Preparation method of vanillin
A technology of vanillin and eugenol, which is applied in the field of vanillin preparation, can solve the problems of serious pollution and production capacity, and achieve the effects of low pollution, stable reaction, and easy scale-up production
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[0020] The invention provides a kind of preparation method of vanillin, specifically implement according to the following steps:
[0021] Step 1, the preparation of isoeugenol potassium salt
[0022] In a clean and dry three-necked flask equipped with a reflux device, add eugenol, raise the temperature to 100°C-110°C, stir magnetically, and add 55% KOH solution dropwise. Continue to stir for 2.5h-3.5h at a temperature of -110°C to obtain a yellow-black viscous solution, which is isoeugenol potassium salt, wherein the volume ratio of eugenol to KOH solution is 1:1-2:1;
[0023] Step 2, the preparation of intermediate product vanillin potassium salt
[0024] Add deionized water and KOH solution to the three-necked flask containing isoeugenol potassium salt, the solution turns yellow, slowly lower the temperature to 45°C-55°C, and stir quickly to fully dissolve the oil; then pour into the solution Potassium ferrate was added to the mixture, and magnetically stirred for 15min-45...
Embodiment 1
[0032] A preparation method of vanillin, which is specifically implemented according to the following steps: in a clean and dry three-necked flask equipped with a reflux device, add 25 milliliters (0.1617 moles) of eugenol, heat up to 105 ° C, magnetically stir, and drop 16 milliliters (0.157 moles) 55% KOH solution, after the dropwise addition, a dark green solution was obtained, and then continued stirring at 105°C for 3 hours to obtain a yellow-black viscous solution, which was isoeugenol potassium salt; Add the KOH solution of 10 gram deionized water and 100 gram 32% (0.5714 moles) in the there-necked flask of potassium phenolate, solution turns yellow, temperature is slowly down to 50 ℃, stirs rapidly, makes oily thing fully dissolve; Then Add 48 grams (0.242 moles) of potassium ferrate to the solution, and stir magnetically for 30 minutes at room temperature to obtain vanillin potassium salt; add the above-mentioned vanillin potassium salt in the there-necked flask and qu...
Embodiment 2
[0034]A preparation method of vanillin, which is specifically implemented according to the following steps: in a clean and dry three-necked flask equipped with a reflux device, add eugenol, heat up to 100°C, stir magnetically, add 55% KOH solution dropwise, add dropwise After completion, a dark green solution was obtained, and then continued to stir for 2.5 h at a temperature of 100° C. to obtain a yellow-black viscous solution, which was isoeugenol potassium salt, wherein the volume ratio of eugenol and KOH solution was 1: 1; Add deionized water and KOH solution to the three-necked flask containing isoeugenol potassium salt, the solution turns yellow, slowly lower the temperature to 45°C, stir quickly to fully dissolve the oily substance; then pour into the solution Add potassium ferrate, magnetically stir 15min under normal temperature, obtain vanillin potassium salt, wherein, the mass volume ratio (g / ml) of deionized water and eugenol is 1:5; The mass volume ratio (g / ml) of ...
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