Classifications

• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
  • C01C1/00—Ammonia; Compounds thereof
  • C01C1/02—Preparation, purification or separation of ammonia
  • C01C1/12—Separation of ammonia from gases and vapours
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  • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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  • B01D53/34—Chemical or biological purification of waste gases
  • B01D53/46—Removing components of defined structure
  • B01D53/54—Nitrogen compounds
  • B01D53/58—Ammonia
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  • B01J20/0233—Compounds of Cu, Ag, Au
  • B01J20/0237—Compounds of Cu
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  • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
  • B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
  • B01J20/0288—Halides of compounds other than those provided for in B01J20/046
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• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
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Definitions

• the present invention relates to a novel adsorbent composition for use in selective adsorption of ammonia, the manufacture of the ammonia selective adsorbent composition and a separation process employing the same. More specifically, the present invention relates to a copper(I) containing adsorbent composition having a high selectivity for ammonia and also having highly improved adsorption capacity for ammonia as well as having improved regeneration properties, and a process for producing the same.
• the present invention relates to an ammonia separation process employing a specially prepared adsorbent composition to effectively separate and recover ammonia from a gas mixture of ammonia and at least one other gas selected from the group consisting of air, nitrogen, carbon dioxide, methane, hydrogen, argon, helium, ethane, and propane as well as solvent vapors commonly known as VOC compounds, in an efficient manner using a copper(I) containing adsorbent composition having a high adsorption capacity for ammonia.
• a specially prepared adsorbent composition to effectively separate and recover ammonia from a gas mixture of ammonia and at least one other gas selected from the group consisting of air, nitrogen, carbon dioxide, methane, hydrogen, argon, helium, ethane, and propane as well as solvent vapors commonly known as VOC compounds
• Ammonia (NH 3 ) is widely used in chemical industiy as a raw material for the synthesis of various chemicals including fertilizers, melamine and urea. Almost all ammonia utilizing chemical processes produce also ammonia containing gas mixtures, in which it is necessary to separate ammonia gas from other gases. Additionally, the ammonia manufacturing processes, e.g. Haber-Bosch process, produce ammonia containing gas mixtures, which are essential to separate and recover because of process competitiveness.
• the ammonia separation is conventionally accomplished by cryogenic separation in which a gas mixture is liquefied by cooling and the resulting liquid mixture is then subjected to distillation at a low temperature to obtain each gas component separately.
• cryogenic separation is unsatisfactory, because it has the following drawbacks: (1) A large amount of electric power is required for separation.
• ammonia is also separated from gas mixtures by wet absorption techniques known to those skilled in the art, for example, gas scrubbers.
• the absorption processes can be irreversible or reversible. If the ammonia gas is absorbed, e.g., in acidic solution, which converts the ammonia gas to a soluble ammonia salt in a chemical reaction, the process is typically irreversible and re-use is not possible.
• the reversible absorption processes also exist, where ammonia is absorbed in an aqueous solution or an organic solvent, such as polyhydric alcohols, and it is desorbed, e.g., by heating. These processes are unsatisfactory, however, because they are difficult to operate, the investment cost of apparatus is high, and the absorbing solutions are unstable in use.
• Gas adsorption is a separation process, which consists of passing a gas stream through a solid adsorbent bed, so that a gas component is adsorbed and the gas component depleted effluent gas stream is obtained. Thereafter, the adsorbed gas is desorbed, in other words, regenerated from the solid adsorbent by heating and/or by depressurising.
• the adsorption processes can eliminate the drawbacks accompanying the ciyogenic and abso ⁇ tion separations.
• the ammonia separation and recovery by adsorption differs from other gas adsorption processes, e.g.
• ammonia as a polar molecule is adsorbed very strongly onto many conventional adsorbents, e.g. zeolites, alumina, and silica gel as well as ion-exchange resins in H+, Co(II), Cu(II), Ni(II), and Zn(II) forms (S.Kamata and M.Tashiro, J.Chem.Soc.Jpn., Ind.Chem.Soc, 73, 1083(1970)).
• zeolites e.g. zeolites, alumina, and silica gel
• ion-exchange resins in H+, Co(II), Cu(II), Ni(II), and Zn(II) forms (S.Kamata and M.Tashiro, J.Chem.Soc.Jpn., Ind.Chem.Soc, 73, 1083(1970)).
• Activated carbons behave differently in the ammonia adsorption compared to the other conventional adsorbents.
• the ammonia adso ⁇ tion isotherms of activated carbons are almost linear. Therefore, they are easy to regenerate even by depressurising.
• the ammonia selectivity and the adso ⁇ tion capacity of activated carbons are low, especially, at low pressures, and high bed volumes are needed in adso ⁇ tion columns. It can be said the problems in the ammonia separation and recovery by adso ⁇ tion are related to the poor selectivity, low capacity and regenerability of the conventional adsorbents.
• the regeneration is carried out by direct contact of said adsorbent with a concentrated hot stream of ammonia-containing gases at 150 °C.
• the high pressure is needed to achieve the high capacity for the adsorbent as well as the high temperature in the regeneration for releasing a sufficient amount of ammonia gas.
• U.S. Pat. No. 4,758,250 discloses ammonia separation processes, which utilize anion-exchange polymer adsorbents. It is, however, well known that the anion- exchange polymers are expensive and unstable at elevated temperature. Therefore, it is impractical and uneconomical to use the anion-exchange polymers in the ammonia adso ⁇ tion processes.
• EP-570 835 suggests the use of Fe(II), Fe(III), Co(II), Ni(II), Cr(II), Cr(III), Mn(II), Zn(II), Cu(I) or Cu(II) salts supported on an amo ⁇ hous oxide, such as Si0 2 , A1 0 3 , or silica-aluminas, for the selective separation of ammonia in a gas or liquid phase. These adsorbents are prepared directly by impregnation using an aqueous solution of the mentioned salts. The method presented in EP-570 835 is applicable only for water-soluble salts, e.g., Cu(II) salts.
• This invention overcomes the above drawbacks by providing a novel adsorbent, which has an unexpectedly high ammonia selectivity and capacity, but is still easy to regenerate as will be described in greater detail below.
• the present invention provides a process for the separation of ammonia from a gas mixture with a solid copper(I) containing adsorbent composition, in which copper predominantly is in oxidation state I.
• the process comprises contacting a gas mixture with a solid adsorbent composition prepared as described hereinafter.
• the contacting of the gas mixture and the solid adsorbent composition occurs under conditions such that the ammonia is adsorbed onto the solid adsorbent composition.
• the gas mixture contains ammonia and at least one other gas preferably selected from the group consisting of air, nitrogen, carbon dioxide, water, methane, hydrogen, argon, helium, ethane, and propane.
• the separating and recovering of ammonia from offgases in melamine preparation is possible.
• a melamine plant is not needed to be built near a urea plant.
• the preferred temperature and pressure are such that carbamate formation is prevented.
• the temperature can for example be within the range of 100-250 °C and the pressure, depending on possible pretreatments, can for example be within the range of 1-200 bar.
• the ammonia separation can be carried out by techniques, which are per se known in the art, such as the pressure swing adso ⁇ tion (PSA) or vacuum swing adso ⁇ tion (VSA) process.
• PSA pressure swing adso ⁇ tion
• VSA vacuum swing adso ⁇ tion
• the process of the invention for separating ammonia from a gas mixture, which is passed through one or more copper(I) containing adsorbent beds comprising the steps of:
• step (3) repressurising said adsorbent bed(s) to the pressure of adso ⁇ tion.
• said adsorbent bed(s) is/are purged with ammonia in step 2(a).
• the repressurising can be performed by passing the feed gas or a non-adsorbing or weakly-adsorbing gas into the adsorbent bed(s).
• the pressure of the deso ⁇ tion step can e.g. be one fifth or less, preferably one tenth or less than the pressure of the adso ⁇ tion step.
• the present invention provides high capacity, selective and easily regenerable copper(I) containing ammonia adsorbent compositions.
• the present invention provides methods for the preparation of high capacity, selective and easily regenerable copper(I) containing ammonia adsorbent compositions.
• the said adsorbent compositions comprise copper(I) bound to a solid support.
• the said adsorbent may also be the solid mixture of copper(I) compound and an other compound.
• the solid adsorbent compositions can be prepared by three methods. Firstly, an inorganic or an organic support selected from the group consisting of activated carbon, polymer, amo ⁇ hous oxide or crystalline material is impregnated with a solution of a cupric compound. Thereafter, the copper(II)-impregnated support is heated at an elevated temperature under inert, oxidative or reductive atmosphere.
• the solid adsorbent compositions can be prepared by heating a solid mixture containing a cuprous or cupric compound and an inorganic or organic support, and if necessary, reducing the copper(II) compound to copper(I).
• the solid adsorbent compositions can be prepared by ion-exchanging an inorganic or an organic support with a soluble cupric solution. Thereafter, the copper(II)-exchanged support is heated at an elevated temperature and, if necessary, reduced to copper(I) form.
• Fig. 1 shows the adso ⁇ tion isotherm of a CuCl/Si0 2 adsorbent of the present invention
• Fig. 2 shows the adso ⁇ tion isotherm of a commercial 5 A zeolite adsorbent
• Fig. 3 A shows the adso ⁇ tion equilibrium isotherms of a Cu(I)Cl/Al 2 0 3 adsorbent of the present invention and a Cu(II)Cl 2 /Si0 2 adsorbent, at 383 °K
• Fig. 3B shows the adso ⁇ tion equilibrium isotherms of the same adsorbents as in Fig. 3A at 423 °K
• Fig. 4 shows the adso ⁇ tion equilibrium isotherms of a Cu(I)Cl/Al 2 0 3 adsorbent of the present invention at high pressure
• Fig. 5 shows the adso ⁇ tion equilibrium isotherms of a Cu(I) adsorbent of the present invention
• Fig. 6 shows the C0 adso ⁇ tion on a Cu(I)Cl/Al 2 0 adsorbent of the present invention and a Cu(II)Cl 2 /Si0 2 adsorbent.
• the present invention is a process for selective ammonia separation from gas mixtures containing ammonia and at least one other component, which uses novel copper(I) containing compositions, in which copper predominantly is in oxidation state I.
• the process comprises contacting a gas mixture with a solid adsorbent composition prepared as described hereinafter.
• the contacting of the gas mixture and the solid adsorbent composition occurs under conditions such that the ammonia is adsorbed onto the solid adsorbent composition.
• the gas mixture contains ammonia and at least one other gas selected from the group consisting of air, nitrogen, carbon dioxide, water, methane, hydrogen, argon, helium, ethane, and propane.
• this invention is directed to the preparation and use of copper(I) containing compositions that have a high selectivity and capacity as well as are easily regenerable for ammonia separation by adso ⁇ tion.
• the adsorbent compositions can be used in pressure-swing adso ⁇ tion (PSA), vacuum-swing adso ⁇ tion (VSA) and temperature swing adso ⁇ tion (TSA) types of processes. Actually, all these processes are methods, how to operate the adso ⁇ tion separation of a desired gas from a gas mixture. They do not dete ⁇ nine whether the separation is possible or not. The adsorbent determines this.
• the PSA process comprises adsorbing the desired gas onto an adsorbent at a high pressure (above 1.013 bar) and then, desorbing the adsorbed gas by depressurising.
• a plurality of columns packed with the adsorbent are installed and in each adso ⁇ tion column, a series of operations of pressurising- adso ⁇ tion-purging-depressurising is repeated so as to effect a continuous separation and recovery of the product gas.
• the VSA process is similar as the PSA process except the adso ⁇ tion step can be carried out at 1.013 bar or above, and the depressurising is always performed by evacuating.
• the desired gas is first adsorbed onto an adsorbent at a low temperature and then, by raising the temperature of the adso ⁇ tion system, the adsorbed gas is desorbed. It is possible enhance the regeneration by utilizing the heat released at the adso ⁇ tion step. The utilized heat can remain inside the bed in the adso ⁇ tion step, or it can be removed from the bed in the adso ⁇ tion step and transferred back in the regeneration step. In the previous processes, the regeneration can also be carried out by purging using a non-adsorbing or weakly-adsorbing gas. It is also possible to enhance the prevailing regeneration mechanism by an additional purging and/or heating. Additionally, the combinations of the previous processes are possible, such as VTSA, PTSA, and the like. The adsorbent composition according this invention is also feasible to use in rotating wheel type adso ⁇ tion processes.
• the adso ⁇ tion separation by the adsorbent composition according this invention can be carried out by the PSA or VSA processes.
• the gas mixture is passed through one or more adsorbent beds in a sequence of steps comprising: (1) adsorbing ammonia from the gas mixture in the said adsorbent bed composition, (2) desorbing the said adsorbent bed after adso ⁇ tion, (a) by purging the adsorbent bed with product, i.e., ammonia, and (b) by depressurising the adsorbent bed to recover ammonia, and (3) repressurising the adsorbent bed to the adso ⁇ tion pressure e.g. by passing a non-adsorbing or weakly-adsorbing gas into the adsorbent bed.
• adsorbent compositions not only have a high adso ⁇ tion capacity for ammonia, but also have an ability to remove that at very low partial pressures of the ammonia. Most of them are capable of reducing the ammonia content in a gas mixture to as low as 10 ppm by volume or even lower.
• the form of the adsorbent is not critical.
• the adsorbent may be of any of granular, spherical and particulate forms.
• the adsorbent may be of any other form than the above mentioned forms, e.g. honeycomb, structured packing, membrane or massive form prepared by the molding or pelletising of the adsorbent having a granular, spherical or particulate form.
• Non-limiting examples of those materials that can be used as the support for the adsorbent composition of the present invention are as follows: natural or synthetic zeolites, silica gel, silica, alumina, activated alumina, silica-alumina gel, porous aluminium phosphate, clay minerals, such as montmorillonite, titania, charcoal, activated carbon, polymer, such as cation exchange resin, organic-inorganic hybrid composition, such as sulphonated polystyrene grafted silica and the like.
• Preferred zeolites include, e.g., zeolite A, zeolite X, zeolite Y, dealuminated Y zeolite, zeolite omega, zeolite ZSM, mordenite, silicalite, and their mixtures.
• the cations present in zeolites can be NH ions, H + ions, Na + ions, K + ions, Ca 2+ ions, Mg 2+ ions, Cu + ions, Cu 2+ ions, Ag + ions, Fe 2+ ions, Fe 3+ ions, and combinations of thereof.
• the solid adsorbent composition employed in the process of this invention comprises a cuprous compound or mixture of thereof supported on the above described support.
• Cuprous compound can be introduced onto the support by techniques known to those skilled in the art, e.g., impregnation, ion-exchange or thermal dispersion. These techniques are illustrated in detail hereinafter.
• the starting zeolite, silica-alumina, silica, silica gel, activated alumina, alumina, clay mineral, polymer, hybrid, charcoal and activated carbon support of this invention are available commercially or can be synthesised according to procedures well documented in the art.
• cuprous ions are an essential component of the solid adsorbent composition in this invention. Impregnation, thermal dispersion and ion- exchange, described hereinafter, may be employed to introduce copper into the support. In the case of ion-exchange and impregnation, typically, a water-soluble cupric compound is employed because cuprous compounds are not sufficiently soluble or stable, especially in water. It is obvious that if a cupric compound is impregnated or ion-exchanged into the support, then the reduction of copper(II) is required to obtain copper(I), the more desirable form of copper.
• ion-exchange is taken to mean a technique whereby metal ions, specifically copper ions in this case, actually replace a portion or essentially all of the cations of the zeolite, ion-exchange resin or sulphonated polystyrene grafted silica.
• Ion-exchange can be carried out by stirring or slurrying the zeolite or the ion-exchange resin or the sulphonated polystyrene grafted silica with an excess of a solution containing a soluble copper(II) compound.
• the ion-exchange can also be carried out continuously in a column. In both cases the concentration of solutions will vary depending upon the desired degree of ion-exchange, but typically range from about 0.01 M to about 10 M. Heating may also be beneficial in some cases to enhance the ion-exchange.
• the ion-exchanged adsorbent is dried at a temperature in the range from about 50 °C to about 120 °C to remove excess and adsorbed solvent. Alternatively, before drying the ion-exchanged adsorbent can be washed with water to remove nonbounded compounds. After drying, the ion-exchanged adsorbent is heated at a temperature in the range from about 80 °C to about 800 °C under inert, oxidative or reductive atmosphere and, if necessary, reduced to convert a portion of the copper(II) to copper(I) form. The reduction can be carried out with any reducing agent and reductive atmosphere that is capable of this conversion.
• Non-limiting examples of oxidative and inert atmospheres are air and nitrogen, respectively.
• Non-limiting examples of reducing agents and reductive atmospheres include hydrogen, carbon monoxide, and ammonia, nitrogen, helium, argon or mixture of thereof.
• the reduction temperature ranges from about 80 ° to about 500 °C.
• the ion-exchange resins and sulphonated polystyrene grafted silica are applied the temperatures below 120 °C as well as for the zeolites the whole range is applicable.
• the soluble cupric compound may be cupric halides, cupric oxide, cupric carboxylates, cupric basic salts, copper(II) amine complex salts, cupric sulphate, and cupric nitrate or mixture of thereof.
• the cupric compound is cupric halide, cupric sulphate or cupric nitrate.
• the amount of copper in the form of copper compound in the adsorbent compositions according this invention can be 1 to 95 w-%.
• a thermal dispersion may be employed.
• a mixture containing the copper compound and the above described support is used.
• the mixture is prepared simply by mixing a solid powder form of the copper compound with the solid support.
• the mixture can also be obtained by adding to the solid support a solution or suspension of the copper compound in a suitable solvent and thereafter removing the solvent from the resultant mixture by heating and/or pumping.
• Many cuprous compounds and cupric compounds or their mixtures can be used as the copper compound.
• Non-limiting examples of the copper compound which can be suitably utilized in the practice of this invention include, e.g., cuprous halides, such as cuprous chloride, cuprous bromide, cuprous fluoride, and cuprous iodide; cuprous oxide; cuprous carboxylates, such as cuprous carbonate, cuprous formate, and cuprous acetate; cupric halides, such as cupric chloride, cupric bromide, cupric iodide, and cupric fluoride; cupric oxide; cupric carboxylates, such as cupric acetate and cupric formate; cupric basic salts, such as basic copper(II) carbonate, basic copper(II) acetate and basic copper(II) phosphate; and copper(II) amine complex salts, such as hexamine co ⁇ per(II) chloride as well as cupric sulphate, cupric nitrate, and the like.
• cuprous halides such as cuprous chloride, cuprous bromide
• a fairly large class of solid materials may be utilized. However, it is desirable that the surface area of those materials used as a support is greater than 100 m 2 g "1 .
• Non-limiting examples of those materials that can be used as the support for the adsorbent composition of the present invention are as follows: natural or synthetic zeolites, silica gel, silica, alumina, activated alumina, silica-alumina gel, porous aluminium phosphate, clay minerals, titania, charcoal, activated carbon and the like.
• Preferred zeolites include, e.g., zeolite A, zeolite X, zeolite Y, dealuminated Y zeolite, zeolite omega, zeolite ZSM, mordenite, silicalite, and their mixtures.
• the cations present in zeolites can be NH ⁇ + ions, H + ions, Na + ions, K + ions, Ca + ions, Mg 2+ ions, Cu + ions, Cu 2+ ions, Ag + ions, Fe 2+ ions, Fe + ions, and combinations of thereof.
• the amount of copper in the form of the copper compound is preferably from 1 to 200 w-%, more preferably from 5 to 90 w-%.
• the above prepared mixture containing the copper compound and the support is subjected to heating.
• the heating temperature determines, whether the preparing the adsorbent composition is the solid-solid, liquid-solid or vapor-solid method. If the heating temperature is below the melting temperature of the copper compound, the preparing takes place by the solid-solid method. As before, if the heating temperature is below or above the vaporising temperature of the copper compound, the preparing is conducted by the liquid-solid method or the vapour-solid method, respectively. In all cases the support is stayed as a solid form. Generally, the heating temperature is greater than 150 °C, but lower than the decomposition temperature of the compound.
• the heating step is preferably performed at a temperature, which ranges from about 200 °C to about 800 °C.
• the time needed for heating ranges from about 1 minute to about 100 hours, preferably from about 10 minutes to about 50 hours.
• the copper compound and the support can be mixed continuously, occasionally or they are not mixed at all.
• the mixing can be carried out pneumatically or mechanically, e.g., in the rotating oven or drum.
• the heating can be carried out in a suitable reducing atmosphere, such as carbon monoxide, hydrogen, acetylene, ethene, ammonia, nitrogen, helium, argon or mixture of thereof.
• a suitable reducing atmosphere such as carbon monoxide, hydrogen, acetylene, ethene, ammonia, nitrogen, helium, argon or mixture of thereof.
• Most preferable reducing atmosphere is carbon monoxide, hydrogen and ethene.
• the heating can be carried out in a suitable inert atmosphere or in vacuum.
• the suitable inert atmosphere is nitrogen, methane, argon, helium, carbon dioxide, or a mixture of thereof.
• the heating can also be carried out simply in air, in an inert atmosphere or in vacuum.
• the reduction of these compositions can be conducted by means of any known reduction process in the art, e.g., by heating at temperatures greater than 100 °C at a reductive atmosphere, such as carbon monoxide, hydrogen, acetylene, ethene, ammonia, nitrogen, helium, argon or mixture of thereof.
• a reductive atmosphere such as carbon monoxide, hydrogen, acetylene, ethene, ammonia, nitrogen, helium, argon or mixture of thereof.
• Impregnation refers to a technique whereby a metal compound, which means in this invention a soluble copper(II) compound, is deposited on the surface and throughout the pore structure of the support, but predominantly on the surface. Impregnation can be effected by dipping the support into an excess of a solution of a copper compound, such as the chloride, nitrate, acetate or sulphate. Preferably, more precise control is achieved by a technique called “dry impregnation” or “impregnation to incipient wetness". In this method the support is sprayed with a quantity of the copper(II) solution corresponding to the total known pore volume, or slightly less. The impregnation can also be carried out by using dispersing agents, such as carboxylic acids and sugars.
• the support is usually dried at a temperature ranging from about 50 °C to about 120 °C to remove excess and adsorbed solvent.
• the copper(II)-impregnated support essentially comprises a solid mixture containing a copper(II) compound and a support.
• the dried, impregnated support is heated under inert or oxidative atmosphere.
• the heating temperature ranges from about 80 °C to about 800 °C.
• the heating temperature is 200 °C to 500 °C.
• the needed time ranges from about 1 hour to about 24 hours.
• the heating can be carried out in a suitable reducing atmosphere, such as carbon monoxide, hydrogen, acetylene, ethene, ammonia, and a combination of thereof.
• a suitable reducing atmosphere such as carbon monoxide, hydrogen, acetylene, ethene, ammonia, and a combination of thereof.
• Most preferable reducing atmosphere is carbon monoxide, hydrogen and ethene.
• the impregnated copper(II) carrier is reduced to copper(I).
• Any reducing agent which can accomplish the reduction efficiently is acceptable, including hydrogen, ammonia, olefinic hydrocarbons, such as butene, propylene, and butadiene; alcohols, such as propanol, and aldehydes, nitrogen, helium, argon or mixture of thereof.
• carbon monoxide, hydrogen, ammonia and ethene is used.
• the reducing conditions are found to be specific to the reducing agent.
• the copper(I) adsorbent is usually stripped under nitrogen gas at a temperature from about 100 °C to about 250 °C, for a time ranging from about 30 minutes to about 12 hours.
• the soluble cupric compound may be cupric halides, cupric oxide, cupric carboxylates, cupric basic salts, copper(II) amine complex salts, cupric sulphate, and cupric nitrate or mixture of thereof.
• the cupric compound is cupric halide, cupric sulphate or cupric nitrate.
• the amount of copper in the form of copper compound in the adsorbent compositions prepared via impregnation can be 1 to 95 w-%.
• Copper(II) adsorbent composition namely Cu(II)Cl 2 /Si0 was prepared by mixing 20.2 g of pulverised CuCl 2 • 2 H 2 0 with 80.1 g of silica gel (mean pore size 60 A and particle size 0.2-0.5 mm). The mixture was heated under nitrogen gas flow at 280 °C for 23 hours. After heating, it was found that the CuCl 2 salt was evenly spread at the surface of silica gel.
• Copper(I) adsorbent composition namely Cu(I)Cl/Al 2 0 3 was prepared by mixing 20.8 g of pulverised CuCl with 59.2 g of alumina. The mixture was heated under nitrogen gas flow at 570 °C for 23 hours. After heating, it was found that the CuCl salt was evenly spread at the surface of alumina.
• Co ⁇ per(I) adsorbent composition was prepared by mixing 20 g of dried 5A zeolite with 20 g of 1 M Cu(N0 3 ) 2 * 3 H 2 0 solution in a beaker. This mixture was dried in a heating chamber at 110 °C for 4 hours. Subsequently, the mixture was transferred into Nabertherm oven for calcination at 275 °C for 24 h. After cooling, the adsorbent composition was reduced with hydrogen in a pressure reactor at 7 bar for 8 hours. The Cu(I) content was measured to be 4.5 wt-%.
• Adso ⁇ tion isotherm of the adsorbent composition CuCl/Si0 2 prepared in example 1 was measured volumetrically at 25 °C by the pressure-volume method using a glass apparatus.
• the adso ⁇ tion isotherm is shown in Fig. 1.
• the adso ⁇ tion isotherm form of the CuCl/Si0 adsorbent composition is su ⁇ risingly advantageous.
• the isotherm is approximately linear, especially, at pressures of above 30 000 Pa, which enables the easy regeneration of ammonia from the adsorbent composition as well as the use of the adsorbent composition in the separation of high ammonia concentrations.
• the CuCl/Si0 adsorbent composition has a high ammonia capacity, which enables the smaller size columns in separation processes and, thus, decreases the investment cost of processes.
• Adso ⁇ tion isotherms were measured also for a commercial 5A zeolite adsorbent at 25 °C by the same method as previously. The results are presented only for a comparison to illustrate the favourableness of the adsorbent compositions according to the present invention.
• the adso ⁇ tion isotherm of commercial 5A zeolite adsorbent at 25 °C is shown in Fig. 2.
• the adso ⁇ tion isotherm forms of zeolites as well as of ⁇ -Al 2 0 3 are extremely favourable for adso ⁇ tion, namely irreversible, which means the regeneration of these adsorbents is difficult enforcing to employ low vacuum and/or high temperature.
• Table 1 shows three successive adso ⁇ tion-regeneration cycles for the 5A zeolite.
• the last adso ⁇ tion step 4 was performed only to find out the adsorbent bed capacity after regeneration step 3.
• the adso ⁇ tion-regeneration cycle 1 corresponded to a process, where 10.3% ammonia in air mixture was fed to the adsorbent bed until an ammonia breakthrough occurred. Immediately after the breakthrough the feed was stopped and the adsorbent bed was purged by a cocurrent 100% ammonia gas feed to remove a diluting air from the bed.
• the adsorbent bed was regenerated by heating at 125 °C and by evacuating at 11 mbar for 35 minutes with a countercurrent purge air flow of 10.8 mL min "1 .
• Table 1 shows that the breakthrough capacity in the adso ⁇ tion step 1 was 3.55 mmol NH 3 g "1 , the total capacity was 7.34 mmol NH 3 g "1 determined by 100% ammonia feed, and the recovered ammonia amount in the regeneration 1 was 84.5%.
• the adso ⁇ tion-regeneration cycle 1 the adsorbent bed was saturated directly by 100% ammonia gas feed without passing 10.3% ammonia into a column at the beginning as above. This was not required, since the total bed capacity is same in both cases.
• the regeneration was carried out at 12 mbar for 5 minutes, which released 43.2% of ammoma gas.
• the regeneration step 3 was made as the step 1 except the regeneration time was 5 minutes.
• the recovery of ammonia was 69.2%.
• Table 2 shows eight successive adso ⁇ tion-regeneration cycles carried out by the adsorbent composition, CuCl/Si0 which was prepared in the same manner as in example 1.
• the adso ⁇ tion step 1 a gas mixture containing 10.3% ammoma and 89.7% air by volume was passed through the column The feed was stopped after an ammonia breakthrough point was achieved. The breakthrough capacity of the adsorbent bed was 2,40 mmol NH g "1 . After the adso ⁇ tion step the regeneration was performed at 10 mbar for 5 minutes, which released 25.3% of ammonia.
• the adso ⁇ tion step of the adso ⁇ tion-regeneration cycle 2 10.3% ammonia mixture was fed in the same way as in the step 1 until the breakthrough occurred.
• the regeneration was carried out by heating at 126 °C and by evacuating at 10 mbar with 10.8 mL min "1 purge air flow. This released 87.5% of ammonia from the adsorbent bed.
• the adsorbent bed was saturated by 10.3% ammonia gas mixture to the breakthrough point followed by the saturation of 100% ammoma to the equilibrium.
• the total capacity of the CuCl/Si0 2 adsorbent composition was considerably higher than 5A zeolite with 100% ammonia feed, namely 11.4 mmol NH 3 g "1 .
• the adsorbent bed was evacuated at 10 mbar for 5 minutes, and, su ⁇ risingly the recovery of ammonia was 10.1% compared to the value of 43.2% of the 5A zeolite in the corresponding experiment.
• Combined regeneration by heating at 125 °C and by evacuating at 10 mbar with 10.8 mL min "1 purge air flow was studied in the regeneration steps 4 and 7.
• the ammonia recoveiy of the step 4 and 7 was 92.1% and 99.1%, respectively. These values are considerably higher than the 5 A zeolite in the corresponding experiment, namely 69.2%.
• the regeneration step 5 purified the adsorbent bed completely by heating at 125 °C and by high volume air flow.
• the total bed capacity in the adso ⁇ tion step 8 was 11.66 mmol NH 3 g "1 . This confirms that the adsorbent composition according the present invention is stable in several successive adso ⁇ tion-regeneration cycles.
• Fig. 3A shows the adso ⁇ tion equilibrium isotherms at 383 °K
• Fig 3B shows the adso ⁇ tion equilibrium isotherms at 423 °K for the Cu(I) and Cu(II) adsorbents compositions.
• the Cu(I) adsorbent composition adsorbs clearly more ammonia than the Cu(II) adsorbent composition. Since the adsorbed amount of carbon dioxide is nil on the Cu(I) adsorbent compositions and the ammonia capacity of Cu(I) adsorbent composition is higher than that of the Cu(II) adsorbent composition, the productivity of Cu(I) adsorbent composition will be higher in a large-scale ammonia separation process. The productivity can be defined as the amount of produced pure ammonia gas in an hour per the amount of adsorbent composition.
• Ammonia adso ⁇ tion equilibria at high pressure were determined volumetrically for the Cu(I)Cl/Al 2 0 3 adsorbent composition which was prepared in Example 2.
• the adso ⁇ tion equilibrium isotherm is shown in Fig 4 which shows that the used adso ⁇ tion composition is feasible at high pressure conditions, as well.
• the adso ⁇ tion equilibrium isotherm of ammonia on the Cu(I) adsorbent composition prepared in Example 3 was determined volumetrically at 25 °C.
• the adso ⁇ tion equilibrium isotherm is shown in Fig. 5.
• the ammonia gas diffusivities were determined by batch uptake experiments for the Cu(I)Cl/Al 0 3 and Cu(II)Cl 2 /Si0 2 adsorbent compositions which were prepared in Example 2 and Reference Example 1, respectively.
• the diffusivity for the Cu(I)Cl/Al 2 0 3 was found to be 6.04- 10 "9 mV 1 and for Cu(II)Cl 2 /Si0 2 it was
• feed gas i.e. a gas mixture from the melamine process containing 50% ammonia and 50% carbon dioxide by volume at 200 °C; (2) adso ⁇ tion with feed gas at 100 bar;
• step 1 the average values for ammonia recovery and purity were 90-95% and 99.5-99.9%, respectively.

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