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Recovering process for Gram-waste water

A waste water and process technology, applied in water/sewage treatment, water/sludge/sewage treatment, chemical instruments and methods, etc., can solve the problems of polluting the environment, difficult separation and recycling, etc., achieve high yield, reduce three wastes, Simple to use effects

Inactive Publication Date: 2005-08-03
ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the water phase of the Grignard reaction contains a large amount of chlorine, bromine, and magnesium ions, it is difficult to separate and recover, forming a large amount of Grignard wastewater and polluting the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] In a 1000 ml three-necked flask, add 200 ml of anhydrous ether, 22 g of magnesium and 110 g of bromoethane, then stir for 0.5 hour, then slowly add 100 ml of ether solution containing 39.6 g of methylheptenyl alcohol, stir 3 hours, then dropwise added 100 milliliters of diethyl ether solution containing 72 grams of C14 aldehyde, stirred for another 2.5 hours, controlled temperature at 60° C., then added 500 milliliters of aqueous solution containing 120 grams of ammonium bromide for hydrolysis. Separate the layers, and recover the solvent from the organic phase to obtain 94 g of the product, with a yield of 91%. The aqueous phase was first concentrated, then 220 grams of concentrated sulfuric acid was added, and then 100 grams of absolute ethanol was added dropwise at 100° C. to obtain 210 grams of bromoethane with a yield of 96%. Then the reactant was cooled to 20° C., suction filtered, and dried to obtain 93 grams of magnesium sulfate, with a yield of 98%.

Embodiment 3

[0018] In a 1000 ml three-necked flask, add 200 ml of anhydrous ether, 22 g of magnesium and 110 g of bromoethane, then stir for 0.5 hour, then slowly add 100 ml of ether solution containing 39.6 g of methylheptenyl alcohol, stir After 3 hours, 100 milliliters of ether solution containing 72 grams of C14 aldehyde was added dropwise, stirred for another 2.5 hours, and the temperature was controlled at 60° C. Then, 400 milliliters of aqueous solution containing 120 grams of ammonium bromide was added for hydrolysis. Separate the layers, and recover the solvent from the organic phase to obtain 94 g of the product, with a yield of 91%. The aqueous phase was first concentrated, then 200 grams of concentrated sulfuric acid was added, and then 100 grams of absolute ethanol was added dropwise at 90° C. to obtain 205 grams of bromoethane with a yield of 93%. Then the reactant was cooled to 30° C., suction filtered, and dried to obtain 90 g of magnesium sulfate with a yield of 95%.

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PUM

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Abstract

The present invention discloses Grignard process of recovering waste water as one radically improved technological process. The Grignard process includes hydrolysis with ammonium bromide aqua to recover bromine ion via preparing bromoethane and recovering magnesium ion via preparing magnesium sulfate, so as to recover ions from Grignard waste water. The said process is simple, high in yield and low in cost.

Description

technical field [0001] The invention relates to a new process for recovering waste water in Grignard reaction. Background technique [0002] The Grignard reaction is an important class of reactions for the preparation of various alcohols. In the production of vitamin A, β-carotene, vitamin E and other products, Grignard reaction is often used for synthesis. For example, in the synthesis of vitamin A, Roche company adopts the technical route of C14+C6, that is, C14 aldehyde and C6 alcohol undergo Grignard reaction to obtain the key intermediate of vitamin A, and then undergo partial hydrogenation, acetylation, bromination, hydrolysis, etc. Get vitamin A. The process is mature and the yield is relatively stable. It is the main production method of vitamin A in the world. The key to this reaction is the Grignard reaction. In the traditional method, C6 alcohol, magnesium and ethyl bromide are often used to react to form a Grignard reagent, whic...

Claims

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Application Information

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IPC IPC(8): C02F1/58
Inventor 李浩然陈志荣胡柏剡
Owner ZHEJIANG UNIV
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