机械力化学法制备活性炭的研究
发布时间：2018-07-14 07:11
【摘要】：本文以杉木屑为原料,分别采用机械力化学磷酸法、氯化锌法和助活化剂(磷酸-硝酸钾)法制备了高吸附性能的活性炭。依据响应面法原理,使用Design-Expert软件的筛选重要因子设计(Plackett-Burman Design) (PBD)模式和中心组合设计(Box-Behnken Design) (BBD)模式、中心复合设计(Central Composite Design) (CCD)模式和建立试验数学模型,对机械力化学法制备活性炭的有关影响因素进行试验优化设计,并进行试验验证分析,探讨了影响机械力化学法活性炭孔隙结构和碘吸附值、亚甲基蓝吸附值等各种制备因素,确定了制备活性炭的最佳工艺条件。 对于机械力化学技术磷酸法制备活性炭,对碘吸附值模型的预测值与试验真实值之间的相关性为98.66%,该模型能够解释97.31%的响应值变化,说明模型拟合程度良好；得出的最佳制备工艺参数为：酸屑比2.00,研磨时间22.00 min,活化温度406.00℃,磷酸浓度20.00%,活性炭的碘吸附值达到1331.23mg/g。对于亚甲基蓝模型的决定系数为0.9910,调整系数为0.9820,最佳制备工艺条件为：酸屑比2.60,研磨时间29.00 min,活化温度390.00℃,磷酸浓度22.50%,制得的活性炭样品的亚甲基蓝吸附值为21.50ml/0.1g。 机械力化学技术氯化锌法制备活性炭,碘吸附值模型的预测值与试验真实值之间的相关性为99.38%,该模型解释了98.79%的响应值变化,表明该模型有良好的拟合程度；最佳制备工艺条件为：锌屑比2.70,研磨时间34.00min,活化温度593.00℃,活化时间1.90 h,活性炭的碘吸附值为1189.23mg/g。对于亚甲基蓝模型的决定系数为0.9927,调整系数为0.9858,最佳制备工艺条件是：锌屑比1.80,研磨时间22.00 min,活化温度672.00℃,活化时间1.22 h,活性炭的亚甲基蓝吸附值为24.30ml/0.1g。 机械力化学技术助活化剂(磷酸-硝酸钾)法制备活性炭,碘吸附值模型的预测值与试验真实值之间的相关性达97.99%,该模型能解释96.12%响应值的变化,说明模型拟合较好；酸屑比为2.60,助剂用量为14.00%,研磨时间为19.00min,磷酸浓度为15.00%,活化温度400.00℃,活化时间60.00 min时,活性炭的碘吸附值达到1007.86mg/g。亚甲基蓝吸附值模型的预测值与试验真实值之间的相关性为98.65%,该模型解释了97.40%的响应值变化,该模型有良好的拟合程度；在酸屑比为2.60,助剂用量为9.00%,研磨时间为40.00min,磷酸浓度为23.00%,活化温度400.00℃,活化时间60.00min时时活性炭的亚甲基蓝吸附值为23.00ml/0.1g。 通过对三种活性炭制备方法最优条件下碘值和亚甲基蓝的吸附值的对比发现,采用机械力化学技术磷酸法制备活性炭时,活性炭的碘吸附值最大,为1331.23mg/g；机械力化学技术助活化剂(磷酸-硝酸钾)法制备活性炭时,活性炭的亚甲基蓝吸附值最大,为24.30ml/0.1g。 另一方面,对上述制备的活性炭用比表面积及孔隙分析仪、扫描电子显微镜(SEM)、傅立叶红外光谱仪(FT-IR)等作进一步表征,为机械力化学法制备高性能活性炭提供了理论依据。
[Abstract]:The high adsorption activated carbon was prepared by mechanical chemical phosphoric acid method, zinc chloride method and activator (phosphoric acid nitrate). According to the principle of response surface method, the selection of important factor design (Plackett-Burman Design) (PBD) model and central combination design (Box-Behnken De) based on the principle of response surface method (Design-Expert software) Sign) (BBD) mode, the Central Composite Design (CCD) model and the establishment of the experimental mathematical model, the influence factors of the active carbon prepared by the mechanochemical method are optimized. The experimental verification and analysis are carried out. The pore structure of the activated carbon and the iodine adsorption value of the mechanochemical method and the methylene blue absorption are discussed. The optimum conditions for the preparation of activated carbon were determined by various preparation factors.
The correlation between the predicted value of the iodine adsorption value model and the true value of the test is 98.66% for the preparation of activated carbon by the mechanical chemical technology phosphoric acid method. The model can explain the change of the response value of 97.31%, indicating the good fitting degree of the model, and the optimum preparation parameters are as follows: the acid chip ratio is 2, the grinding time is 22 min, and the activation temperature is 40. At 6 C, the concentration of phosphoric acid is 20%. The adsorption value of activated carbon is reached to 1331.23mg/g. for the methylene blue model and the adjustment coefficient is 0.9820. The optimum preparation conditions are as follows: the acid chip ratio 2.60, the grinding time 29 min, the activation temperature 390, and the phosphoric acid concentration 22.50%, and the methylene blue adsorption value of the activated carbon samples is 2. 1.50ml/0.1g.
The relationship between the predicted value of iodine adsorption value model and the true value of the test is 99.38%. The model explains the change of the response value of 98.79%, which shows that the model has a good fitting degree, and the optimum preparation process is as follows: the ratio of the zinc chip ratio is 2.70, the grinding time is 34.00min, and the activation temperature is 593 C. The activation time is 1.90 h, the iodine adsorption value of activated carbon is 1189.23mg/g. for the methylene blue model, the coefficient of determination is 0.9927, the adjustment coefficient is 0.9858. The optimum preparation conditions are: the zinc chip ratio 1.80, the grinding time 22 min, the activation temperature 672, 1.22 h, and the methylene blue adsorption value of active carbon is 24.30ml/0.1g.
Mechanical chemical technology is used to prepare activated carbon by activating agent (phosphoric acid nitrate) method. The correlation between the predicted value of iodine adsorption value model and the true value of the test is 97.99%. This model can explain the change of 96.12% response value, which shows that the model fit well, the ratio of the acid chip is 2.60, the dosage of auxiliary is 14%, the grinding time is 19.00min, and the concentration of phosphoric acid is 15. When the activation temperature is 400 C and the activation time is 60 min, the correlation between the iodine adsorption value of activated carbon and the model of 1007.86mg/g. methylene blue adsorption value and the true value of the test is 98.65%. The model explains the change of the response value of 97.40%, the model has a good degree of fitting, the ratio of the acid chips is 2.60, the additive dosage is 9%. When the grinding time is 40.00min, the phosphoric acid concentration is 23%, the activation temperature is 400 C, and the activation time is 60.00min, the methylene blue adsorption value of activated carbon is 23.00ml/0.1g.
By comparing the adsorption values of the iodine value and Ya Jiaji blue under the optimum conditions of three activated carbons, it is found that when the activated carbon is prepared by the mechanical chemical technology phosphoric acid method, the adsorption value of the active carbon is the largest, which is 1331.23mg/g. When the activated carbon is prepared by the mechanochemical technology (phosphoric acid potassium nitrate), the active carbon is Ya Jiaji. Blue adsorption value is the largest, 24.30ml/0.1g.
On the other hand, the specific surface area and pore analyzer, scanning electron microscope (SEM) and Fu Liye infrared spectrometer (FT-IR) were used to characterize the activated carbon prepared above, which provided a theoretical basis for the preparation of high performance activated carbon by mechanochemical method.
【学位授予单位】：福建农林大学
【学位级别】：硕士
【学位授予年份】：2011
【分类号】：TQ424.14
本文编号：2120879
[Abstract]:The high adsorption activated carbon was prepared by mechanical chemical phosphoric acid method, zinc chloride method and activator (phosphoric acid nitrate). According to the principle of response surface method, the selection of important factor design (Plackett-Burman Design) (PBD) model and central combination design (Box-Behnken De) based on the principle of response surface method (Design-Expert software) Sign) (BBD) mode, the Central Composite Design (CCD) model and the establishment of the experimental mathematical model, the influence factors of the active carbon prepared by the mechanochemical method are optimized. The experimental verification and analysis are carried out. The pore structure of the activated carbon and the iodine adsorption value of the mechanochemical method and the methylene blue absorption are discussed. The optimum conditions for the preparation of activated carbon were determined by various preparation factors.
The correlation between the predicted value of the iodine adsorption value model and the true value of the test is 98.66% for the preparation of activated carbon by the mechanical chemical technology phosphoric acid method. The model can explain the change of the response value of 97.31%, indicating the good fitting degree of the model, and the optimum preparation parameters are as follows: the acid chip ratio is 2, the grinding time is 22 min, and the activation temperature is 40. At 6 C, the concentration of phosphoric acid is 20%. The adsorption value of activated carbon is reached to 1331.23mg/g. for the methylene blue model and the adjustment coefficient is 0.9820. The optimum preparation conditions are as follows: the acid chip ratio 2.60, the grinding time 29 min, the activation temperature 390, and the phosphoric acid concentration 22.50%, and the methylene blue adsorption value of the activated carbon samples is 2. 1.50ml/0.1g.
The relationship between the predicted value of iodine adsorption value model and the true value of the test is 99.38%. The model explains the change of the response value of 98.79%, which shows that the model has a good fitting degree, and the optimum preparation process is as follows: the ratio of the zinc chip ratio is 2.70, the grinding time is 34.00min, and the activation temperature is 593 C. The activation time is 1.90 h, the iodine adsorption value of activated carbon is 1189.23mg/g. for the methylene blue model, the coefficient of determination is 0.9927, the adjustment coefficient is 0.9858. The optimum preparation conditions are: the zinc chip ratio 1.80, the grinding time 22 min, the activation temperature 672, 1.22 h, and the methylene blue adsorption value of active carbon is 24.30ml/0.1g.
Mechanical chemical technology is used to prepare activated carbon by activating agent (phosphoric acid nitrate) method. The correlation between the predicted value of iodine adsorption value model and the true value of the test is 97.99%. This model can explain the change of 96.12% response value, which shows that the model fit well, the ratio of the acid chip is 2.60, the dosage of auxiliary is 14%, the grinding time is 19.00min, and the concentration of phosphoric acid is 15. When the activation temperature is 400 C and the activation time is 60 min, the correlation between the iodine adsorption value of activated carbon and the model of 1007.86mg/g. methylene blue adsorption value and the true value of the test is 98.65%. The model explains the change of the response value of 97.40%, the model has a good degree of fitting, the ratio of the acid chips is 2.60, the additive dosage is 9%. When the grinding time is 40.00min, the phosphoric acid concentration is 23%, the activation temperature is 400 C, and the activation time is 60.00min, the methylene blue adsorption value of activated carbon is 23.00ml/0.1g.
By comparing the adsorption values of the iodine value and Ya Jiaji blue under the optimum conditions of three activated carbons, it is found that when the activated carbon is prepared by the mechanical chemical technology phosphoric acid method, the adsorption value of the active carbon is the largest, which is 1331.23mg/g. When the activated carbon is prepared by the mechanochemical technology (phosphoric acid potassium nitrate), the active carbon is Ya Jiaji. Blue adsorption value is the largest, 24.30ml/0.1g.
On the other hand, the specific surface area and pore analyzer, scanning electron microscope (SEM) and Fu Liye infrared spectrometer (FT-IR) were used to characterize the activated carbon prepared above, which provided a theoretical basis for the preparation of high performance activated carbon by mechanochemical method.
【学位授予单位】：福建农林大学
【学位级别】：硕士
【学位授予年份】：2011
【分类号】：TQ424.14
【引证文献】
相关硕士学位论文 前1条
1 王彦威;茶叶基功能性吸附材料的研究[D];福建农林大学;2012年
，本文编号：2120879
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