Synthesis of n-butyl acetate by esterification
I. INTRODUCTION
n-butyl acetate, as an important organic compound, has been widely used in many fields. Synthesis of n-butyl acetate by esterification reaction, exploring its optimization of synthesis conditions and influencing factors, is of great significance to improve product quality and production efficiency.
Second, experimental principle
Esterification reaction between acetic acid ($CH_3COOH $) and n-butyl alcohol ($C_4H_9OH $) under the action of catalyst, resulting in n-butyl acetate ($CH_3COOC_4H_9 $) and water ($H_2O $). The reaction equation is: $CH_3COOH + C_4H_9OH\ underset {\ Delta} {\ overset {catalyst} {\ rightleftharpoons}} CH_3COOC_4H_9 + H_2O $. This reaction is a reversible reaction. In order to increase the yield of n-butyl acetate, measures such as excess of a reactant or timely removal of the water generated by the reaction can be taken.
III. Experimental Materials and Instruments
1. ** Experimental Materials **: glacial acetic acid, n-butanol, concentrated sulfuric acid (as catalyst), saturated sodium carbonate solution, saturated saline, anhydrous magnesium sulfate (desiccant).
2. ** Experimental Instruments **: round bottom flask, spherical condenser, water separator, thermometer, separation funnel, distillation device (including distillation flask, straight condenser, liquid receiving tube, conical bottle, etc.).
IV. Experimental Steps
1. ** Esterification reaction **: In a dry round-bottom flask, add a certain amount of glacial acetic acid, n-butanol and a few drops of concentrated sulfuric acid in turn. After mixing evenly, install a spherical condenser and a water separator, and heat the reflux reaction. During the reaction, observe the change of water level in the water separator, and separate the water generated by the reaction in time to promote the reaction to proceed in the positive direction.
2. ** Crude product separation **: After the reaction is completed, wait for the reaction solution to cool to room temperature, and transfer it to the separation funnel. Wash first with a saturated sodium carbonate solution to neutralize the unreacted acetic acid and reduce the solubility of n-butyl acetate. After stratification, separate the lower aqueous phase. The organic phase is then washed with saturated salt water. The purpose is to wash away the residual sodium carbonate and reduce the amount of anhydrous magnesium sulfate used in subsequent drying. Finally, the organic phase is transferred to a dry conical flask, and an appropriate amount of anhydrous magnesium sulfate is added to dry until the liquid is clarified.
3. ** Distillation and Refinement **: Transfer the dried crude product to a distillation flask, install a distillation device, and heat the distillation. Collect the fraction within a specific temperature range, which is the refined n-butyl acetate product.
V. Experimental Results and Discussion
1. ** Yield Calculation **: Calculate the actual mass of the product by measuring the volume of the collected n-butyl acetate product and combining its density. According to the feed amount of acetic acid or n-butanol in the reaction, the theoretical yield is calculated according to the stoichiometric relationship, and then the yield is obtained. Yield = (actual yield/theoretical yield) × 100%.
2. ** Analysis of influencing factors **:
- ** Catalyst dosage **: Concentrated sulfuric acid dosage is too small, the catalytic effect is not obvious, and the reaction rate is slow; excessive dosage will lead to an increase in side reactions, affecting product purity and yield.
- ** Reactant ratio **: The ratio of acetic acid to n-butanol has an effect on the yield. Increasing the amount of a reactant can shift the equilibrium towards the formation of n-butyl acetate, but too much increase will cause waste of raw materials and increase the difficulty of subsequent separation.
- ** Reaction time and temperature **: The reaction time is too short, the reaction does not reach equilibrium, and the yield is low; the reaction time is too long, which may trigger side reactions. If the temperature is too high, it is also easy to lead to side reactions; if the temperature is too low, the reaction rate is slow. It is necessary to control the appropriate reaction time and temperature to improve the yield.
Sixth, Conclusion
n-butyl acetate was successfully synthesized by esterification reaction. The influence of various factors on the synthesis reaction was clarified during the experiment. Under optimized conditions, the yield and purity of n-butyl acetate can be improved. This experiment provides some reference for related organic synthesis research and industrial production, and is helpful to further explore more efficient and environmentally friendly n-butyl acetate synthesis methods.