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Manufacturing method of bis(2-ethylhexyl) terephthalate

A technology of di- and ethylhexyl terephthalate, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, to achieve the effects of reducing reaction time, improving filtration rate, and increasing reaction rate

Active Publication Date: 2014-09-24
CHANG CHUN PLASTICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The main purpose of the present invention is to provide a kind of simple and convenient equipment, the manufacture method of bis(2-ethylhexyl terephthalate) that promotes esterification reaction rate and promotes filtration efficiency, to solve above-mentioned method, still exist the need to improve Reaction rate, improving the filtration efficiency of esterified products

Method used

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  • Manufacturing method of bis(2-ethylhexyl) terephthalate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028]In a 3L autoclave equipped with stirrer, thermometer, back pressure valve manometer, oil-water separator, return line, nitrogen flow controller, condenser and 30cm filling fractionation column, 1333.2g (10.24mole) Isooctyl alcohol (also known as 2-ethylhexanol, 2-EH), 531.5g (3.20mole) of pure terephthalic acid (PTA), 3.07g (relative to the total weight of the reaction system alcohol and acid reactants TyzorPC-64 (phosphate titanate chelate, Ti=5.0%, purchased from DORF KETAL CO.) catalyst equivalent to Ti=82ppm) was put into the reaction kettle. The reaction kettle was fully stirred under nitrogen flow and pressurized to a gauge pressure of 4.0kg / cm 2 , make the temperature rise to 232°C within 1 hour (starting esterification distillation temperature), the water and alcohol mixture brought out by the nitrogen flow begins to condense in the oil-water separator after filling the fractionation column and the condenser, and the upper alcohol mixture is refluxed The pipe is...

Embodiment 2

[0030] Use the same reactor and reaction compound as in Example 1, but replace the packed fractionation column with a 30cm single tube, and the catalyst system uses Tyzor TE (two (triethanolamine) diisopropyl titanate chelate), Ti = 8.2%, purchased from DORF KETAL CO. product). 1333.2g (10.24mole) of 2-EH, 531.5g (3.20mole) of PTA and 1.87g of Tyzor TE (Ti=82ppm) were put into the reactor. The reaction kettle is fully stirred under nitrogen flow and pressurized to a gauge pressure of .4.0kg / cm 2 , and heated up to 233°C in 1 hour, the water and alcohol mixture brought out by the nitrogen flow began to pass through the single tube (meaning the column without filler) and the condenser, and then condensed in the oil-water separator, and the upper alcohol mixture was led by the return pipe Return to the reactor to ensure that the reaction 2-EH / PTA is maintained at a fixed molar ratio of 3.2 / 1, and the water in the lower layer is continuously distilled out of the oil-water separat...

Embodiment 3

[0032] A reactor was used as in Implementation 1, but Tyzor IAM (trialkoxyphosphate butyl titanate dimer, Ti=8.8%, purchased from DORF KETAL CO.) was used as catalyst. 1333.2g (10.24mole) of 2-EH, 531.5g (3.20mole) of PTA and 1.68g of Tyzor IAM (Ti=82ppm) were put into the reactor. The reaction kettle was fully stirred under nitrogen flow and pressurized to a gauge pressure of 3.0kg / cm 2 , and heated up to 227°C within 1 hour, the water and alcohol mixture brought out by the nitrogen flow began to condense in the oil-water separator after filling the fractionation column and condenser, and the upper alcohol mixture was led back to the reactor through the return pipe to ensure the reaction 2 -EH / PTA is maintained at a fixed molar ratio of 3.2 / 1, and the water in the lower layer is continuously distilled out of the oil-water separator and taken out for metering. The reaction continues to heat up to 250°C, and after 3.7 hours, remove water from the separator and measure 116 mill...

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Abstract

The invention relates to a manufacturing method of bis(2-ethylhexyl) terephthalate, which comprises: performing an esterification reaction of terephthalic acid and 2-ethyl hexanol in the presence of a chelating catalyst. The method of the invention can increase the reaction speed, improve the filtering efficiency of the esterified product, and prepare bis(2-ethylhexyl) terephthalate with low hue (APHA).

Description

technical field [0001] The present invention relates to a kind of method of manufacturing terephthalate bis(2-ethylhexyl); particularly a kind of method that utilizes the chelate type catalyst of titanium or zirconium to manufacture terephthalate bis(2-ethylhexyl) method. Background technique [0002] Bis(2-ethylhexyl terephthalate) (also known as diisooctyl terephthalate, referred to as DOTP) is a non-toxic plasticizer that can be used in food containers. It has the same properties as polyvinyl chloride (PVC) ) and other polymer materials have good compatibility, low volatility and excellent electrical properties. DOTP can be prepared from 2-ethylhexanol and terephthalic acid (TPA) under pressure and in the presence of a catalyst. [0003] In order to improve the reaction efficiency of the esterification reaction of terephthalic acid in the prior art, for example, in Japanese Patent Application Publication No. JP2004300078A, it is disclosed that a high boiling point solve...

Claims

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Application Information

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IPC IPC(8): C07C69/82C07C67/08
CPCC07C67/08C07C69/82
Inventor 杨崇基林永昇王景平杜绍明赖一江
Owner CHANG CHUN PLASTICS
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