機械力化學法制備活性炭的研究
發(fā)布時間：2018-07-14 07:11
【摘要】：本文以杉木屑為原料,分別采用機械力化學磷酸法、氯化鋅法和助活化劑(磷酸-硝酸鉀)法制備了高吸附性能的活性炭。依據(jù)響應(yīng)面法原理,使用Design-Expert軟件的篩選重要因子設(shè)計(Plackett-Burman Design) (PBD)模式和中心組合設(shè)計(Box-Behnken Design) (BBD)模式、中心復合設(shè)計(Central Composite Design) (CCD)模式和建立試驗數(shù)學模型,對機械力化學法制備活性炭的有關(guān)影響因素進行試驗優(yōu)化設(shè)計,并進行試驗驗證分析,探討了影響機械力化學法活性炭孔隙結(jié)構(gòu)和碘吸附值、亞甲基藍吸附值等各種制備因素,確定了制備活性炭的最佳工藝條件。 對于機械力化學技術(shù)磷酸法制備活性炭,對碘吸附值模型的預(yù)測值與試驗真實值之間的相關(guān)性為98.66%,該模型能夠解釋97.31%的響應(yīng)值變化,說明模型擬合程度良好；得出的最佳制備工藝參數(shù)為：酸屑比2.00,研磨時間22.00 min,活化溫度406.00℃,磷酸濃度20.00%,活性炭的碘吸附值達到1331.23mg/g。對于亞甲基藍模型的決定系數(shù)為0.9910,調(diào)整系數(shù)為0.9820,最佳制備工藝條件為：酸屑比2.60,研磨時間29.00 min,活化溫度390.00℃,磷酸濃度22.50%,制得的活性炭樣品的亞甲基藍吸附值為21.50ml/0.1g。 機械力化學技術(shù)氯化鋅法制備活性炭,碘吸附值模型的預(yù)測值與試驗真實值之間的相關(guān)性為99.38%,該模型解釋了98.79%的響應(yīng)值變化,表明該模型有良好的擬合程度；最佳制備工藝條件為：鋅屑比2.70,研磨時間34.00min,活化溫度593.00℃,活化時間1.90 h,活性炭的碘吸附值為1189.23mg/g。對于亞甲基藍模型的決定系數(shù)為0.9927,調(diào)整系數(shù)為0.9858,最佳制備工藝條件是：鋅屑比1.80,研磨時間22.00 min,活化溫度672.00℃,活化時間1.22 h,活性炭的亞甲基藍吸附值為24.30ml/0.1g。 機械力化學技術(shù)助活化劑(磷酸-硝酸鉀)法制備活性炭,碘吸附值模型的預(yù)測值與試驗真實值之間的相關(guān)性達97.99%,該模型能解釋96.12%響應(yīng)值的變化,說明模型擬合較好；酸屑比為2.60,助劑用量為14.00%,研磨時間為19.00min,磷酸濃度為15.00%,活化溫度400.00℃,活化時間60.00 min時,活性炭的碘吸附值達到1007.86mg/g。亞甲基藍吸附值模型的預(yù)測值與試驗真實值之間的相關(guān)性為98.65%,該模型解釋了97.40%的響應(yīng)值變化,該模型有良好的擬合程度；在酸屑比為2.60,助劑用量為9.00%,研磨時間為40.00min,磷酸濃度為23.00%,活化溫度400.00℃,活化時間60.00min時時活性炭的亞甲基藍吸附值為23.00ml/0.1g。 通過對三種活性炭制備方法最優(yōu)條件下碘值和亞甲基藍的吸附值的對比發(fā)現(xiàn),采用機械力化學技術(shù)磷酸法制備活性炭時,活性炭的碘吸附值最大,為1331.23mg/g；機械力化學技術(shù)助活化劑(磷酸-硝酸鉀)法制備活性炭時,活性炭的亞甲基藍吸附值最大,為24.30ml/0.1g。 另一方面,對上述制備的活性炭用比表面積及孔隙分析儀、掃描電子顯微鏡(SEM)、傅立葉紅外光譜儀(FT-IR)等作進一步表征,為機械力化學法制備高性能活性炭提供了理論依據(jù)。
[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.
【學位授予單位】：福建農(nóng)林大學
【學位級別】：碩士
【學位授予年份】：2011
【分類號】：TQ424.14
本文編號：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.
【學位授予單位】：福建農(nóng)林大學
【學位級別】：碩士
【學位授予年份】：2011
【分類號】：TQ424.14
【引證文獻】
相關(guān)碩士學位論文 前1條
1 王彥威;茶葉基功能性吸附材料的研究[D];福建農(nóng)林大學;2012年
，本文編號：2120879
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