CN103537273B - Denitrating catalyst of a kind of collaborative demercuration and preparation method thereof - Google Patents

Denitrating catalyst of a kind of collaborative demercuration and preparation method thereof Download PDF

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CN103537273B
CN103537273B CN201310462781.1A CN201310462781A CN103537273B CN 103537273 B CN103537273 B CN 103537273B CN 201310462781 A CN201310462781 A CN 201310462781A CN 103537273 B CN103537273 B CN 103537273B
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ammoniacal liquor
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gel
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CN103537273A (en
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刘小伟
徐明厚
赵波
斯俊平
王超
周子健
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Huazhong University of Science and Technology
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Abstract

A denitrating catalyst for collaborative demercuration, comprises the vanadic anhydride that mass percent is 5% ~ 10%, the molybdenum trioxide of 5% ~ 10%, and all the other compositions are titanium dioxide.The preparation method of above-mentioned catalyst is: positive for metatitanic acid four butyl esters, absolute ethyl alcohol, ammoniacal liquor, citric acid solution are mixed and shake the colloidal sol obtaining titaniferous; Inclined vanadium propylhomoserin, molybdenum trioxide are dissolved in ammoniacal liquor respectively and obtain mixed solution, then mixed solution is imported in colloidal sol, after concussion, drying, obtain gel; This catalyst is obtained after gel calcining, grinding.The denitrating catalyst of collaborative demercuration provided by the invention, can significantly improve the efficiency of catalytic oxidation mercury, and control SO 2be oxidized to SO 3ratio, and the component of catalyst is simple, reasonable mixture ratio, with low cost.Sol-gel process for the preparation of above-mentioned catalyst provided by the invention, the good dispersion of each component in obtained catalyst, achieves each active component Uniform Doped on a molecular scale well.

Description

Denitrating catalyst of a kind of collaborative demercuration and preparation method thereof
Technical field
The present invention relates to denitrating catalyst of a kind of collaborative demercuration and preparation method thereof, belong to atmosphere pollution purification techniques field.
Background technology
Coal is the abundantest a kind of fossil fuel resource of content, and China is coal production maximum in the world and country of consumption, and from the nineties in last century, coal production and the consumption figure of China are just sure to occupy No. 1 in the world for a long time.And the operation of coal burning particularly coal-burning power plant, can bring serious problem of environmental pollution, mercury and the nitrogen oxide of coal-burning power plant's discharge are that human activity is discharged into main source in air.Due to the mercury of discharging into the atmosphere enters behind biosphere can enrichment in human body, the nervous system of human body is damaged, serious harm health.And nitrogen oxide (NO x) local environment such as acid rain and photochemical fog problem can be caused, bring serious threat to the existence of the mankind.Based on this, country defines the discharge standard of mercury and nitrogen oxide first in thermal power plant's pollutant emission standard of promulgation in 2011, and wherein the discharge standard of mercury is 0.03mg/Nm 3, the discharge standard of nitrogen oxide is 100mg/Nm 3.
Mercury is mainly present in coal-fired flue-gas with three kinds of forms: Elemental Mercury (Hg 0), particle mercury (Hg p) and bivalent mercury (Hg 2+).Wherein, particle mercury (Hg p) be easy to be removed by electrostatic precipitator or sack cleaner with particle, bivalent mercury (Hg 2+) easily removed by wet desulphurization device (FGD) because of soluble in water, only have Elemental Mercury (Hg 0) due to its strong volatility and be insoluble to water-based, existing smoke eliminator is difficult to be removed.Therefore, the technical barrier removed of Mercury In Coal Combustion Flue Gas, mainly concentrates on removing Elemental Mercury in flue gas.The removal methods of current control coal-burning power plant Elemental Mercury mainly contains two kinds: absorption method and oxidizing process.It is that a kind of effect adsorbs demercuration method preferably that active carbon sprays into, but it is expensive, and the flying dust being mixed with higher carbon content is difficult to be used effectively.Oxidizing process demercuration first utilizes catalyst that Elemental Mercury Catalytic Oxygen is changed into bivalent mercury, then uses wet desulphurization device (WFGD) to remove bivalent mercury.Oxidizing process demercuration is the main method that current coal-fired flue-gas Elemental Mercury removes.
NO in coal-fired flue-gas xremoval methods generally adopt selective catalytic reduction, be improve reaction efficiency, general auxiliary denitrating catalyst (take vanadic anhydride as main active, titanium dioxide is matrix, also known as SCR catalyst).Denitrating catalyst is at reductive NO xwhile have the performance of oxidizing simple substance mercury concurrently, but, under typical SCR temperature window (350 DEG C-400 DEG C), the NO of denitrating catalyst xalthough percent reduction can reach more than 80%, but can only reach 20%-50% to the oxidation efficiency of Elemental Mercury, its main cause be the optimum temperature of denitrating catalyst mercury oxide lower than 300 DEG C, thus can not at reductive NO xappropriate working temperature (350 DEG C-400 DEG C) be issued to desirable mercury oxidation efficiency.
In addition, due in denitrating catalyst, if the content of main active vanadic anhydride is higher, then the SO in coal-fired flue-gas 2be oxidized to SO 3ratio can obviously increase, and SO 3the reactive metal oxide on denitrating catalyst surface can be made to generate sulfate, thus make catalyst poisoning, so in traditional SCR denitration, the content of vanadium is general all lower than 3%.Because in denitrating catalyst, the content of active material vanadic anhydride is less, the oxidation activity site that can be supplied to Elemental Mercury is seldom corresponding, causes the oxidation efficiency of Elemental Mercury to reduce further.Thus, use the smoke eliminator of existing coal-burning power plant and traditional denitrating catalyst, be difficult to make the Elemental Mercury in flue gas reach the discharge standard of national regulation.
Application for a patent for invention " a kind of denitrating catalyst of double demercuration ", date of publication: 2012.3.7, publication No.: CN102366722A, disclose a kind of denitrating catalyst of double demercuration, chemical general formula is: MX n-V 2o 5-Y/TiO 2, wherein, M is selected from metal unit Fe, Cu, Mn or Co; X is halogen Cl or Br; Y is WO 3or MoO 3, n=2 ~ 4; Weight proportion is: M1 ~ 10, V1 ~ 1.5, W or Mo7.5 ~ 8.5, TiO 275 ~ 100.This catalyst MCl nor MBr ndipping V 2o 5-WO 3/ TiO 2or V 2o 5-MoO 3/ TiO 2, drying, roasting are made.This catalyst owing to the addition of transition metal halide, then can utilize the wherein strong oxidizing property of Cl or Br and the redox property of transition metal, by nonvalent mercury Hg 0be oxidized to Hg 2+overcome and the impact of the halide of traditional K, Na on SCR catalyst acid activity point, ensure that catalytic activity, thus make catalyst keep higher denitration efficiency under the flue gas of 300 ~ 450 DEG C, make again the oxygenation efficiency of Hg bring up to 85.1% ~ 93.8% by traditional less than 30% simultaneously, greatly improve catalytic efficiency, the SCR denitration of transition metal halide process simultaneously can not increase SO 2/ SO 3conversion ratio, avoids catalyst poisoning and secondary pollution.
But also there are obvious shortcomings and deficiencies in above-mentioned catalyst: one is add transition metal halide as oxidant, considerably increases catalyst cost; Two is main active V 2o 5content lower (1 ~ 1.5%), V 2o 5the oxidation efficiency of oxidizing simple substance mercury is lower; Although three is with the addition of WO in the catalyst 3or MoO 3but, fail clear and definite its at reductive NO x, oxidizing simple substance mercury reaction in the catalytic action played and Catalysis Principles, thus also fail to provide above-mentioned substance rational proportion in the catalyst.
Summary of the invention
Technical purpose of the present invention is intended to solve existing denitrating catalyst and adopts the shortcomings and deficiencies such as the cost that transition metal halide exists for oxidizing simple substance mercury as oxidant is higher, active component proportioning is unreasonable, denitrating catalyst of a kind of collaborative demercuration and preparation method thereof is provided, the active component of this catalyst is made up of vanadic anhydride and molybdenum trioxide, by interpolation and the rational proportion of molybdenum trioxide, make catalyst can significantly improve the efficiency of catalytic oxidation mercury while keeping good catalytic denitration performance, and can effective control SO 2be oxidized to SO 3ratio, and the component of catalyst is simple, reasonable mixture ratio, with low cost.
The present invention is the technical scheme that actualizing technology object adopts: a kind of denitrating catalyst of collaborative demercuration, it is characterized in that: described catalyst comprises the vanadic anhydride that mass percent is 5% ~ 10%, mass percent is the molybdenum trioxide of 5% ~ 10%, and all the other compositions in described catalyst are titanium dioxide.
A denitrating catalyst for collaborative demercuration, described catalyst is ground into 100 ~ 325 orders.
For the preparation of a method for the denitrating catalyst of collaborative demercuration, comprise the following steps:
(1) Homogeneous phase mixing under 40 DEG C of conditions by positive for the metatitanic acid of determined volume four butyl esters and isopyknic absolute ethyl alcohol, obtains mixed liquor;
(2) according to ammoniacal liquor and positive four butyl esters of metatitanic acid with volume ratio be the ratio of 1:3, ammoniacal liquor steps for importing (1) obtained in mixed liquor, in 40 DEG C of environment, shakes 1h, obtain the Sol A of titaniferous;
(3) configuration quality concentration is the citric acid solution of 10%, gets and the isopyknic citric acid solution of ammoniacal liquor in step (2), imports in Sol A, shake 10min, obtain sol B under 40 DEG C of conditions;
(4) the inclined vanadium propylhomoserin solid that v element content is 5 ~ 10 weight portions is taken, be dissolved in the isopyknic salpeter solution of ammoniacal liquor in step (2), obtain solution A, take the molybdenum trioxide of 5 ~ 10 weight portions, be dissolved in the isopyknic ammoniacal liquor of ammoniacal liquor in step (2), obtain solution B;
(5) it is in the sol B of 80 ~ 90 weight portions that solution A step (4) obtained, B successively import titanium elements content, then add red fuming nitric acid (RFNA) and will regulate pH value to 1, and under 40 DEG C of conditions, shake 5h, be then warming up to 70 DEG C and under 70 DEG C of conditions dry 48h, obtain gel;
(6) gel that step (5) obtains is placed in Muffle furnace, is warming up to 400 DEG C, calcining 5h, grinding, obtains this catalyst.
For the preparation of a method for the denitrating catalyst of collaborative demercuration, in described step (5), gel heats up according to the heating rate of 6 DEG C/min.
Although titanium vanadium-molybdenum catalyst is applied to some extent in prior art, but prior art did not carry out correlation theory research on the interpolation of molybdenum for the impact of mercury oxidation, thus also fail to obtain the Catalysis Principles of molybdenum in vanadium titanium catalyst and catalytic effect, naturally also fail to obtain molybdenum rational proportion in the catalyst.
Applicant of the present invention finds through research, after adding molybdenum trioxide, be conducive to the architectural characteristic improving catalyst in traditional titanium vanadium catalyst, adds catalyst surface acid site, in titanium vanadium catalyst, can the main active substances of mercury oxide be vanadic anhydride, and in titanium vanadium-molybdenum catalyst, except vanadic anhydride generation effect, molybdenum trioxide and vanadium molybdenum complex all can be beneficial to the oxidation of mercury, thus significantly can promote the oxidation efficiency of Elemental Mercury.The more important thing is, molybdenum not only can not participate in SO 2oxidation, and the interpolation of molybdenum causes the improvement of catalyst structure, is unfavorable for SO 2in catalyst surface absorption, thus prevent SO 2further to SO 3transformation, thus the interpolation of molybdenum not only can not increase, can reduce SO on the contrary 2to SO 3level of conversion.So, under the prerequisite of adding molybdenum, the content of main active vanadic anhydride can also be improved further, thus realize SO simultaneously 2be oxidized to SO 3ratio maintain the prerequisite of reduced levels under, significantly improve the oxidation efficiency of Elemental Mercury.
Applicant of the present invention by great many of experiments, to have studied add molybdenum in titanium vanadium-molybdenum catalyst after catalyst at high temperature height SO 2the impact of mercury oxide under condition.Experimental result shows, after the molybdenum of interpolation 5% ~ 10%, even if the content of vanadic anhydride reaches in 5% ~ 10%(prior art be generally no more than 3%), SO 2be oxidized to SO 3ratio still maintain low-level within 2%, and simultaneously, NO xpercent reduction can reach 85 ~ 90%, and mercury oxidation rate can reach 75 ~ 82%.Experimental result also shows, when the content of molybdenum is 5% ~ 10%, keeps higher and roughly similar level to the oxidation efficiency of mercury; When molybdenum content lower than 5% time or higher than 10% time, mercury oxidation efficiency is all lower.Therefore molybdenum optimum proportioning is in the catalyst 5% ~ 10%.
Compare with prior art titanium vanadium-molybdenum catalyst, catalyst provided by the invention is without the need to adding transition metal halide, by means of only the content of rational proportion molybdenum trioxide, improve the content of vanadic anhydride simultaneously, active component molybdenum trioxide and vanadic anhydride just can be made to reach best catalytic effect, thus under solving hot conditions mercury oxidation rate too low and oxygenate content is higher time SO 2be oxidized to SO3 ratio comparatively high-technology problem, and significantly reduce the product cost of catalyst.
In the present invention, the preparation method of catalyst is sol-gel process, then shaping to catalyst sample calcining, and prior art SCR catalyst preparation method is generally infusion process, sol-gel process is the good dispersion of each component in the catalyst prepared relative to the advantage of infusion process, achieve each active component Uniform Doped on a molecular scale in catalyst well.
Detailed description of the invention
Embodiment 1 catalyst (TV of the present invention 5m 5) preparation
According to the following steps:
(1) Homogeneous phase mixing under 40 DEG C of conditions by positive for the metatitanic acid of determined volume four butyl esters and isopyknic absolute ethyl alcohol, obtains mixed liquor;
(2) according to ammoniacal liquor and positive four butyl esters of metatitanic acid with volume ratio be the ratio of 1:3, ammoniacal liquor steps for importing (1) obtained in mixed liquor, in 40 DEG C of environment, shakes 1h, obtain the Sol A of titaniferous;
(3) configuration quality concentration is the citric acid solution of 10%, gets and the isopyknic citric acid solution of ammoniacal liquor in step (2), imports in Sol A, shake 10min, obtain sol B under 40 DEG C of conditions;
(4) the inclined vanadium propylhomoserin solid that v element content is 5 weight portions is taken, be dissolved in the isopyknic salpeter solution of ammoniacal liquor in step (2), obtain solution A, take the molybdenum trioxide of 5 weight portions, be dissolved in the isopyknic ammoniacal liquor of ammoniacal liquor in step (2), obtain solution B;
(5) it is in the sol B of 90 weight portions that solution A step (4) obtained, B successively import titanium elements content, then adds red fuming nitric acid (RFNA) and regulates pH value to 1, and shake 5h under 40 DEG C of conditions, be then warming up to 70 DEG C and under 70 DEG C of conditions dry 48h, obtain gel;
(6) gel that step (5) obtains is placed in Muffle furnace, is warming up to 400 DEG C with the heating rate of 6 DEG C/min, calcining 5h, grinding, is then milled to 100 ~ 325 orders by the product after calcining, obtains catalyst TV 5m 5.
Embodiment 2 catalyst (TV of the present invention 5m 10) preparation
According to the following steps:
Step (1) ~ (3) are with embodiment 1;
(4) the inclined vanadium propylhomoserin solid that v element content is 5 weight portions is taken, be dissolved in the isopyknic salpeter solution of ammoniacal liquor in step (2), obtain solution A, take the molybdenum trioxide of 10 weight portions, be dissolved in the isopyknic ammoniacal liquor of ammoniacal liquor in step (2), obtain solution B;
(5) it is in 85 weight portion sol B that solution A step (4) obtained, B successively import titanium elements content, then ph value of mixture to 1 will be regulated with red fuming nitric acid (RFNA), and under 40 DEG C of conditions, shake 5h, be then warming up to 70 DEG C and under 70 DEG C of conditions dry 48h, obtain gel;
(6) gel that step (5) obtains is placed in Muffle furnace, is warming up to 400 DEG C with the heating rate of 6 DEG C/min, calcining 5h, grinding, is then milled to 100 ~ 325 orders by the product after calcining, obtains catalyst TV 5m 10.
Embodiment 3 catalyst (TV of the present invention 10m 5) preparation
According to the following steps:
Step (1) ~ (3) are with embodiment 1;
(4) the inclined vanadium propylhomoserin solid that v element content is 10 weight portions is taken, be dissolved in the isopyknic salpeter solution of ammoniacal liquor in step (2), obtain solution A, take the molybdenum trioxide of 5 weight portions, be dissolved in the isopyknic ammoniacal liquor of ammoniacal liquor in step (2), obtain solution B;
(5) it is in 85 weight portion sol B that solution A step (4) obtained, B successively import titanium elements content, then ph value of mixture to 1 will be regulated with red fuming nitric acid (RFNA), and under 40 DEG C of conditions, shake 5h, be then warming up to 70 DEG C and under 70 DEG C of conditions dry 48h, obtain gel;
(6) gel that step (5) obtains is placed in Muffle furnace, is warming up to 400 DEG C with the heating rate of 6 DEG C/min, calcining 5h, grinding, is then milled to 100 ~ 325 orders by the product after calcining, obtains catalyst TV 10m 5.
Embodiment 4 catalyst (TV of the present invention 10m 10) preparation
According to the following steps:
Step (1) ~ (3) are with embodiment 1;
(4) the inclined vanadium propylhomoserin solid that v element content is 10 weight portions is taken, be dissolved in the isopyknic salpeter solution of ammoniacal liquor in step (2), obtain solution A, take the molybdenum trioxide of 10 weight portions, be dissolved in the isopyknic ammoniacal liquor of ammoniacal liquor in step (2), obtain solution B;
(5) it is in 80 weight portion sol B that solution A step (4) obtained, B successively import titanium elements content, then ph value of mixture to 1 will be regulated with red fuming nitric acid (RFNA), and under 40 DEG C of conditions, shake 5h, be then warming up to 70 DEG C and under 70 DEG C of conditions dry 48h, obtain gel;
(6) gel that step (5) obtains is placed in Muffle furnace, is warming up to 400 DEG C with the heating rate of 6 DEG C/min, calcining 5h, grinding, is then milled to 100 ~ 325 orders by the product after calcining, obtains catalyst TV 10m 10.
Comparative example 1 catalyst (TV 5) preparation
According to the following steps:
Step (1) ~ (3) are with embodiment 1;
(4) take the inclined vanadium propylhomoserin solid that v element content is 5 weight portions, be dissolved in the isopyknic salpeter solution of ammoniacal liquor in step (2), obtain solution A;
(5) it is in 95 weight portion sol B that the solution A that step (4) obtained imports titanium elements content, then will regulate ph value of mixture to 1 with red fuming nitric acid (RFNA), and shake 5h under 40 DEG C of conditions, be then warming up to 70 DEG C and under 70 DEG C of conditions dry 48h, obtain gel;
(6) gel that step (5) obtains is placed in Muffle furnace, is warming up to 400 DEG C with the heating rate of 6 DEG C/min, calcining 5h, grinding, is then milled to 100 ~ 325 orders by the product after calcining, obtains catalyst TV 5.
Comparative example 2 catalyst (TV 10) preparation
According to the following steps:
Step (1) ~ (3) are with embodiment 1;
(4) take the inclined vanadium propylhomoserin solid that v element content is 10 weight portions, be dissolved in the isopyknic salpeter solution of ammoniacal liquor in step (2), obtain solution A;
(5) it is in 90 weight portion sol B that the solution A that step (4) obtained imports titanium elements content, then will regulate ph value of mixture to 1 with red fuming nitric acid (RFNA), and shake 5h under 40 DEG C of conditions, be then warming up to 70 DEG C and under 70 DEG C of conditions dry 48h, obtain gel;
(6) gel that step (5) obtains is placed in Muffle furnace, is warming up to 400 DEG C with the heating rate of 6 DEG C/min, calcining 5h, grinding, is then milled to 100 ~ 325 orders by the product after calcining, obtains catalyst TV 10.
Catalyst activity test experiments
Fixed bed reactors are tested the activity of six catalyst prepared by four embodiments of the present invention and two comparative examples respectively, and test event comprises: mercury oxidation rate, NO xpercent reduction and SO 2be oxidized to SO 3ratio.Test condition is: simulated flue gas flow is 0.9Nm 3/ h; Simulated flue gas composition is 0.04%NO, 0.04%NH 3, 6%O 2, 13%CO 2, 8%H 2o, 0.08%SO 2, 0.002%HCl, 55 μ g/Nm 3; Reaction temperature is 350 DEG C; The catalyst amount of single test is 0.3g.Test result is as shown in the table:
Embodiment Contrast is real Embodiment Embodiment 2 Contrast is real Embodiment 1 Embodiment 2
Execute example 1 1 Execute example 2
Catalyst TV 5 TV 5M 5 TV 5M 10 TV 10 TV 10M 5 TV 10M 10
Mercury oxidation rate 53% 81% 75% 49% 82% 78%
NO xPercent reduction 89% 90% 85% 91% 86% 88%
SO 2Oxygenation efficiency 3% 2% 1.5% 6% 1.5% 1.8%
As can be seen from the above table: under the prerequisite of not adding molybdenum, when improving content to 5 ~ 10% of vanadium, although NO xpercent reduction can reach the higher level of about 90%, but the oxygenation efficiency of mercury can only reach about 50%, and SO 2oxygenation efficiency reaches 3% ~ 6%, far beyond required standard; Improve after content of vanadium is increased to 5 ~ 10% when interpolation 5 ~ 10% molybdenum, titanium vanadium catalyst is (350 DEG C ~ 400 DEG C) under typical SCR temperature window, NO xpercent reduction can keep the higher level of 85 ~ 91%, and the efficiency of simultaneous oxidation mercury is significantly increased to 75 ~ 82%, and SO 2oxygenation efficiency maintains the low-level within 2%, and the property indices of obvious vanadium titanium molybdenum catalyst provided by the invention has reached very satisfied level all.

Claims (2)

1. prepare the method for the denitrating catalyst of collaborative demercuration for one kind, it is characterized in that: described catalyst comprises the vanadic anhydride that mass percent is 5% ~ 10%, mass percent is the molybdenum trioxide of 5% ~ 10%, all the other compositions in described catalyst are titanium dioxide, and the preparation method of described catalyst comprises the following steps:
(1) Homogeneous phase mixing under 40 DEG C of conditions by positive for the metatitanic acid of determined volume four butyl esters and isopyknic absolute ethyl alcohol, obtains mixed liquor;
(2) according to ammoniacal liquor and positive four butyl esters of metatitanic acid with volume ratio be the ratio of 1:3, ammoniacal liquor steps for importing (1) obtained in mixed liquor, in 40 DEG C of environment, shakes 1h, obtain the Sol A of titaniferous;
(3) configuration quality concentration is the citric acid solution of 10%, gets and the isopyknic citric acid solution of ammoniacal liquor in step (2), imports in Sol A, shake 10min, obtain sol B under 40 DEG C of conditions;
(4) the inclined vanadium propylhomoserin solid that v element content is 5 ~ 10 weight portions is taken, be dissolved in the isopyknic salpeter solution of ammoniacal liquor in step (2), obtain solution A, take the molybdenum trioxide of 5 ~ 10 weight portions, be dissolved in the isopyknic ammoniacal liquor of ammoniacal liquor in step (2), obtain solution B;
(5) it is in the sol B of 80 ~ 90 weight portions that solution A step (4) obtained, B successively import titanium elements content, then add red fuming nitric acid (RFNA) and will regulate pH value to 1, and under 40 DEG C of conditions, shake 5h, be then warming up to 70 DEG C and under 70 DEG C of conditions dry 48h, obtain gel;
(6) gel that step (5) obtains is placed in Muffle furnace, is warming up to 400 DEG C, calcining 5h, grinding, obtains this catalyst.
2. a kind of method preparing the denitrating catalyst of collaborative demercuration according to claim 1, is characterized in that: in described step (6), gel heats up according to the heating rate of 6 DEG C/min.
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