利用微乳化電層析進行苯甲酸系列化合物的分析研究

The research of the analysis of aromatic acid series compounds by microemulsion electrokinetic chromatography.

魏麒修(Chi-Hsiu Wei)

指導教授 ： 黃悉雅

中原大學/理學院/化學系/碩士(2006年)

https://doi.org/10.6840/CYCU.2006.00463

摘要

本研究以微乳化電層動層析法開發分析苯甲酸系列化合物的方法，其包含苯甲酸，對醛基苯甲酸，對甲基苯甲酸，鄰-，間-，對-苯二甲酸，與1,2,3-，1,2,4-，1,3,5-苯三甲酸等。這些苯甲酸系列化合物為工業上製造聚酯絲、聚酯粒、塑化劑、染料、香料、樹脂及防腐劑的重要原料，且廣用於我們日常生活中。對苯二甲酸現今廣用於製造人造絲以紡織成為衣服。而對苯二甲酸製程之氧化段中所產生之其他苯甲酸系列化合物，嚴重影響聚酯絲的聚合生產與產品品質，並生成於氧化段的觸媒母液中，且不純物大量生成時會抑制或干擾反應，而降低生產率。如能適當控制不純物的濃度，便能減少高價觸媒母液的排放量而有效降低生產成本。至此我們為獲得最佳微乳化電動層析法的分離效果，測試微乳化溶液的組成、毛細管溫度、電壓、管柱長度等變因對分離苯甲酸系列化合物移動速率之影響，且證明該分離效能是微胞電層析方法(MEKC)所無法達到的。最後以0.975%正辛烷、3.7%十二烷基硫酸鈉(SDS)、5.0%環己醇與90.375% pH 2.0 (50mM)磷酸鹽溶液所配製成的微乳化溶液，在26℃的毛細管溫度，40cm毛細管長度與18kV應電壓下獲得九種成份的基線分離。最後本研究已證明上述方法可有效測定在PTA製程的回收觸媒母液中之苯甲酸系列化合物的成份，也就是觸媒母液中之不純物分析。

關鍵字

對苯二甲酸 ； 苯甲酸系列化合物 ； 微乳化電層析

並列摘要

In this study, a microemulsion electrokinetic chromatographic method was developed to analyze nine aromatic acid series compounds including benzoic acid, terephthalaldehydic acid, 4-Methylbenzoic acid, phthalic acid, isophthalic acid, terephthalic acid, 1,2,3-, 1,2,4-, and 1,3,5-benzenetricarboxylic acid. These aromatic compounds were important raw material, and were used to produce polyester fiber, polyester pellets, plasticizer, dyes, perfumes, resin, and preservatives, which have widely used in our daily life. Terephthalic acid was able to be used to produce the man-made fiber, and then was made up the clothes further. The others aromatic acid compounds which were also produced in oxidation plant of terephthalic acid process, affected significantly the polymerization of polyester production and the quality of product. As these aromatic compounds in the mother liquor of oxidation plant with higher concentration could suppress and interfere to the oxidation reaction of p-xylene, and then reduced the rate of production. Since the mother liquor were expensive, thus control the concentration of impurities in the mother liquor was more important, then the purge amount of mother liquor determined the production cost. Therefore, The effect of compositions of microemulsion solution, capillary temperature, applied voltage, and the length of column of capillary on the mobilities of aromatic acid series compounds were examined in order to achieve optimal MEEKC separations. A separation baseline of nice aromatic acids could be obtained by a microemulsion solution composed of 0.975% n-octane, 3.7% sodium dodecyl sulfate (SDS), 5.0% cyclohexanol and 90.375% phosphate solution of pH2 (50mM) under capillary temperature of 26℃ , 40cm capillary length and applied voltage of 18kV, whereas the separation performance of the nine aromatic acid compounds were able to be achieved by MEKC method. Finally, this study has demonstrated that the above method can successfully determine the contents of aromatic acids series compounds in recycled mother liquor of PTA (Purified Terephthalic Acid) production, i.e. the impurities analysis of mother liquor.

並列關鍵字

Aromatic acid ； MEEKC ； PTA

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