 wt% of the Pt-Mn bimetallic catalyst.
The embodiment also provides a preparation method of the Pt-Mn bimetallic catalyst, which comprises the following steps:
(1) manganese nitrate is prepared into solution, anatase TiO is added2Dipping for 5h, drying for 5h at 120 ℃, and roasting for 4h at 500 ℃ to obtain a manganese-titanium agent;
(2) preparing chloroplatinic acid into a solution, adding the manganese-titanium agent obtained in the step (1) to dip for 4 hours, drying at 100 ℃ for 4 hours, and roasting at 500 ℃ for 4 hours to obtain the Pt-Mn bimetallic catalyst.
Example 2
This example provides a low loading Pt-Mn bimetallic catalyst for CO oxidation in the anatase TiO form2The carrier is a first active component, the first active component is Pt and oxides of Pt, and the second active component is manganese oxide; the content of Mn element in the Pt-Mn bimetallic catalyst is 0.50 wt% and the content of Pt element in the Pt-Mn bimetallic catalyst is 0.10 wt% based on 100 wt% of the Pt-Mn bimetallic catalyst.
The embodiment also provides a preparation method of the Pt-Mn bimetallic catalyst, which comprises the following steps:
(1) manganese nitrate is prepared into solution, anatase TiO is added2Dipping for 5h, drying for 5h at 120 ℃, and roasting for 4h at 500 ℃ to obtain a manganese-titanium agent;
(2) preparing chloroplatinic acid into a solution, adding the manganese-titanium agent obtained in the step (1) to dip for 4 hours, drying at 100 ℃ for 4 hours, and roasting at 500 ℃ for 4 hours to obtain the Pt-Mn bimetallic catalyst.
Example 3
This example provides a low loading Pt-Mn bimetallic catalyst for CO oxidation in the anatase TiO form2The carrier is a first active component, the first active component is Pt and oxides of Pt, and the second active component is manganese oxide; the content of Mn element in the Pt-Mn bimetallic catalyst is 0.10 wt%, and the content of Pt element in the Pt-Mn bimetallic catalyst is 0.20 wt%, wherein the mass of the Pt-Mn bimetallic catalyst is 100 wt%.
The embodiment also provides a preparation method of the Pt-Mn bimetallic catalyst, which comprises the following steps:
(1) manganese nitrate is prepared into solution, anatase TiO is added2Dipping for 5h, drying for 5h at 120 ℃, and roasting for 4h at 500 ℃ to obtain a manganese-titanium agent;
(2) preparing chloroplatinic acid into a solution, adding the manganese-titanium agent obtained in the step (1) to dip for 4 hours, drying at 100 ℃ for 4 hours, and roasting at 500 ℃ for 4 hours to obtain the Pt-Mn bimetallic catalyst.
Example 4
This example provides a Pt-Mn bimetallic catalyst that is based on anatase TiO2As a carrier, theOne active component is Pt and oxides of Pt, and the second active component is manganese oxide; the mass of the Pt-Mn bimetallic catalyst is 100 wt%, the percentage content of Mn element in the Pt-Mn bimetallic catalyst is 0.60 wt%, and the percentage content of Pt element in the Pt-Mn bimetallic catalyst is 0.02 wt%.
The embodiment also provides a preparation method of the Pt-Mn bimetallic catalyst, which comprises the following steps:
(1) preparing manganese chloride into solution, adding anatase TiO2Dipping for 10h, drying at 80 ℃ for 4h, and roasting at 400 ℃ for 2h to obtain a manganese-titanium agent;
(2) preparing platinum nitrate into a solution, adding the manganese-titanium catalyst obtained in the step (1) to dip for 12 hours, drying at 90 ℃ for 5 hours, and roasting at 400 ℃ for 3 hours to obtain the Pt-Mn bimetallic catalyst.
Comparative example 1
The present comparative example is different from example 1 in that the operation of step (2) is not performed, i.e., the Pt-Mn bimetallic catalyst does not include the first active component, the catalyst obtained in the present comparative example is a Mn-based catalyst having a Mn element content of 0.88 wt% based on 100 wt% of the mass of the Mn-based catalyst, and the rest is the same as example 1.
Comparative example 2
The comparative example differs from example 1 in that the operation of step (1) is not performed, i.e., the second active component is not included in the Pt-Mn bimetallic catalyst, the catalyst obtained in the comparative example is a Pt-based catalyst having a Pt element content of 0.88 wt% based on 100 wt% by mass of the Pt-based catalyst, and the rest is the same as example 1.
Comparative example 3
This comparative example is different from example 1 in that the content of Mn element in the Pt-Mn bimetallic catalyst is 1 wt%, and the rest is the same as example 1.
Comparative example 4
The present comparative example provides a Pt-Mn bimetallic catalyst, the preparation method of which comprises the steps of:
manganese nitrate and chloroplatinic acid are prepared into solutionAdding anatase type TiO into the solution2Dipping for 5h, drying for 5h at 120 ℃, and roasting for 4h at 500 ℃ to obtain the Pt-Mn bimetallic catalyst.
The rest is the same as in example 1.
Comparative example 5
The present comparative example provides a Pt-Mn bimetallic catalyst, the preparation method of which comprises the steps of:
(1) preparing chloroplatinic acid into solution, adding anatase type TiO2Dipping for 5h, drying for 5h at 120 ℃, and roasting for 4h at 500 ℃ to obtain a Pt-based catalyst;
(2) preparing manganese nitrate into a solution, adding the Pt-based catalyst obtained in the step (1) to dip for 4 hours, drying for 4 hours at 100 ℃, and roasting for 4 hours at 500 ℃ to obtain the Pt-Mn bimetallic catalyst.
The rest is the same as in example 1.
Application example 1
The Pt-Mn bimetallic catalyst obtained in example 1 is used for CO oxidation performance test of industrial flue gas, the concentration of CO in simulated flue gas is 7000ppm, and the simulated flue gas also contains 16% of O based on the total volume of the simulated flue gas being 100%2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Application example 2
The Pt-Mn bimetallic catalyst obtained in example 1 is used for CO oxidation performance test of industrial flue gas, and CO concentration in simulated flue gas is 7000ppm, SO2The concentration is 50ppm, and the simulated smoke gas also contains 16 percent of O based on the total volume of the simulated smoke gas as 100 percent2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Application example 3
The Pt-Mn bimetallic catalyst obtained in example 1 is used for CO oxidation performance test of industrial flue gas, and CO concentration in simulated flue gas is 7000ppm, SO2The concentration is 500ppm, and the total volume of the simulated smoke isThe simulated smoke also contains 16 percent of O based on 100 percent2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Application example 4
The Pt-Mn bimetallic catalyst obtained in example 2 is used for CO oxidation performance test of industrial flue gas, the concentration of CO in simulated flue gas is 7000ppm, and the simulated flue gas also contains 16% of O based on the total volume of the simulated flue gas being 100%2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Application example 5
The Pt-Mn bimetallic catalyst obtained in example 2 is used for CO oxidation performance test of industrial flue gas, and CO concentration in simulated flue gas is 7000ppm, SO2The concentration is 50ppm, and the simulated smoke gas also contains 16 percent of O based on the total volume of the simulated smoke gas as 100 percent2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Application example 6
The Pt-Mn bimetallic catalyst obtained in example 2 is used for CO oxidation performance test of industrial flue gas, and CO concentration in simulated flue gas is 7000ppm, SO2The concentration is 500ppm, and the simulated smoke gas also contains 16 percent of O based on the total volume of the simulated smoke gas as 100 percent2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Application example 7
The Pt-Mn bimetallic catalyst obtained in example 3 is used for CO oxidation performance test of industrial flue gas, the concentration of CO in simulated flue gas is 7000ppm, and the simulated flue gas also contains 16% of O based on the total volume of the simulated flue gas being 100%2And 10% of H2O，N2To be loadedGas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Application example 8
The Pt-Mn bimetallic catalyst obtained in example 3 is used for CO oxidation performance test of industrial flue gas, and CO concentration in simulated flue gas is 7000ppm, SO2The concentration is 50ppm, and the simulated smoke gas also contains 16 percent of O based on the total volume of the simulated smoke gas as 100 percent2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Application example 9
The Pt-Mn bimetallic catalyst obtained in example 3 is used for CO oxidation performance test of industrial flue gas, and CO concentration in simulated flue gas is 7000ppm, SO2The concentration is 500ppm, and the simulated smoke gas also contains 16 percent of O based on the total volume of the simulated smoke gas as 100 percent2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Application example 10
The Pt-Mn bimetallic catalyst obtained in example 4 is used for CO catalytic oxidation performance test of industrial flue gas, the concentration of CO in simulated flue gas is 7000ppm, and the simulated flue gas also contains 16% of O based on the total volume of the simulated flue gas being 100%2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of the CO catalytic oxidation performance test are shown in Table 1.
Application example 11
The Pt-Mn bimetallic catalyst obtained in example 4 is used for CO catalytic oxidation performance test of industrial flue gas, and the concentration of CO in simulated flue gas is 7000ppm and SO2The concentration is 50ppm, and the simulated smoke gas also contains 16 percent of O based on the total volume of the simulated smoke gas as 100 percent2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of the CO catalytic oxidation performance test are shown in Table 1.
Application example 12
The Pt-Mn bimetallic catalyst obtained in example 4 is used for CO catalytic oxidation performance test of industrial flue gas, and the concentration of CO in simulated flue gas is 7000ppm and SO2The concentration is 500ppm, and the simulated smoke gas also contains 16 percent of O based on the total volume of the simulated smoke gas as 100 percent2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of the CO catalytic oxidation performance test are shown in Table 1.
Comparative example 1 was used
The Mn-based catalyst obtained in the comparative example 1 is used for testing the CO oxidation performance of industrial flue gas, the concentration of CO in simulated flue gas is 7000ppm, and the simulated flue gas also contains 16% of O based on the total volume of the simulated flue gas being 100%2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Comparative example 2 was used
The Mn-based catalyst obtained in the comparative example 1 is used for testing the CO oxidation performance of industrial flue gas, and the CO concentration in simulated flue gas is 7000ppm and SO2The concentration is 50ppm, and the simulated smoke gas also contains 16 percent of O based on the total volume of the simulated smoke gas as 100 percent2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Comparative example 3 of application
The Mn-based catalyst obtained in the comparative example 1 is used for testing the CO oxidation performance of industrial flue gas, and the CO concentration in simulated flue gas is 7000ppm and SO2The concentration is 500ppm, and the simulated smoke gas also contains 16 percent of O based on the total volume of the simulated smoke gas as 100 percent2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3Catalytic oxidation in a/h atmosphere with CO oxygenThe results of the chemical property test are shown in table 1.
Comparative example 4 of application
The Pt-based catalyst obtained in the comparative example 2 is used for testing the CO oxidation performance of industrial flue gas, the concentration of CO in the simulated flue gas is 7000ppm, and the simulated flue gas also contains 16% of O based on the total volume of the simulated flue gas being 100%2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Comparative example 5 of application
The Pt-based catalyst obtained in the comparative example 2 is used for testing the CO oxidation performance of industrial flue gas, and the concentration of CO in simulated flue gas is 7000ppm and SO2The concentration is 50ppm, and the simulated smoke gas also contains 16 percent of O based on the total volume of the simulated smoke gas as 100 percent2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Comparative example 6 of application
The Pt-based catalyst obtained in the comparative example 2 is used for testing the CO oxidation performance of industrial flue gas, and the concentration of CO in simulated flue gas is 7000ppm and SO2The concentration is 500ppm, and the simulated smoke gas also contains 16 percent of O based on the total volume of the simulated smoke gas as 100 percent2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Comparative example 7 was used
The Pt-Mn bimetallic catalyst obtained in the comparative example 3 is used for testing the CO oxidation performance of industrial flue gas, the concentration of CO in the simulated flue gas is 7000ppm, and the simulated flue gas also contains 16% of O based on the total volume of the simulated flue gas being 100%2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Comparative example 8 of application
The Pt-Mn bimetallic catalyst obtained in the comparative example 3 is used for testing the CO oxidation performance of industrial flue gas, and the concentration of CO in simulated flue gas is 7000ppm and SO2The concentration is 50ppm, and the simulated smoke gas also contains 16 percent of O based on the total volume of the simulated smoke gas as 100 percent2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Comparative example 9 of application
The Pt-Mn bimetallic catalyst obtained in the comparative example 3 is used for testing the CO oxidation performance of industrial flue gas, and the concentration of CO in simulated flue gas is 7000ppm and SO2The concentration is 500ppm, and the simulated smoke gas also contains 16 percent of O based on the total volume of the simulated smoke gas as 100 percent2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Comparative example 10 was used
The Pt-Mn bimetallic catalyst obtained in the comparative example 4 is used for CO oxidation of industrial flue gas, the concentration of CO in the simulated flue gas is 7000ppm, and the simulated flue gas also contains 16% of O based on the total volume of the simulated flue gas being 100%2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Comparative example 11 was used
The Pt-Mn bimetallic catalyst obtained in the comparative example 4 is used for CO oxidation of industrial flue gas, and the concentration of CO in simulated flue gas is 7000ppm and SO2The concentration is 50ppm, and the simulated smoke gas also contains 16 percent of O based on the total volume of the simulated smoke gas as 100 percent2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Comparative example 12 was used
Pt-Mn bimetallic catalyst obtained in comparative example 4The chemical agent is used for CO oxidation of industrial flue gas, and the concentration of CO in simulated flue gas is 7000ppm and SO2The concentration is 500ppm, and the simulated smoke gas also contains 16 percent of O based on the total volume of the simulated smoke gas as 100 percent2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Comparative example 13 of application
The Pt-Mn bimetallic catalyst obtained in the comparative example 5 is used for CO oxidation of industrial flue gas, the concentration of CO in the simulated flue gas is 7000ppm, and the simulated flue gas also contains 16% of O based on the total volume of the simulated flue gas being 100%2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Comparative example 14 of application
The Pt-Mn bimetallic catalyst obtained in the comparative example 5 is used for CO oxidation of industrial flue gas, and the concentration of CO in simulated flue gas is 7000ppm and SO2The concentration is 50ppm, and the simulated smoke gas also contains 16 percent of O based on the total volume of the simulated smoke gas as 100 percent2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Comparative example 15 was used
The Pt-Mn bimetallic catalyst obtained in the comparative example 5 is used for CO oxidation of industrial flue gas, and the concentration of CO in simulated flue gas is 7000ppm and SO2The concentration is 500ppm, and the simulated smoke gas also contains 16 percent of O based on the total volume of the simulated smoke gas as 100 percent2And 10% of H2O，N2Is used as carrier gas; at 240 ℃ of the catalytic oxidation furnace, the flue gas flow rate is 1000Nm3The catalytic oxidation is carried out in the atmosphere of/h, and the results of CO oxidation performance tests are shown in Table 1.
Table 1 shows the results of the CO oxidation performance tests of application examples 1 to 12 and application comparative examples 1 to 15, in which the CO removal rate is the ratio of the difference between the CO concentration before catalytic oxidation and the CO concentration after catalytic oxidation to the CO concentration before catalytic oxidation.
TABLE 1
Figure BDA0003258773630000181
Figure BDA0003258773630000191
It can be seen from the above examples 1-4 and application examples 1-12 that the Pt-Mn bimetallic catalyst provided by the present invention has high water and sulfur resistance, CO oxidation efficiency and stability.
As can be seen from comparison between application example 4 and application examples 1 and 7, the Pt-Mn bimetallic catalyst has the most appropriate contents of Mn element and Pt element, and when the Mn element content is 0.50 wt% and the Pt element content is 0.10 wt%, the Pt-Mn bimetallic catalyst has better CO oxidation efficiency and higher CO removal rate; meanwhile, the comparison of the application examples 5-6 with the application examples 2-3 and the application examples 8-9 shows that the appropriate content of Mn element and Pt element is also beneficial to improving the water-resistant and sulfur-resistant performance of the Pt-Mn bimetallic catalyst, and when the simulated flue gas contains 10% of H2O and a certain amount of SO2In the case of application examples 5 to 6, the sulfur resistance was better and the stability was higher at 50ppm and 500ppm of SO2The removal rate of CO under the concentration is higher than that of the application examples 2-3 and 8-9.
As can be seen from comparison between application example 1 and application comparative examples 1 and 4, the CO removal rate of the catalyst containing only the first active component or the second active component is significantly reduced as compared with the Pt — Mn bimetallic catalyst provided by the present invention; meanwhile, as can be seen from the comparison between application examples 2 to 3 and application comparative examples 5 to 6, when the Pt-Mn bimetallic catalyst does not contain the first group of active components or the second group of active components, the sulfur resistance effect of the catalyst is along with the simulation of SO in flue gas2The concentration increase is also obviously reduced, the CO removal rate is obviously reduced, and the sulfur-resistant effect of the Pt-Mn bimetallic catalyst provided by the invention cannot be achieved.
By application example 1 and application control example 7, application examples 2 to 3, and applicationAs is clear from the comparison of comparative examples 8 to 9, the content of Mn element in the Pt-Mn bimetallic catalyst cannot be made too high, and when the content of Mn element is made too high, it tends to be liable to occur in TiO2A larger coating layer is formed on the surface of the carrier, so that most of Pt element is directly contacted with Mn element, and the Pt element and TiO are blocked2Contact of support and TiO2The sulfur resistance of the support was exerted, and therefore, comparative examples 7 to 9 were applied to different SO' s2The removal rate of CO at the concentration is lower than that of the invention.
As can be seen from the comparison between application example 1 and application control example 10, and between application examples 2 to 3 and application control examples 11 to 12, the preparation method of the Pt-Mn bimetallic catalyst affects the CO oxidation efficiency and the sulfur resistance of the Pt-Mn bimetallic catalyst obtained by the stepwise impregnation method in example 1, in which TiO is first introduced2The carrier is soaked in a manganese nitrate solution for roasting and then soaked in a chloroplatinic acid solution for roasting, so that the first active component and the second active component are favorably roasted in TiO2The arrangement on the carrier plays the synergistic effect of Pt and Mn, has better CO oxidation efficiency and sulfur resistance, and therefore, the carrier is applied to different SO in examples 1-32The CO removal rate tested at concentration is relatively high; comparative example 4 direct preparation of TiO2The carrier is immersed in the mixed solution of manganese nitrate and chloroplatinic acid, and the CO oxidation efficiency and the sulfur resistance of the prepared Pt-Mn bimetallic catalyst can not reach the effect of the invention.
As can be seen from the comparison of application example 1 with application control example 13, application examples 2 to 3, and application control examples 14 to 15, the impregnation sequence of the Mn source solution and the Pt source solution affects the CO oxidation efficiency and the sulfur resistance of the prepared Pt-Mn bimetallic catalyst, so that a part of the Pt active species is covered with the Mn species, thereby affecting the catalytic activity and the sulfur resistance thereof, and thus the sulfur resistance and the CO oxidation efficiency of the Pt-Mn bimetallic catalyst of comparative example 5 are inferior to those of example 1.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.

Claims (10)

1. A preparation method of a Pt-Mn bimetallic catalyst is characterized by comprising the following steps:
(1) adding TiO into the mixture2Soaking the carrier in a Mn source solution, and roasting to obtain a manganese-titanium agent;
(2) dipping the manganese-titanium agent obtained in the step (1) in a Pt source solution, and roasting to obtain a Pt-Mn bimetallic catalyst;
wherein the content of Mn element in the Pt-Mn bimetallic catalyst is 0.10-0.80 wt% based on 100 wt% of the Pt-Mn bimetallic catalyst.
2. The preparation method according to claim 1, wherein the content of the Mn element in the Pt-Mn bimetallic catalyst is 0.40 to 0.60 wt% based on 100 wt% of the mass of the Pt-Mn bimetallic catalyst.
3. The method according to claim 1 or 2, wherein the content of the Pt element in the Pt-Mn bimetallic catalyst is 0.02 to 0.20 wt%, preferably 0.08 to 0.12 wt%, based on 100 wt% of the mass of the Pt-Mn bimetallic catalyst.
4. The method according to any one of claims 1 to 3, wherein the TiO in the step (1)2The carrier is anatase type TiO2；
Preferably, the Mn source of step (1) comprises any one of manganese nitrate, manganese sulfate or manganese chloride or a combination of at least two thereof.
5. The production method according to any one of claims 1 to 4, wherein the time for the impregnation in step (1) is 2 to 24 hours;
preferably, after the impregnation and before the roasting in the step (1), the preparation method further comprises drying, wherein the drying temperature is 80-120 ℃, and the drying time is 2-5 h;
preferably, the roasting temperature in the step (1) is 450-600 ℃;
preferably, the roasting time in the step (1) is 2-10 h.
6. The production method according to any one of claims 1 to 5, wherein the Pt source of step (2) comprises any one of platinum nitrate, platinum chloride or chloroplatinic acid or a combination of at least two thereof.
7. The production method according to any one of claims 1 to 6, wherein the time for the impregnation in step (2) is 2 to 24 hours;
preferably, after the impregnation and before the roasting in the step (2), the preparation method further comprises drying, wherein the drying temperature is 80-120 ℃, and the drying time is 2-5 h;
preferably, the roasting temperature in the step (2) is 450-600 ℃;
preferably, the roasting time in the step (2) is 2-10 h.
8. The method of any one of claims 1 to 7, comprising the steps of:
(1) preparing Mn source solution, adding anatase TiO2Dipping for 2-24h, drying for 2-5h at 80-120 ℃, and then roasting for 2-10h at 450-600 ℃ to obtain a manganese-titanium agent;
(2) preparing a Pt source solution, adding the manganese-titanium agent in the step (1) to dip for 2-24h, drying at 80-120 ℃ for 2-5h, and then roasting at 450-600 ℃ for 2-10h to obtain the Pt-Mn bimetallic catalyst.
9. A Pt-Mn bimetallic catalyst obtained by the process according to any one of claims 1 to 8, characterized in that it comprises TiO2A carrier, a first active component and a second active component;
the first active component is a Pt simple substance and/or an oxide of Pt, and the second active component is a manganese oxide.
10. The application of the Pt-Mn bimetallic catalyst of claim 9 in the field of CO oxidation treatment of industrial flue gas;
preferably, the concentration of CO in the industrial flue gas is 7000-9000ppm and SO based on the total volume of the industrial flue gas2In a concentration of 0 to 500ppm, preferably 50 to 500 ppm;
h in the industrial flue gas is calculated by taking the total volume of the industrial flue gas as 100 percent2The content of O is 5-20%.
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