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Method for homogeneous synthesis of di (2-ethylhexyl) terephthalate

A technology of terephthalic acid and tetrabutyl titanate, 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 human carcinogenesis and high energy consumption in the reaction process, and achieve improved efficiency, The effect of shortening the reaction time and reducing energy consumption

Active Publication Date: 2021-08-10
JIANGNAN UNIV +1
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  • Application Information

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Problems solved by technology

However, the main problems in the industrial preparation of DOTP are: the reaction is a heterogeneous reaction of solid-liquid mixing, its industrial reaction time is twice that of DOP, and the energy consumption of the reaction process is high.
[0004] Global fossil fuels are becoming increasingly depleted. At present, the main plasticizer used in my country is DOP, but the raw material of DOP is fossil resources. Due to its non-renewable nature and the fact that DOP has been found to be carcinogenic to humans in recent years, it is widely used in Europe and the United States. DOP in other countries and regions has been banned from being used in children's toys, medical equipment, etc.

Method used

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  • Method for homogeneous synthesis of di (2-ethylhexyl) terephthalate
  • Method for homogeneous synthesis of di (2-ethylhexyl) terephthalate
  • Method for homogeneous synthesis of di (2-ethylhexyl) terephthalate

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Experimental program
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Effect test

Embodiment 1

[0026] Embodiment 1 homogeneously prepares the method for DOTP

[0027] In a three-necked flask equipped with stirring, condensation and a thermometer, add 0.1mol (16.6g) of PTA, NMP 0.6mol (59.48g), 0.3mol of isooctyl alcohol, and add acid alcohol total mass 1wt% when the temperature rises to 180°C The tetrabutyl titanate was kept warm for 0.5h, and then the temperature was raised to 220°C for reaction. After 4h of reaction, the acid value of the system no longer decreased, and the reaction was stopped at this time. After cooling and centrifuging, the crude product is washed and neutralized with 5% aqueous sodium bicarbonate solution; finally, vacuum distillation is carried out at -0.1Mpa, 160°C, and 5% activated carbon is added for decolorization at -0.1Mpa, 70°C to obtain the final product. The esterification rate of the product obtained is 99.6%.

Embodiment 2

[0029] Referring to Example 1, using the amounts of NMP shown in Table 1 respectively, and other conditions unchanged, corresponding esterification was carried out. The results are shown in Table 1.

[0030] Table 1

[0031] PTA: NMP (molar ratio) Esterification rate 1：1 99.82 1：2 99.86 1：3 99.79 1：4 97.11 1：5 98.95 1：6 99.60

[0032] The method for comparative example 1 heterogeneous phase preparation DOTP

[0033] Esterification in a solid-liquid heterogeneous system: In a three-necked flask equipped with stirring, condensation and a thermometer, add 0.1 mol of PTA, 0.3 mol of iso-octanol, and add 1% of the total mass of titanic acid when the temperature rises to 180°C Tetrabutyl ester was kept warm for 0.5h, and then the temperature was raised to 220°C for reaction. After 8h of reaction, the acid value of the system no longer decreased, and the reaction was stopped at this time. After cooling and centrifuging, washing and neu...

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Abstract

The invention discloses a method for homogeneous synthesis of di (2-ethylhexyl) terephthalate, and belongs to the technical field of plasticizer DOTP preparation. According to the method disclosed by the invention, a specific and suitable solvent NMP is used, tetrabutyl titanate is taken as a catalyst, an acid alcohol raw material is catalyzed for esterification, reaction only needs 4 hours, the reaction acid value is reduced to 1mg KOH / g, and the esterification rate of the obtained product reaches 99%. Compared with a heterogeneous esterification reaction of DOTP without a solvent, the method has the advantages that the reaction time is shortened by half, the energy consumption of the reaction is greatly reduced, and the heat loss in the reaction process is reduced. According to the method, the existing heterogeneous reaction is converted into homogeneous reaction, the esterification reaction efficiency is greatly improved, the reaction time is shortened, an excellent esterification effect is achieved, and the method has a wide application prospect in industry.

Description

technical field [0001] The invention relates to a method for homogeneously synthesizing bis(2-ethylhexyl) terephthalate and belongs to the technical field of plasticizer DOTP preparation. Background technique [0002] With the continuous development of the plasticizer industry, bis(2-ethylhexyl) terephthalate (DOTP) has gradually replaced diisooctyl phthalate (DOP) in recent years and has appeared in the public eye. However, the main problems in the current industrial preparation of DOTP are: the reaction is a heterogeneous reaction of solid-liquid mixing, its industrial reaction time is twice that of DOP, and the energy consumption of the reaction process is high. [0003] However, there is no relevant mature technology to solve the problems of long esterification reaction time and high energy consumption of DOTP. The purpose of this patent is to find a suitable solvent to be used in the esterification reaction of DOTP to change the heterogeneous reaction into a homogeneou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/82
CPCC07C67/08C07C69/82
Inventor 蒋平平冯珊张萍波沈劲贤范义益
Owner JIANGNAN UNIV
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