高脱色竹质活性炭的复合工艺制备及性能表征
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摘要
活性炭是一种具有丰富孔结构、高吸附能力、高表面活性的吸附剂,它是利用含碳材料作为原料,通过物理或化学方法对原料进行活化得到的。随着人们环保意识的增强,活性炭应用领域愈来愈广、需求量越来越大,对活性炭的吸附性能要求也越来越高,寻求一种廉价、易得的原料通过新活化工艺制得高脱色性能活性炭成为迫切要求。竹子不仅具有生长周期短,而且我国具有丰富的竹类资源,且其废弃物没有得到很好的利用将会造成污染,将其加以开发利用具有极大的经济效益和社会效益。
本文根据工业上成熟的化学活化法,采用磷酸活化与氯化锌活化结合、磷酸活化与氢氧化钾活化结合的两步法复合工艺制备竹质活性炭。考察制备工艺条件对活性炭产品表面结构和吸附性能的影响,研究了浸渍时间、浸渍率、活化温度、活化时间对产品亚甲基蓝脱色力、碘吸附值、焦糖脱色力的影响,从而获得磷酸活化与氯化锌活化结合、磷酸活化与氢氧化钾活化结合的两步法的最佳工艺条件。并且分析比较了不同复合工艺最佳产品的比表面积、孔隙结构、孔径分布、表面结构、官能团和吸附等温线的情况。
实验结果表明,采用磷酸活化与氯化锌活化结合的两步法复合工艺制备竹质活性炭最佳制备工艺为浸渍率150%,第一步磷酸活化温度500℃、活化时间30min,第二步氯化锌活化温度400℃、活化时间30min。采用磷酸活化与氢氧化钾活化结合的两步法复合工艺制备竹质活性炭最佳制备工艺为第一步浸渍率100%,磷酸活化温度400℃、活化时间30min,第二步浸渍率300%,氢氧化钾活化温度700℃、活化时间15min。第二步采用氢氧化钾为活化剂制备的活性炭具有丰富的微孔结构和巨大的比表面积2279m~2/g,对染料废水的吸附性能也最好,而第二步采用氯化锌为活化剂制备的活性炭具有丰富的微、中孔结构和较宽的孔结构,并且对焦糖脱色优于第二步采用氢氧化钾为活化剂制备的活性炭。
采用两种活化法结合的复合制备工艺制得的活性炭都有丰富的表面官能团,并且对染料废水都有较好的脱色吸附能力。磷酸与氯化锌活化法结合制备样品HZ5433150以及磷酸与氢氧化钾活化法结合制备样品HK8在酸性品红染料废水中的平衡时间分别为250min和100min,当平衡浓度为140mg/L时,饱和吸附量分别为100mg/g和172mg/g,样品的吸附等温线用Freundlich模型比Langmuir模型能更好地拟合实验值。在碱性品红废水中样品的平衡时间分别为500min和400min,当平衡浓度为100mg/L时,饱和吸附量分别为180mg/g和280mg/g,样品的吸附等温线用Langmuir模型比Freundlich模型能更好地拟合实验值。
两步法复合制备工艺制备竹质活性炭,在工艺或者性能上都比采用单一活化法有了较大的改进。
The activated carbon is a kind of sorbent with abundant porosity, high adsorption capability and high surface activity. It is made from carbon raw material and can be produced through physical or chemical activation methods. The activated carbon is applied extensively in chemical industry and generally the application related to the activated carbon needs large amount of activated carbon. Since the application demand of activated carbon becomes higher, the low-priced raw material and the new activation method to prepare activated carbon with better capability become important. The bamboo can be used as the raw material because of its short growth period and abundant resource in Southern China.
The activated carbon is prepared from bamboo sawdust by two-step process method in this thesis. The activated carbon is characterized by methylene blue number, iodine number and caramel decolorization. The optimum preparation conditions such as impregnation time, activation temperature, impregnation ratio and activation time are obtained by detailed experiments. Meanwhile the other properties, such as specific surface area, internal porosity, pore size distribution, functional groups and adsorbing isothermal, are studied in detail by the experiment. The activated carbons are prepared using different activating agents. The optimum preparation conditions corresponding to H_3P0_4 and ZnCl_2 used as activating agent are-H_3P0_4/bamboo sawdust 150%, the impregnation ratio of ZnCl_2/the carbonized material 150%, the activation temperature at first stage 500℃and at second stage 400°C, and the total activation time 60 min. The optimum preparation conditions corresponding to H_3PO_4 and KOH used as activating agent are H_3P0_4/bamboo sawdust 100%, the impregnation ratio of KOH /the carbonized material 300%, the activation temperature at first stage 400℃with activation time 30 min, at second stage 700℃with activation time 15 min. The activated carbon produced by H_3P0_4/ KOH activation method has big porosity and specific surface area, and its adsorption capability to dye wastewater is better. The activated carbon produced by H_3P0_4/ZnCl_2 activation method has abundant micropores and mesopores, and its caramel decolorization capability is better than the former.
To the two kinds of complex preparation methods, both haverich surface function groups and good fading adsorption capability to dye wastewater. The equilibrium time of H_3P0_4/ZnCl_2 and H_3P0_4/K0H sample in the acidic pinkish red dye wastewater is 250 min and 100 min respectively. When the equilibrium concentration is 140 mg/L, the saturated adsorption quantity is 100 mg/g and 172 mg/g respectively. The experimental data on the adsorption equilibrium isotherms of both samples can be fitted well by the Freundlich isotherm equation.
The equilibrium time in the alkalinity pinkish red wastewater are 500min and 400 min respectively corresponding to different activating agents: H_3P0_4/ZnCl_2 and H_3P0_4/K0H. When the equilibrium concentration is 100 mg/L, the saturated adsorption quantity is 180 mg/g and 280 mg/g respectively. The experimental data on the adsorption equilibrium isotherms corresponding to both samples also can be fitted well by the Langmuir isotherm equation.
In general, for the activated carbon made from bamboo, two-step preparation method, technics and adsorption capability are better than one-step activation method through the study in this thesis.
本文根据工业上成熟的化学活化法,采用磷酸活化与氯化锌活化结合、磷酸活化与氢氧化钾活化结合的两步法复合工艺制备竹质活性炭。考察制备工艺条件对活性炭产品表面结构和吸附性能的影响,研究了浸渍时间、浸渍率、活化温度、活化时间对产品亚甲基蓝脱色力、碘吸附值、焦糖脱色力的影响,从而获得磷酸活化与氯化锌活化结合、磷酸活化与氢氧化钾活化结合的两步法的最佳工艺条件。并且分析比较了不同复合工艺最佳产品的比表面积、孔隙结构、孔径分布、表面结构、官能团和吸附等温线的情况。
实验结果表明,采用磷酸活化与氯化锌活化结合的两步法复合工艺制备竹质活性炭最佳制备工艺为浸渍率150%,第一步磷酸活化温度500℃、活化时间30min,第二步氯化锌活化温度400℃、活化时间30min。采用磷酸活化与氢氧化钾活化结合的两步法复合工艺制备竹质活性炭最佳制备工艺为第一步浸渍率100%,磷酸活化温度400℃、活化时间30min,第二步浸渍率300%,氢氧化钾活化温度700℃、活化时间15min。第二步采用氢氧化钾为活化剂制备的活性炭具有丰富的微孔结构和巨大的比表面积2279m~2/g,对染料废水的吸附性能也最好,而第二步采用氯化锌为活化剂制备的活性炭具有丰富的微、中孔结构和较宽的孔结构,并且对焦糖脱色优于第二步采用氢氧化钾为活化剂制备的活性炭。
采用两种活化法结合的复合制备工艺制得的活性炭都有丰富的表面官能团,并且对染料废水都有较好的脱色吸附能力。磷酸与氯化锌活化法结合制备样品HZ5433150以及磷酸与氢氧化钾活化法结合制备样品HK8在酸性品红染料废水中的平衡时间分别为250min和100min,当平衡浓度为140mg/L时,饱和吸附量分别为100mg/g和172mg/g,样品的吸附等温线用Freundlich模型比Langmuir模型能更好地拟合实验值。在碱性品红废水中样品的平衡时间分别为500min和400min,当平衡浓度为100mg/L时,饱和吸附量分别为180mg/g和280mg/g,样品的吸附等温线用Langmuir模型比Freundlich模型能更好地拟合实验值。
两步法复合制备工艺制备竹质活性炭,在工艺或者性能上都比采用单一活化法有了较大的改进。
The activated carbon is a kind of sorbent with abundant porosity, high adsorption capability and high surface activity. It is made from carbon raw material and can be produced through physical or chemical activation methods. The activated carbon is applied extensively in chemical industry and generally the application related to the activated carbon needs large amount of activated carbon. Since the application demand of activated carbon becomes higher, the low-priced raw material and the new activation method to prepare activated carbon with better capability become important. The bamboo can be used as the raw material because of its short growth period and abundant resource in Southern China.
The activated carbon is prepared from bamboo sawdust by two-step process method in this thesis. The activated carbon is characterized by methylene blue number, iodine number and caramel decolorization. The optimum preparation conditions such as impregnation time, activation temperature, impregnation ratio and activation time are obtained by detailed experiments. Meanwhile the other properties, such as specific surface area, internal porosity, pore size distribution, functional groups and adsorbing isothermal, are studied in detail by the experiment. The activated carbons are prepared using different activating agents. The optimum preparation conditions corresponding to H_3P0_4 and ZnCl_2 used as activating agent are-H_3P0_4/bamboo sawdust 150%, the impregnation ratio of ZnCl_2/the carbonized material 150%, the activation temperature at first stage 500℃and at second stage 400°C, and the total activation time 60 min. The optimum preparation conditions corresponding to H_3PO_4 and KOH used as activating agent are H_3P0_4/bamboo sawdust 100%, the impregnation ratio of KOH /the carbonized material 300%, the activation temperature at first stage 400℃with activation time 30 min, at second stage 700℃with activation time 15 min. The activated carbon produced by H_3P0_4/ KOH activation method has big porosity and specific surface area, and its adsorption capability to dye wastewater is better. The activated carbon produced by H_3P0_4/ZnCl_2 activation method has abundant micropores and mesopores, and its caramel decolorization capability is better than the former.
To the two kinds of complex preparation methods, both haverich surface function groups and good fading adsorption capability to dye wastewater. The equilibrium time of H_3P0_4/ZnCl_2 and H_3P0_4/K0H sample in the acidic pinkish red dye wastewater is 250 min and 100 min respectively. When the equilibrium concentration is 140 mg/L, the saturated adsorption quantity is 100 mg/g and 172 mg/g respectively. The experimental data on the adsorption equilibrium isotherms of both samples can be fitted well by the Freundlich isotherm equation.
The equilibrium time in the alkalinity pinkish red wastewater are 500min and 400 min respectively corresponding to different activating agents: H_3P0_4/ZnCl_2 and H_3P0_4/K0H. When the equilibrium concentration is 100 mg/L, the saturated adsorption quantity is 180 mg/g and 280 mg/g respectively. The experimental data on the adsorption equilibrium isotherms corresponding to both samples also can be fitted well by the Langmuir isotherm equation.
In general, for the activated carbon made from bamboo, two-step preparation method, technics and adsorption capability are better than one-step activation method through the study in this thesis.
引文
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