Treatment method for recovering tetrahydrofuran from grignard reaction
A tetrahydrofuran and Grignard reaction technology, applied in the chemical industry, can solve the problems of increased filtration, excessive alkali content, easy to block pipelines, etc., and achieve the effect of reducing the cost of raw materials
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Embodiment 1
[0013] Embodiment 1: About 1000 liters of hydrous tetrahydrofuran (water content 7.6%) obtained from the Grignard reaction normal pressure or reduced pressure, join in the static dehydration processor 1 of volume 1500 liters, each layer of semicircular sieve plate 2 in advance respectively Place 50 kilograms of sodium hydroxide, leave standstill, separate lye from stratifier 3 every 1 hour, detect moisture after about 10 hours and be 0.18%, pump 4 is delivered to about 800 in the fractionating still 5 of volume 1000 liters liters, directly pass into water vapor for heating and distillation, the vaporized steam passes through the fractionation column 6 (inner diameter 250mm, effective height 1.5 meters, with stainless steel packing inside), and then condenses through the condenser 7, and about 40 liters of the fraction before 66°C is put into the former fraction About 720 liters of cuts in storage tank 8, 66-68 ℃ are put into positive fraction storage tank 9, and about 40 liters...
Embodiment 2
[0014] Embodiment 2: place a total of 100 kilograms of sodium hydroxide on the sieve plate 2 of the static dehydration processor 1 in embodiment 1, then add about 1000 liters of aqueous tetrahydrofuran (water content 7.6%), leave standstill, every 1 hour Separate the lye from the stratifier 3, and after about 15 hours, it is detected that the moisture content is 0.15%, and it is transported to about 800 liters in the fractionation still 5 with a volume of 1000 liters by a pump 4, and directly feeds water vapor for heating and distillation, and the vaporized steam After passing through fractionation column 6 (inner diameter 250mm, effective height 1.5m, with stainless steel packing inside), and then condensed by condenser 7, about 40 liters of the fraction before 66°C is put into the front fraction storage tank 8, and about 720 liters of fraction at 66-68°C Put into positive fraction storage tank 9, keep about 40 liters at the bottom of the kettle, and redistill after merging wi...
Embodiment 3
[0015] Embodiment 3: About 1000 liters of hydrous tetrahydrofuran (water content 7.6%) obtained from Grignard reaction normal pressure or decompression, join in the static dehydration processor 1 of volume 1500 liters, each layer of semicircular sieve plate 2 each in advance Place 50 kilograms of anhydrous calcium chloride, let it stand, separate the lye from the stratifier 3 every 1 hour, and detect that the moisture content is 0.17% after about 12 hours, and the pump 4 is transported to the fractionation still 5 with a volume of 1000 liters About 800 liters are directly passed into steam for heating and distillation. The vaporized steam passes through fractionation column 6 (inner diameter 250 mm, effective height 1.5 meters, with stainless steel packing inside), and then condenses through condenser 7. About 38 liters of distillate before 66 ° C are put into Forward cut storage tank 8, about 718 liters of cuts of 66-68 ℃ are put into positive cut storage tank 9, and about 44 ...
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