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High-purity carboxylic acid ester and method for producing same

Inactive Publication Date: 2018-09-27
MITSUBISHI GAS CHEM CO INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patent describes a way to make a high-purity carboxylic acid ester with low levels of metal and anionic impurities. This makes it suitable for a wide range of applications, including in the electronics industry for use as synthetic raw materials, cleaning agents, and solvents. It can also be used as a treatment agent in the production of integrated circuits. The technical effect of this patent is to provide a more purified carboxylic acid ester to meet the demands of various industrial applications.

Problems solved by technology

However, carboxylic acid esters conventionally used have high concentrations of metal impurities and anionic impurities, and have problems in which, for example, these cannot be used in applications for semiconductors.
Therefore, the method is insufficient as a method for purifying a carboxylic acid ester.
However, the Na concentration after purification is 50 ppb or less and does not satisfy the concentration of metal impurities required for applications for semiconductors (1 ppb or less), and therefore the method is insufficient as a method for purifying a carboxylic acid ester.
However, the document describes only Fe and Pd as metal impurities that can be removed, and does not describe removal of impurities including other alkali metals.
Therefore, the method is insufficient as a method for purifying a carboxylic acid ester.
Thus, there is no known method for highly purifying a carboxylic acid ester.

Method used

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  • High-purity carboxylic acid ester and method for producing same

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0030]As a pretreatment, each of an H-type strongly acidic cation-exchange resin (trade name: 15JS-HG DRY, manufactured by Organo Corporation) and a free base type weakly basic anion-exchange resin (trade name: B20-HG DRY, manufactured by Organo Corporation) was put into ethyl lactate separately and immersed therein for 1 hour or longer while being gently stirred suitably. After that, one FEP column having an inner diameter of 16 mm was filled with 10 ml of strongly acidic cation-exchange resin, and each of two FEP columns having an inner diameter of 16 mm was filled with 10 ml of weakly basic anion-exchange resin. After that, ethyl lactate was flowed through the weakly basic anion-exchange resin (I), the strongly acidic cation-exchange resin (II) and the weakly basic anion-exchange resin (III) in this order at 25° C. with SV=20 Hr−1 as shown in FIG. 1. Respective concentrations of impurities after flowing through are shown in Table 1. From Table 1, it is understood that all the met...

example 2

[0031]As a pretreatment, each of an H-type strongly acidic cation-exchange resin (trade name: 15JS-HG DRY, manufactured by Organo Corporation) and a free base type weakly basic anion-exchange resin (trade name: B20-HG DRY, manufactured by Organo Corporation) was put into methyl hydroxyisobutyrate separately and immersed therein for 1 hour or longer while being gently stirred suitably. After that, one FEP column having an inner diameter of 16 mm was filled with 10 ml of strongly acidic cation-exchange resin, and each of two FEP columns having an inner diameter of 16 mm was filled with 10 ml of weakly basic anion-exchange resin. After that, methyl hydroxyisobutyrate was flowed through the weakly basic anion-exchange resin (I), the strongly acidic cation-exchange resin (II) and the weakly basic anion-exchange resin (III) in this order at 25° C. with SV=20 Hr−1 as shown in FIG. 1. Respective concentrations of impurities after flowing through are shown in Table 2. From Table 2, it is und...

example 3

[0033]An H-type strongly acidic cation-exchange resin (trade name: 15JS-HG DRY, manufactured by Organo Corporation) and a free base type weakly basic anion-exchange resin (trade name: B20-HG DRY, manufactured by Organo Corporation) were pretreated with methyl hydroxyisobutyrate in a manner similar to that in Example 2. After that, one FEP column having an inner diameter of 16 mm was filled with 10 ml of strongly acidic cation-exchange resin, and another FEP column having an inner diameter of 16 mm was filled with 10 ml of weakly basic anion-exchange resin. After that, methyl hydroxyisobutyrate was flowed through the strongly acidic cation-exchange resin (II) and the weakly basic anion-exchange resin (III) in this order at 25° C. with SV=20 Hr−1. Respective concentrations of impurities after flowing through are shown in Table 4. From Table 4, it is understood that all the metals described therein were highly removed. The anion content was highly removed during time between when flowi...

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Abstract

The present invention makes it possible to provide a high-purity carboxylic acid ester in which the Ag, Al, Au, Ca, Cr, Cu, Fe, K, Mg, Na, Sn, and Zn contents as metal impurity contents are each less than 1 ppb and the anionic impurity content is less than 1 ppm. The present invention also makes it possible to provide a method for producing a high-purity carboxylic acid ester, the method including a step for bringing a crude carboxylic acid ester that contains anionic impurities and Ag, Al, Au, Ca, Cr, Cu, Fe, K, Mg, Na, Sn, and Zn as metal impurities into contact with a cation-exchange resin (II), followed by a step for bringing the crude carboxylic acid ester into contact with an anion-exchange resin (III).

Description

TECHNICAL FIELD[0001]The present invention relates to a method for purifying a carboxylic acid ester, wherein the metal impurity content and the anionic impurity content are reduced. The carboxylic acid ester of the present invention is useful for a wide range of applications such as synthetic raw materials, cleaning agents for electronic components and solvents for paints, adhesives and the like. Further, it is used as a treatment agent for cleaning of a semiconductor substrate, etching, development of a photoresist and the like in the production of integrated circuits and large-scale integrated circuits. In particular, in applications for semiconductors, very high purity is required because of contamination of semiconductor substrates, and a high-purity carboxylic acid ester containing impurities in an amount as small as possible is required.BACKGROUND ART[0002]However, carboxylic acid esters conventionally used have high concentrations of metal impurities and anionic impurities, ...

Claims

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Application Information

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IPC IPC(8): C07C67/56C07C69/68B01J39/26B01J41/20
CPCC07C67/56C07C69/68B01J39/26B01J41/20B01J47/028B01J41/07C07C69/675B01J39/05B01J39/18B01J41/12
Inventor MUNEYASU, KUNIAKI
Owner MITSUBISHI GAS CHEM CO INC
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