富钙生物油脱硫脱硝机理研究
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摘要
燃煤电厂是SO2和NOx排放的重要来源,随着目前环保要求越来越严格,燃煤电厂SO2和NOx的脱除己势在必行。
炉内喷钙是我国众多中小型燃煤机组及工业锅炉常用的脱硫方式,脱硫剂采用石灰石。然而石灰石脱硫存在着钙利用率低、脱硫效率不高和无法同时脱硝等问题。国外研究表明有机酸钙盐(如乙酸钙等)在具有较高的脱硫能力的同时,还具备一定的脱硝能力,非常适合用于燃煤锅炉污染物的脱除。然而制备有机酸钙盐需要大量有机酸,而有机酸生产成本太高,这限制了有机酸在工业上的应用,所以此种方法目前还停留在理论研究阶段。
生物油中含有丰富的有机酸,将其与钙基吸收剂反应可制备出在一种富含有机酸钙盐的“富钙生物油”,可用于有机酸钙盐的替代品,从而解决有机钙盐生产成本过高的问题。
本文以富钙生物油为研究对象,首先对富钙生物油制备过程的影响因素作用规律进行了研究,考察了石灰石粒径、生物油pH值、反应温度对富钙生物油的制备过程的影响,指出生物油pH值与反应温度在制备富钙生物油过程中起着关键的作用,较小pH值的生物油与较高的反应温度有利于富钙生物油中钙离子浓度的增加。对制备出的富钙生物油成分分析表明,富钙生物油中主要含有Ca、H、O、C等元素,富钙生物油中除有机羧酸钙盐外,还含有醇、苯、酚类等物质。
对富钙生物油煅烧过程进行了研究,表明富钙生物油的煅烧可以分为四个阶段。第一阶段是<200℃时富钙生物油的脱水阶段,第二阶段是温度在200℃～400℃时,富钙生物油中部分残留生物油的分解析出,也包括部分分解温度较低的有机羧酸钙盐的分解。第三阶段为400℃左右时,富钙生物油的有机羧酸钙盐分解阶段。最后是碳酸钙的分解阶段。随着升温速率的增大,富钙生物油分解的后两个阶段分解起始温度都有所提高。粒径对富钙生物油煅烧特性的影响较小。CO2气氛对富钙生物油碳酸钙分解阶段表现出明显的抑制作用。对富钙生物油后两个阶段分解动力学进行了分析,表明后两个分解阶段符合相边界反应的收缩圆柱体模型。富钙生物油煅烧产物孔结构受其煅烧过程的影响非常明显,特别是有机羧酸钙盐的快速分解阶段,在此温度区间内(400～600℃),富钙生物油中残留高分子碳氢化物沉积效应与有机气体释放产生气释作用共存,但沉积效应占主导,导致富钙生物油煅烧产物孔隙特性随温度的增加反而下降。然而即使如此,富钙生物油煅烧产物孔隙还是优于同等条件下CaCO3煅烧产物。
富钙生物油热重反应器与小型固定床反应器上脱硫结果显示,富钙生物油最佳脱硫温度应该在900℃左右,富钙生物油脱硫反应可以被分成三个阶段：分别为表面脱硫阶段、二氧化硫缓慢扩散阶段、反应中止阶段。二氧化硫缓慢扩散阶段在富钙生物油脱硫反应中起决定性的作用。采用晶粒模型模拟了富钙生物油脱硫过程,模拟过程与实验结果比较吻合。然后用主成分分析法建立的综合评价方法评估了富钙生物油脱硫反应活性,结果表明,富钙生物油脱硫性能主要由孔隙率、CaO含量、比表面积与平均孔径比值决定。
在小型反应器上进行了富钙生物油同时脱硫脱硝研究,实验结果表明,钙生物油脱硫效率在900～950℃内取得最大值,为90%左右。脱硝效率在1200～1250℃内达到最大值,为50%左右。富钙生物油同时脱硫脱硝钙硫比在2～3之间较为适宜。贫氧气氛下有利于富钙生物油同时脱硫脱硝效率的提高。相同实验条件下,三种钙基同时脱硫脱硝性能大小顺序为富钙生物油>醋酸钙>石灰石。石灰石粒径越小越有利于制备出的富钙生物油脱硫脱硝,pH较小、酸性较强生物油也有利于富钙生物油脱硫脱硝效率的提高,制备温度的提高也可增加富钙生物油脱硫的性能,在50℃左右制备富钙生物油即可。
对富钙生物油再燃脱硝过程进行了数值模拟,结果表明温度和氧量是影响富钙生物油还原NOx的主要因素。在贫氧情况下有利于富钙生物油NOx还原效率的提高,而温度对富钙生物油还原NOx效率的影响程度与过量空气系数有关,过量空气系数在0.6～0.8,温度在1100～1400℃范围内,是富钙生物油理想脱硝区间。富钙生物油再燃脱硝分为两个阶段,在快速反应阶段,富钙生物油煅烧过程中生成的CH2CO继续分解为H、HO2, HCCO等物质,降低了NOx的浓度。而在沿程反应阶段,NO的还原主要以反应式H+NO+M=>HNO+M为主。
Coal-fired power plants are the primary sources of SO2 and NOx emissions. With the increasingly stringent environmental requirements, the simultaneous removal of SO2 and NOx from coal-fired power plant has been imperatived.
Spraying limestone inside furnace is the most commonly method to reduce SO2 emissions in china numerous small and medium-sized industrial coal-fired boilers. But desulfurization by limestone has the disadvantage of low desulfurization efficiency and the problem that can not denitration simultaneously. Researches abroad indicated that organic calcium salts (such as calcium acetate) had high desulfurization efficiency and certain denitration efficiency simultaneously, which were very suitable for coal-fired boilers absorbents. But a large number of organic acids will be need for preparing organic acids calcium salts, and the cost of producing organic acids is too high, which causes the fact that this method is still in academic research stage.
The bio-oil can be obtained easily by rapid pyrolysis of any kind of biomass in the absence of oxygen. The bio-oil mainly contains acetic acid, formic acid, propionic acid and a small amount of benzoic acid, which can react with Ca(OH)2 or CaCO3 and the product contains numerous organic acids calcium salts, which called" calcium-enriched bio-oil(CEB)". It can be act as a succedaneum for organic acids calcium salts.
This paper focuses on the novel organic calcium "calcium-enriched bio-oil(CEB)", which is capable of desulfurization and denitrification simultaneously. The effect principles of factors on preparating of CEB were investigated firstly. Limestone particle size and pH value of bio-oil and reaction temperature were investigated during the process of CEB preparation. Bio-oil pH value and reaction temperature play a key role in the process, the smaller pH value of bio-oil and high temperature are conducive to increase calcium concentration. The results of CEB components analysis indicated that CEB mainly contain Ca, H, O, C. The test results of CEB molecular structure showed that CEB mainly contain organic acids calcium salts, but also containing alcohol, benzene, phenol and other substances.
The calcination process of CEB was investigated by thermogravimetric analyzer, the results showed that CEB calcination process could be divided into four stages, which were dehydration of CEB, CO2 and H2O precipitation from part component of bio-oil, decomposition of organic carboxylic acid calcium salt, decomposition of calcium carbonate respectively. Heating rate and particle size had little effect on CEB decomposition processes, but CO2 had significantly inhibitory effect on CEB decomposition processes. The kinetics of the second and third stage was studied, and the kinetic parameters were calculated. The mechanism functions were also determined by both the universal integral method and the differential equation method. The results indicate that the shrinking cylinder model with surface reaction rate controlling mechanism was the model fitting the latter two stages during CEB calcination process. The calcium oxide particles obtained from decomposition and calcination of CEB were analyzed by different methods to determine their physicochemical characteristics. Pore structure parameters indicated that decomposition of organic carboxylic acid calcium salt had important influences on product pore structure. The cavitations effected by gas precipitation and carbonization deposition phenomenon of macromolecular compound coexist in the range of 450～600℃, but the latter dominated. The carbonization deposition phenomenon of macromolecular compound mainly occurred in the range of 500～600℃. After 600℃, with the decomposition of calcium carbonate and carbon dioxide release, new micropores had been formed in calcined product. Under the same calcination temperature the pore characteristics of CEB calcined product obviously superior to calcium carbonate.
CEB desulfurization process was investigated on thermogravimetric analyzer and a small fixed bed reactor. The results showed that CEB desulfurization temperature should be the best around at 900℃, and CEB desulfurization process could be divided into three stages:surface desulfurization, sulfur dioxide slow diffusion stage and the reaction suspension stage. Slow diffusion phase of sulfur dioxide plays a decisive role in CEB desulfurization process. Grain model had been used to simulate CEB desulfurization process, and simulant results in good agreement with the experimental results. Then evaluation method established by principal component analysis was used to assess the reaction activity of CEB desulfurization, the results showed that CEB desulfurization performance mainly decided by the CaO content, the ratio of specific surface area and average pore size, porosity.
CEB desulfurization and denitrification simultaneously was was investigated on a small fixed bed reactor. The reuslts showed that during CEB desulfurization process SO2 precipitation decline with temperature increasing in initial combustion stage, SO2 precipitation increase with temperature increasing in late combustion stage. SO2 precipitation peak gradually moves up with the increase of excess air ratio. The active group CHi generated by the decomposition of organic gases during CEB calcination process had obvious reduction effect to NOx first precipitation peak, while the CaO formed by CEB calcination process had a dual role on NOx second precipitation peak.1150℃was the appropriate temperature for CEB denitrification; poor oxygen atmosphere was conducive to CEB denitrification efficiency.
CEB reburning process was simulated, the results showed that the temperature and atmosphere were major factors on NOx reduction; poor oxygen condition was conducive to CEB denitrification efficiency. While the effect of the temperature related with excess air ratio, excess air ratio of 0.6 to 0.8 and the temperature in the range of 1100～1400℃were idea condition for CEB denitrification. CEB reburning process could be divided into two stages, in the rapid response stage, CH2CO generated during CEB calcination process continue to decompose as H, HO2, HCCO, which reduce the NOx concentration.
炉内喷钙是我国众多中小型燃煤机组及工业锅炉常用的脱硫方式,脱硫剂采用石灰石。然而石灰石脱硫存在着钙利用率低、脱硫效率不高和无法同时脱硝等问题。国外研究表明有机酸钙盐(如乙酸钙等)在具有较高的脱硫能力的同时,还具备一定的脱硝能力,非常适合用于燃煤锅炉污染物的脱除。然而制备有机酸钙盐需要大量有机酸,而有机酸生产成本太高,这限制了有机酸在工业上的应用,所以此种方法目前还停留在理论研究阶段。
生物油中含有丰富的有机酸,将其与钙基吸收剂反应可制备出在一种富含有机酸钙盐的“富钙生物油”,可用于有机酸钙盐的替代品,从而解决有机钙盐生产成本过高的问题。
本文以富钙生物油为研究对象,首先对富钙生物油制备过程的影响因素作用规律进行了研究,考察了石灰石粒径、生物油pH值、反应温度对富钙生物油的制备过程的影响,指出生物油pH值与反应温度在制备富钙生物油过程中起着关键的作用,较小pH值的生物油与较高的反应温度有利于富钙生物油中钙离子浓度的增加。对制备出的富钙生物油成分分析表明,富钙生物油中主要含有Ca、H、O、C等元素,富钙生物油中除有机羧酸钙盐外,还含有醇、苯、酚类等物质。
对富钙生物油煅烧过程进行了研究,表明富钙生物油的煅烧可以分为四个阶段。第一阶段是<200℃时富钙生物油的脱水阶段,第二阶段是温度在200℃～400℃时,富钙生物油中部分残留生物油的分解析出,也包括部分分解温度较低的有机羧酸钙盐的分解。第三阶段为400℃左右时,富钙生物油的有机羧酸钙盐分解阶段。最后是碳酸钙的分解阶段。随着升温速率的增大,富钙生物油分解的后两个阶段分解起始温度都有所提高。粒径对富钙生物油煅烧特性的影响较小。CO2气氛对富钙生物油碳酸钙分解阶段表现出明显的抑制作用。对富钙生物油后两个阶段分解动力学进行了分析,表明后两个分解阶段符合相边界反应的收缩圆柱体模型。富钙生物油煅烧产物孔结构受其煅烧过程的影响非常明显,特别是有机羧酸钙盐的快速分解阶段,在此温度区间内(400～600℃),富钙生物油中残留高分子碳氢化物沉积效应与有机气体释放产生气释作用共存,但沉积效应占主导,导致富钙生物油煅烧产物孔隙特性随温度的增加反而下降。然而即使如此,富钙生物油煅烧产物孔隙还是优于同等条件下CaCO3煅烧产物。
富钙生物油热重反应器与小型固定床反应器上脱硫结果显示,富钙生物油最佳脱硫温度应该在900℃左右,富钙生物油脱硫反应可以被分成三个阶段：分别为表面脱硫阶段、二氧化硫缓慢扩散阶段、反应中止阶段。二氧化硫缓慢扩散阶段在富钙生物油脱硫反应中起决定性的作用。采用晶粒模型模拟了富钙生物油脱硫过程,模拟过程与实验结果比较吻合。然后用主成分分析法建立的综合评价方法评估了富钙生物油脱硫反应活性,结果表明,富钙生物油脱硫性能主要由孔隙率、CaO含量、比表面积与平均孔径比值决定。
在小型反应器上进行了富钙生物油同时脱硫脱硝研究,实验结果表明,钙生物油脱硫效率在900～950℃内取得最大值,为90%左右。脱硝效率在1200～1250℃内达到最大值,为50%左右。富钙生物油同时脱硫脱硝钙硫比在2～3之间较为适宜。贫氧气氛下有利于富钙生物油同时脱硫脱硝效率的提高。相同实验条件下,三种钙基同时脱硫脱硝性能大小顺序为富钙生物油>醋酸钙>石灰石。石灰石粒径越小越有利于制备出的富钙生物油脱硫脱硝,pH较小、酸性较强生物油也有利于富钙生物油脱硫脱硝效率的提高,制备温度的提高也可增加富钙生物油脱硫的性能,在50℃左右制备富钙生物油即可。
对富钙生物油再燃脱硝过程进行了数值模拟,结果表明温度和氧量是影响富钙生物油还原NOx的主要因素。在贫氧情况下有利于富钙生物油NOx还原效率的提高,而温度对富钙生物油还原NOx效率的影响程度与过量空气系数有关,过量空气系数在0.6～0.8,温度在1100～1400℃范围内,是富钙生物油理想脱硝区间。富钙生物油再燃脱硝分为两个阶段,在快速反应阶段,富钙生物油煅烧过程中生成的CH2CO继续分解为H、HO2, HCCO等物质,降低了NOx的浓度。而在沿程反应阶段,NO的还原主要以反应式H+NO+M=>HNO+M为主。
Coal-fired power plants are the primary sources of SO2 and NOx emissions. With the increasingly stringent environmental requirements, the simultaneous removal of SO2 and NOx from coal-fired power plant has been imperatived.
Spraying limestone inside furnace is the most commonly method to reduce SO2 emissions in china numerous small and medium-sized industrial coal-fired boilers. But desulfurization by limestone has the disadvantage of low desulfurization efficiency and the problem that can not denitration simultaneously. Researches abroad indicated that organic calcium salts (such as calcium acetate) had high desulfurization efficiency and certain denitration efficiency simultaneously, which were very suitable for coal-fired boilers absorbents. But a large number of organic acids will be need for preparing organic acids calcium salts, and the cost of producing organic acids is too high, which causes the fact that this method is still in academic research stage.
The bio-oil can be obtained easily by rapid pyrolysis of any kind of biomass in the absence of oxygen. The bio-oil mainly contains acetic acid, formic acid, propionic acid and a small amount of benzoic acid, which can react with Ca(OH)2 or CaCO3 and the product contains numerous organic acids calcium salts, which called" calcium-enriched bio-oil(CEB)". It can be act as a succedaneum for organic acids calcium salts.
This paper focuses on the novel organic calcium "calcium-enriched bio-oil(CEB)", which is capable of desulfurization and denitrification simultaneously. The effect principles of factors on preparating of CEB were investigated firstly. Limestone particle size and pH value of bio-oil and reaction temperature were investigated during the process of CEB preparation. Bio-oil pH value and reaction temperature play a key role in the process, the smaller pH value of bio-oil and high temperature are conducive to increase calcium concentration. The results of CEB components analysis indicated that CEB mainly contain Ca, H, O, C. The test results of CEB molecular structure showed that CEB mainly contain organic acids calcium salts, but also containing alcohol, benzene, phenol and other substances.
The calcination process of CEB was investigated by thermogravimetric analyzer, the results showed that CEB calcination process could be divided into four stages, which were dehydration of CEB, CO2 and H2O precipitation from part component of bio-oil, decomposition of organic carboxylic acid calcium salt, decomposition of calcium carbonate respectively. Heating rate and particle size had little effect on CEB decomposition processes, but CO2 had significantly inhibitory effect on CEB decomposition processes. The kinetics of the second and third stage was studied, and the kinetic parameters were calculated. The mechanism functions were also determined by both the universal integral method and the differential equation method. The results indicate that the shrinking cylinder model with surface reaction rate controlling mechanism was the model fitting the latter two stages during CEB calcination process. The calcium oxide particles obtained from decomposition and calcination of CEB were analyzed by different methods to determine their physicochemical characteristics. Pore structure parameters indicated that decomposition of organic carboxylic acid calcium salt had important influences on product pore structure. The cavitations effected by gas precipitation and carbonization deposition phenomenon of macromolecular compound coexist in the range of 450～600℃, but the latter dominated. The carbonization deposition phenomenon of macromolecular compound mainly occurred in the range of 500～600℃. After 600℃, with the decomposition of calcium carbonate and carbon dioxide release, new micropores had been formed in calcined product. Under the same calcination temperature the pore characteristics of CEB calcined product obviously superior to calcium carbonate.
CEB desulfurization process was investigated on thermogravimetric analyzer and a small fixed bed reactor. The results showed that CEB desulfurization temperature should be the best around at 900℃, and CEB desulfurization process could be divided into three stages:surface desulfurization, sulfur dioxide slow diffusion stage and the reaction suspension stage. Slow diffusion phase of sulfur dioxide plays a decisive role in CEB desulfurization process. Grain model had been used to simulate CEB desulfurization process, and simulant results in good agreement with the experimental results. Then evaluation method established by principal component analysis was used to assess the reaction activity of CEB desulfurization, the results showed that CEB desulfurization performance mainly decided by the CaO content, the ratio of specific surface area and average pore size, porosity.
CEB desulfurization and denitrification simultaneously was was investigated on a small fixed bed reactor. The reuslts showed that during CEB desulfurization process SO2 precipitation decline with temperature increasing in initial combustion stage, SO2 precipitation increase with temperature increasing in late combustion stage. SO2 precipitation peak gradually moves up with the increase of excess air ratio. The active group CHi generated by the decomposition of organic gases during CEB calcination process had obvious reduction effect to NOx first precipitation peak, while the CaO formed by CEB calcination process had a dual role on NOx second precipitation peak.1150℃was the appropriate temperature for CEB denitrification; poor oxygen atmosphere was conducive to CEB denitrification efficiency.
CEB reburning process was simulated, the results showed that the temperature and atmosphere were major factors on NOx reduction; poor oxygen condition was conducive to CEB denitrification efficiency. While the effect of the temperature related with excess air ratio, excess air ratio of 0.6 to 0.8 and the temperature in the range of 1100～1400℃were idea condition for CEB denitrification. CEB reburning process could be divided into two stages, in the rapid response stage, CH2CO generated during CEB calcination process continue to decompose as H, HO2, HCCO, which reduce the NOx concentration.
引文
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