Method for recovering and refining sodium bromide from dipropyl cyanoacetate mixture

A technology of dipropyl cyanoacetate and mixture, which is applied in the direction of alkali metal bromide, etc., can solve the problems that sodium bromide color impurities and organic impurities cannot be completely removed, and are easy to agglomerate, and achieve less impurities, white color, The effect of high purity

Active Publication Date: 2015-05-27
湖南省湘中制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is: sodium bromide color impurities and organic impurities cannot be

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Centrifuge and separate 2000L of dipropyl cyanoacetate mixture, dissolve about 240kg of sodium bromide collected in 300L of water, add hydrobromic acid to adjust the pH value to 6-6.5, stir for 5 minutes, add propyl ether 20 ㎏, 10kg of n-pentane, vigorously stirred for 30 minutes, and allowed to stand for stratification. Separate the water layer and pump it into the decolorization tank, heat up to boil for 1 hour, cool to 80°C, add 7 kg of activated carbon and diatomaceous earth mixed decolorizer (weight ratio 1:0.4), keep at 75-80°C for 1 hour for decolorization, and filter. The filtrate was spray-dried to obtain white powder anhydrous sodium bromide.

Embodiment 2

[0017] Dissolve 100kg of sodium bromide collected by centrifugation in 150kg of water, add hydrobromic acid to adjust the pH to 6-6.5, stir for 5 minutes, add 6kg of propyl ether and 3kg of petroleum ether, and stir vigorously for 30 minutes. Let stand to layer. Separate the water layer, pump it into the decolorization tank, heat up and boil for 1 hour, cool to 80°C, add 1kg of activated carbon and 0.4kg of diatomaceous earth, keep at 75-80°C for 30 minutes for decolorization, and filter. Add 54 kg of isopropanol to the filtrate, stir evenly, add 200 kg of concentrated sulfuric acid at 10-15 °C dropwise, raise the temperature to 65 °C and keep it for 3 hours, then distill. The distillate was washed with water, dried with anhydrous sodium sulfate, and filtered to obtain 2-bromopropane.

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Abstract

The invention provides a method for recovering refining sodium bromide from dipropyl cyanoacetate mixture. The method comprises the following steps: filtering a dipropyl cyanoacetate mixture containing sodium bromide, filtering and colleting sodium bromide, dissolving sodium bromide, adjusting the pH value to 6-6.5 by hydrobromic acid, adding an extraction agent of an ether and alkane mixture, stirring for mixing, standing and layering; separating water liquid, boiling, cooling to 80 DEG C, adding an active carbon and diatomite mixed decolorizing agent, decolorizing at 50-80 DEG C, filtering, and conducting spray drying on the filtrate to obtain a white powdered anhydrous sodium bromide with high purity and high recycling rate.

Description

technical field [0001] The invention relates to a method for recovering and refining sodium bromide from dipropyl cyanoacetate mixtures. Background technique [0002] A large amount of by-products sodium bromide, ethanol and a small amount of monopropyl cyanoacetate, sodium monopropyl cyanoacetate, sodium dipropyl cyanoacetate, etc. are produced in the production process of dipropyl cyanoacetate, and the product mixture also includes Various organic impurities and colored impurities brought by raw materials. The by-product sodium bromide is a solid substance in the mixture, which was usually recovered by filtration or centrifugal separation and then drying in the past. Recovered sodium bromide directly replaces industrial sodium bromide for recycling in the preparation of hydrobromic acid, organic bromides such as brominated alkanes, etc., and the bromide products produced in this way often contain many impurities, which affect subsequent production, such as low yield, The...

Claims

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Application Information

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IPC IPC(8): C01D3/10
Inventor 尹文乐曾慧罗聪
Owner 湖南省湘中制药有限公司
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