蛭石@淀粉碳化物复合材料的制备及优化

杜慧聪; 韦开放; 黄晶晶; 刘云鹤; 王伟; 蓝平; 蓝丽红

doi:10.12476/kczhly.202208260543

蛭石@淀粉碳化物复合材料的制备及优化

广西民族大学化学化工学院，广西多糖材料与改性重点实验室，广西　南宁　530008

基金项目: 国家自然科学基金项目(51464006)；国家级大学生创新训练项目（202010608011）

详细信息

作者简介: 杜慧聪（1997-），女，硕士，蛭石复合材料的制备及应用

通讯作者: 蓝丽红（1972-），女，教授，矿物复合材料制备及应用。

中图分类号: TD985

收稿日期: 2022-08-26

刊出日期: 2025-06-25

Preparation and Optimization of Vermiculite @ Starch Carbide Composites

School of Chemistry and Chemical Engineering, Guangxi Minzu University, Guangxi Key Laboratory of Polysaccharide Materials and Modification, Nanning, Guangxi 530008, China

More Information

Corresponding author: LAN Lihong, lanlihong2004@163.com

Received Date: 26 August 2022

Publish Date: 25 June 2025

摘要

摘要:
以蛭石为基底，以淀粉为碳化源，通过水热碳化法制备了蛭石@淀粉碳化物复合材料，并用扫描电镜(SEM)、红外光谱(FTIR)以及比表面积（BET）对复合材料进行了表征。再以苯酚为吸附剂采用响应面法优化复合材料的制备工艺参数。实验结果表明，蛭石@碳化淀粉复合材料的较佳制备工艺参数为，淀粉与蛭石的质量比 3∶1、碳化时间15 h、碳化温度 200 ℃；较佳吸附量 16.52 mg/g，苯酚的去除率99.13%。复合材料的比表面积比原蛭石稍有下降，变化不大，电镜和红外光谱图表明淀粉碳化物成功的负载在蛭石的表面。
- 蛭石 /
- 淀粉 /
- 复合材料 /
- 制备工艺优化
Abstract:
Vermiculite@starch carbide composites were prepared by hydrothermal carbonization of vermiculite and starch. The prepared composites were washed alternately with deionized water and absolute ethanol. The results of scanning electron microscopy (SEM) and infrared spectroscopy (FTIR) showed that starch carbide was successfully loaded on the surface of vermiculite. The preparation process of the composite was optimized by single factor and response surface method based on the phenol adsorbability index of the composite, and the optimal preparation process parameters were obtained as follows: The mass ratio of starch to vermiculite was 2.97∶1, the carbonization time was 15.66 h, and the carbonization temperature was 196.47 ℃. At these conditions, the composite material has the best adsorption performance for phenol, and its adsorption capacity for phenol is 16.521 mg/g, which is 4.304 mg/g higher than that of natural vermiculite.
- vermiculite /
- starch /
- composite material /
- optimization of preparation process

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图 1 三种材料的SEM

Figure 1.

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图 2 三种材料的FTIR

Figure 2.

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图 3 投加质量比对吸附量的影响

Figure 3.

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图 4 碳化时间对吸附量的影响

Figure 4.

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图 5 碳化温度对吸附量的影响

Figure 5.

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图 6 吸附量实测值与预测值对比

Figure 6.

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图 7 （AB）质量比和碳化时间的恒值线图与3D曲面

Figure 7.

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图 8 （AC）质量比和碳化温度的恒值线图与3D曲面

Figure 8.

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图 9 （BC）碳化时间和碳化温度的恒值线图与3D曲面

Figure 9.

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图 10 投加量对吸附率的影响

Figure 10.

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表 1 实验方案

Table 1. Test scheme

因子	水平
因子	-1	0	1
A	2.5∶1	3.0∶1	3.5∶1
B/h	12	16	20
C/℃	190	200	210

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表 2 实验设计和对应响应值

Table 2. Test design and corresponding response values

序号	A	B/h	C/℃	吸附能力/(mg/g)
1	0	0	0	16.473 4
2	1	0	1	15.183 3
3	0	-1	-1	15.356 2
4	0	0	0	16.280 8
5	1	-1	0	15.701 9
6	1	0	-1	15.280 6
7	0	0	0	16.058 5
8	-1	0	1	15.480 4
9	1	1	0	13.561 5
10	-1	-1	0	14.685 7
11	0	1	-1	15.701 9
12	0	0	0	16.585 5
13	-1	1	0	15.102 3
14	-1	0	-1	15.388 6
15	0	0	0	16.145 9
16	0	1	1	12.620 9
17	0	-1	1	14.875 4

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表 3 实验方差结果

Table 3. Test results of variance

方差来源	方差和	df	均方差	F值	P值
Model	14.67	9	1.63	6.41	0.011 4	显著
A	0.108	1	0.108	0.4247	0.535 4
B	1.65	1	1.65	6.48	0.038 3	*
C	1.59	1	1.59	6.25	0.041	*
AB	1.63	1	1.63	6.43	0.039	*
AC	0.008 9	1	0.008 9	0.035 1	0.856 6
BC	1.69	1	1.69	6.64	0.036 6	*
A²	0.762 9	1	0.762 9	3	0.126 9
B²	5.28	1	5.28	20.77	0.002 6	**
C²	1.27	1	1.27	5.01	0.060 3
余量	1.78	7	0.254 4
失拟误差	1.59	3	0.529	10.93	0.051 4	不显著
纯误差	0.193 6	4	0.048 4
Cor 总计	16.45	16
注：表中代表较大影响(P-value＜0.05)；*代表极大影响(P-value＜0.01)。

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表 4 实验验证结果

Table 4. Test verification results

序列	吸附量/ (mg/g)	吸附率/%	平均吸附量/ (mg/g)	平均吸附率/%
1	16.533	99.20
2	16.528	99.17	16.521	99.13
3	16.503	99.02

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