基于Box-Behnken响应面法的邻甲氧基肉桂醛合成工艺优化研究

黄梦贤; 陈伟珠; 晋文慧; 洪专; 陈晖; 袁勇军; 方华

doi:10.13748/j.cnki.issn1007-7693.20233421

基于Box-Behnken响应面法的邻甲氧基肉桂醛合成工艺优化研究

Optimization of Synthesis Process of 2-Methoxycinnamaldehyde Based on Box-Behnken Response Surface Methodology

摘要

摘要:
目的采用Box-Behnken响应面法优化邻甲氧基肉桂醛合成工艺。
方法在单因素试验基础上，以邻甲氧基肉桂醛产率为响应值，选取催化剂用量、KOH用量和反应时间为自变量，采用Box-Behnken中心组合设计实验方案，并建立数学模型，对工艺条件进行优化分析。
结果影响响应值的因素主次顺序为催化剂用量、反应时间、KOH用量。通过回归方程得到0.5 g邻甲氧基苯甲醛与0.30 g乙醛合成邻甲氧基肉桂醛的最佳条件为反应时间2 h，催化剂苄基三乙基氯化铵用量4 mg，0.2 g·mL⁻¹ KOH用量为0.2 mL(40 mg KOH)，在此条件下产率为49.60%，模型预测产率为46.55%，绝对偏差为3.05%。
结论本研究所建立的模型对邻甲氧基肉桂醛合成工艺优化是可靠、有效的。

Abstract:
OBJECTIVE To optimize the synthesis process of 2-methoxycinnamaldehyde by Box-Behnken response surface methodology.
METHODS On the basis of single factor experiments, a Box-Behnken central combination design experimental scheme was adopted, with the yield of 2-methoxycinnamaldehyde as the response value, the catalyst dosage, KOH dosage and reaction time as independent variables. Then a mathematical model was established to optimize and analyze the process conditions.
RESULTS The order of factors affecting the response value was catalyst dosage, reaction time, and KOH dosage. The optimal conditions for the synthesis of 2-methoxycinnamaldehyde from 0.5 g O-anisaldehyde and 0.30 g acetaldehyde were obtained as follows: reaction time 2 h, catalyst benzyltriethylammonium chloride 4 mg, 0.2 g·mL⁻¹ KOH 0.2 mL(40 mg KOH). Under this condition, the yield of 2-methoxycinnamaldehyde was 49.60%, and the model predicted a yield of 46.55% with an absolute deviation of 3.05%.
CONCLUSION The model established by this research is reliable and effective for optimizing the synthesis process of 2-methoxycinnamaldehyde.

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