Process for preparation of esters solvent

An ester solvent and a technology for esterification reaction are applied in the field of high boiling point ester solvents and their preparation, which can solve the problems of low metal content and acid content, and achieve the effects of efficient preparation and simple purification operation.

Inactive Publication Date: 2009-08-26
DAICEL CHEM IND LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When used as a solvent in electronic materials such as semiconductor resists, color resists, and inkjet inks for LCDs, the metal content must be controlled at the ppb level. Conventional purification methods cannot fully meet the low metal requirements for electronic materials. content, acid content

Method used

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  • Process for preparation of esters solvent

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preparation example Construction

[0030] The preparation method of ester solvent

[0031] Hereinafter, the preparation method of the ester solvent of the present invention will be described with reference to the accompanying drawings when necessary. figure 1 It is a schematic diagram of an example of a device (batch distillation device) suitable for the preparation method of ester solvent of the present invention. Using this batch distillation apparatus, the reaction and subsequent distillation purification can be efficiently performed. exist figure 1 Among them, symbol 1 represents a distillation pot (hereinafter referred to as a distillation pot) capable of reacting alcohol and acid inside, symbol 2 represents a distillation tower, symbol 3 represents a vacuum unit, symbol 4 represents a decanter, and symbol 4-1 represents a decanter The water layer in the decanter, symbol 4-2 represents the organic layer in the decanter. Reference numeral 5 denotes a pump, and reference numerals 6 and 7 denote heat excha...

Embodiment 1

[0053] 100 parts by weight of cyclohexanol, 66 parts by weight of acetic acid, 2 parts by weight of p-toluenesulfonic acid monohydrate, and 19 parts by weight of isobutyl acetate were put into a still. The pressure at the top of the distillation column was decompressed to 40kPa.A for total reflux. If water is generated in the distillate, the distillate is subjected to liquid-liquid separation in a decanter. The organic layer was refluxed at the top of the tower, and the water layer was discharged from the system. When water is no longer generated, it is considered that the dehydration esterification reaction is completed, and the reaction stock solution is obtained.

[0054] The reaction stock solution was directly used figure 1 equipment for batch distillation. Isobutyl acetate and acetic acid were separated by overhead distillation. At this time, the reflux ratio is designed to be 0.5, the upper limit of the still temperature is 150°C, and the pressure is reduced step by...

Embodiment 2

[0057] 100 parts by weight of 1,3-butanediol, 147 parts by weight of acetic acid, 4 parts by weight of p-toluenesulfonic acid monohydrate, and 28 parts by weight of isobutyl acetate were put into a still. The pressure at the top of the distillation column was decompressed to 40kPa.A for total reflux. If water is generated in the distillate, the distillate is subjected to liquid-liquid separation in a decanter. The organic layer was refluxed at the top of the tower, and the water layer was discharged from the system. When water is no longer generated, it is considered that the dehydration esterification reaction is completed, and the reaction stock solution is obtained.

[0058] The reaction stock solution was directly used figure 1 equipment for batch distillation. Isobutyl acetate and acetic acid were separated by overhead distillation. At this time, the reflux ratio is designed to be 0.5, the upper limit of the still temperature is 150°C, and the pressure is reduced step...

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Abstract

The present invention provides high boiling point esters solvent with low content of sodium and acid and high-efficiency industry method for preparing the same. The esters solvent can be used in electronic material field with requirement of high-purity quality. Process for preparation of esters solvent is, at the presence of acid catalyst, putting the esterification reaction stock solution got from esterification of alcohol and acid into distilling tower and distilling to get esters solvent, wherein, the reaction stock solution used for distil purifying without neutralization treatment, and after removing low boiling point ingredients by distillation, distilling off the esters solvent via sidetrack distillate pipe disposed in central part of the distilling tower.

Description

technical field [0001] The invention relates to a high-purity high-boiling-point ester solvent required for electronic materials such as semiconductor resists, color resists, and ink-jet inks for LCDs and a preparation method thereof. Background technique [0002] The ester solvent is prepared by the dehydration reaction of alcohol and acid. This reaction is usually carried out in the presence of an acid catalyst. In order to prepare a high-purity ester solvent, distillation and purification are usually carried out after the reaction. However, when the above-mentioned ester has a high boiling point, there is a problem that the acid content increases due to thermal deterioration during distillation (thermal decomposition of the ester, etc.). In a system where an acid catalyst exists, the thermal decomposition of the product is obvious. In order to efficiently prepare high-purity ester solvents, the acid catalyst must be removed before distillation. Conventionally, as a metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C67/54C07C69/14C07C69/16
CPCC07C67/08C07C67/54
Inventor 牧泽克宪
Owner DAICEL CHEM IND LTD
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