A method for recovering magnesium chloride and co-producing tetrahydrofuran from Grignard reaction waste residue

A technology of tetrahydrofuran and Grignard reaction, applied in magnesium chloride, magnesium halide, organic chemistry and other directions

Active Publication Date: 2021-05-18
SHANDONG WEIFANG RAINBOW CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It not only solves the problem of solid waste pollution, but also obtains high-value products without secondary pollution, creating higher economic benefits and meeting the requirements of sustainable development

Method used

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  • A method for recovering magnesium chloride and co-producing tetrahydrofuran from Grignard reaction waste residue
  • A method for recovering magnesium chloride and co-producing tetrahydrofuran from Grignard reaction waste residue
  • A method for recovering magnesium chloride and co-producing tetrahydrofuran from Grignard reaction waste residue

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Experimental program
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Effect test

Embodiment 1

[0025] Embodiment 1: carry out experiment as follows:

[0026] 1) Dissolving: In pass N 2 Under the condition of protection, the complex waste residue is added to the dissolving water at a rate of 10-100kg / min, and a small amount of hydrogen peroxide is added to the dissolving water to oxidize trimethylphosphorus into stable trimethylphosphine. The fully reacted trimethylphosphorus can be oxidized and absorbed by entering the tail gas spray absorption device with nitrogen; the rate of waste residue feeding is controlled during the dissolution process, and at the same time, circulating water is passed outside the dissolution kettle to cool down, and the dissolution temperature is controlled below 40°C;

[0027] 2) Recovery of tetrahydrofuran by rectification: The dissolved material is rectified to recover tetrahydrofuran. During rectification, the liquid phase temperature is 68-75 °C and the material starts to boil, and the gas phase temperature is 62-63 °C to collect fractions...

Embodiment 2

[0031] Three batches of experiments were carried out using the above steps, and the experimental results are as follows:

[0032]

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Abstract

The invention relates to a method for recovering magnesium chloride and co-producing tetrahydrofuran from Grignard reaction waste residue. The method comprises the following specific steps: step 1, dissolving: passing through N 2 Under the condition of protection, the waste residue of the complex is gradually added to the dissolved water, and a small amount of hydrogen peroxide is added to the dissolved water to oxidize trimethylphosphorus into stable trimethylphosphine, and a small amount of unreacted trimethylphosphorus can be Nitrogen enters the tail gas spray absorption device to be oxidized and absorbed; step 2, rectification and recovery of tetrahydrofuran: the dissolved material is rectified to recover tetrahydrofuran, and then a small amount of water is distilled to achieve the crystallization state of the substrate; step 3, magnesium chloride hexahydrate slices: bottom After the temperature of the product rises to a certain temperature, the solidification crystallization condition of magnesium chloride hexahydrate is reached, and it can be directly cooled and sliced ​​to obtain magnesium chloride hexahydrate. By adopting the technical scheme of the invention, while recovering the magnesium chloride in the Grignard reaction waste residue, tetrahydrofuran can be co-produced to increase the recovery benefit.

Description

technical field [0001] The invention relates to a method for recovering magnesium chloride from Grignard reaction waste residue to co-produce tetrahydrofuran, and belongs to the field of solid waste resource utilization. Background technique [0002] In the field of fine chemical industry, Grignard reaction is a commonly used reaction in the production of chemical products, but in the process of Grignard reaction, solid pollutants of magnesium chloride will be produced, which contain tetrahydrofuran and other substances. If not handled properly, it will be Serious pollution to the environment. [0003] Patent CN101638400B "A Method for Recovering THF from Grignard Reaction Waste Residue Magnesium Chloride" introduces a method for recovering tetrahydrofuran from Grignard reagents, first distilling and then rectifying, and purifying tetrahydrofuran products with a purity of up to 99.8% from the waste residue. Although this method is good, it does not fundamentally solve the p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F5/30C07D307/08
CPCC01F5/30C01P2006/80C07D307/08
Inventor 孙国庆侯永生宋伟庞立飞时成义李盼盼
Owner SHANDONG WEIFANG RAINBOW CHEM
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