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| Synthesis process optimization and characterization of pentaerythritol isostearate catalyzed by p-toluenesulfonic acid |
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| DOI： |
| KeyWord:p-toluenesulfonic acid esterification isostearic acid pentaerythritol isostearate |
| FundProject:国家自然科学基金资助项目（21978112） |
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| Abstract: |
| In order to improve the existing production process of pentaerythritol isostearate, which has the problems of long reaction time, high reaction temperature and low efficiency, the synthesis of pentaerythritol isostearate by esterification of pentaerythritol with isostearic acid catalyzed by p-toluenesulfonic acid was carried out.The esterification process conditions were optimized using single factor experiment and orthogonal experiment with esterification rate of isostearic acid as the index.The crude product of esterification was purified by deacidification, the crude product was analyzed by infrared spectroscopy, and the purified product was analyzed by mass spectrometry, thermogravimetric analysis, and its performance indexes were also determined.The results showed that the optimal process conditions were obtained as follows: reaction time 5 h, reaction temperature 140 ℃, dosage of catalyst 1%(based on the total mass of substrates), and the molar ratio value of isostearic acid to pentaerythritol 4.3. Under these conditions, the esterification rate was 99.27% and the acid value of the crude product was 13.26 mgKOH/g.The infrared spectroscopy results indicated that the esterification reaction synthesized pentaerythritol isostearate, and mass spectrometry identification results showed that the main synthesized product was pentaerythritol tetraisostearate. After deacidification, the acid value of the product was reduced to 3.23 mgKOH/g, which was close to that of the commercial product. The results of thermogravimetric analysis and the performance indexes showed that the purified product had excellent thermal stability, good viscosity-temperature properties, excellent low-temperature fluidity and good safety. The optimized process of synthesis of pentaerythritol isostearate catalyzed by p-toluenesulfonic acid had advantages of low energy consumption and high product quality. |
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