CN112264002A - SCR catalyst and modification method for zero-valent mercury oxidation capacity thereof - Google Patents
SCR catalyst and modification method for zero-valent mercury oxidation capacity thereof Download PDFInfo
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- CN112264002A CN112264002A CN202011305740.8A CN202011305740A CN112264002A CN 112264002 A CN112264002 A CN 112264002A CN 202011305740 A CN202011305740 A CN 202011305740A CN 112264002 A CN112264002 A CN 112264002A
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- valent mercury
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- 239000003054 catalyst Substances 0.000 title claims abstract description 62
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052753 mercury Inorganic materials 0.000 title claims abstract description 38
- 230000003647 oxidation Effects 0.000 title claims abstract description 17
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 17
- 238000002715 modification method Methods 0.000 title abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 50
- 238000002791 soaking Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000000178 monomer Substances 0.000 claims abstract description 16
- 238000007605 air drying Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 32
- 238000004321 preservation Methods 0.000 claims description 23
- 238000001816 cooling Methods 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 abstract description 11
- 239000003546 flue gas Substances 0.000 abstract description 11
- 229910000420 cerium oxide Inorganic materials 0.000 abstract description 4
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 abstract description 4
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 abstract description 4
- 238000013461 design Methods 0.000 abstract description 2
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 description 6
- 239000011148 porous material Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical group 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- 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
- B01D53/8665—Removing heavy metals or compounds thereof, e.g. mercury
-
- B01J35/56—
Abstract
The invention provides an SCR catalyst and a modification method of the SCR catalyst for zero-valent mercury oxidation capacity, which are reasonable in design, simple and effective and capable of enhancing the zero-valent mercury oxidation capacity of the SCR catalyst in flue gas. The modification method comprises the step of S1, placing the honeycomb SCR catalyst monomer in 1-2mol/L of Ce (NO)3)3Soaking in the solution; and S2, soaking fully, air-drying, and then calcining to obtain the modified catalyst. According to the modification method, on the basis of the original denitration catalyst, cerium nitrate can be attached to the denitration catalyst through soaking, cerium oxide is obtained through calcination, the oxidation capability of the catalyst is improved, and therefore zero-valent mercury can be better oxidized through cerium oxide during denitration to obtain divalent mercuryThe mercury is simple and efficient in operation method, and can meet the requirement of removing gaseous zero-valent mercury at present.
Description
Technical Field
The invention relates to modification of an SCR denitration catalyst in the thermal power industry, in particular to an SCR denitration catalyst and a modification method of the SCR denitration catalyst on zero-valent mercury oxidation capacity.
Background
Mercury is a trace element in coal, and the shape distribution of mercury in coal-fired flue gas is different due to different coal types. Mercury in coal-fired flue gas exists mainly in 3 forms: particulate mercury (Hg)p) Bivalent mercury (Hg)2+) Gaseous elemental mercury (Hg)0)。HgpThe mercury bonded on the surface of the particles can be removed by using dust removal equipment; hg is a mercury vapor2+Is easily soluble in water, can be removed in a wet desulphurization system, and Hg2+Part or all of the carbon particles in the flue gas can be adsorbed by the granular carbon, and the carbon particles adsorbed with mercury can be removed by dust removal equipment; gaseous Hg0Is insoluble in water, has extremely strong volatility, has long existence time in the atmosphere and long transmission distance, is difficult to be removed by the prior flue gas purification equipment, and is easy to form long-term pollution. Therefore, the mercury removal after combustion has great dependence on the form distribution of mercury in flue gas, and the difficulty is that Hg0To strengthen Hg removal0To HgpAnd Hg2+The conversion of (a) facilitates the removal of mercury.
Selective Catalytic Reduction (SCR) is the mainstream technology for denitration of coal-fired power plants in China, and the commercial SCR catalyst which is most widely applied at present is a metal oxide catalyst, and the main component of the catalyst is V2O5-WO3/TiO2. Researches find that part of Hg in flue gas passes through SCR catalyst0Will be oxidized to Hg2+The catalyst has a promoting effect on the removal of mercury in WFGD, but the prior response catalyst is mainly used for completing denitration, has insufficient oxidation capability on zero-valent mercury and cannot completely meet the removal requirement of the zero-valent mercury.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the SCR catalyst and the modification method of the SCR catalyst on the zero-valent mercury oxidation capacity, the design is reasonable, the method is simple and effective, and the oxidation capacity of the SCR catalyst on the zero-valent mercury in the flue gas is enhanced.
The invention is realized by the following technical scheme:
a method for modifying the zero-valent mercury oxidizing ability of SCR catalyst includes,
s1, placing the honeycomb SCR catalyst monomer in 1-2mol/L Ce (NO)3)3Soaking in the solution;
and S2, soaking fully, air-drying, and then calcining to obtain the modified catalyst.
Preferably, in S1, the honeycomb SCR catalyst monomer is mixed with Ce (NO)3)3The proportion of the solution is 30-35 g: 1L of the compound.
Preferably, in S1, the honeycomb SCR catalyst monomer is at least Ce (NO)3)3The solution was soaked for 3 hours.
Preferably, in S2, the material is soaked sufficiently and then naturally dried at room temperature.
Preferably, in S2, the calcination step is as follows,
s21, heating from room temperature to the heat preservation temperature, wherein the heating rate is less than 3 ℃/min;
s22, preserving heat for at least 24h at the heat preservation temperature;
s23, heating from the heat preservation temperature to the calcination temperature, wherein the heating rate is less than 3 ℃/min;
s24, calcining for at least 48h at the calcining temperature;
and S25, naturally cooling to room temperature.
Further, the temperature of the heat preservation is 110-.
Further, the calcination temperature is 300-400 DEG C
An SCR catalyst prepared by the method of any one of the preceding claims.
Compared with the prior art, the invention has the following beneficial technical effects:
according to the modification method, on the basis of the original denitration catalyst, cerium nitrate can be attached to the denitration catalyst through soaking, cerium oxide is obtained through calcination, the oxidation capability of the catalyst is improved, so that zero-valent mercury can be better oxidized through cerium oxide during denitration, divalent mercury is obtained, the operation method is simple and efficient, and the requirement for removing gaseous zero-valent mercury at present can be met.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
The method mainly comprises three steps of catalyst impregnation, air drying and calcination.
S1, placing the honeycomb SCR catalyst monomer in 1-2mol/L Ce (NO)3)3Soaking in the solution;
and S2, fully soaking, air-drying and calcining to obtain the modified catalyst.
In S1, the honeycomb SCR catalyst monomer and Ce (NO)3)3The proportion of the solution is 30-35 g: 1L of the compound. The honeycomb SCR catalyst monomer is at least in Ce (NO)3)3The solution was soaked for 3 hours.
And S2, fully soaking, and naturally drying at room temperature. The calcination process is also that the heat preservation treatment is carried out firstly and then the calcination is carried out, and the steps are as follows,
s21, heating from room temperature to the heat preservation temperature, wherein the heating rate is less than 3 ℃/min;
s22, preserving heat for at least 24h at the heat preservation temperature; preferably, the temperature is 110-.
S23, heating from the heat preservation temperature to the calcination temperature, wherein the heating rate is less than 3 ℃/min;
s24, calcining for at least 48h at the calcining temperature; preferably, the calcination temperature is 300-400 ℃.
And S25, naturally cooling to room temperature.
The invention also discloses the SCR catalyst prepared by the method.
Example 1
In the preferred embodiment, the catalyst modification is illustrated by comparison. A piece of honeycomb SCR catalyst monomer which runs 24000h is taken as a material, the intercept of the catalyst monomer is 6.88mm, the pore diameter is 6.22mm, and the specific surface area is 53.88m2Two 6X 6 well small catalytic samples A and B were taken from this.
1302.8g Ce (NO) was weighed out3)3·6H2And O, dissolving in a beaker by adding a proper amount of water, diluting to 3L by constant volume, and pouring back to the beaker.
And (3) putting the sample B into a beaker, soaking for about 3 hours, taking out, naturally drying at room temperature, and then putting into a resistance furnace for calcining to obtain a modified catalyst sample. The specific calcination process is as follows:
slowly heating from room temperature to 1100 ℃, wherein the heating rate is less than 3 ℃/min;
II, preserving the heat for 24 hours at 110 ℃;
III, heating from 110 ℃ to 300 ℃, wherein the heating rate is less than 3 ℃/min;
IV, calcining for 48 hours at 300 ℃;
and V, naturally cooling to room temperature.
The BET specific surface area, the single-site specific surface area, the pore volume and the pore diameter of sample A were 53.88m2/g、52.66m2/g、0.252ml/g、16.4nm。
The BET specific surface area, the single-site specific surface area, the pore volume and the pore diameter of the modified sample B were 53.88m2/g、52.66m2/g、0.252ml/g、16.4nm。
Carrying out a comparison test on the sample A and the improved sample B in simulated smoke to simulate O in the smoke2The concentration is 6%, the HCl concentration is 120-150 ppm, the temperature is 100-400 ℃, and the maximum mercury oxidation rate of the sample A is 73.0% at 350 ℃; the modified sample B reaches the maximum mercury oxidation rate of 84.7 percent at 350 ℃, and the mercury oxidation rate is increased by 16.0 percent compared with the sample A. Thereby obtaining Ce (NO) by impregnation3)3Solution modified SCR catalyst for Hg in flue gas0The oxidation capacity of the device is obviously improved, thereby being beneficial to subsequent equipment to remove mercury in the flue gas and reducing the emission concentration of mercury in the flue gas.
The following description of the catalyst modification was made by controlling the key parameters on the basis of example 1.
Example 2
S1, mixing the honeycomb SCR catalyst monomer according to the weight ratio of 30 g: 1L of Ce (NO) at a ratio of 2mol/L3)3Soaking in the solution for 3 hours;
and S2, fully soaking, naturally drying at room temperature, and calcining to obtain the modified catalyst.
The calcination step is as follows,
s21, heating from room temperature to the heat preservation temperature, wherein the heating rate is less than 3 ℃/min;
s22, preserving heat for 24 hours at the heat preservation temperature; the holding temperature was 120 ℃.
S23, heating from the heat preservation temperature to the calcination temperature, wherein the heating rate is less than 3 ℃/min;
s24, calcining for 48 hours at the calcining temperature; the calcination temperature was 360 ℃.
And S25, naturally cooling to room temperature.
Example 3
S1, mixing the honeycomb SCR catalyst monomer according to the weight ratio of 33 g: 1L of Ce (NO) at a concentration of 1.5mol/L3)3Soaking in the solution for 3 hours;
and S2, fully soaking, naturally drying at room temperature, and calcining to obtain the modified catalyst.
The calcination step is as follows,
s21, heating from room temperature to the heat preservation temperature, wherein the heating rate is less than 3 ℃/min;
s22, preserving heat for 30h at the heat preservation temperature; the holding temperature was 130 ℃.
S23, heating from the heat preservation temperature to the calcination temperature, wherein the heating rate is less than 3 ℃/min;
s24, calcining for 50h at the calcining temperature; the calcination temperature was 300 ℃.
And S25, naturally cooling to room temperature.
Example 4
S1, mixing the honeycomb SCR catalyst monomer according to the weight ratio of 35 g: 1L of Ce (NO) at a ratio of 2mol/L3)3Soaking in the solution for 4 hours;
and S2, fully soaking, naturally drying at room temperature, and calcining to obtain the modified catalyst.
The calcination step is as follows,
s21, heating from room temperature to the heat preservation temperature, wherein the heating rate is less than 3 ℃/min;
s22, preserving heat for 26h at the heat preservation temperature; the holding temperature was 110 ℃.
S23, heating from the heat preservation temperature to the calcination temperature, wherein the heating rate is less than 3 ℃/min;
s24, calcining for 56 hours at the calcining temperature; the calcination temperature was 400 ℃.
And S25, naturally cooling to room temperature.
Example 5
S1, mixing the honeycomb SCR catalyst monomer according to the weight ratio of 34 g: 1L of Ce (NO) at a ratio of 1mol/L3)3Soaking in the solution for 5 hours;
and S2, fully soaking, naturally drying at room temperature, and calcining to obtain the modified catalyst.
The calcination step is as follows,
s21, heating from room temperature to the heat preservation temperature, wherein the heating rate is less than 3 ℃/min;
s22, preserving heat for 40h at the heat preservation temperature; the holding temperature was 115 ℃.
S23, heating from the heat preservation temperature to the calcination temperature, wherein the heating rate is less than 3 ℃/min;
s24, calcining for 48 hours at the calcining temperature; the calcination temperature was 330 ℃.
And S25, naturally cooling to room temperature.
Claims (8)
1. A method for modifying the zero-valent mercury oxidation capability of an SCR catalyst is characterized by comprising the following steps,
s1, placing the honeycomb SCR catalyst monomer in 1-2mol/L Ce (NO)3)3Soaking in the solution;
and S2, fully soaking, air-drying and calcining to obtain the modified catalyst.
2. The method for modifying zero-valent mercury oxidation capacity of SCR catalyst of claim 1, wherein in S1, the honeycomb SCR catalyst monomer is mixed with Ce (NO)3)3The proportion of the solution is 30-35 g: 1L of the compound.
3. The method for modifying zero-valent mercury oxidation capacity of SCR catalyst of claim 1, wherein in S1, the honeycomb SCR catalyst monomer is at least Ce (NO)3)3The solution was soaked for 3 hours.
4. The method for modifying zero-valent mercury oxidizing ability of an SCR catalyst according to claim 1, wherein the SCR catalyst is air-dried at room temperature after being soaked sufficiently in S2.
5. The method for modifying zero-valent mercury oxidizing ability of SCR catalyst of claim 1, wherein in S2, the calcination step is as follows,
s21, heating from room temperature to the heat preservation temperature, wherein the heating rate is less than 3 ℃/min;
s22, preserving heat for at least 24h at the heat preservation temperature;
s23, heating from the heat preservation temperature to the calcination temperature, wherein the heating rate is less than 3 ℃/min;
s24, calcining for at least 48h at the calcining temperature;
and S25, naturally cooling to room temperature.
6. The method as claimed in claim 5, wherein the holding temperature is 110-130 ℃.
7. The method as claimed in claim 5, wherein the calcination temperature is 300-400 ℃.
8. An SCR catalyst prepared by the process of any one of claims 1 to 7.
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| CN202011305740.8A CN112264002A (en) | 2020-11-19 | 2020-11-19 | SCR catalyst and modification method for zero-valent mercury oxidation capacity thereof |
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| CN202011305740.8A CN112264002A (en) | 2020-11-19 | 2020-11-19 | SCR catalyst and modification method for zero-valent mercury oxidation capacity thereof |
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|---|---|---|---|---|
| CN102350340A (en) * | 2011-10-19 | 2012-02-15 | 国电科学技术研究院 | Composite smoke denitration catalyst capable of oxidizing zero-valence mercury |
| CN103433081A (en) * | 2013-08-08 | 2013-12-11 | 涿州西热环保催化剂有限公司 | Regeneration method for honeycomb type SCR (Selective Catalytic Reduction) denitration catalyst |
| WO2015051363A1 (en) * | 2013-10-04 | 2015-04-09 | University Of Cincinnati | Method and system for removing gaseous mercury in flue gases |
| US20150343378A1 (en) * | 2014-05-30 | 2015-12-03 | Ada Carbon Solutions, Llc | Catalytically enhanced compositions for efficient removal of contaminants in flue gas streams |
| CN105289278A (en) * | 2015-11-06 | 2016-02-03 | 河北工业大学 | Method for oxidizing elemental mercury by improving gas selective catalytic reduction (SCR) denitration processing system |
| CN106390964A (en) * | 2016-08-26 | 2017-02-15 | 华能国际电力股份有限公司 | Preparation method of denitration and demercuration integrated catalyst powder |
-
2020
- 2020-11-19 CN CN202011305740.8A patent/CN112264002A/en active Pending
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| CN102350340A (en) * | 2011-10-19 | 2012-02-15 | 国电科学技术研究院 | Composite smoke denitration catalyst capable of oxidizing zero-valence mercury |
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Non-Patent Citations (3)
| Title |
|---|
| SHIBO ZHANG ET.AL: "Enhancement of CeO2 modified commercial SCR catalyst for synergistic mercury removal from coal combustion flue gas", 《RSC ADVANCED》 * |
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Application publication date: 20210126 |