CN105148954A - Low-temperature efficient SCR denitration catalyst and preparation method thereof - Google Patents
Low-temperature efficient SCR denitration catalyst and preparation method thereof Download PDFInfo
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- CN105148954A CN105148954A CN201510601870.9A CN201510601870A CN105148954A CN 105148954 A CN105148954 A CN 105148954A CN 201510601870 A CN201510601870 A CN 201510601870A CN 105148954 A CN105148954 A CN 105148954A
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Abstract
The invention discloses a low-temperature efficient SCR denitration catalyst and a preparation method thereof. The catalyst is prepared from attapulgite, tetrabutyl titanate, acetylacetone, absolute ethyl alcohol, hydrochloric acid, ammonium fluoride and ammonia water. The preparation method comprise the following steps that 1, the attapulgite is processed through ultrasonic treatment and acid treatment for purification; 2, the attapulgite, the tetrabutyl titanate, the acetylacetone and the absolute ethyl alcohol are mixed and stirred to enable the attapulgite to be compounded with titanium dioxide through a sol-gel method; 3, compounds of the attapulgite and the titanium dioxide are put in an ammonium fluoride solution for water-bath immersion treatment at a certain temperature; 4, an immersed compound catalyst is calcined in a muffle furnace, and then the catalyst is prepared. The catalyst can be used for catalyzing conversion of nitrogen oxide in flue gas of a coal-fired power plant, the production cost is low, operation is easy, the efficiency is high, and the greater application value and market prospect are achieved.
Description
Technical field
The present invention relates to the technical field of Air Pollutants removal of nitrogen oxide, particularly relate to a kind of preparation method of low-temperature SCR catalyst for denitrating flue gas, be applicable to the coal-burning boiler low-temperature flue gas process such as thermal power plant, cement plant.
Background technology
In recent years, the develop rapidly along with industrial technology makes the mankind, and to the demand of fire coal, oil, natural gas, also year increases gradually, adds the surge of vehicles number, inevitably causes serious pollution to atmospheric environment.Nitrogen oxide (NO
x) be one of main chief culprit causing air environmental pollution, acid rain, photochemical fog, gray haze can be caused and great harm is caused to human health and animal and plant growth, wherein the flue gas of discharged from coal-fired boiler is that NO_x in Air Environment mainly must one of be originated, and accounts for 46%.
At present, SCR (SCR) method is most widely used the most effective general denitration technology, mainly by reducing agent NH
3mix with flue gas in injection of flue gas, under catalyst action, NH
3at a certain temperature selectively with NO
xthere is redox reaction and generate N
2and H
2o, relates generally to reaction as follows:
The selection of catalyst is link important in SCR denitration method, and most popular is at present metal oxide denitrating catalyst, mainly contains V
2o
5/ TiO
2, V
2o
5-WO
3/ TiO
2, V
2o
5-MoO
3/ TiO
2deng, this kind of catalyst activity temperature requirement is higher at about 400 DEG C, and production cost is expensive, and in addition, catalyst activity is also subject to steam, SO
2deng impact, therefore the unaffected SCR catalyst developed under low temperature environment obviously has realistic meaning.
Summary of the invention
In order to overcome the deficiencies in the prior art, the object of this invention is to provide a kind of preparation method of efficient cryogenic SCR denitration, low temperature SCR denitration catalyst prepared by the method has good low-temperature denitration performance.
A kind of efficient cryogenic SCR denitration of the present invention, is characterized in that: described catalyst body material is attapulgite and titanium dioxide compound, and helper component is fluorine.
The present invention also provides described efficient cryogenic SCR denitration preparation method, comprises the following steps:
Step 1, be distributed in 200ml deionized water by under 20g attapulgite Ultrasonic Conditions, add the hydrochloric acid solution 20ml that mass fraction is 37% more wherein, after uniform temperature water-bath back flow reaction, filtration washing is extremely neutral and dry, obtains the attapulgite after purifying for subsequent use;
Step 2, by 1g purify attapulgite join in 50ml beaker, add butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and deionized water wherein again, in room temperature, stirring reaction obtains colloidal sol and becomes gel again, and after being dried by gained gel, calcining and grinding obtains attapulgite and titanium dioxide compound is for subsequent use;
Step 3, be dissolved in 20ml deionized water by a certain amount of ammonium fluoride, add attapulgite and the titanium dioxide compound of preparation wherein, ammoniacal liquor regulates pH=10, impregnation process under uniform temperature;
After step 4, impregnation, to composite catalyst filtration washing to neutral and move to baking oven and carry out drying, then move into Muffle furnace with calcining, the SCR denitration of obtained Fluorin doped attapulgite and titanium dioxide.
As preferred preparation method, the back flow reaction described in step 1 is reflux 12 hours in 60 DEG C of water-baths.
As preferred preparation method, the consumption of the butyl titanate described in step 2, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and deionized water is respectively 8.8ml, 15ml, 10ml and 10ml.
As preferred preparation method, the calcining heat described in step 2 is 400 DEG C, and heating rate is 10-15 DEG C/min, and calcination time is 8 hours.
As preferred preparation method, the ammonium fluoride consumption described in step 3 is the mol ratio of butyl titanate and ammonium fluoride is 10 ~ 1:1.
As preferred preparation method, the uniform temperature described in step 3 is room temperature 25 DEG C, and dip time is 24 hours.
As preferred preparation method, the calcining heat described in step 4 is 300 DEG C, and heating rate is 10-15 DEG C/min, and calcination time is 6 hours.
It is the reaction of nitrogen that above-mentioned catalyst can be used for reduction of nitrogen oxide in coal-fired power plant's catalysis flue gas.
The present invention chooses attapulgite and replaces vanadium base class oxide and titanium dioxide to carry out compound, attapulgite is cheap and easy to get, cost greatly reduces relative to vanadium base class oxide, and attapulgite is a kind of layer chain richness magnesium silicate clay mineral, in needle-like or threadiness, there is larger specific area, there is-OH the tissue that can react on surface, special layer chain structure can produce flourishing zeolites duct, and there is general sticky soil characteristics, be commonly used for the carrier of adsorbent, catalyst and catalyst.
Compared with existing SCR denitration technology of preparing, the present invention has following beneficial effect:
(1) attapulgite cheap and easy to get and titanium dioxide compound is selected, greatly reduce the preparation cost of catalyst, preparation technology is simple, avoid the loss of resource in preparation process to greatest extent, specific area and the pore volume of the attapulgite after hydrochloric acid is purified increase (see table 1) greatly, thus add catalyst surface active site;
The specific area of table 1 attapulgite, hydrochloric acid-attapulgite and pore-size distribution
(2) using butyl titanate as the presoma of titanium dioxide, make butyl titanate can fully mix with it using acetylacetone,2,4-pentanedione as organic solvent, be hydrolyzed with attapulgite, fluorine under the effect of ethanol and distilled water, condensation reaction, form colloidal sol, make through ageing to be slowly polymerized between micelle to form gel, then preparing gained catalyst through calcining, drying;
(3) using ammonium fluoride as the presoma of fluorine, the doping of fluorine element can increase the acidic active sites of catalyst surface, thus produces a large amount of Lacking oxygen, further increases the catalytic performance of catalyst;
(4) prepare gained catalyst relative to using SCR catalyst widely at present, active catalytic temperature window reduces, thus avoids catalyst and easily covered by high-temperature dust and lost efficacy, and extends the service life of catalyst;
(5) coal-burning boiler produce flue gas in because temperature is more than 100 DEG C, wherein steam can be mingled with, the existence of steam can stop on a catalyst in course of reaction, the performance of conventional catalyst can should be the stop of steam and greatly reduce, and catalyst of the present invention can have good resistance to steam through experimental verification.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in more detail, but embodiments of the present invention are not limited only to this.
All first, purification processes is carried out to attapulgite in following enforcement, through following treatment step: be distributed in 200ml deionized water by under 20g attapulgite Ultrasonic Conditions, add the hydrochloric acid solution 20ml that mass fraction is 37% more wherein, after uniform temperature water-bath back flow reaction, filtration washing is extremely neutral and dry, obtains the attapulgite after purifying for subsequent use.
Embodiment 1
(1) attapulgite that 1g purifies is joined in 50ml beaker, add 8.8ml butyl titanate, 15ml absolute ethyl alcohol, 10ml acetylacetone,2,4-pentanedione and 10ml deionized water more wherein, in room temperature stirring reaction obtain colloidal sol become again gel gained gel is dried after calcining and grinding obtain attapulgite and titanium dioxide compound is for subsequent use;
(2) be dissolved in 20ml deionized water by 9.54g ammonium fluoride, add the attapulgite/titanium dioxide compound of preparation wherein, ammoniacal liquor regulates pH=10, impregnation process 24 hours at room temperature 25 DEG C;
(3), after impregnation, to composite catalyst filtration washing to neutral and move to baking oven and carry out drying, Muffle furnace is put into 300 DEG C of calcinings 6 hours, the SCR denitration of the obtained Fluorin doped attapulgite of grinding and titanium dioxide;
(4) assigned temperature window is carried out to above-mentioned catalyst and carry out SCR denitration catalytically active assessment;
(5) get 0.5g catalyst sample to load in fixed bed quartz tube reactor, reactor puts into temperature programmed control reacting furnace, controls range of reaction temperature between 80-240 DEG C; After stable 80 DEG C, 100 DEG C, 120 DEG C, 140 DEG C, 160 DEG C, 180 DEG C, 200 DEG C, 220 DEG C, 240 DEG C time, gather concentration data by flue gas analyzer, calculate the removal efficiency of nitrogen oxide;
(6) control of evaluating catalyst condition is: the flue gas of simulation respectively consists of φ (O
2)=3%, NO is 500-600ppm, N
2for Balance Air, overall flow rate is 400-600ml/min, and maintenance air speed is 25000h
-1;
(7) Study of Catalyst controls by water vapor conditions influence condition: the flue gas of simulation respectively consists of φ (O
2)=3%, NO is 500-600ppm, φ (steam)=1%, N
2for Balance Air, overall flow rate is 400-600ml/min, and maintenance air speed is 25000h
-1;
(8) evaluating catalyst result is as following table 2, wherein 160 DEG C time, removal of nitrogen oxide efficiency is 91% to the maximum, and under steam existence condition, catalytic efficiency still can reach 88%.
Table 2 evaluating catalyst result
Embodiment 2
(1) attapulgite that 1g purifies is joined in 50ml beaker, add 8.8ml butyl titanate, 15ml absolute ethyl alcohol, 10ml acetylacetone,2,4-pentanedione and 10ml deionized water more wherein, in room temperature stirring reaction obtain colloidal sol become again gel gained gel is dried after calcining and grinding obtain attapulgite and titanium dioxide compound is for subsequent use;
(2) be dissolved in 20ml deionized water by 7.63g ammonium fluoride, add the attapulgite/titanium dioxide compound of preparation wherein, ammoniacal liquor regulates pH=10, impregnation process 24 hours at room temperature 25 DEG C;
(3), after impregnation, to composite catalyst filtration washing to neutral and move to baking oven and carry out drying, Muffle furnace is put into 300 DEG C of calcinings 6 hours, the SCR denitration of the obtained Fluorin doped attapulgite of grinding and titanium dioxide;
(4) assigned temperature window is carried out to above-mentioned catalyst and carry out SCR denitration catalytically active assessment;
(5) get 0.5g catalyst sample to load in fixed bed quartz tube reactor, reactor puts into temperature programmed control reacting furnace, controls range of reaction temperature between 80-240 DEG C; After stable 80 DEG C, 100 DEG C, 120 DEG C, 140 DEG C, 160 DEG C, 180 DEG C, 200 DEG C, 220 DEG C, 240 DEG C time, gather concentration data by flue gas analyzer, calculate the removal efficiency of nitrogen oxide;
(6) control of evaluating catalyst condition is: the flue gas of simulation respectively consists of φ (O
2)=3%, NO is 500-600ppm, N
2for Balance Air, overall flow rate is 400-600ml/min, and maintenance air speed is 25000h
-1;
(7) Study of Catalyst controls by water vapor conditions influence condition: the flue gas of simulation respectively consists of φ (O
2)=3%, NO is 500-600ppm, φ (steam)=1%, N
2for Balance Air, overall flow rate is 400-600ml/min, and maintenance air speed is 25000h
-1;
(8) evaluating catalyst result is as following table 3, and wherein during 140-160 DEG C, removal of nitrogen oxide efficiency is 96% to the maximum, and under steam existence condition, catalytic efficiency still can reach 95%.
Table 3 evaluating catalyst result
Embodiment 3
(1) attapulgite that 1g purifies is joined in 50ml beaker, add 8.8ml butyl titanate, 15ml absolute ethyl alcohol, 10ml acetylacetone,2,4-pentanedione and 10ml deionized water more wherein, in room temperature stirring reaction obtain colloidal sol become again gel gained gel is dried after calcining and grinding obtain attapulgite and titanium dioxide compound is for subsequent use;
(2) be dissolved in 20ml deionized water by 5.74g ammonium fluoride, add the attapulgite/titanium dioxide compound of preparation wherein, ammoniacal liquor regulates pH=10, impregnation process 24 hours at room temperature 25 DEG C;
(3), after impregnation, to composite catalyst filtration washing to neutral and move to baking oven and carry out drying, Muffle furnace is put into 300 DEG C of calcinings 6 hours, the SCR denitration of the obtained Fluorin doped attapulgite of grinding and titanium dioxide;
(4) assigned temperature window is carried out to above-mentioned catalyst and carry out SCR denitration catalytically active assessment;
(5) get 0.5g catalyst sample to load in fixed bed quartz tube reactor, reactor puts into temperature programmed control reacting furnace, controls range of reaction temperature between 80-240 DEG C; After stable 80 DEG C, 100 DEG C, 120 DEG C, 140 DEG C, 160 DEG C, 180 DEG C, 200 DEG C, 220 DEG C, 240 DEG C time, gather concentration data by flue gas analyzer, calculate the removal efficiency of nitrogen oxide;
(6) control of evaluating catalyst condition is: the flue gas of simulation respectively consists of φ (O
2)=3%, NO is 500-600ppm, N
2for Balance Air, overall flow rate is 400-600ml/min, and maintenance air speed is 25000h
-1;
(7) Study of Catalyst controls by water vapor conditions influence condition: the flue gas of simulation respectively consists of φ (O
2)=3%, NO is 500-600ppm, φ (steam)=1%, N
2for Balance Air, overall flow rate is 400-600ml/min, and maintenance air speed is 25000h
-1; (8) evaluating catalyst result is as following table 4, wherein 160 DEG C time, removal of nitrogen oxide efficiency is 96% to the maximum, and under steam existence condition, catalytic efficiency still can reach 91%.
Table 4 evaluating catalyst result
Embodiment 4
(1) attapulgite that 1g purifies is joined in 50ml beaker, add 8.8ml butyl titanate, 15ml absolute ethyl alcohol, 10ml acetylacetone,2,4-pentanedione and 10ml deionized water more wherein, in room temperature stirring reaction obtain colloidal sol become again gel gained gel is dried after calcining and grinding obtain attapulgite and titanium dioxide compound is for subsequent use;
(2) be dissolved in 20ml deionized water by 3.82g ammonium fluoride, add the attapulgite/titanium dioxide compound of preparation wherein, ammoniacal liquor regulates pH=10, impregnation process 24 hours at room temperature 25 DEG C;
(3), after impregnation, to composite catalyst filtration washing to neutral and move to baking oven and carry out drying, Muffle furnace is put into 300 DEG C of calcinings 6 hours, the SCR denitration of the obtained Fluorin doped attapulgite of grinding and titanium dioxide;
(4) assigned temperature window is carried out to above-mentioned catalyst and carry out SCR denitration catalytically active assessment;
(5) get 0.5g catalyst sample to load in fixed bed quartz tube reactor, reactor puts into temperature programmed control reacting furnace, controls range of reaction temperature between 80-240 DEG C; After stable 80 DEG C, 100 DEG C, 120 DEG C, 140 DEG C, 160 DEG C, 180 DEG C, 200 DEG C, 220 DEG C, 240 DEG C time, gather concentration data by flue gas analyzer, calculate the removal efficiency of nitrogen oxide;
(6) control of evaluating catalyst condition is: the flue gas of simulation respectively consists of φ (O
2)=3%, NO is 500-600ppm, N
2for Balance Air, overall flow rate is 400-600ml/min, and maintenance air speed is 25000h
-1;
(7) Study of Catalyst controls by water vapor conditions influence condition: the flue gas of simulation respectively consists of φ (O
2)=3%, NO is 500-600ppm, φ (steam)=1%, N
2for Balance Air, overall flow rate is 400-600ml/min, and maintenance air speed is 25000h
-1;
(8) evaluating catalyst result is as following table 5, wherein 160 DEG C time, removal of nitrogen oxide efficiency is 91% to the maximum, and under steam existence condition, catalytic efficiency still can reach 87%.
Table 5 evaluating catalyst result
Embodiment 5
(1) attapulgite that 1g purifies is joined in 50ml beaker, add 8.8ml butyl titanate, 15ml absolute ethyl alcohol, 10ml acetylacetone,2,4-pentanedione and 10ml deionized water more wherein, in room temperature stirring reaction obtain colloidal sol become again gel gained gel is dried after calcining and grinding obtain attapulgite and titanium dioxide compound is for subsequent use;
(2) be dissolved in 20ml deionized water by 1.91g ammonium fluoride, add the attapulgite/titanium dioxide compound of preparation wherein, ammoniacal liquor regulates pH=10, impregnation process 24 hours at room temperature 25 DEG C;
(3), after impregnation, to composite catalyst filtration washing to neutral and move to baking oven and carry out drying, Muffle furnace is put into 300 DEG C of calcinings 6 hours, the SCR denitration of the obtained Fluorin doped attapulgite of grinding and titanium dioxide;
(4) assigned temperature window is carried out to above-mentioned catalyst and carry out SCR denitration catalytically active assessment;
(5) get 0.5g catalyst sample to load in fixed bed quartz tube reactor, reactor puts into temperature programmed control reacting furnace, controls range of reaction temperature between 80-240 DEG C; After stable 80 DEG C, 100 DEG C, 120 DEG C, 140 DEG C, 160 DEG C, 180 DEG C, 200 DEG C, 220 DEG C, 240 DEG C time, gather concentration data by flue gas analyzer, calculate the removal efficiency of nitrogen oxide;
(6) control of evaluating catalyst condition is: the flue gas of simulation respectively consists of φ (O
2)=3%, NO is 500-600ppm, N
2for Balance Air, overall flow rate is 400-600ml/min, and maintenance air speed is 25000h
-1;
(7) Study of Catalyst controls by water vapor conditions influence condition: the flue gas of simulation respectively consists of φ (O
2)=3%, NO is 500-600ppm, φ (steam)=1%, N
2for Balance Air, overall flow rate is 400-600ml/min, and maintenance air speed is 25000h
-1;
(8) evaluating catalyst result is as following table 6, and wherein during 140-160 DEG C, removal of nitrogen oxide efficiency is 93% to the maximum, and under steam existence condition, catalytic efficiency still can reach 88%.
Table 6 evaluating catalyst result
Claims (8)
1. an efficient cryogenic SCR denitration, is characterized in that: described catalyst body material is attapulgite and titanium dioxide compound, and helper component is fluorine.
2. the preparation method of efficient cryogenic SCR denitration according to claim 1, is characterized in that, comprise the steps:
Step 1, be distributed in 200ml deionized water by under 20g attapulgite Ultrasonic Conditions, add the hydrochloric acid solution 20ml that mass fraction is 37% more wherein, after uniform temperature water-bath back flow reaction, filtration washing is extremely neutral and dry, obtains the attapulgite after purifying for subsequent use;
Step 2, by 1g purify attapulgite join in 50ml beaker, add butyl titanate, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and deionized water wherein again, in room temperature stirring reaction obtain colloidal sol become again gel gained gel is dried after calcining and grinding obtain attapulgite and titanium dioxide compound is for subsequent use;
Step 3, be dissolved in 20ml deionized water by a certain amount of ammonium fluoride, add attapulgite and the titanium dioxide compound of preparation wherein, ammoniacal liquor regulates pH=10, impregnation process under uniform temperature;
After step 4, impregnation, to composite catalyst filtration washing to neutral and move to baking oven and carry out drying, then move into Muffle furnace with calcining, the SCR denitration of obtained Fluorin doped attapulgite and titanium dioxide.
3. the preparation method of efficient cryogenic SCR denitration according to claim 2, is characterized in that: the back flow reaction described in step 1 is reflux 12 hours in 60 DEG C of water-baths.
4. the preparation method of efficient cryogenic SCR denitration according to claim 2, is characterized in that: the consumption of the butyl titanate described in step 2, absolute ethyl alcohol, acetylacetone,2,4-pentanedione and deionized water is respectively 8.8ml, 15ml, 10ml and 10ml.
5. the preparation method of efficient cryogenic SCR denitration according to claim 2, is characterized in that: the calcining heat described in step 2 is 400 DEG C, and heating rate is 10-15 DEG C/min, and calcination time is 8 hours.
6. the preparation method of efficient cryogenic SCR denitration according to claim 2, is characterized in that: the ammonium fluoride consumption described in step 3 is the mol ratio of butyl titanate and ammonium fluoride is 10 ~ 1:1.
7. the preparation method of efficient cryogenic SCR denitration according to claim 2, is characterized in that: the uniform temperature described in step 3 is room temperature 25 DEG C, and dip time is 24 hours.
8. the preparation method of efficient cryogenic SCR denitration according to claim 2, is characterized in that: the calcining heat described in step 4 is 300 DEG C, and heating rate is 10-15 DEG C/min, and calcination time is 6 hours.
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| CN106540684A (en) * | 2016-12-06 | 2017-03-29 | 北京国电龙源环保工程有限公司 | High activity honeycomb fashion SCR catalyst and preparation method thereof |
| CN106732541A (en) * | 2016-12-07 | 2017-05-31 | 盐城复华环保产业开发有限公司 | Method for preparing low-temperature selective catalytic reduction denitration catalyst by ultrasonic impregnation method |
| CN107042102A (en) * | 2016-12-07 | 2017-08-15 | 盐城复华环保产业开发有限公司 | Selective catalytic reduction low-temperature denitration catalyst and preparation method thereof |
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| CN109111693A (en) * | 2018-06-29 | 2019-01-01 | 江苏德溢利新材料科技有限公司 | A kind of glass reinforced plastic photovoltaic bracket that high-ductility is weather-proof |
| CN109111651A (en) * | 2018-06-29 | 2019-01-01 | 江苏德溢利新材料科技有限公司 | A kind of weather-proof plastics photovoltaic bracket of high-ductility |
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| CN106540684A (en) * | 2016-12-06 | 2017-03-29 | 北京国电龙源环保工程有限公司 | High activity honeycomb fashion SCR catalyst and preparation method thereof |
| CN106540684B (en) * | 2016-12-06 | 2019-05-10 | 北京国电龙源环保工程有限公司 | The preparation method of high activity honeycomb fashion SCR catalyst |
| CN106732541A (en) * | 2016-12-07 | 2017-05-31 | 盐城复华环保产业开发有限公司 | Method for preparing low-temperature selective catalytic reduction denitration catalyst by ultrasonic impregnation method |
| CN107042102A (en) * | 2016-12-07 | 2017-08-15 | 盐城复华环保产业开发有限公司 | Selective catalytic reduction low-temperature denitration catalyst and preparation method thereof |
| CN108912608A (en) * | 2018-06-29 | 2018-11-30 | 江苏德溢利新材料科技有限公司 | A kind of the glass reinforced plastic photovoltaic bracket and its processing technology of modification |
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| CN114433071A (en) * | 2021-12-29 | 2022-05-06 | 江苏世清环保科技有限公司 | Denitration catalyst prepared by taking attapulgite as carrier and preparation method thereof |
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