A kind of preparation method of vitamin E
A vitamin and catalyst technology is applied in the field of vitamin E preparation to achieve the effects of reducing waste water, good reaction selectivity and high reaction yield
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Embodiment 1
[0034] In the reaction vessel, add 91.31g (0.6mol) trimethylhydroquinone and 14.87g 3-sulfonic acid propyltrimethylamine chloride zincate [HO 3 S-(CH 2 ) 3 -NMe 3 ][Cl 2ZnCl 2 ], stirred, heated to 99°C under the protection of nitrogen, and slowly added dropwise 177.92g (0.6mol) of isophytic alcohol for 45 minutes. After the reaction is finished, let it stand for cooling, then take the upper and lower layer liquids to recover the solvent under reduced pressure, and obtain the product and the catalyst respectively.
[0035] The product is sampled, and the sample method refers to GB / T 9454-2008, gas chromatography, and the condensation reaction yield is 96.5%.
Embodiment 2
[0037] Add successively 91.31g (0.6mol) trimethylhydroquinone and 14.87g 3-sulfonic acid propyltrimethylamine chloride zincate [HO 3 S-(CH 2 ) 3 -NMe 3 ][Cl 2ZnCl 2 ], stirred, heated to 40° C. under the protection of argon, slowly added dropwise 177.92 g (0.6 mol) of isophytic alcohol for 1 hour, and kept the reaction for 3 hours after the dropwise addition was completed. After the reaction is finished, let it stand for cooling, then take the upper and lower layer liquids to recover the solvent under reduced pressure, and obtain the product and the catalyst respectively.
[0038] The product is sampled, and the sample method refers to GB / T 9454-2008, gas chromatography, and the condensation reaction yield is 92.0%.
Embodiment 3
[0040] Add successively 91.31g (0.6mol) of trimethylhydroquinone and 14.87g of 3-sulfonic acid propyltrimethylamine dissolved in 530ml of heptane / ethylene carbonate (5:4v / v) mixed solvent in the reaction vessel Chlorozincate [HO 3 S-(CH 2 ) 3 -NMe 3 ][Cl 2ZnCl 2 ], stirred, heated to 140° C. under the protection of helium, and added dropwise 177.92 g (0.6 mol) of isophytic alcohol for 20 minutes. After the dropwise addition, the mixture was incubated for 40 minutes. After the reaction is finished, let it stand for cooling, then take the upper and lower layer liquids to recover the solvent under reduced pressure, and obtain the product and the catalyst respectively.
[0041]The product is sampled, and the sample method refers to GB / T 9454-2008, gas chromatography, and the condensation reaction yield is 92.3%.
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