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碳基脱硫剂的制备和常低温下脱硫性能研究
论文作者:童鞋论文网  论文来源:www.txlunwenw.com  发布时间:2019/10/26 13:30:15  

摘要:本文采用稻壳活性炭为原料,通过活化制备了改性活性炭,并对 改性前后的比表面积、孔体积、孔径进行分析对比。结果表明,改性后,比表面积、微孔体积分别提升了 33.0 和 34.6 倍,含氧基团含量提升,羧基团含量提升 7.67 倍,酚羟基团含量提升 4.92 倍,内脂基团含量提升 5.87 倍。探究了不同活化方法、活化剂种类、活化剂浓 度、焙烧温度对于脱除 CS2性能的影响。当焙烧温度为 650 ℃,采用 分步法,活化剂选用 1mol/L 的 K2CO3时,脱除CS2硫容最佳,达到 了 21.0mg/g。制备过程中生物质分解,产生挥发气体造成稻壳失重, 最终失重率为 81.87%。 采用浸渍法制备了碳基脱硫剂。考察了浸渍液体积、Cu 活性物负载量、焙烧温度、水汽含量、脱硫温度对于吸附 CS2性能的影响。 活化后,比表面积下降,微孔体积下降,孔径分布以 0.5-1nm 为主。 采用等体积浸渍法,负载量为 5%,焙烧温度为 500 ℃, 水汽浓度为 6.8g/cm3, 脱硫温度40 ℃时, 吸附CS2性能最佳,硫容达到43.3mg/g。 采用恒温均相沉淀、氮气氛围下羟基氧化铁法、室温直接沉淀法 制备了三种碳基脱硫剂,直接沉淀法脱除 H2S 效果最佳,制备得到的 碳基脱硫剂 BJH 平均孔径最小,为 1.93nm,微孔孔体积最高,达到 了 0.1588mL/g。探究了 Fe 负载量、焙烧温度对于吸附 H2S 性能的影 响。当 Fe 负载量为 40%,焙烧温度为500 ℃,吸附 H2S 性能最佳, 硫容达到了279.90mg/g。随着焙烧温度的上升,脱除 H2S 性能先上 升后下降, 由于载体C的存在, Fe活性物的形态转化为Fe(OH)3、 Fe2O3 无定形态,继续转化为 Fe2O3晶态,在 500 ℃时转化为 Fe2O3晶态和Fe3O4共存。Cu 活性物的形态从 Cu 盐向无定形态 CuO,晶体态 Cu2O 转化,最终转化为 Cu0,造成脱除 H2S 活性的下降。 采用超声分散,制备了 C/ATP 复合载体碳基脱硫剂,可以均匀 混合。通过 XRD、TG、TEM 和 BET 等测试方法探究了 C 和 ATP 比 例、焙烧温度、水汽含量、脱硫温度对于吸附 CS2、COS、H2S 性能的影响。最佳脱硫性能脱硫剂的 C/ATP 比例为 4C:1ATP,CS2、COS、 H2S 硫容达到了 13.45mg/g、56.3mg/g、313.28mg/g。随着焙烧温度的升高,脱除 COS 和 CS2 的性能先升高后下降,最佳焙烧温度为 500 ℃,Fe 活性物以 Fe2O3和 Fe3O4存在、Cu 活性物以Cu2O 形式存 在,600 ℃下脱硫性能不佳的原因 Cu0的出现、凹凸棒土坍塌引起的微孔孔容的下降。最佳水汽含量和脱硫温度分别为 0g/m3和 150 ℃。

使用失活动力学模型可以对数据进行拟合,计算出的模拟硫化过程与 实际硫化过程吻合。制备的复合载体脱硫剂应用于工业尾气脱硫,使用时间为 177 天,可以完全脱除 H2S,控制 COS 浓度在 3ppm 以下。

In this paper, modified activated carbonwas prepared via the activation of rice husk activated carbon, and the specificsurface area, pore volume and pore size before and after the modification wereanalyzed and compared. The results show that after the modification, thespecific surface area and micro pore volume increased 33.0 and 34.6 times, thecontent of oxygen-containing groups increased, the carboxyl group contentincreased 7.67 times, the phenolic hydroxyl group content increased 4.92 times,and the content of lactone groups increased 5.87 times. The effects ofdifferent activation methods, activator types, activator concentrations,andcalcination temperatures onthe performance of CS2 removal were investigated.When the calcination temperature was 650 °C, the stepwise method was adopted,and the chosen activator was 1 mol/L K2CO3, the best sulfur capacity wasdemonstrated on the sulfur removal of CS2, which was 21.0 mg/g. During thepreparation process, the biomass was decomposed, and the generated volatile gasled to the weightlossofthericehusk,andthefinalweightlosswas81.87%. Thecarbon-based desulfurizing agent was prepared via the impregnation method. Theeffects of impregnation volume, Cu active loading, calcination temperature,water vapor content and reaction temperature onthe performance of CS2adsorptionwere studied.After the activation,thespecificsurfacearea decreased,theporevolumedecreased, and the pore size distribution was mainly 0.5-1 nm.When the isovolumetric impregnation was applied, the loading was 5%, thecalcination temperature was 500 °C, the water vapor concentration was 6.8g/cm3, and the reaction temperature was 40 °C, the CS2 adsorptionwasthebestandthesulfurcapacityreached43.3mg/g. Three types of carbon-baseddesulfurizers were synthesized via constant temperature homogeneousprecipitation, hydroxyl iron oxide method under nitrogen atmosphere and roomtemperature direct

precipitation. The direct precipitationmethod is the best to remove H2S; the preparedcarbon-baseddesulfurizer BJH hasthesmallest average pore sizeof1.93nm,andthelargestmicroporevolumereaching0.1588mL/g. The effects of Fe loading andcalcination temperature on the H2S adsorption performance were inspected. TheH2S adsorption performance was the best, and the sulfur capacity reached 279.90mg/g when the Fe loading was 40% and the calcination temperature was 500 °C.With the increase of the calcination temperature, the H2S removal performancefirst rose and then decreased. Due to the presence of the support C, the formofactiveFewasconvertedfromFesalttoFe(OH)3,thenamorphousFe2O3, and further into Fe2O3 crystalline state, at 500 °C it was convertedinto Fe2O3 crystalline form which coexisted with Fe3O4. The active Cu wastransformed from Cu salt to amorphous CuO, further to crystalline Cu2O, andeventually to Cu0, resulting in a decrease of H2S removal activity. The C/ATPcomposite supported carbon-based desulfurizer was prepared via ultrasonicdispersion and then mixed uniformly. The effects of C and ATP ratio, calcinationtemperature, water vapor content and reaction temperature on the CS2, COS andH2S adsorption properties were investigated by XRD, TG, TEM and BET. Theoptimum desulfurizationperformanceof thedesulfurizer was achievedwithC/ATPratio of 4C: 1ATP, the sulfur capacity of CS2, COS, H2S reached 13.45 mg/g,56.3 mg/g, 313.28 mg/g, respectively. As the calcination temperature increased,the performance of COS and CS2 removal increased first and then decreased, theoptimum calcination temperature was 500 °C, active Fe existed as Fe2O3 andFe3O4, active Cu was in the form of Cu2O, and the poor desulfurizationperformance at 600 °C was due to the appearance of Cu0 and the decrease of thepore volume caused by the collapse of the attapulgite clay. The optimum watervapor content and reaction temperature were 0 g/m3 and 150 °C, respectively.

关键词:碳基脱硫剂;Fe;复合载体;工业尾气脱硫

Carbon-based desulfurizer;Fe;composite carrier;Industrialendgasdesulfurization

上一篇:低温铁基复合脱硫剂的制备及脱硫性能研究     下一篇:提高MFC产电量及阳极电子传递机制的研究
 
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