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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

Active Publication Date: 2012-01-18
河南华商药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method adds the amount of the inorganic strong base that forms alkali-saturated solution amount and is difficult for controlling, and alkali amount is insufficient, and low water content can't reach, and alkali amount is excessive, easily blocks pipeline, and easily obtains turbid suspension under stirring condition, still needs Add filtering and other operations

Method used

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  • Treatment method for recovering tetrahydrofuran from grignard reaction
  • Treatment method for recovering tetrahydrofuran from grignard reaction

Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

A treatment method for recovering tetrahydrofuran from a grignard reaction. Water-containing tetrahydrofuran recovered from a grignard reaction is dehydrating by a static dehydration treater; the static dehydration treater is provided with a sieve plate and a stratification machine; the dehydrant of sodium hydroxide or anhydrous calcium chloride is placed on the sieve plate; a static treatment manner is adopted; and fractionation treatment is performed to obtain qualified tetrahydrofuran. With the technical scheme of the invention, the recovery rate of tetrahydrofuran is up to 90-96%; the tetrahydrofuran content is more than 99.7%; the water content is less than 0.1%; since the using amount of tetrahydrofuran is large and the price is high, the recovery of tetrahydrofuran from a grignard reaction realizes the recycling, and greatly reduces raw material cost; the alkaline liquor obtained during the treatment process is in an absolutely saturated condition, has minimal residual tetrahydrofuran, and can be used in other neutralization reactions; a saturated calcium chloride aqueous solution is obtained by using anhydrous calcium chloride, and can be used for the supplement of frozen saline. Therefore, the invention is more economical, and is more applicable to industrial application.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a treatment method for tetrahydrofuran recovered from Grignard reaction. Background technique [0002] In the fine chemical production process, tetrahydrofuran is generally used as the solvent for the Grignard reaction, and tetrahydrofuran participates in the reaction, wherein the oxygen atom in tetrahydrofuran forms a coordination bond with the magnesium atom, which needs to be hydrolyzed to generate products, and at the same time free tetrahydrofuran is released. Through atmospheric or reduced pressure distillation, recovery of tetrahydrofuran containing water. Since the Grignard reaction requires anhydrous THF, the recovered THF containing water cannot be directly reused, and because THF is miscible with water and forms an azeotrope, the recovery and treatment of THF is generally quite difficult and expensive. [0003] At present, the recovery and treatment of tet...

Claims

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Application Information

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IPC IPC(8): C07D307/08
Inventor 夏玉良张建臣王景民夏文涛
Owner 河南华商药业有限公司
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