Separation and Purification of Essential Oil by Supercritical Pressure Swing Adsorption

超临界变压吸附分离纯化精油

• 批准号: 08555194
• 负责人: GOTO Motonobu
• 金额: $ 7.1万
• 依托单位: Kumamoto University
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Scientific Research (A)
• 财政年份: 1996
• 资助国家: 日本
• 起止时间: 1996 至 1998
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-08555194/
• 关键词: Supercritical Fluid; Carbon Dioxide; Pressure Swing Adsorption; Orange Oil; Deterpenation; Simulation; Silica gel; Concentration factor; 脱テルベン; シトラスオイル

A new technique for fractionation of citrus oil was proposed. A pressure swing adsorption process in supercritical carbon dioxide (SC-C0_2) was developed with silica gel as adsorbent. The adsorption-desorption process of major solutes in orange oil 011 silica gel was evaluated by the tracer response technique and the breakthrough analysis. Linalool (aroma) was more selectively adsorbed on silica gel than limonene (terpene). The adsorption equilibrium constant was increased with the increase in temperature or the decrease in pressure. The apparent heat of adsorption was calculated from the van't Hoff plot. The intraparticle effective diffusivity for linalool was larger than that of limonene. Mass transport properties showed that the contribution of axial dispersion resistance on the broadening of the chromatographic response peak decreased with the increase in Reynolds number, resulting in the relative importance of intraparticle diffusion resistance. Adsorption isotherm of orange oil w … More as obtained by breakthrough analysis at 313 K and 8.8 MPa. The adsorption isotherm was represented by the Langmuir equation. The density dependency of the adsorption equilibrium constant enabled the extrapolation to the various conditions. Dynamic behaviors of adsorption of orange oil in SC-C0_2 at 313 K and 8.8 MPa and desorption of solutes at 313 K and 19.4 MPa were measured.A continuous cyclic operation (Pressure Swing Adsorption) between the adsorption at a lower pressure and the desorption at a higher pressure, involving the rinse step to remove the solutes in the void region of the adsorber, was demonstrated for citrus oil processing with silica gel adsorbent in SC-CO_2. Effects of feed concentration and half cycle time on the concentration factor of oxygenated compounds were studied. Terpeneless citrus oil was successfully obtained in the desorption step and blowdown step. The increase in half cycle time increased the concentration factor. Higher concentration factor up to 25 was obtained, and tile concentration factor satisfied the commercially required value. The mathematical model for the citrus oil processing by a pressure swing adsorption in SC-CO_2 agreed well with the experimental results. Calculated concentration profile of the solutes in the column showed that the regeneration of the adsorbent was not sufficient and the portion of the utilized adsorbent for tile cyclic operation was small. Adsorption process operated at a higher flow rate of CO_2 during the desorption step may recover the adsorbed valuable solutes. The proposed system showed the feasibility of the continuous operation of the cyclic adsorption process. Less

提出了一种柑橘油分级分离的新工艺。以硅胶为吸附剂，在超临界CO2中进行变压吸附。采用示踪响应技术和穿透分析法研究了主要溶质在橙子油011硅胶上的吸附-解吸过程。芳樟醇（香气）比柠檬烯（萜烯）更有选择性地吸附在硅胶上。吸附平衡常数随温度的升高或压力的降低而增大。表观吸附热由范特霍夫图计算。芳樟醇的颗粒内有效扩散系数大于柠檬烯的颗粒内有效扩散系数。传质性质表明，轴向扩散阻力对色谱响应峰展宽的贡献随雷诺数的增加而减小，导致粒内扩散阻力的相对重要性。橙子油在水溶液中的吸附等温线 ...更多信息 在313 K和8.8 MPa下通过穿透分析获得。吸附等温线符合Langmuir方程。吸附平衡常数的密度依赖性使得能够外推到各种条件。测定了橙子油在313 K、8.8 MPa超临界CO2中的吸附动力学行为和在313 K、19.4 MPa超临界CO2中的解吸动力学行为。（变压吸附）在较低压力下的吸附和较高压力下的解吸之间，包括冲洗步骤以去除吸附器的空隙区域中的溶质，在超临界CO_2条件下，采用硅胶吸附剂处理柑桔油。研究了进料浓度和半循环时间对含氧化合物浓缩因子的影响。在解吸步骤和排污步骤中成功地获得了无萜柑橘油。半周期时间的增加增加了浓缩因子。浓缩倍数可达25以上，满足工业要求。建立的超临界CO2变压吸附法处理柑桔油的数学模型与实验结果吻合较好。计算的柱内溶质浓度分布表明，吸附剂的再生不充分，用于循环操作的吸附剂的比例很小。在解吸阶段，在较高的CO_2流量下操作的吸附过程可以回收被吸附的有价值的溶质。该系统表明了循环吸附过程连续运行的可行性。少

项目成果

Masaki Sato et al.: "New Fraction process of citrus oil by pressure Swing adsorption in Supercritical curbon Dioxidi." Chemical Engineering Science. 53・24. 4095-4104 (1998)

Masaki Sato 等人：“超临界二氧化硫中变压吸附的柑橘油新分馏工艺”53・24 (1998)。

Masaki Sato et al.: "New Fractionation Process of Citrus Oil by Pressure Swing Adsorption in Supercritical Carbon Dioxide" Chemical Engineering Science. 53. 4095-4104 (1998)

Masaki Sato 等人：“超临界二氧化碳变压吸附柑橘油分馏新工艺”化学工程科学。

Masaki Sato et al.: "Extraction and Adsorption Processes for the Fractionation of Citrus oil with Supercritical Carbon Dioxide" Memoirs of the Faculty of Eng.42. 1-35 (1997)

Masaki Sato 等人：“用超临界二氧化碳分馏柑橘油的萃取和吸附过程”工程学院回忆录.42。

Masaki Sato, Motonobu Goto, Akio Kodama, Tsutomu Hirose: "Extraction and adsorption Processes for the franctionation of citrus oil with supercritical carbon dioxide" 熊本大学工学部紀要. 42. 1-35 (1997)

Masaki Sato、Motonobu Goto、Akio Kodama、Tsutomu Hirose：“用超临界二氧化碳分馏柑橘油的提取和吸附过程”熊本大学工程学院公告 42. 1-35 (1997)。

Masaki Sato, Motonobu Goto, Akio Kodama, Tsutomu Hirose: "Fractionation of citrus peel oil by supercritical pressure swing adsorption" Proc. 4th Italian Conf. on Supercrit. Fluids and their Appl.Capri. 39-46 (1997)

Masaki Sato、Motonobu Goto、Akio Kodama、Tsutomu Hirose：“通过超临界变压吸附对柑橘皮油进行分馏”Proc。