首页|"安息香和二苯乙二酮的制备及表征"实验的改进与创新

"安息香和二苯乙二酮的制备及表征"实验的改进与创新

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安息香及二苯乙二酮的制备与表征是综合化学实验中涉及到有机合成的经典实验项目。然而现有的实验方案存在反应原料需要减压蒸馏纯化、安息香产率低、二苯乙二酮的合成时间较长的不足,为此,进行了创新设计和改进。用饱和碳酸氢钠溶液洗涤纯化了原料苯甲醛,调控氢氧化钠的滴加速度和滴加温度,并且采用逐步升温法优化合成了安息香,进而以安息香为原料,运用微波辐射法合成了二苯乙二酮。结果表明:用饱和碳酸氢钠可纯化原料苯甲醛;在室温下控制氢氧化钠溶液的滴加时间在20 min,逐步加热至70 ℃,反应60 min合成的安息香产率约为50%,产率提高了 15%;再以制备的安息香为原料,优化了二苯乙二酮的合成条件,微波辐射反应16 min时,其产率约为90%,反应时间明显缩短。通过改进和创新,实验设计更加合理,培养了学生综合实验技能和自主探究的能力。
Improvement and Innovation of Experiment Preparation and Characterization of Benzoin and Benzil
The preparation and characterization of benzoin and benzil is a classic experimental project involving organic synthesis in comprehensive chemical experiments.However,there are some shortcomings in the existing experimental scheme,such as the purification of reaction raw materials by vacuum distillation,low yield of benzoin,long synthesis time of benzil.To this end,the innovative design and improvement were carried out.The raw material benzaldehyde was purified with saturated sodium bicarbonate solution instead of vacuum distillation,and the dropping speed and dropping temperature of sodium hydroxide were regulated.Benzoin was optimized and synthesized using a stepwise warming method,and then benzil was synthesized with benzoin as precursor by microwave irradiation.The results showed that the raw material benzaldehyde can be purified with saturated sodium bicarbonate.The dropping time of sodium hydroxide solution was controlled at room temperature for 20 min.The yield of benzoin by heating to 70 ℃ gradually and holding for 60 min was about 50%,which was 15%higher than that by conventional method.Taking as-prepared benzoin as raw material,the synthesis conditions of benzil were optimized.When microwave irradiation for 16 min,the yield of benzil was about 90%,the reaction time was significantly shortened.The experimental design has become more reasonable through improvement and innovation,which enhances students'comprehensive experimental skills and independent exploration ability.

benzoinmicrowave irradiationbenzyl

陈小燕、周惠良、马强、海舍舍、屈丽

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宁夏大学化学化工学院,化学国家级实验教学示范中心,宁夏 银川 750021

安息香 微波辐射 二苯乙二酮

2025

广州化工
广州市化工行业协会 广州市化学化工学会 广州市化学工业研究所

广州化工

影响因子:0.358
ISSN:1001-9677
年,卷(期):2025.53(1)