Adsorption Processes. Ali Ahmadpour Chemical Eng. Dept. Ferdowsi University of Mashhad

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1 Adsorption Processes Ali Ahmadpour Chemical Eng. Dept. Ferdowsi University of Mashhad

2 Contents Introduction Principles of adsorption Types of adsorption Definitions Brief history Adsorption isotherms Mechanism of separation Industrial adsorbents Adsorption applications Adsorber Desorption methods 2

3 Introduction Separation is a process that transforms a mixture of substances into two or more products that differ from each other in composition. Separation steps account for the major production costs in chemical and petrochemical industries. There are several industrial separation processes. Adsorption is one of the separation technique used for separating gas mixtures based on the solid surface forces. 3

4 Principles of adsorption Adsorption is a surface phenomenon and defined as the increase in concentration of a particular component at the surface or interface between two phases. Adsorption mechanisms are generally categorized as either physisorption, chemisorption, or electrostatic adsorption. Only physical adsorption is encountered in gas separation. 4

5 Cont. Weak molecular forces, such as Van der Waals forces, provide the driving force for physical adsorption. A chemical reaction forms a chemical bond between the compound and the surface of the solid in chemisorption. Electrostatic adsorption involves the adsorption of ions through Coulombic forces, and is normally referred to as ion exchange. In liquids, interactions between the solute and the solvent also play an important role in establishing the degree of adsorption. 5

6 Cont. The amount of adsorption that occurs is dependent on particular characteristics of the adsorbate and adsorbent. The amount of adsorption that takes place on the solid follows various isotherms or kinetic rates. 6

7 Types of adsorption Physical adsorption (Physisorption): The adsorbate is weakly bound onto the adsorbent by a combination of Van der Waals forces and electrostatic forces. No covalent bonds are formed and heat is released upon adsorption. Chemical adsorption (Chemisorption): There is covalent interaction of gas molecule and the surface of the adsorbent which gives scope for much larger increases in adsorption capacity. 7

8 General features of physical & chemical adsorptions Physisorption Low heat of adsorption (< 2 or 3 times latent heat of evaporation). Non-specific. Monolayer or multilayer. No dissociation of adsorbed species. Only significant at relatively low temperatures. Rapid, non-activated, reversible. No electron transfer, although polarization of sorbate may occur. Chemisorption High heat of adsorption (> 2 or 3 times latent heat of evaporation). Highly specific. Monolayer only. May involve dissociation. Possible over a wide range of temperatures. Activated, may be slow and irreversible. Electron transfer leading to bond formation between sorbate and surface. 8

9 Definitions Adsorbate: The complex of adsorptive and adsorbent, i.e., the adsorbing agent in loaded state. Adsorbent: Porous solid having lattice vacancies of uniform size and of molecular dimensions. They selectively adsorb molecules of a certain shape. Adsorption: The reversible attachment of small particles (molecules, atoms, ions) to a solid, the adsorbent. Examples are the attachment of water vapor to a drying agent or the attachment of organic molecules to a zeolite for the purpose of exhaust treatment. Adsorptive: The substance that is to be adsorbed, still in the fluid phase, e.g., solvent molecules. 9

10 Cont. Load: The amount of material adsorbed in the adsorbate, usually expressed in g per g of non-loaded adsorbent or as a percentage figure. For example, zeolite 3A typically can take up water up to 25% of its weight. The maximum load depends on the nature of the adsorbing material and the adsorbed material, the total pressure, the temperature and the competition by other adsorbed substances, e.g., water. Desorption: The release of attached particles from the surface of the adsorbing agent and the transition to the fluid state; reversal of adsorption. Adsorption and desorption are in a state of relative equilibrium; the two processes always occur together. 10

11 Cont. Fluid phase: The fluid medium around the adsorbing material which contains adsorbates (in most cases it is water or air). Kinetics: Mathematical description of the speed of a process, in connection with adsorption, mainly the description of the speed at which a particle moves from the fluid phase to the place of adsorption. Isotherm: Mapping the state of equilibrium of an adsorbing agent with an adsorbed substance against the partial pressure of the adsorbed substance in the fluid phase at constant temperature (isotherm). The isotherm is the most important parameter for design but it alone is not sufficient. 11

12 Brief history 1930s: Recognizing the ability of porous solids to reversibly adsorb large volumes of vapor and gas. 1950s: Investigating the adsorptive properties of coals and carbonized polymers, introducing process for recovery of aromatic hydrocarbons. 1960s: Purification of air and industrial vent gases by shape selective molecular sieves. 1970s: Significant increase in the range and scale of gas separation processes. 1980s-now: A vast growth in separation process technology, mathematical modeling and new 12 adsorbents.

13 Pore structure of adsorbent Based on IUPAC classification: Micropore d <2 nm Mesopore 2 < d <50 nm Macropore d >50 nm 13

14 The difference between Adsorption & Absorption Adsorption is the attraction between the outer surface of a solid particle and a fluid molecule, whereas absorption is the uptake of the fluid molecule into the physical structure of the solid. 14

15 Adsorption of particles from a gas to a solid surface The adsorbate is in a state of equilibrium with the fluid phase, i.e., gas or liquid. The more the adsorbing material is loaded, the higher is its vapor pressure. Very low loads represent a single-place adsorption. In this range, the vapor pressure of the adsorption substance is proportional to the load, which formally corresponds to Henry's law. If pore condensation occurs, the vapor pressure of the adsorption substance enters the range of the vapor pressure of the liquid phase. 15

16 16

17 Cont. How much substance can be taken up by the adsorbing substance, depends on three factors: Temperature: Higher temperatures reduce the load because the adsorption process releases heat. Therefore, it is possible to release the adsorbed material by increasing the temperature. Chemical interaction: The properties of the adsorbing material and the adsorbed substance (polarity), determine the degree of interaction between both. Partial pressure: The higher the concentration of the adsorbed material in the gaseous phase the more material is adsorbed. Reversely, if the concentration of the adsorbed material is low in the gaseous phase, some adsorbed material is released from the adsorbing surface. This means that the adsorbing material can be regenerated with pure gas. 17

18 Cont. The mathematical presentation of concentration versus pressure is referred to as adsorption isotherm. The adsorption isotherm does not describe time-related factors because it reflects an equilibrium state. It is generated by determining the amount of molecules attaching to the adsorbing material after hours of establishing the equilibrium in a static gas atmosphere. 18

19 Adsorption isotherms The mathematical presentation of the context between the adsorptive and the load is referred to as adsorption isotherm. It is plotted at constant temperature. 19

20 Working capacity The working capacity for a gas is the difference in adsorption capacity and desorption capacity. The adsorbent needs to have a good working selectivity (ratio of one gas working capacity to another gas working capacity). 20

21 Cont. Initially there is a linear relationship between the partial pressure and the amount of adsorbed substance and that the adsorbing material is saturated and no more molecules are attached from a certain concentration level. The best-known theoretical prediction is Langmuir's isotherm. This isotherm is one of the most frequently used models. Under practical conditions, the curves take on most different shapes and can even become a hysteresis for desorption, at the onset of pore condensation. The progression of the isotherm depends on the adsorbing material and temperature. A rule of thumb is that the adsorption capacity drops to one half if the temperature goes up by K. 21

22 Forces and energies in adsorption Dispersion (attractive) forces Adsorbate-Adsorbate interaction Adsorbate-Adsorbent interaction Repulsion forces Adsorbate-Adsorbate interaction Adsorbate-Adsorbent interaction 22

23 Mechanism of separation The adsorptive separation is achieved by one of three mechanisms: steric, kinetic, or equilibrium effect. The steric effect derives from the molecular sieving properties of zeolites and molecular sieves. In this case only small and properly shaped molecules can diffuse into the adsorbent, whereas other molecules are totally excluded. Kinetic separation is achieved by virtue of the differences in diffusion rates of different molecules. In this case, the pore size needs to be precisely tailored to lie between the kinetic diameters of the two molecules that are to be separated. Equilibrium separations are based on the differences in adsorbed amounts on the equilibrium. 23

24 Steric separation Steric adsorption is unique with zeolites because of the uniform pore size in the structure. Two largest applications are: Drying with 3A zeolite Separation of n-paraffin from iso-paraffin with 5A zeolite 24

25 Kinetic separation Kinetic separation is possible with carbon molecular sieve because of distribution of pore sizes. The kinetic selectivity is measured by the ratio of the micropores or intracrystalline diffusivities for the components considered. 25

26 Equilibrium separation The separation factor in equilibrium adsorption is: AB X Y A A / X / Y B B X A = mole fraction of component A in adsorbed phase at equilibrium Y A = mole fraction of component A in fluid phase at equilibrium 26

27 Adsorption at equilibrium 27

28 Kinetic separation 28

29 Selective separation 29

30 Industrial adsorbents 30

31 Cont. The past two decades have shown an explosion in the development of new nanoporous materials: mesoporous molecular sieves, zeolites, pillared clays, sol gel-derived metal oxides, and new carbon materials (carbon molecular sieves, super-activated carbon, activated carbon fibers, carbon nanotubes, fullerenes and heterofullerenes, microporous glasses and graphite nanofibers). 31

32 Adsorptive gas separation Gas separations are a major production cost in the chemical industry today. Production of industrial gases by pressure swing adsorption (PSA), is expected to grow much faster than by the conventional method, cryogenic distillation (because of much lower cost for low capacity plants). An economic gas separation process depends primarily on the adsorbent with: High selectivity High capacity Long life 32

33 Adsorbents The porous solid of a given adsorption process is a critical variable. The success or failure of the process depends on how the solid performs in both equilibria and kinetics. A solid with good capacity but slow kinetics is not a good choice as it takes adsorbate molecules too long a time to reach the particle interior. A solid with fast kinetics but low capacity is not good either as a large amount of solid is required for a given throughput. Thus, a good solid is the one that provides good adsorptive capacity as well as good kinetics. 33

34 Cont. To satisfy these two requirements, the following aspects must be satisfied: the solid must have reasonably high surface area or micropore volume the solid must have relatively large pore network for the transport of molecules to the interior (macropores) Most practical solids commonly used in industries do satisfy these two criteria, with solids such as activated carbon, zeolite, alumina and silica gel. 34

35 Alumina Alumina adsorbent is normally used in industries requiring the removal of water from gas stream. This is due to the high functional group density on the surface, providing active sites for polar molecules (such as water). There are a variety of alumina available, but the common solid used in drying is γ-alumina. The characteristic of a typical γ-alumina is given below. 35

36 Silica gel Silica gel is a hard glassy substance and is milky white in color which is made from the coagulation of a colloidal solution of silicic acid. The term gel simply reflects the conditions of the material during the preparation step, not the nature of the final product. This adsorbent is used in most industries for water removal due to its strong hydrophilicity of surface towards water. Some applications of silica gel are: water removal from air drying of non-reactive gases drying of reactive gases adsorption of hydrogen sulfide oil vapor adsorption adsorption of alcohols 36

37 Activated carbon Activated carbon is one of the most complex solids but it is the most versatile because of its extremely high surface area and micropore volume. Moreover, its bimodal (sometimes trimodal) pore size distribution provides good access of sorbate molecules to the interior. The structure of AC is complex and it is basically composed of an amorphous structure and a graphite-like microcrystalline structure. The graphitic structure is important from the capacity point of view as it provides "space" in the form of slit-shaped channel to accommodate molecules. Because of the slit shape the micropore size for activated carbon is reported as the micropore half-width rather than radius as in the case of alumina or silica gel. Although the basic configuration of the graphitic layer in activated carbon is similar to that of pure graphite, there are some deviations, for example the interlayer spacing ranges from 0.34nm to 0.35nm. 37

38 Cont. Commercial activated carbon has a very wide range of properties depending on the application. For liquid phase applications, due to the large molecular size of adsorbate, activated carbons used should have larger mesopore volume and larger average pore radius. Typical characteristics of activated carbon used in gas separation 38

39 Zeolite Zeolite, another widely adsorbent, can be found naturally or made synthetically. Application of natural zeolite is not as widely as that of synthetic zeolite because of the more specificity of the synthetic zeolite. There are many types of synthetic zeolite, such as type A, X, Y, mordenite, ZSM, etc. The typical characteristics of the zeolite A 39

40 Adsorption applications Gas separation N 2 from air O 2 from air n-paraffin separation Gas drying Air drying Solvent drying Drying of cracked gas Gas recovery H 2 recovery Solvent recovery from air Gas sweetening CO 2 from NG Xylene separation 40

41 Commercial adsorption processes and sorbents used 41

42 Cont. 42

43 Cont. 43

44 Some separation and purification applications by new sorbents 44

45 Adsorber 45

46 Cont. Objectives for the development of adsorbents and adsorbent processes can be summarized as follows: Adsorbents Process 46

47 Desorption methods TSA Thermal Swing Adsorption: the desorption is triggered by an increase in temperature. This is energy intensive and slow since the entire mass of adsorbent must be heated. VSA Vacuum Swing Adsorption: the desorption is triggered by creating a near-vacuum. One advantage is that this system will operate at near ambient temperature, so require less energy. Another advantage is that the energy used is applied only to adsorbed molecule and so it is thermodynamically more efficient than TSA. PSA Pressure Swing Adsorption: the desorption is triggered by a decrease in pressure, usually from an elevated level to near atmospheric pressure. 47

48 Cont. ESA Electrical Swing Adsorption: the desorption is triggered by an applied voltage. This method has the advantage of being fast and require less energy. Different separation process configurations are possible depending on the temperature and pressure of the effluent gas stream. 48

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