Method for recovering tetrahydrofuran from Grignard reaction waste residue of magnesium chloride

A technology of tetrahydrofuran and Grignard reaction, applied in the direction of organic chemistry, can solve the problems of difficult separation of magnesium and tetrahydrofuran, inability to recycle tetrahydrofuran, large loss of tetrahydrofuran, etc., and achieve the effect of high price, large amount of consumption, and reduction of product raw material cost

Inactive Publication Date: 2010-02-03
SHANGHAI YIMIN CHEM
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  • Summary
  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0006] Stable in nature, even if heated above 100°C, it is difficult to separate magnesium from THF, and THF cannot be recovered
THF loss is lar

Method used

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  • Method for recovering tetrahydrofuran from Grignard reaction waste residue of magnesium chloride
  • Method for recovering tetrahydrofuran from Grignard reaction waste residue of magnesium chloride
  • Method for recovering tetrahydrofuran from Grignard reaction waste residue of magnesium chloride

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Experimental program
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Embodiment

[0035] Step 1, dissolving and distilling, tetrahydrofuran is freed from magnesium chloride waste residue:

[0036] Such as figure 1 Shown is a schematic diagram of the structure of a dissolving still, which includes a glass-lined reactor 1 with a volume of 3000L to 5000L. An anchor stirrer 2 is set inside the reactor 1, and a condenser 3 is provided in the still. device 3 is 10m 2 Enamel chip condenser, the distilled product is received by receiver.

[0037] Add 1500kg of Grignard reaction waste residue magnesium chloride and 3000kg of water into the reaction kettle 1 of the above-mentioned dissolving distillation kettle, start stirring after sealing, turn on the cooling water of the glass-lined sheet condenser 3, stir for about half an hour, all the solids are dissolved, and heat through the jacket steam , the internal temperature is about 70°C, until the tetrahydrofuran vaporizes, escapes from the solution, and enters the condenser 3 in the form of steam, and after being c...

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Abstract

The invention relates to a method for recovering tetrahydrofuran from Grignard reaction waste residue of magnesium chloride. The method comprises the following steps: (1) dissolving and distilling: respectively adding the waste residue of magnesium chloride and water to a reaction kettle; stirring to be fully dissolved; heating so that tetrahydrofuran solvent is dissociated and continuously vaporized; then, condensing into liquid, receiving to obtain a crude product A; (2) drying and dewatering: drying by alkali and a molecular sieve until water content is smaller than 0.1 percent; standing still and precipitating, transferring clear liquid at an upper layer to a filter; filtering to obtain a crude product B; (3) rectifying: transferring the crude product B to a tower kettle of a rectifying tower; heating to vaporize and regurgitate the tetrahydrofuran in the rectifying tower; slowly distilling a front cut fraction after regurgitation is lasted for 1-2 hours until the tetrahydrofuran content is larger than 99.8 percent, and starting to collect a boiling reagent to obtain the rectified tetrahydrofuran. The technical scheme of the invention greatly lowers the unit consumption of thetetrahydrofuran in the Grignard reaction and has simple and convenient treatment method and low cost.

Description

technical field [0001] The invention relates to a solvent recovery method, in particular to a method for recovering tetrahydrofuran from Grignard reaction waste residue magnesium chloride. Background technique [0002] In fine chemical production, the Grignard reaction is a very important reaction. The magnesium chloride solid waste produced in the reaction is generally difficult to recycle and the treatment cost is expensive. In industrial production, tetrahydrofuran is generally used as a solvent for Grignard reactions, but due to the formation of coordination bonds between oxygen atoms and magnesium atoms in tetrahydrofuran in the reaction, it can be expressed as [0003] [0004] Therefore, in the finally separated Grignard reaction waste residue magnesium chloride solid, each molecule of magnesium is combined with two molecules of tetrahydrofuran, which can be expressed as [0005] [0006] The property is stable, even if it is heated above 100°C, it is difficult...

Claims

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Application Information

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IPC IPC(8): C07D307/08
Inventor 王士杰周琦邵秀龙
Owner SHANGHAI YIMIN CHEM
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