1, 2-hexanediol as well as purification method and application thereof
A purification method and technology for hexanediol, applied in the field of 1,2-hexanediol and its purification, can solve the problems of low yield, large loss and the like
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Embodiment 1
[0026] Step 1: Preparation of 1,2-hexanediol crude product
[0027] In a 500mL three-necked flask, equipped with a thermometer, dropping funnel, and a low-temperature reflux condenser. 140.0 g of 88% formic acid and 75.0 g of 1-hexene were sequentially added at room temperature. The temperature was raised to 50° C. with stirring, and 110.0 g of 30% hydrogen peroxide was slowly added dropwise. Stir at 55°C until the reaction is complete. 275.0 g of 40% NaOH aqueous solution was added dropwise, and the mixture was stirred at 20-25° C. for 1 hour after the drop was completed. The reaction system was left to stand for stratification, and the upper layer was taken and rectified under vacuum to obtain 47.6 g of product main fraction, GC purity 99.56%, moisture 0.23%, and main fraction yield 45.33%.
[0028] Step 2: Purify crude 1,2-hexanediol by adding sodium borohydride
[0029] In a 500mL three-necked flask, add 320g of the product obtained in step (1), slowly add 0.64g of sod...
Embodiment 2
[0030] Example 2 Purification of 1,2-hexanediol crude product by adding potassium borohydride
[0031] Step 1: Preparation of 1,2-hexanediol crude product
[0032] In a 500mL three-necked flask, equipped with a thermometer, dropping funnel, and a low-temperature reflux condenser. 140.0 g of 88% formic acid and 75.0 g of 1-hexene were sequentially added at room temperature. The temperature was raised to 50° C. with stirring, and 110.0 g of 30% hydrogen peroxide was slowly added dropwise. Stir at 55°C until the reaction is complete. 275.0 g of 40% NaOH aqueous solution was added dropwise, and the mixture was stirred at 20-25° C. for 1 hour after the drop was completed. The reaction system was left to stand for stratification, and the upper layer was taken and rectified under vacuum to obtain 47.6 g of product main fraction, GC purity 99.56%, moisture 0.23%, and main fraction yield 45.33%.
[0033] Step 2: Purify the crude product of 1,2-hexanediol by adding potassium borohyd...
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