Synthesis process of pentaerythritol tetra(2-ethylhexanoate)

A technology of pentaerythritol tetra- and isooctanoate, which is applied in the separation/purification of carboxylic acid esters, the preparation of carboxylic acid esters, and the preparation of organic compounds, etc., and can solve the problems of non-compliance with green chemistry, difficulty in industrial production, unfavorable industrial production, etc. , to achieve the effect of good catalytic effect, sufficient reaction and easy control

Inactive Publication Date: 2018-03-09
PANJIN HONGDING CHEM CO LTD
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

Due to the steric hindrance of branched chain fatty acids, it is difficult to carry out the reaction completely, so it is very necessary to develop a synthesis process suitable for industrialized production of pentaerythritol tetraisocaprylate
[0003] The synthesis of pentaerythritol tetraisocaprylate is generally synthesized in organic solvents, which does not meet the technical requirements of green chemistry and easily causes environmental pollution
And generally metal oxides, sulfuric acid, etc. are selected as catalysts. In the production of reagents, there are defects such as expensive reagents, high corrosion, and low yields, which are not conducive to industrial production.
[0004] It can be seen that the existing synthetic routes are not easy to industrialized production

Method used

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  • Synthesis process of pentaerythritol tetra(2-ethylhexanoate)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Preparation of solid superacid catalyst.

[0021] Take 25g TiCl 4 Dissolve in water, then hydrolyze with dilute ammonia water to become alkaline (PH=11), let stand for 24 h, filter and wash to obtain a large amount of white precipitate. The solid was dried at 120 °C and ground into powder. Then add it to the concentrated sulfuric acid solution of 0.5 M cerium sulfate, react for 10 h, filter and dry, put it in the muffle furnace to roast, and obtain the superacid catalyst SO 4 2- / TiO 2 / Ce.

[0022] (2) Synthesis of pentaerythritol tetraisocaprylate.

[0023] Pentaerythritol (100 g) and isooctanoic acid (529 g) were added to the reaction vessel, and then the catalyst (10 g) prepared in the above step was added to the reaction vessel, the reaction temperature was 150 °C, and the reaction was carried out for 13 h. After the reaction was completed, the heating was stopped to obtain the crude product.

[0024] (3) Post-processing of products.

[0025] The reacti...

Embodiment 2

[0027] (1) Preparation of solid superacid catalyst.

[0028] Take 50g TiCl 4 Dissolve in water, then hydrolyze with dilute ammonia water to become alkaline (PH=10), let it stand for 24 hours, filter and wash, and get a large amount of white precipitate. The solid was dried at 110 °C and ground into powder. Then add it to the concentrated sulfuric acid solution of 0.5 M cerium sulfate, react for 11 h, filter and dry, put it in a muffle furnace and roast it to obtain the superacid catalyst SO 4 2- / TiO 2 / Ce.

[0029] (2) Synthesis of pentaerythritol tetraisocaprylate.

[0030] Add pentaerythritol (200 g) and isooctanoic acid (1.19 g) into the reaction vessel, then add the catalyst (15 g) prepared in the above step to the reaction vessel, the reaction temperature is 120 ° C, react for 11 h, stop heating after the reaction to obtain the crude product .

[0031] (3) Post-processing of products.

[0032] The reaction solution is filtered, and the catalyst is filtered out a...

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Abstract

The invention relates to a method for synthesizing esters, in particular to a method for synthesizing pentaerythritol tetraisocaprylate. The synthesis steps include: preparation of solid superacid catalyst; synthesis of pentaerythritol tetraisooctanoate; post-treatment of products. The synthetic route of pentaerythritol tetraisocaprylate is simple, the conditions are mild, and it is easy to control. The source of raw materials is abundant and the price is low, which directly reduces the production cost. The purity of the synthesized pentaerythritol tetraisooctanoate is higher than 99%, and the yield is 80%. The synthetic route is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for synthesizing esters, in particular to a method for synthesizing pentaerythritol tetraisocaprylate. Background technique [0002] Pentaerythritol tetraisocaprylate has good thermal stability, biodegradability and anti-wear and anti-friction properties. It can not only be used as a high-temperature plasticizer, but also a green lubricating oil base oil with excellent properties. It has been obtained in the aviation field. widely used. Due to the steric hindrance of branched-chain fatty acids, it is difficult to complete the reaction, so it is necessary to develop a synthetic technique suitable for industrial production of pentaerythritol tetraisocaprylate. [0003] The synthesis of pentaerythritol tetraisocaprylate is generally synthesized in an organic solvent, which does not meet the technical requirements of green chemistry and easily causes environmental pollution. And generally metal oxides, sulfuric acid, etc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C67/48C07C69/33B01J27/053
CPCC07C67/08B01J27/053C07C67/48C07C69/33
Inventor 于智勇何延胜刘晓丹
Owner PANJIN HONGDING CHEM CO LTD
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