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Method for preparing tetraoctyl pyromellitate

A technology for pyromellitic acid and tetraoctyl ester, which is applied in the field of preparation of tetraoctyl pyromellitic acid, can solve the problems of pollution, complex catalyst preparation process, poor product quality and the like, and achieves high purity, good product quality, The effect of less energy and water consumption

Inactive Publication Date: 2015-04-22
CHAOHU XIANGFENG PLASTIC AIDS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above-mentioned traditional production process of TOPM has shortcomings such as serious pollution, complex catalyst preparation process, and poor product quality (color up to 200#)

Method used

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  • Method for preparing tetraoctyl pyromellitate

Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment 1

[0026] A laboratory preparation example of tetraoctyl pyromellitate, comprising the steps of:

[0027] Step 1. Esterification

[0028] Add 0.7 mol (178 g) of pyromellitic acid and 3.5 mol (455 g) of 2-ethylhexanol into a 1000 ml glass three-neck flask equipped with a stirrer, thermometer, condenser, and water separator, and heat at 160°C 3 g of tetraisopropyl titanate catalyst was added, and the reaction time was 2.5 hours at 220° C., and the measured acid value of the product was 0.20 mgKOH / g.

[0029] Wherein the catalyst can be not only tetraisopropyl titanate, but also one or more of titanium metal compounds and tin metal compounds, and the titanium metal compounds include tetrabutyl titanate, tetraisopropyl titanate, titanium Tetramethyl ester and titanium dioxide, etc., the tin metal compounds include stannous oxalate, stannous oxide, dibutyltin oxide and dibutyltin phthalate, etc.

[0030] Step two, dealcoholization

[0031] At 160-220°C, dealcoholization under norma...

specific Embodiment 2

[0039] A kind of industrial production example of tetraoctyl pyromellitate, comprises the steps:

[0040] Step 1. Esterification

[0041] Add 1.2 tons of pyromellitic acid and 3.1 tons of 2-ethylhexanol into a stainless steel esterification reaction kettle with a packing tower and a condenser with a volume of 6 cubic meters, raise the temperature to 160°C, and add 6 Kg of titanic acid Tetraisopropyl ester catalyst. At 220° C., esterification reaction was carried out for 3 hours. The acid value measured by sampling was 0.22 mgKOH / g.

[0042]Wherein the catalyst can be not only tetraisopropyl titanate, but also one or more of titanium metal compounds and tin metal compounds, and the titanium metal compounds include tetrabutyl titanate, tetraisopropyl titanate, titanium Tetramethyl ester and titanium dioxide, etc., the tin metal compounds include stannous oxalate, stannous oxide, dibutyltin oxide and dibutyltin phthalate, etc.

[0043] Step two, dealcoholization

[0044] At ...

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Abstract

The invention discloses a method for preparing tetraoctyl pyromellitate. The method comprises the following steps: putting pyromellitic acid and 2-ethyl hexanol into a reaction vessel, heating to 150-170 DEG C, adding a catalyst and carrying out esterification reaction at a temperature of between 190 and 220 DEG C until the acid value is less than 0.25 mg KOH / g, wherein the catalyst is one or more of a titanium compound and a tin compound; carrying out natural atmospheric dealcoholization to remove excess 2-ethyl hexanol, controlling the dealcoholization temperature at 160-220 DEG C, sampling and testing the acid value and when the acid value is 0.2 mg KOH / g or less, stopping the dealcoholization process; neutralizing the product at 90-100 DEG C, and separating an aqueous phase; introducing high-purity steam and purifying; adding a porous material into the obtain product for adsorbing and decolorizing and carrying out solid-liquid separation to obtain the tetraoctyl pyromellitate product. The method is low in pollution and the high-quality and high-purity product can be obtained.

Description

technical field [0001] The invention relates to a preparation method of tetraoctyl pyromellitate, which belongs to the technical field of fine chemicals. The product is a plastic additive, which is used as a plasticizer for high heat-resistant PVC and is suitable for PVC plastic products with special heat-resistant requirements. Among them, the heat resistance and volume resistivity of PVC products can be greatly improved. Background technique [0002] Plasticizer is an ester substance that is added to high polymers (such as plastics, coatings, etc.) to increase their plasticity and flow properties during processing and molding, and to make the finished product flexible. Tetraoctyl pyromellitate (hereinafter referred to as TOPM) is an environmentally friendly special plasticizer with excellent performance. Due to the particularity of its molecular structure, it has high volume resistance, low volatility, high flash point, and non-flammability. , It can be completely wetted ...

Claims

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Application Information

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IPC IPC(8): C07C69/76C07C67/08
CPCC07C67/08C07C67/52C07C67/54C07C67/56C07C67/60C07C69/76
Inventor 潘学松
Owner CHAOHU XIANGFENG PLASTIC AIDS
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