CN102120116A - Denitration catalyst-supported compound filter material and preparation method thereof - Google Patents

Denitration catalyst-supported compound filter material and preparation method thereof Download PDF

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CN102120116A
CN102120116A CN 201110044471 CN201110044471A CN102120116A CN 102120116 A CN102120116 A CN 102120116A CN 201110044471 CN201110044471 CN 201110044471 CN 201110044471 A CN201110044471 A CN 201110044471A CN 102120116 A CN102120116 A CN 102120116A
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filtrate
compound
pps
denitrating catalyst
titanyl sulfate
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林锦贤
蔡伟龙
郑玉婴
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Fuzhou University
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Abstract

The invention provides a preparation technique of a catalyst-supported compound filter material, which belongs to the technical field of functional filter materials and is used for solving the problems of complex tail gas purification system and high treatment cost in the prior art. In the method, firstly a MnOx/TiO2 catalyst is prepared by a coprecipitation method, and then the catalyst is supported on the surface of the filter material by an immersion method, therefore, thus the filter material has a denitration function.

Description

Compound filtrate of a kind of load denitrating catalyst and preparation method thereof
Technical field
The invention belongs to the function filter material technical field, specially refer to the technology of making filtrate with a kind of denitrating catalyst attached to filter material surface with denitration function.
Background technology
As everyone knows, NOx is one of source of atmospheric pollution, human beings'health is constituted greatly threaten.All there is strict restriction various countries to the discharging of NOx, and standard is more and more tighter.Therefore, in the last few years, people had done number of research projects aspect flue-gas denitrification.The measure that reduces the NOx discharging at present mainly is divided into 2 kinds: burning control and flue-gas denitrification.The means of burning control are mainly and adopt that low NOx burner, flue gas recirculation, burning are burnt again, fractional combustion etc.; The method of flue-gas denitrification comprises: selective catalytic reduction (SCR), SNCR method (SNCR), red-hot carbon reduction method, wet type complexed absorption method etc.
In numerous denitride technologies, SCR is the highest, the most ripe denitride technology of nitric efficiency.The SCR method is under the special catalyst effect, optionally NOx is reduced to N with ammonia or other reducing agent 2And H 2The method of O.Because it has high efficiency and practicality, has now become the research focus in denitrogenation field.
But the present method that the general employing of control of pollutant is removed separately.Can cause the raising of the big and treatment cost of the complexity, floor space of factory's tail flue gas cleaning system thus.
In the flue gas ash removal field, sack cleaner has become the first-selection of flue gas ash removal, and the fiber source that filtrate has that technological process is simple, speed of production fast, output and labor productivity height, cost are low, available is wide, technology is grasped easily, advantage such as more than the product variety, and increase of production is very fast in worldwide in recent years.Existing deduster can only dedusting, and the NOx in the flue gas is not had the removal effect.
Summary of the invention
The objective of the invention is to provide a kind of denitrating catalyst to combine, obtain the method for the compound filtrate of catalyst, promoted the performance of filtrate on the one hand, make it have catalytic action with filtrate; On the other hand, filtrate provide gas and catalyst fabulous contact the place, reduce the restriction of gas diffusion, can reduce the catalyst that reacts required.
The technical solution used in the present invention is:
A kind of compound filtrate of load denitrating catalyst, described compound filtrate is to be carrier with the filtrate, load has the compound filtrate of denitrating catalyst, and described denitrating catalyst is manganese, the titanium composite oxide that makes with coprecipitation, and the load capacity of described denitrating catalyst is 35 ~ 80mg/cm 2
Described filtrate is a PPS+P84 macromolecule compound spiked felt filtrate, be to be raw material with polyimides (P84) fiber and polyphenylene sulfide (PPS) fiber, wherein the PPS:P84 mass ratio is 1:0.05 ~ 0.3, is prepared from through shredding, compound batch mixing, combing, lapping, acupuncture, thermal finalization and the press polish of singing.
Comparatively concrete, compound filtrate of the present invention can prepare by the following method:
(1) in the aqueous solution of titanyl sulfate and manganese acetate, drip 20 ~ 30wt% ammoniacal liquor, the control endpoint pH is 10 ~ 11, stir filter behind 1 ~ 3h, after the filter cake washing, 100 ~ 120 ℃ of down dry 5 ~ 7h again in 450 ~ 550 ℃ of roasting 4 ~ 8h, compressing tablet, to sieve be 0.5 ~ 0.8mm size particles, makes manganese, titanium composite oxide; In the aqueous solution of described titanyl sulfate and manganese acetate, the mass ratio of titanyl sulfate and manganese acetate is 0.5 ~ 1.5:1, and total mass fraction of described titanyl sulfate and manganese acetate is 13 ~ 20%;
(2) be that polyphenylene sulfide (PPS) fiber and polyimides (P84) fiber of 1:0.05 ~ 0.3 is raw material with the mass ratio, prepare PPS+P84 macromolecule compound spiked felt filtrate through shredding, compound batch mixing, combing, lapping, acupuncture, thermal finalization and the press polish of singing;
(3) in deionized water, add manganese, the titanium composite oxide that step (1) makes, stir and make the maceration extract of mass fraction 0.79 ~ 1.82%, getting the PPS+P84 macromolecule compound spiked felt filtrate that makes in the step (2) then is submerged in the maceration extract fully, soak 22 ~ 26h, after 60 ℃ ~ 120 ℃ vacuum drying, make load capacity at 35 ~ 80mg/cm 2Between the compound filtrate of load denitrating catalyst.
In the described step (3), maceration extract is with the filtrate vacuum drying, manganese, titanium composite oxide in the maceration extract all are adsorbed on the filtrate, so load capacity is calculated divided by the area that immerses the PPS+P84 macromolecule compound spiked felt filtrate in the maceration extract by the manganese of preparation maceration extract in the adding deionized water, the all-mass of titanium composite oxide.In practical operation, load capacity is a preset value, under the certain situation of filtrate area, can reach default load capacity by the manganese in the control adding deionized water, the quality of titanium composite oxide.
In the described step (1), the mass ratio of titanyl sulfate and manganese acetate is 0.5 ~ 1.5:1, preferred 0.5 ~ 1:1, most preferably 0.98:1.
Further, the present invention also provides the preparation method of the compound filtrate of described load denitrating catalyst, and described method is:
(1) titanyl sulfate is dissolved in the water under 50 ~ 70 ℃ of temperature fully, add manganese acetate again, after stirring 1 ~ 3h, obtain the aqueous solution of titanyl sulfate and manganese acetate, drip 20 ~ 30wt% ammoniacal liquor then, the control endpoint pH is 10 ~ 11, stir filter behind 1 ~ 3h, after the filter cake washing, 100 ~ 120 ℃ of down dry 5 ~ 7h again in 450 ~ 550 ℃ of roasting 4 ~ 8h, compressing tablet, to sieve be 0.5 ~ 0.8mm size particles, makes manganese, titanium composite oxide; In the aqueous solution of described titanyl sulfate and manganese acetate, the mass ratio of titanyl sulfate and manganese acetate is 0.5 ~ 1.5:1, and total mass fraction of described titanyl sulfate and manganese acetate is 13 ~ 20%;
(2) be that polyphenylene sulfide (PPS) fiber and polyimides (P84) fiber of 1:0.05 ~ 0.3 is raw material with the mass ratio, prepare PPS+P84 macromolecule compound spiked felt filtrate through shredding, compound batch mixing, combing, lapping, acupuncture, thermal finalization and the press polish of singing;
(3) in deionized water, add manganese, the titanium composite oxide that step (1) makes, stir the maceration extract that 1 ~ 3h makes mass fraction 0.79 ~ 1.82%, getting the PPS+P84 macromolecule compound spiked felt filtrate that makes in the step (2) then is submerged in the maceration extract fully, soak 22 ~ 26h, after 60 ℃ ~ 120 ℃ vacuum drying, make load capacity at 35 ~ 80mg/cm 2Between the compound filtrate of load denitrating catalyst.
The compound filtrate of load denitrating catalyst provided by the invention can be used simultaneously as dedusting agent and denitrfying agent.
The denitrating catalyst that the present invention adopts is manganese, the titanium composite oxide MnO with the coprecipitation preparation x/ TiO 2The advantage of this catalyst is: catalyst has bigger specific area, pore volume and total acid content, and pore-size distribution is the most concentrated, MnO xCan be at TiO 2Apparent height disperses, and denitration activity is best.
The compound filtrate of load denitrating catalyst provided by the invention has promoted the performance of filtrate on the one hand, makes it have catalytic action; On the other hand, filtrate provide gas and catalyst fabulous contact the place, reduce the restriction of gas diffusion, can reduce the catalyst that reacts required.And the present invention uses easyly, to using the equipment of sack cleaner, only ordinary filter need be changed into compound filtrate provided by the invention, can finish removing of oxynitrides, and required improvement cost is less.
Description of drawings
In Fig. 1 catalyst activity property testing, self-control tubular type SCR reactor assembly figure.Among the figure, 1 is N 2, 2 is O 2, 3 is NH 3, 4 is NO, and 5 is mass flowmenter, and 6 is triple valve, and 7 is thermocouple, and 8 is digital temperature programmer, and 9 is reactor, and 10 is analytical instrument, 11 is exhaust apparatus.
The compound process of preparing filter material flow chart of Fig. 2 load denitrating catalyst.
The specific embodiment
Come technical scheme of the present invention is described further with specific embodiment below, but protection scope of the present invention is not limited thereto.
PPS+P84 macromolecule compound spiked felt filtrate in the following example prepares by the following method: polyphenylene sulfide (PPS) fiber and polyimides (P84) fiber that with the mass ratio are 1:0.05 ~ 0.3 are raw material, prepare PPS+P84 macromolecule compound spiked felt filtrate through shredding, compound batch mixing, combing, lapping, acupuncture, thermal finalization and the press polish of singing.
Embodiment 1
Get the 3.26g titanyl sulfate and add in the 50mL water, under 60 ℃ of water-baths, stir, it is dissolved fully, add the 5g manganese acetate then, fully stir 2h.Drip 25% (mass fraction) ammoniacal liquor, the control endpoint pH is 10 ~ 11, continues to stir 2h.Filter, washing, with the solid that obtains at 110 ℃ of dry 6h down, 500 ℃ of roasting 6h, then compressing tablet, to sieve be 0.5~0.8mm size particles, is MnO x/ TiO 2
The MnO that in the 10mL deionized water, adds the 0.079g gained x/ TiO 2, stir 2h under the room temperature, make maceration extract, be a slice circle, diameter 17mm then, area is 0.000227m 2PPS+P84 macromolecule compound spiked felt filtrate immerse 24h in the maceration extract fully, after 60 ℃ of vacuum drying, make the compound filtrate of load denitrating catalyst then.Making catalyst loadings is 35mg/cm 2
Catalyst is estimated in self-control tubular type SCR reactor.NO and NH 3Volume fraction is 0.05 %, O 2Volume fraction is 5 %, and all the other are N 2, gas flow rate is 226mL min -1, temperature is set to 150 ℃, and recording the denitration rate with Britain's KM940 flue gas analyzer then is 60%.
Embodiment 2
Get the 3.26g titanyl sulfate and add in the 50mL water, under 60 ℃ of water-baths, stir, it is dissolved fully, add the 5g manganese acetate then, fully stir 2h.Drip 25% (mass fraction) ammoniacal liquor, the control endpoint pH is 10~11, continues to stir 2h.Filter, washing, with the solid that obtains at 110 ℃ of dry 6h down, 500 ℃ of roasting 6h, then compressing tablet, to sieve be the MnO of 0.5 ~ 0.8mm particle diameter x/ TiO 2Particle.
The MnO that in the 10mL deionized water, adds the 0.114g gained x/ TiO 2, stir 2h under the room temperature, make maceration extract, be a slice diameter 17mm then, area is 0.000227m 2Round shape PPS+P84 macromolecule compound spiked felt filtrate immerse 24h in the maceration extract fully, therefore (filtrate with the maceration extract evaporate to dryness, need not take out filtrate) makes the compound filtrate of load denitrating catalyst then after 120 ℃ of vacuum drying.Making catalyst loadings is 50mg/cm 2
Catalyst is estimated in self-control tubular type SCR reactor.NO and NH 3Volume fraction is 0.05 %, O 2Volume fraction is 5 %, and all the other are N 2, gas flow rate is 226mL min -1, temperature is set to 200 ℃, and recording the denitration rate with Britain's KM940 flue gas analyzer then is 73%.
Embodiment 3
Get the 4.90g titanyl sulfate and add in the 50mL water, under 50 ℃ of water-baths, stir, it is dissolved fully, add the 5g manganese acetate then, fully stir 1h.Drip 30% (mass fraction) ammoniacal liquor, the control endpoint pH is 10~11, continues to stir 3h.Filter, washing, with the solid that obtains at 100 ℃ of dry 7h down, 550 ℃ of roasting 4h, then compressing tablet, to sieve be the MnO of 0.5 ~ 0.8mm particle diameter x/ TiO 2Particle.
The MnO that in the 10mL deionized water, adds the 0.114g gained x/ TiO 2, stir 2h under the room temperature, make maceration extract, be a slice diameter 17mm then, area is 0.000227m 2Round shape PPS+P84 macromolecule compound spiked felt filtrate immerse 22h in the maceration extract fully, therefore (filtrate with the maceration extract evaporate to dryness, need not take out filtrate) makes the compound filtrate of load denitrating catalyst then after 100 ℃ of vacuum drying.Making catalyst loadings is 50mg/cm 2
Catalyst is estimated in self-control tubular type SCR reactor.NO and NH 3Volume fraction is 0.05 %, O 2Volume fraction is 5 %, and all the other are N 2, gas flow rate is 226mL min -1, temperature is set to 200 ℃, and recording the denitration rate with Britain's KM940 flue gas analyzer then is 92%.
Embodiment 4
Get the 3.26g titanyl sulfate and add in the 50mL water, under 70 ℃ of water-baths, stir, it is dissolved fully, add the 5g manganese acetate then, fully stir 3h.Drip 20% (mass fraction) ammoniacal liquor, the control endpoint pH is 10~11, continues to stir 1h.Filter, washing, with the solid that obtains at 120 ℃ of dry 5h down, 450 ℃ of roasting 8h, then compressing tablet, to sieve be the MnO of 0.5 ~ 0.8mm particle diameter x/ TiO 2Particle.
The MnO that in the 10mL deionized water, adds the 0.182g gained x/ TiO 2, stir 2h under the room temperature, make maceration extract, be a slice diameter 17mm then, area is 0.000227m 2Round shape PPS+P84 macromolecule compound spiked felt filtrate immerse 26h in the maceration extract fully, after 80 ℃ of vacuum drying, make the compound filtrate of load denitrating catalyst then.Making catalyst loadings is 80mg/cm 2
Catalyst is estimated in self-control tubular type SCR reactor.NO and NH 3Volume fraction is 0.05 %, O 2Volume fraction is 5 %, and all the other are N 2, gas flow rate is 226mL min -1, temperature is set to 200 ℃, and recording the denitration rate with Britain's KM940 flue gas analyzer then is 87%.
Activity rating:Catalyst is estimated in self-control tubular type SCR reactor.Reactor is an external electric, the other thermocouple measuring temperature of placing of reaction tube beds, and the experimental provision flow process is shown in Fig. 1.Catalyst granules granularity 0.5 ~ 0.8 mm, loadings is 0.4 ~ 0.6g.Form with steel gas cylinder simulated flue gas, comprise NO, O in the flue gas 2, N 2, NH 3Be reducing gas, NO and N H 3Volume fraction is 0.04 ~ 0.06 %, O 2Volume fraction is 4 ~ 6 %, and all the other are N 2, gas flow rate is 226mL min -1, temperature is controlled between 100 ~ 225 ℃, and gas flow, composition are regulated and control by mass flowmenter.Britain KM940 flue gas analyzer is adopted in gas analysis, and in order to guarantee data stability and accuracy, each operating mode is stablized 25 ~ 35 min at least.
Table 1 different catalysts load capacity and temperature are to the influence of denitration rate:
Figure 124813DEST_PATH_IMAGE001
From table 1 data as can be seen, this product has improved the denitration rate of filtrate greatly, and catalyst loadings is big more, and the denitration rate is high more; Under the identical situation of load capacity, when the ratio of the amount of substance of Mn and Ti was 1:1.5 in the catalyst, temperature denitration rate in the time of 200 ℃ was the highest.

Claims (5)

1. the compound filtrate of a load denitrating catalyst, it is characterized in that: described compound filtrate is to be carrier with the filtrate, load has the compound filtrate of denitrating catalyst, described denitrating catalyst is manganese, the titanium composite oxide that makes with coprecipitation, and the load capacity of described denitrating catalyst is 35 ~ 80mg/cm 2
2. the compound filtrate of load denitrating catalyst as claimed in claim 1, it is characterized in that described filtrate is a PPS+P84 macromolecule compound spiked felt filtrate, be to be raw material with polyimides (P84) fiber and polyphenylene sulfide (PPS) fiber, wherein the PPS:P84 mass ratio is 1:0.05 ~ 0.3, is prepared from through shredding, compound batch mixing, combing, lapping, acupuncture, thermal finalization and the press polish of singing.
3. the compound filtrate of load denitrating catalyst as claimed in claim 1 is characterized in that described compound filtrate prepares by the following method:
(1) in the aqueous solution of titanyl sulfate and manganese acetate, drip 20 ~ 30wt% ammoniacal liquor, the control endpoint pH is 10 ~ 11, stir filter behind 1 ~ 3h, after the filter cake washing, 100 ~ 120 ℃ of down dry 5 ~ 7h again in 450 ~ 550 ℃ of roasting 4 ~ 8h, compressing tablet, to sieve be 0.5 ~ 0.8mm size particles, makes manganese, titanium composite oxide; In the aqueous solution of described titanyl sulfate and manganese acetate, the mass ratio of titanyl sulfate and manganese acetate is 0.5 ~ 1.5:1, and total mass fraction of described titanyl sulfate and manganese acetate is 13 ~ 20%;
(2) be that polyphenylene sulfide (PPS) fiber and polyimides (P84) fiber of 1:0.05 ~ 0.3 is raw material with the mass ratio, prepare PPS+P84 macromolecule compound spiked felt filtrate through shredding, compound batch mixing, combing, lapping, acupuncture, thermal finalization and the press polish of singing;
(3) in deionized water, add manganese, the titanium composite oxide that step (1) makes, stir and make the maceration extract of mass fraction 0.79 ~ 1.82wt%, getting the PPS+P84 macromolecule compound spiked felt filtrate that makes in the step (2) then is submerged in the maceration extract fully, soak 22 ~ 26h, after 60 ℃ ~ 120 ℃ vacuum drying, make load capacity at 35 ~ 80mg/cm 2Between the compound filtrate of load denitrating catalyst.
4. the preparation method of the compound filtrate of load denitrating catalyst as claimed in claim 1 is characterized in that described method is:
(1) titanyl sulfate is dissolved in the water under 50 ~ 70 ℃ of temperature fully, add manganese acetate again, after stirring 1 ~ 3h, obtain the aqueous solution of titanyl sulfate and manganese acetate, drip 20 ~ 30wt% ammoniacal liquor then, the control endpoint pH is 10 ~ 11, stir filter behind 1 ~ 3h, after the filter cake washing, 100 ~ 120 ℃ of down dry 5 ~ 7h again in 450 ~ 550 ℃ of roasting 4 ~ 8h, compressing tablet, to sieve be 0.5 ~ 0.8mm size particles, makes manganese, titanium composite oxide; In the aqueous solution of described titanyl sulfate and manganese acetate, the mass ratio of titanyl sulfate and manganese acetate is 0.5 ~ 1.5:1, and total mass fraction of described titanyl sulfate and manganese acetate is 13 ~ 20%;
(2) be that polyphenylene sulfide (PPS) fiber and polyimides (P84) fiber of 1:0.05 ~ 0.3 is raw material with the mass ratio, prepare PPS+P84 macromolecule compound spiked felt filtrate through shredding, compound batch mixing, combing, lapping, acupuncture, thermal finalization and the press polish of singing;
(3) in deionized water, add manganese, the titanium composite oxide that step (1) makes, stir the maceration extract that 1 ~ 3h makes mass fraction 0.79 ~ 1.82wt%, getting the PPS+P84 macromolecule compound spiked felt filtrate that makes in the step (2) then is submerged in the maceration extract fully, soak 22 ~ 26h, after 60 ℃ ~ 120 ℃ vacuum drying, make load capacity at 35 ~ 80mg/cm 2Between the compound filtrate of load denitrating catalyst.
5. the compound filtrate while of load denitrating catalyst as claimed in claim 1 is as the application of dedusting agent and denitrfying agent.
CN 201110044471 2011-02-24 2011-02-24 Denitration catalyst-supported compound filter material and preparation method thereof Pending CN102120116A (en)

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CN105013249B (en) * 2015-07-02 2017-01-11 辽宁鸿盛环境技术集团股份有限公司 Nitre and dioxin-removal PPS composite felt functional filtering material and preparation method thereof
CN105013249A (en) * 2015-07-02 2015-11-04 辽宁鸿盛环境技术集团股份有限公司 Nitre and dioxin-removal PPS composite felt functional filtering material and preparation method thereof
CN105401248A (en) * 2015-11-30 2016-03-16 安徽省元琛环保科技有限公司 Nanofiber having catalytic function and applied to filter material and preparation method of nanofiber
CN105521659A (en) * 2016-03-11 2016-04-27 安徽省元琛环保科技有限公司 Modified filter material with low-and-medium-temperature SCR denitration activity and preparation method thereof
CN105854873A (en) * 2016-05-11 2016-08-17 四川大学 Low-temperature high-efficiency metal composite oxide denitration catalyst and preparation method thereof
CN105854873B (en) * 2016-05-11 2019-05-07 四川大学 A kind of composite oxide of metal denitrating catalyst of efficient cryogenic and preparation method thereof
WO2018045672A1 (en) * 2016-09-12 2018-03-15 福州大学 Method for in-situ generation of nanoflower-like manganese dioxide catalyst on filter material
US11565241B2 (en) 2016-09-12 2023-01-31 Fuzhou University Method for in-situ generation of nanoflower-like manganese dioxide catalyst on filter material
CN107261644A (en) * 2017-06-23 2017-10-20 山东大学 A kind of difunctional composite filtering material fiber of low temperature dedusting denitration and preparation method
CN109759053A (en) * 2019-01-21 2019-05-17 北京工业大学 A kind of preparation method of filter cloth load vanadium titanium-based catalytic denitration material
WO2021093286A1 (en) * 2019-11-12 2021-05-20 南京杰科丰环保技术装备研究院有限公司 Integrated filter material, preparation method and application
CN115337712A (en) * 2022-07-29 2022-11-15 北京工业大学 Filter material for preparing load low-temperature SCR catalyst by suction filtration method, detection and application

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Application publication date: 20110713