CN106731234B - A kind of preparation method of binary denitration sulfur resistant catalyst composite filtering material - Google Patents

A kind of preparation method of binary denitration sulfur resistant catalyst composite filtering material Download PDF

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CN106731234B
CN106731234B CN201611126118.4A CN201611126118A CN106731234B CN 106731234 B CN106731234 B CN 106731234B CN 201611126118 A CN201611126118 A CN 201611126118A CN 106731234 B CN106731234 B CN 106731234B
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CN106731234A (en
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郑玉婴
郑伟杰
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Fuzhou University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8621—Removing nitrogen compounds
    • B01D53/8625—Nitrogen oxides
    • B01D53/8628—Processes characterised by a specific catalyst
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/889—Manganese, technetium or rhenium
    • B01J23/8892—Manganese
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/10—Filtering material manufacturing

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Abstract

The present invention provides a kind of preparation methods of binary denitration sulfur resistant catalyst composite filtering material.Using the polyphenyl thioether filter material by surfactant processing as carrier, KMnO4And MnSO4·H2O and (NH4)6Mo7O24·4H2O is catalyst precursor, and using deionized water as solvent, compound filter material is made by high temperature and pressure hydro-thermal method.The present invention is due to using binary denitration sulfur resistant catalyst, denitration sulfur resistance more better than single component catalyst, and using the method for high temperature and pressure hydro-thermal, be conducive to catalyst in the generation and load on polyphenyl thioether filter material surface, the load capacity of catalyst is greater than 5mg/cm2When all can get preferable denitration performance.Reaction synthesis process of the present invention is quickly and easy to operate, and composite filtering material obtained is suitable for dedusting agent and denitrfying agent.

Description

A kind of preparation method of binary denitration sulfur resistant catalyst composite filtering material
Technical field
The invention belongs to functional composite filtering material technical field, it is related specifically to prepare a kind of binary denitration sulfur resistant catalyst The preparation method of composite filtering material.
Background technique
China is the country an of oil starvation, few gas, rich coal, and coal is the main energy sources in China, the burning meeting of coal feedstock Generate a large amount of pollutant, 87% sulfur dioxide in air pollutants（SO2）, 71% carbon monoxide（CO）, 67% nitrogen oxidation Object（NOx）Flue dust with 60% derives from the burning of coal feedstock.Most pollutant is oxynitrides, NOxWith SO2, CO it is eponymous, become and cause one of primary pollution source of air pollution, mainly include nitric oxide（NO）, nitrogen dioxide（NO2） And nitrous oxide（N2O）, wherein NO accounts for 90-95%, NO2Account for 5-10%, and N2O only has 1% or so.NO in airxTo people Class health and ecological environment have serious harm.NO is the gas of colorless and odorless, with the oxygen binding ability in hemoglobin It is very strong, the oxygen carrying capacity of blood can be seriously affected and stimulate the eyes of people, respirator official rank, cell carcinogenesis can be induced when serious. In addition, NO is also easy to spontaneous in air be oxidized to NO2, to cause more serious consequence.
Another part pollutant is sulfide, and element sulphur is in final coal-fired flue-gas with SO2Form exists.SO2It is a kind of colourless Gas with intense irritation smell is easily soluble in the blood and other stickiness liquid of human body.SO in atmosphere2It will lead to breathing Road inflammation, bronchitis, pulmonary emphysema, eye conjunctiva inflammation etc..Also teen-age immunity can simultaneously reduced, disease resistance becomes It is weak. SO2Under the action of oxidant, light, sulfate aerosol can be generated, sulfate aerosol can make one pathogenic, increase patient The death rate.According to Economic Cooperation Development Organization（OECD）Research, when sulfate year concentration in 10 μ g/m3When left and right, often subtract Few 10% concentration can make the death rate reduce by 0.5%； SO2It can also stick with the floating dust in atmosphere, suck and have when human body respiration SO2Floating dust, SO can be made2Toxicity enhancing.Studies have shown that in the SO of high concentration2Under the influence of, plant generates acute hazard, leaf Piece surface generates necrotic plaque, or directly makes plant leaf blade is withered to fall off；In low concentration SO2Under the influence of, the growth function of plant It is affected, yield is caused to decline, deterioration.
It is used to handle exhaust gas caused by absorption coal-fired boiler in power plant and waste incineration at present and mainly selects filtrate, wherein gathers Diphenyl sulfide（PPS）Filtrate is the preferred material on current coal-fired boiler in power plant and waste incineration filter bag, because it is with high temperature resistant, anti- Hydrolysis, high fire-retardance, acid and alkali-resistance excellent properties.However, high-temperature area of the temperature window of commercial catalyst at 300-400 DEG C, Much higher than the use temperature of polyphenyl thioether filter material（170 DEG C or so）；In addition, the inert molecular structure of polyphenylene sulfide also makes its surface It is difficult to fix catalyst granules.Therefore, research and develop efficient cryogenic binary denitration sulfur resistant catalyst and its with filtrate The research emphasis that complex technique becomes.
The vanadium titanium System Catalyst light-off temperature having been commercialized is high（>300℃）, it is difficult to it is answered in smoke processing system end With, and installation and operation is costly.Therefore, economy is high and is suitable for the low-temperature SCR technology of end-o f-pipe -control as researcher The hot spot of concern.Carrier-free Mn-MoOxCatalyst recorded in many documents its in low temperature efficient denitration efficiency, take off Nitre ability NOx at 120 DEG C can be almost completely converted into N2The first choice of denitration process, but without suitable technology by its at Function is applied on filtrate.Therefore the breakthrough utilization high temperature and pressure hydro-thermal method of this patent is supported on filtrate.
Summary of the invention
The invention aims to prepare efficient denitration sulfur resistive binary catalyst and polyphenylene sulfide（PPS）It combines One step of catalyst is loaded to polyphenylene sulfide by way of hydro-thermal method by method（PPS）Surface, due to the hydro-thermal of high temperature and pressure Method, make Mn-MoOxCatalyst is uniformly secured in PPS area load, and out of stock rate with higher and preferable sulfur resistive effect Fruit.
The technical solution adopted by the present invention is that：
A kind of preparation method of binary denitration sulfur resistant catalyst composite filtering material：With the polyphenylene sulfide by surfactant processing Ether is carrier, KMnO4And MnSO4·H2O and (NH4)6Mo7O24·4H2O is catalyst precursor, using deionized water as solvent, is led to It crosses high-temperature high pressure water thermal method and compound filter material is made.
Specific step is as follows：
（1）Claim 0.0273g lauryl sodium sulfate to be dissolved in 50ml deionized water, is then placed in the polyphenyl for being cut into sequin Thioether filtrate is ultrasonically treated 1h, further takes out and be dried for standby；
（2）By Ammonium Molybdate Tetrahydrate（(NH4)6Mo7O24·4H2O）It is added in the beaker for filling 20ml deionized water, and It is put into stirrer, stirs 5min at room temperature, after completely dissolution to Ammonium Molybdate Tetrahydrate, the KMnO of configuration 0.2M is added4Solution 20 ~ 80ml, and 10min is stirred at room temperature.
（3）It is stirred evenly after 10min to solution, configures the MnSO of 0.006 ~ 0.024mol4·H2O solution 30ml is simultaneously surpassing It is dissolved under acoustic environment, uniformly mixed solution before being added later, while processed PPS filtrate before addition, then in room temperature Lower stirring 15min.
（4）Uniformly mixed solution is poured into polytetrafluoroethylliner liner, in being put into autoclave, is placed in 180 DEG C true 18h is reacted in empty drying box, takes out autoclave later, and it is to be measured to be cooled to the clean drying of room temperature opening reaction kettle taking-up PPS filtrate.
Further, it counts in mass ratio, polyphenylene sulfide：Potassium permanganate=1:1.5-2.5.
Further, the Mn in solution:The molar ratio of Mo is 1 ~ 3:1.
The filtrate be polyphenylene sulfide needle punched filter material, be using polyphenylene sulfide fibre as raw material, through shredding, compound mixing, Combing, lapping, needle thorn, thermal finalization and press polish of singing are prepared, and 40 μm of average pore size.
The composite filtering material can be used as dedusting agent and denitrfying agent application simultaneously, and the load capacity of catalyst is greater than 5mg/cm2 When all can get preferable denitration performance.
The present invention pre-processes polyphenylene thioether PPS filtrate using surfactant SDS, its surface is made to obtain more activity Oxygen-containing functional group, such as hydroxyl, carboxyl etc..Since the presence of these oxygen-containing functional groups makes inert polyphenylene sulfide surface originally It is activated, and (NH can be absorbed by electrostatic effect4)6Mo7O24·4H2O and MnSO4·H2Mo in O4+And Mn2+, for it Catalyst is generated in PPS filter material surface afterwards, and basis is provided.
Beneficial effects of the present invention：
1, compared to the out of stock filtrate based on unitary Mn base, during denitration, SO in exhaust gas2Easy and NO_x Reduction by Effective Catalyst MnOxReaction forms MnSO4, catalyst deactivation, the out of stock rate for resulting in filtrate are greatly reduced at this time, or even almost Denitration performance is lost, this law is due to having added rare earth element Mo, and Mo is the sulfur resistive agent of current mainstream, has good sulfur resistive effect Fruit, therefore make it have denitration sulfur resistance more better than single component catalyst.
2, catalyst is to be supported on polyphenylene sulfide by high temperature and pressure hydro-thermal method（PPS）On, first is that passing through pyroreaction It is catalyst in PPS Surface Creation, second is that being supported on remaining catalyst in solution on PPS by suppressing.It efficiently utilizes, surely Fixed load.
3, reaction synthesis process and operation are all very simple, and its rapid reaction, reaction vessel generally use simply, and There are no pollution to the environment for synthetic, and the filter material surface load capacity after synthesis is uniformly and secured, and out of stock rate is high.
4, the catalyst generated in synthesis process can recycle use, environment-friendly high-efficiency.
Detailed description of the invention
In the test of Fig. 1 catalyst activity, tubular type SCR reactor assembly figure is made by oneself.In figure, 1 is gas source；2 be pressure reducing valve；3 For mass flowmenter；4 be mixer；5 be air preheater；6 be catalytic bed；7 be filtrate；8 be flue gas analyzer.；Fig. 2 is Element M n:Mo molar ratio 2:The scanning electron microscope (SEM) photograph of the sample prepared when 1.
Specific embodiment
It is several specific embodiments of the invention below, further illustrates the present invention, but the present invention is not limited only to this.
PPS Nomex filtrate in the following example is prepared as follows to obtain：It is original with polyphenylene sulfide (PPS) fiber Nomex filtrate, average pore size is prepared through shredding, compound mixing, combing, lapping, needle thorn, thermal finalization and press polish of singing in material 40μm。
Embodiment 1
0.0273g lauryl sodium sulfate is claimed to be added in 50ml deionized water first, being then placed in and being cut into quality is 0: The PPS filtrate disk of 4213g is ultrasonically treated 1h, has handled taking-up and has been dried for standby.20ml deionized water is weighed again, and 250ml is added Beaker in.Then precise Ammonium Molybdate Tetrahydrate（(NH4)6Mo7O24·4H2O）1.7651g is added magneton and stirs 5min, Until solution is uniformly mixed.Configuration concentration is the liquor potassic permanganate 20ml of 0.2M, by the solution matched ultrasound or is shaken It shakes to solute and is completely dissolved, in the beaker before being added, be mixed together stirring 4min.It is reconfigured the sulfuric acid monohydrate of 0.006mol Manganese 30ml is added in solution uniformly mixed before, at this time the Mn in solution:The ratio of Mo is 1:1, the PPS that will be dried before Filtrate disk is added thereto, and is placed in and is stirred 15min at room temperature, and solution is sepia after mixing.
It is to be mixed uniformly after, transfer the solution into polytetrafluoroethylliner liner, post package be sealed in autoclave, place 18h is reacted in 180 DEG C of vacuum oven, is placed in cools down at room temperature after reaction, opens autoclave after being cooled to room temperature PPS filtrate is taken out, and is cleaned with deionized water and ethyl alcohol, dry 4h is placed in 105 DEG C, it is to be tested.The quality meter of potassium permanganate It calculates as follows：0.2×0.02×158=0.632g.
The denitration performance of composite filtering material is evaluated in self-control tubular type SCR reactor.NO and NH3Volume fraction is 0.05 %, O2Volume fraction is 5 %, remaining is N2, gas flow rate 700mLmin-1, temperature setting is 140 DEG C, uses Britain It is 69% that KM940 flue gas analyzer, which measures denitrification rate,；Temperature setting is 160 DEG C, denitrification rate 80%, and temperature setting is 180 DEG C, is taken off Nitre rate is 99%.And sulfur resistive ability is tested in 180 DEG C of interval 30min, last out of stock rate is basically stable at 44%.
Embodiment 2
Claim 0.0273g lauryl sodium sulfate to be added in 50ml deionized water first, is then placed in and is cut into quality and is The PPS filtrate disk of 0.6320g is ultrasonically treated 1h, has handled taking-up and has been dried for standby.The addition of 20ml deionized water is weighed again In the beaker of 250ml.Then precise Ammonium Molybdate Tetrahydrate（(NH4)6Mo7O24·4H2O）1.7651g magneton stirring is added 5min, until solution is uniformly mixed.Configuration concentration be 0.2M liquor potassic permanganate 40ml, by the solution matched ultrasound or Person, which rocks to solute, to be completely dissolved, and in the beaker before being added, is mixed together stirring 4min.It is reconfigured a hydration of 0.012mol Manganese sulfate 30ml is added in solution uniformly mixed before, at this time the Mn in solution:The ratio of Mo is 2:1, by what is dried before PPS filtrate disk is added thereto, and is placed in and is stirred 15min at room temperature, and solution is sepia after mixing.
It is to be mixed uniformly after, transfer the solution into polytetrafluoroethylliner liner, post package be sealed in autoclave, place 18h is reacted in 180 DEG C of vacuum oven, is placed in cools down at room temperature after reaction, opens autoclave after being cooled to room temperature PPS filtrate is taken out, and is cleaned with deionized water and ethyl alcohol, dry 4h is placed in 105 DEG C, it is to be tested.The quality meter of potassium permanganate It calculates as follows：0.2×0.04×158=1.264g.
The denitration performance of composite filtering material is evaluated in self-control tubular type SCR reactor.NO and NH3Volume fraction is 0.05 %, O2Volume fraction is 5 %, remaining is N2, gas flow rate 700mLmin-1, temperature setting is 140 DEG C, uses Britain It is 77% that KM940 flue gas analyzer, which measures denitrification rate,；Temperature setting is 160 DEG C, denitrification rate 100%.And it is spaced at 180 DEG C 30min tests sulfur resistive ability, and last out of stock rate is basically stable at 55%.
Embodiment 3
Claim 0.0273g lauryl sodium sulfate to be added in 50ml deionized water first, is then placed in and is cut into quality and is The PPS filtrate disk of 1.011g is ultrasonically treated 1h, has handled taking-up and has been dried for standby.20ml deionized water is weighed again, and 250ml is added Beaker in.Then precise Ammonium Molybdate Tetrahydrate（(NH4)6Mo7O24·4H2O）1.7651g is added magneton and stirs 5min, Until solution is uniformly mixed.Configuration concentration is the liquor potassic permanganate 80ml of 0.2M, by the solution matched ultrasound or is shaken It shakes to solute and is completely dissolved, in the beaker before being added, be mixed together stirring 4min.It is reconfigured the sulfuric acid monohydrate of 0.009mol Manganese 30ml is added in solution uniformly mixed before, at this time the Mn in solution:The ratio of Mo is 2.5:1, by what is dried before PPS filtrate disk is added thereto, and is placed in and is stirred 15min at room temperature, and solution is sepia after mixing.
It is to be mixed uniformly after, transfer the solution into polytetrafluoroethylliner liner, post package be sealed in autoclave, place 18h is reacted in 200 DEG C of vacuum oven, is placed in cools down at room temperature after reaction, opens autoclave after being cooled to room temperature PPS filtrate is taken out, and is cleaned with deionized water and ethyl alcohol, dry 4h is placed in 105 DEG C, it is to be tested.The quality meter of potassium permanganate It calculates as follows：0.2×0.08×158=2.528g.
The denitration performance of composite filtering material is evaluated in self-control tubular type SCR reactor.NO and NH3Volume fraction is 0.05 %, O2Volume fraction is 5 %, remaining is N2, gas flow rate 700mLmin-1, temperature setting is 140 DEG C, uses Britain It is 70% that KM940 flue gas analyzer, which measures denitrification rate,；Temperature setting is 160 DEG C, denitrification rate 81%；Temperature setting is 180 DEG C, is taken off Pin rate is 100%.And sulfur resistive ability is tested in 180 DEG C of interval 30min, last out of stock rate is basically stable at 48%.
Embodiment 4
Claim 0.0273g lauryl sodium sulfate to be added in 50ml deionized water first, is then placed in and is cut into quality and is The PPS filtrate disk of 1.011g is ultrasonically treated 1h, has handled taking-up and has been dried for standby.20ml deionized water is weighed again, and 250ml is added Beaker in.Then precise Ammonium Molybdate Tetrahydrate（(NH4)6Mo7O24·4H2O）1.7651g is added magneton and stirs 5min, Until solution is uniformly mixed.Configuration concentration is the liquor potassic permanganate 80ml of 0.2M, by the solution matched ultrasound or is shaken It shakes to solute and is completely dissolved, in the beaker before being added, be mixed together stirring 4min.It is reconfigured the sulfuric acid monohydrate of 0.014mol Manganese 30ml is added in solution uniformly mixed before, at this time the Mn in solution:The ratio of Mo is 3:1, the PPS that will be dried before Filtrate disk is added thereto, and is placed in and is stirred 15min at room temperature, and solution is sepia after mixing.
It is to be mixed uniformly after, transfer the solution into polytetrafluoroethylliner liner, post package be sealed in autoclave, place 18h is reacted in 200 DEG C of vacuum oven, is placed in cools down at room temperature after reaction, opens autoclave after being cooled to room temperature PPS filtrate is taken out, and is cleaned with deionized water and ethyl alcohol, dry 4h is placed in 105 DEG C, it is to be tested.The quality meter of potassium permanganate It calculates as follows：0.2×0.08×158=2.528g.
The denitration performance of composite filtering material is evaluated in self-control tubular type SCR reactor.NO and NH3Volume fraction is 0.05 %, O2Volume fraction is 5 %, remaining is N2, gas flow rate 700mLmin-1, temperature setting is 140 DEG C, uses Britain It is 66% that KM940 flue gas analyzer, which measures denitrification rate,；Temperature setting is 160 DEG C, denitrification rate 77%；Temperature setting is 180 DEG C, is taken off Pin rate is 99%.And sulfur resistive ability is tested in 180 DEG C of interval 30min, last out of stock rate is basically stable at 47%.
Activity rating：Catalyst is evaluated in self-control tubular type SCR reactor.Reactor is external electric, reaction Thermocouple measuring temperature is placed by pipe catalyst bed, experimental provision process is as shown in Figure 1.It is formed with steel gas cylinder simulated flue gas, It include NO, O in flue gas2、N2、NH3For reducing gas, NO and NH3Volume fraction is 0.04-0.06%, O2Volume fraction is 4- 6%, remaining is N2, gas flow rate 700mLmin-1, temperature control is between 120 ~ 200 DEG C, and gas flow, composition are by quality stream Meter regulation and control.Gas analysis uses Britain KM940 flue gas analyzer, in order to guarantee the stability and accuracy of data, At least stable 30min of each operating condition.
Influence of 1 various factors of table to composite filtering material denitrification rate（Reaction temperature is 180 DEG C）：
As can be seen from Table 1, it when 140 DEG C, as the molar ratio of two metallic elements is continuously increased, takes off Nitre rate is with the trend for occurring first increasing to reduction after a maximum value, 1:2 there is maximum value.And to 180 DEG C, all reach 100% denitrification rate substantially.And best sulfur resistance is shown at 180 DEG C.

Claims (4)

1. a kind of preparation method of binary denitration sulfur resistant catalyst composite filtering material, it is characterised in that：By at surfactant The polyphenyl thioether filter material of reason is carrier, KMnO4And MnSO4·H2O and (NH4)6Mo7O24·4H2O is catalyst precursor, to go Ionized water is solvent, and compound filter material is made by high temperature and pressure hydro-thermal method；The polyphenyl thioether filter material is with polyphenylene sulfide Fiber is raw material, is prepared through shredding, compound mixing, combing, lapping, needle thorn, thermal finalization and press polish of singing, average pore size 40 μm；Specific preparation process is as follows：
（1）Claim 0.0273g lauryl sodium sulfate to be dissolved in 50ml deionized water, is then placed in the polyphenylene sulfide for being cut into sequin Filtrate is ultrasonically treated 1h, further takes out and be dried for standby；
（2）By (NH4)6Mo7O24·4H2O is dissolved in 20ml deionized water, stirs and evenly mixs 5min；
（3）Prepare the KMnO of 0.2M420 ~ 80ml of solution, and and step（2）Solution is mixed together stirring 4min；
（4）Prepare the MnSO of 0.006 ~ 0.024mol4·H2O solution 30ml, with step（3）Mixed liquor mixing, while by step （1）Polyphenyl thioether filter material disk be added thereto, be placed in and stir 15min at room temperature, after mixing solution be sepia；
（5）By step（4）Mixed solution is transferred in polytetrafluoroethylliner liner, and post package is sealed in autoclave, is placed in 18h is reacted in 180 ~ 200 DEG C of vacuum oven, room temperature is cooling after reaction, takes out polyphenyl thioether filter material, and use deionization Water and ethyl alcohol are cleaned, and dry 4h is placed in 105 DEG C.
2. the preparation method of binary denitration sulfur resistant catalyst composite filtering material according to claim 1, it is characterised in that：By matter Amount is than meter, polyphenyl thioether filter material：Potassium permanganate=1:1.5-2.5.
3. the preparation method of binary denitration sulfur resistant catalyst composite filtering material according to claim 1, it is characterised in that：Solution In Mn:The molar ratio of Mo is 1 ~ 3:1.
4. a kind of application of the binary denitration sulfur resistant catalyst composite filtering material of the preparation of preparation method according to claim 1, feature It is：The composite filtering material is applied to dedusting agent and denitrfying agent.
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