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1 HA NOI UNIVERSITY OF SCIENCE AND TECHNOLOGY SCHOOL OF CHEMICAL ENGINEERING DEPARTMENT OF PHARMACEUTICAL CHEMISTRY AND PESTICIDES TECHNOLOGY ACADEMIC ESSAY EXTRACTION TECHNIQUES Instructor: Dr Dinh Thi Phuong Anh Student: Ngo Thi Thuy Student ID: 20175228 HÀ NỘI.1/2022 Contents Solid-liquid extraction ( ionic liquid) 1.1 Denifintion .5 1.1.1 Ionic liquids (ILs) .5 1.2 Solid- liquid Extraction Process 1.2.1Principle of Solid – Liquid Extraction .8 1.2.2 Solid- liquid Extraction Process 1.3 Solid-Liquid Extraction Equipment .9 1.4.Applications of Solid-Liquid Extraction(Ionic-liquid) .17 1.5.Example .18 Microwave-assisted extraction .23 2.1 Introduction 23 2.2 Principles of Microwave-Assisted Extraction 24 2.3 Microwave extraction process 27 2.4 Microwave Assisted Extraction equipment 29 2.3.1 Soxhlet Extractor 29 2.3.2 Dynamic extractor 31 2.5.Application of MAE .35 2.6.Example 36 Perstraction 40 3.1 Introduction 40 3.1.2 Denifintion : .41 3.2 Principles of Pertraction 42 3.3 Process of perstraction .43 3.4.Specific advantages and disadvantages 44 3.4.1 Advantages .44 3.4.2 Disadvantages 44 3.5.Perstraction equipment 44 3.6 Applications of Perstraction 46 3.7.Example 46 Solid-liquid extraction 1.1 Denifintion ➢ Solid-Liquid Extraction is a solid-liquid contact mass transfer operation in which solute particles are transferred from solid to liquid ➢ Solid-liquid extraction is also called Leaching ➢ Solid-liquid extraction works on the principle of difference in solubility of specified solids in liquids ➢ The liquid used for solid-liquid extraction is called the solvent The Solid which carries solute particles is called an insoluble solid (Inc, 2009) 1.1.1 Ionic liquids (ILs) Ionic liquids (ILs) are widely recognized solvents due to their extended list of excellent properties, and their success comesmainly fromtheir unique and fascinating characteristics as non-molecular solvents, a negligible vapor pressure associated to a high thermal stability, tunable viscosity and miscibility with water and organic solvents These properties are the result of being molten salts that are liquid below 100 ◦C which generally consist of organic cation (e.g imidazolium, pyrrolidinium, pyridinium, tetraalkyl ammonium or tetraalkyl phosphonium) and inorganic or organic anion (e.g tetrafluoroborate, hexafluorophosphate, bromide) In addition, the high number of possible combination provides a long list of ILs with different polarity, hydrophobicity and viscosity, among others For this reason ILs are known as “designer solvents” Table The structures of the ILs applied in extraction and separation: 1.2 Solid- liquid Extraction Process 1.2.1 Principle of Solid – Liquid Extraction Solid-Liquid Extraction occurs in two steps: • Contacting solvent and solid to effect a transfer of a solute (leaching) • The separation of the solution from the remaining solid (washing) ❖ Factors Affect Solid-Liquid Extraction Operation Solid: Solid used for solid-liquid extraction can be porous or nonporous The solute may be distributed on a solid surface or inside pores of solid Recovery of solute from the solid surface is easier than from pores of solid Pores of solid create another mass transfer resistance for the solvent to go in and for the solute to come out Solid particle's size also plays an important role in the operation Recovery of solute from small size solid particles are easier and more effective than bigger particle sizes Solvent: The solvent used for operation is also an important parameter to take into consideration in operation The solvent which contains desirable properties which are listed below is more preferred Temperature: Temperature is also an important parameter in solid-liquid extraction because the solubility of solid particles is also dependent on temperature Mixing: Mixing of solid particles and liquid solvent decides the effectiveness of contact which is also important for parameter solid-liquid extraction More thorough mixing confirms more contact between solid and liquid and this results in higher mass transfer 1.2.2 Solid- liquid Extraction Process ➢ Solid-liquid extraction there are steps Size reduction of solids Mixing of solids with solvent Liquid Overflow and underflow separation Solvent recovery from overflow and underflow ➢ Solid-liquid phase extraction is achieved through the interaction of three components: • the sorbent • the analyte • the solvent ➢ Type of ionlic liquid extraction This section is thus divided into three parts based on the most frequently employed extraction processes: ➢ simple IL-based SLE; ➢ IL-based MAE; ➢ IL-based UAE 1.3.Solid-Liquid Extraction Equipment 1.3.1 Soxhlet Extractor The Soxhlet extractor is used for liquid-solid extractions when the compound to be extracted has limited solubility in the chosen solvent and the impurities are insoluble During the extraction, solvent vapour will flow up the distillation path, into the main chamber and up into the condenser where it will condense and drip down The solvent will fill the main chamber, dissolving some of the desired compound from the solid sample Once the chamber is almost full, it is emptied by the siphon, returning the solvent to the round bottom flask to begin the process again Each time the extraction is repeated, more of the desired compound is dissolved, leaving the insoluble impurities in the thimble This is how a compound is removed from the sample 10 The Soxhlet extractor will run continuously once set up correctly: Load the sample material containing the desired compound into the thimble Place the thimble into the main chamber of the Soxhlet extractor Add the chosen solvent to a round bottom flask and place onto a heating mantle ➢ Attach the Soxhlet extractor above the round bottom flask ➢ Attach a reflux condenser above the extractor, with cold water entering at the bottom and exiting above ➢ Now the apparatus is set up, heat the solvent to reflux and leave to extract for the required amount of time ➢ ➢ ➢ ➢ ... Extraction Process 1.3 Solid-Liquid Extraction Equipment .9 1.4.Applications of Solid-Liquid Extraction( Ionic-liquid) .17 1.5.Example .18 Microwave-assisted extraction. .. The structures of the ILs applied in extraction and separation: 1.2 Solid- liquid Extraction Process 1.2.1 Principle of Solid – Liquid Extraction Solid-Liquid Extraction occurs in two steps: • Contacting... 23 2.2 Principles of Microwave-Assisted Extraction 24 2.3 Microwave extraction process 27 2.4 Microwave Assisted Extraction equipment 29 2.3.1 Soxhlet Extractor