CN113893844A - NH with ethane as auxiliary reducing agent3-SCR denitration catalyst and preparation method thereof - Google Patents

NH with ethane as auxiliary reducing agent3-SCR denitration catalyst and preparation method thereof Download PDF

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CN113893844A
CN113893844A CN202111180395.4A CN202111180395A CN113893844A CN 113893844 A CN113893844 A CN 113893844A CN 202111180395 A CN202111180395 A CN 202111180395A CN 113893844 A CN113893844 A CN 113893844A
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sio
tio
ethane
scr denitration
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范宏
侍大海
许琦
瞿赞
乐成芝
宋夫交
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Yancheng Institute of Technology
Yancheng Lanfeng Environmental Engineering Technology Co Ltd
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    • B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8621—Removing nitrogen compounds
    • B01D53/8625—Nitrogen oxides
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    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
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    • B01D2251/206—Ammonium compounds
    • B01D2251/2062—Ammonia
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract

The invention discloses NH taking ethane as an auxiliary reducing agent3Preparing a mixed solution of tetrabutyl titanate and ethyl orthosilicate according to a certain molar ratio, dropwise adding the mixed solution into deionized water under strong stirring, stirring and ultrasonically dispersing, placing the sol in a dark place for aging for 24 hours, heating and evaporating at a constant temperature of 80 ℃ in a water bath for 12 hours, and then drying and roasting; ultrasonically dipping by using sulfuric acid, washing by using deionized water, drying at 80 ℃, roasting at 550 ℃ for 2 hours, grinding and screening to obtain the composite carrier TiO2‑SiO2Weighing the composite carrier and cerium nitrate, adding deionized water with the same volume, uniformly stirring for 12 h, drying and calcining to obtain 10wt% CeO2/TiO2‑SiO2A catalyst.

Description

NH with ethane as auxiliary reducing agent3-SCR denitration catalyst and preparation method thereof
Technical Field
The invention belongs to the technical field of SCR (selective catalytic reduction) flue gas denitration, and particularly relates to NH taking ethane as an auxiliary reducing agent3-SCR denitration catalyst and a preparation method thereof.
Background
Nitrogen oxides (NOx) are one of the major atmospheric pollutants, and their emissions not only cause acid precipitation and affect human health, but also exacerbate photochemical smog and urban haze pollution. Since NOx is relatively stable in chemical properties and can be transported in the atmosphere for a long time and over a long distance, the problem of regional atmospheric pollution is exacerbated, and it is planned to clearly specify NOx as a control target of the total amount of pollution and to perform ultra-low emission. Although the blue sky guard war is won and the concentration of NOx in the atmosphere is obviously reduced, the NOx treatment is still required to be enhanced, and the power is contributed to the joint defense and joint control of the atmospheric pollution.
The NOx emission source is mainly coal-fired flue gas, the research and development and industrialization of a low-nitrogen combustion technology and a Selective Catalytic Reduction (SCR) denitration technology have been rapidly developed in recent ten years, the self-design, the manufacture, the installation and the debugging are realized, and the NOx emission source becomes a first-choice and mainstream technology for controlling the NOx in the thermal power industry in China. Low NOx combustion technology is a technology that improves combustion equipment or controls combustion conditions to reduce the concentration of NOx in the combustion exhaust. The main factors influencing the generation of NOx in the combustion process are the combustion temperature, the retention time of the flue gas and the O in the flue gas2NHi, CHi, CO, C and H2The concentration, the degree of mixing, and the like, and therefore, any techniques for suppressing the generation of NOx by changing the above combustion conditions are low-nitrogen combustion techniques.
SCR is the most mature flue gas denitration technology at present, and is a denitration method after a furnace, and the principle of the method is that NOx is selectively reduced into nitrogen and water by using a reducing agent under the action of a catalyst. The reducing agent for SCR denitration comprises ammonia water, urea, CO, hydrocarbons and the like, wherein the ammonia water and the urea are mature in technology and most widely applied as the reducing agent, and the ammonia water or the urea is adopted as the reducing agent in the domestic large-scale coal-fired boiler flue gas SCR denitration system, so that the defect that the reaction temperature is high and the SCR denitration system is not suitable for low-temperature flue gas denitration is overcome. Hydrocarbon gases have received much attention because of their good low temperature activity and relatively low cost.
Disclosure of Invention
Ethane has a wide temperature range of activity if at NH3On the basis of SCR, ethane is introduced as an auxiliary reducing agent, so that the activity of the catalyst at low temperature is expected to be improved. Meanwhile, in the aspect of engineering implementation, only a reducing agent storage and supply system in the original SCR denitration equipment needs to be modified, so that the cost is low, and the feasibility is realized in economy. Aiming at the defects of the prior art, the invention provides NH taking ethane as an auxiliary reducing agent3-SCR denitration catalyst and preparation method thereof to realize NO at low temperatureXThe removal is efficient.
NH with ethane as auxiliary reducing agent3SCR denitration catalyst, CeO2/TiO2-SiO2From 10% by weight of CeO2And 90wt% TiO2-SiO2And (4) forming.
NH with ethane as auxiliary reducing agent3-a method for preparing an SCR denitration catalyst, comprising the steps of:
step 1, weighing tetrabutyl titanate and tetraethoxysilane according to the molar ratio n (Ti) to n (Si) =1-4:1, and mixing and stirring the tetrabutyl titanate and tetraethoxysilane uniformly to obtain a mixed solution;
step 2, dropwise adding the mixed solution obtained in the step 1 into deionized water under the stirring condition, stirring for 1 hour to obtain white emulsion, and performing ultrasonic dispersion on the white emulsion to obtain white sol A;
and 3, aging the white sol A in a dark place for 24 hours, taking out, heating and evaporating at the constant temperature of 80 ℃ in a water bath kettle for 12 hours, and then drying and roasting to obtain the composite carrier TiO2-SiO2A precursor of (a);
step 4, carrying out TiO recombination on the carrier obtained in the step 32-SiO2The precursor is dipped in 0.25 mol/L sulfuric acid, ultrasonic treatment is carried out for 2 hours, then the precursor is washed for 3 to 5 times by deionized water, dried at the temperature of 80 ℃ and roasted at the temperature of 550 ℃ for 2 hours, and then grinding and screening are carried out to obtain the composite carrier TiO2-SiO2；
Step 5, weighing the composite carrier TiO obtained in the step 42-SiO2And cerium nitrate, composite carrier TiO2-SiO2Adding deionized water with the same volume as cerium element at a mass ratio of 10:1, uniformly stirring for 12 h, drying and calcining to obtain CeO2/TiO2-SiO2A catalyst.
In the step 2, the ultrasonic dispersion time of the white emulsion is 1 h.
The heating rate during the roasting in the step 4 is 5 ℃/min.
In the step 4, the dosage of the sulfuric acid is as follows: TiO composite carrier per gram2-SiO2The precursor of (a) corresponds to 5 ml of sulfuric acid; roasting to obtain composite carrier TiO2-SiO2Grinding and sieving to 50-60 mesh.
In the step 5, the drying temperature is 110 ℃, and the calcination is carried out for 4 hours at the temperature of 400 ℃.
Compared with the prior art, the invention has the following advantages: (1) CeO (CeO)2/TiO2-SiO2Catalyst in NH3Higher activity and lower cost in SCR reactions; (2) ethane has a wide range of active temperatures, at NH3On the basis of SCR, ethane is introduced as an auxiliary reducing agent, so that the activity of the catalyst at low temperature is improved; (3) in the aspect of engineering implementation, only a reducing agent storage and supply system in the original SCR denitration equipment needs to be modified, so that the cost is low, and the feasibility is realized economically.
Drawings
FIG. 1 shows the XRD pattern of the catalyst (a CeO)2/TiO2-SiO2-1, b CeO2/TiO2-SiO2-2, c CeO2/TiO2-SiO2-3, d CeO2/TiO2-SiO2-4)。
Figure 2 NO conversion versus temperature for different catalysts.
FIG. 3 catalyst CeO2/TiO2-SiO2-3 curves of NO conversion with temperature under different reducing atmospheres.
Detailed Description
The present invention will be further described with reference to specific examples and comparative examples. The present invention will be better understood from the following examples. However, those skilled in the art will readily appreciate that the specific material ratios, process conditions and results thereof described in the examples are illustrative only and should not be taken as limiting the invention as detailed in the claims.
Example 1
(1) Weighing tetrabutyl titanate and tetraethoxysilane according to the molar ratio of n (Ti) to n (Si) to 1:1, and uniformly mixing and stirring to obtain a mixed solution;
(2) dropwise adding the mixed solution into deionized water under strong stirring, continuously stirring for 1 h to obtain white emulsion, and dispersing the emulsion in an ultrasonic oscillation tank for 1 h to obtain white sol;
(3) aging the sol in the dark for 24 h, taking out, heating and evaporating at a constant temperature of 80 ℃ in a water bath for 12 h, drying the product at 80 ℃, roasting at 550 ℃ for 2 h, wherein the heating rate is 5 ℃/min;
(4) ultrasonically dipping for 2 h (5 ml/g carrier) by using 0.25 mol/L sulfuric acid, washing for 3-5 times by using deionized water, drying at 80 ℃, roasting for 2 h at 550 ℃, grinding and screening to 50-60 meshes to obtain the composite carrier TiO2-SiO2；
(5) Weighing TiO composite carrier according to the mass ratio of 10:12-SiO2And cerium nitrate, adding deionized water with the same volume, uniformly stirring for 12 h, drying at 110 ℃, calcining for 4 h at 400 ℃ to obtain 10wt% CeO2/TiO2-SiO2Catalyst, labelled CeO2/TiO2-SiO2-1。
Example 2
(1) Weighing tetrabutyl titanate and tetraethoxysilane according to the molar ratio of n (Ti) to n (Si) to 2:1, and uniformly mixing and stirring to obtain a mixed solution;
(2) dropwise adding the mixed solution into deionized water under strong stirring, continuously stirring for 1 h to obtain white emulsion, and dispersing the emulsion in an ultrasonic oscillation tank for 1 h to obtain white sol;
(3) aging the sol in the dark for 24 h, taking out, heating and evaporating at a constant temperature of 80 ℃ in a water bath for 12 h, drying the product at 80 ℃, roasting at 550 ℃ for 2 h, wherein the heating rate is 5 ℃/min;
(4) ultrasonically dipping for 2 h (5 ml/g carrier) by using 0.25 mol/L sulfuric acid, washing for 3-5 times by using deionized water, drying at 80 ℃, roasting for 2 h at 550 ℃, grinding and screening to 50-60 meshes to obtain the composite carrier TiO2-SiO2；
(5) Weighing the composite carrier and cerium nitrate according to the mass ratio of 10:1, adding deionized water with the same volume, uniformly stirring for 12 h, drying at 110 ℃, calcining at 400 ℃ for 4 h to obtain 10wt% CeO2/TiO2-SiO2Catalyst, labelled CeO2/TiO2-SiO2-2。
Example 3
(1) Weighing tetrabutyl titanate and tetraethoxysilane according to the molar ratio of n (Ti) to n (Si) to 3:1, and uniformly mixing and stirring to obtain a mixed solution;
(2) dropwise adding the mixed solution into deionized water under strong stirring, continuously stirring for 1 h to obtain white emulsion, and dispersing the emulsion in an ultrasonic oscillation tank for 1 h to obtain white sol;
(3) aging the sol in the dark for 24 h, taking out, heating and evaporating at a constant temperature of 80 ℃ in a water bath for 12 h, drying the product at 80 ℃, roasting at 550 ℃ for 2 h, wherein the heating rate is 5 ℃/min;
(4) ultrasonically dipping for 2 h (5 ml/g carrier) by using 0.25 mol/L sulfuric acid, washing for 3-5 times by using deionized water, drying at 80 ℃, roasting for 2 h at 550 ℃, grinding and screening to 50-60 meshes to obtain the composite carrier TiO2-SiO2；
(5) Weighing the composite carrier and the cerium nitrate according to the mass ratio of 10:1, adding deionized water with the same volume, uniformly stirring for 12 h, drying at 110 ℃, calcining for 4 h at 400 ℃,10wt% of CeO was obtained2/TiO2-SiO2Catalyst, labelled CeO2/TiO2-SiO2-3。
Example 4
(1) Weighing tetrabutyl titanate and tetraethoxysilane according to the molar ratio of n (Ti) to n (Si) to 4:1, and uniformly mixing and stirring to obtain a mixed solution;
(2) dropwise adding the mixed solution into deionized water under strong stirring, continuously stirring for 1 h to obtain white emulsion, and dispersing the emulsion in an ultrasonic oscillation tank for 1 h to obtain white sol;
(3) aging the sol in the dark for 24 h, taking out, heating and evaporating at a constant temperature of 80 ℃ in a water bath for 12 h, drying the product at 80 ℃, roasting at 550 ℃ for 2 h, wherein the heating rate is 5 ℃/min;
(4) ultrasonically dipping for 2 h (5 ml/g carrier) by using 0.25 mol/L sulfuric acid, washing for 3-5 times by using deionized water, drying at 80 ℃, roasting for 2 h at 550 ℃, grinding and screening to 50-60 meshes to obtain the composite carrier TiO2-SiO2；
(5) Weighing the composite carrier and cerium nitrate according to the mass ratio of 10:1, adding deionized water with the same volume, uniformly stirring for 12 h, drying at 110 ℃, calcining at 400 ℃ for 4 h to obtain 10wt% CeO2/TiO2-SiO2Catalyst, labelled CeO2/TiO2-SiO2-4。
Testing the NH of the catalyst in the temperature range of 150 ℃ and 500 DEG C3SCR denitration Performance and NH with ethane as an auxiliary reducing agent3-SCR denitration performance. NH of catalyst3SCR denitration performance is carried out in a tubular fixed bed reactor, the pipe diameter is 14 mm, and the simulated flue gas consists of 500 ppm NH3、500 ppm NO、3% O2Equilibrium gas N2The total flow of gas is 500 mL/min, the amount of the loaded catalyst is 0.60 mL respectively, and the space velocity is 50000 h-1. NH with ethane as co-reductant3SCR denitration Performance test 50ppm, 100ppm and 150 ppm of ethane were added to the simulated flue gas, respectively, with the other components and conditions being kept the same.
CeO2/TiO2-SiO2The XRD pattern of the catalyst is shown in figure 1, and the crystal forms of the sample respectively correspond to anatase TiO2The (101), (004), (200), (211), (204) crystal planes of (a). And, TiO2-SiO2CeO samples with relative proportions of 1:1, 2:12/TiO2-SiO2-1 and CeO2/TiO2-SiO2-2 presence of cubic fluorite CeO in XRD pattern2Characteristic diffraction peak of (2), but with TiO2-SiO2Increase in relative proportion, disappearance of the peak and TiO2The peak intensity in the vicinity of 2 θ =25 ° is reduced due to the active component CeO2With the support TiO2The interaction of (A) is enhanced to inhibit TiO2Grain growth, TiO estimated according to the Sheer equation in Table 12The average grains also confirmed this conclusion. In addition, SiO does not appear in an XRD pattern2Due to the fact that the silica exists mainly in an amorphous state.
TABLE 110% average crystallite size distribution of titanium dioxide (anatase) in CeO2/TiO2-SiO2 catalyst
Catalyst and process for preparing same Crystal face 2θ (°) FMWH (rad)a D (nm)b
CeO2/TiO2-SiO2(1:1) 101 25.22 0.01179 12.2
CeO2/TiO2-SiO2(2:1) 101 25.24 0.01251 11.5
CeO2/TiO2-SiO2(3:1) 101 25.30 0.01291 11.0
CeO2/TiO2-SiO2(4:1) 101 25.28 0.01453 9.80
a The full width at half maximum after the correction,b average crystal grain size
FIG. 2 shows CeO2/TiO2-SiO2NH of the catalyst at 150 ℃ and 500 DEG C3-SCR denitration performance map. As can be seen from the figure, the catalyst exhibited the best denitration activity at around 350 ℃. CeO (CeO)2/TiO2-SiO2The best performance of the-3 catalyst is 94.3%.
FIG. 3 shows a catalyst CeO2/TiO2-SiO2-3 curves of NO conversion with temperature under different reducing atmospheres. After addition of ethane as an auxiliary reductant, CeO2/TiO2-SiO2-3 at low temperature the NO conversion increases, the optimum denitration activity occurs near 300 ℃, the optimum denitration temperature decreases by 50 ℃, the optimum addition of ethane is 100ppm, and the optimum NO conversion for this case is 92.6%.

Claims (7)

1. NH with ethane as auxiliary reducing agent3SCR denitration catalyst, CeO2/TiO2-SiO2From 10% by weight of CeO2And 90wt% TiO2-SiO2And (4) forming.
2. NH with ethane as an auxiliary reductant as claimed in claim 13-a method for preparing an SCR denitration catalyst, comprising the steps of:
step 1, weighing tetrabutyl titanate and tetraethoxysilane according to the molar ratio n (Ti) to n (Si) =1-4:1, and mixing and stirring the tetrabutyl titanate and tetraethoxysilane uniformly to obtain a mixed solution;
step 2, dropwise adding the mixed solution obtained in the step 1 into deionized water under the stirring condition, stirring for 1 hour to obtain white emulsion, and performing ultrasonic dispersion on the white emulsion to obtain white sol A;
and 3, aging the white sol A in a dark place for 24 hours, taking out, heating and evaporating at the constant temperature of 80 ℃ in a water bath kettle for 12 hours, and then drying and roasting to obtain the composite carrier TiO2-SiO2A precursor of (a);
step 4, carrying out TiO recombination on the carrier obtained in the step 32-SiO2The precursor is dipped in 0.25 mol/L sulfuric acid, ultrasonic treatment is carried out for 2 hours, then the precursor is washed for 3 to 5 times by deionized water, dried at the temperature of 80 ℃ and roasted at the temperature of 550 ℃ for 2 hours, and then grinding and screening are carried out to obtain the composite carrier TiO2-SiO2；
Step 5, weighing the composite carrier TiO obtained in the step 42-SiO2And cerium nitrate, composite carrier TiO2-SiO2Adding deionized water with the same volume as cerium element at a mass ratio of 10:1, uniformly stirring for 12 h, drying and calcining to obtain CeO2/TiO2-SiO2A catalyst.
3. NH with ethane as an auxiliary reductant according to claim 23The preparation method of the SCR denitration catalyst is characterized in that in the step 2, the white emulsion is subjected to ultrasonic dispersion for 1 hour.
4. NH with ethane as an auxiliary reductant according to claim 23The preparation method of the SCR denitration catalyst is characterized in that the heating rate in the roasting in the step 4 is 5 ℃/min.
5. NH with ethane as an auxiliary reductant according to claim 23The preparation method of the SCR denitration catalyst is characterized in that in the step 4, the dosage of sulfuric acid is as follows: TiO composite carrier per gram2-SiO2The precursor of (a) corresponds to 5 ml of sulfuric acid; roasting to obtain composite carrier TiO2-SiO2Grinding and sieving to 50-60 mesh.
6. NH with ethane as an auxiliary reductant according to claim 23The preparation method of the SCR denitration catalyst is characterized in that in the step 5, the drying temperature is 110 ℃, and the calcination is carried out for 4 hours at the temperature of 400 ℃.
7. The application of the NH3-SCR denitration catalyst taking ethane as an auxiliary reducing agent according to claim 1 in NO conversion is used for assisting in realizing the NO removal rate of 92.6% at 300 ℃ by taking ethane as an auxiliary reduction auxiliary agent.
CN202111180395.4A 2021-10-11 2021-10-11 NH with ethane as auxiliary reducing agent3-SCR denitration catalyst and preparation method thereof Pending CN113893844A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115414923A (en) * 2022-09-19 2022-12-02 常州大学 Heterogeneous TiO for the synthesis of polycarbonate diols 2 /SiO 2 Catalyst and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102101048A (en) * 2011-01-25 2011-06-22 清华大学 Cerium-based denitration catalyst with titanium-silicon compound oxide as carrier and preparation and application thereof
CN103537279A (en) * 2013-10-15 2014-01-29 北京工业大学 Low temperature denitration catalytic addictive and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102101048A (en) * 2011-01-25 2011-06-22 清华大学 Cerium-based denitration catalyst with titanium-silicon compound oxide as carrier and preparation and application thereof
CN103537279A (en) * 2013-10-15 2014-01-29 北京工业大学 Low temperature denitration catalytic addictive and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115414923A (en) * 2022-09-19 2022-12-02 常州大学 Heterogeneous TiO for the synthesis of polycarbonate diols 2 /SiO 2 Catalyst and preparation method thereof
CN115414923B (en) * 2022-09-19 2024-02-13 常州大学 Heterogeneous TiO for synthesizing polycarbonate diol 2 /SiO 2 Catalyst and preparation method thereof

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