A kind of esterification reaction method and its application in the preparation of wintergreen oil and diethyl oxalate
A technology of esterification reaction and wintergreen oil, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of high catalyst price, difficult raw material CO, and high reactor requirements, and achieve reaction yield High, low cost, low reaction temperature effect
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Embodiment 1
[0038] Refer to attached figure 1 .
[0039] Composition of raw materials: 900g of salicylic acid, 800g of methanol and 600g of boron gangue powder.
[0040] Preparation method of wintergreen oil:
[0041] S1. Add salicylic acid and methanol into the reaction kettle, start stirring, slowly add boron gangue powder, heat to 60°C for esterification reaction for 4 hours, and stop the reaction after the acid in the reaction system is consumed;
[0042] S2. The system in step S1 is subjected to atmospheric distillation at 85° C. to recover methanol;
[0043] S3. The system in step S2 is subjected to solid-liquid separation, the filtrate and filter residue are collected, and the filtrate is refined to be worth 923g of wintergreen oil, with a yield of 95%. The refining method is stripping, and the water vapor can be recycled after condensation;
[0044] S4. Wash the filter residue three times with the methanol recovered in step S2 to obtain metaboric acid, collect the washing liqui...
Embodiment 2
[0049] Composition of raw materials: 1000g of salicylic acid, 800g of methanol and 660g of boron gangue powder.
[0050] Preparation method of wintergreen oil:
[0051] S1. Add salicylic acid and methanol into the reaction kettle, start stirring, slowly add boron gangue powder, heat to 60°C for esterification reaction for 4 hours, and stop the reaction after the acid in the reaction system is consumed;
[0052] S2. The system in step S1 is subjected to atmospheric distillation at 85° C. to recover methanol;
[0053] S3. The system in step S2 is subjected to solid-liquid separation, the filtrate and filter residue are collected, and the filtrate is refined to be worth 1036g of wintergreen oil, with a yield of 96%. The refining method is steam stripping, which can be recycled after condensation of water vapor;
[0054] S4. Wash the filter residue three times with the methanol recovered in step S2 to obtain metaboric acid, collect the washing liquid, merge it with the methanol r...
Embodiment 3
[0057] Composition of raw materials: 950g of salicylic acid, 800g of methanol and 630g of boron gangue powder.
[0058] Preparation method of wintergreen oil:
[0059] S1. Add salicylic acid and methanol into the reaction kettle, start stirring, slowly add boron gangue powder, heat to 60°C for esterification reaction for 4 hours, and stop the reaction after the acid in the reaction system is consumed;
[0060] S2. The system in step S1 is subjected to atmospheric distillation at 85° C. to recover methanol;
[0061] S3. The system in step S2 is subjected to solid-liquid separation, the filtrate and filter residue are collected, and the filtrate is refined to be worth 1004g of wintergreen oil, with a yield of 98%. The refined method is distilled under reduced pressure, and the distillate is wintergreen oil. The residue is heavy oil;
[0062] S4. Wash the filter residue three times with the methanol recovered in step S2 to obtain metaboric acid, collect the washing liquid, merg...
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