响应面优化核-壳结构TiO2@SiO2的制备工艺

doi:10.11962/1006-4990.2019-0564

Abstract

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

CLC Number:

TQ134.11

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.

Figures/Tables 12

References 13

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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

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

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