CN106944036B - Preparation process of clover-shaped strip-shaped low-temperature flue gas denitration catalyst - Google Patents
Preparation process of clover-shaped strip-shaped low-temperature flue gas denitration catalyst Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 54
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 239000003546 flue gas Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000008367 deionised water Substances 0.000 claims abstract description 23
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 18
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- OGUCKKLSDGRKSH-UHFFFAOYSA-N oxalic acid oxovanadium Chemical compound [V].[O].C(C(=O)O)(=O)O OGUCKKLSDGRKSH-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000011812 mixed powder Substances 0.000 claims abstract description 12
- 238000004898 kneading Methods 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims abstract description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004327 boric acid Substances 0.000 claims abstract description 8
- 239000003365 glass fiber Substances 0.000 claims abstract description 8
- 239000004310 lactic acid Substances 0.000 claims abstract description 8
- 235000014655 lactic acid Nutrition 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000000465 moulding Methods 0.000 claims abstract description 6
- 235000010215 titanium dioxide Nutrition 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 14
- 238000001354 calcination Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 abstract description 2
- KEQXNNJHMWSZHK-UHFFFAOYSA-L 1,3,2,4$l^{2}-dioxathiaplumbetane 2,2-dioxide Chemical compound [Pb+2].[O-]S([O-])(=O)=O KEQXNNJHMWSZHK-UHFFFAOYSA-L 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 17
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 9
- 239000007789 gas Substances 0.000 description 4
- 229910001868 water Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 238000004056 waste incineration Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- 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
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
-
- B01J35/30—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Abstract
A cloverleaf-shaped strip-shaped low-temperature flue gas denitration catalyst is prepared by adding titanium dioxide, glass fiber, boric acid, silicon dioxide powder and pseudo-boehmite into a kneading machine, stirring, and uniformly mixing to obtain milk-white mixed powder; then adding the vanadyl oxalate solid into deionized water, and stirring until the vanadyl oxalate is completely dissolved to obtain a solution 1; adding lactic acid into deionized water to form a solution 2; then adding the solution 1, the solution 2 and deionized water into the milky mixed powder, and uniformly stirring by using a kneading machine to obtain a bulk pug; finally, a strip-shaped extruder is used for extruding and molding the pug mass to obtain a strip-shaped catalyst; the extruded strip catalyst is dried for 12 hours at normal temperature, and then dried and calcined to obtain the cloverleaf-shaped strip catalyst, and the prepared cloverleaf-shaped strip catalyst has the advantages of high strength, difficult pulverization, long service life, higher flue gas denitration efficiency, simple preparation process and good application prospect.
Description
Technical Field
The invention relates to the technical field of nitrogen oxide control of environmental protection, in particular to a preparation process of a clover-shaped strip-shaped low-temperature flue gas denitration catalyst.
Background
Nitrogen Oxides (NO)x) Is one of the main harmful substances polluting the atmosphere and is also a significant factor directly causing haze days, ozone damage and air pollution in various parts of China. At present, flue gas denitration is one of effective methods for controlling emission of nitrogen oxides, wherein Selective Catalytic Reduction (SCR) is used for flue gas denitration due to the advantages of high denitration efficiency, good selectivity, stable and reliable operation and the likeThe method is widely applied in the process of nitre. The most mature catalyst currently used is V2O5/TiO2Or at V2O5/TiO2Catalysts modified on the basis of these, but such catalysts have higher activity only at operating temperatures above 350 ℃ because of the vanadium loading of 1% or less. However, a large number of industrial furnaces, such as glass furnaces, refuse burning power plants, etc., have low exhaust gas temperatures<250 ℃) and needs to adopt a heat source to reheat the flue gas, which increases the operating cost.
The cloverleaf-shaped strip catalyst has larger bulk density, can effectively increase the contact area of gas and the catalyst, and improves the catalytic efficiency. However, the mechanical strength of the trilobe-shaped stripe catalyst is slightly inferior to that of the coated honeycomb catalyst. Therefore, the development of the clover-shaped strip denitration catalyst applied to the low-temperature condition has practical application significance.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation process of a clover-shaped strip-shaped low-temperature flue gas denitration catalyst, the prepared catalyst has high strength, is not easy to pulverize, has high denitration efficiency, and can be widely applied to flue gas denitration of glass furnaces, waste incineration power plants and the like under a low-temperature condition.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation process of a clover-shaped strip-shaped low-temperature flue gas denitration catalyst comprises the following steps:
the method comprises the following steps: adding titanium dioxide, glass fiber, boric acid, silicon dioxide powder and pseudo-boehmite into a kneading machine for stirring, and uniformly mixing to obtain milky mixed powder;
step two: adding vanadyl oxalate solid into deionized water, wherein the mass of the vanadyl oxalate solid is 10-20% of that of the titanium white powder, and the using amount of the deionized water is 20-30% of that of the titanium white powder, stirring until the vanadyl oxalate is completely dissolved, and marking as a solution 1;
step three: adding lactic acid into deionized water, wherein the amount of the lactic acid is 1-3% of the mass of the titanium dioxide, and the amount of the deionized water is 3-6% of the mass of the titanium dioxide, and marking the formed solution as a solution 2;
step four: adding the solution 1, the solution 2 and deionized water into the milky white mixed powder obtained in the step one, and uniformly stirring by using a kneading machine to obtain a bulk pug;
step five: extruding and molding the pug mass by using a strip extruder to obtain a strip catalyst; drying the extruded strip-shaped catalyst for 12h at normal temperature, and then drying and calcining to obtain the cloverleaf-shaped strip-shaped catalyst.
The mass of the glass fiber added in the step one is 2-7% of the mass of the titanium dioxide, the total mass of the boric acid and the silicon dioxide powder is 5-20% of the mass of the titanium dioxide, and the mass of the pseudo-boehmite is 1-6% of the mass of the titanium dioxide.
V formed after the vanadyl oxalate solid added in the step two is roasted2O5The loading amount of the catalyst is 2 to 7 percent.
The total ion water amount added in the second step, the third step and the fourth step is 30-40% of the mass of the titanium dioxide.
In the fifth step, the drying temperature is 60-120 ℃, the drying time is 2-6 h, the calcining temperature is 400-550 ℃, and the calcining time is 4-8 h.
Compared with the prior art, the invention has the following advantages:
1. the cloverleaf-shaped strip catalyst prepared by the invention has high strength, the compression mechanical strength can reach 115N/cm-145N/cm, the pulverization is not easy, and the service life is long.
2. The cloverleaf-shaped strip catalyst prepared by the invention has large contact area with gas, higher flue gas denitration efficiency and high air speed of 6000h-1，SO2100ppm of water and 5% of water, a conversion of 95% at 200 ℃. And the preparation process is simple, and the application prospect is good.
Detailed Description
The following examples are provided to explain embodiments of the present invention in detail.
Example one
A preparation process of a clover-shaped strip-shaped low-temperature flue gas denitration catalyst comprises the following steps:
the method comprises the following steps: adding 200g of titanium dioxide, 4g of glass fiber, 2.5g of boric acid, 7.5g of silicon dioxide powder and 2g of pseudo-boehmite into a kneading machine for stirring, and uniformly mixing to obtain milky mixed powder;
step two: adding 28g of vanadyl oxalate solid into 50ml of deionized water, and stirring at 50 ℃ until the vanadyl oxalate is completely dissolved, and marking as a solution 1;
step three: adding 2.4mL of lactic acid into 10mL of deionized water, and marking the mixed solution as a solution 2;
step four: adding the solution 1, the solution 2 and 10mL of deionized water into the milky white mixed powder obtained in the step one, and uniformly stirring by using a kneading machine to obtain a bulk pug;
step five: extruding and molding the pug mass by using a strip extruder to obtain a strip catalyst; drying the extruded strip-shaped catalyst for 12 hours at normal temperature, and then drying the extruded strip-shaped catalyst for 2 hours in an oven at the temperature of 80 ℃; and putting the dried strip-shaped catalyst into a muffle furnace, and calcining for 4 hours at 400 ℃ to obtain the clover-shaped strip-shaped catalyst.
Example two
A preparation process of a clover-shaped strip-shaped low-temperature flue gas denitration catalyst comprises the following steps:
the method comprises the following steps: adding 200g of titanium dioxide, 6g of glass fiber, 5g of boric acid, 15g of silicon dioxide powder and 3g of pseudo-boehmite into a kneader, stirring, and uniformly mixing to obtain milky mixed powder;
step two: adding 30g of vanadyl oxalate solid into 50ml of deionized water, and stirring at 50 ℃ until the vanadyl oxalate is completely dissolved, and marking as a solution 1;
step three: adding 2.4mL of lactic acid into 10mL of deionized water, and marking the mixed solution as a solution 2;
step four: adding the solution 1, the solution 2 and 20mL of deionized water into the milky white mixed powder obtained in the step one, and uniformly stirring by using a kneading machine to obtain a bulk pug;
step five: extruding and molding the pug mass by using a strip extruder to obtain a strip catalyst, drying the extruded strip catalyst for 12 hours at normal temperature, and then drying the extruded strip catalyst for 4 hours in an oven at 100 ℃; and putting the dried strip-shaped catalyst into a muffle furnace, and calcining for 6h at 450 ℃ to obtain the clover-shaped strip-shaped catalyst.
EXAMPLE III
A preparation process of a clover-shaped strip-shaped low-temperature flue gas denitration catalyst comprises the following steps:
the method comprises the following steps: adding 200g of titanium dioxide, 6g of glass fiber, 5g of boric acid, 15g of silicon dioxide powder and 5g of pseudo-boehmite into a kneader, stirring, and uniformly mixing to obtain milky mixed powder;
step two: adding 32g of vanadyl oxalate solid into 50ml of deionized water, and stirring at 50 ℃ until the vanadyl oxalate is completely dissolved, and marking as a solution 1;
step three: adding 2.4mL of lactic acid into 10mL of deionized water, and marking the mixed solution as a solution 2;
step four: adding the solution 1, the solution 2 and 20mL of deionized water into the milky white mixed powder obtained in the step one, and uniformly stirring by using a kneading machine to obtain a bulk pug;
step five: extruding and molding the pug mass by using a strip extruder to obtain a strip catalyst; drying the extruded strip-shaped catalyst for 12 hours at normal temperature, and then drying the extruded strip-shaped catalyst for 4 hours in an oven at the temperature of 80 ℃; and putting the dried strip-shaped catalyst into a muffle furnace, and calcining for 6h at 500 ℃ to obtain the clover-shaped strip-shaped catalyst.
The results of the activity test and the strength test of the trilobe-shaped catalyst strips prepared in the first, second and third examples are shown in table 1.
Table 1 results of activity test and strength test of the bar catalysts at low temperature
| Catalyst and process for preparing same | Denitration efficiency at 170 ℃ (%) | Denitration efficiency at 200 ℃ (%) | Mechanical strength against compression (N/cm) |
| Example one | 76.2 | 94.6 | 117.8 |
| Example two | 75.2 | 95.0 | 130.7 |
| EXAMPLE III | 76.9 | 96.4 | 147.9 |
Reaction conditions are as follows: the temperature is 150-300 ℃, and the space velocity is 6000h-1NO content 500ppm, NH3Content 500ppm, SO2Content 100ppm, H2O content 5%, N2Is the balance gas. As can be seen from Table 1, the clover-shaped strip catalyst prepared by the method of the present invention has high compressive mechanical strength and good denitration efficiency at low temperature.
Claims (3)
1. A preparation process of a clover-shaped strip-shaped low-temperature flue gas denitration catalyst is characterized by comprising the following steps:
the method comprises the following steps: adding titanium dioxide, glass fiber, boric acid, silicon dioxide powder and pseudo-boehmite into a kneading machine for stirring, and uniformly mixing to obtain milky mixed powder;
step two: adding vanadyl oxalate solid into deionized water, wherein the mass of the vanadyl oxalate solid is 10-20% of that of the titanium white powder, and the using amount of the deionized water is 20-30% of that of the titanium white powder, stirring until the vanadyl oxalate is completely dissolved, and marking as a solution 1;
step three: adding lactic acid into deionized water, wherein the amount of the lactic acid is 1-3% of the mass of the titanium dioxide, and the amount of the deionized water is 3-6% of the mass of the titanium dioxide, and marking the formed solution as a solution 2;
step four: adding the solution 1, the solution 2 and deionized water into the milky white mixed powder obtained in the step one, and uniformly stirring by using a kneading machine to obtain a bulk pug;
step five: extruding and molding the pug mass by using a strip extruder to obtain a strip catalyst; drying the extruded strip-shaped catalyst for 12 hours at normal temperature, and then drying and calcining to obtain a cloverleaf-shaped strip-shaped catalyst;
the mass of the glass fiber added in the step one is 2-7% of the mass of the titanium dioxide, the total mass of the boric acid and the silicon dioxide powder is 5-20% of the mass of the titanium dioxide, and the mass of the pseudo-boehmite is 1-6% of the mass of the titanium dioxide;
v formed after the vanadyl oxalate solid added in the step two is roasted2O5The loading amount of the catalyst is 2 to 7 percent.
2. The process for preparing a clover-shaped strip-shaped low-temperature flue gas denitration catalyst according to claim 1, which is characterized in that: the total deionized water added in the second step, the third step and the fourth step accounts for 30-40% of the mass of the titanium dioxide.
3. The process for preparing a clover-shaped strip-shaped low-temperature flue gas denitration catalyst according to claim 1, which is characterized in that: in the fifth step, the drying temperature is 60-120 ℃, the drying time is 2-6 h, the calcining temperature is 400-550 ℃, and the calcining time is 4-8 h.
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| CN201061759Y (en) * | 2007-04-04 | 2008-05-21 | 中国石油化工股份有限公司 | Clover-shaped catalyzer |
| CN104174442A (en) * | 2014-08-27 | 2014-12-03 | 清华大学 | Low-temperature flue gas denitration catalyst forming process |
| KR20150097311A (en) * | 2014-02-18 | 2015-08-26 | 한국생산기술연구원 | Fabrication method of SCR catalyst and Mold with fine-structure |
| CN204816561U (en) * | 2015-06-30 | 2015-12-02 | 中国石油天然气股份有限公司 | Cloverleaf pattern catalyst |
| CN105964243A (en) * | 2016-06-16 | 2016-09-28 | 上海净球环保科技有限公司 | Method for preparing denitration catalyst from discarded vanadium and titanium based denitration catalyst |
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| CN105107514B (en) * | 2015-08-17 | 2018-12-14 | 成都金鑫天蓝科技有限公司 | A kind of non-vanadium denitration preformed catalyst of honeycomb, preparation method and its usage |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201061759Y (en) * | 2007-04-04 | 2008-05-21 | 中国石油化工股份有限公司 | Clover-shaped catalyzer |
| KR20150097311A (en) * | 2014-02-18 | 2015-08-26 | 한국생산기술연구원 | Fabrication method of SCR catalyst and Mold with fine-structure |
| CN104174442A (en) * | 2014-08-27 | 2014-12-03 | 清华大学 | Low-temperature flue gas denitration catalyst forming process |
| CN204816561U (en) * | 2015-06-30 | 2015-12-02 | 中国石油天然气股份有限公司 | Cloverleaf pattern catalyst |
| CN105964243A (en) * | 2016-06-16 | 2016-09-28 | 上海净球环保科技有限公司 | Method for preparing denitration catalyst from discarded vanadium and titanium based denitration catalyst |
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