CN101804297B - Preparation, use and reproduction method of reproducible load type flue gas desulfurization agent - Google Patents
Preparation, use and reproduction method of reproducible load type flue gas desulfurization agent Download PDFInfo
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- CN101804297B CN101804297B CN2010101424582A CN201010142458A CN101804297B CN 101804297 B CN101804297 B CN 101804297B CN 2010101424582 A CN2010101424582 A CN 2010101424582A CN 201010142458 A CN201010142458 A CN 201010142458A CN 101804297 B CN101804297 B CN 101804297B
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Abstract
The invention discloses a preparation, use and reproduction method of a reproducible load type flue gas desulfurization agent, which comprises the following steps: adding activated carbon which accounts for 15 to 60 percent of the weight of attapulgite powder into the attapulgite powder with the grain diameter of 45mum; mixing the materials; adding water for stirring and forming; drying the materials for 3 to 5 hours at 105 DEG C; then, roasting the materials for 2 to 5 hours at 300 to 500 DEG C to obtain carriers; placing the carriers into 0.2 to 1.0mol/L Ce(NO3)3 solution for isometric impregnation for 2 to 6 hours; firstly, drying the materials at 60 DEG C for 3 hours; then, drying the materials at 105 DEG C for 5 hours; finally, roasting the materials for 3 hours in nitrogen gas atmosphere at 200 to 400 DEG C to obtain the desulfurization agents; loading the desulfurization agents into a reaction vessel; introducing normal pressure flue gas at 120 to 300 DEG C, wherein the airspeed is between 600 and 80000h<-1>, the desulfurization rate is between 85 and 92 percent, and the saturated sulfur capacity is between 3.2 and 6.7g/100g; and loading the inactivated desulfurization agents into the reaction vessel to carry out reproduction in the nitrogen gas atmosphere at the temperature between 250 and 350 DEG C. The desulfurization agent of the invention can solve the problems of low desulfurization rate, few circulation times, high investment, high operation cost and the like of the existing flue gas desulfurization agent, and is applicable to the conditions of discharge temperature and high airspeed of flue gas of industrial coal burning boilers.
Description
Technical field
The present invention relates to preparation and the use and the renovation process of fume desulfurizing agent, be specifically related to a kind of preparation and use and renovation process of reproducible load type flue gas desulfurization agent.
Background technology
China is production of energy big country, also is energy-consuming big country, and energy-consuming accounts for 10% of the whole world at present.In the energy resource structure system of China, coal accounts for 75% of whole energy resource structure system, much larger than oil, natural gas and waterpower.Whole nation SO
290% of discharge capacity is come spontaneous combustion coal.Therefore, reduce SO
2The key of discharge capacity is SO in the control coal-fired flue-gas
2Generation and discharging.Strategic height is mentioned in the work that present China will prevent and treat coal-fired sulfur dioxide pollution, and SO is administered in research and development
2The new method of polluting has also become the task of top priority.
Up to the present, the countries in the world researcher has proposed more than 100 kind of low concentration SO
2Fume desulphurization method, the exploitation degree does not wait from the laboratory scale to the industrialization degree, but the method for flue gas desulfurization is broadly divided into three major types usually: one type is wet method, promptly adopts liquid-absorbant such as washings such as water or aqueous slkali to remove sulfur dioxide; One type is semidry method, and it is the moisture that utilizes in the obvious heat of smoke evaporation lime slurry, lime and SO simultaneously
2Reaction generates the powdered calcium sulfite, and it has the characteristics of wet method and dry method concurrently; Another kind of is dry method, with powdery or granular absorbent, adsorbent or catalyst to remove SO
2Wet desulphurization technology comparative maturity, the commercial application of existing decades is historical, operating cost is high, water consumption is big, accessory substance that generate is prone to cause shortcomings such as secondary pollution but exist, and the potentiality that further develop are little; Dry method and semidry method technology have that investment is low, technology is simple, easy to maintenance, advantage such as the desulfuration efficiency scope is wide, reliable, adaptability is strong, get more and more people's extensive concerning, but semidry method fundamentally do not solve the reproducible utilization problem of resource; Dry desulfurization process majority belongs to gas-solid reaction, and speed is relatively low, and flue gas reaction time in reactor is long; But the flue gas after the desulfurization is not lowered the temperature, and does not need to heat again, and power consumption is few; Can satisfy the requirement of discharging diffusion, in addition, desulfurization by dry method has also that no fouling, dewfall, obstruction, reliability are high, secondary pollution advantage such as less; Therefore, the developmental research desulfurization by dry method becomes the developing direction of flue gas desulfurization technique, and this method also receives people's favor day by day.
Dry desulfurization is mostly by the SO in desulfurizing agent absorption or the absorption flue gas
2, the desulfurizing agent after saturated is regenerated, and reclaims SO during regeneration
2Further processing and utilization.The most economical configuration of coal burning flue gas desulfurization system should be after dedusting, and corresponding temperature 120-300 ℃, this configuration reduces the process energy consumption greatly.More CeO is reported in research in recent years
2/ γ-Al
2O
3, CuO/Al
2O
3Activated coke (charcoal) etc., ZL200510087043.9 discloses CeO like patent
2/ γ-Al
2O
3Desulfurizing agent and preparation method thereof, Zhengzhou University's journal (engineering version) 2005,26 (1): 108-112 has reported CuO/Al
2O
3Desulfurizing agent, but CeO
2/ γ-Al
2O
3And CuO/Al
2O
3Desulphurizing activated temperature requirement higher (>300 ℃); Carbon, Vol, 31, No1,1993,31 (1): 47-51 reports activated coke (charcoal), activated coke (charcoal) near normal temperature to SO
2Bigger absorption Sulfur capacity is arranged, but temperature rising Sulfur capacity descends sharply, its Sulfur capacity is quite low in the time of 200 ℃; Patent ZL99104245.X has reported a kind of method for preparing desulfurizing agent with raw material of wood-charcoal material such as active carbon, activated coke or NACFs as carrier loaded cupric oxide; Its reactivity temperature can be at 120-250 ℃; Desulfurization degree is more than 80%, but because raw material of wood-charcoal material intensity is low, abrasion are high; It is few to recycle number of times, and production cost is high; Attapulgite is a kind of silicate mineral that contains Shuifu County's magnalium, has unique layer chain molecule structure, and crystal is needle-like, fibrous, and specific area is big; Adsorptivity is strong, and has stronger viscosity, chemical industry progress, 2009; 28 (1): 159-162 has reported that producing attapulgite with Gansu is matrix, is aided with activated alumina, forming agent, through granulation back loading CuO, has made a kind of NEW TYPE OF COMPOSITE adsorption desulfurizing agent; Result of study shows, when attapulgite content (mass fraction) accounts for 60%, sintering temperature is 600-700 ℃, and transition metal maceration extract mass fraction is about 15%; And when the desulfurizing agent moisture content was 15%-30%, its Sulfur capacity maximum can reach 17%, and there are 2 deficiencies in this research; The one, the too high attapulgite that causes of sintering temperature caves in, and specific area reduces, and finally causes adsorbance to reduce; Lose the distinctive performance of attapulgite, and energy consumption is high, the 2nd, only remove SO in the laboratory
2Industrial applications research is not simulated in research.Up to the present do not appear in the newspapers as yet with attapulgite and the application study of active carbon composite load reactive metal oxides in flue gas desulfurization technique.
Summary of the invention
The objective of the invention is to: preparation and use and renovation process that a kind of reproducible load type flue gas desulfurization agent is provided; The desulfurizing agent that adopts this preparation method to make is used for flue gas desulfurization; Can solve that existing fume desulfurizing agent desulfurization degree is low, cycle-index is few, problems such as investment and operating cost height; Use under suitable industry coal-boiler flue gas exhaust gas temperature, the high-speed condition, have high desulfurization activity.
Technical solution of the present invention is made up of following steps:
(1) preparation of desulfurizing agent carrier; In particle diameter is the attapulgite powder of 45 μ m, add active carbon, the active carbon addition is the 15-60% of attapulgite weight, mixes the back and adds an amount of water and stir into pasty state; Put into the make-up machine moulding; Earlier in baking oven in 105 ℃ of dry 3-5 hours, again in nitrogen atmosphere in 300-500 ℃ of roasting 2-5 hour, process carrier;
(2) carrier is put into the Ce (NO that concentration is 0.2-1.0mol/L
3)
3In the solution, adopted incipient impregnation 2-5 hour, earlier 60 ℃ of dryings 3 hours, then 105 ℃ of dryings 5 hours, at last in nitrogen atmosphere in 200-400 ℃ of roasting 3 hours, desulfurizing agent.
The method for using of desulfurizing agent of the present invention is: desulfurizing agent is packed in fixed bed or the moving-burden bed reactor, and reaction temperature is controlled at 120-300 ℃, feeds the normal pressure flue gas, and air speed is 600-80000h
-1, saturated Sulfur capacity 3.2-6.7g/100g.
The renovation process of desulfurizing agent of the present invention is: with the desulfurizing agent of inactivation pack into fixed bed or moving-burden bed reactor, in ammonia atmosphere, regenerate for temperature 250-350 ℃.
The present invention compared with prior art has following advantage:
1, desulfurization degree is high, and desulfurization degree reaches 85-92%;
2, this desulfurizing agent can directly utilize the temperature of flue gas to carry out desulphurization reaction, and operating cost is low.
3, desulfurizing agent is easy to regeneration, can use repeatedly, and production cost is low, does not cause secondary pollution.
The specific embodiment
Below in conjunction with specific embodiment further explain technical solution of the present invention, it is the restriction to technical solution that these embodiment should not be construed as.
Embodiment 1:
, particle diameter adds active carbon in being the attapulgite powder of 45 μ m; The addition of active carbon is 15% of an attapulgite weight; Mix the back and add an amount of water and stir into pasty state, put into the make-up machine moulding, earlier in baking oven in 105 ℃ of dryings 3 hours; Again in nitrogen atmosphere in 300 ℃ of following roastings 2 hours, process carrier; The carrier of processing is put into the Ce (NO of 0.2mol/L
3)
3In the solution, adopted incipient impregnation 2 hours,, 105 ℃ of dryings 5 hours, in nitrogen atmosphere, made desulfurizing agent in 3 hours at last then in 200 ℃ of roastings earlier 60 ℃ of dryings 3 hours.
Above-mentioned desulfurizing agent 1 gram is packed in the fixed bed reactors, is warming up to 120 ℃ of ventilatory responses, simulated flue gas consist of SO
2520ppm, O
25%, H
2O 3%, N
2Surplus, gas flow 310ml/min, desulfurization time 30min, desulfurization degree are 85%, saturated Sulfur capacity 3.2g/100g.
With the desulfurizing agent of the above-mentioned inactivation fixed bed reactors of packing into, temperature rises to 250 ℃ and feeds ammonias, regenerates at ammonia atmosphere; Desulfurizing agent after the regeneration, reusable more than 50 times, the SO that restores
2And NH
3Generate ammonium salt.
Embodiment 2:
, particle diameter adds active carbon in being the attapulgite powder of 45 μ m; The addition of active carbon is 25% of an attapulgite weight; Mix the back and add an amount of water and stir into pasty state, put into the make-up machine moulding, earlier in baking oven in 105 ℃ of dryings 4 hours; Again in nitrogen atmosphere in 350 ℃ of following roastings 2 hours, process carrier; The carrier of processing is put into the Ce (NO of 0.5mol/L
3)
3In the solution, adopted incipient impregnation 3 hours,, 105 ℃ of dryings 5 hours, in nitrogen atmosphere, made desulfurizing agent in 3 hours at last then in 250 ℃ of roastings earlier 60 ℃ of dryings 3 hours.
Above-mentioned desulfurizing agent 1 gram is packed in the fixed bed reactors, is warming up to 200 ℃ of ventilatory responses, simulated flue gas consist of SO
2520ppm, O
25%, H
2O 3%, N
2Surplus, gas flow 310ml/min, desulfurization time 38min, desulfurization degree are 87%, saturated Sulfur capacity 3.6g/100g.
With the desulfurizing agent of the above-mentioned inactivation fixed bed reactors of packing into, temperature rises to 200 ℃ and feeds ammonias, regenerates at ammonia atmosphere; Desulfurizing agent after the regeneration, reusable more than 50 times, the SO that restores
2And NH
3Generate ammonium salt.
Embodiment 3:
, particle diameter adds active carbon in being the attapulgite powder of 45 μ m; The addition of active carbon is 35% of an attapulgite weight; Mix the back and add an amount of water and stir into pasty state, put into the make-up machine moulding, earlier in baking oven in 105 ℃ of dryings 5 hours; Again in nitrogen atmosphere in 400 ℃ of following roastings 3 hours, process carrier; The carrier of processing is put into the Ce (NO of 0.7mol/L
3)
3In the solution, adopted incipient impregnation 4 hours,, 105 ℃ of dryings 5 hours, in nitrogen atmosphere, made desulfurizing agent in 3 hours at last then in 300 ℃ of roastings earlier 60 ℃ of dryings 3 hours.
Above-mentioned desulfurizing agent 1 gram is packed in the fixed bed reactors, is warming up to 250 ℃ of ventilatory responses, simulated flue gas consist of SO
2520ppm, O
25%, H
2O 3%, N
2Surplus, gas flow 310ml/min, desulfurization time 40min, desulfurization degree are 88%, saturated Sulfur capacity 5.3g/100g.
With the desulfurizing agent of the above-mentioned inactivation fixed bed reactors of packing into, temperature rises to 250 ℃ and feeds ammonias, regenerates at ammonia atmosphere; Desulfurizing agent after the regeneration, reusable more than 50 times, the SO that restores
2And NH
3Generate ammonium salt.
Embodiment 4:
, particle diameter adds active carbon in being the attapulgite powder of 45 μ m; The addition of active carbon is 45% of an attapulgite weight; Mix the back and add an amount of water and stir into pasty state, put into the make-up machine moulding, earlier in baking oven in 105 ℃ of dryings 3 hours; Again in nitrogen atmosphere in 450 ℃ of following roastings 5 hours, process carrier; The carrier of processing is put into the Ce (NO of 0.8mol/L
3)
3In the solution, adopted incipient impregnation 5 hours,, 105 ℃ of dryings 5 hours, in nitrogen atmosphere, made desulfurizing agent in 3 hours at last then in 350 ℃ of roastings earlier 60 ℃ of dryings 3 hours.
Above-mentioned desulfurizing agent 1 gram is packed in the fixed bed reactors, is warming up to 300 ℃ of ventilatory responses, simulated flue gas consist of SO
2520ppm, O
25%, H
2O 3%, N
2Surplus, gas flow 310ml/min, desulfurization time 42min, desulfurization degree are 90%, saturated Sulfur capacity 6.5g/100g.
With the desulfurizing agent of the above-mentioned inactivation fixed bed reactors of packing into, temperature rises to 280 ℃ and feeds ammonias, regenerates at ammonia atmosphere; Desulfurizing agent after the regeneration, reusable more than 50 times, the SO that restores
2And NH
3Generate ammonium salt.
Embodiment 5:
, particle diameter adds active carbon in being the attapulgite powder of 45 μ m; The addition of active carbon is 55% of an attapulgite weight; Mix the back and add an amount of water and stir into pasty state, put into the make-up machine moulding, earlier in baking oven in 105 ℃ of dryings 4 hours; Again in nitrogen atmosphere in 500 ℃ of following roastings 2 hours, process carrier; The carrier of processing is put into the Ce (NO of 0.9mol/L
3)
3In the solution, adopted incipient impregnation 6 hours,, 105 ℃ of dryings 5 hours, in nitrogen atmosphere, made desulfurizing agent in 3 hours at last then in 400 ℃ of roastings earlier 60 ℃ of dryings 3 hours.
Above-mentioned desulfurizing agent 1 gram is packed in the fixed bed reactors, is warming up to 270 ℃ of ventilatory responses, simulated flue gas consist of SO
2520ppm, O
25%, H
2O 3%, N
2Surplus, gas flow 310ml/min, desulfurization time 50min, desulfurization degree are 92%, saturated Sulfur capacity 6.7g/100g.
With the desulfurizing agent of the above-mentioned inactivation fixed bed reactors of packing into, temperature rises to 350 ℃ and feeds ammonias, regenerates at ammonia atmosphere; Desulfurizing agent after the regeneration, reusable more than 50 times, the SO that restores
2And NH
3Generate ammonium salt.
Embodiment 6:
, particle diameter adds active carbon in being the attapulgite powder of 45 μ m; The addition of active carbon is 60% of an attapulgite weight; Mix the back and add an amount of water and stir into pasty state, put into the make-up machine moulding, earlier in baking oven in 105 ℃ of dryings 5 hours; Again in nitrogen atmosphere in 400 ℃ of following roastings 4 hours, process carrier; The carrier of processing is put into the Ce (NO of 1.0mol/L
3)
3In the solution, adopted incipient impregnation 6 hours,, 105 ℃ of dryings 5 hours, in nitrogen atmosphere, made desulfurizing agent in 3 hours at last then in 400 ℃ of roastings earlier 60 ℃ of dryings 3 hours.
Above-mentioned desulfurizing agent 1 gram is packed in the fixed bed reactors, is warming up to 300 ℃ of ventilatory responses, simulated flue gas consist of SO
2520ppm, O
25%, H
2O 3%, N
2Surplus, gas flow 310ml/min, desulfurization time 50min, desulfurization degree are 91%, saturated Sulfur capacity 6.1g/100g.
With the desulfurizing agent of the above-mentioned inactivation fixed bed reactors of packing into, temperature rises to 350 ℃ and feeds ammonias, regenerates at ammonia atmosphere; Desulfurizing agent after the regeneration, reusable more than 50 times, the SO that restores
2And NH
3Generate ammonium salt.
Claims (3)
1. the preparation method of a reproducible load type flue gas desulfurization agent is characterized in that this preparation method is made up of following steps:
(1) preparation of desulfurizing agent carrier; In particle diameter is the attapulgite powder of 45 μ m, add active carbon, the active carbon addition is the 15-60% of attapulgite weight, mixes the back and adds an amount of water and stir into pasty state; Put into the make-up machine moulding; Earlier in baking oven in 105 ℃ of dry 3-5 hours, again in nitrogen atmosphere in 300-500 ℃ of roasting 2-5 hour, process carrier;
(2) carrier is put into the Ce (NO that concentration is 0.2-1.0mol/L
3)
3In the solution, adopted incipient impregnation 2-6 hour, earlier 60 ℃ of dryings 3 hours, then 105 ℃ of dryings 5 hours, at last in nitrogen atmosphere in 200-400 ℃ of roasting 3 hours, desulfurizing agent.
2. the method for using of a reproducible load type flue gas desulfurization agent that obtains according to the preparation method of claim 1; The method for using that it is characterized in that this desulfurizing agent is: desulfurizing agent is packed in fixed bed or the moving-burden bed reactor; Reaction temperature is controlled at 120-300 ℃; Feed the normal pressure flue gas, air speed is 600-80000h
-1, desulfurization degree 85-92%, saturated Sulfur capacity 3.2-6.7g/100g.
3. the renovation process of a reproducible load type flue gas desulfurization agent that obtains according to the preparation method of claim 1; The renovation process that it is characterized in that this desulfurizing agent is: with the desulfurizing agent of inactivation pack into fixed bed or moving-burden bed reactor, in ammonia atmosphere, regenerate for temperature 250-350 ℃.
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CN102641651A (en) * | 2012-03-30 | 2012-08-22 | 四川大学 | Low-temperature active carbon-based desulfurizing agent and preparation method thereof |
CN104190478B (en) * | 2014-09-10 | 2016-09-21 | 清华大学 | A kind of denitration desulphurized aetivated carbon catalyst recovery process |
CN105032445A (en) * | 2015-07-24 | 2015-11-11 | 四川大学 | Mn-Ni bimetal doped activated carbon base desulfurization catalyst and preparation method thereof |
CN106822972A (en) * | 2015-12-07 | 2017-06-13 | 山东联星能源集团有限公司 | A kind of preparation method of air purifying preparation |
CN110614090A (en) * | 2019-09-26 | 2019-12-27 | 杨皓 | Process for activating, deactivating and removing organic matter active carbon by using gas boiler flue gas |
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CN1727054A (en) * | 2005-07-25 | 2006-02-01 | 北京北航天汇科技孵化器有限公司 | High effective reproducible agent of flue gas desulfurization and preparation method |
CN101181684A (en) * | 2007-12-06 | 2008-05-21 | 上海大学 | Absorption catalyst for desulfurization of smoke gas and preparation method thereof |
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