CN101804289B - Preparation of flue gas desulfurizer and use and regeneration method thereof - Google Patents
Preparation of flue gas desulfurizer and use and regeneration method thereof Download PDFInfo
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- CN101804289B CN101804289B CN2010101424489A CN201010142448A CN101804289B CN 101804289 B CN101804289 B CN 101804289B CN 2010101424489 A CN2010101424489 A CN 2010101424489A CN 201010142448 A CN201010142448 A CN 201010142448A CN 101804289 B CN101804289 B CN 101804289B
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Abstract
The invention discloses preparation of a flue gas desulfurizer and use and a regeneration method thereof, comprising the following steps: adding 10-50wt% of active carbon in attapulgite power with the grain size of 45 mu m; mixing uniformly and adding proper amount of water to stir to be pasty; forming in a forming machine; drying for 3-5 hours at the temperature of 105 DEG C in a baking oven; baking for 2-5 hours at the temperature of 300-500 DEG C in nitrogen atmosphere so as to obtain a carrier; putting the carrier in 0.8-2.2 mol/L Cu(NO3)2 solution, soaking for 2-6 hours with the same volume; drying for 3 hours at the temperature of 60 DEG C, drying for 5 hours at the temperature of 105 DEG C, and baking for 3 hours at the temperature of 200-400 DEG C in nitrogen atmosphere so as to obtain the desulfurizer; putting the desulfurizer in a reactor at the reaction temperature of 120-300 DEG C, normally pressing smoke gas, wherein the air speed is 600-80000 h<-1>, the percentage of desulfurization is 80-92%, and the saturation sulfur capacity is 3.0-6.5g/100g; putting the inactive desulfurizer in the reactor at the temperature of 250-350 DEG C, and regenerating ammonia atmosphere. The desulfurizer carries out desulfurization reaction with the temperature of flue gas directly; the percentage of desulfurization is high, the regeneration is easy and the production run cost is low.
Description
Technical field
The present invention relates to a kind of preparation and application and renovation process of desulfurizing agent, be specifically related to a kind of preparation and application and renovation process of fume desulfurizing 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; Flue gas after the desulfurization is not lowered the temperature, and does not need to heat (power consumption is few) again, can satisfy the requirement of discharging diffusion; In addition, desulfurization by dry method also has advantages such as no fouling, dewfall, obstruction, reliability are high, secondary pollution is few, 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 120-250 ℃, not only the process energy consumption is low in this configuration, and can reduce dust poisoning desulfurizing agent.Studied more CuO/Al in recent years
2O
3, CeO
2/ γ-Al
2O
3, activated coke (charcoal) etc., like the chemistry of fuel journal, 2003,31 (5): 385-389 has reported CuO/Al
2O
3Desulfurizing agent, patent ZL200510087043.9 discloses CeO
2/ γ-Al
2O
3Desulfurizing agent and preparation method thereof, but CuO/Al
2O
3And CeO
2/ γ-Al
2O
3Desulphurizing activated temperature requirement also 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 120-300 ℃; 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; The 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, 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 both at home and abroad with attapulgite and the industrial applied research 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 application and renovation process that a kind of fume desulfurizing agent is provided; The desulfurizing agent that adopts this preparation method to make is used for flue gas desulfurization; Use under suitable industry coal-boiler flue gas exhaust gas temperature, the high-speed condition; Have high desulfurization activity, can solve that existing fume desulfurizing agent desulfurization degree is low, cycle-index is few, problems such as investment and operating cost height.
The preparation method of desulfurizing agent 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 10-50% of attapulgite quality, mixes the back and adds an amount of water and stir into pasty state; Put into the make-up machine moulding; In baking oven,, in nitrogen atmosphere,, process carrier in 300-500 ℃ of roasting 2-5 hour in 105 ℃ of dry 3-5 hours;
(2) carrier is put into the Cu (NO that concentration is 0.8-2.2mol/L
3)
2In the solution, adopt incipient impregnation after 2-6 hour, 60 ℃ of dryings 3 hours, then 105 ℃ of dryings 5 hours again in nitrogen atmosphere in 200-400 ℃ of roasting 3 hours, desulfurizing agent.
The application process of desulfurizing agent of the present invention is following: 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, desulfurization degree is at 80-92%, saturated Sulfur capacity 3.0-6.5g/100g.
The renovation process of desulfurizing agent of the present invention is following: with the desulfurizing agent of inactivation pack into fixed bed or moving-burden bed reactor, regenerate at ammonia atmosphere, temperature is controlled at 250-350 ℃.
The present invention compared with prior art has following advantage:
1, desulfurization degree is high, and desulfurization degree reaches 80-92%;
2, this desulfurizing agent can directly utilize the temperature of flue gas to carry out desulphurization reaction, so 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
Following specific embodiment further specifies technical solution of the present invention, and these embodiment are interpreted as not being the restriction to technical scheme.
Embodiment 1:
, particle diameter adds active carbon in being the attapulgite powder of 45 μ m; The addition of active carbon is 10% of an attapulgite quality; Mix the back and add an amount of water and stir into pasty state, put into the make-up machine moulding, in baking oven in 105 ℃ of dryings 3 hours; In nitrogen atmosphere,, process carrier in 300 ℃ of roastings 2 hours; The carrier of processing is put into the Cu (NO of 0.8mol/L
3)
2In the solution, adopt incipient impregnation after 2 hours,, in nitrogen atmosphere, made desulfurizing agent in 3 hours again in 5 hours 105 ℃ of dryings then in 200 ℃ of roastings 60 ℃ of dryings 3 hours.
Desulfurizing agent 0.5 gram is packed in the fixed bed reactors, is warming up to 120 ℃ of ventilatory responses, simulated flue gas consist of SO
2500ppm, O
25%, H
2O 3%, N
2Surplus, gas flow 300ml/min, desulfurization time 30min, desulfurization degree are 80%, saturated Sulfur capacity 3.0g/100g.
With the desulfurizing agent of the inactivation fixed bed reactors of packing into, temperature rises to 250 ℃ and feeds ammonias, regenerate at ammonia atmosphere, and the 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 20% of an attapulgite quality; Mix the back and add an amount of water and stir into pasty state, put into the make-up machine moulding, in baking oven in 105 ℃ of dryings 4 hours; In nitrogen atmosphere,, process carrier in 350 ℃ of roastings 3 hours; The carrier of processing is put into the Cu (NO of 1.0mol/L
3)
2In the solution, adopt incipient impregnation after 3 hours,, in nitrogen atmosphere, made desulfurizing agent in 3 hours again in 5 hours 105 ℃ of dryings then in 250 ℃ of roastings 60 ℃ of dryings 3 hours.
Desulfurizing agent 0.5 gram is packed in the fixed bed reactors, is warming up to 150 ℃ of ventilatory responses, simulated flue gas consist of SO
2500ppm, O
25%, H
2O 3%, N
2Surplus, gas flow 300ml/min, desulfurization time 35min, desulfurization degree are 83%, saturated Sulfur capacity 3.5g/100g.
With the desulfurizing agent of the inactivation fixed bed reactors of packing into, temperature rises to 280 ℃ and feeds ammonias, regenerate at ammonia atmosphere, and the 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 quality; Mix the back and add an amount of water and stir into pasty state, put into the make-up machine moulding, in baking oven in 105 ℃ of dryings 5 hours; In nitrogen atmosphere,, process carrier in 400 ℃ of roastings 3 hours; The carrier of processing is put into the Cu (NO of 1.3mol/L
3)
2In the solution, adopt incipient impregnation after 5 hours,, in nitrogen atmosphere, made desulfurizing agent in 3 hours again in 5 hours 105 ℃ of dryings then in 300 ℃ of roastings 60 ℃ of dryings 3 hours.
Desulfurizing agent 0.5 gram is packed in the fixed bed reactors, is warming up to 200 ℃ of ventilatory responses, simulated flue gas consist of SO
2500ppm, O
25%, H
2O 3%, N
2Surplus, gas flow 300ml/min, desulfurization time 38min, desulfurization degree are 87%, saturated Sulfur capacity 5.0g/100g.
With the desulfurizing agent of the inactivation fixed bed reactors of packing into, temperature rises to 300 ℃ and feeds ammonias, regenerate at ammonia atmosphere, and the 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 40% of an attapulgite quality; Mix the back and add an amount of water and stir into pasty state, put into the make-up machine moulding, in baking oven in 105 ℃ of dryings 5 hours; In nitrogen atmosphere,, process carrier in 450 ℃ of roastings 5 hours; The carrier of processing is put into the Cu (NO of 1.5mol/L
3)
2In the solution, adopt incipient impregnation after 6 hours,, in nitrogen atmosphere, made desulfurizing agent in 3 hours again in 5 hours 105 ℃ of dryings then in 350 ℃ of roastings 60 ℃ of dryings 3 hours.
Desulfurizing agent 0.5 gram is packed in the fixed bed reactors, is warming up to 250 ℃ of ventilatory responses, simulated flue gas consist of SO
2500ppm, O
25%, H
2O 3%, N
2Surplus, gas flow 300ml/min, desulfurization time 40min, desulfurization degree are 90%, saturated Sulfur capacity 6.1g/100g.
With the desulfurizing agent of the inactivation fixed bed reactors of packing into, temperature rises to 350 ℃ and feeds ammonias, regenerate at ammonia atmosphere, and the 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 50% of an attapulgite quality; Mix the back and add an amount of water and stir into pasty state, put into the make-up machine moulding, in baking oven in 105 ℃ of dryings 4 hours; In nitrogen atmosphere,, process carrier in 500 ℃ of roastings 2 hours; The carrier of processing is put into the Cu (NO of 2.2mol/L
3)
2In the solution, adopt incipient impregnation after 6 hours,, in nitrogen atmosphere, made desulfurizing agent in 3 hours again in 5 hours 105 ℃ of dryings then in 400 ℃ of roastings 60 ℃ of dryings 3 hours.
Desulfurizing agent 0.5 gram is packed in the fixed bed reactors, is warming up to 250 ℃ of ventilatory responses, simulated flue gas consist of SO
2500ppm, O
25%, H
2O 3%, N
2Surplus, gas flow 300ml/min; Desulfurization time 50min, desulfurization degree are 92%, saturated Sulfur capacity 6.5g/100g.
With the desulfurizing agent of the inactivation fixed bed reactors of packing into, temperature rises to 350 ℃ and feeds ammonias, regenerate at ammonia atmosphere, and the desulfurizing agent after the regeneration, reusable more than 50 times, the SO that restores
2And NH
3Generate ammonium salt.
Claims (1)
1. the preparation method of a fume desulfurizing 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 10-50% of attapulgite quality, mixes the back and adds an amount of water and stir into pasty state; Put into the make-up machine moulding; In baking oven,, in nitrogen atmosphere,, process carrier in 300-500 ℃ of roasting 2-5 hour in 105 ℃ of dry 3-5 hours;
(2) carrier is put into the Cu (NO of 0.8-2.2mol/L
3)
2In the solution, adopt incipient impregnation after 2-6 hour, 60 ℃ of dryings 3 hours, then 105 ℃ of dryings 5 hours again in nitrogen atmosphere in 200-400 ℃ of roasting 3 hours, desulfurizing agent.
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| CN103447072B (en) * | 2013-08-23 | 2014-12-03 | 淮阴工学院 | Preparation method of Fe-NaY-C-attapulgite compound flue gas denitrification catalyst |
| CN103566879A (en) * | 2013-09-26 | 2014-02-12 | 蚌埠华纺滤材有限公司 | Expanded perlite modified activated carbon automobile exhaust desulfurizing agent, and preparation method thereof |
| CN105435739B (en) * | 2014-09-28 | 2018-02-16 | 中国石化扬子石油化工有限公司 | One kind is used for hydrogen sulfide remover and preparation method thereof in normal temperature water-less environment |
| CN104289232A (en) * | 2014-10-10 | 2015-01-21 | 南京正森环保科技有限公司 | Environment-friendly active carbon catalyst as well as preparation method and application thereof to flue gas mercury removal |
| CN105617986B (en) * | 2014-12-01 | 2019-04-23 | 中国石化扬子石油化工有限公司 | A kind of preparation method of composite activated carbon hydrogen sulfide remover |
| CN106554832A (en) * | 2015-09-24 | 2017-04-05 | 刘从荡 | A kind of preparation method of concave-convex bar methane desulfurizing dessicant |
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| CN105903324A (en) * | 2016-05-18 | 2016-08-31 | 天津普瑞特净化技术有限公司 | Copper oxide loaded active carbon desulfurizing agent and preparation process thereof |
| CN106146519B (en) * | 2016-06-22 | 2017-12-26 | 江苏科技大学 | Preparation, sign and the application of bivalent manganese fluorescent material of the one kind based on 1,4 diethyl of dibromo 1,4 diazabicylo [2.2.2] octane |
| CN114558442A (en) * | 2022-03-02 | 2022-05-31 | 通化鑫鸿新材料有限公司 | Preparation method and application of high-activity nano calcium-based desulfurizer |
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| ES2340678T3 (en) * | 2003-10-15 | 2010-06-08 | Haldor Topsoe A/S | CATALYST SUPPORT MATERIAL, PREPARED CATALYSTS FROM THE SAME, AND PROCESS FOR THE TREATMENT OF A FIREPLACE GAS. |
| CN100415344C (en) * | 2004-05-28 | 2008-09-03 | 长春东狮科贸实业有限公司 | Active carbon desulfurizing agent and application thereof |
| CN100348300C (en) * | 2005-07-25 | 2007-11-14 | 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 |
| CN101249373B (en) * | 2007-12-07 | 2010-12-15 | 唐山师范学院 | Flue gas desulfurization agent preparation method |
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