CN101676024A - Faviform ammonia-method selective-catalytic-reduction denitrified catalyst and preparation method thereof - Google Patents

Faviform ammonia-method selective-catalytic-reduction denitrified catalyst and preparation method thereof Download PDF

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CN101676024A
CN101676024A CN200810212081A CN200810212081A CN101676024A CN 101676024 A CN101676024 A CN 101676024A CN 200810212081 A CN200810212081 A CN 200810212081A CN 200810212081 A CN200810212081 A CN 200810212081A CN 101676024 A CN101676024 A CN 101676024A
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catalyst
faviform
catalytic
ammonia
selective
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CN200810212081A
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Chinese (zh)
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马少丹
赵晓林
孙海军
何冬青
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晶锐瓷业(北京)有限公司
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Abstract

The invention relates to a faviform ammonia-method selective-catalytic-reduction denitrified catalyst and a preparation method thereof. The invention is characterized in that the catalyst uses TiO2 with a special specific surface area as the carrier and uses V2O5 and WO3 as the catalyst and the cocatalyst, various assistants favorable for the catalyst to form, disperse and perforate are simultaneously added, and the faviform denitrified catalyst is obtained in short drying time and calcination time. The catalyst comprises the following components in weight percent: 80-99% of TiO2, 0.1-2% of V2O5 and 5-10% of WO3. The method selects the TiO2 with the special specific surface area as the carrier, simultaneously adds the proper forming assistants and combines the special preparation techniqueso as to obtain the faviform denitrified catalyst with high strength and favorable forming performance and enhance the denitration activity of the catalyst; when the trial denitration test is carriedout on the faviform denitrified catalyst in a small-size coal burning boiler, the airspeed is 5000/hr, and the concentration of NOX is about 100 ppmv; when the fume temperature is 350 DEG C, the denitration efficiency reaches 95%; and after long-term operation, the denitration efficiency is still above 80%.

Description

A kind of Faviform ammonia-method selective-catalytic-reduction denitrified catalyst and preparation method thereof

Technical field

The present invention relates to a kind of Faviform ammonia-method selective-catalytic-reduction denitrified catalyst and preparation method thereof

Background technology

Nitrogen oxide (NOx) is one of major pollutants of atmospheric environment, it is one of main source of acid rain, can cause serious destruction to environment, for human, nitrogen oxide belongs to toxic and harmful, and human body directly sucks, and can damage nervous centralis and lung tissue, NOx in the atmosphere also can generate the bigger photochemical fog of toxicity under certain condition, causes the withered and crowd's death of plant.Nitrogen oxide mainly comes from the industrial processes of vehicle exhaust, heat power station and other industrial fuel combustions and nitric acid, nitrogenous fertilizer, explosive, maximum with the quantity that produces in the fuel combustion process, account for more than 30%, wherein the 70% direct burning that comes from coal.SCR (SCR) method that with NH3 is reducing agent is the effective method of present denitrating flue gas, and it mainly adopts V 2O 5-WO 3/ TiO 2Catalyst, such catalyst eighties of last century the seventies and eighties has begun industrialization production abroad, has good activity and anti-water and SO2 performance.

Present commercial V 2O 5-WO 3/ TiO 2Class SCR denitrating catalyst mainly contains three kinds of forms: honeycomb fashion, flat and corrugated plate dst.Flat and corrugated plate dst catalyst is to coat certain thickness active material on the metallic support surface, and metallic supports does not have catalytic activity, so its persistence and wear resistance are relatively poor; Simultaneously owing to when practical application, be subject to the specification of floor height, the flexibility deficiency, two-layer catalyst setting in each framework is for later replacing brings certain inconvenience.The honeycomb fashion catalyst has uniform physical chemistry structure, possess stronger anti-poisoning capability and wearability, thereby service life is longer, and the production technology of extruded type makes it possess the ability that volume and performance are complementary, and needs how long just can cut as required.And, because the major accident of catalyst is caused by the burning of dust stratification that generally the honeycomb fashion catalyst can be not combustion-supporting owing to all being made by ceramics based active material, and is safe and reliable; Flat and corrugated plate dst catalyst has metal architecture, can cause the destruction of whole catalyst during breaking out of fire.

Chinese east Dongfang Boiler (Group) Co., Ltd. of electric group in 2005 and German KWH build Chengdu Dongfang KWH Environmental Protection Catalysts Co., Ltd jointly, a complete set of technology and equipment of introducing German KWH company.The intervention of offshore company has caused not autonomous on China's technology and equipment, causes passive on economic right, can suppress the growth of Chinese domestic enviromental protection enterprise, and China does not still have the vanadium based denitration catalyst of industrialized independent intellectual property right.Therefore accelerate the denitrating catalyst of the national independent intellectual property right of research, become the significant problem that each enviromental protection enterprise of China and R﹠D institution need to be resolved hurrily.

At present domestic patent about denitrating catalyst of having applied for has tens of kinds more than, the patent disclosure of Chinese patent application CN03122008.8 a kind of extrusion molding of honeycomb molded body cellular catalyst for treating waste gas good, that constitute by the powder of titanium dioxide and/or titanium composite oxide with raw material and the catalyst that uses high de-agglomeration activity this raw material, that have organic halogen compound and high denitrification activity.At 300 ℃, air speed is 10000hr -1Situation under, denitration efficiency preferably reaches 95%, but the TiO of this kind denitrating catalyst that this patent is announced 2The powder process complexity is to carrier TiO 2The character of powder requires comparatively harsh.The patent disclosure of Chinese patent application numbers 200710097827.9 a kind of Ti-base catalyst and preparation method who is used for coal steam-electric plant smoke SCR denitration.This catalyst is with 80~99% TiO 2With 1~20% sieve and silica-sesquioxide be carrier, extrude and be honeycomb ceramics, then with the method for dipping at honeycomb ceramics surface-coated active component V 2O 5And WO 3Owing to be surface-coated, so the vanadium load capacity is higher, and wear-corrosion resistance is poor.

Summary of the invention

The objective of the invention is to, according to present status in China, provide a kind of preparation technology simple relatively, intensity height, Faveolate denitration catalyst that denitration activity is high and preparation method thereof.

The Faviform ammonia-method selective-catalytic-reduction denitrified catalyst that the present invention proposes is characterized in that described catalyst is with TiO 2Be carrier, V 2O 5Be active component, WO 3Be co-catalyst.

Said catalyst carrier TiO 2With Detitanium-ore-type TiO 2Be raw material, specific area is at 90m 2About/g, content is 80% of catalyst weight percentage composition.

Above-mentioned activity of such catalysts component V 2O 5Form with ammonium metavanadate adds, and content is the 0.1%-5% of catalyst weight percentage composition, co-catalyst WO 3Form with ammonium paratungstate adds, and content is the 1%-20% of catalyst weight percentage composition.

Above-mentioned catalyst adds various auxiliary agents such as clay, methylcellulose, PEO, Ludox, glass fibre, MEA in preparation process.

The Faviform ammonia-method selective-catalytic-reduction denitrified catalyst that the present invention proposes is characterized in that catalyst preparation process comprises the steps:

(1) preparation of carrier slurry

Get TiO 2Powder is to add 60 ℃ warm water under 60~80 ℃ of water bath condition to stir in temperature, obtains the carrier slurry;

(2) adding of the load of active component and other auxiliary agents

Get in whipping process in the carrier slurry that ammonium metavanadate and ammonium paratungstate slowly join step (1), add various auxiliary agents then, it is suitable to continue to be stirred to water content;

(3) pug mill mixes with old

Transfer in the vacuum deairing machine through the suitable slurry that is stirred to water content in the step (2) and mix, keeping old under the constant situation of humidity, continue then to mix then, it is half an hour that pug is practiced the system time at every turn, the old time is 8 hours, so repeatedly for several times, obtains practicing the pug that makes;

(4) extrusion molding

Practicing the pug that makes in the step (3) is honeycomb ceramics through extruder for shaping.

(5) drying of catalyst and roasting

The honeycomb ceramics of extrusion molding is dry in the controlled drying box of controlled humidity, rate of drying in the step (4), baking temperature is 60~100 ℃, and be 3~6 days drying time, calcines through electric furnace again, 300~600 ℃ of roasting 12~24h obtain final honeycombed catalyst.

The present invention selects the anatase titanium dioxide TiO with certain specific surface area for use 2Be carrier, add the V of different amounts 2O 5Special slurrying, drying and roasting technique, prepared the honeycomb-shaped SCR denitrating catalyst that processability is good, intensity is big, denitration efficiency is high, overcome the fragility and a cracking difficult problem of ceramic material in the catalyst activation temperature interval, simultaneously through pilot-scale experiment as can be known this catalyst have more lasting activity, be installed in small scall coal-fired boiler, air speed is 5000/hr, NO XConcentration is about 100ppmv, and when flue-gas temperature was 350 ℃, after the long-time running, denitration effect was still more than 80%.

The specific embodiment

Below in conjunction with embodiment technical characterictic of the present invention is further specified:

Embodiment 1

Get TiO 2Powder is to add 60 ℃ warm water under 80 ℃ of water bath condition to stir in temperature, obtains the carrier slurry; Get ammonium metavanadate and ammonium paratungstate and slowly join in the carrier slurry that stirs in whipping process, the addition of ammonium metavanadate and ammonium paratungstate is converted into V 2O 5Later and the TiO with WO3 2Ratio be 1: 4: 45, add various auxiliary agent clays, methylcellulose, PEO, Ludox, glass fibre, MEA then, continue to be stirred to transfer in the vacuum deairing machine after water content suits and mix, practicing the system time is half an hour, practice the pug that makes and keeping old under the constant situation of humidity, the old time is 8 hours, continues then to mix, so repeatedly for several times; Final to practice the pug that makes be honeycomb ceramics through extruder for shaping, and dry in the controlled drying box of controlled humidity, rate of drying then, baking temperature is 60 ℃, be 6 days drying time, through the electric furnace calcining, 550 ℃ of roasting 12h obtain final honeycombed catalyst again.

The catalyst denitration activity method of testing that makes is: in the small scall coal-fired boiler of trying out during the honeycomb catalyst for preparing is installed in, test is through the concentration of NO in the flue gas before the catalyst and the concentration of the NO after the process catalyst respectively, thereby calculate the conversion ratio of NO, obtain the denitration efficiency of catalyst.

Can obtain from the denitration test result, be 350 ℃ in flue-gas temperature, and NO concentration is about 100ppmv, and air speed is under the condition of 5000/hr, and initial denitration efficiency reaches 90%.After 200 hours, test its denitration efficiency, still more than 80%.

Embodiment 2

Get TiO 2Powder is to add 60 ℃ warm water under 70 ℃ of water bath condition to stir in temperature, obtains the carrier slurry; Get ammonium metavanadate and ammonium paratungstate and slowly join in the carrier slurry that stirs in whipping process, the addition of ammonium metavanadate and ammonium paratungstate is converted into V 2O 5Later and the TiO with WO3 2Ratio be 1: 8: 91, add various auxiliary agent clays, methylcellulose, PEO, Ludox, glass fibre, MEA then, continue to be stirred to transfer in the vacuum deairing machine after water content suits and mix, practicing the system time is half an hour, practice the pug that makes and keeping old under the constant situation of humidity, the old time is 8 hours, continues then to mix, so repeatedly for several times; Final to practice the pug that makes be honeycomb ceramics through extruder for shaping, and dry in the controlled drying box of controlled humidity, rate of drying then, baking temperature is 80 ℃, be 5 days drying time, through the electric furnace calcining, 500 ℃ of roasting 24h obtain final honeycombed catalyst again.

The catalyst denitration activity method of testing that makes is with embodiment 1.In flue-gas temperature is 350 ℃, and NO concentration is about 100ppmv, air speed be under the condition of 5000/hr denitration efficiency more than 90%.

Embodiment 3

Get TiO 2Powder is to add 60 ℃ warm water under 70 ℃ of water bath condition to stir in temperature, obtains the carrier slurry; Take by weighing the ammonium paratungstate and the ammonium metavanadate powder of respective quality, slowly join concentration be under 60 ℃ of water-baths in 5% the oxalic acid solution, after waiting to dissolve, join in the above-mentioned slurry again and continue to stir, the addition of ammonium metavanadate and ammonium paratungstate is converted into V 2O 5Later and the TiO with WO3 2Ratio be 1.6: 8: 80, add various auxiliary agent clays, methylcellulose, PEO, Ludox, glass fibre, MEA then, continue to be stirred to transfer in the vacuum deairing machine after water content suits and mix, practicing the system time is half an hour, practice the pug that makes and keeping old under the constant situation of humidity, the old time is 8 hours, continues then to mix, so repeatedly for several times; Final to practice the pug that makes be honeycomb ceramics through extruder for shaping, and dry in the controlled drying box of controlled humidity, rate of drying then, baking temperature is 60 ℃, be 3 days drying time, through the electric furnace calcining, 450 ℃ of roasting 24h obtain final honeycombed catalyst again.

The catalyst denitration activity method of testing that makes is with embodiment 1.In flue-gas temperature is 350 ℃, and NO concentration is about 100ppmv, and air speed is that denitration efficiency is 87% under the condition of 5000/hr.

Embodiment 4

Take by weighing the TiO of certain mass 2Powder stirs under 60 ℃ of water-baths and obtains carrier TiO 2Slurry.The ammonium paratungstate that takes by weighing respective quality then joins in the above-mentioned slurry and continues to stir, and the ammonium paratungstate addition is converted into after the WO3 and TiO 2Ratio be 1: 10, stir later slurry in drying box 100 ℃ dry 2 hours down, 500 ℃ of calcinings 5 hours down in Muffle furnace then, calcined product sieves through grinding, obtains WO3/TiO 2Powder.Getting the following powder of 100 quantitative orders is to add 60 ℃ warm water under 80 ℃ of water bath condition to stir in temperature, obtains the carrier slurry; In whipping process, get the ammonium metavanadate powder and slowly join in the carrier slurry that stirs ammonium metavanadate, ammonium paratungstate and TiO 2Ratio be 1: 4: 40, add various auxiliary agent clays, methylcellulose, PEO, Ludox, glass fibre, MEA then, continue to be stirred to transfer in the vacuum deairing machine after water content suits and mix, practicing the system time is half an hour, practice the pug that makes and keeping old under the constant situation of humidity, the old time is 8 hours, continues then to mix, so repeatedly for several times; Final to practice the pug that makes be honeycomb ceramics through extruder for shaping, and dry in the controlled drying box of controlled humidity, rate of drying then, baking temperature is 60 ℃, be 4 days drying time, through the electric furnace calcining, 500 ℃ of roasting 20h obtain final honeycombed catalyst again.

The catalyst denitration activity method of testing that makes is with embodiment 1.In flue-gas temperature is 350 ℃, and NO concentration is about 100ppmv, and air speed is that denitration efficiency is 85% under the condition of 5000/hr.

Embodiment 5

Get TiO 2Powder is to add 60 ℃ warm water under 80 ℃ of water bath condition to stir in temperature, obtains the carrier slurry; Get ammonium metavanadate and ammonium paratungstate and slowly join in the carrier slurry that stirs in whipping process, the addition of ammonium metavanadate and ammonium paratungstate is converted into V 2O 5Later and the TiO with WO3 2Ratio be 1.6: 8: 80, add various auxiliary agent clays, methylcellulose, PEO, Ludox, glass fibre, MEA then, continue to be stirred to transfer in the vacuum deairing machine after water content suits and mix, practicing the system time is half an hour, practice the pug that makes and keeping old under the constant situation of humidity, the old time is 8 hours, continues then to mix, so repeatedly for several times; Final to practice the pug that makes be honeycomb ceramics through extruder for shaping, and dry in the controlled drying box of controlled humidity, rate of drying then, baking temperature is 60 ℃, be 6 days drying time, through the electric furnace calcining, 550 ℃ of roasting 24h obtain final honeycombed catalyst again.

The catalyst denitration activity method of testing that makes is with embodiment 1.In flue-gas temperature is 350 ℃, and NO concentration is about 100ppmv, and air speed is that denitration efficiency is 95% under the condition of 5000/hr.

Claims (6)

1 one kinds of Faviform ammonia-method selective-catalytic-reduction denitrified catalysts is characterized in that described catalyst is with TiO 2Be carrier, V 2O 5Be active component, WO 3Be co-catalyst.
2 Faviform ammonia-method selective-catalytic-reduction denitrified catalysts according to claim 1, described catalyst carrier TiO 2With Detitanium-ore-type TiO 2Be raw material, specific area is at 90m 2About/g, content is 80% of catalyst weight percentage composition.
3 Faviform ammonia-method selective-catalytic-reduction denitrified catalysts according to claim 1, active component V 2O 5Form with ammonium metavanadate adds, and content is the 0.1%-5% of catalyst weight percentage composition, co-catalyst WO 3Form with ammonium paratungstate adds, and content is the 1%-20% of catalyst weight percentage composition.
4 Faviform ammonia-method selective-catalytic-reduction denitrified catalysts according to claim 1, described catalyst adds various auxiliary agents such as clay, methylcellulose, PEO, Ludox, glass fibre, MEA in preparation process.
5 Faviform ammonia-method selective-catalytic-reduction denitrified catalysts according to claim 1 is characterized in that catalyst preparation process comprises the steps:
(1) preparation of carrier slurry
Get TiO 2Powder adds water and stirs under water bath condition, obtain the carrier slurry;
(2) adding of the load of active component and other auxiliary agents
Get in whipping process in the carrier slurry that ammonium metavanadate and ammonium paratungstate slowly join step (1), add various auxiliary agents then, it is suitable to continue to be stirred to water content;
(3) pug mill mixes with old
Transfer in the vacuum deairing machine through the suitable slurry that is stirred to water content in the step (2) and mix, keeping old under the constant situation of humidity, continue then to mix then, so repeatedly for several times, obtain practicing the pug that makes;
(4) extrusion molding
Practicing the pug that makes in the step (3) is honeycomb ceramics through extruder for shaping.
(5) drying of catalyst and roasting
The honeycomb ceramics of extrusion molding is dry in the controlled drying box of controlled humidity, rate of drying in the step (4), obtains final honeycombed catalyst through the electric furnace calcining again.
6 preparation methods according to the Faviform ammonia-method selective-catalytic-reduction denitrified catalyst described in the claim 5 is characterized in that:
In the described step (1) to TiO 2The water that adds in the powder is that temperature is 60 ℃ a warm water, and carrier slurry whipping process is to carry out under 60~80 ℃ condition of water bath heating;
The experienced at every turn system time of pug is half an hour in the described step (3), and the old time is 8 hours;
In described step (5) dry run, the method for taking controlled humidity slowly to heat up, baking temperature is 60~100 ℃, be 3~6 days drying time, again through electric furnace calcining, 300~600 ℃ of roasting 12~24h.
CN200810212081A 2008-09-17 2008-09-17 Faviform ammonia-method selective-catalytic-reduction denitrified catalyst and preparation method thereof CN101676024A (en)

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CN103586016A (en) * 2013-11-14 2014-02-19 索平 Honeycomb type selective catalytic reduction denitration catalyst and preparation method thereof
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