Acid transesterification of oils with ethanol on carbon catalysts

O. Fedoryshyn
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Abstract

The main advantages and disadvantages of solid-phase catalysts for transesterification reactions of oils with alcohols are analyzed. Tests of the sulfonated and phosphated solid - phase catalysts synthesized by us in the transesterification reaction of rapeseed oil with 96% ethanol in order to obtain biodiesel were carried out. The chemical resistance of sulfonated synthetic (S-SCS) and synthesized from natural raw materials (S-KAU) catalysts was compared. The reasons for low chemical resistance of sulfonated carbon-containing materials are determined. Synthetic S-SCS catalysts proved to be the least stable. Regeneration of phosphated samples was performed by washing the catalyst from oil residues and reaction products in a boiling solution of 0.1 M alkali, followed by repeated washing with distilled water to slightly alkaline pH. Then, after drying, the obtained material was used as a source for re-synthesis of the catalyst. The ethanolysis reaction was carried out in autoclaves under pressure at a temperature of 150-160oC with a process duration of 5-7 hours. The ratio of catalyst to starting oil was chosen 1:15 (g : ml). The oil-alcohol ratio was 3: 4, vol. The volume of the autoclave was 45 ml. The maximum conversion under these test conditions in the first cycle for sulfonated catalysts was 100%, and for phosphated - 94%. A carbon-containing catalyst on a ceramic support has been developed, which can be regenerated by firing the carbon-containing material and applying a new one. This catalyst showed the highest chemical resistance, withstanding 7 cycles, while the conversion fell by 14% (from 89 to 75%). For more efficient use of the catalyst, the scheme of flow-circulation installation of transesterification of oils and fats of biological origin with alcohols was proposed.
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油与乙醇在碳催化剂上的酸酯交换反应
分析了用于油与醇酯交换反应的固相催化剂的主要优缺点。以菜籽油为原料,以96%乙醇为原料进行酯交换反应,对合成的磺化和磷酸化固相催化剂进行了试验研究。比较了磺化合成催化剂(S-SCS)和天然原料催化剂(S-KAU)的耐化学性。分析了磺化含碳材料耐化学性低的原因。合成S-SCS催化剂稳定性最差。将催化剂从油渣和反应产物中分离出来,在0.1 M碱的沸腾溶液中洗涤,再用蒸馏水反复洗涤至微碱性,得到的物料干燥后作为催化剂再合成的原料。乙醇解反应在高压灭菌器中进行,温度为150-160℃,过程持续时间为5-7小时。催化剂与启动油的比例为1:15 (g: ml)。油醇比为3:4,体积。高压灭菌器体积为45 ml。在这些测试条件下,磺化催化剂第一次循环的最大转化率为100%,磷酸化催化剂的最大转化率为94%。研制了一种陶瓷载体上的含碳催化剂,该催化剂可以通过烧制含碳材料再涂覆新的含碳材料来再生。该催化剂表现出最高的耐化学性,可承受7次循环,但转化率下降了14%(从89%降至75%)。为了更有效地利用催化剂,提出了生物源性油脂与醇酯交换的流动循环装置方案。
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