A method for improving the reaction efficiency of a terephthalate plasticizer

A technology of terephthalate and terephthalic acid, applied in the field of terephthalate plasticizer, can solve the problems of long reaction time, side reactions, increased production process, etc., and shorten the esterification reaction time , low odor characteristics, the effect of increasing yield

Active Publication Date: 2018-10-12
NANYA PLASTICS CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The currently commonly used terephthalic acid-based plasticizers, for example, di-isooctyl terephthalate (DOTP; Di(2-ethylhexyl) terephthalate), are environmentally friendly plasticizers, and DOTP plasticizers are derived from Phthalic acid (PTA) and 2-ethylhexanol (2EH) esterification synthesis reaction, PTA is insoluble in 2EH and common solvents, so the esterification synthesis is a heterogeneous solid-liquid phase reaction, PTA is easy to Precipitation and agglomeration. In addition, limited by the solubility of PTA in 2EH, the reaction only occurs between the interface between PTA and 2EH, resulting in extremely slow esterification reaction rate and long reaction time
At present, titanate is mostly used as a catalyst in the industrial production of DOTP, and the reaction time is at least 5 hours, so the problems of incompatibility between PTA and 2EH and long synthesis reaction time have not been solved.
[0003] Regarding the method for improving the reactivity of dioctyl terephthalate, in the CN102329233B patent, quaternary ammonium salt ionic liquids are used as cocatalysts and solubilizers, but ionic liquids may produce side reactions or interact with catalysts during the esterification process, and in In the final purification stage of the process, static separation must be carried out, which has the disadvantages of increasing the production process and prolonging the production time.

Method used

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  • A method for improving the reaction efficiency of a terephthalate plasticizer
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  • A method for improving the reaction efficiency of a terephthalate plasticizer

Examples

Experimental program
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Effect test

Embodiment 1

[0029] As in the formula in Table 1, first use a homogenizer to subdivide the terephthalic acid (PTA) composition, (1) get 119 grams of terephthalic acid (PTA), and 119 grams of slurry solvent 2-ethylhexyl After the alcohol (2EH) is mixed, the homogenizer (specification: 3000-6000rpm, frequency: 50-60Hz) is subdivided and treated 6 times to form a PTA slurry with an average particle size of PTA in the slurry of 107.3 μm. After taking out, (2) take another 161 grams of 2EH as the slurry solvent added outside, and clean the PTA slurry residue left by the homogenizer. Get 0.6 grams of TIPT (tetraisopropyl titanate) as a catalyst, mix (1) and (2) slurries and feed them into a four-necked flask simultaneously with the catalyst, and the reaction temperature is changed from 180 to 180 ℃ is gradually raised to 225 ℃, and the reaction time is 2.5 hours, including: after reacting for 1.5 hours at a reaction pressure of 1013 millibars (mbar), and then reacting for 1 hour at a reaction pr...

Embodiment 2

[0031] Formulation composition as in Table 1, the same as in Example 1, except that the PTA / 2EH slurry was treated 9 times with a homogenizer to form a slurry with an average particle size of PTA of 103.2 μm. The results are shown in Table 1.

Embodiment 3

[0033] The formula composition shown in Table 1 is the same as that of Example 1, except that the composition ratio of PTA / 2EH slurry is 1:1.3. The average particle size of PTA in the PTA slurry is 108.6 μm. The results are shown in Table 1.

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Abstract

The invention provides a method for improving the reaction efficiency of a terephthalate plasticizer. A homogenizer is used to refine PTA in a mixture containing the PTA and C6-C10 alcohol multiple times to a grain size of 80-110 [mu]m. Esterification reaction is performed in the presence of a titanium metal catalyst. Compared with the conventional producing method, the method has the advantages that the esterification reaction time is at least shortened by more than 37.5%, the purity of a terephthalate plasticizer finished product synthesized through esterification is more than 99.5%, the physical properties such as acid value, hue, refractive index and the like all meet standards, and the product has a low odor characteristic.

Description

technical field [0001] The invention relates to a terephthalate plasticizer, which consists of terephthalic acid (hereinafter referred to as PTA) subdivided to a particle size between 80-110 μm and a straight chain or branched chain of 6 to 10 carbons. Alcohol (hereinafter referred to as C6-C10 alcohol) esterification synthesis. Background technique [0002] The currently commonly used terephthalic acid-based plasticizers, such as di-isooctyl terephthalate (DOTP; Di(2-ethylhexyl) terephthalate), are environmentally friendly plasticizers, and DOTP plasticizers are derived from Phthalic acid (PTA) and 2-ethylhexanol (2EH) esterification synthesis reaction, PTA is insoluble in 2EH and common solvents, so the esterification synthesis is a heterogeneous solid-liquid phase reaction, PTA is easy to Precipitation and agglomeration. In addition, limited by the solubility of PTA in 2EH, the reaction only occurs between the interface between PTA and 2EH, resulting in extremely slow es...

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 廖德超庄荣仁林训民
Owner NANYA PLASTICS CORP
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