CN103316585B - A kind of method of organic pollution in nanometer mineral material Purge gas - Google Patents
A kind of method of organic pollution in nanometer mineral material Purge gas Download PDFInfo
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Abstract
A kind of method of organic pollution in nanometer mineral material Purge gas, it is characterized in that, preparing particle diameter within the scope of 0.5-10mm has ferriferous oxide, an iron sulfide granular material of nano-pore structure, granular material diluted acid is flooded, then load and form filtering layer in a reservoir, the filter course that waste gas containing volatile organic contaminant penetrates through nano-pore structure iron mineral material after mixing with the hydrogen peroxide of volatilization is formed, in filter course, there is the reaction of heterogeneous Fenton oxidation, thoroughly remove volatile organic matter.
Description
One, technical field
The invention belongs to environmental technology field, be specifically related to purification of volatile organic pollutant technology and material.
Two, background technology
Volatile organic matter (VOCs) typically refers to the organic compound that boiling point under normal pressure is 50-260 DEG C, as alkane, alkene, aromatic hydrocarbon, chlorinated aromatic hydrocarbons and saturated, undersaturated aldehyde, ketone etc.VOCs is mainly derived from the waste gas of the industry discharges such as oil, chemical industry, papermaking, paint, mining, metal plating and weaving, and the waste gas that numerous vehicles discharge.
According to statistics, between 2005-2010, China's VOCs total emission volumn is about 2650-3100 ten thousand tons, and China in 2010 only application of paints process just to air release VOCs about 3,880,000 tons, in volatile organic waste gas always discharges, occupy significant proportion.Five compounds such as benzene homologues, alcohol, vinegar, ether, ketone are the main components of current application of paints discharge organic exhaust gas, and account for 29% of total amount, 19%, 13%, 10% and 11% respectively, wherein 31% is poisonous and harmful substance, based on toluene and dimethylbenzene.Along with social development and people are to the raising of environmental quality requirement, strict environmental regulation has been formulated in the discharge of countries in the world to organic exhaust gas, as the U.S., Japan, Germany etc. have all formulated strict organic exhaust gas discharge standard, particularly common with supervirulent industrial organic exhaust gas to benzene homologues, polycyclic aromatic hydrocarbon, Polychlorinated biphenyls, dioxin etc., cause the concern of people and environmental worker especially.U.S.Clean Air amendment (l990) requires in the toxic air contaminant of 189 kinds of priority acccess control of monitoring, about has 100 kinds for volatile organic contaminant; Define the emission limit of 33 kinds of pollutants in " discharge standard of air pollutants " that China enacts and enforces for 1997 altogether, wherein just comprise the multiple VOCs such as benzene homologues (benzene, toluene and dimethylbenzene).The control of current China atmosphere pollution and improvement focus mostly in the technical research and commercial introduction of the flue gas ash removal, desulphurization and denitration etc. of the large-scale stationary source such as power plant and boiler, volatile organic waste gas by contrast, the discharge as benzene homologues organic exhaust gas does not cause enough attention.Therefore exploiting economy, efficiently VOCs treatment technology, by the air quality improving China, the control and the improvement that realize atmosphere pollution have important environment, economy and social effect.
In gas, the method for organic pollution purified treatment mainly contains two classes: a class is absorption method, and another kind of is destruction method.Absorption method mainly contains charcoal absorption, pressure-variable adsorption, condensation method and membrane separation technique, and absorption method is separated VOCs by methods such as physical method pressure, temperature, selective absorbent and permoselective membranes.Destruction method has high-temperature combustion method, catalysis low-temperature combustion method, catalytic oxidation, biological oxidation and integrated technology.Volatile organic matter mainly by chemistry or biochemical reaction, is transformed into carbon dioxide and water with catalyst, heat or microorganism by destruction method.In these pollution control technologies, that studies more and extensive employing has heat damage method, absorption method, absorption process, condensation method etc., and the new control technology formed in recent years has biomembrance process, ozone decomposed method, corona method, plasma decomposition etc.
The heat that catalysis low-temperature combustion method produces is difficult to maintain self-heating, and still need just can reach temperature required to gas-heated, energy consumption is higher.Absorption method has that removal efficiency is high, purification thoroughly, the advantage promoted of low, the technical maturity of energy consumption and being easy to, there is good environment and economy benefit, shortcoming is that treatment facility is huge and flow process complicated, when having micelle material or other impurity in waste gas, adsorbent is easy to lose efficacy, and have to pass through reprocessing during material regeneration and easily cause secondary pollution, thus add the cost of process.Absorption process utilizes gaseous contaminant to have good dissolubility in some liquid solvent, using liquid as absorbent, make harmful components in waste gas by liquid absorption, thus reach the object of separating contaminants Purge gas, but still there are the volatilization of lyosoption and the regeneration issues of absorbent.Biological degradation method cost is lower, but the biodegradable of a lot of organic pollution is not high, limits the utilization of bioanalysis.Photocatalytic oxidation obtains to be studied widely, but this method is also also existing more shortcoming in the purification of VOCs, such as, the organic intermediate products such as ketone, aldehyde, acid can be produced in photocatalysis oxidation reaction process, secondary pollution may be caused, in addition, photocatalytic oxidation can only process for the VOCs that concentration is lower, and catalyst also exists easy inactivation, is difficult to shortcomings such as fixing.The feature of plasma technique is that operation process is simple, and plant maintenance used is more convenient, and workflow is short and operability good, but this method exists some drawbacks: energy consumption is higher, and capacity usage ratio needs further to be improved; The accessory substance of electric discharge may cause secondary pollution, such as, can produce NO
x, CO, O
3deng gas.
Three, summary of the invention
The present invention aims to provide a kind of purification of volatile organic pollutant method, and technical problem to be solved is the suitable catalysis material of design and technique can remove in gas volatile organic contaminant by the mode of catalysis hydrogen peroxide chemical oxidation.
Technical solution problem of the present invention adopts following technical scheme:
Shell of reactor (1), air inlet (2), perforation air distribution plate (3), ferriferous oxide filter material layer (4), gas outlet (5), hydrogen peroxide storage pond (6), hydrogen peroxide charge door (7).
In Purge gas, the method for organic pollution is:
Gas enters from injection port (2), and the hydrogen peroxide stored up in pond (6) with hydrogen peroxide contacts;
By regulating hydrogen peroxide concentration, intake velocity, air inlet and the hydrogen peroxide solution way of contact in storage pool to regulate and control the evaporation rate of hydrogen peroxide, make the 100-110% of the amount of hydrogen peroxide in gas hydrogen peroxide theoretical amount needed for oxidation organic pollution;
The hydrogen peroxide of volatilization and gas and vapor permeation evenly together with by bore a hole air distribution plate (3), gas through the fixing filtering layer that nanometer mineral material particles is housed, by the heterogeneous Fenton's reaction oxidize volatile organic pollution of nanometer mineral material.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, inventor make use of hydrogen peroxide this feature of certain volatility, reactor lower part arranges hydrogen peroxide storage pool, charge air flow contacts with hydrogen peroxide, part volatilization hydrogen peroxide and gas and vapor permeation, regulate and control the evaporation rate of hydrogen peroxide by hydrogen peroxide concentration, intake velocity, air inlet and the hydrogen peroxide solution way of contact in storage pool, the oxidation for organic pollution provides the oxidant of applicable ratio.Hydrogen peroxide and air inlet are closed evenly completely very much, are conducive to improving reaction rate.
2, organic pollution method in Purge gas of the present invention, key uses nanometer mineral material as catalyst hydrogen peroxide oxidation purifying contaminated thing.Nanometer mineral material used has nanocrystalline and nano-pore, belongs to nano structural material, has larger specific area and reactivity, shows very excellent catalytic activity, improves gas-solid phase Fenton oxidation effect; Nanometer mineral material preparation method used is simple, and raw material is the mineral resources of rich reserves, and as limonite ore, pyrite Ore, wide material sources, preparation cost is low.
3, the nanometer mineral material used is particle diameter 0.5-5mm particle, and filling becomes fixing filtering layer, and filtering layer porosity is large, and air resistance is little.
4, low-concentration hcl or sulfuric acid or the nitric acid nanometer mineral material filtrate to filling is used to process, make nanometer mineral material surface presentation acid, improve the efficiency of catalysis hydrogen peroxide oxidation organic pollution, because be more conducive to the reaction of hydrogen peroxide oxidation organic pollution under acid condition.
Four, accompanying drawing explanation
The structure of reactor schematic diagram of Fig. 1 nanometer mineral material purifying volatile gaseous contaminant: 1-shell; 2-air inlet; 3-bores a hole air distribution plate; 4-nanometer mineral material packing layer; 5-gas outlet; 6-hydrogen peroxide storage pond; Mouth added by 7-hydrogen peroxide.
The X ray diffracting spectrum of Fig. 2 Nanoscale Iron mineral material, shows the Nomenclature Composition and Structure of Complexes feature of nano mineral materials used.
Several Nanoscale Iron mineral material of Fig. 3 catalysis hydrogen peroxide oxidation methane efficiency (in gas, methane volumetric mark is 5%)
(in gas, toluene concentration is 2.43g/Nm to several Nanoscale Iron mineral material of Fig. 4 catalysis hydrogen peroxide oxidation toluene efficiency
3)
Five, detailed description of the invention
Embodiment 1:
It is 0.5 ~ 1mm particle (Fig. 2) that limonite ore is broken, screening obtains particle diameter.
Particle 2% hydrogen nitrate dipping of preparation, drain, be packed into reactor top.
In Purge gas, the device of organic pollution as shown in Figure 1,1-shell; 2-air inlet; 3-bores a hole air distribution plate; 4-nanometer mineral material filtering layer; 5-gas outlet; 6-hydrogen peroxide storage pond; 7-hydrogen peroxide charge door.
With air pump, air is passed through the formalin of 0.1%, use mass flowmenter adjusting gas flow, obtain containing formaldehyde 334mg/m
3analog gas.
Analog gas containing formaldehyde is entered from air inlet (2), and the hydrogen peroxide stored up in pond (6) with hydrogen peroxide contacts, and in storage pond, hydrogen peroxide concentration is set as that 15% tests; Volatilization hydrogen peroxide and gas and vapor permeation evenly together with by bore a hole air distribution plate (3) again pass nanometer mineral material filtering layer, the organic contamination dirt in catalysis hydrogen peroxide oxidation gas.
The gas distilled water of discharging from purifier gas outlet (5) absorbs, and by the amount of formaldehyde in acetylacetone,2,4-pentanedione spectrophotometry solution, calculate according to concentration of formaldehyde in gas flow and solution middle concentration of formaldehyde of giving vent to anger, formaldehyde clearance is greater than 90%.
Embodiment 2:
It is 1.0 ~ 5mm particle that broken for limonite ore, screening are obtained particle diameter, and sampling 50g puts into Muffle furnace and within 1 hour, obtains by receiving the nanometer mineral material (Fig. 2) of nano-pore that brilliant bloodstone forms, high-specific surface area 300 DEG C of calcinings.
Nanometer mineral material particles 5% hydrogen nitrate dipping of preparation, drain, be packed into reactor top.
With air pump, air is passed through the formalin of 0.1%, use mass flowmenter adjusting gas flow, obtain containing formaldehyde 334mg/m
3analog gas.
Analog gas containing formaldehyde is entered from air inlet (2), and the hydrogen peroxide stored up in pond (6) with hydrogen peroxide contacts, and in storage pond, hydrogen peroxide concentration is set as that 30% tests; Volatilization hydrogen peroxide and gas and vapor permeation evenly together with by bore a hole air distribution plate (3) again pass nanometer mineral material filtering layer, the organic contamination dirt in catalysis hydrogen peroxide oxidation gas.
The gas distilled water of discharging from purifier gas outlet (5) absorbs, and by the amount of formaldehyde in acetylacetone,2,4-pentanedione spectrophotometry solution, calculate according to concentration of formaldehyde in gas flow and solution middle concentration of formaldehyde of giving vent to anger, formaldehyde clearance is greater than 95%.
Embodiment 3:
It is 0.5 ~ 1mm particle that broken for limonite ore, screening are obtained particle diameter, and sampling 50g puts into tube furnace, passes into hydrogen 300 DEG C calcining 2 hours, obtains by receiving the nanometer mineral material of nano-pore that brilliant magnetic iron ore and Nanoscale Iron form, high-specific surface area.
The nanometer mineral material particles of preparation is flooded with 5% sulfuric acid, drains, be packed into reactor top;
With air pump, air is passed through the formalin of 0.1%, use mass flowmenter adjusting gas flow, obtain the analog gas containing formaldehyde.
Enter from air inlet (2) containing the analog gas of formaldehyde, hydrogen peroxide store up in pond (6) with hydrogen peroxide contacts, store up hydrogen peroxide concentration in pond be set as 5 respectively, 10,15% different concentration tests; Volatilization hydrogen peroxide and gas and vapor permeation evenly together with by bore a hole air distribution plate (3) again pass nanometer mineral material filtering layer, the organic contamination dirt in catalysis hydrogen peroxide oxidation gas.
The gas distilled water of discharging from purifier gas outlet (5) absorbs, and by the amount of formaldehyde in acetylacetone,2,4-pentanedione spectrophotometry solution, calculate according to concentration of formaldehyde in gas flow and solution middle concentration of formaldehyde of giving vent to anger, formaldehyde clearance is greater than 95%.
Embodiment 4:
It is 0.5 ~ 1mm particle that broken for pyrite ore, screening are obtained particle diameter, and sampling 50g puts into tube furnace, passes into nitrogen, 550 DEG C of calcinings 1 hour, obtains by receiving the nanometer mineral material (Fig. 2) of nano-pore that brilliant magnetic iron ore forms, high-specific surface area.
The nanometer mineral material particles of preparation is flooded with 0.5% sulfuric acid, drains, be packed into reactor top;
With air pump, air is passed through the formalin of 0.1%, use mass flowmenter adjusting gas flow, obtain the analog gas containing formaldehyde.
Enter from air inlet (2) containing the analog gas of formaldehyde, hydrogen peroxide store up in pond (6) with hydrogen peroxide contacts, store up hydrogen peroxide concentration in pond be set as 5 respectively, 10,15% different concentration tests; Volatilization hydrogen peroxide and gas and vapor permeation evenly together with by bore a hole air distribution plate (3) again pass nanometer mineral material filtering layer, the organic contamination dirt in catalysis hydrogen peroxide oxidation gas.
The gas distilled water of discharging from purifier gas outlet (5) absorbs, and by the amount of formaldehyde in acetylacetone,2,4-pentanedione spectrophotometry solution, calculate according to concentration of formaldehyde in gas flow and solution middle concentration of formaldehyde of giving vent to anger, formaldehyde clearance is greater than 95%.
Embodiment 5:
It is 0.5 ~ 1mm particle that broken for pyrite ore, screening are obtained particle diameter, and sampling 50g puts into tube furnace, passes into nitrogen, 550 DEG C of calcinings 1 hour, obtains by receiving the nanometer mineral material (Fig. 2) of nano-pore that brilliant magnetic iron ore forms, high-specific surface area.
The nanometer mineral material particles of preparation is flooded with 0.5% sulfuric acid, drains, be packed into reactor top;
Pure methane Standard Gases, air are controlled to be configured as the mist that volume fraction is 1%, 2%, 3%, 4%, 5% respectively by mass flowmenter, analog gas containing methane is entered from injection port (2), the hydrogen peroxide stored up in pond (6) with hydrogen peroxide contacts, in Chu Chi, hydrogen peroxide concentration is 5%, volatilization hydrogen peroxide and gas and vapor permeation evenly together with by bore a hole air distribution plate (3) again pass nanometer mineral material filtering layer, the methane in catalysis hydrogen peroxide oxidation gas.
From the gas chromatographic that purifier outlet (5) is discharged, when methane volumetric mark is less than 5%, methane clearance is greater than 95%(Fig. 3).
Embodiment 6:
It is 0.5 ~ 1mm particle that broken for pyrite ore, screening are obtained particle diameter, and sampling 50g puts into tube furnace, passes into nitrogen, 550 DEG C of calcinings 1 hour, obtains by receiving the nanometer mineral material of nano-pore that brilliant magnetic iron ore forms, high-specific surface area.
The nanometer mineral material particles of preparation is flooded with 0.1% sulfuric acid, drains, be packed into reactor top.With air pump, the air of 10mL/min is obtained the gas containing high concentration toluene by neat liquid toluene, this gas is controlled to mix in hybrid bottle with another road air by mass flowmenter, obtains 10mg/m
3, 100mg/m
3, 500mg/m
3, 1000mg/m
3, 5000mg/m
3the analog gas of different concentration of formaldehyde, analog gas containing toluene is entered reactor from injection port (2), the hydrogen peroxide stored up in pond (6) with hydrogen peroxide contacts, in Chu Chi, hydrogen peroxide concentration is 5%, volatilization hydrogen peroxide and gas and vapor permeation evenly together with by bore a hole air distribution plate (3) again pass nanometer mineral material filtering layer, by Fenton's reaction catalysis hydrogen peroxide oxidation toluene.
Resolve with carbon disulfide after the gas charcoal absorption that purifier outlet (7) is discharged, then use gas chromatographic analysis, toluene concentration and removal efficiency after computing, toluene removal rate 95%(Fig. 4).
Claims (2)
1. the method for organic pollution in nanometer mineral material Purge gas, is characterized in that: to have the ferriferous oxide of nano-pore structure or iron sulfide granular materials for catalyst, the organic pollution in catalysis hydrogen peroxide oxidation waste gas; Purifier comprises shell of reactor (1), air inlet (2), perforation air distribution plate (3), nanometer mineral material filter material layer (4), gas outlet (5), hydrogen peroxide storage pond (6), hydrogen peroxide charge door (7);
In its Purge gas, the method for organic pollution is:
(1) prepare nanometer mineral material, natural limonite ore is broken, screening, obtains the particle of 0.5-5mm, changes nanometer bloodstone into as catalysis material at 250-500 DEG C of calcining 1h;
Or using obtain 0.5-5mm limonite particle under reducing atmosphere 300-700 DEG C of calcining change nano magnetite into as catalysis material;
Or pyrite Ore is broken, screening obtains the particle of 0.5-5mm, 550-800 DEG C of calcining 1h changes nano magnetic pyrite into;
(2) above-mentioned graininess nanometer mineral material filling is become fixing filtering layer;
(3) with the hydrochloric acid of mass concentration 0.1-5% or sulfuric acid or nitric acid or phosphoric acid, make nanometer mineral material surface presentation acid;
(4) need the gas of purification to enter from air inlet (2), hydrogen peroxide store up in pond (6) with hydrogen peroxide contacts, the hydrogen peroxide of volatilization and gas and vapor permeation evenly together with pass through to bore a hole air distribution plate (3);
(5) mist is again through the fixing filtering layer that nanometer iron mineral material granule is housed, thickness of filter bed 5-50cm, nanometer mineral filtrate heterogeneous catalysis hydrogen peroxide oxidation volatile organic contaminant.
2. the method for organic pollution in nanometer mineral material Purge gas according to claim 1, by regulating hydrogen peroxide concentration, intake velocity, air inlet and the hydrogen peroxide solution way of contact in hydrogen peroxide storage pond to regulate and control the evaporation rate of hydrogen peroxide, make the 100-110% of the amount of hydrogen peroxide in gas hydrogen peroxide theoretical amount needed for oxidation organic pollution.
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