Preparation of Sucrose Carbide/Sepiolite Composite and the Optimization of Response Surface Methodology
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摘要: 以蔗糖和海泡石为实验原材料，利用水热碳化法制备出新型蔗糖碳化物/海泡石复合材料，冷冻真空干燥法干燥样品。利用XRD、IR、SEM、BET对样品进行表征。以亚甲基蓝作为吸附质，通过单因素和响应面法优化制备的工艺。综合实验结果表明，蔗糖碳化物能够成功的被负载到海泡石表面制备出蔗糖碳化物/海泡石复合材料，其制备最优工艺条件为：蔗糖与海泡石质量比为3.5：1.0，碳化时间为8 h，碳化温度为220℃，对亚甲基蓝的最优吸附量为42.983 mg/g；各因素对复合材料吸附亚甲基蓝性能的影响顺序为：蔗糖与海泡石质量比>碳化时间>碳化温度，并且发现复合材料对亚甲基蓝的吸附效果优于现有的文献报导值。Abstract: Using sucrose and sepiolite as experimental raw materials, a new sucrose carbide/sepiolite composite material was prepared by hydrothermal carbonization method, and the composite material was dried by freeze vacuum drying method. The composite samples were characterized by XRD, IR, SEM and BET, and methylene blue was selected as adsorbate to investigate its adsorption properties. The preparation technical conditions of the composite were optimized by the single factor experiment and the response surface methodology. The results showed that the optimum preparation conditions were as follows. Sucrose carbide could be successfully loaded on the surface of sepiolite to prepare sucrose carbide/sepiolite composite. The optimum adsorption capacity of methylene blue is 42.983 mg/g (composite) with the mass ratio of sucrose to sepiolite of 3.5:1.0, the carbonization time of 8 h, and the carbonization temperature of 220 ℃. The order of the influence of the factors on the adsorption properties of methylene blue was: mass ratio of sucrose to sepiolite > carbonization time > carbonization temperature. It could be found that the adsorption effect of composite materials on methylene blue was superior to the values reported in the existing literature.
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Key words:
- sepiolite /
- sucrose /
- hydrothermal carbonization /
- composite
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表 1 响应面试验因素水平设计表
Table 1. Design table of factors and levels of response surface experiments
Factor Level -1 0 1 A 3.0：1.0 3.5：1.0 4.0：1.0 B/h 4 8 12 C/℃ 210 220 230 
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表 2 响应面试验设计及相对应响应值表
Table 2. Response surface experimental design table and corresponding response values
SN A/(g·g-1) B/h C/℃ Adsorption capacity/(mg·g-1) 1 0 0 0 43.081 7 2 0 -1 1 42.532 3 3 -1 -1 0 42.019 1 4 -1 0 -1 42.243 9 5 0 1 -1 42.793 2 6 1 -1 0 42.123 0 7 1 0 -1 42.333 0 8 1 0 1 42.250 3 9 0 -1 -1 42.547 2 10 0 1 1 42.581 1 11 -1 1 0 41.997 9 12 0 0 0 43.032 9 13 -1 0 1 42.163 3 14 0 0 0 43.005 3 15 0 0 0 43.020 1 16 1 1 0 42.165 4 17 0 0 0 43.035 0
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表 3 响应面试验数据方差分析表
Table 3. Analysis of data variance of response surface experiments
Variance
sourceSum of
squaresdf Mean
squareF value P value Model 2.36 9 0.26 144.48 < 0.0001 significant A 0.069 1 0.069 38.14 0.0005 ** B 0.035 1 0.035 19.20 0.0032 ** C 0.012 1 0.012 6.42 0.0390 * AB 0.019 1 0.019 10.46 0.0144 * AC 0.00171 1 0.00171 0.94 0.3642 BC 0.009722 1 0.009722 5.35 0.0539 A2 1.65 1 1.65 906.01 < 0.0001 ** B2 0.33 1 0.33 182.42 < 0.0001 ** C2 0.084 1 0.084 46.13 0.0003 ** Residual 0.013 7 0.001816 Lack of Fit 0.009423 3 0.003141 3.82 0.1141 Not significant Pure Error 0.003289 4 0.0008224 Cor Total 2.37 16 注：表中*代表显著(P值＜0.05)；**代表极显著(P值＜0.01)。
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表 4 验证试验结果
Table 4. Results of verification experiments
SN Adsorption capacity/(mg·g-1) Average adsorption capacity/(mg·g-1) 1 42.897 2 43.069 42.983 3 42.982
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