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Method for removing sensitive impurities in esters reagent and prolonging expiration date

A shelf life and reagent technology, applied in the separation/purification of carboxylic acid esters, organic chemistry, etc., can solve the problems of ester quality decline, short shelf life, waste of manpower and material resources, etc., to achieve large processing capacity, good preservation, and favorable preservation Effect

Active Publication Date: 2017-01-11
SINOPHARM CHEM REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, moisture, oxygen, acidic or alkaline gases in the atmospheric environment will dissolve into the product due to insufficient sealing during storage and transportation, which will further hydrolyze the ester, resulting in an increase in the content of impurities such as acid, water, and alcohol in the product, and a decrease in the quality of the ester. , resulting in short shelf life and unstable quality
[0003] In the process of scientific research and analysis, ester compounds stored for more than one year are often refined through deacidification, rectification and other operations, resulting in waste of manpower and material resources and environmental pollution.

Method used

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  • Method for removing sensitive impurities in esters reagent and prolonging expiration date

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The method of removing sensitive impurities in ethyl acetate to prolong the shelf life:

[0017] (1) Ethyl acetate flows through the free-flow electrophoresis device (600mm*800mm, operating voltage 110V, operating current 1A), the flow rate is 1000g per hour, and the treatment solution in the middle 50mm-750mm is collected;

[0018] (2) 1kg basic molecular sieve (16%KF / NaY: Na-MCM-41:10X is 40wt%: 5wt%: 55wt%) is loaded into a deacidification and drying column with a diameter of 50mm, and 45kg ethyl acetate is repeatedly passed through Column, product central control: acidity ≤ 0.0005mmol / g (calculated as H+), moisture ≤ 0.05%;

[0019] (3) Under the protection of nitrogen, the microfiltration is successively circulated through a 5 μm fiber microfiltration column, and then filtered through a 0.5 μm inorganic filter membrane, and then packaged to obtain the product.

Embodiment 2

[0021] The method of removing sensitive impurities in ethyl oxalate to prolong the shelf life:

[0022] (1) Ethyl oxalate flows through the free-flow electrophoresis device (600mm*800mm, operating voltage 110V, operating current 1.5A), the flow rate is 1000g per hour, and the treatment solution in the middle 100mm-700mm is collected;

[0023] (2) 1kg basic molecular sieve (16%KF / NaY: Na-MCM-41:10X is 40wt%: 6wt%: 54wt%) is loaded into a deacidification and drying column with a diameter of 50mm, and 35kg ethyl oxalate is repeatedly passed through Column, product central control: acidity ≤ 0.0005mmol / g (calculated as H+), moisture ≤ 0.05%;

[0024] (3) Under the protection of nitrogen, the microfiltration is successively circulated through a 5 μm fiber microfiltration column, and then filtered through a 0.5 μm inorganic filter membrane, and then packaged to obtain the product.

Embodiment 3

[0026] Methods to remove sensitive impurities in triacetin and prolong shelf life:

[0027] (1) Glyceryl triacetate flows through the free-flow electrophoresis device (600mm*800mm, operating voltage 110V, operating current 2A), the flow rate is 1000g per hour, and the treatment solution in the middle 100mm-700mm is collected;

[0028] (2) 1kg basic molecular sieve (16%KF / NaY: Na-MCM-41:10X is 45wt%: 5wt%: 50wt%) is loaded into a deacidification and drying column with a diameter of 50mm, so that 30kg triacetin is repeatedly Column passing, product control: acidity ≤ 0.0005mmol / g (calculated as H+), moisture ≤ 0.05%;

[0029] (3) Under the protection of nitrogen, the microfiltration is successively circulated through a 5 μm fiber microfiltration column, and then filtered through a 0.5 μm inorganic filter membrane, and then packaged to obtain the product.

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Abstract

The invention belongs to the technical field of fine chemical engineering, and particularly relates to a method for removing sensitive impurities in an esters reagent and prolonging expiration date. The method comprises the following steps: (1) enabling the esters reagent to flow through a free flow electrophoresis apparatus, and removing inorganic salt impurities in the esters reagent; (2) enabling the esters reagent to pass through a basic molecular sieve, and removing residual acid, water and organic matter impurities; and (3) carrying out microfiltration treatment on the esters reagent under the condition of nitrogen protection, and then packing in a sealed manner. The method is environmentally friendly and pollution-free, and is large in treatment amount, and the expiration date of treated esters products is long.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a method for removing sensitive impurities in ester reagents and prolonging the shelf life. Background technique [0002] Due to the synthesis process or environmental influence, the ester compound products contain acid, moisture, and trace inorganic salts. These impurities will cause the hydrolysis of the esters, and the inorganic salts have catalytic performance. In addition, moisture, oxygen, acidic or alkaline gases in the atmospheric environment will dissolve into the product due to insufficient sealing during storage and transportation, which will further hydrolyze the ester, resulting in an increase in the content of impurities such as acid, water, and alcohol in the product, and a decrease in the quality of the ester. , resulting in short shelf life and unstable quality. [0003] In the process of scientific research and analysis, ester compounds store...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/48C07C69/14C07C69/18C07C69/36
CPCC07C67/48C07C69/14C07C69/18C07C69/36
Inventor 郭建国凌芳陈宗艳马骏
Owner SINOPHARM CHEM REAGENT