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Solvent crystallization of palm based dihydroxystearic acid (DHSA)-effects on crystal morphology and particle size distribution

机译:棕榈基二羟基硬脂酸(DHSA)的溶剂结晶-对晶体形态和粒度分布的影响

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In recent years, oleo based chemicals have made its presence felt among the ever blooming personal care segment, slowly but gradually chipping into the industry once dominated by petrol based chemicals. In particular, the industry has shown considerable interests in hydroxyl fatty acids due to their different behavior compared with ordinary fatty acids. Hydroxyl fatty acids and their derivatives are multipurpose intermediates in the synthesis of fine chemical products and one of the possible derivatives is known as dihydroxystearic acid (DHSA). In Malaysia, palm based DHSA is produced from epoxidation of oleic acid with formic acid, followed by hydrolysis of the epoxide. The crude waxy DHSA is purified by employing solvent crystallization. This study focuses on the use of ethanol and ethanol/water mixture as solvents. The crystallization process was carried out employing two different cooling conditions, i.e. rapid cooling (rapid crystallization) and natural cooling (slow crystallization). The chemical and physical properties of the DHSA crystals produced were evaluated in terms of crystal size distribution (CSD) and scanning electron microscopy (SEM). The results revealed that purification of DHSA through crystallization using ethanol and ethanol/water mixture as solvents was successfully achieved. The crystallization process when carried out with natural cooling mode performed better than that when carried out with rapid cooling mode and the best DHSA to ethanol ratio was of 1.0:1.0 as the combination produced the narrowest CSD curve with largest average crystal particle size.
机译:近年来,油基化学品已在不断发展的个人护理领域中占有一席之地,但在以汽油基化学品为主导的行业中,它却缓慢但逐渐地渗入该行业。特别地,由于羟基脂肪酸与普通脂肪酸相比的不同行为,因此该行业对羟基脂肪酸表现出了极大的兴趣。羟基脂肪酸及其衍生物是精细化工产品合成中的多用途中间体,一种可能的衍生物称为二羟基硬脂酸(DHSA)。在马来西亚,基于棕榈酸的DHSA由油酸与甲酸环氧化,然后水解环氧生成。粗蜡状DHSA通过使用溶剂结晶来纯化。这项研究的重点是使用乙醇和乙醇/水混合物作为溶剂。结晶过程是采用两种不同的冷却条件进行的,即快速冷却(快速结晶)和自然冷却(缓慢结晶)。根据晶体尺寸分布(CSD)和扫描电子显微镜(SEM)评估了所产生的DHSA晶体的化学和物理性质。结果表明,成功地通过使用乙醇和乙醇/水混合物作为溶剂的结晶来纯化DHSA。在自然冷却模式下进行的结晶过程比在快速冷却模式下进行的结晶过程更好,并且最佳的DHSA /乙醇比率为1.0:1.0,因为该组合产生了最窄的CSD曲线,具有最大的平均晶体粒径。

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