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Method for synthesizing dioctyl terephthalate through esterification

A technology of diisooctyl phthalate and terephthalic acid, which is applied in the field of esterification and synthesis of diisooctyl terephthalate plasticizer, can solve the problem that PTA and isooctanol are incompatible, not getting attention and Research, there is no report on synthesis technology, etc., to achieve the effect of catalyst recovery and reuse, fast reaction speed and reduced energy consumption

Active Publication Date: 2011-04-06
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 attention to and studied, and there has been no relevant synthesis technology report, so the problem of long synthesis reaction time has not been solved so far. solve

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] This embodiment includes the following steps:

[0023] 1. Preparation of butylpyridinium chloride ionic liquid catalyst

[0024] In a 500mL three-necked glass flask equipped with a stirring, thermometer and condenser, add an equal volume of chlorobutane and 80mL of pyridine, stir and react at 80°C for 48h, filter the colorless crystals, and wash them twice with ethyl acetate , Distilled and dried to obtain butylpyridine chloride.

[0025] Then, in a 250mL three-necked flask equipped with a stirrer, add 20g of butylpyridine chloride and 66g of stannous chloride, and react at 80°C for half an hour to obtain butylpyridine chloride stannous chloride ionic liquid .

[0026] 2. Synthesis of DOTP

[0027] In a 500mL glass three-necked flask equipped with stirring, a thermometer, a condenser, and an alcohol-water separator, add 2-ethylhexanol and terephthalic acid in amounts of 200mL and 70g, respectively (PTA:2-EH=1:2.4) . 23 g (10%) of butylpyridinium chloride stannous c...

Embodiment 2

[0032] This embodiment includes the following steps:

[0033] 1. Preparation of butylpyridinium chloride ionic liquid catalyst

[0034] In a 500mL three-necked glass flask equipped with a stirring, thermometer and condenser, add an equal volume of chlorobutane and 80mL of pyridine, stir and react at 80°C for 48h, filter the colorless crystals, and wash them twice with ethyl acetate , Distilled and dried to obtain butylpyridine chloride.

[0035] Then, in a 250mL three-necked flask equipped with a stirrer, add 20g of butylpyridine chloride and 66g of stannous chloride, and react at 80°C for half an hour to obtain butylpyridine chloride stannous chloride 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 200mL and 79g, respectively (PTA:2-EH=1:2.1) . 37 g (15%) of butylpyridinium chloride st...

Embodiment 3

[0042] This embodiment includes the following steps:

[0043] 1. Preparation of butylpyridinium chloride ionic liquid catalyst

[0044] In a 500mL three-necked glass flask equipped with a stirring, thermometer and condenser, add an equal volume of chlorobutane and 80mL of pyridine, stir and react at 80°C for 48h, filter the colorless crystals, and wash them twice with ethyl acetate , Distilled and dried to obtain butylpyridine chloride.

[0045] Then, in a 250mL three-necked flask equipped with a stirrer, add 20g of butylpyridine chloride and 66g of stannous chloride, and react at 80°C for half an hour to obtain butylpyridine chloride stannous chloride ionic liquid .

[0046] 2. Synthesis of DOTP

[0047] 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 75g, respectively (PTA:2-EH=1:2.2) . Add 8 g of butylpyridinium chloride stannou...

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Abstract

The invention discloses a method for synthesizing dioctyl terephthalate through esterification, which is characterized by taking terephthalic acid and 2-ethylhexanol as raw materials, and synthesizing dioctyl terephthalate through esterification by using a chloride butyl pyridine stannous chloride ionic liquid as a catalyst. The synthesis method of the invention has the characteristics of quick response speed, high conversion rate, reusable catalyst, no pollution and environmental protection.

Description

technical field [0001] The invention relates to a method for synthesizing a diisooctyl terephthalate plasticizer through esterification. Background technique [0002] Diisooctyl terephthalate is a new type of green plasticizer for PVC developed in recent years. It has good compatibility with PVC resin due to its high insulation, low volatility, heat resistance, cold resistance, extraction resistance, and good flexibility. Capacitance and other advantages have attracted more and more attention from the plastics industry, and it has become the most important substitute for diisooctyl phthalate (DOP). [0003] Esterification with terephthalic acid (PTA) and isooctyl alcohol 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), discloses a method of using phthalic acid and 2-ethylhexanol (is...

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孙亚飞左霜钱程林文俊张晓玲李留陈盈
Owner HUAQIAO UNIVERSITY
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