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Catalyst used for production of high-purity terephthalic acid di(2-ethylhexyl) acrylate

A terephthalic acid di-catalyst technology, applied in the direction of physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, carboxylate preparation, etc., can solve the problem that the content is difficult to achieve and affects product purity, etc. question

Inactive Publication Date: 2010-12-29
江苏雷蒙新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When tetrabutyl titanate is used as a catalyst, the catalytic effect is better, and the esterification time is generally 6-8 hours, but there is always a small amount of monobutyl-octyl terephthalate in the reactant, and its content is generally 0.15% left and right, which affects the purity of the product, making it difficult to achieve a content of more than 99.5%

Method used

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  • Catalyst used for production of high-purity terephthalic acid di(2-ethylhexyl) acrylate
  • Catalyst used for production of high-purity terephthalic acid di(2-ethylhexyl) acrylate
  • Catalyst used for production of high-purity terephthalic acid di(2-ethylhexyl) acrylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1 A mixture of 70% tetraisopropyl titanate and 30% tetrabutyl titanate is used as a catalyst (the amount is also 0.43% of PTA, i.e. 3g), the specific operation is:

[0027] Add 700g of PTA, 1650g of octanol, and 2g of active carbon into a 3-liter flask with a stirrer and a distillation device, stir and rapidly heat the mixture in the flask to 170°C, add a mixed catalyst (70% tetraisopropyl titanate and 30% titanium ester tetrabutyl ester mixture) 1.8g for esterification reaction, when the temperature of the mixture in the flask was raised to 205°C, 1.2g of catalyst was added, the esterification time was 6 hours, 153.5ml of reaction water was removed by distillation, and the mixture was The temperature rises to about 225°C, and the acid value of the material is 0.08mgKOH / g, stop heating, cool down to 90°C, add 700ml of 3% NaOH lye (about 40% of the total material), stir for 30min, and stand still for 1 Hours, the lower layer of alkaline water was removed. Add th...

Embodiment 2

[0029] Example 2 The mixed titanate ester of 75% tetraisopropyl titanate and 25% tetrabutyl titanate was also used as a catalyst, the amount of which was also 0.43% of PTA, i.e. 3g), the specific operation was:

[0030] Add 700g of PTA, 1650g of octanol, and 2g of active carbon into a 3-liter flask with a stirrer and a distillation device, stir and rapidly heat the mixture in the flask to 170°C, add a mixed catalyst (75% tetraisopropyl titanate and 25% mixture of titanium ester tetrabutyl ester) 1.8g for esterification reaction, when the temperature of the mixture in the flask was raised to 205°C, 1.2g of catalyst was added, the esterification time was 6 hours, 153.5ml of reaction water was removed by distillation, and the mixture The temperature of the material rises to about 225°C, and the acid value of the material is 0.08mgKOH / g, stop heating, cool down to reduce the temperature of the material to 90°C, add 700ml of 3% NaOH lye (about 40% of the total material), stir for 30...

Embodiment 3

[0033] Embodiment 3 Referring to the manufacturing method of Example 1 or 2, the catalyst used in the process is a combination of tetraisopropyl titanate and tetrabutyl phthalate, and the weight ratio of tetraisopropyl titanate and tetrabutyl phthalate It is 50:50, the amount of catalyst added is 0.2% of the weight of purified terephthalic acid, the temperature of the first addition is 175 ° C, the amount of addition is 60% of the total amount of catalyst, the remaining catalyst is added for the second time, and the temperature The temperature is 203°C, and the purity of the obtained product is 99.5811%.

[0034] The gas chromatographic detection of the product obtained at last refers to the attached Figure 4 .

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Abstract

The invention relates to a catalyst used for production of high-purity terephthalic acid di(2-ethylhexyl) acrylate, which belongs to a catalyst for a synthesis process in the chemical industry. The catalyst is a mixed titanic acid ester consisting of tetraisopropyl titanate and tetrabutyl phthalate, wherein the weight ratio of the tetraisopropyl titanate to the tetrabutyl phthalate is 50-80:50-20. An ester exchange reaction is performed in an esterification process and most of isopropyl nitrate is substituted by monooctyl esters when the reaction is finished, so that a high-purity product can be obtained.

Description

technical field [0001] The invention belongs to a catalyst for a synthesis process in the chemical industry, in particular to a catalyst for preparing an environmentally friendly plasticizer with higher purity—bis(2-ethyl)hexyl terephthalate. Background technique [0002] Di(2-ethyl)hexyl terephthalate, also known as dioctyl terephthalate, or DOTP for short, is mainly used as a plasticizer for PVC. With the further improvement of human's toxicological understanding of chemicals and environmental awareness, the proportion of traditional o-phthalic plasticizers is greatly reduced year by year, and they are replaced by environmentally friendly plasticizers such as DOTP, ATBC, and DINCH. As an environmentally friendly plasticizer with excellent performance and moderate cost performance, DOTP is being rapidly recognized by the market and has grown significantly. [0003] There are three main ways to synthesize DOTP: one is to use waste terephthalic acid (pool material, floor mat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07C69/82C07C67/08
Inventor 周永芳陈平曹立军
Owner 江苏雷蒙新材料有限公司
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