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Process for producing diisooctyl terephthalate

The technology of a kind of diisooctyl phthalate and its production method is applied in the production field of diisooctyl terephthalate, which can solve the problems of large amount of catalyst, long reaction time, and poor color of the product, and achieve the purpose of improving activity, tower The effect of small resistance and low energy consumption

Inactive Publication Date: 2015-01-07
NANJING COLLEGE OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the shortcomings of the existing esterification process, such as long reaction time, poor product color, large amount of catalyst, and special need for subsequent adsorption and decolorization steps, the present invention provides a catalyst with high surface area mesoporous carbon or porous titanium dioxide as a carrier. A new method for synthesizing diisooctyl terephthalate by negative pressure esterification with tube tower instead of conventional packed tower

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 100 parts by weight of purified terephthalic acid and 160 parts by weight of isooctyl alcohol are heated and stirred in an esterification tank, and the temperature is raised to 150 ° C, and 8 parts by weight of mesoporous carbon-supported n-butyl titanate catalyst (titanic acid The weight percentage of n-butyl ester is 4%, and the BET surface area is 1100m 2 / g, the pore volume is 1.1cm 3 / g, the average pore diameter is 3.2nm), and pressure is 0.5atm, and temperature is 215 ℃ and iso-octanol reflux conditions and reacts 2.5 hours, gets the sample in still and records acid value 0.04mg KOH / g termination reaction;

[0024] The esterification feed solution is cooled to 100°C, washed with water to neutrality, filtered to remove catalyst and impurities, and iso-octanol and water are removed at 0.3 atm to obtain a product with a purity of 99.8%. The yield is 86.5%, and the chromaticity (platinum Cobalt) is 8, the density is 0.986g / cm 3 .

Embodiment 2

[0026] Heat and stir 150 parts by weight of purified terephthalic acid and 280 parts by weight of isooctyl alcohol in an esterification tank, heat up to 170°C, and add 9 parts by weight of porous TiO 2 The supported titanate catalyst (n-butyl titanate weight percentage is 7%, BET surface area is 140m 2 / g, the pore volume is 0.4cm 3 / g, the average pore diameter is 9nm), at a pressure of 0.3atm, a temperature of 210°C and iso-octanol reflux conditions for 1.5 hours to react, get the sample in the kettle to record the acid value of 0.05mgKOH / g to terminate the reaction; The chemical solution was cooled to 90°C, washed with water until neutral, filtered to remove catalyst and impurities, and iso-octanol and water were removed at 0.4 atm to obtain a product with a purity of 99.9%, a yield of 88.1%, and a chromaticity (platinum-cobalt) 9, the density is 0.987g / cm 3 .

Embodiment 3

[0028] Heat and stir 200 parts by weight of purified terephthalic acid and 300 parts by weight of isooctyl alcohol in an esterification tank, heat up to 170°C, and add 9 parts by weight of TiO 2 Nanotube supported titanate catalyst (tetraisopropyl titanate weight percentage is 7%, BET surface area is 290m 2 / g, the pore volume is 1.0cm 3 / g, the average pore diameter is 14nm), at a pressure of 0.3atm, a temperature of 205 ° C and isooctanol reflux conditions to react for 1 hour, get the sample in the kettle to record an acid value of 0.03mg KOH / g to terminate the reaction; The chemical solution was cooled to 90°C, washed with water until neutral, filtered to remove catalyst and impurities, and iso-octanol and water were removed at 0.4 atm to obtain a product with a purity of 99.9%, a yield of 89.6%, and a chroma (platinum-cobalt) 7, the density is 0.987g / cm 3 .

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Abstract

The invention discloses a process for producing diisooctyl terephthalate. The process comprises the steps of carrying out esterification in the presence of tetrabutyl titanate catalyst loaded by mesoporous carbon with a high surface area or porous titania, carrying out the rectification, separation, neutralization and impurity removing of isooctyl alcohol and water and the like in a negative-pressure tabulation tower. The esterification reaction in the production process disclosed by the invention can be finished within 3 hours, the reaction and separation processes are simple, the yield is high, diisooctyl terephthalate obtained according to the process for producing diisooctyl terephthalate has the purity higher than 99.8 percent, and the first-grade quality rate of the product reaches 100 percent.

Description

technical field [0001] The invention belongs to the field of plasticizer production, and in particular relates to a production method of diisooctyl terephthalate. Background technique [0002] Di-octyl terephthalate is an important polyvinyl chloride plasticizer, and its processing performance is similar to that of commonly used dioctyl phthalate. However, diisooctyl terephthalate has better heat resistance, cold resistance, compatibility with rubber and plastic, and electrical insulation properties; more importantly, its structure does not contain phthalic acid, which is banned by Western countries. From the 1980s to the present, the production method of di-isooctyl terephthalate has received extensive attention from academia and industry. [0003] The production methods of diisooctyl terephthalate mainly include direct esterification, transesterification, alcohol exchange after pyrolysis of polyethylene terephthalate (PET) and diisooctyl terephthaloyl chloride. additive ...

Claims

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Application Information

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IPC IPC(8): C07C69/82C07C67/08B01J32/00B01J35/10B01J31/12
CPCC07C67/08C07C69/82
Inventor 陆新华邱忆宁刘经伟胡瑾孙宏顺
Owner NANJING COLLEGE OF CHEM TECH
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