Fe3O4负载ZnO催化剂的制备及其催化合成松香甘油酯的研究

doi:10.3969/j.issn.0253-2417.2020.06.002

Abstract

Abstract:

A series of magnetic catalysts were prepared with Fe₃O₄ as magnetic center and ZnO as activity center, and the structures and compositions were characterized by TEM, XRD and XPS. The catalytic performances of the prepared catalysts were studied. The results showed that Fe₃O₄@SiO₂-ZnO was of the best catalytic activity and stability. At the same time, the influences of factors on the synthesis of rosin glyceride, such as zinc source and its loading amount, different reaction conditions, were investigated. The results showed that when Fe₃O₄@SiO₂-ZnO(ZnAc₂)(zinc acetate as the zinc source, the theoretical load of zinc source 0.25 g) was catalyst, the reaction temperature was 240 ℃, the reaction time was 5 h, and the catalyst dosage was 0.2 g, the esterification rate and the acid value of rosin glyceride was 81.5% and 38.6 mg/g, respectively. The catalyst Fe₃O₄@SiO₂-ZnO₂(ZnAc₂) had good stability. After repeated use for 5 times, the esterification rate remained above 80%.

Key words: rosin, esterification reaction, magnetic catalyst, acid catalysis

CLC Number:

TQ35

Shitao YU, Haoxue ZOU, Yaya LI, Huimin ZHANG, Yujing WANG. Preparation of Rosin Glyceride Catalyzed by Fe₃O₄ Supported ZnO[J]. Chemistry and Industry of Forest Products, 2020, 40(6): 8-14.

Figures/Tables 9

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References 18

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序号 No.	温度/℃ temperature	时间/h time	催化剂用量/g catalyst amount	锌源负载量/g zinc source loading	酸值/(mg·g^-1) acid value	酯化率/% esterification rate
1	240	5	0.30	0.10	187.0	9.0
2	240	5	0.30	0.25	57.2	72.3
3	240	5	0.30	0.60	109.1	47.2
4	240	5	0.20	0.25	38.2	81.5
5	240	5	0.25	0.25	75.3	63.5
6	240	5	0.35	0.25	62.3	69.8
7	240	5	0.40	0.25	55.6	73.1
8	240	3	0.20	0.25	96.4	53.3
9	240	4	0.20	0.25	87.1	57.8
10	240	6	0.20	0.25	40.9	80.2
11	240	7	0.20	0.25	39.9	81.0
12	220	5	0.20	0.25	89.4	56.7
13	230	5	0.20	0.25	65.7	68.2
14	250	5	0.20	0.25	43.6	78.9
15	260	5	0.20	0.25	41.2	80.1

项目 items		单位总酸量¹⁾/mmol total acid per unit	酸值/(mg·g^-1) acid value	酯化率/% esterification rate
对照 contrast	— ZnO		109.4 83.2	47.0 59.7
催化剂类型 catalyst type	Fe₃O₄-ZnO(ZnAc₂) Fe₃O₄@SiO₂-ZnO(ZnAc₂)	7.5 56.3	46.0 38.6	77.7 81.5
锌源 zinc sources	ZnAc₂ ZnCl₂ ZnSO₄ Zn(NO₃)₂	56.3(0.5) 44.2(0.1) 50.8(0.2) 49.1(0.1)	38.6 74.3 54.1 59.6	81.5 64.0 73.8 71.1
ZnAc₂负载量 loading of ZnAc₂	0.10 g 0.25 g 0.45 g 0.60 g	0 56.3 34.9 30.4	109 38.6 52.6 73.6	47 81.5 74.5 64.4

回收次数 recycling times	酸值/(mg·g^-1) acid value	酯化率/% esterification rate
1	38.6	81.3
2	39.7	80.8
3	40.2	80.5
4	39.0	81.1
5	39.1	81.1

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Preparation of Rosin Glyceride Catalyzed by Fe₃O₄ Supported ZnO

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Preparation of Rosin Glyceride Catalyzed by Fe₃O₄ Supported ZnO