Experimental Report on Synthesis of Ethyl Acetate
** Abstract **: This report records the experimental process of synthesizing ethyl acetate with [specific reactants] in detail, including experimental principles, experimental steps, experimental data recording and processing, as well as analysis and discussion of experimental results. It aims to explore the optimal conditions and related influencing factors of the synthesis reaction.
1. To master the synthesis principle and method of ethyl acetate.
2. Familiar with basic operations such as reflux and distillation.
3. Learn to identify the purity of the product by measuring refractive index and other means.
Second, the experimental principle
The esterification reaction between acetic acid and ethanol under the catalysis of concentrated sulfuric acid produces ethyl acetate. The reaction formula is as follows:
\ [CH_ {3} COOH + C_ {2} H_ {5} OH\ underset {\ Delta} {\ overset {H_ {2} SO_ {4}} {\ rightleftharpoons}} CH_ {3} COOC_ {2} H_ {5} + H_ {2} O\]
The reaction is a reversible reaction. In order to improve the yield of ethyl acetate, it is usually used to increase the concentration of the reactant (such as adding excess ethanol) or continuously remove the product (such as evaporating the azeotrope of ethyl acetate and water in time) to promote the equilibrium to move in the direction of positive reaction.
III. Experimental instruments and pharmaceuticals
1. ** Instruments **: round bottom flask, spherical condenser tube, distillation head, straight condenser tube, connecting tube, conical flask, liquid separation funnel, thermometer, Abbe refractometer, etc.
2. ** Pharmaceuticals **: glacial acetic acid, anhydrous ethanol, concentrated sulfuric acid, saturated sodium carbonate solution, saturated salt water, saturated calcium chloride solution, anhydrous magnesium sulfate.
IV. Experimental steps
1. ** Esterification reaction **
- In a dry 100 mL round-bottom flask, add 12 mL of anhydrous ethanol, slowly add 4 mL of concentrated sulfuric acid, shake while adding, mix well, then add 8 mL glacial acetic acid, and put in 2 - 3 zeolites.
- Install the reflux device as shown in the picture, and heat the reflux on low heat for about 30 min.
2. ** Preparation of the crude product **
- After the reaction is completed, wait for the reaction solution to cool to room temperature, and pour it into the separation funnel.
- Wash the reaction solution several times with 10 mL of saturated sodium carbonate solution, gently oscillate, paying attention to deflation, until the pH of the organic phase is neutral.
- Wash once more with 10 mL of saturated table salt water, followed by two washes with 10 mL of saturated calcium chloride solution. After each wash, let stand and layer, and separate the lower liquid.
3. ** Drying and distillation of the product **
- Pour the upper organic phase into a dry conical flask, add an appropriate amount of anhydrous magnesium sulfate and dry for about 15 min.
- Filter the dried liquid into a 50 mL distillation flask, add zeolite, install a distillation device, collect fractions at 73 - 78 ° C, weigh and record the yield.
4. ** Determination of refractive index **
- The refractive index of the product was determined using an Abbe refractometer and compared with the literature values.
V. Record and treatment of experimental data
1. ** Record of yield **: The actual yield is [X] g, and the theoretical yield is calculated according to the reaction formula according to the amount of glacial acetic acid and ethanol.
2. ** Yield calculation **: Yield =\ (\ frac {actual yield} {theoretical yield}\ times100 \%\) = \(\ frac {X} {Y}\ times100 \%\) = [ Z]%
3. ** Refractive index measurement **: The measured product refractive index is [n], the literature value is [n literature], the relative error =\ (\ frac {| n - n literature |} {n literature}\ times100 \%\) = [ error value]%
VI. Results and discussion
1. ** Yield analysis **: The yield of this experiment is [Z]%. Compared with the theoretical yield, [analyze the reasons for the high and low yield, such as whether the proportion of reactants is appropriate, whether the reaction time is sufficient, whether there is a loss in the separation process, etc.].
2. ** Refractive index analysis **: The relative error of the refractive index of the product is [error value]% compared with the literature value. [The possible reasons for the analysis error, such as the influence of instrument error, sample purity, temperature at the time of measurement, etc.].
3. ** Experimental Improvement **: Based on the results of this experiment, [proposed measures to improve the experiment, such as optimizing the proportion of reactants, improving the separation method, improving the precision of reaction temperature control, etc.] can be considered to improve the yield and purity of ethyl acetate.
VII. CONCLUSION
Through this experiment, ethyl acetate was successfully synthesized, and its synthesis method and related operation skills were mastered. Through the analysis of experimental data, the factors affecting the reaction yield and product purity were understood, and corresponding improvement measures were proposed, which provided a reference for similar experiments in the future.
