Preparation method of diethylene glycol dibenzoate
A technology of diethylene glycol dibenzoate and benzoic acid, which is applied in the field of preparation of diethylene glycol dibenzoate, can solve the problems of post-processing, troublesome operation, high reaction temperature, and high product cost, and achieve post-processing The effect of simple process, low reaction temperature and low product cost
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Embodiment 1
[0021] Put 1000g of benzoic acid and 430g of diethylene glycol in a 2L three-necked bottle, and the ratio of feeding is 2:1.05. When stirring, heat up (oil bath temperature 180-200°C), add 20g of heteropolyacid as a catalyst, and then add Saturated hydrocarbon cyclohexane is used as 80g of water-carrying agent, the temperature is adjusted to 145-160°C, and the temperature is kept for 10-15h to complete the reaction. At a temperature of 145-160°C, the dehydration agent is decompressed to obtain the crude product DEDB, which is deacidified by calcium carbonate, sodium carbonate, alkaline resin or sodium hydroxide, and traditionally decolorized to obtain DEDB.
Embodiment 2
[0023] Put 1000g of benzoic acid and 480g of diethylene glycol into a 2L three-necked bottle, the ratio of the feed is 2:1.1, heat up while stirring (oil bath temperature 100-120°C), add 32g of hydrochloric acid as a catalyst, and then add saturated hydrocarbon Water-carrying agent cyclohexane 90g, keep warm for 6-8h, adjust the temperature to 90-100°C to complete the reaction. At this temperature, the hydrocarbon water-carrying agent is removed under reduced pressure to obtain the crude product DEDB, which is deacidified by calcium carbonate, sodium carbonate, alkaline resin or sodium hydroxide, and DEDB is obtained by traditional decolorization.
Embodiment 3
[0025] In the three-necked bottle of 2L, drop into 1000g benzoic acid, 480g diethylene glycol, feed ratio is 2: 1.1, heat up (oil bath temperature 120-140 ℃) under the situation of stirring, add hydrochloric acid 20g and p-toluenesulfonic acid 8g as catalyst, and then add 50 g of n-hexane, a saturated hydrocarbon water-carrying agent, adjust the temperature to 90-100° C., and keep the temperature for 12-16 hours to complete the reaction. At this temperature, the hydrocarbon water-carrying agent is removed under reduced pressure to obtain the crude product DEDB, which is deacidified by calcium carbonate, sodium carbonate, alkaline resin or sodium hydroxide, and DEDB is obtained by traditional decolorization.
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