Preparation method for high-purity isocaprylic acid

A technology of isooctanoic acid and high purity, applied in the field of preparation of isooctanoic acid, can solve the problems of low product purity, poor quality, difficult removal of 2-ethylhexenoic acid, etc., and achieve the effect of simple process and high product quality

Active Publication Date: 2019-03-08
WANHUA CHEM GRP CO LTD
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0010] The object of the present invention is to provide a kind of preparation method of high-purity isooctanoic acid, to solve the difficult removal of impurity 2-ethylhexenoic acid in isooctanoic acid in the production process of isooctanoic acid at present, the problem such as product purity is low, poor quality

Method used

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  • Preparation method for high-purity isocaprylic acid

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Effect test

Embodiment 1

[0035] 2-Ethylhexanal hydrogenation solution obtained by condensation and hydrogenation of n-butyraldehyde, a total of 100g, wherein the content of 2-ethyl-2-hexenal is 0.1wt%, 2-ethyl-3-hydroxyhexanal Content 0.1wt%, 2-ethylhexanal content 90wt%, other 9.8wt%. The hydrogenation solution was mixed with 2g of water, added to the reaction kettle, mixed with 2g of acid clay powder catalyst, the reaction temperature was 100°C, and reacted for 30min, and the catalyst powder was separated from the reaction solution to obtain a mixture solution.

[0036] In a dry 1L three-neck flask, add 80g of the above-mentioned 2-ethylhexanal mixture, place it in a water bath, and stir it mechanically under a nitrogen atmosphere. After the temperature rises to 30°C, start to introduce air with a flow rate of 11.6g / h, keep the reaction temperature at 30-35°C by adding cooling water to the water bath, and react at normal pressure for 8 hours to obtain the 2-ethylhexanoic acid oxidation reaction sol...

Embodiment 2

[0038] 2-Ethylhexanal hydrogenation solution obtained by condensation and hydrogenation of n-butyraldehyde, a total of 100g, wherein the content of 2-ethyl-2-hexenal is 0.5wt%, 2-ethyl-3-hydroxyhexanal Content 0.2wt%, 2-ethylhexanal content 91wt%, other 8.3wt%. The hydrogenation solution is mixed with 5g of water, and sent into a tubular reactor filled with 10mL cation exchange resin, and the space velocity of the hydrogenation solution mixture is 1.0h -1 , the reaction temperature is 130°C, and a mixture solution is obtained after the reaction.

[0039] In a dry 1L three-neck flask, add 80g of the above-mentioned 2-ethylhexanal mixture, place it in a water bath, and stir it mechanically under a nitrogen atmosphere. After the temperature rises to 30°C, start to introduce air with a flow rate of 12.2g / h, keep the reaction temperature at 30-35°C by adding cooling water to the water bath, and react at normal pressure for 6 hours to obtain the 2-ethylhexanoic acid oxidation reac...

Embodiment 3

[0041] 2-Ethylhexanal hydrogenation liquid obtained by condensation and hydrogenation of n-butyraldehyde, a total of 100g, wherein the content of 2-ethyl-2-hexenal wt1%, the content of 2-ethyl-3-hydroxyhexanal 0.3wt%, 2-ethylhexanal content 92.5wt%, other 6.2wt%. The hydrogenation solution was mixed with 8g of water, and sent into a tubular reactor filled with 10mL acidic alumina particle catalyst. The space velocity of the hydrogenation solution mixture was 2.0h-1, and the reaction temperature was 150°C. After the reaction, a mixture solution was obtained.

[0042] According to the method of Example 1, the mixture was oxidized by air to obtain the 2-ethylhexanoic acid oxidation reaction solution, which was subjected to vacuum distillation and separation, and the water and 2-ethyl-3-hydroxyhexanoic acid were first separated under normal pressure. The azeotrope was separated by rectification under reduced pressure. The pressure was 5000 Pa (gauge pressure), the reflux ratio was...

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Abstract

The invention provides a preparation method for high-purity isocaprylic acid. The preparation method for the high-purity isocaprylic acid is characterized by comprising the following steps: mixing 2-ethyl hexanal which is obtained by performing condensation and hydrogenation on n-butyl aldehyde and a certain amount of water; then, enabling the mixture to be in contact with an acid catalyst, so that a small amount of 2-ethyl-2-hexanal contained in the 2-ethyl hexanal is converted into 2-ethyl-3-hydroxyl-hexanal; then, oxiding the treated 2-ethyl hexanal mixture, and then performing rectification and separation; and enabling the 2-ethyl-3-hydroxyacetic acid to be azeotropic with the water to separate the 2-ethyl-3-hydroxyacetic acid from isocaprylic acid so as to purify the isocaprylic acid.Through the method, a high-purity and high-quality isocaprylic acid product can be obtained; and moreover, the process flow is simple and the method can be used for industrial production.

Description

technical field [0001] The invention relates to a preparation method of isooctanoic acid, which belongs to the field of product purification. Background technique [0002] Isooctanoic acid is an important organic chemical product, which can be widely used in coatings, plastics, leather, medicine, wood, chemical fiber, pesticides and other fields, but most of it is used to produce metal salts of isooctanoic acid. Because isooctanoate has a more obvious drying effect than naphthenate, it is widely used in the coating industry to meet people's demand for high-grade light-colored coatings. In medicine, isooctanoic acid is mainly used as a salt-forming reagent for the synthesis of penicillin sodium salt by solvent method. In addition, glyceryl isooctanoate is an excellent plasticizer. With the development of industry and agriculture, the demand for isooctanoic acid is increasing year by year, which has great potential for development. [0003] The industrial production of isooc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/235C07C51/44C07C53/126C07C45/74C07C47/21C07C45/69C07C47/02
CPCC07C45/69C07C45/74C07C51/235C07C51/44C07C53/126C07C47/21C07C47/02
Inventor 刘超丛鑫何光文王泽圣董科崔乾王鹏余炎冰
Owner WANHUA CHEM GRP CO LTD
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