响应面优化核-壳结构TiO2@SiO2的制备工艺

doi:10.11962/1006-4990.2019-0564

无机盐工业 ›› 2020, Vol. 52 ›› Issue (10): 77-83.doi: 10.11962/1006-4990.2019-0564

响应面优化核-壳结构TiO₂@SiO₂的制备工艺

徐林冲(),袁爱群(),吴胜富,黄增尉,白丽娟,韦冬萍

广西民族大学化学化工学院,广西南宁 530006

收稿日期:2020-04-18 出版日期:2020-10-10 发布日期:2020-11-24
通讯作者: 袁爱群
作者简介:徐林冲（1993— ）,男,硕士研究生,主要从事材料化学研究;E-mail： xulc333@126.com。
基金资助:
国家自然基金项目(21666006)

Preparation process of core-shell structure TiO₂@SiO₂ optimized by response surface experiment

Xu Linchong(),Yuan Aiqun(),Wu Shengfu,Huang Zengwei,Bai Lijuan,Wei Dongping

School of Chemistry and Chemical Engineering,Guangxi University for Nationalities,Nanning 530006,China

Received:2020-04-18 Online:2020-10-10 Published:2020-11-24
Contact: Yuan Aiqun

摘要/Abstract

摘要：

以金红石二氧化钛为核、硅酸钠作为包覆剂,并流法制备核-壳结构TiO₂@SiO₂。采用单因素实验探究pH、温度、搅拌速率、包覆时间、二氧化钛初始浓度、包覆剂用量及陈化时间7个因素对产品酸溶率的影响,响应面实验优化制备工艺,用TEM、XPS、SEM、XRD、FT-IR、UV-vis等手段对产物进行表征。结果表明,固定搅拌速率为300 r/min、包覆时间为60 min、二氧化钛初始质量浓度为200 g/L,各因素对酸溶率的影响次序由大到小为：包覆剂用量、温度、pH、陈化时间,在较优工艺条件包覆剂用量为4.41%、温度为83.65 ℃、pH为9.59、陈化时间为25.62 h下,产物的酸溶率为3.43%。壳层为无定形二氧化硅、厚度约为5 nm左右的致密膜,以Ti—O—Si化学键合在二氧化钛核的表面,核-壳结构的TiO₂@SiO₂具有更高的紫外屏蔽能力。

关键词: TiO₂, TiO₂@SiO₂, 核-壳结构

Abstract:

Core-shell structure TiO₂@SiO₂ was prepared by parallel flow method using rutile TiO₂ as the core and sodium silicate as the coating agent.The influence of seven single factors including pH,temperature,stirring rate,coating time,initial concentration of TiO₂,coating amount and aging time on acid solubility of products were explored by single factor experiment.The preparation process was optimized by response surface experiment.The obtained product was characterized by TEM,XPS,SEM,XRD,FT-IR and UV-Vis.The results showed that when mixing rate was 300 r/min,the coating time was 60 min and the initial mass concentration of TiO₂ was 200 g/L,the order of influence of the four factors was as follows: coating dose> coating temperature>pH>aging time.The optimal conditions were as follows: the content of coating agent was 4.41%,the temperature was 83.65 ℃,the pH was 9.59 and the aging time was 25.62 h.Under the conditions,the acid solubility of the product reached 3.43%.The shell layer was amorphous SiO₂ with a thickness of about 5 nm and was chemically bonded on the surface of TiO₂ nucleus by Ti-O-Si.Core-shell structure TiO₂@SiO₂ has the higher UV shielding capability.

Key words: TiO₂, TiO₂@SiO₂, core-shell structure

中图分类号:

TQ134.11

徐林冲,袁爱群,吴胜富,黄增尉,白丽娟,韦冬萍. 响应面优化核-壳结构TiO₂@SiO₂的制备工艺[J]. 无机盐工业, 2020, 52(10): 77-83.

Xu Linchong,Yuan Aiqun,Wu Shengfu,Huang Zengwei,Bai Lijuan,Wei Dongping. Preparation process of core-shell structure TiO₂@SiO₂ optimized by response surface experiment[J]. Inorganic Chemicals Industry, 2020, 52(10): 77-83.

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参考文献 13

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来源	平方和	自由度	均方	F值	P值	显著性
模型	88.39	14	6.31	112.42	<0.000 1	**
A	7.00	1	7.00	124.61	<0.000 1	**
B	16.24	1	16.24	289.09	<0.000 1	**
C	38.86	1	38.86	691.96	<0.000 1	**
D	5.68	1	5.68	101.21	<0.000 1	**
AB	3.03	1	3.03	53.91	<0.000 1	**
AC	2.42	1	2.42	43.05	<0.000 1	**
AD	0.060	1	0.060	1.07	0.317 6
BC	0.81	1	0.81	14.42	0.001 8	**
BD	0.41	1	0.41	7.29	0.016 4	*
CD	0.055	1	0.055	0.98	0.337 1
A²	3.91	1	3.91	69.60	<0.000 1	**
B²	5.37	1	5.37	95.63	<0.000 1	**
C²	7.89	1	7.89	140.44	<0.000 1	**
D²	1.85	1	1.85	33.01	<0.000 1	**
残差	0.84	15	0.056
失拟项	0.65	10	0.065	1.72	0.284 6
纯误差	0.19	5	0.038
总和	89.24	29

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响应面优化核-壳结构TiO₂@SiO₂的制备工艺

Preparation process of core-shell structure TiO₂@SiO₂ optimized by response surface experiment

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参考文献 13

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推荐阅读 10

序号	A pH	B 温度/℃	C 包覆剂用量/%	D 陈化时间/h	酸溶率/ %
1	10.0	75	3.5	18	10.07
2	10.0	75	3.5	30	9.29
3	9.5	80	4.0	12	6.52
4	9.5	80	4.0	24	4.64
5	9.5	80	4.0	24	4.16
6	10.0	85	4.5	30	3.32
7	9.5	80	4.0	36	4.14
8	9.5	80	3.0	24	9.06
9	10.0	85	3.5	18	7.54
10	10.0	85	3.5	30	5.97
11	9.0	85	3.5	30	5.43
12	9.5	80	4.0	24	4.27
13	10.5	80	4.0	24	6.81
14	9.0	75	4.5	18	4.92
15	10.0	75	4.5	30	5.75
16	9.5	80	4.0	24	4.46
17	9.5	80	4.0	24	4.17
18	9.5	70	4.0	24	7.95
19	9.0	85	3.5	18	6.20
20	9.0	75	4.5	30	4.56
21	9.0	85	4.5	18	4.97
22	8.5	80	4.0	24	4.79
23	10	85	4.5	18	4.69
24	9.5	80	5.0	24	3.81
25	9.5	90	4.0	24	4.17
26	10.0	75	4.5	18	5.98
27	9.0	85	4.5	30	3.94
28	9.0	75	3.5	30	6.43
29	9.0	75	3.5	18	7.24
30	9.5	80	4.0	24	4.49

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