CN105080605A - Preparation method for high-temperature flue gas denitrification catalyst and product of high-temperature flue gas denitrification catalyst - Google Patents
Preparation method for high-temperature flue gas denitrification catalyst and product of high-temperature flue gas denitrification catalyst Download PDFInfo
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Abstract
The invention relates to a preparation method for a high-temperature flue gas denitrification catalyst and belongs to the technical field of flue gas denitrification. The preparation method comprises the following two steps: preparing a precursor; and preparing a catalyst. According to the technical scheme, the preparation method comprises the steps: by taking V2O5 as a main active component and Nb2O5 and MoO3 as an auxiliary active component, preparing the precursor of V2O5, Nb2O5 and MoO3; and then mixing the precursor by titanium tungsten powder taking TiO2 and WO3 as main components through extrusion molding, drying and water removal and roasting processes to prepare the catalyst. The problem that the SCR denitration efficiency is relatively low when the flue gas temperature of a coal-fired power plant is 280-300 DEG C is solved. Moreover, in the catalyst preparation process, a microwave drying technology is adopted to overcome the defect of cracking and uneven size distribution caused by temperature gradient in a conventional drying technology, so that the drying time is shortened and the production efficiency is improved. The invention further relates to a denitrification catalyst prepared by the method, so that the low-temperature activity of the catalyst is improved and the active temperature window is expanded, and the preparation method has beneficial technical effects.
Description
Technical field
The present invention relates to a kind of high-temperature flue gas denitrating catalyst preparation method, the invention still further relates to denitrating catalyst prepared by a kind of the method, belong to gas denitrifying technology field.
Background technology
Nitrogen oxide (the NO discharged in flue gas
x), not only can cause a series of environmental pollution, as broken ring ozone layer, acid rain, greenhouse effects, photochemical fog etc., and plant growth can be endangered, cause the breathing problem of the mankind.NO
xthe source of discharge is mainly from electric power, heating power production and supply industry.In recent years due to NO
xdischarge the social concern caused day by day remarkable, State Bureau of Environmental Protection is to NO
xreduce discharging and propose stricter requirement, along with country is to NO
xdischarge standard more and more higher; according to " national environmental protection " 12 " planning " requirement, during " 12 ", China's nitrogen oxide emission will reduce 10%, by 2015 years; the discharge capacity of nitrogen oxide reduces to 2046.2 ten thousand tons, therefore current China NOx carry effect reduce discharging extremely urgent.SCR denitration technology, because denitration efficiency is high, good selective, therefore, has nowadays become the mainstream technology of denitrating flue gas.
At present; coal-burning power plant's SCR denitration reactor mainly adopts the high temperature height dust-laden arrangement (after being usually arranged on economizer, before air preheater) of 300 DEG C ~ 420 DEG C; but for the operating mode of middle high temperature height dust-laden; especially flue-gas temperature at 280 DEG C ~ 300 DEG C time there is no actual effective solution, often cause shutting down or discharging situation about exceeding standard.For the situation that high temperature V-Ti system denitrating catalyst low-temperature catalytic activity is lower, develop the good catalyst for denitrating flue gas of middle high-temperature behavior very necessary.
Catalyst base substrate drying removing wherein most of unnecessary moisture content after extrusion molding, proceed to guipure roasting in kilns again, the steam drying technique that current industry is commonly used need carry out the long-time drying of about 10 days under the lower temperature of 60 DEG C ~ 80 DEG C, to ensure that the outside diffusion rate of base substrate internal moisture is identical with surperficial moisture content evaporation rate, prevent the contraction of ectonexine inequality from easily causing the phenomenon of the cracking of base substrate, thus have that drying time is long, energy consumption is large, heat the shortcomings such as uneven, base substrate is easy to crack.
Summary of the invention
For solving problems of the prior art, the invention provides a kind of preparation method improving high-temperature flue gas denitrating catalyst low temperature active, concrete technical scheme is as follows:
A kind of high-temperature flue gas denitrating catalyst preparation method, comprises the steps,
Step one, prepared by precursor, according to following parts by weight:
Mix, add thermal agitation, treat that solid all dissolves, complete precursor preparation;
Step 2, catalyst preparing,
According to following mass fraction:
Carry out the mixing pug obtaining mixing, anhydrate through extrusion molding, drying, roasting technique, complete catalyst preparing.
As the improvement of technique scheme, in the mixing pug obtained of described step 2, the mass percent of active ingredient is:
As the improvement of technique scheme, a kind of cosolvent of described step is MEA or acetamide.
As the improvement of technique scheme, in described step 2, additive is the mixture of sodium carboxymethylcellulose, polyethylene glycol oxide, 50% lactic acid, glass fibre.
As the improvement of technique scheme, in described step one, after each component mixing, heating is stirred to 80 DEG C ~ 100 DEG C, and insulation 6min ~ 60min all dissolves to solid.
As the improvement of technique scheme, in described step 2, dry dewatering technology is: the idiosome of extrusion molding is carried out microwave drying.
As the improvement of technique scheme, dry dewatering technology in described step 2, microwave treatment power is 80W ~ 400W, microwave time 10min ~ 180min.
As the improvement of technique scheme, in described step 2, extruding-out process is: first pug is carried out pre-extruded through screen filtration, and then carry out vacuum extruding form, the vacuum of vacuum extruding form is-0.2Mpa ~-0.02Mpa, extruded velocity is 1m/s ~ 2m/s, obtains the honeycomb catalyst base substrate of dense uniform.
As the improvement of technique scheme, described roasting technique is: idiosome drying anhydrated is by mesh-belt kiln roasting, and sintering temperature is 450 DEG C ~ 620 DEG C.
Technique scheme is passed through with V
2o
5be main active component, with Nb
2o
5, MoO
3for helping active fraction preparation V
2o
5, Nb
2o
5and MoO
3precursor, be then TiO with main component by presoma
2, WO
3titanium tungsten powder carry out mixing, anhydrate through extrusion molding, drying, roasting technique, complete catalyst preparing, solve the coal-fired plant flue gas temperature problem that SCR denitration efficiency is lower 280 DEG C ~ 300 DEG C time, beneficial effect is remarkable, simultaneously, by adopting microwave drying technology in catalyst preparation process, not only overcome the defect of cracking that conventional drying techniques causes due to thermograde and size distribution inequality, and shorten drying time, improve production efficiency, there are wide market prospects.
Present invention also offers a kind of denitrating catalyst utilizing above-mentioned preparation method to produce, this denitrating catalyst can adapt to the catalytic environment of flue-gas temperature 280 DEG C ~ 300 DEG C time, improve the low temperature active of denitrating catalyst, widen the active temperature windows of denitrating catalyst, there is useful technique effect.
Accompanying drawing explanation
Fig. 1 is the process chart of a kind of high-temperature flue gas denitrating catalyst of the present invention preparation method.
Detailed description of the invention
As shown in Figure 1, the invention provides a kind of high-temperature flue gas denitrating catalyst preparation method, comprise the steps,
Step one, prepared by precursor, according to following parts by weight:
Mix, heating is stirred to 80 DEG C ~ 100 DEG C, and insulation 6min ~ 60min all dissolves to solid, completes precursor preparation;
Step 2, catalyst preparing,
According to following mass fraction:
Carry out the mixing pug obtaining mixing, wherein titanium tungsten powder is carrier, and effect is active component in supported catalyst, TiO in titanium tungsten powder
2for Detitanium-ore-type, WO
3content is 2% ~ 8%, and specific area is 85m
2/ g ~ 95m
2/ g, then anhydrate through extrusion molding, drying, roasting technique, complete catalyst preparing.
In above-mentioned preparation method, a kind of cosolvent of step is MEA or acetamide, in step 2, additive is the mixture of sodium carboxymethylcellulose, polyethylene glycol oxide, 50% lactic acid, glass fibre, and in the mixing pug obtained of described step 2, the mass percent of active ingredient is, TiO
230% ~ 90%, V
2o
50.5% ~ 5%WO
31% ~ 10%, Nb
2o
51% ~ 20%, MoO
31% ~ 20%.
In the above-described embodiments, in step 2, dry dewatering technology is: the idiosome of extrusion molding is carried out microwave drying, and microwave treatment power is 80W ~ 400W, microwave time 10min ~ 180min.Heating object itself can be made to become heater for use microwave drying and hydrone is best to microwave absorption, fast compared to existing steam drying processing speed, the time is short, efficiency is high, homogeneous heating, blank forming are effective, overcome the defect of cracking that thermograde causes and size distribution inequality, have broad application prospects.
Further, in step 2, extruding-out process is: first pug is carried out pre-extruded through screen filtration, and then carry out vacuum extruding form, the vacuum of vacuum extruding form is-0.2Mpa ~-0.02Mpa, extruded velocity is 1m/s ~ 2m/s, obtains the honeycomb catalyst base substrate of dense uniform.Described roasting technique is: idiosome drying anhydrated is by mesh-belt kiln roasting, and sintering temperature is 450 DEG C ~ 620 DEG C.
Present invention also offers a kind of denitrating catalyst, this denitrating catalyst uses above-mentioned preparation method to make, this catalyst can adapt to the catalytic environment of flue-gas temperature 280 DEG C ~ 300 DEG C time, solve high temperature V-Ti system denitrating catalyst in prior art underway low-temperature catalyzed time active lower problem, improve the low temperature active of denitrating catalyst, widen the active temperature windows of denitrating catalyst.
Embodiment one
Step one, takes 13.4kg ammonium metavanadate, 15.6kg ammonium heptamolybdate, 6.6kg niobium oxalate, 15kg MEA, mixes with 80kg deionized water, and heating is stirred to 90 DEG C, and insulation 30min all dissolves to solid, finally obtains V
2o
5, Nb
2o
5and MoO
3precursor I;
Step 2, take 600kg titanium tungsten powder, 50kg glass fibre, 1.75kg carboxymethyl cellulose, 7.5kg polyethylene glycol oxide, 7.5kg50% lactic acid, adding the precursor I that 200kg deionized water, 60kg ammoniacal liquor and step one obtain carries out mixing, time is 60min, is mixed and has certain plastic mud material; By plastic mud material through screen filtration formula pre-extruded, remove large granular impurity, and moisture and component are mixed further; Carry out vacuum extruding form again, vacuum is-0.1Mpa, and extruded velocity is 1.5m/s, obtains the honeycomb catalyst base substrate of dense uniform; Catalyst base substrate is carried out microwave drying, and microwave treatment power is 300W, and the processing time is 1h, removes the most of moisture in base substrate; Finally, through mesh-belt kiln roasting, sintering temperature is 550 DEG C, obtains the ceramic honeycomb catalyst I with certain mechanical strength.
Be that the catalyst I of 50mm is placed in flue gas activity rating device by length, the clearance of catalyst n O at testing 290 DEG C, simulated flue gas consists of 600ppmNO, 600ppmNH
3, 6%O
2(N
2for Balance Air), air speed is 3000h
-1, test result is in table 1.
Embodiment two
Step one, takes 13.4kg ammonium metavanadate, 15.6kg ammonium heptamolybdate, 6.6kg niobium oxalate, 15kg MEA, mixes with 80kg deionized water, and heating is stirred to 90 DEG C, and insulation 30min all dissolves to solid, finally obtains V
2o
5, Nb
2o
5and MoO
3precursor II;
Step 2, take 600kg titanium tungsten powder, 50kg glass fibre, 1.75kg carboxymethyl cellulose, 7.5kg polyethylene glycol oxide, 7.5kg50% lactic acid, adding the precursor II that 200kg deionized water, 60kg ammoniacal liquor and step one obtain carries out mixing, time is 60min, is mixed and has certain plastic mud material; By plastic mud material through screen filtration formula pre-extruded, then carry out vacuum extruding form, vacuum is-0.1Mpa, and extruded velocity is 1.5m/s, obtains the honeycomb catalyst base substrate of dense uniform; Catalyst base substrate is carried out microwave drying, and microwave treatment power is 200W, and the processing time is 2h, removes the most of moisture in base substrate; Finally, through mesh-belt kiln roasting, sintering temperature is 550 DEG C, obtains the ceramic honeycomb catalyst II with certain mechanical strength.
The method of testing of catalyst II according to embodiment one tested, test result is in table 1.
Embodiment three
Step one, takes 13.4kg ammonium metavanadate, 7.8kg ammonium heptamolybdate, 13.2kg niobium oxalate, 15kg MEA, mixes with 80kg deionized water, and heating is stirred to 80 DEG C, and insulation 60min all dissolves to solid, finally obtains V
2o
5, Nb
2o
5and MoO
3precursor III;
Step 2, take 600kg titanium tungsten powder, 50kg glass fibre, 1.75kg carboxymethyl cellulose, 7.5kg polyethylene glycol oxide, 7.5kg50% lactic acid, adding the precursor III that 200kg deionized water, 60kg ammoniacal liquor and step one obtain carries out mixing, time is 60min, is mixed and has certain plastic mud material; By plastic mud material through screen filtration formula pre-extruded, then carry out vacuum extruding form, vacuum is-0.2Mpa, and extruded velocity is 1m/s, obtains the honeycomb catalyst base substrate of dense uniform; Catalyst base substrate is carried out microwave drying, and microwave treatment power is 400W, and the processing time is 10min, removes the most of moisture in base substrate; Finally, through mesh-belt kiln roasting, sintering temperature is 450 DEG C, obtains the ceramic honeycomb catalyst III with certain mechanical strength.
The method of testing of catalyst III according to embodiment one tested, test result is in table 1.
Embodiment four
Step one, takes 13.4kg ammonium metavanadate, 15.6kg ammonium heptamolybdate, 13.2kg niobium oxalate, 15kg MEA, mixes with 80kg deionized water, and heating is stirred to 100 DEG C, and insulation 6min all dissolves to solid, finally obtains V
2o
5, Nb
2o
5and MoO
3precursor IV;
Step 2, take 600kg titanium tungsten powder, 50kg glass fibre, 1.75kg carboxymethyl cellulose, 7.5kg polyethylene glycol oxide, 7.5kg50% lactic acid, adding the precursor IV that 200kg deionized water, 60kg ammoniacal liquor and step one obtain carries out mixing, time is 60min, is mixed and has certain plastic mud material; By plastic mud material through screen filtration formula pre-extruded, then carry out vacuum extruding form, vacuum is-0.02Mpa, and extruded velocity is 2m/s, obtains the honeycomb catalyst base substrate of dense uniform; Catalyst base substrate is carried out microwave drying, and microwave treatment power is 80W, and the processing time is 2.5h, removes the most of moisture in base substrate; Finally, through mesh-belt kiln roasting, sintering temperature is 450 DEG C, obtains the ceramic honeycomb catalyst IV with certain mechanical strength.
The method of testing of catalyst IV according to embodiment one tested, test result is in table 1.
Embodiment five
Step one, takes 1kg ammonium metavanadate, 1kg ammonium heptamolybdate, 1kg niobium oxalate, 1kg acetamide, mixes with 20kg deionized water, and heating is stirred to 90 DEG C, and insulation 30min all dissolves to solid, finally obtains V
2o
5, Nb
2o
5and MoO
3precursor V;
Step 2, take 190kg titanium tungsten powder, 8kg glass fibre, 1.75kg carboxymethyl cellulose, 2.5kg polyethylene glycol oxide, 2.5kg50% lactic acid, adding the precursor V that 100kg deionized water, 5kg ammoniacal liquor and step one obtain carries out mixing, time is 60min, is mixed and has certain plastic mud material; By plastic mud material through screen filtration formula pre-extruded, then carry out vacuum extruding form, vacuum is-0.1Mpa, and extruded velocity is 1.5m/s, obtains the honeycomb catalyst base substrate of dense uniform; Catalyst base substrate is carried out microwave drying, and microwave treatment power is 200W, and the processing time is 2h, removes the most of moisture in base substrate; Finally, through mesh-belt kiln roasting, sintering temperature is 620 DEG C, obtains the ceramic honeycomb catalyst V with certain mechanical strength.
The method of testing of catalyst V according to embodiment one tested, test result is in table 1.
Embodiment six
Step one, takes 30kg ammonium metavanadate, 30kg ammonium heptamolybdate, 25kg niobium oxalate, 30kg acetamide, mixes with 200kg deionized water, and heating is stirred to 90 DEG C, and insulation 30min all dissolves to solid, finally obtains V
2o
5, Nb
2o
5and MoO
3precursor VI;
Step 2, take 900kg titanium tungsten powder, 50kg glass fibre, 1.75kg carboxymethyl cellulose, 7.5kg polyethylene glycol oxide, 7.5kg50% lactic acid, adding the precursor VI that 400kg deionized water, 90kg ammoniacal liquor and step one obtain carries out mixing, time is 60min, is mixed and has certain plastic mud material; By plastic mud material through screen filtration formula pre-extruded, then carry out vacuum extruding form, vacuum is-0.1Mpa, and extruded velocity is 1.5m/s, obtains the honeycomb catalyst base substrate of dense uniform; Catalyst base substrate is carried out microwave drying, and microwave treatment power is 200W, and the processing time is 2h, removes the most of moisture in base substrate; Finally, through mesh-belt kiln roasting, sintering temperature is 550 DEG C, obtains the ceramic honeycomb catalyst VI with certain mechanical strength.
The method of testing of catalyst VI according to embodiment one tested, test result is in table 1.
Honeycomb catalyst prepared by table 1 different formulations and different microwave treatment is active
Claims (10)
1. a high-temperature flue gas denitrating catalyst preparation method, is characterized in that, comprises the steps,
Step one, prepared by precursor, according to following parts by weight:
Ammonium metavanadate 1 ~ 30 part
Ammonium heptamolybdate 1 ~ 30 part
Niobium oxalate 1 ~ 25 part
Cosolvent 1 ~ 30 part
Deionized water 20 ~ 200 parts
Mix, add thermal agitation, treat that solid all dissolves, complete precursor preparation;
Step 2, catalyst preparing,
According to following mass fraction:
Titanium tungsten powder 50% ~ 70%
Precursor 10 ~ 15%
Additive 1 ~ 5%
Deionized water 20 ~ 30%
Ammoniacal liquor 1 ~ 5%
Carry out the mixing pug obtaining mixing, anhydrate through extrusion molding, drying, roasting technique, complete catalyst preparing.
2. a kind of high-temperature flue gas denitrating catalyst preparation method as claimed in claim 1, is characterized in that, in the mixing pug obtained of described step 2, the mass percent of active ingredient is:
TiO
230%～90%
V2O
50.5%～5%
WO
31%～10%
Nb2O
51%～20%
MoO
31%～20%。
3. a kind of high-temperature flue gas denitrating catalyst preparation method as claimed in claim 1, is characterized in that, a kind of cosolvent of described step is MEA or acetamide.
4. a kind of high-temperature flue gas denitrating catalyst preparation method as claimed in claim 1, is characterized in that, in described step 2, additive is the mixture of sodium carboxymethylcellulose, polyethylene glycol oxide, 50% lactic acid, glass fibre.
5. a kind of high-temperature flue gas denitrating catalyst preparation method as claimed in claim 1, is characterized in that, in described step one, after each component mixing, heating is stirred to 80 DEG C ~ 100 DEG C, and insulation 6min ~ 60min all dissolves to solid.
6. a kind of high-temperature flue gas denitrating catalyst preparation method according to any one of claim 1-5, it is characterized in that, in described step 2, dry dewatering technology is: the idiosome of extrusion molding is carried out microwave drying.
7., as claim requires a kind of high-temperature flue gas denitrating catalyst preparation method as described in 6, it is characterized in that, dry dewatering technology in described step 2, microwave treatment power is 80W ~ 400W, microwave time 10min ~ 180min.
8. a kind of high-temperature flue gas denitrating catalyst preparation method as claimed in claim 6, it is characterized in that, in described step 2, extruding-out process is: first pug is carried out pre-extruded through screen filtration, and then carry out vacuum extruding form, the vacuum of vacuum extruding form is-0.2Mpa ~-0.02Mpa, extruded velocity is 1m/s ~ 2m/s, obtains the honeycomb catalyst base substrate of dense uniform.
9. a kind of high-temperature flue gas denitrating catalyst preparation method as claimed in claim 6, it is characterized in that, described roasting technique is: idiosome drying anhydrated is by mesh-belt kiln roasting, and sintering temperature is 450 DEG C ~ 620 DEG C.
10., as a kind of application rights requires the denitrating catalyst that the high-temperature flue gas denitrating catalyst preparation method according to any one of 1 ~ 9 produces, it is characterized in that, described denitrating catalyst is made according to this preparation method.
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| CN106807356A (en) * | 2017-01-24 | 2017-06-09 | 东南大学 | A kind of low temperature SCR denitration catalyst and its methods for making and using same |
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| CN110124661A (en) * | 2019-04-26 | 2019-08-16 | 昆明贵研催化剂有限责任公司 | A kind of method that room temperature prepares vanadia-based SCR catalysts |
| CN113996309A (en) * | 2021-11-23 | 2022-02-01 | 国能龙源催化剂江苏有限公司 | Preparation method of high-strength SCR catalyst for CO collaborative removal |
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| CN116020440A (en) * | 2022-11-11 | 2023-04-28 | 国能无锡环保科技有限公司 | Preparation method and application of denitration catalyst |
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| CN114433056A (en) * | 2022-01-26 | 2022-05-06 | 浙江科卓环保科技有限公司 | Preparation method of wide-temperature-zone honeycomb type SCR denitration catalyst |
| CN116020440A (en) * | 2022-11-11 | 2023-04-28 | 国能无锡环保科技有限公司 | Preparation method and application of denitration catalyst |
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