Method for preparing isooctanoic acid

A technology of isooctanoic acid and octanoic acid, used in the preparation of carboxylate, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of long reaction time, low yield, poor catalytic effect, etc., and achieve reasonable recovery and utilization of products. The effect of high purity and short reaction time

Inactive Publication Date: 2008-02-20
河南庆安化工高科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the process of synthesizing isooctanoic acid can be roughly divided into two types: one is to produce isooctyl aldehyde or isooctenal as a raw material, but because isooctyl aldehyde is mostly an intermediate in the chemical production process, there is no commercial product supply, Therefore this method is more suitable for large-scale chemical production with the intermediate product isooctylaldehyde; the other is to catalyze the production of isooctanoic acid with octanol as raw material, such as potassium permanganate oxidation method, nitric acid oxidation method, high-pressure dehydrogenation oxidation method , Atmospheric pressure dehydrogenation oxidation method, catalytic dehydrogenation oxidation method, but these processes often have problems such as long reaction time, poor catalytic effect, low yield, unreasonable discharge of waste residue and exhaust gas, and difficulty in large-scale production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 250g of isooctyl alcohol, 172g of caustic soda, 1.6g of zinc acetate, and then add 250g of isooctyl alcohol into a 2000ml autoclave. After condensing, discharge it outside. When no hydrogen gas is released during the reaction, keep the pressure for 40 minutes, lower the temperature to below 120°C, then reduce the pressure in the kettle to normal pressure, add 500ml of distilled water, and stir for 30 minutes to obtain an aqueous solution of sodium isooctanoate.

[0019] Add 350g of distilled water to another flask, slowly add 250g of concentrated sulfuric acid under stirring, keep the temperature in the flask not exceeding 80°C, slowly pour the reactants in the autoclave into the flask, control the reaction temperature to 70°C, react for 40min, and move to Separating funnel, keep the temperature at rest for 1 hour, then separate layers to remove the water phase, recover the refined sodium sulfate after water phase treatment; wash the oil phase with distilled water at...

Embodiment 2

[0021] Add 300g of isooctyl alcohol, 220g of caustic soda, 2.4g of zinc acetate, and then add 300g of isooctyl alcohol into a 2000ml autoclave. The reactor is filled with nitrogen, and the reaction is carried out at 260°C and 3.2MPa. After condensing, discharge it outside. When no hydrogen gas is released during the reaction, keep the pressure for 50 minutes, lower the temperature to below 120°C, then reduce the pressure in the kettle to normal pressure, add 500ml of distilled water, and stir for 30 minutes to obtain an aqueous solution of sodium isooctanoate.

[0022] Add 350g of distilled water into another flask, slowly add 250g of concentrated sulfuric acid under stirring, keep the temperature in the flask not exceeding 80°C, slowly pour the reactants in the autoclave into the flask, control the reaction temperature to 70°C, react for 30min, and move to Separating funnel, keep the temperature at rest for 1 hour, then separate layers to remove the water phase, recover the re...

Embodiment 3

[0024] Add 400g of iso-octanol, 280g of caustic soda, 3.25g of zinc acetate, and then add 400g of iso-octanol into a 2000ml high-pressure reactor, fill the reactor with nitrogen, and carry out the reaction at 255°C and 3MPa, and the generated hydrogen is condensed After the reaction, when no hydrogen gas is released, keep the pressure for 30 minutes, lower the temperature to below 120°C, then reduce the pressure in the kettle to normal pressure, add 500ml of distilled water, and stir for 30 minutes to obtain an aqueous solution of sodium isooctanoate.

[0025] Add 400g of distilled water to another flask, slowly add 330g of concentrated sulfuric acid under stirring, keep the temperature in the flask not exceeding 80°C, slowly pour the reactants in the autoclave into the flask, control the reaction temperature to 70°C, react for 40min, and move to Separating funnel, keep the temperature at rest for 1 hour, then separate layers to remove the water phase, recover the refined sodiu...

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Abstract

The invention relates to an isooctyl acid preparation method: isooctyl alcohol and sodium hydroxide are positioned in an inert atmosphere for reaction, with zinc acetate being the catalyst and the temperature being 250-260 DEG C and the pressure being 2.8-3.2 MPa, until no hydrogen is produced, after which the reaction continues under the same pressure for 30-50min, then the reaction product is acidized at normal pressure and at a temperature of 65-80 DEG C, thereby acquiring the crude isooctyl acid which is finely distilled and purified to produce the fine isooctyl acid. The reaction time of the method is short, and the production cycle is essentially confined to 8-10 hours; the method has high purity, as much as 99.5 percent, high yield, fundamentally non-pollution and reasonably recyclable by-products.

Description

(1) Technical field [0001] The invention relates to a preparation method of isooctanoic acid. (2) Background technology [0002] At present, the process of synthesizing isooctanoic acid can be roughly divided into two types: one is to produce isooctyl aldehyde or isooctenal as a raw material, but because isooctyl aldehyde is mostly an intermediate in the chemical production process, there is no commercial product supply, Therefore this method is more suitable for large-scale chemical production with the intermediate product isooctylaldehyde; the other is to catalyze the production of isooctanoic acid with octanol as raw material, such as potassium permanganate oxidation method, nitric acid oxidation method, high-pressure dehydrogenation oxidation method , Atmospheric pressure dehydrogenation oxidation method, catalytic dehydrogenation oxidation method, but these processes often have problems such as long reaction time, poor catalytic effect, low yield, unreasonable discharge...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/126C07C51/00
Inventor 刘冰宋广勋司俊杰姚俊营王艳丽
Owner 河南庆安化工高科技股份有限公司
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