苯甲酸、对甲苯胺、乙酰苯胺三组分分离实验教学设计

doi:10.3866/PKU.DXHX201904048

Abstract

Abstract:

Separation and purification is the key step in organic synthesis, which is 90% of the total work. To train undergraduates' laboratory skill of separation and purification from the crude product or mixture and improve their understanding ability of using the theory of extraction, distillation, recrystallization, the "Separation of three organic component mixtures" is arranged by the organic chemistry teaching group at the College of Chemistry and Chemical Engineering, Central South University. Students include the five-year and eight-year medical clinic, pharmaceutical and applied chemistry. In this paper, the two teaching schemes of acid and alkali separation in this experiment are discussed in detail, and the laboratory teaching effects of the two schemes are compared.

Key words: Three components, Separation and purification, Organic laboratory teaching, ¹H NMR characterization

MSC2000:

Lihui Jiang,Guohui Chen,Weihong Wang,Yingping Zou,Yiming Luo. Design of Separation Experiment of Three Components of Benzoic Acid, p-Methylaniline and Acetanilide[J].University Chemistry, 2020, 35(1): 98-104.

试剂	分子量	熔点/℃	沸点/℃	相对密度	溶解性
对甲苯胺	107.15	44.45	200	0.9619	微溶于水，易溶于乙酸、乙醚
苯甲酸	122.12	122.13	249	1.2659	微溶于水，易溶于乙酸、乙醚
乙酰苯胺	135.17	114.3	304	1.2190	溶于热水，易溶于乙醚
乙酸乙酯	88.11	-83	77	0.902	水中8.3 g·100 mL^-1 (20 ℃)

学号	η/%
学号	对甲苯胺	苯甲酸	乙酰苯胺
01	55	34	38
02	48	69	26
03	72	64	62
04	47	53	39
05	48	35	35
06	59	73	84
07	57	28	60
08	57	71	40
09	50	42	53
10	52	62	64
11	68	58	43
12	0	85	54
13	69	47	42
14	56	79	30
15	78	52	76
16	57	68	46
17	47	36	54
18	70	58	61
19	67	52	89
20	54	70	47
21	101	36	68
22	56	61	42
23	81	62	34
24	59	60	67
25	130	60	25
26	66	70	60
27	73	50	47
28	58	51	38
29	69	61	89
30	28	35	88

回收率	人数
回收率	对甲苯胺	苯甲酸	乙酰苯胺
10%以下	2	0	4
10%–20%	0	1	0
20%–30%	2	8	3
30%–40%	3	14	9
40%–50%	25	28	33
50%–60%	36	35	34
60%–70%	29	24	21
70%–80%	15	9	10
80%–90%	3	0	5
90%–100%	0	0	0
100%以上	4	0	0

回收率	人数
回收率	对甲苯胺	苯甲酸	乙酰苯胺
10%以下	5	0	7
10%–20%	6	0	0
20%–30%	4	0	6
30%–40%	11	5	30
40%–50%	20	7	32
50%–60%	37	33	13
60%–70%	25	44	19
70%–80%	7	26	5
80%–90%	3	3	4
90%–100%	0	0	2
100%以上	0	0	0

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Design of Separation Experiment of Three Components of Benzoic Acid, p-Methylaniline and Acetanilide

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