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Production method of dioctyl terephthalate

A technology of dioctyl phthalate and purified terephthalic acid, which is applied in the field of preparing dioctyl terephthalate from metal complex solid-supported catalytic synthesis of purified terephthalic acid, can solve the problems of poor product quality, pollution, Complicated technological process and other problems, to achieve the effect of high quality rate, low product pollution and high product purity

Inactive Publication Date: 2012-10-03
ANHUI XIANGFENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional dioctyl terephthalate (DOTP) process has shortcomings such as serious pollution, complicated process flow, and poor product quality (the color is 200#)

Method used

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  • Production method of dioctyl terephthalate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A kind of production method of dioctyl terephthalate, comprises the steps:

[0018] 1) Put purified terephthalic acid and 2-ethylhexanol into the esterification reaction kettle in a weight ratio of 1:1, heat while stirring, and when the temperature gradually rises to 174, 198 and 205°C, add titanium Tetrabutyl acetate, stannous oxalate and hydrous aluminum oxide, the total amount added is 0.27% of the total weight of terephthalic acid and 2-ethylhexanol, the esterification temperature is controlled at 210°C, and the reaction is carried out for 8 hours. When the acid value is low At 0.3mgKOH / g, the esterification reaction ends and enters the refining process;

[0019] 2) Reduce the temperature of the material in the above step to below 100°C, transfer it to a neutralization tank, and wash it with water at 90°C to remove excess reaction alcohol. After separating the water phase, add an inorganic filter, and use it immediately Porous materials for decolorization and adsor...

Embodiment 2

[0023] A kind of production method of dioctyl terephthalate, comprises the steps:

[0024] 1) Put purified terephthalic acid and 2-ethylhexanol into the esterification reaction kettle in a weight ratio of 1:1.45, heat while stirring, and when the temperature gradually rises to 175, 195, and 200°C, add titanium Acetate tetraisopropyl ester, stannous oxide and sodium hydroxide, adding the total amount is 0.22% of the total weight of terephthalic acid and 2-ethylhexanol, the esterification temperature is controlled at 218 ° C, reacted for 7 hours, when the acid value When it is lower than 0.3mgKOH / g, the esterification reaction ends and enters the refining process;

[0025] 2) After reducing the temperature of the material treated in the previous step to below 100°C, transfer it to a neutralization tank, and wash it with water at 170°C to remove excess reaction alcohol. After separating the water phase, add an inorganic filter , used for decolorization and adsorption of porous m...

Embodiment 3

[0029] A kind of production method of dioctyl terephthalate, comprises the steps:

[0030] 1) Put purified terephthalic acid and 2-ethylhexanol into the esterification reaction kettle in a weight ratio of 1:1.09, heat while stirring, and when the temperature gradually rises to 175, 198 and 205°C, add titanium Acid tetramethyl ester, dioxyl tin oxide and sodium aluminate, adding the total amount is 0.16% of the total weight of terephthalic acid and 2-ethylhexanol, the esterification temperature is controlled at 215 ° C, and reacted for 7 hours, when the acid When the value is lower than 0.3mgKOH / g, the esterification reaction ends and enters the refining process;

[0031] 2) Reduce the temperature of the material treated in the above step to below 100°C, transfer it to a neutralization tank, and wash it with water at 175°C to remove excess reaction alcohol. After separating the water phase, add an inorganic filter, That is, the porous material used for decolorization and adsor...

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Abstract

The invention provides a production method of dioctyl terephthalate. The production method comprises the steps 1) of feeding fine terephthalic acid and 2-ethyl hexyl alcohol into an esterfying reaction kettle by the weight ratio of 1 to 1-1.8, heating while stirring, adding catalyst when the temperature is increased to 170-210 DEG C, controlling the esterfying temperature within the range of 190-200 DEG C, reacting for 7-13h, and stopping esterfying when the acid value is less than 0.3mg KOH / g; and 2) of transferring the mixture into a neutralizing refining kettle after the temperature of the mixture is reduced below 100 DEG C, neutralizing and rinsing by water at 80-100 DEG C, removing superfluous reaction alcohol, separating water phase, adding a porous absorbing material, stirring, separating solid from liquid, so as to obtain a high-quality pure DOPT (dioctyl terephthalate) product, wherein the catalyst is reusable; the production method has the characteristics of low product pollution, high quality, and high product purity.

Description

technical field [0001] The invention relates to a production method of dioctyl terephthalate, in particular to a production method for preparing dioctyl terephthalate by solid-carrying and catalytically synthesizing purified terephthalic acid with a metal complex. Background technique [0002] Plasticizer is an ester substance that is added to high polymers (such as rubber, plastics, coatings, etc.) to increase their plasticity and flow properties during processing and to make the finished product flexible. [0003] Dioctyl terephthalate (abbreviation: DOTP) is an environmentally friendly special plasticizer with excellent performance. Due to the difference in molecular structure, it has high volume resistance, low volatility and can be compatible with PVC wire sheath and formula The filler in it is completely wetted, has a high flash point, and is non-flammable. The low-temperature flexibility and low-temperature resistance of the plasticized polyvinyl chloride resin PVC ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/82C07C67/08
Inventor 潘学松
Owner ANHUI XIANGFENG NEW MATERIALS
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