CN101628202B - Nanoparticle surface modified active semi-coke compound desulfurization denitrification agent and preparation method thereof - Google Patents
Nanoparticle surface modified active semi-coke compound desulfurization denitrification agent and preparation method thereof Download PDFInfo
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Abstract
The invention provides a nanoparticle surface modified active semi-coke compound desulfurization denitrification agent, which is compounded by active semi-coke and nanoparticle. The invention improves desulfurization efficiency by the high specific surface area, the catalysis characteristic and the oxidizzation characteristic of nano materials, and can catalytically oxidize nitric oxide in smoke, thereby achieving the aim of denitrification.
Description
Technical field
The invention belongs to technical field of coal chemical industry, specifically, relate to a kind of nanoparticle surface modified active semi-coke compound desulfurization denitrification agent and preparation technology thereof.
Background technology
The sulphur pollution of fire coal has been developed the method for many improvement both at home and abroad, dividing according to technology has dry method, semidry method and wet method three classes.
The wet desulphurization agent is to control SO at present in the world
2The main sulfur method that pollute, control acid rain endangers mainly comprises: lime/gypsum method, ammoniacal liquor method, sodium sulfite round-robin method, magnesia-magnefite process, seawater method etc.Wet desulphurization technology possess skills maturation, desulfuration efficiency advantages of higher, still, the processing of the waste water after the desulfurization exists problems such as huge as equipment, that energy consumption is high, cost is big.The at present main wet desulphurization technology that adopts of China wherein mainly adopts the lime/gypsum method, though desulfuration efficiency height, technology maturation exists a large amount of problems: at first be need discharge a large amount of CO when preparation CaO
2, the product of its desulfurizing agent is a gypsum, because quality is loose, so desulfurated plaster do not have the economic worth of recovery and causes discarding, and the discarded desulfurated plaster of stacking storage occupies a large amount of soils, discharges noxious material easily simultaneously, causes secondary pollution; China is a lack of sulfur big country at present besides, and the sulphur in the flue gas then is wasted along with generating gypsum.Though other wet desulphurization technology also exist lot of advantages, influenced by economy, region etc., do not widely apply.
Semidry method is the fume desulphurization method that removes sulfur dioxide in flue gas in the gas, liquid, solid three-phase, and desulfurization product is the dry powder shape.Semidry method mainly contains in-furnace calcium spraying and adds afterbody humidification method, rotary spraying technique, recirculating fluidized bed and flue gas suspension method etc.These methods all have the pluses and minuses of oneself separately, or desulfuration efficiency is lower or operating cost than problems such as height, it uses restriction to some extent.
Desulfurization by dry method is to utilize solid absorbent to remove the fume desulphurization method of sulfur dioxide in flue gas by gas-solid absorption absorption.Compare with wet desulfurizing process, dry desulfurizing process has that system is simple, investment cost is low, floor space is little, the temperature height of flue gas after desulfurization, the advantages such as discharging that help flue gas, although desulfurization by dry method also exists shortcoming, for example the utilization rate of desulfuration efficiency and absorbent is lower, but by a series of improvement research, desulfurization by dry method can satisfy present environmental requirement.Dry method mainly contains cupric oxide/alumina method, iron oxide composite metal oxide method, fuse salt absorption process, absorbent charcoal based material catalysis absorption method etc.Owing to have low Sulfur capacity, operating cost more high shortcoming, use up till now by the heavy industrialization of still being unrealized for preceding several method.
Advantages such as charcoal base desulfur technology has that technological process is short, sorbent consumption is few, small investment, desulfuration byproduct comprehensive utilization are simple relatively.Therefore, charcoal base desulfur technology has attracted various countries to pay close attention to widely.Desulfurizing agent is the core and key of charcoal base desulfur technology, and it has determined the desulfuration efficiency and the desulfurization process of desulfurizing agent.Therefore, the research of carbon base desulfurizer becomes the research emphasis and the difficult point of charcoal base desulfur technology.
At present, the carbon base desulfurizer of having tested and having used comprises: active carbon, NACF, carbon molecular sieve, activated coke (semicoke), expanded graphite etc.In general, the common feature of the commercial active carbon of using is the needed surface oxygen functional group deficiency of oxidation, thereby causes desulfuration efficiency low.Therefore, must carry out activation processing to change the chemical characteristic on surface to the surface of active carbon.On this basis, the desulfurizing agent that works out has the iodine of containing active carbon, nitrogenous active carbon, activated carbon fiber etc.Yet these desulfurizing agents have pluses and minuses separately, as short and operating cost height (containing iodine or nitrogen active carbon) in service life, and price expensive (activated carbon fiber), perhaps desulfuration efficiency is low etc.Therefore, the high carbon base desulfurizer of development cost performance is crucial.
Existing studies show that, under the bigger situation of carbon base desulfurizer specific area, the catalytic oxidation that is adsorbed on the sulfur dioxide of charcoal material surface is often being controlled the efficient of desulfurization, and therefore, the catalytic oxidation characteristic that how to improve the carbon base desulfurizer surface is to improve the key factor of desulfuration efficiency.
Summary of the invention
Shortcoming at above mentioned carbon base desulfurizer, develop a kind of nanoparticle surface modified active semi-coke compound desulfurization denitrification agent, it utilizes the high-specific surface area of nano material and catalysis thereof, oxidation characteristic to improve desulfuration efficiency, nitric oxide in simultaneously can the catalytic oxidation flue gas, thus play the purpose of denitration.
Another object of the present invention is to provide a kind of preparation method of nanoparticle surface modified active semi-coke compound desulfurization denitrification agent.
A kind of nanoparticle surface modified active semi-coke compound desulfurization denitrification agent of the present invention adopts nano particle and active carbocoal to be composited, and described nano particle is CeO
2, MnO
2Or Fe
2O
3In one or more.
Its existing way of nano particle is that (nano wire is a kind of nanoscale (10 for the nano particle of semicoke finishing or nano wire
-9Rice) line), its addition is the 0.01-5% of gross weight, preferably 0.01-3%.
Semicoke is the product of coal through low temperature distillation (final temperature is about 700 ℃), and this process is also referred to as the carbonization process of coal.Active carbocoal or semicoke catalyst are the products that obtains through activation processing again on the basis of charing.At present directly begin to carry out from feed coal, also have and further process from existing semicoke or active carbocoal for the active carbocoal Preparation of catalysts is existing.Compound desulfurization denitrification agent of the presently claimed invention directly utilizes industrial active carbocoal, forms by nano-sized surface modification and activation.
In general, the industry active carbocoal often utilizes the general industry semicoke to carry out the steam activation processing and forms, promptly starvation in autoclave at 400-800 ℃ of steam that feeds pressure 10-40atm (physical atmosphere), promotes the improvement of carbon based material micropore and surface property.
The present invention directly adopts the industrial active carbocoal of method for preparing, selects the particle that diameter is 5～15mm.Nano particle is incorporated into the active carbocoal surface improving its catalysis, oxidation susceptibility mutually as modifying, thereby efficiently removes sulfur in smoke and nitric oxide.
The preparation method of a kind of nanoparticle surface modified active semi-coke compound desulfurization denitrification agent of the present invention adopts the hydro-thermal method of present comparative maturity or sol-gel process preparation to comprise CeO
2, Fe
2O
3Or MnO
2Precursor liquid Deng nano particle; Pass through dipping or hydro-thermal technology again at active carbocoal surface recombination nano particle (or nano wire), thereby prepare the compound desulfurization denitrification agent that nano surface is modified.
The preparation method of nanoparticle surface modified active semi-coke compound desulfurization denitrification agent of the present invention can adopt the compound or hydrothermal growth process of dipping.
Described dipping composite algorithm, comprise the steps: active carbocoal under inert atmosphere conditions, purify 10-30min in the 100-300 ℃ of temperature range, immerse 30-360min in the precursor liquid that contains Nano sol then, leach back dry 60-180min under 100-200 ℃, impregnation process is to the content of required composite nanoparticle, then at 300-600 ℃ of sintering temperature 60-180min repeatedly.
Described hydrothermal growth process, comprise the steps: in water heating kettle, the active carbocoal immersion is contained in the precursor liquid of Nano sol, active carbocoal and Nano sol precursor liquid volume ratio are between 1: 1～1: 3, under 60-300 ℃, reaction growth 60-360min leaches after the hydro-thermal reaction and modifies complete semicoke, dry 60-180min under 100-200 ℃ is then at 300-600 ℃ of sintering temperature 60-180min.
Adopt the preparation of hydro-thermal method or sol-gel process to comprise CeO
2, Fe
2O
3Or MnO
2Deng the precursor liquid of nano particle, described precursor liquid is to contain the CeO that concentration is 0.4-0.6mol/L
2, Fe
2O
3Or MnO
2Deng Nano sol.
The present invention adopts the compound of active carbocoal and nano particle, and nano particle plays the effect of catalysis, oxidation to sulfur dioxide and nitric oxide.Described nano particle is grown up at active carbocoal surface forming core with forms such as nano particle or nano wires, and realization nano particle and active carbocoal are combined closely.Active carbocoal of the present invention is through overactivation, thereby has the suitable surface texture and the active carbocoal of pore structure.
Adopt active carbocoal desulfurization denitrification agent of the present invention to carry out desulfurization and handle advantage such as have that technological process is short, sorbent consumption is few, small investment, desulfuration byproduct comprehensive utilization are simple relatively; Nano particle (nano particle, nano wire etc.) has high-specific surface area and reaches sulfur dioxide, nitric oxide catalysed oxidn.Nano particle/active semi-coke compound desulfurization denitrification agent not only can remove sulfur in smoke, also can remove simultaneously the nitric oxide in the flue gas, thereby realization desulfurization and denitrification integral, and can realize the catalyzed conversion of nitrogen oxide and carbon monoxide etc. to a certain extent, therefore have good market prospects.
Description of drawings
Fig. 1 is the process chart of the nano-sized surface modification active carbocoal desulfurization denitrification agent of dipping composite algorithm preparation of the present invention;
Fig. 2 is the process chart of the nano-sized surface modification active semi-coke compound desulfurization denitrification agent of hydrothermal growth process preparation of the present invention;
Fig. 3-1, Fig. 3-2 is the embodiment of the invention 1 described CeO
2The shape appearance figure of the active semi-coke compound desulfurization denitrification agent that nano grain surface is modified;
Fig. 4 is the embodiment of the invention 2 described Fe
2O
3And MnO
2The shape appearance figure of composite nanoparticle surface modified active semi-coke compound desulfurization denitrification agent;
Fig. 5 is desulfurization performance experiment process figure of the present invention;
Fig. 6 is the conversion ratio of a flue gas desulfurization of nanoparticle surface modified active semi-coke compound desulfurization denitrification agent of the present invention, wherein: the a-active carbocoal; B-finishing CeO
2C-finishing CeO
2Nano wire and particle are compound; D-finishing Fe
2O
3And MnO
2Composite nanoparticle; E-finishing Fe
2O
3Nano particle and nano wire.
The specific embodiment
Following examples are used to illustrate the present invention, but are not used for limiting the scope of the invention.
Embodiment 1 dipping composite algorithm prepares CeO
2Nano-particle modified active semi-coke compound desulfurization denitrification agent.
Adopt technical process shown in Figure 1, use the dipping composite algorithm at active carbocoal surface recombination CeO
2Nano particle.
The active carbocoal that adopts the steam activation method to produce is desulfurizing agent carbon based material (available from a Yanzhou Mining Group), selects the active carbocoal particle of diameter 5-15mm, and under argon gas atmosphere, 150 ℃ of dry 60min are to remove ash content.
Use sol-gel process to prepare the CeO of concentration simultaneously as 0.4mol/L
2The Nano sol precursor liquid, wherein dispersant is a polyethylene glycol, pH is controlled between the 4-5.
Active carbocoal after the purified treatment is immersed CeO
2360min. in the Nano sol precursor liquid.Through after the leaching, in drying box through 150 ℃ of dry 120min.Weigh, if can not reach the weight of required composite nanoparticle, can the repeated impregnations process several times to reaching requirement.With final compound good active carbocoal at 600 ℃ of sintering temperature 120min..After measured, the addition of nano particle is 1% of a gross weight.
If it is compound to use this method to carry out other nano particles, equally according to flow process shown in Figure 1, the precursor liquid of using required composite nanoparticle instead gets final product, and its addition can be adjusted between the 0.01-5% of gross weight.
Nano particle to gained compound desulfurization denitrification agent surface combines with substrate, uses ESEM (SEM), and transmission electron microscope (TEM) carries out the sign of pattern.
Fig. 3-1, Fig. 3-2 is the CeO of active carbocoal finishing
2Nano particle SEM pattern, the result shows that we have obtained CeO
2Nanoparticle surface modified compound desulfurization denitrification agent.
Then, the performance of the nanoparticle surface modified compound desulfurization denitrification agent that obtains is tested, estimated, specific embodiments is as follows:
Performance to the resulting compound desulfurization denitrification agent of the present invention is tested, and flow process as shown in Figure 5.The experimental provision of power plant's generating fume emission is simulated in assembling voluntarily, to carry out the test of desulfurization performance.The experimental system of simulation is made up of three parts: air distribution system, add thermally desulfurizing partly and the flue gas analysis part of detecting.
This experiment obtains the mist of different proportioning sulfur dioxide by the flow of flowmeter adjusting pure nitrogen, oxygen, carbon dioxide and sulfur dioxide gas.Mix nitrogen, carbon dioxide and oxygen in the experimentation earlier, carry a certain amount of water vapour by water bath with thermostatic control again and come the simulated flue gas water vapour, mix the flue gas that obtains simulating afterwards with sulfur dioxide.Utilize the flue gas analysis system that the sulfur dioxide in the gas before and after the desulfurization is tested respectively, to obtain all kinds of parameter indexs of desulfurization.
Compound desulfurization denitrification agent is removed SO
2Performance evaluation adopt the dynamic adsorption experiment of flue gas, promptly the desulfurizing agent of certain content is placed in the stainless steel tube, place stainless steel tube one tube furnace reactor to react again.SO in the flue gas
2By NH
4SO
3NH
2(NH
4)
2SO
4Mixed solution absorbs to be analyzed with iodometric titrationiodimetry titration again.Adopt SO
2Conversion ratio characterize the desulfurization performance index of desulfurization denitrification agent, and the sulfur dioxide removal rate is mapped over time, shown in the b line among Fig. 6.
The regenerative response of compound desulfurization denitrification agent of the present invention adopts water seaoning.After desulphurization reaction finishes,, emit its pH value of water gaging, repeat to be upgraded to about 7 up to the pH value several times, water is drained only regeneration ending the desulfurization denitrification agent 20-60min that is soaked in water.Then the desulfurization denitrification agent after the regeneration is repeated its desulfurization performance of above-mentioned experimental measurement.
Embodiment 2 hydrothermal growth process prepare Fe
2O
3And MnO
2The active semi-coke compound desulfurization denitrification agent of composite nanoparticle finishing.
According to technical process shown in Figure 2, use hydrothermal growth process at active carbocoal finishing Fe
2O
3And MnO
2Composite nanoparticle.
Choosing diameter is the active carbocoal particle of the steam activation method production of 5-15mm, is 1: 3 ratio then with active carbocoal and Nano sol precursor liquid volume ratio, active carbocoal is immersed fill MnSO
4, KMnO
4And FeCl
3In the water heating kettle of mixed solution, three's concentration is respectively: 0.006mol/L, 0.004mol/L, 0.005mol/L, and use polyethylene glycol as dispersant.Regulator solution pH8,140 ℃ of control growth temperatures, insulation 360min.Leach behind the growth ending, it is clean to spend deionised water, and dry 120min. under 150 ℃ temperature gets final product at 600 ℃ of sintering temperature 120min. again.After measured, the addition of nano particle is 0.5% of a gross weight.
If it is compound to use this method to carry out other nano particles, equally according to flow process shown in Figure 2, the precursor liquid of using required composite nanoparticle instead gets final product, and its addition can be adjusted between the 0.01-5% of gross weight or between 0.01-3%.
Nano particle to gained compound desulfurization denitrification agent surface combines with substrate, uses ESEM (SEM), and transmission electron microscope (TEM) characterizes, and obtains SEM result as shown in Figure 4, shows that we have obtained Fe
2O
3And MnO
2The active semi-coke compound desulfurization denitrification agent of composite nanoparticle finishing.
The performance that obtains compound desulfurization denitrification agent is carried out test and evaluation, and technological process and implementation method are all identical with embodiment 1, and the test result drawing is analyzed, as the d line among Fig. 6.
The test example
With the desulfurized effect drafting pattern 6 of several nanoparticle surface modified compound desulfurization denitrification agents of gained of the present invention, wherein, the a-active carbocoal; B-finishing CeO
2(embodiment 1); C-finishing CeO
2Nano wire and particle are compound; D-finishing Fe
2O
3And MnO
2Composite nanoparticle (embodiment 2); E-finishing Fe
2O
3Nano particle and nano wire.C, e adopt hydrothermal growth process among the embodiment 2 among the figure, and different nano particles are compound to the active carbocoal surface.Through the calculating of weighing, the content of control institute composite nanoparticle is 0.9～1%.
As can be seen, the flue gas desulfurization effect of nanoparticle surface modified active semi-coke compound desulfurization denitrification agent will be better than the desulfurization conversion ratio before modifying far away, has the practical application meaning.Simultaneously, also can find out finishing Fe
2O
3And MnO
2Composite nanoparticle is than independent decorated nanometer CeO
2Particle has better catalytic effect.
Though above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (5)
1. a nanoparticle surface modified active semi-coke compound desulfurization denitrification agent is characterized in that, it adopts nano particle and active carbocoal to be composited, and described nano particle is CeO
2, MnO
2Or Fe
2O
3In one or more.
2. compound desulfurization denitrification agent according to claim 1 is characterized in that, described nano particle addition is the 0.01-5% of gross weight.
3. compound desulfurization denitrification agent according to claim 1 and 2 is characterized in that, described nano particle addition is the 0.01-3% of gross weight.
4. the method for preparing any described compound desulfurization denitrification agent of claim 1-3, it is characterized in that, with active carbocoal under inert atmosphere conditions, purify 10-30min down in 100-300 ℃, immerse 30-360min in the precursor liquid that contains Nano sol then, leach back dry 60-180min under 100-200 ℃, impregnation process is to the content of required nano particle, at last at 300-600 ℃ of sintering temperature 60-180min repeatedly; Described precursor liquid is to contain the CeO that concentration is 0.4-0.6mol/L
2, Fe
2O
3Or MnO
2Nano sol.
5. the method for preparing any described compound desulfurization denitrification agent of claim 1-3, it is characterized in that, in water heating kettle, the active carbocoal immersion is contained in the precursor liquid of Nano sol, under 60-300 ℃, reaction growth 60-360min leaches then and modifies complete semicoke, dry 60-180min under 100-200 ℃ is then at 300-600 ℃ of sintering temperature 60-180min; Described precursor liquid is to contain the CeO that concentration is 0.4-0.6mol/L
2, Fe
2O
3Or MnO
2Nano sol.
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| CN102974359A (en) * | 2012-11-16 | 2013-03-20 | 北京石油化工学院 | Simultaneous desulfurization and denitration catalyst and preparation method thereof |
| CN103691410B (en) * | 2014-01-09 | 2015-09-30 | 中国矿业大学(北京) | rare earth modified semicoke coal powder material and preparation method thereof |
| CN103990374A (en) * | 2014-05-12 | 2014-08-20 | 孙立刚 | Novel desulfurization, denitrification, decarburization and dust removal purification combined device for coal-fired flue gas |
| CN104014347B (en) * | 2014-06-10 | 2015-02-11 | 太原理工大学 | Preparation method of catalyst for lightening of biomass tar heavy component |
| CN106238033A (en) * | 2016-07-29 | 2016-12-21 | 北京大学 | Active carbocoal low-temperature denitration agent of Cerium Oxide Nanotubes and preparation method and application is modified on surface |
| CN106669364B (en) * | 2016-12-14 | 2017-12-15 | 苏州佑君环境科技有限公司 | A kind of desulfurization denitrification agent and its preparation method and application |
| CN107442069B (en) * | 2017-09-08 | 2020-05-22 | 西安建筑科技大学 | Preparation method of sintered flue gas denitration carbonaceous adsorption material |
| CN113070072B (en) * | 2021-03-30 | 2023-10-27 | 西安建筑科技大学 | Catalyst for desulfurization and denitrification and preparation method thereof |
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