CN104190363B - A kind of calcium base decarbonization, desulfuration agent and method of modifying thereof and application - Google Patents
A kind of calcium base decarbonization, desulfuration agent and method of modifying thereof and application Download PDFInfo
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- CN104190363B CN104190363B CN201410419064.5A CN201410419064A CN104190363B CN 104190363 B CN104190363 B CN 104190363B CN 201410419064 A CN201410419064 A CN 201410419064A CN 104190363 B CN104190363 B CN 104190363B
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Abstract
The present invention relates to gas solid separation field, particularly relate to flue gas decarbonization desulfuration field, more specifically relate to a kind of calcium base decarbonization, desulfuration agent and method of modifying thereof and application, the method improves Ca-base adsorbent adsorption capacity effectively.Calcium base decarbonization, desulfuration agent method of modifying of the present invention, adopting lime stone after calcining, is 1:(2.0-3.0 with the mass ratio of ionic liquid) carry out mixed leaching, dry, finished product.The decarbonization, desulfuration agent of preparation greatly can improve adsorbance and the removal efficiency of adsorbent, and have abundant raw material source, easily buy, low price, the features such as method of modifying is simple, are applicable to flue gas decarbonization desulfurization.
Description
Technical field:
The present invention relates to gas solid separation field, particularly relate to the decarbonization, desulfuration field of flue gas, more specifically relate to a kind of calcium base decarbonization, desulfuration agent method of modifying.
Background technology:
Containing CO in the flue gas such as coal-burning power plant, metallurgy industry
2and SO
2deng sour gas, SO
2being one of Air Pollutant Discharge, is the formation source of acid rain, CO
2being main greenhouse gas, is one of main cause causing climate change at present.Along with the raising day by day that environmental protection requires Air Pollutant Emission, in gas cleaning process, how to select decarbonization, desulfuration technique effectively and rationally, to reach the purification object of flue gas decarbonization desulfurization compared with Low investment and operating cost, both made SO in flue gas
2discharge meets the regulation of discharging standards, can reduce CO again
2discharge capacity is the key issue that current coal-burning power plant, metallurgy industry etc. develop in a healthy way.Therefore, various high-performance CO
2and SO
2the exploitation of trapping agent is one of theme of this area research, in recent years, Ca-base adsorbent due to the performance of its uniqueness be the heat subject of this area research and development always.
For same flue gas, decarburization and desulfurization are carried out respectively, have realized industrialized flue gas decarbonization mainly amine method (i.e. MEA washing method) at present, have belonged to wet method.Flue gas desulfurization has by the method that the kind of desulfurizing agent is common: with CaCO
3calcium method based on (lime stone), the magnesium processes based on MgO, with Na
2sO
3based on sodium method, with NH
3based on ammonia process, the organic alkaline process based on organic base.The commercialization flue gas desulfurization of more than 90% adopts calcium method desulfur technology in the world, and calcium method is divided into wet method, dry method and half-dried (half is wet) method.Wet technique adopts containing the solution of absorbent or slurries smoke treatment, and this method has that decarbonization, desulfuration reaction speed is fast, equipment simple, removal efficiency advantages of higher, but ubiquity seriously corroded, operation and maintenance cost are high and cause secondary pollution problems.Desulfurization by dry method is that the process of absorption process and product is carried out all under anhydrous conditions, this method have discharge without waste sewage, equipment corrosion is lighter, flue-gas temperature is without the advantage such as obviously reducing, secondary pollution is few, but the problem such as it is low to there is desulfuration efficiency, and reaction speed is comparatively slow, equipment is huge.In addition, also have semi-dry desulphurization technology to refer to desulfurizing agent desulfurization in the dry state, regenerate under wet condition (as washing regenerating active carbon flow process), or desulfurization under wet condition, under dry state, process the flue gas desulfurization technique of desulfurization product (as spray drying process).Particularly desulfurization under wet condition, under dry state, process the semidry method of desulfurization product, with its advantage that existing wet desulphurization reaction speed is fast, desulfuration efficiency is high, have again that dry method is discharged without sewage spent acid, an easy-to-handle advantage of desulfurization afterproduct and be subject to people and pay close attention to widely.Absorb in sulfureous in flue gas and oxycarbide at chemical dry, the performance absorbing (absorption) agent fundamentally determines CO
2and SO
2the efficiency of capture operation, thus has very high requirement to the performance absorbing (absorption) agent.Chemical absorbing CO is carried out for flue gas
2and SO
2process, in order to strengthen mass transport process, improving removal efficiency, improving the utilization rate of calcium, reduce investment and the operating cost of equipment, certain requirement be it is also proposed to absorption (absorption) device and operating process.
Ca-base adsorbent has great advantage at commercial Application tool, and it can realize the trapping of carbon sulphur, CO
2and SO
2directly seal up for safekeeping, have arresting efficiency high, energy-conservation, low in raw material price, adsorbent cost is low, economy advantages of higher.But Ca-base adsorbent is in adsorption process, its trapping ability can decay gradually, and adsorbent causes sintering when higher temperature, and adsorption capacity worsens.Visible adsorbent, in microstructure and attribute, as surface area, pore volume and structure and surface area, all can impact response characteristic.The initial reaction activity of adsorbent is important, and its trapping characteristic plays an important role.Therefore, in order to improve the reactivity of adsorbent and reduce adsorbent amount, the microstructure improving Ca-base adsorbent is an important channel.
Summary of the invention:
A kind of flue gas is the object of the present invention is to provide to remove CO
2and SO
2ca-base adsorbent, this adsorbent improves Ca-base adsorbent adsorption capacity and removal efficiency effectively.
The above-mentioned flue gas that another object of the present invention is to provide removes CO
2and SO
2the method of modifying of Ca-base adsorbent.
The present invention is and an object is to provide flue gas and removes CO
2and SO
2the application of Ca-base adsorbent.
The scheme of concrete technology of the present invention is as follows:
A kind of calcium base decarbonization, desulfuration agent method of modifying, the step of described preparation method, preparation process is as follows:
1) pulverize: lime stone is ground into powder in pulverizer;
2) calcine: upper step powder is placed in Muffle furnace, is warming up to calcining heat gradually, calcining heat is 750-1100 DEG C; Calcine 30min at such a temperature, be cooled to room temperature for subsequent use;
3) mixed leaching: Alcohol amine type sulfamic acid ionic liquid is added in a stirred vessel, upper step calcined product is slowly added in Alcohol amine type sulfamic acid ionic liquid container, add while stirring, make calcined product and ionic liquid mixing, wherein the mass ratio of lime stone and ionic liquid is 1:(2.0-3.0); Container is warming up to mixed leaching temperature 60-80 DEG C, stirs lower mixed leaching 20-30h, generates coagulant liquid;
4) dry: the coagulant liquid decompress filter upper step obtained, filtrate retains, and can continue to use as maceration extract, and filter cake is placed in baking oven, at N
2under 80-120 DEG C of torrefying temperature, 12-24h is dried in atmosphere;
5) finished product: dry thing compressing tablet granulating, obtain modified calcium-based adsorbent.
The present invention designs further and is:
Described Alcohol amine type sulfamic acid ionic liquid, its structure is:
R in formula
1, R
2and R
3be respectively alkyl or the alkyl group of H or hydroxyl, but three can not be H or alkyl group simultaneously; R and R ' is respectively H or alkyl group, and alkyl is containing 1-3 carbon.
Described Alcohol amine type sulfamic acid ionic liquid is preferably taken as: amino taurine monoethanolamine, amino taurine diethanol amine, amino taurine triethanolamine, amino taurine methyl diethanolamine, aminopropanesulfonic acid monoethanolamine, aminopropanesulfonic acid diethanol amine, amino fourth sulfonic acid monoethanolamine or methylamino propane sulfonic acid monoethanolamine.
Step 2) in calcination process programming rate be 15 DEG C/min.
Step 3) in mixed dipped journey stir speed (S.S.) 90-150r/min.
Step 5) in dry thing compressing tablet and become 0.5-1mm granular solid matter.
The invention still further relates to calcium base decarbonization, desulfuration agent prepared by said method.
The invention still further relates to the application of this calcium base decarbonization, desulfuration agent, CO in flue gas can be removed efficiently
2and SO
2.
The present invention compared to existing technology tool has the following advantages:
Present inventor has done great many of experiments and research work in Ca-base adsorbent modification, proposes one can remove CO simultaneously
2and SO
2the method of modifying of Ca-base adsorbent, modified Ca-base adsorbent has higher adsorption capacity and removal efficiency, at present at gas cleaning CO
2and SO
2field has no and uses and report.
The maceration extract that the present invention adopts is new type functional Alcohol amine type sulfamic acid ionic liquid, is the green high-efficient solvent of generally acknowledging at present, and this ionic liquid can form network structure thing on porous CaO surface, accelerates CO
2and SO
2material diffusion, transmission and the rate of adsorption, play material carrier and catalytic action.After tested, modified calcium-based adsorbent mass transfer rate is 2.3-3.9 times of common Ca-base adsorbent.
The functional alcohol amine type sulfamic acid ionic liquid that the present invention proposes, due to the effect of hydroxyl, sulfonic group and amino in ionic liquid chemical constitution, the flue gas of modified calcium-based adsorbent to high-moisture has patience, and common Ca-base adsorbent is under the effect of water, surface forms pastel, affect material diffusion, transmit and the rate of adsorption, and modified calcium-based adsorbent does not affect by water content, the utilization rate which increasing calcium with extend adsorbent service life.Such as, in simulated flue gas, 2-3%H is increased
2o (i.e. water vapour), after tested, the calcium utilization of modified calcium-based adsorbent and service life be respectively the 1.4-2.0 of common Ca-base adsorbent doubly and 2-3 times.
Modified calcium-based adsorbent adsorbance of the present invention and removal efficiency are all higher than common Ca-base adsorbent, and adsorbance is greater than 0.6g/g, is up to 6.7g/g, SO
2removal efficiency is greater than 98%, is up to 99.7%, CO
2removal efficiency is greater than 85%, and be 1.28-1.76 times of common Ca-base adsorbent, the Ca-base adsorbent of this method modification can remove CO in flue gas efficiently
2and SO
2.
Accompanying drawing illustrates:
Fig. 1 is the flow process of calcium base decarbonization, desulfuration agent method of modifying of the present invention.
Detailed description of the invention:
Below in conjunction with accompanying drawing, the present invention is described in further detail.
In following example, natural limestone is commercial commodity, Main Ingredients and Appearance CaCO
3mass percentage 80%-88%.
Embodiment 1
150 natural limestones as shown in Figure 1, are pulverized into about 80 order powder, are walked stand-by under powder by preparation flow of the present invention in pulverizer.450g amino taurine monoethanolamine ionic liquid is added in stirred vessel stand-by.The flour limestone obtained is placed in Muffle furnace, heat up gradually, programming rate is 15 DEG C/min, and temperature reaches calcining heat 1000 DEG C, calcination time is 30min, be cooled to room temperature, added while stirring at leisure in ionic liquid container by calcined product, container is warming up to mixed leaching temperature 60 C, stir speed (S.S.) 150r/min, make calcined product and ionic liquid mixing, mixed leaching time 20h, generates coagulant liquid.By coagulant liquid decompress filter, filter cake is placed in baking oven, at N
2dry at 80 DEG C of temperature in atmosphere, dry time 12h.To dry product compressing tablet on type mechanical tableting machine and become 0.5-1mm granular solid matter, particle is finished product Ca-base adsorbent.
Embodiment 2
150 natural limestones are pulverized into about 80 order powder in pulverizer, walks stand-by under powder.375g amino taurine diethanol amine ionic liquid is added in stirred vessel stand-by.The flour limestone obtained is placed in Muffle furnace, heat up gradually, programming rate is 15 DEG C/min, and temperature reaches calcining heat 1100 DEG C, calcination time is 30min, be cooled to room temperature, added while stirring at leisure in ionic liquid container by calcined product, container is warming up to mixed leaching temperature 70 C, stir speed (S.S.) 120r/min, make calcined product and ionic liquid mixing, mixed leaching time 24h, generates coagulant liquid.By coagulant liquid decompress filter, filter cake is placed in baking oven, at N
2dry at 100 DEG C of temperature in atmosphere, dry time 20h.To dry product compressing tablet on type mechanical tableting machine and become 0.5-1mm granular solid matter, particle is finished product Ca-base adsorbent.
Embodiment 3
150 natural limestones are pulverized into about 80 order powder in pulverizer, walks stand-by under powder.300g amino taurine triethanolamine-ion liquid is added in stirred vessel stand-by.The flour limestone obtained is placed in Muffle furnace, heat up gradually, programming rate is 15 DEG C/min, and temperature reaches calcining heat 900 DEG C, calcination time is 30min, be cooled to room temperature, added while stirring at leisure in ionic liquid container by calcined product, container is warming up to mixed leaching temperature 80 DEG C, stir speed (S.S.) 110r/min, make calcined product and ionic liquid mixing, mixed leaching time 26h, generates coagulant liquid.By coagulant liquid decompress filter, filter cake is placed in baking oven, at N
2dry at 120 DEG C of temperature in atmosphere, dry time 24h.To dry product compressing tablet on type mechanical tableting machine and become 0.5-1mm granular solid matter, particle is finished product Ca-base adsorbent.
Embodiment 4
150 natural limestones are pulverized into about 80 order powder in pulverizer, walks stand-by under powder.420g amino taurine methyl diethanolamine ionic liquid is added in stirred vessel stand-by.The flour limestone obtained is placed in Muffle furnace, heat up gradually, programming rate is 15 DEG C/min, and temperature reaches calcining heat 750 DEG C, calcination time is 30min, be cooled to room temperature, added while stirring at leisure in ionic liquid container by calcined product, container is warming up to mixed leaching temperature 80 DEG C, stir speed (S.S.) 90r/min, make calcined product and ionic liquid mixing, mixed leaching time 28h, generates coagulant liquid.By coagulant liquid decompress filter, filter cake is placed in baking oven, at N
2dry at 90 DEG C of temperature in atmosphere, dry time 16h.To dry product compressing tablet on type mechanical tableting machine and become 0.5-1mm granular solid matter, particle is finished product Ca-base adsorbent.
Embodiment 5
150 natural limestones are pulverized into about 80 order powder in pulverizer, walks stand-by under powder.390g aminopropanesulfonic acid monoethanolamine ionic liquid is added in stirred vessel stand-by.The flour limestone obtained is placed in Muffle furnace, heat up gradually, programming rate is 15 DEG C/min, and temperature reaches calcining heat 800 DEG C, calcination time is 30min, be cooled to room temperature, added while stirring at leisure in ionic liquid container by calcined product, container is warming up to mixed leaching temperature 70 C, stir speed (S.S.) 100r/min, make calcined product and ionic liquid mixing, mixed leaching time 30h, generates coagulant liquid.By coagulant liquid decompress filter, filter cake is placed in baking oven, at N
2dry at 110 DEG C of temperature in atmosphere, dry time 18h.To dry product compressing tablet on type mechanical tableting machine and become 0.5-1mm granular solid matter, particle is finished product Ca-base adsorbent.
Embodiment 6
150 natural limestones are pulverized into about 80 order powder in pulverizer, walks stand-by under powder.330g aminopropanesulfonic acid diethanol amine ionic liquid is added in stirred vessel stand-by.The flour limestone obtained is placed in Muffle furnace, heat up gradually, programming rate is 15 DEG C/min, and temperature reaches calcining heat 850 DEG C, calcination time is 30min, be cooled to room temperature, added while stirring at leisure in ionic liquid container by calcined product, container is warming up to mixed leaching temperature 75 DEG C, stir speed (S.S.) 100r/min, make calcined product and ionic liquid mixing, mixed leaching time 26h, generates coagulant liquid.By coagulant liquid decompress filter, filter cake is placed in baking oven, at N
2dry at 110 DEG C of temperature in atmosphere, dry time 20h.To dry product compressing tablet on type mechanical tableting machine and become 0.5-1mm granular solid matter, particle is finished product Ca-base adsorbent.
Embodiment 7
150 natural limestones are pulverized into about 80 order powder in pulverizer, walks stand-by under powder.360g amino fourth sulfonic acid monoethanolamine ionic liquid is added in stirred vessel stand-by.The flour limestone obtained is placed in Muffle furnace, heat up gradually, programming rate is 15 DEG C/min, and temperature reaches calcining heat 1100 DEG C, calcination time is 30min, be cooled to room temperature, added while stirring at leisure in ionic liquid container by calcined product, container is warming up to mixed leaching temperature 80 DEG C, stir speed (S.S.) 95r/min, make calcined product and ionic liquid mixing, mixed leaching time 24h, generates coagulant liquid.By coagulant liquid decompress filter, filter cake is placed in baking oven, at N
2dry at 100 DEG C of temperature in atmosphere, dry time 20h.To dry product compressing tablet on type mechanical tableting machine and become 0.5-1mm granular solid matter, particle is finished product Ca-base adsorbent.
Embodiment 8
150 natural limestones are pulverized into about 80 order powder in pulverizer, walks stand-by under powder.300g methylamino propane sulfonic acid monoethanolamine ionic liquid is added in stirred vessel stand-by.The flour limestone obtained is placed in Muffle furnace, heat up gradually, programming rate is 15 DEG C/min, and temperature reaches calcining heat 950 DEG C, calcination time is 30min, be cooled to room temperature, added while stirring at leisure in ionic liquid container by calcined product, container is warming up to mixed leaching temperature 80 DEG C, stir speed (S.S.) 90r/min, make calcined product and ionic liquid mixing, mixed leaching time 24h, generates coagulant liquid.By coagulant liquid decompress filter, filter cake is placed in baking oven, at N
2dry at 120 DEG C of temperature in atmosphere, dry time 20h.To dry product compressing tablet on type mechanical tableting machine and become 0.5-1mm granular solid matter, particle is finished product Ca-base adsorbent.
Test case one:
Finished product Ca-base adsorbent prepared by Example 1-8 is tested respectively as follows: get 60g finished product Ca-base adsorbent and load fixed bed reactors, pass into simulated flue gas and carry out performance evaluation.Fixed bed reactors process conditions are: flue gas pressures 0.12MPa, flow 200mL/min, composition 12%CO
2, 0.1%SO
2, 3%O
2, all the other are N
2, adsorption temp 80 DEG C.Measure adsorbance and removal efficiency.
Get the common Ca-base adsorbent (natural limestone calcined product) that 60g do not carry out modification equally and load fixed bed reactors, pass into simulated flue gas and carry out performance evaluation.Fixed bed reactors process conditions are: flue gas pressures 0.12MPa, flow 200mL/min, composition 12%CO
2, 0.1%SO
2, 3%O
2, all the other are N
2, adsorption temp 80 DEG C.Measure adsorbance and removal efficiency.The adsorbance measured and removal efficiency data as a comparison.
Performance and the common Ca-base adsorbent of modified calcium-based adsorbent compare, and evaluation result is shown in Table 1.
Table 1 modified calcium-based adsorbent Evaluation results
Result shows: modified calcium-based adsorbent adsorbance and removal efficiency are all higher than common Ca-base adsorbent, and adsorbance is greater than 0.6g/g, are up to 6.7g/g, SO
2removal efficiency is greater than 98%, is up to 99.7%, CO
2removal efficiency is greater than 85%, and be 1.28-1.76 times of common Ca-base adsorbent, the Ca-base adsorbent of this method modification can remove CO in flue gas efficiently
2and SO
2.
Claims (8)
1. a calcium base decarbonization, desulfuration agent method of modifying, is characterized in that: the step of this method of modifying is as follows:
1) pulverize: agstone is broken into powder;
2) calcine: upper step powder is placed in Muffle furnace, is warming up to calcining heat gradually, calcining heat is 750-1100 DEG C; Calcine 30min at such a temperature, be cooled to room temperature for subsequent use;
3) mixed leaching: Alcohol amine type sulfamic acid ionic liquid is added in a stirred vessel, upper step calcined product is slowly added in Alcohol amine type sulfamic acid ionic liquid container, add while stirring, make calcined product and ionic liquid mixing, wherein the mass ratio of lime stone and ionic liquid is 1:(2.0-3.0); Container is warming up to mixed leaching temperature 60-80 DEG C, stirs lower mixed leaching 20-30h, generates coagulant liquid;
4) dry: the coagulant liquid decompress filter upper step obtained, filter cake is placed in baking oven, at N
2under 80-120 DEG C of torrefying temperature, 12-24h is dried in atmosphere;
5) finished product: dry thing compressing tablet granulating, obtain modified calcium-based adsorbent.
2. calcium base decarbonization, desulfuration agent method of modifying according to claim 1, it is characterized in that: described Alcohol amine type sulfamic acid ionic liquid, its structure is:
R in formula
1, R
2and R
3be respectively alkyl or the alkyl group of H or hydroxyl, but three can not be H or alkyl group simultaneously; R and R ' is respectively H or alkyl group, and alkyl is containing 1-3 carbon.
3. calcium base decarbonization, desulfuration agent method of modifying according to claim 2, is characterized in that: described Alcohol amine type sulfamic acid ionic liquid is chosen for: amino taurine monoethanolamine, amino taurine diethanol amine, amino taurine triethanolamine, amino taurine methyl diethanolamine, aminopropanesulfonic acid monoethanolamine, aminopropanesulfonic acid diethanol amine, amino fourth sulfonic acid monoethanolamine or methylamino propane sulfonic acid monoethanolamine.
4. calcium base decarbonization, desulfuration agent method of modifying according to claim 3, is characterized in that: step 2) in calcination process programming rate be 15 DEG C/min.
5. calcium base decarbonization, desulfuration agent method of modifying according to claim 3, is characterized in that: step 3) in mixed dipped journey stir speed (S.S.) 90-150r/min.
6. calcium base decarbonization, desulfuration agent method of modifying according to claim 3, is characterized in that: step 5) in dry thing compressing tablet and become 0.5-1mm granular solid matter.
7. the calcium base decarbonization, desulfuration agent prepared by the arbitrary described method of claim 1-6.
8. the application of calcium base decarbonization, desulfuration agent in flue gas in decarbonization, desulfuration described in claim 7.
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| CN101537339A (en) * | 2009-03-18 | 2009-09-23 | 浙江大学 | Preparation of CaTiO3-coated calcium oxide-based CO2 absorbent |
| CN102674424A (en) * | 2012-04-28 | 2012-09-19 | 浙江大学 | Method for preparing nanometer calcium carbonate slurry by using waste gypsum as calcium sources, products and application |
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