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Method for preparing plasticizer 1, 2, 4-benzenetricarboxylicacid tris(2-propyl heptyl) ester

A technology of trimellitic acid tris and trimellitic anhydride, which is applied to the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of industrial production level, low output, high raw material price, and restricted application, and achieve Reduce production costs, reduce raw material costs, and achieve superior low-temperature performance

Inactive Publication Date: 2013-04-03
JIANGNAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the variety of trimellitate plasticizers in my country is relatively single, and the industrial production level and output are very low, and it is limited to the production of tris(2-ethyl)hexyl trimellitate (TOTM). It is relatively high, and its application is restricted economically. Therefore, finding and developing low-cost, high-performance substitutes has become a research direction for many manufacturers.

Method used

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  • Method for preparing plasticizer 1, 2, 4-benzenetricarboxylicacid tris(2-propyl heptyl) ester
  • Method for preparing plasticizer 1, 2, 4-benzenetricarboxylicacid tris(2-propyl heptyl) ester
  • Method for preparing plasticizer 1, 2, 4-benzenetricarboxylicacid tris(2-propyl heptyl) ester

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Experimental program
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Embodiment 1

[0031] Add 4.8kg of trimellitic anhydride, 25.3kg of 2-propylheptanol (the molar ratio of trimellitic anhydride to 2-propylheptanol is 1:3.2), 0.0192kg of tetra-n-butyl titanate, 0.0075kg of activated carbon, and attapulgite in the reaction kettle 0.0075kg, used to absorb oxygen and decolorize, stir and raise the temperature to 200℃~220℃, the reaction time is 4h, the esterification rate reaches 99.1%; the crude product is washed with neutralization alkali and water, and the mass fraction of neutralization alkali washing is 5 % sodium bicarbonate aqueous solution at a temperature of 50°C to 70°C, washed with deionized water or distilled water at a temperature of 60°C to 90°C; dealcoholized by vacuum distillation at a temperature of 170°C and a vacuum of 0.09MPa. After extraction again, it is finally filtered to obtain a light yellow product, tris(2-propylheptyl) trimellitate.

Embodiment 2

[0033] Add 4.8kg of trimellitic anhydride, 31.66kg of 2-propylheptanol (the molar ratio of trimellitic anhydride to 2-propylheptanol is 1:4), 0.0288kg of tetraisopropyl titanate, 0.029kg of activated carbon, and attapulgite in the reaction kettle 0.029kg, used to absorb oxygen and decolorize, stir and heat up to a temperature of 200°C~220°C, reaction time 4h, esterification rate reaches 99.6%; the crude product is washed with neutralization alkali and water, and the mass fraction of neutralization alkali washing is 5 % sodium bicarbonate aqueous solution at a temperature of 50°C to 70°C, washed with deionized water or distilled water at a temperature of 60°C to 90°C; dealcoholized by vacuum distillation at a temperature of 170°C and a vacuum of 0.09MPa. After extraction again, it is finally filtered to obtain a light yellow product, tris(2-propylheptyl) trimellitate.

Embodiment 3

[0035] Add 4.8kg of trimellitic anhydride, 35.62kg of 2-propylheptanol (the molar ratio of trimellitic anhydride to 2-propylheptanol is 1:4.5), 0.0288kg of titanate (of which 0.0192kg of tetraisopropyl titanate, Tetra-n-butyl titanate 0.0096kg), activated carbon 0.0404kg, attapulgite 0.0404kg, used to absorb oxygen and decolorize, stir and heat up to a temperature of 200 ° C ~ 220 ° C, the reaction time is 6 hours, and the esterification rate reaches 99.4%; the crude product Carry out neutralization alkali washing and water washing, neutralization alkali washing uses sodium bicarbonate aqueous solution with a mass fraction of 5%, the temperature is 50 ° C ~ 70 ° C, water washing uses deionized water or distilled water, the temperature is 60 ° C ~ 90 ° C; decompression Dealcoholization by distillation at a temperature of 170°C and a vacuum of 0.09MPa. After the alcohol no longer comes out, filter at last to obtain a light yellow product, tris(2-propylheptyl)trimellitate.

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Abstract

A method for preparing a plasticizer 1, 2, 4-benzenetricarboxylicacid tris(2-propyl heptyl) ester belongs to the technical field of chemical synthesis. The method comprises the steps: by adopting trimellitic anhydride and 2-propyl heptanol as main reaction raw materials, mixing and heating in the presence of a titanate catalyst, activated carbon and attapulgite to esterify to obtain a 1, 2, 4-benzenetricarboxylicacid tris(2-propyl heptyl) ester crude product after reaction is finished; and carrying out neutralizing, alkali washing and washing on the crude product in turn, distilling at reduced pressure to remove the excessive alcohol, and filtering to obtain the 1, 2, 4-benzenetricarboxylicacid tris(2-propyl heptyl) ester finished product. The method has the advantages of available and low price selected raw materials, small catalyst usage, no obvious corrosiveness, small environmental pollution and the like, and is convenient for operation and energy-saving. The obtained product has small volatility, extraction resistance and transfer resistance and has advantages which are similar to those of a polyester catalyst; and moreover, the compatibility, processability and lower temperature performance of the obtained product are comparable to those of phthalic acid ester, and the obtained product has a wide application.

Description

technical field [0001] The invention discloses a preparation method of plasticizer tris(2-propylheptyl) trimellitate, which belongs to the technical field of chemical synthesis. [0002] It specifically relates to a trimellitate plasticizer with good extraction resistance, good migration resistance, good thermal stability, excellent low-temperature performance, non-toxic and environment-friendly. Its preparation method is to use trimellitic anhydride and 2-propylheptanol to synthesize tris(2-propylheptyl) trimellitate through esterification under the catalysis of titanate, and then neutralize the resulting crude product, wash it with water, and depressurize it. After dealcoholization and filtration, a light yellow oily product was obtained. Background technique [0003] Plasticizers are functional products that are added to high molecular polymers to increase the plasticity of materials, make them easy to process, and endow products with softness. They are widely used in pl...

Claims

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Application Information

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IPC IPC(8): C07C69/76C07C67/08
Inventor 蒋平平叶媛园陈云斌冯烈苗红艳
Owner JIANGNAN UNIV
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