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Synthesis method of tridecyl trimellitate

A technology for the synthesis of tridecyl tripentellitate, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of high production costs, cumbersome reactions, and harsh conditions, and achieve operational Convenience, mild reaction conditions, and simple process

Inactive Publication Date: 2013-07-24
范强 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current synthetic methods either need to use expensive raw materials, and the production cost is relatively high; or the reaction is cumbersome, the conditions are harsh, and the yield is low.

Method used

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  • Synthesis method of tridecyl trimellitate

Examples

Experimental program
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Effect test

Embodiment 1

[0013] Add 67 g of trimellitic anhydride, then 300 g of tridecyl alcohol into the three-necked flask, and finally add 0.2% catalyst tetrabutyl titanate whose mass is the total mass of trimellitic anhydride and tridecyl alcohol. Then connect the water separator, start stirring, pass nitrogen protection, and at the same time raise the temperature to 200-210°C and keep it warm. The water separator continuously removes the water generated by the reaction, and the esterification reaction ends when no water comes out. Then lower the temperature to 120°C, change the water separation reaction device into a vacuum distillation device, and dealcoholize under reduced pressure and vacuum until almost no tridecyl alcohol fraction is distilled out (tridecyl alcohol can be recycled). Then the whole system was cooled to 90°C, added a small amount of KOH aqueous solution to wash, and then transferred to a separatory funnel for extraction and layering. The lower water layer was removed, and the...

Embodiment 2

[0015] 100 g of trimellitic anhydride was added to the three-necked flask, then 450 g of tridecyl alcohol was added, and finally a catalyst p-toluenesulfonic acid whose mass was 1.0% of the total mass of trimellitic anhydride and tridecyl alcohol was added. Then connect the water separator, start stirring, pass nitrogen protection, and at the same time raise the temperature to 210-220°C and keep it warm. The water separator continuously removes the water generated by the reaction, and the esterification reaction ends when no water comes out. Then lower the temperature to 120°C, change the water separation reaction device into a vacuum distillation device, and dealcoholize under reduced pressure and vacuum until almost no tridecyl alcohol fraction is distilled out (tridecyl alcohol can be recycled). Then the whole system was cooled to 90°C, added a small amount of KOH aqueous solution to wash, and then transferred to a separatory funnel for extraction and layering. The lower wa...

Embodiment 3

[0017] Add 50 g of trimellitic anhydride in the three-necked flask, then add 225 g of tridecyl alcohol, and finally add catalyst sulfuric acid whose mass is 2% of the total mass of trimellitic anhydride and tridecyl alcohol. Then connect the water separator, start stirring, pass nitrogen protection, and at the same time raise the temperature to 200-210°C and keep it warm. The water separator continuously removes the water generated by the reaction, and the esterification reaction ends when no water comes out. Then lower the temperature to 120°C, change the water separation reaction device into a vacuum distillation device, and dealcoholize under reduced pressure and vacuum until almost no tridecyl alcohol fraction is distilled out (tridecyl alcohol can be recycled). Then the whole system was cooled to 90°C, added a small amount of KOH aqueous solution to wash, and then transferred to a separatory funnel for extraction and layering. The lower water layer was removed, and the up...

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Abstract

The invention discloses a synthesis method of tridecyl trimellitate. The synthesis steps are as follows: adding trimellitic anhydride and tridecyl alcohol into a reaction container according to the molar ratio of 1: (3-5), then adding a catalyst, performing esterification and dehydration under the protection of nitrogen, and utilizing a water separator to continuously remove water generated by reaction, wherein the esterification temperature is 190-220 DEG C, and the reaction is performed till no generation of the water; and then, reducing the temperature to 120 DEG C, further performing decompression, distillation and dealcoholization till no evaporation of the tridecyl alcohol, reducing the temperature to 90 DEG C, and then washing, extracting and drying to obtain the tridecyl trimellitate. According to the synthesis method disclosed by the invention, the trimellitic anhydride is taken as a raw material, and the esterification and the dehydration are performed with the tridecyl alcohol under the condition of the catalyst. The synthesis method has the advantages of mild conditions during the whole reaction, convenience in operation and high total yield of above 85%, and a product is obtained after dealcoholization and washing with water. The synthesis method disclosed by the invention has the advantages of simple process, easiness in formation of large-scale production and wide application prospects.

Description

Technical field [0001] The present invention involves a synthesis method of a trigenate thirty ester, which is the field of organic compound synthesis technology. Background technique [0002] Trimetal thirty -thirtyrate is a high -viscosity and almost colorless moisturizer. It is very closed, which makes the product feel as thick as a blanket.Good sex, can directly play color pulp, which can prevent the color of the lipstick from layered and the product is bright.At present, the synthetic method may need to be expensive, and the cost of production is relatively high; Invention content [0003] In order to solve the lack of existing technology, the purpose of the present invention is to provide a synthesis method of trigenate thyanate that is simple, low, high, and easy to produce. [0004] In order to achieve the above goals, the invention is achieved through the following technical solutions: [0005] The synthesis method of a trigenate thirty ester is characterized by the spe...

Claims

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Application Information

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IPC IPC(8): C07C69/76C07C67/08
Inventor 范强陈金良
Owner 范强
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