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Method for preparing gradient grade acetonitrile

An acetonitrile and gradient technology, applied in the purification/separation of carboxylic acid nitriles, organic chemistry, etc., can solve the problems of difficult treatment, secondary pollution of the environment, and large amount of adsorbent usage, and achieve fewer processing steps, reduced production costs, and overall Effect of Yield Improvement

Active Publication Date: 2018-04-20
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above-mentioned methods, in the process of preparing gradient-grade acetonitrile from industrial acetonitrile, the adsorption method has been adopted, but the types of adsorbents used are different. Because the output of gradient-grade acetonitrile in industrial production is relatively large, the amount of adsorbent used is also relatively large. A large amount of solid waste will be generated, causing secondary pollution to the environment
Some enterprises also use fuming sulfuric acid as a water-absorbing agent, which will produce a large amount of high-concentration waste acid containing nitrile, which is difficult to deal with.

Method used

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  • Method for preparing gradient grade acetonitrile
  • Method for preparing gradient grade acetonitrile
  • Method for preparing gradient grade acetonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Add industrial acetonitrile to the hydrolysis-oxidation reaction kettle, and add anhydrous sodium hydroxide accounting for 3.5% of industrial acetonitrile, heat and reflux for 2 hours, add potassium permanganate accounting for 1.5wt ‰ of industrial acetonitrile and heat to reflux After 2 hours, 5% of the former fraction was removed by heating and distillation, and 90 wt% of the crude fraction was collected.

[0034] (2) Add this fraction to the acid-base regulating tank again, neutralize to solution acidity 0.015mmol / 100g with 98wt% sulfuric acid accounting for crude fraction 1wt‰, then, heat distillation to remove the former fraction of 5% amount, collect and obtain 90wt % of fractions.

[0035] (3) Enter the rectifying device through the acetonitrile treated by acid adjustment, reflux for 2 hours, then remove 10% of the amount of the front fraction with the reflux ratio of 12:1, and collect the gradient grade of 85wt% amount with the reflux ratio of 8:1 Acetonitr...

Embodiment 2

[0039] (1) Add industrial acetonitrile to the hydrolysis-oxidation reaction kettle, and add anhydrous sodium hydroxide accounting for 1.5% of industrial acetonitrile, heat and reflux for 2 hours, add potassium permanganate accounting for 1.5wt ‰ of industrial acetonitrile and heat to reflux After 2 hours, 5% of the former fraction was removed by heating and distillation, and 90 wt% of the crude fraction was collected.

[0040] (2) Add this fraction to the acid-base regulating kettle again, neutralize to solution acidity 0.015mmol / 100g with 98wt% sulfuric acid accounting for crude fraction 0.5wt‰, then, heat and distill to remove the former fraction of 5% amount, collect and obtain 90 wt% fraction.

[0041](3) Enter the rectification device through the acetonitrile treated by acid adjustment, and reflux for 2 hours. Then, remove 10% of the front fraction with a reflux ratio of 12:1, and collect a gradient of 85% wt with a reflux ratio of 8:1 grade acetonitrile. The total yiel...

Embodiment 3

[0045] (1) Add industrial acetonitrile to the hydrolysis-oxidation reaction kettle, and add anhydrous sodium hydroxide accounting for 3.5% of industrial acetonitrile, heat and reflux for 2 hours, add potassium permanganate accounting for 1.5wt ‰ of industrial acetonitrile and heat to reflux After 2 hours, 5% of the former fraction was removed by heating and distillation, and 90% of the crude fraction was collected.

[0046] (2) the cut is added to the acid-base adjustment kettle again, neutralized to solution acidity 0.01mmol / 100g with 98wt% sulfuric acid accounting for the crude fraction 2wt‰, then, the preceding cut of 5% amount is removed by heating and distillation, and 90% is collected % of fractions.

[0047] (3) Enter the rectification device through the acetonitrile treated by acid adjustment, and reflux for 2 hours. Then, remove 10% of the front fraction with a reflux ratio of 12:1, and collect a gradient of 85% wt with a reflux ratio of 8:1 grade acetonitrile. The ...

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Abstract

The invention discloses a method for preparing gradient grade acetonitrile. The method disclosed by the invention comprises the following steps: carrying out a hydrolysis reaction between a commercialproduct acetonitrile and a strong base under reflux conditions, and directly adding potassium permanganate into the hydrolysis system to continuously perform heating reflux so as to carry out an oxidizing reaction; distilling to obtain a coarse acetonitrile fraction after the oxidizing reaction is ended, regulating the pH value of the coarse acetonitrile fraction with 98wt% sulfuric acid, neutralizing carboxylate entrained in distillation in the previous section into carboxylic acid, and distilling to collect the fraction; and finally, enabling the collected fraction to enter a rectifying still to be rectified, thereby obtaining the gradient grade acetonitrile. According to the method disclosed by the invention, the gradient grade acetonitrile can be efficiently obtained, and the gradientgrade acetonitrile is high in yield.

Description

technical field [0001] The invention relates to the technical field of solvent refining, in particular to a method for preparing gradient grade acetonitrile. Background technique [0002] Gradient-grade acetonitrile is one of the mobile phases commonly used in high performance liquid chromatography. Therefore, gradient-grade acetonitrile is required to have the characteristics of high purity and low UV absorption. With the development of my country's chemical industry, the purity detection of chemical products is used as mobile phase. The amount of acetonitrile is increasing, but there are very few companies in my country that can produce gradient-grade acetonitrile, and gradient-grade acetonitrile is mainly imported to meet the demand. In addition, the pretreatment in the prior art of preparing gradient grade acetonitrile all adopts adsorption process, because, the use amount of adsorbent is large, regeneration efficiency is low, will produce a large amount of adsorbent soli...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/03C07C253/34
CPCC07C253/34C07C255/03
Inventor 金东元李润航许兆华魏丽胡晓钧
Owner SHANGHAI INST OF TECH