CN102755898A - Semiconductor control rectifier (SCR) denitration catalytic agent applicable to high ash-laden gas condition and preparation method thereof - Google Patents
Semiconductor control rectifier (SCR) denitration catalytic agent applicable to high ash-laden gas condition and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a semiconductor control rectifier (SCR) denitration catalytic agent applicable to a high ash-laden gas condition and a preparation method thereof and belongs to the technical field of catalysis. A surface active agent, a sizing agent, a lubricating agent and the like are added when a vanadium tungsten titanium system denitration catalytic agent is prepared, a secondary micro structure and reasonable pore diameter distribution are formed through secondary drying and burning, and the SCR denitration catalytic agent applicable to the high ash-laden gas condition is prepared. The bore diameter of prepared denitration catalytic agent is no less than 6.4mm, extrusion pressure at extrusion molding is small, surface is smooth, frictional factor is small, adherence of dust on the surface of the catalytic agent is difficult, clogging and poisoning risks of the honeycomb-type catalytic agent under the high ash-laden gas condition are reduced, added metallic oxide further improves anti-poisoning capability of the catalytic agent, adaptability of the denitration catalytic agent under the high ash-laden gas condition is improved, and the denitration catalyst technology breaks through under the high ash-laden gas condition.
Description
Technical field
The present invention relates to a kind of SCR denitrating catalyst that is applicable to high ash-laden gas condition and preparation method thereof, the honeycomb fashion denitrating catalyst that uses this kind method preparation at dust content up to 30 ~ 55g/Nm
3In time, still has good nitrogen oxide removal efficiency and resists the stifled anti-poisoning performance of ash, belongs 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 can't satisfy the requirement of existing discharge standard, and the coal-burning power plant uses SCR (SCR) technology because of its high-efficiency reliable denitration performance has begun at home.The cardinal principle of SCR is with NH
3Be reducing agent, under the effect of denitrating catalyst, optionally with NO
xBe reduced into N
2
At present most widely used is vanadium tungsten titanium catalyst, because its catalyst activity temperature is higher, scope thereby is used in thermal power plant and to be adopted high dust-laden arrangement about 300 ~ 430 ℃, promptly is arranged in after the boiler economizer, before the air preheater.Though catalyst has higher activity and anti-sulphur water repelling property on this position; But residing flue gas environmental condition is more abominable; Heavy metal concentration higher like dust concentration, dust absorption is more high, makes catalyst be under easy to wear, the easy condition of stopping up, being prone to poison, and makes catalyst need frequent regular maintenance (as blowing grey cleaning); And shortened service life greatly, increased operating cost.The catalyst edge hardening bath of Jiangsu Longyuan Catalyst Co., Ltd.'s invention has solved the easy to wear problem (patent No. CN101474581) of catalyst under high ash-laden gas condition well; In order to continue to solve easy obstruction and the easy situation of poisoning that the SCR denitrating catalyst exists under high ash-laden gas condition; The present invention has studied a kind of preparation method who is applicable to the SCR denitrating catalyst of high ash-laden gas condition, and is significant.
Summary of the invention
The objective of the invention is to overcome above-mentioned weak point, a kind of preparation method who is applicable to the SCR denitrating catalyst of high ash-laden gas condition is provided, use the denitrating catalyst aperture of this method preparation to be not less than 6.4mm; Have secondary micro-structural and rational pore-size distribution; Smooth surface, coefficient of friction is little, is unfavorable for dust adhering at catalyst surface; Reduced stifled ash and the poisoning risk of catalyst under high ash-laden gas condition, make the honeycomb fashion catalyst at dust content up to 30 ~ 55g/Nm
3In time, still has good nitrogen oxide removal efficiency and resists the stifled anti-poisoning performance of ash, improved the adaptability of denitrating catalyst under high ash-laden gas condition.
According to technical scheme provided by the invention, be applicable to the preparation method of the SCR denitrating catalyst of high ash-laden gas condition, step is by weight:
(1) preparation of ammonium metavanadate solution: take by weighing 2.6 ~ 5.2 parts of ammonium metavanadates, 70 ~ 90 ℃ with the ammonium metavanadate stirring and dissolving that takes by weighing in the aqueous solution that contains 1 ~ 2.6 part of monoethanolamine; The concentration of aqueous solution of said monoethanolamine is 0.1 ~ 5g/mL;
(2) preparation of metallic salt solution: get in the deionized water that 0 ~ 10 part of metallic salt is dissolved in 0 ~ 80 part;
(3) mixed once: take by weighing 80 ~ 95 parts of nano grade titanium tungsten powders; Add 2 ~ 5 parts of surfactants therein, 90 ~ 100 parts of deionized waters are heated to 70 ~ 90 ℃; Stirring 20 ~ 40min when keeping constant temperature makes mixture become graininess; Add 3 ~ 15 parts of glass fibres more therein, the back that stirs adds the ammonium metavanadate solution of step (1) preparation, metallic salt solution and 5 ~ 10 parts of sizing agents of step (2) preparation, is heated to 70 ~ 90 ℃ after the mixing; Keep constant temperature to stir simultaneously to mixture and become graininess, form one time micro-structural;
(4) once extrude drying and calcining: the micro-structural that step (3) is obtained is extruded into strip and block on extruder; With its dry 8 ~ 20h under 50 ~ 70 ℃ of conditions, under 300 ~ 400 ℃ of conditions, calcine 4 ~ 8h then, the solid after obtaining calcining;
(5) secondary mixes: the solid that step (4) obtains is pulverized, added 5 ~ 15 parts of adhesives therein, and 5 ~ 10 parts of sizing agents, 1 ~ 5 part of lubricant, stirring to mixture becomes graininess, forms the secondary micro-structural;
(6) secondary is extruded drying and calcining: the secondary micro-structural that step (5) is obtained is equipped with at front end carries out the hot-extrudable cellular solid that becomes on the extruder of catalyst mould; With its dry 5 ~ 10h under 50 ~ 70 ℃ of conditions, dry 8 ~ 12h under 100 ~ 120 ℃ temperature conditions then; Under 550 ~ 700 ℃ of conditions, calcine 4 ~ 8h at last, obtain the SCR denitrating catalyst that product is applicable to high ash-laden gas condition.
Active ingredient formula rate in the said product is following by weight: TiO
270 ~ 90 parts, WO
33 ~ 10 parts, V
2O
52 ~ 4 parts, 0 ~ 10 part of metal oxide, 3 ~ 15 parts in glass fibre.
Said metallic salt is the nitrate of Ni, Sr, Co, Cr and Cu or one or more the mixture in the acetate.
Said surfactant is the alkyl dimethyl betaine, the mixture of one or more in alkyl dimethyl sulfoethyl betaine and the sodium dodecyl aminopropionitrile, and it mainly is a lubrication, cooperates expressing technique.
Said sizing agent is an emulsion rosin, the mixture of one or more in fibrin reaction glue and the AKD emulsion.
Said adhesive is a cellulose esters, polyvinyl alcohol, the mixture of one or more in epoxy resin and the polyacrylate.
Said lubricant is an indanthrene, polyurea grease, the mixture of one or more in fatty acid amide and the oleic acid.
The content of trioxygen-containing tungsten is 5% ~ 8% in the said nano grade titanium tungsten powder, handles through conducting modification of surface hydroxy group, and the BET specific area is less than 70m
2/ g, the X-ray diffraction peak height is greater than 160mm.
The glass diameter of said glass fibre is 10 ~ 13 μ m.
Said catalyst mould is that the discharge end of Jiangsu Longyuan Catalyst Co., Ltd. invention has a kind of in the ceramic honeycomb catalyst mould (CN201353824) of chamfering or rounding, and its aperture is not less than 6.4mm.
The present invention has following advantage: the catalyst aperture of the present invention's preparation is not less than 6.4mm; After redrying and calcining, form secondary micro-structural and rational pore-size distribution; In the preparation process, add adhesive, extrusion pressure was little when sizing agent and lubricant etc. made extrusion molding, smooth surface; Coefficient of friction is little; Be unfavorable for that dust in the adhering to of catalyst surface, has reduced stifled ash and the poisoning risk of honeycomb fashion catalyst under high ash-laden gas condition, the metal oxide of interpolation has also further improved the anti-poisoning capability of catalyst.Therefore, the honeycomb fashion catalyst that uses the preparation of this method at dust content up to 30 ~ 55g/Nm
3In time, still has good nitrogen oxide removal efficiency and resists the stifled anti-poisoning performance of ash, improved the adaptability of denitrating catalyst under high ash-laden gas condition, realizes the breakthrough of denitrating catalyst technology under high ash-laden gas condition.
The specific embodiment
Below in conjunction with specific embodiment the present invention is described further.
Ammonium metavanadate is available from Dalian milky way metal material Co., Ltd in following examples; Monoethanolamine is available from the fertile chemical industry Co., Ltd of Zibo Lay; Metallic salt is available from Chemical Reagent Co., Ltd., Sinopharm Group; The titanium tungsten powder is available from Sichuan Huatie Vanadium Titanium Technology Co., Ltd.; Surfactant is available from Shanghai Ke Huagong Co., Ltd of heap of stone; Glass fibre is available from the emerging fiberglass products in Nanjing Co., Ltd; Sizing agent is available from Qingzhou vast and boundless chemical industry of gold Co., Ltd, and adhesive is available from Wuxi City Kang Heng chemicals Co., Ltd; Lubricant is available from the big trade Co., Ltd in storehouse, Shanghai.
Embodiment 1 is applicable to the preparation method of the SCR denitrating catalyst of high ash-laden gas condition, comprises following processing step:
(1) preparation of ammonium metavanadate solution: take by weighing ammonium metavanadate 2.6kg, 90 ℃ with the ammonium metavanadate stirring and dissolving that takes by weighing in the aqueous solution of 1.2kg monoethanolamine, the concentration of aqueous solution of monoethanolamine is 1g/mL;
(2) preparation of metallic salt solution: get 5.8kg nickel nitrate and 2.0kg strontium nitrate and be dissolved in the deionized water of 40L;
(3) mixed once: take by weighing the nano grade titanium tungsten powder 90kg of trioxygen-containing tungsten quality 5%, add 2kg alkyl dimethyl betaine therein, the 90L deionized water; Be heated to 75 ℃; Keep constant temperature to stir simultaneously and made mixture become graininess in 20 minutes, add the 5.5kg glass fibre more therein, the back that stirs adds the ammonium metavanadate solution of preparation in the step (1); The metallic salt solution of preparation in the step (2); 5kg emulsion rosin is heated to 75 ℃, keeps constant temperature to stir simultaneously to mixture and becomes graininess;
(4) once extrude drying and calcining: the solid that step (3) is obtained simply is extruded into strip and block on extruder; Drying is 10 hours under 50 ℃ of conditions; Under 300 ℃ of conditions, calcined 5 hours then;
(5) secondary mixes: the solid that step (4) obtains is pulverized, added the 6kg cellulose esters therein, and 6kg emulsion rosin, the 1.5kg indanthrene, stirring to mixture becomes graininess;
(6) secondary is extruded drying and calcining: the solid that step (5) is obtained is equipped with at front end and carries out on the extruder of catalyst mould that the aperture is 6.5mm hot-extrudablely becoming cellular; Under 50 ℃ of conditions dry 6 hours, drying 8 hours under 105 ℃ temperature conditions then; Under 570 ℃ of conditions, calcined 8 hours at last, obtain the SCR denitrating catalyst that product is applicable to high ash-laden gas condition.
Wherein, TiO
2Weight accounts for 85.5% in total catalyst weight, WO
3Weight accounts for 4.5% in total catalyst weight, V
2O
5Weight accounts for 2% in total catalyst weight, strontium oxide strontia weight accounts for 1% in total catalyst weight, and nickel oxide weight accounts for 1.5% in total catalyst weight, and glass fibre weight accounts for 5.5% in total catalyst weight.
Active detection is as shown in table 1.
Embodiment 2 is applicable to the preparation method of the SCR denitrating catalyst of high ash-laden gas condition, comprises following processing step:
(1) preparation of ammonium metavanadate solution: take by weighing ammonium metavanadate 5.2kg, 75 ℃ with the ammonium metavanadate stirring and dissolving that takes by weighing in the aqueous solution of 2.6kg monoethanolamine, the concentration of aqueous solution of monoethanolamine is 1.2g/mL;
(2) preparation of metallic salt solution: get 7.8kg cobalt nitrate and 2.0kg strontium nitrate and be dissolved in the deionized water of 35L;
(3) mixed once: take by weighing the nano grade titanium tungsten powder 88kg of trioxygen-containing tungsten quality 6%, add 3kg alkyl dimethyl sulfoethyl betaine therein, the 92L deionized water; Be heated to 80 ℃; Keep constant temperature to stir simultaneously and made mixture become graininess in 24 minutes, add the 5kg glass fibre more therein, the back that stirs adds the ammonium metavanadate solution of preparation in the step (1); The metallic salt solution of preparation in the step (2); 6kg fibrin reaction glue is heated to 80 ℃ after the mixing, keep constant temperature to stir simultaneously to mixture and become graininess;
(4) once extrude drying and calcining: the solid that step (3) is obtained simply is extruded into strip and block on extruder; With the solid that obtains under 60 ℃ of conditions dry 11 hours; Under 350 ℃ of conditions, calcined 6 hours at last;
(5) secondary mixes: the solid that step (4) obtains is pulverized, added the 6kg polyvinyl alcohol therein, and 6kg fibrin reaction glue, the 2kg polyurea grease, stirring to mixture becomes graininess; Form the secondary micro-structural;
(6) secondary is extruded drying and calcining: the solid that step (5) is obtained is equipped with at front end and carries out on the extruder of catalyst mould that the aperture is 6.8mm hot-extrudablely becoming cellular; Under 60 ℃ of conditions dry 7 hours, drying 9 hours under 110 ℃ temperature conditions then; Under 600 ℃ of conditions, calcined 6 hours at last, obtain the SCR denitrating catalyst that product is applicable to high ash-laden gas condition.
Wherein, TiO
2Weight accounts for 82.7% in total catalyst weight, WO
3Weight accounts for 5.3% in total catalyst weight, V
2O
5Weight accounts for 4% in total catalyst weight, strontium oxide strontia weight accounts for 1% in total catalyst weight, and cobalt oxide weight accounts for 2% in total catalyst weight, and glass fibre weight accounts for 5% in total catalyst weight.
Active detection is as shown in table 1.
Embodiment 3 is applicable to the preparation method of the SCR denitrating catalyst of high ash-laden gas condition, comprises following processing step:
(1) preparation of ammonium metavanadate solution: take by weighing ammonium metavanadate 3.9kg, 80 ℃ with the ammonium metavanadate stirring and dissolving that takes by weighing in the aqueous solution of 1.6kg monoethanolamine, the concentration of aqueous solution of monoethanolamine is 0.9g/mL;
(2) preparation of metallic salt solution: get 9.1kg copper nitrate and 4.1kg strontium nitrate and be dissolved in the deionized water of 45L;
(3) mixed once: take by weighing the nano grade titanium tungsten powder 87kg of trioxygen-containing tungsten quality 7%, add the 2.5kg sodium dodecyl aminopropionitrile therein, the 95L deionized water; Be heated to 90 ℃; Keep constant temperature to stir simultaneously and made mixture become graininess in 30 minutes, add the 5kg glass fibre more therein, the back that stirs adds the ammonium metavanadate solution of preparation in the step (1); The metallic salt solution of preparation in the step (2); The 6kgAKD emulsion is heated to 90 ℃ after the mixing, keep constant temperature to stir simultaneously to mixture and become graininess;
(4) once extrude drying and calcining: the solid that step (3) is obtained simply is extruded into strip and block on extruder; Drying is 12 hours under 55 ℃ of conditions; Calcining is 5.5 hours under 380 ℃ of conditions;
(5) secondary mixes: the solid that step (4) obtains is pulverized, added the 6kg polyacrylate therein, and 6kg AKD emulsion, the 2.5kg fatty acid amide, stirring to mixture becomes graininess;
(6) secondary is extruded drying and calcining: the solid that step (5) is obtained is equipped with at front end and carries out on the extruder of catalyst mould that the aperture is 7.1mm hot-extrudablely becoming cellular; Under 55 ℃ of conditions dry 9 hours, drying 10 hours under 108 ℃ temperature conditions then; Under 650 ℃ of conditions, calcined 5.5 hours at last, obtain the SCR denitrating catalyst that product is applicable to high ash-laden gas condition.
Wherein, TiO
2Weight accounts for 80.9% in total catalyst weight, WO
3Weight accounts for 6.1% in total catalyst weight, V
2O
5Weight accounts for 3% in total catalyst weight, strontium oxide strontia weight accounts for 2% in total catalyst weight, and cupric oxide weight accounts for 3% in total catalyst weight, and glass fibre weight accounts for 5% in total catalyst weight.
Active detection is as shown in table 1.
Reaction condition: dustiness 45g/Nm
3, air speed 4,000h
-1, NO content 400ppm, NH
3Content 324ppm, SO
2Content 500ppm, H
2O content 10%, N
2Be balance gas.
Table 1 is applicable to the active testing result of the SCR denitrating catalyst of high ash-laden gas condition
| Catalyst | 320 ℃ of denitration efficiencies (%) | 350 ℃ of denitration efficiencies (%) | 380 ℃ of denitration efficiencies (%) |
| Embodiment one | 79.7 | 80.4 | 80.9 |
| Embodiment two | 80.4 | 80.7 | 80.9 |
| Embodiment three | 80.2 | 80.6 | 80.9 |
Can know by last table, in the reaction atmosphere dustiness up to 45g/Nm
3Condition under, SCR denitrating catalyst prepared according to the methods of the invention still has favorable denitrification efficient.
The above content is merely 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 (9)
1. be applicable to the preparation method of the SCR denitrating catalyst of high ash-laden gas condition, it is characterized in that step is by weight:
(1) preparation of ammonium metavanadate solution: take by weighing 2.6 ~ 5.2 parts of ammonium metavanadates, 70 ~ 90 ℃ with the ammonium metavanadate stirring and dissolving that takes by weighing in the aqueous solution that contains 1 ~ 2.6 part of monoethanolamine; The concentration of aqueous solution of said monoethanolamine is 0.1 ~ 5g/mL;
(2) preparation of metallic salt solution: get in the deionized water that 0 ~ 10 part of metallic salt is dissolved in 0 ~ 80 part;
(3) mixed once: take by weighing 80 ~ 95 parts of nano grade titanium tungsten powders; Add 2 ~ 5 parts of surfactants therein, 90 ~ 100 parts of deionized waters are heated to 70 ~ 90 ℃; Stirring 20 ~ 40min when keeping constant temperature makes mixture become graininess; Add 3 ~ 15 parts of glass fibres more therein, the back that stirs adds the ammonium metavanadate solution of step (1) preparation, metallic salt solution and 5 ~ 10 parts of sizing agents of step (2) preparation, is heated to 70 ~ 90 ℃ after the mixing; Keep constant temperature to stir simultaneously to mixture and become graininess, form one time micro-structural;
(4) once extrude drying and calcining: the micro-structural that step (3) is obtained is extruded into strip and block on extruder; With its dry 8 ~ 20h under 50 ~ 70 ℃ of conditions, under 300 ~ 400 ℃ of conditions, calcine 4 ~ 8h then, the solid after obtaining calcining;
(5) secondary mixes: the solid that step (4) obtains is pulverized, added 5 ~ 15 parts of adhesives therein, and 5 ~ 10 parts of sizing agents, 1 ~ 5 part of lubricant, stirring to mixture becomes graininess, forms the secondary micro-structural;
(6) secondary is extruded drying and calcining: the secondary micro-structural that step (5) is obtained is equipped with at front end carries out the hot-extrudable cellular solid that becomes on the extruder of catalyst mould; With its dry 5 ~ 10h under 50 ~ 70 ℃ of conditions, dry 8 ~ 12h under 100 ~ 120 ℃ temperature conditions then; Under 550 ~ 700 ℃ of conditions, calcine 4 ~ 8h at last, obtain the SCR denitrating catalyst that product is applicable to high ash-laden gas condition.
2. the said SCR denitrating catalyst that is applicable to high ash-laden gas condition of claim 1, it is characterized in that: the active ingredient formula rate in the said product is following by weight: TiO
270 ~ 90 parts, WO
33 ~ 10 parts, V
2O
52 ~ 4 parts, 0 ~ 10 part of metal oxide, 3 ~ 15 parts in glass fibre.
3. be applicable to the preparation method of the SCR denitrating catalyst of high ash-laden gas condition according to claim 1, it is characterized in that said metallic salt is the nitrate of Ni, Sr, Co, Cr and Cu or one or more the mixture in the acetate.
4. be applicable to the preparation method of the SCR denitrating catalyst of high ash-laden gas condition according to claim 1; It is characterized in that: said surfactant is the alkyl dimethyl betaine, the mixture of one or more in alkyl dimethyl sulfoethyl betaine and the sodium dodecyl aminopropionitrile.
5. be applicable to the preparation method of the SCR denitrating catalyst of high ash-laden gas condition according to claim 1, it is characterized in that: said sizing agent is an emulsion rosin, the mixture of one or more in fibrin reaction glue and the AKD emulsion.
6. be applicable to the preparation method of the SCR denitrating catalyst of high ash-laden gas condition according to claim 1, it is characterized in that: said adhesive is a cellulose esters, polyvinyl alcohol, the mixture of one or more in epoxy resin and the polyacrylate.
7. be applicable to the preparation method of the SCR denitrating catalyst of high ash-laden gas condition according to claim 1,
It is characterized in that: said lubricant is an indanthrene, polyurea grease, the mixture of one or more in fatty acid amide and the oleic acid.
8. be applicable to the preparation method of the SCR denitrating catalyst of high ash-laden gas condition according to claim 1, it is characterized in that: the content of trioxygen-containing tungsten is 5% ~ 8% in the said nano grade titanium tungsten powder.
9. be applicable to the preparation method of the SCR denitrating catalyst of high ash-laden gas condition according to claim 1, it is characterized in that: the glass diameter of said glass fibre is 10 ~ 13 μ m.
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| CN111905716B (en) * | 2020-07-31 | 2021-09-24 | 江苏龙净科杰环保技术有限公司 | Thallium poisoning resistant core-shell honeycomb catalyst for cement kiln flue gas denitration and preparation method thereof |
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| CN113996309B (en) * | 2021-11-23 | 2023-12-26 | 国能龙源催化剂江苏有限公司 | Preparation method of high-strength SCR catalyst for CO-removal |
| CN114602459A (en) * | 2022-03-27 | 2022-06-10 | 山东亮剑环保新材料有限公司 | Composite denitration catalyst and production method thereof |
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