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碳基脫硫劑的制備和常低溫下脫硫性能研究
論文作者:童鞋論文網  論文來源:qaly-analyser.com  發布時間:2019/10/26 13:30:15  

摘要:本文采用稻殼活性炭為原料,通過活化制備了改性活性炭,并對 改性前后的比表面積、孔體積、孔徑進行分析對比。結果表明,改性后,比表面積、微孔體積分別提升了 33.0 和 34.6 倍,含氧基團含量提升,羧基團含量提升 7.67 倍,酚羥基團含量提升 4.92 倍,內脂基團含量提升 5.87 倍。探究了不同活化方法、活化劑種類、活化劑濃 度、焙燒溫度對于脫除 CS2性能的影響。當焙燒溫度為 650 ℃,采用 分步法,活化劑選用 1mol/L 的 K2CO3時,脫除CS2硫容最佳,達到 了 21.0mg/g。制備過程中生物質分解,產生揮發氣體造成稻殼失重, 最終失重率為 81.87%。 采用浸漬法制備了碳基脫硫劑。考察了浸漬液體積、Cu 活性物負載量、焙燒溫度、水汽含量、脫硫溫度對于吸附 CS2性能的影響。 活化后,比表面積下降,微孔體積下降,孔徑分布以 0.5-1nm 為主。 采用等體積浸漬法,負載量為 5%,焙燒溫度為 500 ℃, 水汽濃度為 6.8g/cm3, 脫硫溫度40 ℃時, 吸附CS2性能最佳,硫容達到43.3mg/g。 采用恒溫均相沉淀、氮氣氛圍下羥基氧化鐵法、室溫直接沉淀法 制備了三種碳基脫硫劑,直接沉淀法脫除 H2S 效果最佳,制備得到的 碳基脫硫劑 BJH 平均孔徑最小,為 1.93nm,微孔孔體積最高,達到 了 0.1588mL/g。探究了 Fe 負載量、焙燒溫度對于吸附 H2S 性能的影 響。當 Fe 負載量為 40%,焙燒溫度為500 ℃,吸附 H2S 性能最佳, 硫容達到了279.90mg/g。隨著焙燒溫度的上升,脫除 H2S 性能先上 升后下降, 由于載體C的存在, Fe活性物的形態轉化為Fe(OH)3、 Fe2O3 無定形態,繼續轉化為 Fe2O3晶態,在 500 ℃時轉化為 Fe2O3晶態和Fe3O4共存。Cu 活性物的形態從 Cu 鹽向無定形態 CuO,晶體態 Cu2O 轉化,最終轉化為 Cu0,造成脫除 H2S 活性的下降。 采用超聲分散,制備了 C/ATP 復合載體碳基脫硫劑,可以均勻 混合。通過 XRD、TG、TEM 和 BET 等測試方法探究了 C 和 ATP 比 例、焙燒溫度、水汽含量、脫硫溫度對于吸附 CS2、COS、H2S 性能的影響。最佳脫硫性能脫硫劑的 C/ATP 比例為 4C:1ATP,CS2、COS、 H2S 硫容達到了 13.45mg/g、56.3mg/g、313.28mg/g。隨著焙燒溫度的升高,脫除 COS 和 CS2 的性能先升高后下降,最佳焙燒溫度為 500 ℃,Fe 活性物以 Fe2O3和 Fe3O4存在、Cu 活性物以Cu2O 形式存 在,600 ℃下脫硫性能不佳的原因 Cu0的出現、凹凸棒土坍塌引起的微孔孔容的下降。最佳水汽含量和脫硫溫度分別為 0g/m3和 150 ℃。

使用失活動力學模型可以對數據進行擬合,計算出的模擬硫化過程與 實際硫化過程吻合。制備的復合載體脫硫劑應用于工業尾氣脫硫,使用時間為 177 天,可以完全脫除 H2S,控制 COS 濃度在 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.

關鍵詞:碳基脫硫劑;Fe;復合載體;工業尾氣脫硫

Carbon-based desulfurizer;Fe;composite carrier;Industrialendgasdesulfurization

上一篇:低溫鐵基復合脫硫劑的制備及脫硫性能研究     下一篇:提高MFC產電量及陽極電子傳遞機制的研究
 
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