Method for catalytically synthesizing diisooctyl terephthalate under action of ionic liquid

A technology of diisooctyl phthalate and terephthalic acid, applied in the field of catalytic synthesis of diisooctyl terephthalate, can solve the problem that PTA and isooctyl alcohol are incompatible, there is no synthesis technology report, and there is no It has been paid attention to and researched and other issues to achieve the effect of reusable catalyst recovery, reduced energy consumption, and fast reaction speed.

Active Publication Date: 2012-01-25
HUAQIAO UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although many new catalysts have been researched and developed in recent years, the problem of incompatibility between PTA and isooctyl alcohol has not been paid at

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] This embodiment includes the following steps:

[0025] 1. Preparation of quaternary ammonium salt ionic liquid catalyst

[0026] In a 250mL glass three-necked flask equipped with a stirring, thermometer, and condenser tube, add 0.5mol of n-butylamine and a certain amount of deionized water, stir under ice bath, and then use a separatory funnel to add dropwise (2 drops / s) 0.5mol concentrated sulfuric acid, react for 2 hours, and then keep warm for 2 hours. Then the reaction mixture was transferred into a one-necked bottle, and most of the water was removed by rotary evaporation at 70° C., and then vacuum-dried to obtain tributylammonium bisulfate ionic liquid.

[0027] 2. Synthesis of DOTP

[0028] In a 500mL glass three-necked flask equipped with stirring, a thermometer, a condenser, and an alcohol-water separator, the amounts of 2-ethylhexanol and terephthalic acid added were 200mL and 70g, respectively (PTA:2-EH=1:2.9) , then add 11.5g (5%) tributylammonium hydroge...

Embodiment 2

[0033] This embodiment includes the following steps:

[0034] 1. Preparation of quaternary ammonium salt ionic liquid catalyst

[0035] In a 250mL glass three-necked flask equipped with a stirring, thermometer, and condenser tube, add 0.5mol of triethylamine and a certain amount of deionized water, stir under ice bath, and then use a separatory funnel to add dropwise (2 drops / s) 0.5mol concentrated sulfuric acid, react for 2 hours, and then keep warm for 2 hours. Then the reaction mixture was transferred to a one-necked bottle, and most of the water was removed by rotary evaporation at 70° C., and then vacuum-dried to obtain triethylammonium hydrogen sulfate ionic liquid.

[0036] 2. Synthesis of DOTP

[0037] In a 500mL glass three-necked flask equipped with stirring, a thermometer, a condenser, and an alcohol-water separator, the amounts of 2-ethylhexanol and terephthalic acid added were 180mL and 70g, respectively (PTA:2-EH=1:2.7) , and then added 21.4g (10%) triethyl hy...

Embodiment 3

[0042] This embodiment includes the following steps:

[0043] 1. Preparation of quaternary ammonium salt ionic liquid catalyst

[0044] In a 250mL glass three-necked flask equipped with a stirring, thermometer, and condenser, add 0.5mol of trioctylamine and a certain amount of deionized water, stir under ice bath, and then use a separatory funnel to add dropwise (2 drops / s) 0.5mol concentrated sulfuric acid, react for 2 hours, and then keep warm for 2 hours. Then the reaction mixture was transferred into a one-necked bottle, and most of the water was removed by rotary evaporation at 70° C., and then vacuum-dried to obtain trioctylammonium hydrogen sulfate ionic liquid.

[0045] 2. Synthesis of DOTP

[0046] In a 500mL glass three-necked flask equipped with stirring, a thermometer, a condenser, and an alcohol-water separator, the amounts of 2-ethylhexanol and terephthalic acid added were 170mL and 70g, respectively (PTA:2-EH=1:2.6) , and then added 10.2g (5%) trioctyl hydrog...

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PUM

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Abstract

The invention discloses a method for synthesizing diisooctyl terephthalate through esterification, which is characterized by comprising the following step: synthesizing the diisooctyl terephthalate through an esterification reaction by using terephthalic acid and 2-ethylhexanol as raw materials, tetrabutyl titanate as a primary catalyst and a quaternary ammonium salt ionic liquid as a cocatalyst and a solubilizer. The synthetic method provided by the invention has the characteristics that the reaction speed is high; the conversion ratio is high; the ionic liquid can be used repeatedly; the pollution is avoided; and the method is green and environment-friendly.

Description

technical field [0001] The invention relates to a method for catalytically synthesizing diisooctyl terephthalate under the action of an ionic liquid. Background technique [0002] Diisooctyl terephthalate is a new type of green plasticizer for polyvinyl chloride (PVC) developed in recent years. It has high insulation, low volatility, heat resistance, cold resistance, extraction resistance, and good flexibility. It is compatible with PVC resin. Due to its good compatibility and other advantages, it has attracted more and more attention from the plastics industry, and has become the most important substitute for diisooctyl phthalate (DOP). [0003] Esterification with terephthalic acid (PTA) and isooctyl alcohol (2-ethylhexanol, 2-EH) as raw materials is the most important production route for the synthesis of DOTP. [0004] Chinese invention patent "Technology for preparing dioctyl terephthalate plasticizer from terephthalic acid and octanol" (Patent No. ZL200410021429.5), d...

Claims

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Application Information

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IPC IPC(8): C07C69/82C07C67/08
Inventor 林金清方国阳金春英林文俊李留张晓玲罗凤飞王聪聪杨宏飞李汉江
Owner HUAQIAO UNIVERSITY
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