CN105618028A - Catalyst for coke oven smoke denitration and preparation method thereof - Google Patents
Catalyst for coke oven smoke denitration and preparation method thereof Download PDFInfo
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- CN105618028A CN105618028A CN201410606270.7A CN201410606270A CN105618028A CN 105618028 A CN105618028 A CN 105618028A CN 201410606270 A CN201410606270 A CN 201410606270A CN 105618028 A CN105618028 A CN 105618028A
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Abstract
The invention provides a catalyst for coke oven smoke denitration and a preparation method thereof. The catalyst is in the form of an overall coating structure, and has a very high geometrical outer surface. The catalyst still has good low-temperature denitration activity during high-airspeed operation, and is particularly applicable to nitrogen oxide treatment of coke oven smoke. The catalyst provided by the invention is simple in preparation process, high in solid content of blended titanium dioxide slurry, and low in viscosity, and can achieve a titanium oxide uploading capacity of 100-130g/L when used for once immersion coating of a honeycomb ceramic carrier. The prepared overall catalyst has good denitration activity and a very wide temperature window, when used for coke oven smoke denitration, under the condition that the operation airspeed is 8000-16000hr<-1>, the catalyst can achieve a denitration rate of 95-99%.
Description
Technical field
The invention belongs to field of environment protection, be specifically related to a kind of coke oven flue gas denitration Catalysts and its preparation method.
Background technology
Environmental Protection Department has issued " coking chemistry emission of industrial pollutants standard " (GB16171-2012 on June 27th, 2012; hereinafter referred to as new standard); this is that Environmental Protection Department issues the discharge standard that ambient air quality has significant impact again after 2011 " fossil-fuel power plant atmospheric pollutant emission standard " (GB13223-2011). Require that newly-built coal chemical enterprise implemented new standard from 1 day October in 2012, the level of pollution control that existing coal chemical enterprise reaches newly-built enterprise on January 1st, 2015.
New standard has received sternly SO significantly2, NOx emission limit, it is desirable in coke oven chimney combustion tail gas, SO2 concentration is less than 50mg/m3, nitrous oxides concentration is less than 500mg/m3, key area special requirement discharged nitrous oxides concentration is less than 150mg/m3��
In current domestic coal chemical enterprise coke oven flue gas, nitrous oxides concentration is generally at 800��1200mg/m3Between, substantially exceeding the emission limit of new standard-required, flue gas needs denitration to process just can accomplish nitrogen oxides qualified discharge.
SCR (SCR) method is that current tail gas denitration is the most ripe, and a kind of method that denitration efficiency is the highest. Its principle is under the effect of catalyst, sprays into the NH in tail gas3Generation N is reacted with the NOx in flue gas2. Coke-oven plant's ammonia sources is extensive, can conveniently obtain. SCR method is highly suitable for coke oven flue gas denitration.
The denitration efficiency of SCR Fa Yinqigao and technology maturity are at coal-burning power plant flue gas NOxImprovement aspect achieves successfully, at China's large-scale promotion application. Coal-burning power plant's SCR device is generally disposed at high dirt section, and temperature is between 350��400 DEG C, and for adapting to flue gas height ash feature, catalyst configuration is mainly integral extruding type, and pitch is 7��9mm. Compared with coal-burning power plant's flue gas, coke oven flue gas then has the following feature: cigarette temperature is on the low side, and temperature is typically in 260-300 DEG C, even lower at about 200 DEG C sometimes; Containing a small amount of tar in flue gas, dust is few.
Tradition coal-burning power plant with denitrating catalyst operating temperature window between 320��400 DEG C, it is impossible to for coke oven flue gas denitration.
Summary of the invention
It is an object of the invention to for above shortcomings in prior art, it is provided that a kind of coke oven flue gas denitrating catalyst and preparation method thereof. This catalyst is Bulk coat structural formula, mainly by ceramic honey comb matrix, TiO2-SiO2-WO3Coating and active component are constituted. The method low cost, simple, the Bulk coat formula denitrating catalyst prepared has good low-temperature denitration activity, it is adaptable to coke oven flue gas nitrogen oxides is administered.
In order to realize the above-mentioned purpose of the present invention, the invention provides following technical scheme:
A kind of coke oven flue gas denitrating catalyst, this catalyst is integral honeycomb ceramic coating formula catalyst, is made up of honeycomb ceramic carrier, oxide coating and active component.
According to described coke oven flue gas denitrating catalyst, wherein said honeycomb ceramic carrier is mainly cordierite or metal, and its hole density is 100��400 holes/square inch, and described oxide coating is TiO2-SiO2-WO3Composite oxides, described active component is the oxide of vanadium.
The preparation method that present invention simultaneously provides described coke oven flue gas denitrating catalyst, comprises the steps:
(1) roasting at metatitanic acid 500 DEG C is obtained titanium dioxide in 4 hours;
(2) ball milling after titanium dioxide, deionized water, Ludox, ammonia and dispersant is prepared titania slurry;
(3) with after gained titania slurry dipping honeycomb ceramic carrier, blowing out slurry unnecessary in duct, drying roasting obtains the cordierite honeycomb ceramic of loading titanium oxide and silica coating;
(4) prepare the ammonium metatungstate solution of 100��240g/L, with the ceramic honey comb of this solution impregnation loading titanium oxide coating, after drying roasting, obtain WO3/TiO2-SiO2/ cordierite honeycomb ceramic;
(5) mixed solution of preparation ammonium metavanadate and oxalic acid, wherein the concentration of ammonium metavanadate is 70��150g/L, and the concentration of oxalic acid is 140��300g/L, with this solution impregnation WO3/TiO2/ cordierite honeycomb ceramic, obtains V after drying roasting2O5/WO3/TiO2-SiO2/ cordierite honeycomb ceramic denitrating catalyst.
According to the preparation method of described coke oven flue gas denitrating catalyst, wherein in step (2), described dispersant is sodium polyacrylate or ammonium polyacrylate chelated dispersants, and its addition is the 0.5��8% of titania weight, it is preferable that 2��5%.
According to the preparation method of described coke oven flue gas denitrating catalyst, step (2) wherein adds ammonia and adjusts the pH value of slurry 8��12, it is preferable that 9��10.
According to the preparation method of described coke oven flue gas denitrating catalyst, wherein in step (2) solid content of titania slurry 40��50%.
According to the preparation method of described coke oven flue gas denitrating catalyst, wherein in step (2) viscosity of titania slurry at 0.2��0.6 pascal second.
Preparation method according to described coke oven flue gas denitrating catalyst, wherein with titania slurry dip-coating cordierite honeycomb ceramic in step (2), dip-coating makes every liter of honeycomb ceramic body upload 100��130g titanium dioxide after drying, makes every liter of honeycomb ceramic body upload 200��330g titanium dioxide after secondary dip-coating drying and roasting.
The present invention additionally provides the application in described catalyst nitrogen oxides in SCR coke oven discharge flue gas simultaneously, is with ammonia for reducing agent, air speed 8000��16000hr-1, between 230��280 DEG C, reach the denitration rate of 95��99%.
The present invention is directed to the deficiency that traditional coke oven gas denitrifying technology exists, provide a kind of coke oven flue gas denitrating catalyst especially, this catalyst is Bulk coat structural formula, has very high low temperature active and wide temperature window, is 10000hr in air speed-1, the denitration rate of more than 90% can be reached during this catalyst 200 DEG C, fully meet the needs of coke oven flue gas low-temperature denitration. Coke oven flue gas dustiness is very low, uses the heavy duty detergent Bulk coat formula catalyst that this hole density is high, catalyst can be greatly lowered and make consumption, reduce one-time investment. And use this kind of method can be integrated with heat recovery and sweetening process easily.
The invention have the advantage that selection micron order metatitanic acid prepares catalyst as raw material, do not need that raw material is carried out the complex process such as comminution by gas stream, roasting and process. The catalyst pulp solid content modulated is high, and viscosity is low, just can reach the upper carrying capacity of 200��330g titanium dioxide/liter cordierite honeycomb ceramic after general twice coating. Can obtaining the Bulk coat formula denitrating catalyst with regular coating, the denitrating catalyst low-temperature catalytic activity prepared is high, is particularly well-suited to coke oven flue gas denitration.
Accompanying drawing explanation
Fig. 1 be by embodiment 1 preparation denitrating catalyst on conversion rate of NOx with gasinlet temperature change curve;
Fig. 2 be by embodiment 2 preparation denitrating catalyst on conversion rate of NOx with gasinlet temperature change curve.
Detailed description of the invention
The present invention is further illustrated below in conjunction with the drawings and specific embodiments, but not thereby limiting the invention.
Embodiment 1
The preparation of the catalyst of the present invention and determination of activity:
Metatitanic acid obtains titanium dioxide after 500 DEG C of roastings. Ammonia and 1.5g sodium polyacrylate chelated dispersants that Ludox that 30g titanium dioxide, 5g solid content are 30%, 35g deionized water, 1g mass percent concentration are 25% are loaded ball milling 2 hours in ball grinder, obtains the water-based slurry containing titanium dioxide. The viscosity measuring slurry with rotary viscometer is 0.2 pascal second. It is 9.66 that pH meter measures the pH value of slurry. 200cpsi cordierite honeycomb ceramic is cut into the fritter of �� 1.4 �� 2.2cm, it is dipped in the gained water-based slurry containing titanium dioxide after weighing, after 30 seconds, taking-up hot blast blows down remaining slurry in duct, then 3 minutes are dried with microwave drying oven, repeat this process and obtain the honeycomb ceramic body of 2 coatings for 1 time, dried honeycomb ceramic body was in 500 DEG C of roastings 2 hours, and the load capacity recording titanium dioxide of weighing after taking-up is 1.0793g. The ammonium metatungstate solution of preparation 122.5g/L, with this solution impregnation TiO2/ cordierite honeycomb ceramic body, after 30 seconds, taking-up hot blast blows down remaining solution in duct, then dries 3 minutes with microwave drying oven, and in Muffle furnace, 500 DEG C of roastings obtain WO in 2 hours3/TiO2/ cordierite honeycomb ceramic body. Taking 55g ammonium metavanadate, 110g oxalic acid and the mixing of a certain amount of deionized water, heating for dissolving is settled to 500ml and obtains ammonium metavanadate solution. With this solution impregnation WO3/TiO2/ cordierite honeycomb ceramic body, after 30 seconds, taking-up hot blast blows down remaining solution in duct, then dries 3 minutes with microwave drying oven, and in Muffle furnace, 500 DEG C of roastings obtain V in 2 hours2O5/WO3/TiO2/ cordierite honeycomb ceramic denitrating catalyst.
The catalyst denitration activity method of testing prepared is: being loaded in quartz ampoule by Bulk coat formula catalyst, reaction atmosphere is: 500ppmNO+500ppmNH3+ 10%O2+ 15%H2O+N2, regulate raw gas flow and make the air speed reacted be 23000hr-1. Detect NO and the NO of import and export respectively2Concentration, thus calculating total conversion rate of NOx, obtains the denitration efficiency of catalyst. Fig. 1 gives catalyst at denitration efficiency 175��500 DEG C interval.
Comparative example 1
Titanium dioxide used is with embodiment 1. Ludox, 36g deionized water that 30g titanium dioxide, 5g solid content are 30% are loaded ball milling 2 hours in ball grinder, obtain titania slurry, beyond instrument range during by rotary viscometer viscosimetric, more than 5 pascal seconds, slurry is thickness very, it is impossible to for the dip-coating of honeycomb ceramic carrier.
Comparative example 2
Titanium dioxide used is with embodiment 1. The ammonia that Ludox that 30g titanium dioxide, 5g solid content are 30%, 35g deionized water, 1g mass percent concentration are 25% is loaded ball milling 2 hours in ball grinder, obtain titania slurry, the viscosity measuring slurry with rotary viscometer is 0.6 pascal second, the slightly aobvious thickness of slurry, with this slurry dip-coating ceramic honey comb, absorption slip rate is slow, occurs plug-hole phenomenon during purging.
Comparative example 3
Titanium dioxide used is with embodiment 1. Ludox that 30g titanium dioxide, 5g solid content are 30%, 36g deionized water, 1.5g sodium polyacrylate chelated dispersants are loaded ball milling 2 hours in ball grinder, obtain titania slurry, the pH value surveying slurry is 0.75, beyond instrument range during by rotary viscometer viscosimetric, more than 5 pascal seconds, slurry is thickness very, it is impossible to for the dip-coating of honeycomb ceramic carrier.
Embodiment 2
The preparation of the catalyst of the present invention and determination of activity:
The preparation process of titania slurry and catalyst, with embodiment 1, simply replaces the cordierite honeycomb ceramic block of 200cpsi with the 400cpsi cordierite honeycomb ceramic block of �� 1.4 �� 2.2cm size. After twice dip-coating, drying and roasting records carrying capacity on titanium dioxide after taking out and weighing is 1.1348g.
The catalyst denitration activity method of testing prepared is with embodiment 1.
Embodiment 3
Coke oven flue gas denitration industry side line is tested:
Take 60kg titanium dioxide, ammonia, 1.4kg sodium polyacrylate chelated dispersants and 60kg deionized water that Ludox that 10kg solid content is 30%, 2kg mass percent concentration are 25% load ball milling 2 hours in ball grinder, obtain the water-based slurry of titanium dioxide. Being sized to 150 �� 150 �� 150 (mm) with this slurry dip-coating, hole density is the cordierite honeycomb ceramic of 400 holes/square inch. After 2 coatings, microwave drying, roasting obtain TiO2/ cordierite honeycomb ceramic body. Then TiO is impregnated with the ammonium metatungstate solution with embodiment 1 same concentrations2/ cordierite honeycomb ceramic body, microwave drying, obtain WO after Muffle furnace roasting3/TiO2/ cordierite honeycomb ceramic body. Finally impregnate WO with the ammonium metavanadate oxalic acid solution with embodiment 1 same concentrations3/TiO2/ cordierite honeycomb ceramic body, microwave drying, obtain V after Muffle furnace roasting2O5/WO3/TiO2/ cordierite honeycomb ceramic denitrating catalyst. Take in 32 pieces of integer catalyzer point two-layers loading Benitration reactors and carry out the experiment of coke oven flue gas denitration industry side line.
Punch in coke oven chimney baker hole site, take coke oven flue gas with air-introduced machine from this, inlet pipeline is provided with butterfly valve, it is possible to regulate absorbing quantity. In experiment, ammonia source is liquefied ammonia, and system sets a liquid ammonia storage tank, and ammonia is controlled flow by mass flowmenter, adds in flue and enters Benitration reactor after flue gas Homogeneous phase mixing. In Benitration reactor, nitrogen oxides and ammonia reaction generate nitrogen and water, and the flue gas after denitration is discharged by the little chimney connected on blower fan.
Import and export at Benitration reactor and be equipped with sampling line. Can NO, NO in sampling analysis measuring flue gas2��SO2��NH3Concentration.
Industry side line experiment runs 1200 hours, and reactor inlet temperature is at 260 DEG C��280 DEG C, and air speed is 8000��16000hr-1, during experiment, reactor inlet nitrous oxides concentration is at 900��1200mg/m3Between, reactor tail gas outlet nitrous oxides concentration is less than 20mg/m3, denitration rate is basically stable between 98��99%, it is shown that extraordinary denitration effect.
It is described above for principles of the invention and effect thereof are described, not for the restriction present invention. Above-described embodiment all in the thought and scope of the present invention, can be modified and change by any person of ordinary skill in the field. Therefore, the scope of the present invention, should be as the criterion with listed claim.
Claims (9)
1. a coke oven flue gas denitration catalyst, it is characterised in that: this catalyst is integral honeycomb ceramic coating formula catalyst, is made up of honeycomb ceramic carrier, oxide coating and active component.
2. a kind of coke oven flue gas denitration catalyst described in claim 1, it is characterised in that: described honeycomb ceramic carrier is mainly cordierite or metal, and its hole density is 100��400 holes/square inch, and described oxide coating is TiO2-SiO2-WO3Composite oxides, described active component is the oxide of vanadium.
3. the preparation method of a kind of coke oven flue gas denitration catalyst described in claim 1, it is characterised in that: the method comprises the steps:
(1) roasting at metatitanic acid 500 DEG C is obtained titanium dioxide in 4 hours;
(2) ball milling after titanium dioxide, deionized water, Ludox, ammonia and dispersant is prepared titania slurry;
(3) with after gained titania slurry dipping honeycomb ceramic carrier, blowing out slurry unnecessary in duct, drying roasting obtains the cordierite honeycomb ceramic of loading titanium oxide and silica coating;
(4) prepare the ammonium metatungstate solution of 100��240g/L, with the ceramic honey comb of this solution impregnation loading titanium oxide coating, after drying roasting, obtain WO3/TiO2-SiO2/ cordierite honeycomb ceramic;
(5) mixed solution of preparation ammonium metavanadate and oxalic acid, wherein the concentration of ammonium metavanadate is 70��150g/L, and the concentration of oxalic acid is 140��300g/L, with this solution impregnation WO3/TiO2/ cordierite honeycomb ceramic, obtains V after drying roasting2O5/WO3/TiO2-SiO2/ cordierite honeycomb ceramic denitrating catalyst.
4. the preparation method of a kind of coke oven flue gas denitration catalyst described in claim 3, it is characterized in that: in step (2), described dispersant is sodium polyacrylate or ammonium polyacrylate chelated dispersants, and its addition is the 0.5��8% of titania weight, it is preferable that 2��5%.
5. the preparation method of a kind of coke oven flue gas denitration catalyst described in claim 3, it is characterised in that: step (2) adds ammonia and adjusts the pH value of slurry 8��12, it is preferable that 9��10.
6. the preparation method of a kind of coke oven flue gas denitration catalyst described in claim 3, it is characterised in that: in step (2), the solid content of titania slurry is 40��50%.
7. the preparation method of a kind of coke oven flue gas denitration catalyst described in claim 3, it is characterised in that: in step (2), the viscosity of titania slurry is at 0.2��0.6 pascal second.
8. the preparation method of a kind of coke oven flue gas denitration catalyst described in claim 3, it is characterized in that: with titania slurry dip-coating cordierite honeycomb ceramic in step (2), dip-coating makes every liter of honeycomb ceramic body upload 100��130g titanium dioxide after drying, makes every liter of honeycomb ceramic body upload 200��330g titanium dioxide after secondary dip-coating drying and roasting.
9. the application in the nitrogen oxides in SCR coke oven discharge flue gas of a kind of coke oven flue gas denitration catalyst described in claim 1, it is characterised in that: described application is with ammonia for reducing agent, air speed 8000��16000hr-1, between 230��280 DEG C, reach the denitration rate of 95��99%.
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CN109046361A (en) * | 2018-08-28 | 2018-12-21 | 山东泰和水处理科技股份有限公司 | A kind of fatty alcohol TERTIARY AMINATING CATALYST and the preparation method and application thereof |
CN109126801A (en) * | 2018-08-28 | 2019-01-04 | 山东泰和水处理科技股份有限公司 | A kind of tertiary-aminated loaded catalyst of fatty alcohol and its preparation method and application |
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CN109833907B (en) * | 2017-11-29 | 2021-10-15 | 中国科学院大连化学物理研究所 | Low-temperature sulfur-resistant coke oven flue gas denitration catalyst with ammonia storage and storage performance |
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CN109046361A (en) * | 2018-08-28 | 2018-12-21 | 山东泰和水处理科技股份有限公司 | A kind of fatty alcohol TERTIARY AMINATING CATALYST and the preparation method and application thereof |
CN109126801A (en) * | 2018-08-28 | 2019-01-04 | 山东泰和水处理科技股份有限公司 | A kind of tertiary-aminated loaded catalyst of fatty alcohol and its preparation method and application |
CN114682251A (en) * | 2022-03-24 | 2022-07-01 | 青岛华世洁环保科技有限公司 | Light low-temperature SCR denitration catalyst and preparation method thereof |
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