CN102755887B - Preparation method of semiconductor control rectifier (SCR) denitration catalytic agent applicable to high temperature smoke condition - Google Patents
Preparation method of semiconductor control rectifier (SCR) denitration catalytic agent applicable to high temperature smoke condition Download PDFInfo
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Abstract
The invention relates to a preparation method of a semiconductor control rectifier (SCR) denitration catalytic agent applicable to a high temperature smoke condition and belongs to the technical field of catalysis. Graft copolymerization modified starch used when a vanadium tungsten titanium system denitration catalytic agent is prepared, two polymers with different molecular chain lengths and molecular weights are used, tackify and flocculation effects are achieved simultaneously, particle aggregation states of the catalytic agent are optimized combined with a chambering agent, adhesive and the like, acting force between particles is strengthened, mechanical strength and mechanical strength of the catalytic agent under the high temperature environment is greatly improved, pore volume of prepared catalytic agent is larger than 0.35mL/g, firing of the catalytic agent under the high temperature smoke condition can be slowed down, the catalytic agent still has good nitric oxide removal rate and anti-firing performance when the smoke temperature is as high as 400-430 DEG C, adaptability of the denitration catalytic agent under the high temperature smoke condition is improved, and denitration catalyst technology breaks through under the high temperature smoke condition.
Description
Technical field
The present invention relates to a kind of preparation method who is applicable to the SCR denitrating catalyst of high-temperature flue gas condition, use denitrating catalyst prepared by this kind of method still to there is good nitrogen oxide removal efficiency and anti-sintering property in flue-gas temperature during up to 400 ~ 430 ℃, belong to catalysis technical field.
Background technology
Along with country during " 12 " is more and more stricter to the control of discharged nitrous oxides, simple low nitrogen burning technology cannot meet the requirement of existing discharge standard, and SCR (SCR) technology has started coal-burning power plant's application at home because of the denitration performance of its high efficient and reliable.The cardinal principle of SCR is with NH
3for reducing agent, under the effect of denitrating catalyst, optionally by NO
xbe reduced into N
2.
Current most widely used SCR denitrating catalyst is vanadium tungsten titanium catalyst, and because its catalyst activity temperature is higher, scope is 320 ~ 400 ℃ of left and right, thereby adopts high temperature arrangement in thermal power plant's application, after being arranged in boiler economizer, before air preheater.Although catalyst has higher activity and anti-sulphur water repelling property on this position, but residing flue gas environmental condition is more severe, wherein flue-gas temperature can reach more than 400 ℃, sometimes even can reach 450 ℃, denitrating catalyst at high temperature operation for a long time can cause the inevitable sintering of catalyst, cause collapsing and the decline of specific area of catalyst duct structure, and the mechanical strength of catalyst and structural strength are caused to great irreversible damage, catalyst catalytic performance is weakened, greatly shortened the service life of catalyst, increased operating cost.In order to solve the easy-sintering problem of SCR denitrating catalyst under high-temperature flue gas condition, the present invention has studied a kind of preparation method who is applicable to the SCR denitrating catalyst of high-temperature flue gas condition.
Summary of the invention
The present invention is in order to solve the Sintering Problem of SCR denitrating catalyst under high-temperature flue gas condition, a kind of preparation method who is applicable to the SCR denitrating catalyst of high-temperature flue gas condition is provided, the denitrating catalyst that uses the method to prepare has been optimized the particle aggregation state of catalyst, strengthened the active force between particle, make pore volume be greater than 0.35mL/g simultaneously, the ratio that macropore (aperture > 50nm) pore volume accounts for total pore volume is greater than 50%, catalyst pore volume is larger, especially large hole number is more, slowed down the sintering of catalyst under high-temperature flue gas condition, make catalyst in flue-gas temperature, still there is good nitrogen oxide removal efficiency and anti-sintering property during up to 400 ~ 430 ℃, improved the adaptability of denitrating catalyst under high-temperature flue gas condition.
According to technical scheme provided by the invention, a kind of preparation method who is applicable to the SCR denitrating catalyst of high-temperature flue gas condition, preparation process is as follows by weight:
(1) preparation of ammonium metavanadate solution: take 0.39 ~ 1.3 part of ammonium metavanadate, 70 ~ 95 ℃ by the ammonium metavanadate stirring and dissolving taking in the aqueous solution of 0.1 ~ 0.9 part of monoethanolamine, the concentration of aqueous solution of monoethanolamine is 0.2 ~ 2g/mL;
(2) preparation of metallic salt solution: get 0 ~ 10 part of stirring and dissolving of metallic salt in the deionized water of 0 ~ 100 part;
(3) mixed once: take 75 ~ 95 parts of nano grade titanium tungsten powders, add therein 3 ~ 7 parts of lauryl sodium sulfate, after mixing, add 80 ~ 100 parts of deionized waters, be heated to 70 ~ 98 ℃, keep constant temperature to stir simultaneously and within 20 ~ 40 minutes, make mixture become coccoid, add 5 ~ 15 parts of glass fibres, the ammonium metavanadate solution that adds preparation in step (1) after stirring, the metallic salt solution of preparation in step (2), 8 ~ 15 parts of expanding agents, stir and become coccoid to mixture;
(4) once extrude: the solid that step (3) is obtained is extruded into strip and block on extruder;
(5) primary drying: the solid that step (4) is obtained is dried 8 ~ 20 hours under 50 ~ 70 ℃ of conditions;
(6) once calcining: the solid that step (5) is obtained is calcined 4 ~ 8 hours under 300 ~ 400 ℃ of conditions;
(7) secondary mixes: the solid that step (6) is obtained is crushed to micron particles, adds therein 15 ~ 25 parts of Pioloform, polyvinyl acetals, 8 ~ 15 parts of expanding agents, 5 ~ 10 portions of converted starches, 20 ~ 40 parts of ammoniacal liquor that concentration is 15 ~ 30%, are heated to 40 ℃, stir and become coccoid to mixture;
(8) secondary is extruded: the solid that step (7) is obtained is equipped with at front end that on the extruder of catalyst mould, to carry out hot-extrudable one-tenth cellular;
(9) redrying: the solid that step (8) is obtained is dried 5 ~ 10 hours under 50 ~ 70 ℃ of conditions is then dried 7 ~ 12 hours under the temperature conditions of 100 ~ 120 ℃;
(10) secondary clacining: the solid that step (9) is obtained is calcined 4 ~ 8 hours under 550 ~ 700 ℃ of conditions, obtains the SCR denitrating catalyst that product is applicable to high-temperature flue gas condition.
Described product is applicable in the SCR denitrating catalyst of high-temperature flue gas condition, by weight: TiO
2account for 70 ~ 90 parts, WO
3account for 3 ~ 8 parts, V
2o
5account for 0.3 ~ 1 part, oxide accounts for 0 ~ 10 part, and glass fibre accounts for 5 ~ 15 parts.
Described metallic salt is the nitrate of Zr, Nb and Y or one or more the mixture in acetate.
Described expanding agent is methenamine, the mixture of one or more in active carbon and polyethylene glycol.
Described converted starch is the grafting polyacrylic acid copolymerized thing of bydroxyethyl starch ether, the mixture of one or more in the lactide copolymer grafted and HES grafting caprolactone copolymer of HES.
In described nano grade titanium tungsten powder, containing tungstic acid quality, be 5% ~ 8%, through conducting modification of surface hydroxy group, process, BET specific area is less than 70m
2/ g, X-ray diffraction peak height is greater than 160mm.
The glass diameter of described glass fibre is 10 ~ 13 μ m.
Tool of the present invention has the following advantages: catalyst prepared by the present invention has been used the converted starch of graft copolymerization, utilize the polymer of two kinds of different molecular chain lengths and molecular weight, complete the effect of tackify and flocculation simultaneously, coordinate expanding agent and adhesive etc., optimized the particle aggregation state of catalyst, strengthened the active force between particle, greatly strengthened mechanical strength and the structural strength of catalyst in hot environment, the catalyst pore volume of preparation is greater than 0.35mL/g, the ratio that macropore (aperture > 50nm) pore volume accounts for total pore volume is greater than 50%, catalyst pore volume is larger, especially large hole number is more, slowed down the sintering of catalyst under high-temperature flue gas condition, make catalyst in flue-gas temperature, still there is good nitrogen oxide removal efficiency and anti-sintering property during up to 400 ~ 430 ℃, improved the adaptability of denitrating catalyst under high-temperature flue gas condition, realize the breakthrough of denitrating catalyst technology under high-temperature flue gas condition.
The specific embodiment
Below in conjunction with specific embodiment, the invention will be further described.In following examples, ammonium metavanadate is purchased from Dalian milky way metal material Co., Ltd; Monoethanolamine is purchased from Zibo Lai Wo Chemical Co., Ltd.; Metallic salt is purchased from Chemical Reagent Co., Ltd., Sinopharm Group; Titanium tungsten powder is purchased from Sichuan Huatie Vanadium Titanium Technology Co., Ltd.; Lauryl sodium sulfate is purchased from Sinolight Chemical Co., Ltd.; Glass fibre is purchased from Nanjing Xing Xing fiberglass products Co., Ltd; Pioloform, polyvinyl acetal is purchased from Shanghai Run Haoyuan Industrial Co., Ltd.; Expanding agent is purchased from Wuxi City Kang Heng chemicals Co., Ltd and Wuxi Zhi Kang environmental protection equipment Co., Ltd; Converted starch is purchased from Nanjing, Wuxi tower starch Co., Ltd; Ammoniacal liquor is purchased from Wuxi City Ya Sheng Chemical Co., Ltd..
Embodiment 1 is applicable to the preparation method of the SCR denitrating catalyst of high-temperature flue gas condition, comprises following processing step:
(1) preparation of ammonium metavanadate solution: take ammonium metavanadate 0.39kg, 90 ℃ by the ammonium metavanadate stirring and dissolving taking in the aqueous solution of 0.5kg monoethanolamine, the concentration of aqueous solution of monoethanolamine is 0.7g/mL;
(2) preparation of metallic salt solution: get 5.5kg zirconium nitrate stirring and dissolving in the deionized water of 30L;
(3) mixed once: take the nano grade titanium tungsten powder 85kg containing tungstic acid quality 5%, add therein 4kg lauryl sodium sulfate, after mixing, add 90L deionized water, be heated to 75 ℃, keep constant temperature to stir simultaneously and make mixture become graininess in 25 minutes, then add therein 12.7kg glass fibre, the ammonium metavanadate solution that adds preparation in step (1) after stirring, the metallic salt solution of preparation in step (2), 8kg methenamine, stirs and becomes coccoid to mixture;
(4) once extrude: the solid that step (3) is obtained is simply extruded into strip and block on extruder;
(5) primary drying: the solid that step (4) is obtained is dried 9 hours under 55 ℃ of conditions;
(6) once calcining: the solid that step (5) is obtained is calcined 5 hours under 320 ℃ of conditions;
(7) secondary mixes: the solid that step (6) is obtained is crushed to micron particles, add therein 15kg Pioloform, polyvinyl acetal, 8kg methenamine, the grafting polyacrylic acid copolymerized thing of 5kg bydroxyethyl starch ether, 20kg concentration is 18% ammoniacal liquor, be heated to 40 ℃, stir and become coccoid to mixture;
(8) secondary is extruded: the solid that step (7) is obtained is equipped with at front end that on the extruder of catalyst mould, to carry out hot-extrudable one-tenth cellular;
(9) redrying: the solid that step (8) is obtained is dried 7 hours under 55 ℃ of conditions is then dried 8 hours under the temperature conditions of 104 ℃;
(10) secondary clacining: the solid that step (9) is obtained is calcined 7 hours under 560 ℃ of conditions, obtains the SCR denitrating catalyst that product is applicable to high-temperature flue gas condition.
Wherein, TiO
2weight accounts for 80.75%, WO in total catalyst weight
3weight accounts for 4.25%, V in total catalyst weight
2o
5weight accounts for 0.3%, ZrO in total catalyst weight
2weight accounts for 2% in total catalyst weight, and glass fibre weight accounts for 12.7% in total catalyst weight.
Embodiment 2 is applicable to the preparation method of the SCR denitrating catalyst of high-temperature flue gas condition, comprises following processing step:
(1) preparation of ammonium metavanadate solution: take ammonium metavanadate 0.65kg, 78 ℃ by the ammonium metavanadate stirring and dissolving taking in the aqueous solution of 0.25kg monoethanolamine, the concentration of aqueous solution of monoethanolamine is 0.9g/mL;
(2) preparation of metallic salt solution: get 10kg yttrium nitrate stirring and dissolving in the deionized water of 38L;
(3) mixed once: take the nano grade titanium tungsten powder 90kg containing tungstic acid quality 7%, add therein 5kg lauryl sodium sulfate, after mixing, add 93L deionized water, be heated to 83 ℃, keep constant temperature to stir simultaneously and within 26 minutes, make mixture become coccoid, then add therein 6.5kg glass fibre, the ammonium metavanadate solution that adds preparation in step (1) after stirring, the metallic salt solution of preparation in step (2), 9kg active carbon, stirs and becomes coccoid to mixture;
(4) once extrude: the solid that step (3) is obtained is simply extruded into strip and block on extruder;
(5) primary drying: the solid that step (4) is obtained is dried 10 hours under 58 ℃ of conditions;
(6) once calcining: the solid that step (5) is obtained is calcined 5.5 hours under 345 ℃ of conditions;
(7) secondary mixes: the solid that step (6) is obtained is crushed to micron particles, adds therein 19kg Pioloform, polyvinyl acetal, 9kg active carbon, 6kg HES is lactide copolymer grafted, 24kg concentration is 20% ammoniacal liquor, is heated to 40 ℃, stirs and becomes coccoid to mixture;
(8) secondary is extruded: the solid that step (7) is obtained is equipped with at front end that on the extruder of catalyst mould, to carry out hot-extrudable one-tenth cellular;
(9) redrying: the solid that step (8) is obtained is dried 7.5 hours under 64 ℃ of conditions is then dried 9 hours under the temperature conditions of 112 ℃;
(10) secondary clacining: the solid that step (9) is obtained is calcined 6 hours under 610 ℃ of conditions, obtains the SCR denitrating catalyst that product is applicable to high-temperature flue gas condition.
Wherein, TiO
2weight accounts for 83.7%, WO in total catalyst weight
3weight accounts for 6.3%, V in total catalyst weight
2o
5weight accounts for 0.5%, Y in total catalyst weight
2o
3weight accounts for 3% in total catalyst weight, and glass fibre weight accounts for 6.5% in total catalyst weight.
Embodiment 3 is applicable to the preparation method of the SCR denitrating catalyst of high-temperature flue gas condition, comprises following processing step:
(1) preparation of ammonium metavanadate solution: take ammonium metavanadate 1.3kg, 85 ℃ by the ammonium metavanadate stirring and dissolving taking in the aqueous solution of 0.6kg monoethanolamine, the concentration of aqueous solution of monoethanolamine is 1.1g/mL;
(2) preparation of metallic salt solution: get 6.1kg nitric acid niobium stirring and dissolving in the deionized water of 47L;
(3) mixed once: take the nano grade titanium tungsten powder 89kg containing tungstic acid quality 7%, add therein 6kg lauryl sodium sulfate, after mixing, add 92L deionized water, be heated to 95 ℃, keep constant temperature to stir simultaneously and within 32 minutes, make mixture become coccoid, add 8kg glass fibre, the ammonium metavanadate solution that adds preparation in step (1) after stirring, the metallic salt solution of preparation in step (2), 10kg polyethylene glycol, stirs and becomes coccoid to mixture;
(4) once extrude: the solid that step (3) is obtained is simply extruded into strip and block on extruder;
(5) primary drying: the solid that step (4) is obtained is dried 11 hours under 65 ℃ of conditions;
(6) once calcining: the solid that step (5) is obtained is calcined 4.5 hours under 350 ℃ of conditions;
(7) secondary mixes: the solid that step (6) is obtained is crushed to micron particles, add therein 20kg Pioloform, polyvinyl acetal, 10kg polyethylene glycol, 8kg HES grafting caprolactone copolymer, 28kg concentration is 17% ammoniacal liquor, be heated to 40 ℃, stir and become coccoid to mixture;
(8) secondary is extruded: the solid that step (7) is obtained is equipped with at front end that on the extruder of catalyst mould, to carry out hot-extrudable one-tenth cellular;
(9) redrying: the solid that step (8) is obtained is dried 12 hours under 60 ℃ of conditions is then dried 11 hours under the temperature conditions of 115 ℃;
(10) secondary clacining: the solid that step (9) is obtained is calcined 5 hours under 640 ℃ of conditions, obtains the SCR denitrating catalyst that product is applicable to high-temperature flue gas condition.
Wherein, TiO
2weight accounts for 82.77%, WO in total catalyst weight
3weight accounts for 6.23%, V in total catalyst weight
2o
5weight accounts for 1%, Nb in total catalyst weight
2o
5weight accounts for 2% in total catalyst weight, and glass fibre weight accounts for 8% in total catalyst weight.
Application Example 1
Pore volume and the pore-size distribution testing result of embodiment 1-3 catalyst are as shown in table 1.
Table 1 is applicable to pore volume and the pore-size distribution testing result of the SCR denitrating catalyst of high-temperature flue gas condition
| Catalyst | Pore volume (mL/g) | Macropore pore volume ratio (%) |
| Commercial catalyst | 0.272 | 22.1 |
| Embodiment mono- | 0.352 | 53.7 |
| Embodiment bis- | 0.358 | 53.9 |
| Embodiment tri- | 0.371 | 52.6 |
As seen from the above table, by using the converted starch of graft copolymerization, utilize the polymer of two kinds of different molecular chain lengths and molecular weight, complete the effect of tackify and flocculation, coordinate expanding agent and adhesive etc. simultaneously, optimized the particle aggregation state of catalyst, make the catalyst pore volume of preparation be greater than 0.35mL/g, the ratio that macropore (aperture > 50nm) pore volume accounts for total pore volume is greater than 50%, compare conventional catalyst, the catalyst pore volume that utilizes the inventive method to prepare is larger, especially large hole number is more, can effectively slow down the sintering of catalyst under high-temperature flue gas condition.
The active detection of embodiment 1-3 is as shown in table 2.
Table 2 is applicable to the active testing result of the SCR denitrating catalyst of high-temperature flue gas condition
| Catalyst | 400 ℃ of denitration efficiencies (%) | 430 ℃ of denitration efficiencies (%) |
| Commercial catalyst | 55.1 | 60.4 |
| Embodiment mono- | 71.2 | 75.5 |
| Embodiment bis- | 71.5 | 75.8 |
| Embodiment tri- | 71.4 | 75.7 |
Reaction condition: air speed 80,000h
-1, NO content 400ppm, NH
3content 324ppm, SO
2content 500ppm, H
2o content 10%, N
2for Balance Air.
As seen from the above table, compare conventional catalyst, reaction temperature up to the condition of 400 ~ 430 ℃ under, SCR denitrating catalyst prepared according to the methods of the invention has good denitration efficiency.
Above said content is only the basic explanation of the present invention under conceiving, and those skilled in the art can make various modifications within the scope of the appended claims, and any change of therefore doing according to technical scheme of the present invention, all should belong to protection scope of the present invention.
Claims (7)
1.
onethe preparation method who plants the SCR denitrating catalyst that is applicable to high-temperature flue gas condition, is characterized in that preparation process is as follows by weight:
(1) preparation of ammonium metavanadate solution: take 0.39 ~ 1.3 part of ammonium metavanadate, 70 ~ 95 ℃ by the ammonium metavanadate stirring and dissolving taking in the aqueous solution of 0.1 ~ 0.9 part of monoethanolamine, the concentration of aqueous solution of monoethanolamine is 0.2 ~ 2g/mL;
(2) preparation of metal salt solution: get 0 ~ 10 part of stirring and dissolving of slaine in the deionized water of 0 ~ 100 part;
(3) mixed once: take 75 ~ 95 parts of nano grade titanium tungsten powders, add therein 3 ~ 7 parts of lauryl sodium sulfate, after mixing, add 80 ~ 100 parts of deionized waters, be heated to 70 ~ 98 ℃, keep constant temperature to stir simultaneously and within 20 ~ 40 minutes, make mixture become coccoid, add 5 ~ 15 parts of glass fibres, the ammonium metavanadate solution that adds preparation in step (1) after stirring, the metal salt solution of preparation in step (2), 8 ~ 15 parts of expanding agents, stir and become coccoid to mixture;
(4) once extrude: the solid that step (3) is obtained is extruded into strip and block on extruder;
(5) primary drying: the solid that step (4) is obtained is dried 8 ~ 20 hours under 50 ~ 70 ℃ of conditions;
(6) once calcining: the solid that step (5) is obtained is calcined 4 ~ 8 hours under 300 ~ 400 ℃ of conditions;
(7) secondary mixes: the solid that step (6) is obtained is crushed to micron particles, adds therein 15 ~ 25 parts of Pioloform, polyvinyl acetals, 8 ~ 15 parts of expanding agents, 5 ~ 10 portions of converted starches, 20 ~ 40 parts of ammoniacal liquor that concentration is 15% ~ 30%, are heated to 40 ℃, stir and become coccoid to mixture;
(8) secondary is extruded: the solid that step (7) is obtained is equipped with at front end that on the extruder of catalyst mould, to carry out hot-extrudable one-tenth cellular;
(9) redrying: the solid that step (8) is obtained is dried 5 ~ 10 hours under 50 ~ 70 ℃ of conditions is then dried 8 ~ 12 hours under the temperature conditions of 100 ~ 120 ℃;
(10) secondary clacining: the solid that step (9) is obtained is calcined 4 ~ 8 hours under 550 ~ 700 ℃ of conditions, obtains the SCR denitrating catalyst that product is applicable to high-temperature flue gas condition.
2. the preparation method who is applicable to as claimed in claim 1 the SCR denitrating catalyst of high-temperature flue gas condition, is characterized in that: described product is applicable in the SCR denitrating catalyst of high-temperature flue gas condition, by weight: TiO
2account for 70 ~ 90 parts, WO
3account for 3 ~ 8 parts, V
2o
5account for 0.3 ~ 1 part, metal oxide accounts for 0 ~ 10 part, and glass fibre accounts for 5 ~ 15 parts.
3. the preparation method who is applicable to as claimed in claim 1 the SCR denitrating catalyst of high-temperature flue gas condition, is characterized in that: described slaine is the nitrate of Zr, Nb and Y or one or more the mixture in acetate.
4. the preparation method who is applicable to as claimed in claim 1 the SCR denitrating catalyst of high-temperature flue gas condition, is characterized in that: described expanding agent is methenamine, the mixture of one or more in active carbon and polyethylene glycol.
5. be applicable to as claimed in claim 1 the preparation method of the SCR denitrating catalyst of high-temperature flue gas condition, it is characterized in that: described converted starch is the grafting polyacrylic acid copolymerized thing of bydroxyethyl starch ether the mixture of one or more in the lactide copolymer grafted and HES grafting caprolactone copolymer of HES.
6. the preparation method who is applicable to as claimed in claim 1 the SCR denitrating catalyst of high-temperature flue gas condition, is characterized in that: in described nano grade titanium tungsten powder, containing tungstic acid quality, be 5% ~ 8%.
7. the preparation method who is applicable to as claimed in claim 1 the SCR denitrating catalyst of high-temperature flue gas condition, is characterized in that: the glass diameter of described glass fibre is 10 ~ 13 μ m.
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| CN108283921A (en) * | 2018-01-10 | 2018-07-17 | 北京国电龙源环保工程有限公司 | 60 hole SCR denitration modules and preparation method thereof |
| CN108295865B (en) * | 2018-03-02 | 2024-03-22 | 河北工业大学 | Integral honeycomb low-temperature SCR denitration catalyst and preparation method thereof |
| CN109012645A (en) * | 2018-08-09 | 2018-12-18 | 江苏龙净科杰环保技术有限公司 | Perforated tubular denitrating catalyst and preparation method thereof |
| CN109876795A (en) * | 2019-04-04 | 2019-06-14 | 上海理工大学 | A kind of cerium tungsten titanium composite oxide SCR denitration and preparation method thereof |
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