High-purity carboxylic acid ester and method for producing same

Inactive Publication Date: 2018-09-27
MITSUBISHI GAS CHEM CO INC
4 Cites 2 Cited by

AI-Extracted Technical Summary

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 applicatio...
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Benefits of technology

[0017]In the high-purity carboxylic acid ester obtained by the method of the present invention, metal impurities and anionic impurities are highly reduced, and it can be suitably used for many applications in which a carboxylic acid ester is used, in particular, applications in the field of electronics industry. Specifically, it is used for a wide range of applications such as syn...
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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).

Application Domain

Ion-exchange process apparatusChromatographic cation exchangers +5

Technology Topic

Carboxylic esterCationic exchange +3

Image

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

Examples

  • Experimental program(9)

Example

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 metal and anion contents described therein were highly removed.

Example

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 understood that all the metal and anion contents described therein were highly removed.
[0032]Further, the amount of methyl hydroxyisobutyrate flowed through was increased. The anionic impurity concentrations after flowing through are shown in Table 3. According to Table 3, the anion content was highly removed during time between when flowing through was started and when the amount was 2000 ml, but the anion content was increased after the amount reached 2500 ml.

Example

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 flowing through was started and when the amount was 1500 ml, but the anion content was increased after the amount reached 1500 ml.
[0034]According to the results of Examples 2 and 3, the ability to remove the anion content can be more improved in Example 2 in which methyl hydroxyisobutyrate was flowed through the weakly basic anion-exchange resin (I) before it was flowed through the strongly acidic cation-exchange resin (II), and in addition, the life of the anion-exchange resin (III) can be improved.

PUM

PropertyMeasurementUnit
Fraction1.0E-9fraction
Fraction1.0E-6fraction
Fraction8.0E-9fraction

Description & Claims & Application Information

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