Methods for recovering iodine (I2)

Abstract

A flow containing iodine (I2) vapor and at least one of an inert gas and water vapor. One method for recovering iodine (I2) is to bring the flow into contact with an alkaline solution to form an iodide salt. To achieve, to bring the flow into contact with the adsorbent and selectively adsorb water from the flow, to concentrate the flow By contacting it with an acid, water vapor is absorbed from the flow, or iodine (I2) vapor is back sublimated or Condensing to form solid or liquid iodine (I2), or bringing the flow into contact with the material Furthermore, among the absorption of latent heat and sensible heat by a material through its phase change, When performing at least one of the following, iodine (I2) vapor is condensed or backsublimated from the flow. It can include the following:

Description

Technical Field

[0001] (Cross - reference to related applications) This application claims the benefit of U.S. Provisional Patent Application No. 63 / 137,472, filed on January 14, 2021 and claims priority to U.S. Patent Application No. 17 / 5 72,542, filed on January 10, 2022, both of which are hereby incorporated by reference in their entirety into this specification.

[0002] This disclosure relates to a process for recovering iodine (I₂) from processes that use iodine (I₂), particularly from processes used to dry iodine (I₂).<​​​​​​​​​​​​​​​​​​​​​​​​​​​​​​​​​​ This can lead to the formation of this mixture, which is also corrosive and presents a risk to product separation. It can have harmful effects and lead to reduced yields.

[0007] The method used to remove water from iodine (I2) involves the loss of iodine (I2). It can result in this. Therefore, what is needed is iodine (I2) which would normally be lost. This is a method for recovering ) [Overview of the Initiative]

[0008] This application relates to a method for recovering iodine(I2) from processes that use iodine(I2). To provide the law.

[0009] In one embodiment, the method for recovering iodine(I2) involves iodine(I2) vapor and an inert To provide a flow containing at least one of gas and water vapor, and to provide an alkaline solution for the flow. This includes contacting the substance with a liquid to form an iodide salt.

[0010] In another embodiment, the method for recovering iodine(I2) is to use iodine(I2) vapor and water vapor To provide a flow containing and to bring the flow into contact with an adsorbent to selectively adsorb water from the flow. This includes the act of doing something.

[0011] In another embodiment, a method for recovering iodine (I2) involves using an inert gas, water vapor, and iodine To provide a flow containing elementary (I2) vapor, and to bring the flow into contact with concentrated acid to remove water vapor from the flow. This includes absorbing and

[0012] In another embodiment, the method for recovering iodine(I2) is to use iodine(I2) vapor and water vapor To provide a flow containing and to backsublimate or condense iodine (I2) vapor into a solid or liquid including forming elemental iodine (I₂).

[0013] In another embodiment, a method of recovering iodine (I₂) includes providing a stream comprising iodine (I₂) vapor and at least one of an inert gas and water vapor, and contacting the stream with a material such that iodine (I₂) vapor is condensed or reverse sublimated from the stream as the material absorbs latent heat and / or sensible heat through a phase change of the material. including:

[0014] Other embodiments can combine any of the previous embodiments. DETAILED DESCRIPTION OF THE INVENTION

[0015] The present disclosure provides a method for recovering iodine (I₂) from a gas stream such as those used to dry iodine. Methods for drying iodine (I₂) or removing water from iodine (I₂) are disclosed in co-pending U.S. Patent Applications Nos. 63 / 137,463 and 17 / 572,547, both entitled "METHODS FOR REMOVING WATER FROM IODINE (I₂)", the contents of which are hereby incorporated by reference in their entireties. For example, methods for removing water from iodine (I₂) include passing iodine (I₂) through heated nitrogen (N₂), air, carbon dioxide (CO₂), argon, helium, or, for example, pentafluoropropane (HFC-245fa), 2,2-dichloro-1,1,1-trifluoroethane (HCFC-123), 1-chloro- 1,2,2,2-tetrafluoroethane (HCFC-124), pentafluoroethane (HFC-125), 1,1,1,2-tetrafluoroethane (HFC -245fa), 2,2-dichloro-1,1,1-trifluoroethane (HCFC-123), 1-chloro-1,2,2,2-tetrafluoroethane (HCFC-124), pentafluoroethane (HFC-125), 1,1,1,2-tetrafluoroethane (HFC -134a), etc.​ -134a), difluoromethane (HFC-32), hydrogen iodide (HI), and trifluoro Any other gas stream inert to iodine (I2), such as iodomethane (CF3I), and can be included in contact with it.

[0016] Iodine (I2) can be contacted with an inert gas through a multi-stage stripping column. Iodine (I2) is supplied to the top of the multi-stage stripping column, and the inert gas is supplied to the bottom of the column. Countercurrent contact between wet iodine (I2) and dry inert gas gradually increases, thereby removing more water and resulting in iodine (I2) appearing at the bottom of the column [[ID=) with a very low residual water content. A reboiler can be incorporated into the column design to assist in driving out water from iodine (I2). Since the inert gas is initially essentially water-free, it carries away water with it and leaves iodine (I2) with a very low water content. The resulting inert gas stream appears from the top of the column and is carried away with the removed water and some iodine (I2).

[0017] In some embodiments, a series of liquid-vapor contact devices, such as flash drums or bubblers, in which the liquid and vapor in each device contact each other in a countercurrent manner similar to a multi-stage column, can achieve the same effect as the above multi-stage column. The use of successive discrete contact devices can allow for better management of iodine (I2) so that anti-sublimation or solidification can be prevented when the amount of inert gas contacting iodine (I2) is insufficient at temperatures below 116°C.

[0018] In some other embodiments, for example, a single-stage liquid-vapor contact device such as a flash drum A device can be used. In some other embodiments, for example, a flow-through thin-film apparatus. A parallel flow liquid-vapor contact apparatus can be used. In some embodiments, iodine (I 2) The iodine (I2) can come into contact with an inert gas during pneumatic transport, and the iodine The gas used for transport is an inert gas.

[0019] Other suitable gases for use in this method also effectively remove water from iodine(I2). It has a low water content to remove water. It exhibits affinity for water or forms an azeotropic mixture with water. The chemical components that can be produced are also suitable for use in this method.

[0020] This disclosure describes a method for drying iodine (I2) from an inert gas stream. A method of collection is provided. Such a flow involves removing iodine from an inert gas in a drying process. It contains the removed water and some iodine carried along with the inert gas flow. Even if this iodine is not recovered, it could represent a significant loss of iodine from the process. In the drying process, recovering iodine (I2) that would normally be lost is... It brings about an economic process.

[0021] In some embodiments, the inert gas is nitrogen (N2), carbon dioxide, helium, aluminum Gon, air, hydrogen, hydrogen iodide, or any other gas that is inert to iodine (I2) It may include. In some embodiments, the inert gas may include a combination of gases. It is possible.

[0022] The iodine (I2) concentration in an inert gas stream, expressed on an anhydrous basis, is approximately 0.5 mol%, approximately 1 mol%. % ppm, approximately 2 mol%, approximately 3 mol%, approximately 5 mol%, approximately 10 mol%, approximately 15 mol%, approximately 2 0 mol% or as low as about 30 mol%, or about 40 mol%, about 50 mol%, about 60 mol% Heights of approximately 70 mol%, 80 mol%, 90 mol%, or 99 mol%, and For example, approximately 0.5 mol% to approximately 99 mol%, approximately 1 mol% to approximately 90 mol%, and approximately 2 mol% pp. m ~ approximately 80 mol%, approximately 3 mol% ~ approximately 70 mol%, approximately 5 mol% ~ approximately 60 mol%, approximately 10 mol %~approximately 50 mol%, approximately 15 mol%~approximately 40 mol%, approximately 20 mol%~approximately 30 mol%, approximately 10 mol% to approximately 20 mol%, approximately 5 mol% to approximately 15 mol%, or approximately 30 mol% to approximately 60 mol% It may be any range defined between any two of the aforementioned values, such as, preferably, The iodine (I2) concentration in an inert gas stream, expressed on an anhydrous basis, is approximately 3 mol% to approximately 60 mol%. More preferably, the iodine (I2) concentration in the inert gas stream, expressed on an anhydrous basis, The concentration is approximately 5 mol% to 40 mol%. Most preferably, in an inert gas stream expressed on an anhydrous basis. The iodine (I2) concentration is approximately 10 mol% to 20 mol%.

[0023] Recovery of iodine (I2) via treatment with alkaline solution In this method, the inert gas stream is scrubbed with an alkaline solution, and the yogurt from the inert gas stream is removed. By removing iodine(I2), an inert gas containing water vapor and iodine(I2) vapor is produced. The flow is processed. After scrubbing, nitrogen is used to cool and condense the residual water (as dehumidification). (Generally known), and / or by conventional methods such as passing it through a desiccant, The inert gas stream can be dried to remove water. Then, the dry nitrogen will absorb more iodine (I 2) It can be recycled for reuse when drying. The alkaline solution is useful. It can be recovered as a iodide salt product. Iodine in the recovered alkaline solution or dried iodide salt The compound is reacted with sulfuric acid or hydrochloric acid by methods known in the art. This process involves then reacting it with hydrogen peroxide to convert it back into iodine (I2). It is possible.

[0024] Iodide counterions in alkaline solutions include, in particular, sodium, potassium, lithium, It may be magnesium or calcium. In some embodiments, the alkaline solution is For example, sodium hydroxide, potassium hydroxide, lithium hydroxide, magnesium hydroxide, etc. or an aqueous solution formed from calcium hydroxide or a combination thereof. It is possible.

[0025] In some embodiments, hypoiodite ions (e.g., NaOI) are used to form iodides (e.g. For example, to convert sodium sulfite to NaI and sulfate (e.g., Na2SO4), Reducing agents such as Na2SO3 can be used selectively. Among other reducing agents, sub Sodium bisulfate (NaHSO3), potassium sulfite (K2SO3), potassium bisulfite Um (KHSO3), calcium sulfite (Ca(SO3), calcium bisulfite (Ca (HSO3)2, Lithium sulfite (Li2SO3), Lithium bisulfite (LiHSO3) ), magnesium sulfite (Mg(SO3), magnesium bisulfite (Mg(HSO3) Other reducing agents such as (2) may be used.

[0026] Recovery of iodine (I2) via water adsorption using solid adsorbents. In this method, a stream of inert gas containing water vapor and iodine (I2) vapor passes through an adsorbent. This removes virtually all water vapor from the flow. The adsorbent selectively removes water vapor from the flow. Removes it. In some embodiments, the dry inert gas still contains iodine vapor. The sluice stream is recycled for reuse when drying more iodine (I2). In some embodiments, the dry inert gas stream is saturated with iodine (I2). In another embodiment, a dry inert gas stream containing iodine vapor is used to dissolve solid iodine (I2). It is back-sublimated for recovery. The recovered solid iodine (I2) is already dried from the adsorbent. Since it is used, it can be recycled for use in HI production.

[0027] The adsorbent is a molecular sieve (e.g., 3A, 4A, 5A, or XH-9), Lumina, calcium sulfate ("Dryelite"), silica gel, calcium chloride, sodium sulfate You can choose thorium, or any combination thereof.

[0028] When the adsorbent no longer adsorbs water at a sufficient rate, it is desirable to regenerate the adsorbent. When it is convenient to do so, the adsorbent is first heated to absorb The additional iodine adhering to the adhesive is vaporized and recovered by the method disclosed herein (for example, reverse By enabling iodine collection through one or more of the following processes (sublimation, condensation, etc.), it can be regenerated. It is possible. In some embodiments, heating is performed under vacuum to accelerate iodine recovery. It can break. The adsorbent is at a low temperature of about 90°C, about 95°C, about 100°C, or about 105°C. Temperature, or a temperature of about 110°C, about 115°C, or about 120°C, or for example, Approximately 90°C to 120°C, approximately 95°C to 115°C, approximately 100°C to 110°C, approximately 105°C to The aforementioned values ​​include approximately 120°C, approximately 100°C to approximately 120°C, or approximately 90°C to approximately 100°C. It can be heated to any temperature within any range defined between any two of the following values.

[0029] Following the removal of residual iodine, the adsorbent is brought into contact with a high-temperature inert gas such as nitrogen or air. The adsorbent can be regenerated by desorbing water from it. Temperatures as low as 0°C, approximately 175°C, approximately 200°C, approximately 225°C, or approximately 250°C, Temperatures of approximately 275°C, 300°C, 325°C, or 350°C, or for example Approximately 150°C to 350°C, approximately 175°C to 325°C, approximately 200°C to 300°C, approximately 22 The aforementioned ranges include 5°C to approximately 300°C, approximately 150°C to approximately 250°C, or approximately 200°C to approximately 300°C. To heat the adsorbent to a temperature within any range defined between any two of the values ​​of . Therefore, it may be regenerated.

[0030] Recovery of iodine (I2) via water absorption by concentrated acid In this method, a flow of inert gas containing water vapor and iodine (I2) vapor is circulated through concentrated acid. The water vapor is passed through a contactor. The water vapor is absorbed by the concentrated acid, and virtually all of the water vapor is removed from the flow. The iodine vapor is removed. In some embodiments, the dry inert still contains iodine vapor. The gas stream is recycled for reuse when drying more iodine (I2). In some other embodiments, a dry inert gas stream having iodine vapor is used with solid iodine (I2) is back-sublimated to recover it. The recovered solid iodine (I2) is then treated with concentrated acid. Since it has already been dried, it can be recycled for use in HI production.

[0031] Suitable concentrated acids include sulfuric acid (H2SO4), hydroiodic acid (HI), and phosphoric acid (H3PO4). , and metaphosphoric acid (HPO3) are included. For example, if the concentrated acid is sulfuric acid, the concentration of sulfuric acid This can be in the range of 95% to 100%. In some embodiments, sulfuric acid is It is either reum or fuming sulfuric acid.

[0032] The contactor receives an inert gas flow containing water vapor and iodine (I2) vapor from the bottom of the tower. Liquid concentrated acid is supplied to the top of the tower, and water vapor is expelled from the bottom of the tower. Alternatively, it may be a tray tower. Alternatively, the contactor may be a parallel-flow packed tower or a tray tower, here So, both the inert gas stream containing water vapor and iodine (I2) vapor, and the concentrated acid, move the tower in the same direction. It flows in the direction of flow. Alternatively, the contactor has an inert gas flow containing water vapor and iodine (I2) vapor. A mixing tank in which liquid concentrated acid is tightly mixed. Alternatively, a contactor can be used for liquid concentrated acid. The water vapor and yogurt that are drawn into the educator circulate through it. It can be an educator that tightly mixes with an inert gas flow containing elemental (I2) vapor. Contactor It may include multiple contactor units.

[0033] Recovery of iodine (I2) by reverse sublimation In this method, an inert gas stream containing water vapor and iodine (I2) vapor is brought into contact with a cold surface. The iodine is then back-sublimated and recovered as solid iodine (I2). The back-sublimation temperature is The water from iodine (I2) can be frozen at a sufficiently low temperature to maximize the recovery yield. After remelting, the recovered mixture of iodine (I2) and water was divided into two layers: one rich in water and the other rich in water. The layers form a two-phase liquid rich in iodine (I2). The iodine (I2) / water mixture is approximately 114 When remelted at or near 160°C and atmospheric pressure, most of the water evaporates, and iodine... Heated molten iodine (I2) can be easily recycled to the (I2) drying step. ) leaves behind. Alternatively, the lighter water-rich layer can be decanted for disposal, while the lighter water-rich layer is more The heavy iodine(I2)-rich layer can be recycled by returning it to the iodine(I2) drying step. ru.

[0034] The reverse sublimation temperatures are approximately -45°C, -30°C, -10°C, 0°C, 10°C, and 20°C. Which low, or approximately 35°C, 40°C, 50°C, 60°C, 66°C, 80°C, 90°C A temperature of ℃ or approximately 100℃, or for example, approximately -45℃ to approximately 100℃, approximately -30℃ to Approximately 90°C, approximately -20°C to approximately 80°C, approximately -10°C to approximately 66°C, approximately 0°C to approximately 60°C, approximately 10°C ~50℃, 20℃~40℃, 35℃~66℃, 20℃~80℃ or approximately Any range defined between any two of the aforementioned values, such as 10°C to approximately 60°C. This can be a temperature. Preferably, the back sublimation temperature is about 35°C to about 66°C.

[0035] Alternatively, in some embodiments, an inert gas containing water vapor and iodine (I2) vapor is used. The flow selectively condenses iodine (I2) without essentially involving the condensation or solidification of water in the flow. It is subjected to back sublimation at a temperature sufficient to solidify. Then, most of the iodine (I2) becomes solid. It can be collected as such, and the remaining small amount is carried away into a nitrogen / inert gas and water vapor stream. Then, the solid iodine (I2) is remelted and returned to the iodine (I2) drying step for recycling. It is possible.

[0036] In such an embodiment, the back sublimation temperature is approximately 0°C, approximately 10°C, approximately 20°C, approximately 30°C, approximately A low temperature of 35°C, approximately 40°C, approximately 45°C, or approximately 50°C, or approximately 55°C, approximately 60°C, approximately A temperature of around 65°C, approximately 70°C, approximately 80°C, approximately 90°C, or approximately 100°C, or for example, approximately 0℃ to approximately 100℃, approximately 10℃ to approximately 90℃, approximately 20℃ to approximately 80℃, approximately 30℃ to approximately 70℃, approximately 35℃ to approximately 65℃, approximately 40℃ to approximately 60℃, approximately 45℃ to approximately 55℃, approximately 35℃ to approximately 55℃, approximately Between any two of the aforementioned values, such as 20°C to approximately 35°C or approximately 55°C to approximately 90°C. The temperature can be any within the range defined by . Preferably, the back sublimation temperature is about 35°C to about It is 55℃.

[0037] A flow of inert gas effluent containing iodine (I2) undergoes back sublimation, for example, at 65°C and atmospheric pressure. When passing through the apparatus, iodine (I2) can be recovered as a solid free of excess water, and then It can then be remelted and recycled and dried. The yield of iodine (I2) is approximately 89%. This is based on 1000 pounds of iodine. Using I2), the overall iodine (I2) loss during drying is approximately 0.3%, i.e. Low iodine (I2) loss of 3.3 pounds per 1000 pounds of iodine (I2) dried. This will reduce the amount. This loss arises from exhausting the inert gas after back sublimation, and this It contains some residual iodine (I2).

[0038] The reverse sublimation apparatus consists of 10 jacketed glass panels, each 10 feet long and 4-6 inches in diameter. Lined pipe, or other suitable material such as Hastelloy® C It can be constructed from a set of pipes lined (or formed) with material. The system can be operated in batch mode for several cycles per day. The coolant temperature can be between the back sublimation temperature and approximately 175°C, and iodine is recovered by back sublimation. Cooling is performed alternately, followed by heating to remove iodine recovered from the reverse sublimation apparatus.

[0039] Recovery of iodine (I2) by back sublimation in water In this method, the flow of an inert gas containing water vapor and iodine (I2) vapor is reversed. It is brought into contact with water at a temperature low enough to cause sublimation, and then recovered as solid iodine (I2). The recovered mixture of iodine (I2) and water has one layer rich in water and the other layer rich in iodine. A two-phase liquid rich in element (I2) is formed. The two-phase mixture is then separated by liquid-liquid extraction. It is possible. The top layer or water-rich phase is decanted and recycled, and water vapor and iodine (I2) Can be used to bring into contact with more of the flow of inert gas containing vapor. The bottom layer or iodine-rich phase, which still contains undecanted water, It can be heated to melt the element. After melting, the molten iodine content is less than 0.15% by weight. It is presumed to contain water. Then, this molten iodine is subjected to the iodine(I2) drying step. It can be returned and recycled. Alternatively, or additionally, molten iodine can be used as an adsorbent or The water is brought into contact with the absorbent, and most of the remaining water is extracted from the fused iodine into the adsorbent or absorbent. This is possible. The adsorbent or absorbent is, for example, concentrated sulfuric acid or molecular sieve, as described above. This may be anything specified in the details.

[0040] In such an embodiment, water is at approximately 0°C, approximately 5°C, approximately 10°C, approximately 15°C, approximately 20°C, approximately A temperature as low as 25°C, approximately 30°C, approximately 35°C, approximately 40°C, or approximately 45°C, or approximately 50°C °C, approximately 55°C, approximately 60°C, approximately 65°C, approximately 70°C, approximately 75°C, approximately 80°C, approximately 85°C, approximately 90°C A temperature of ℃ or approximately 95℃, or for example, approximately 0℃ to approximately 95℃, approximately 5℃ to approximately 90℃ °C, approximately 10°C to 85°C, approximately 15°C to 80°C, approximately 20°C to 75°C, approximately 25°C to 70°C °C, approximately 30°C to 65°C, approximately 35°C to 60°C, approximately 40°C to 55°C, approximately 45°C to 50°C Between any two of the aforementioned values, such as 5°C to 45°C or 20°C to 30°C. The temperature may be within any defined range. Preferably, the back sublimation temperature is about 5°C to about 45°C. It is °C.

[0041] In some embodiments, the contact is, for example, with glass, or polyethylene, polypropylene. Polymers such as tetrafluoroethylene or polyvinylidene fluoride This may be in a water pool container lined with a luoropolymer. In some embodiments, The container is formed from a suitable metal alloy or polymer.

[0042] Recovery of iodine (I2) by condensation in water In this method, a flow of inert gas containing water vapor and iodine (I2) vapor is used to condense the iodine. When water is brought into contact with iodine (I2) at a temperature low enough to cause shrunk, but high enough to maintain the iodine in a liquid state. Allow to come into contact. The recovered mixture of iodine (I2) and water has one layer rich in water and the other layer This forms a two-phase liquid rich in iodine (I2). The two-phase mixture is then extracted by liquid-liquid extraction. It can be separated. The uppermost layer or water-rich phase is decanted and recycled, and the water vapor and It can be used to bring more of the inert gas flow containing iodine (I2) vapor into contact with it. Next, the bottom layer or iodine-rich phase is returned to the iodine(I2) drying step for recycling. It can be done.

[0043] In such embodiments, water is at approximately 95°C, approximately 100°C, approximately 105°C, approximately 110°C, approximately A low temperature of 115°C or around 120°C, or around 125°C, 130°C, or 135°C. A temperature of around 150°C, approximately 140°C, 145°C, or 150°C, or approximately 95°C to approximately 1 50℃, approximately 100℃ to approximately 145℃, approximately 105℃ to approximately 140℃, approximately 110℃ to approximately 135℃, Approximately 115°C to 130°C, approximately 120°C to 125°C, approximately 110°C to 120°C, approximately 95°C The aforementioned values ​​such as ~115°C, ~130°C to ~150°C, or ~105°C to ~125°C. The temperature can be any range defined between any two of the following. Preferably, the inverse The sublimation temperature is approximately 110°C to 120°C. Water sublimes at temperatures above approximately 100°C under superatmospheric pressure. That is the case.

[0044] In some embodiments, the contact is, for example, with glass, or polyethylene, polypropylene. Polymers such as tetrafluoroethylene or polyvinylidene fluoride This may be in a water pool container lined with a luoropolymer. In some embodiments, The container is formed from a suitable metal alloy or polymer.

[0045] Recovery of I2 by back sublimation or condensation using latent or sensible heat transfer. In this method, a flow of an inert gas containing water vapor and iodine (I2) vapor is passed through the material. When brought into contact, the materials absorb latent heat and / or sensible heat through the phase change of the material, Therefore, when cooling iodine (I2), the iodine (I2) is condensed and / or back-boiled from the flow. To enhance. Suitable materials may include, for example, carbon dioxide (CO2). 2) Initially, it may be in a solid phase at atmospheric pressure (as dry ice), or in a liquid phase at high pressure. It is possible. The contact temperature is preferably sufficient to achieve the water vapor iodine (I2) recovery rate. Selected to produce a flow of water vapor and an inert gas containing iodine (I2) that reaches a low cooling temperature. It will be selected.

[0046] The cooling temperature is approximately -40°C, -30°C, -20°C, -10°C, 0°C, or 1°C. As low as 0°C, or around 20°C, 30°C, 40°C, 50°C, 60°C, or 7°C A temperature of around 0°C, or approximately -40°C to 70°C, approximately -30°C to 60°C, approximately -20°C to 5°C 0℃, approximately -10℃ to approximately 40℃, approximately 0℃ to approximately 30℃, approximately 10℃ to approximately 20℃, approximately 20℃ to approximately 5 Before 0°C, approximately -30°C to approximately 10°C, approximately 30°C to approximately 60°C, or approximately 30°C to approximately 40°C, etc. The temperature may be within any range defined between any two of the values ​​described above. Preferably The cooling temperature is approximately 20°C to 50°C.

[0047] Other suitable materials include, for example, nitrogen, 1,1,1,3,3-pentafluoropropane ( Supercooled liquids such as HFC-245fa, HCFC-244bb, and pentafluoro Ethane (HFC-125), HFC-134a, HFC-32, and trifluoroiodine Other inert halocarbons such as methane (CF3I) are included. Other suitable materials include, for example, For example, nitrogen, carbon dioxide, 1,1,1,3,3-pentafluoropropane (HFC-24) Supercooled gases such as 5fa, and pentafluoroethane (HFC-125), HFC-1 Other inert halocarbons such as 34a, HFC-32, CF3I, and HCFC-244bb. This includes alkanes such as methane, ethane, and propane. In some embodiments, freezing Water can be used.

[0048] Back sublimated or condensed iodine(I2) containing a small amount of substance that has been brought into contact for cooling. It can be removed as is, or melted to facilitate transfer as a molten liquid. In either case, the iodine(I2) is returned to the desired iodine(I2) drying step and recycled. It could happen.

[0049] All methods described herein are used in batch, semi-batch, or continuous processes. Obtain. All methods described herein may be carried out under reduced pressure, atmospheric pressure, or overpressure.

[0050] Although the present invention has been described as relating to an exemplary design, the present invention is intended to convey the spirit of this disclosure. And can be further modified within the scope. Furthermore, this application relates to the relevant technical fields in which the present invention relates. It is not intended to include such deviations from this disclosure that belong to known or customary practices. It is illustrated.

[0051] As used herein, "any range defined between any two of the aforementioned values" The phrase "within the enumeration" means that the values ​​are in the lower part of the enumeration or the higher part of the enumeration Whether or not, any range is any two of the values ​​listed before such a clause. This means that there can be two options to choose from. For example, a pair of values ​​could be two lower values, or two lower values. A higher value, or a lower and higher value, can be selected.

[0052] When used herein, the modifier "about" in relation to quantity refers to the described quantity. It contains a value and has a meaning determined by the context (for example, it relates to the measurement of a particular quantity). (Including at least the degree of the associated error). When used in a broader context, it means "approximately". The modifier can also be thought of as disclosing a range defined by the absolute values ​​of the two endpoints.

[0053] The following non-limiting embodiments may be helpful in illustrating the present disclosure. [Examples]

[0054] Example 1: Predictive example of iodine (I2) recovery by treatment with alkaline solution Samples of inert gases containing water vapor and iodine(I2) vapor are dried. For every 1000 pounds, you get 19 pounds of nitrogen, 30 pounds of iodine (I2), and 2.5 pounds It contains water. This nitrogen effluent is sent to a packed scrubber to remove iodine (I2), 7.6 wt% sodium hydroxide (NaOH) and 11.9 wt% sodium sulfite (Na2 It is converted into a salt solution by reacting it with a circulating alkaline aqueous solution containing SO3. As shown in equation 2 below, ion(I2) reacts with an alkaline solution to form sodium iodide. It produces um and sodium sulfate. Equation 2: I2+2NaOH+Na2SO3--→2NaI+Na2SO4+H2O

[0055] Once the starting alkaline aqueous solution is consumed, the reaction is calculated taking into account the material balance of the reaction. For every 1000 pounds of iodine(I2) dried, the final product having the composition shown in Table 1 below is obtained. A solution of the product is obtained. [Table 1]

[0056] Example 2: Predictive example of iodine (I2) recovery attached to molecular sieves Samples of inert gases containing water vapor and iodine(I2) vapor are dried. 19 pounds of nitrogen, 30 pounds of iodine (I2), and 2.5 pounds per 1000 pounds This contains water. This nitrogen effluent is placed in an 8:1 L / D container filled with 4 Å molecular sieves. It supplies. When operated at 116°C, the water content of the nitrogen effluent is 117,000g of the initial amount. It is estimated that this can be reduced from ppm to less than 1000 ppm by weight. This dry nitrogen is leaking This will result in 99% of the water content being removed by the cyane, and iodine (I 2) It still contains but can be easily reused or recycled into dried iodine (I2). obtain.

[0057] At 116°C and atmospheric pressure, a 4 Å molecular sieve exhibits the static properties shown in Table 2 below. It is estimated to have water capacity, and this is because the residual water content of the regenerated molecular sieve is zero. It is assumed. [Table 2]

[0058] Using the above static adsorption capacity, 1000 ppm by weight was obtained in nitrogen at atmospheric pressure and 116°C. To reach the water content, an integral static charge of 12 pounds of water per 100 pounds of molecular sieve is required. The static capacity is estimated. For continuous dynamic operation, a conservative 50% of the static capacity is used for the material. Residual water content after movement and regeneration, and adsorption due to aging of molecular sieves or co-adsorption of impurities. This is assumed to explain the loss of adhesion efficiency. This allows us to estimate the size of the adsorption bed and the cycle time. To determine the amount needed, it is calculated to be 6 pounds of water per 100 pounds of molecular sieve.

[0059] Example 3: Iodine (I2) recovery using a reverse sublimation apparatus A bench scale featuring a jacketed pipe measuring 4 inches in diameter and 10 inches in length. The reverse sublimation apparatus was constructed with and without a spiral baffle insert. The reverse sublimation apparatus is designed so that iodine (I2) solidifies inside the pipe. Alternatively, reverse The sublimation apparatus can be designed so that iodine (I2) solidifies on the outer surface of the pipe. Commercial-scale designs are typically realized at the commercial level through the use of contact fins or reinforced surface devices. Partly due to the higher heat transfer coefficient, it is expected that performance will increase several times over. It can be done.

[0060] The inlet temperature of the device equipped with baffles was 87.3°C. The main body of the reverse sublimation device was at the inlet. From 40.4°C at the closest end, to 41.1°C at the center of the pipe, and 37.6°C at the outlet end. The range was as follows. The outlet temperature was 38.3°C. In the device without baffles, the inlet temperature The temperature was 94.5°C. The temperature inside the pipe ranged from 40.3°C at the end closest to the inlet to 94.5°C. The temperature ranged from 40.2°C at the center of the pipe to 36.4°C at the pipe closest to the outlet. The mouth temperature was 40.1°C. The average temperature of the reverse sublimation device was approximately 40°C.

[0061] Table 3 below shows bench scale devices with baffles and bench scale devices without baffles. Flow rate and yo for the kale device (with and without baffles, respectively) The data on the amount of porcini(I2) collected is shown below. [Table 3]

[0062] Example 4: Predictive example of iodine (I2) recovery by reverse sublimation Samples of inert gases containing water vapor and iodine(I2) vapor are dried. 19 pounds of nitrogen, 30 pounds of iodine (I2), and 2.5 pounds per 1000 pounds It contains water. This nitrogenous effluent is supplied to a back sublimation device or cold trap and flows into Iodine is added at a temperature selected so that most of the water in the nitrogen effluent feed remains uncondensed. (I2) is coagulated.

[0063] Table 4 below shows the expected iodine (I2) recovery efficiency and the expected iodine (I2) recovery efficiency for the reverse sublimation temperature at atmospheric pressure. Summarize the amount of co-condensed water. The preferred back sublimation temperature for the flow is 35°C to 66°C. At this temperature, a very small amount of incoming water co-condenses with solidified iodine (I2), A high iodine (I2) recovery rate (over 88 percent) is achieved. This allows for further processing. To recycle it by returning it to the desired iodine (I2) drying process without requiring any additional steps. The recovered iodine (I2) is provided. [Table 4]

[0064] Example 5: Predictive example of iodine (I2) recovery by condensation using hot water. Samples of inert gases containing water vapor and iodine(I2) vapor are dried. 19 pounds of nitrogen, 30 pounds of iodine (I2), and 2.5 pounds per 1000 pounds Contains water. Nitrogen effluent is found in hot water pools or containers operating at 116°C and 25 psig. This water temperature is supplied to a jacketed container, a steam coil, or directly to water. This can be maintained by applying water vapor to the gas injection.

[0065] A pool or container of heated water is designed to provide steam-liquid contact. Among the methods, in particular, gentle stirring, gas spraying to promote self-stirring, baffles, In-line mixing with or without a static mixer, or using a circulating emitter It can be carried out.

[0066] Under these operating conditions, nitrogen effluent compensates for water vapor loss when it leaves the heated pool. Therefore, and to provide excess liquid water to come into direct contact with the incoming nitrogen effluent. In addition, 50 pounds of water (fresh replenishment fluids and recycled light water as described below) A phase water is required. An excess of liquid water is used to maintain a temperature of 116°C, and nitrogen effluent is removed. In contrast to the back sublimation or solidification of iodine(I2), this method allows for the condensation of iodine(I2). ru.

[0067] After the nitrogen effluent comes into contact with the hot water, the nitrogen discharged from the hot water pool is essentially all Inflowing nitrogen (19 pounds), 17 pounds of evaporated water vapor, and 1 pound of residual iodine (I 2) It contains and therefore achieves a 97 percent iodine (I2) recovery efficiency.

[0068] After considering the inflowing water along with water evaporation losses and nitrogen leachates, the heated swimming pool is 29 pt The mixture contains iodine (I2) and 35 pounds of water. This mixture is allowed to precipitate for 30 minutes. After decomposition, phase separation is performed to remove the iodine (I2)-rich phase. It is estimated to contain water at a concentration of approximately 2 mole percent or 0.15% by weight. However, However, when the pressure is reduced, most of the residual water is lost with little further loss of iodine (I2). It evaporates from molten liquid iodine (I2) at 16°C. The iodine (I2) recovered in this way ) can be recycled and returned to the desired drying step.

[0069] The lighter, water-rich phase contains 0.05 mole percent or 0.7 wt% dissolved iodine. It is presumed to contain (I2), and this water-rich phase is used in the iodine (I2) recovery process. This method can be reused in batch processes, semi-batch processes, or sequential processes. It can be used as a substitute for "S".

[0070] Example 6: Predictive example of iodine (I2) recovery by back sublimation using cold water Samples of inert gases containing water vapor and iodine(I2) vapor are dried. 19 pounds of nitrogen, 30 pounds of iodine (I2), and 2.5 pounds per 1000 pounds It contains water. The nitrogen effluent is supplied to a pool or container of water operating at 38°C and near atmospheric pressure. This water temperature is controlled by jacketed cooling, cooling coils, ice or dry ice, etc. Maintained by directly adding other cryogenic fluids, or simply by starting with cold water and heating it up to 38°C. It is possible.

[0071] A pool or container of cold water is initially designed to provide a vapor-liquid contact. It is then filled with 300 pounds of water. This is to promote gentle stirring, self-stirring Spraying, baffling, inline mixing with or without static mixer, circulating eddy This can be carried out using a trowel or other suitable method. This large amount of water is used in the handling of the mixture. To facilitate this process, the formation of a mixture containing approximately 10% by weight of solid iodine (I2) is made permanent. It will be selected to be selected.

[0072] After the nitrogen effluent comes into contact with cold water, the nitrogen discharged from the cold water pool is replaced by the incoming nitrogen. Almost all (19 pounds), 0.14 pounds of water vapor, and 0.04 pounds of residual iodine ( It contains I2 and exhibits a 99.8% efficiency in iodine (I2) recovery.

[0073] The cold water pool contains approximately 29 pounds of iodine (I2). This mixture contains lighter water liters. Before phase separation to decant the water-rich phase, it was allowed to settle for 10 minutes. The water-rich phase was then separated at 38°C. It is estimated to contain 0.05% by weight of dissolved iodine (I2) and will be reused in the recovery process. obtain.

[0074] The heavy, wet iodine-rich precipitate can be used as a slurry, or alternatively, as a filtered solid. It can be processed as follows: The wet iodine recovered in the form of slurry or filtered cake is processed at 116°C. By heating it, not only is the solid iodine (I2) melted, but most of the water is also evaporated. This can be done. Remove this molten iodine (I2) and return to the desired drying step for recycling. It is possible. The molten iodine (I2) is estimated to contain less than 0.15% by weight of water. It can be done.

[0075] This cold water method for iodine (I2) recovery can be used in batch, half-batch, or continuous batch processes. It can be executed in a process.

[0076] Example 7: Predictive example of iodine (I2) recovery by back sublimation using solid CO2. From the iodine (I2) drying method described above, the nitrogen effluent used in the drying process is the iodine that is dried. For every 1000 pounds of iodine(I2), you get 19 pounds of nitrogen, 30 pounds of iodine(I2), and It contains 2.5 pounds of water. This nitrogenous effluent is almost at atmospheric pressure and contains dry ice (solid C). It is supplied to a container of O2. Direct contact between dry nitrogen effluent and solid CO2 is a CO2 This results in heating and evaporation. This direct heat transfer leads to the cooling of nitrogen effluent, and iodine This triggers the reverse sublimation of (I2).

[0077] The container was initially filled with approximately 19 pounds of solid CO2, which was about 20% excess cooling. It is calculated that it provides a reduction. The container is designed so that the nitrogen effluent and solid CO2 are in direct contact. It is being measured. This involves gentle stirring, gas spraying to promote self-stirring, baffles, Alternatively, it can be carried out using other methods. The contactor design is also filled with solid CO2. This may include online mixing or other desired equipment.

[0078] After the nitrogen effluent comes into contact with solid CO2 and cools to below 35°C, the emitted nitrogen effluent The difference is that most of the incoming nitrogen (19 pounds), 16 pounds of CO2 vapor, and 2.4 pounds The water vapor and 1.0 pound of residual iodine (I2) are included, and the iodine (I2) recovery efficiency is , which comes out to 96%.

[0079] After depleting solid CO2 or after treating all nitrogen effluents, any remaining solid C Back-sublimated iodine (I2) with O2 and any localized water ice removes CO2 and water. It can be heated to remove the water. The remaining 28 are estimated to contain 2100 ppm by weight of water. 0.5 pounds of iodine (I2) is either removed as is or returned to the desired drying step. It is melted to facilitate its transfer as a liquid for recycling.

[0080] If the remaining iodine (I2) has a higher water content due to the trapped water ice, Iodine (I2) can be heated to 116°C to melt solid iodine (I2). U-ion(I2) is removed as is for recycling by returning to the desired drying step. It is estimated that molten iodine(I2) contains less than 0.15% by weight of solubilized water. ru.

[0081] Table 5 (below) shows the iodine recovered using this method at 66°C, 38°C, and 10°C. It indicates the quantity. [Table 5] *CO2 is 14 lb / hour at a back sublimation temperature of 66°C, and at a back sublimation temperature of 38°C 19 lb / hour, 35 lb / hour, and -40°C reverse sublimation temperature In contrast, it is loaded at a speed of 40 lb / hour.

[0082] Example 8: Predictive example of iodine (I2) recovery by treatment with concentrated acid. Samples of inert gases containing water vapor and iodine(I2) vapor are dried. 19 pounds of nitrogen, 30 pounds of iodine (I2), and 2.5 pounds per 1000 pounds It contains water. This nitrogen effluent is supplied to the bottom of the counterflow packed column. 98% by weight is circulated for heat. The H2SO4 is supplied to the top of the packed column. The supply flow and the entire packed column operate at atmospheric pressure. In this case, it prevents the back sublimation of iodine (I2), which would normally be lost into liquid H2SO4. Therefore, it should be maintained at a high temperature of approximately 116°C or higher.

[0083] The water content of nitrogen leachate decreased from an initial 117,000 ppm by weight to less than 1,000 ppm by weight. It is estimated that this can be reduced to a certain extent. This dry nitrogen is removed by concentrated H2SO4. It has 99% water content and still contains iodine(I2), but it can be easily converted to dry iodine(I2). It can be reused or recycled.

[0084] Depending on the selection of the packing material, the packing tower, approximately 12 inches in diameter and 18 feet in height, is suitable for water and There is more than enough liquid distribution to dry the nitrogen effluent containing iodine. And to achieve mass transfer, 7 GPM / ft 2 98% by weight of circulating H2SO4 When used, the high-temperature H2SO4 circulation flow is calculated to be approximately 2,500 lb / hour.

[0085] Typically, until the circulating H2SO4 reaches a concentration of approximately 95% by weight, For this example scale, 200 gallons or 2,500 lbs of 98% by weight H2SO4 The reservoir is used, and at that point, the used H2SO4 is discarded and replaced with fresh 98% by weight. It is exchanged for H2SO4. An estimated 98% by weight of H2SO4 consumption is due to iodine(I2)1, It is 85 lbs per 000 lbs.

[0086] manner Embodiment 1 is a method for recovering iodine(I2), comprising iodine(I2) vapor and an inert To provide a flow containing at least one of gas and water vapor, and to provide an alkaline solution for the flow. The method includes contacting a liquid to form an iodide salt.

[0087] Embodiment 2 is an alkaline solution comprising sodium hydroxide, potassium hydroxide, lithium hydroxide, and water. Magnesium oxide or calcium hydroxide, sodium sulfite (Na2SO3), sulfur dioxide Sodium bisulfite (NaHSO3), potassium sulfite (K2SO3), potassium bisulfite ( KHSO3), calcium sulfite (Ca(SO3), calcium bisulfite (Ca(HS) O3)2, lithium sulfite (Li2SO3), lithium bisulfite (LiHSO3), bisulfite Magnesium sulfate (Mg(SO3), magnesium bisulfite (Mg(HSO3)2), And aqueous solutions formed from compounds selected from the group consisting of combinations thereof. This is the method described in Embodiment 1.

[0088] Embodiment 3 further comprises converting the iodide in the iodide salt to iodine (I2), The method described in 1 or 2 of the embodiment.

[0089] Embodiment 4 provides a step in which the flow is provided from the iodine (I2) drying process. The flow is a method according to any one of embodiments 1 to 3, wherein the flow contains water vapor.

[0090] Embodiment 5 is the method according to any one of Embodiments 1 to 4, wherein the flow contains an inert gas.

[0091] Embodiment 6 is a method for recovering iodine(I2), wherein iodine(I2) vapor and water vapor are used To provide a flow and to bring the flow into contact with an adsorbent to selectively adsorb water from the flow. It is a method that includes the act of doing something.

[0092] Embodiment 7 provides a step in which the flow is provided from the iodine (I2) drying process. This is the method described in embodiment 6.

[0093] Embodiment 8 involves, after the contact step, iodine(I2) vapor being used in an iodine(I2) drying process. The method according to embodiment 7, further comprising recycling into Seth.

[0094] Embodiment 9 involves, after the contact step, back sublimating the iodine (I2) vapor to produce iodine ( The method according to embodiment 6 or embodiment 7, further comprising recovering I2).

[0095] Embodiment 10 is a molecular sieve of 3A, 4A, 5A, or XH-9, Alumina, calcium sulfate, silica gel, calcium chloride, sodium sulfate, calcium iodide A group consisting of citric acid, magnesium chloride, magnesium iodide, or a combination thereof. The method is selected from any of embodiments 6 to 9.

[0096] Embodiment 11 involves heating the adsorbent to a temperature of 90°C to 120°C to remove the iodine attached to the adsorbent. The water is vaporized, and then the adsorbent is heated to approximately 150°C to 350°C to desorb the water from the adsorbent. The method according to any one of embodiments 6 to 10, further comprising regenerating the adsorbent by doing so. That is the case.

[0097] Embodiment 12 is a method according to any one of Embodiments 6 to 11, wherein the flow further includes an inert gas. be.

[0098] Embodiment 13 is a method for recovering iodine(I2), comprising iodine(I2) vapor and water vapor To provide a flow containing and to bring the flow into contact with concentrated acid to absorb water vapor from the flow. This method includes [the following].

[0099] Embodiment 14 provides a step in which the flow is removed from the iodine (I2) drying process. The method described in Embodiment 13 is provided.

[0100] Embodiment 15 is a step in which, after the contact step, iodine(I2) vapor is used in an iodine(I2) drying process. The method according to embodiment 14, further comprising recycling into a process.

[0101] Embodiment 16 recovers iodine (I2) by reverse sublimating the flow after the contact step. The method according to embodiment 13 or embodiment 14, further comprising doing the following.

[0102] Embodiment 17 is a concentrated acid consisting of sulfuric acid (H2SO4), hydroiodic acid (HI), and phosphoric acid (H3PO4). 4) Any of embodiments 13 to 16 selected from the group consisting of, and metaphosphoric acid (HPO3) The method is as follows.

[0103] Embodiment 18 is the method according to any one of Embodiments 13 to 17, wherein the flow further includes an inert gas. That is the case.

[0104] Embodiment 19 is a method for recovering iodine(I2), comprising iodine(I2) vapor and water vapor To provide a flow containing and to backsublimate or condense iodine (I2) vapor into a solid or liquid This method includes forming iodine (I2).

[0105] Embodiment 20 describes the back sublimation or condensation of iodine (I2) vapor in a flow from approximately -45°C to approximately 100°C. The method according to embodiment 19, which includes bringing the surface into contact at a temperature.

[0106] Embodiment 21 further comprises melting solid iodine (I2) to form a two-phase mixture. This is the method described in Embodiment 20.

[0107] Embodiment 22 involves heating the mixture to 114°C to approximately 160°C to obtain a two-phase mixture from This is the method according to embodiment 19, which evaporates water.

[0108] Embodiment 23 describes a process in which the back sublimation or condensation of iodine (I2) vapor is carried out at a temperature of approximately 0°C to approximately 100°C. By bringing it into contact with the surface at a certain temperature, iodine (I2) is back-sublimated or condensed without condensing water vapor. This is the method according to embodiment 19, which includes causing the action to be performed.

[0109] Embodiment 24 describes a process in which the back sublimation or condensation of iodine (I2) vapor flows at a temperature of approximately 90°C to approximately 150°C. The method according to embodiment 19, comprising condensing iodine (I2) by bringing it into contact with water at a temperature. That is the case.

[0110] Embodiment 25 describes a method in which the back sublimation or condensation of iodine (I2) vapor brings the flow into contact with liquid water, The method according to embodiment 19, comprising the back sublimation of um(I2).

[0111] Embodiment 26 further comprises drying solid or liquid iodine (I2), as described in Embodiments 19-2. The method is one of the methods described in 5.

[0112] Embodiment 27 is the method according to any one of Embodiments 19 to 26, wherein the flow further includes an inert gas. That is the case.

[0113] Embodiment 28 provides a step in which the flow is removed from the iodine (I2) drying process. The method provided is one of the methods described in any of embodiments 19 to 27.

[0114] Embodiment 29 is a method for recovering iodine(I2), comprising iodine(I2) vapor and inactive To provide a flow containing at least one of a gas and water vapor, and to bring the flow into contact with a material. By bringing the materials into contact, the materials absorb latent heat and sensible heat through the phase change of the material. When performing at least one of our processes, iodine (I2) vapor is condensed or backsublimated from the flow. It is a method that includes the act of doing something.

[0115] Embodiment 30 is a step in which the flow reaches a temperature of -40°C to 70°C. The method described in embodiment 29.

[0116] Embodiment 31 is a material in which the material is solid carbon dioxide, ice, supercooled liquid, for example nitrogen, carbon dioxide, 1,1,1,3,3-Pentafluoropropane (HFC-245fa), HCFC-24 4bb, pentafluoroethane (HFC-125), HFC-134a, HFC-32, and trifluoroiodomethane (CF3I), as well as supercooled gases, such as nitrogen, carbon dioxide Carbon, 1,1,1,3,3-pentafluoropropane (HFC-245fa), penta Luoroethane (HFC-125), HFC-134a, HFC-32, CF3I, HCF Selected from the group consisting of C-244bb, alkanes, such as methane, ethane, and propane. This is the method described in Embodiment 29 or Embodiment 30.

[0117] Embodiment 32 provides a step in which the flow is provided from the iodine (I2) drying process. The flow is a method according to any one of embodiments 29 to 31, wherein the flow contains water vapor.

[0118] Embodiment 33 is a flow that includes an inert gas, according to any of Embodiments 29 to 32. ru.

[0119] Embodiment 34 is a method for recovering iodine(I2), wherein the flow is an iodine(I2) drying process The supply from Seth is a flow of iodine (I2) vapor, inert gas, and water vapor. Including providing and bringing the flow into contact with an alkaline solution to form an iodide salt. The alkaline solution contains sodium hydroxide, potassium hydroxide, and sodium sulfite. A group consisting of Na2SO3, potassium sulfite (K2SO3), and combinations thereof. The method involves an aqueous solution formed from selected compounds.

[0120] Embodiment 35 is a method for recovering iodine(I2), which is an iodine(I2) drying process or The purpose is to provide a flow in which iodine (I2) vapor, inert gas, and water vapor It contains air, provides it, and brings the flow into contact with the adsorbent, selectively adsorbing water from the flow. And, after the contact step, iodine(I2) vapor is used in the iodine(I2) drying process. This includes recycling, and the adsorbent is 3A molecular sieve and 4A molecular This method is selected from a group consisting of Larsieves.

[0121] Embodiment 36 involves heating the adsorbent to a temperature of 90°C to 120°C to remove the iodine adhering to the adsorbent. The water is vaporized, and then the adsorbent is heated to approximately 150°C to 350°C to desorb the water from the adsorbent. The method according to embodiment 35 further includes regenerating the adsorbent by doing so.

[0122] Embodiment 37 is a method for recovering iodine(I2), which is an iodine(I2) drying process or The purpose is to provide a flow in which iodine (I2) vapor, inert gas, and water vapor By incorporating gas, providing it, and bringing the flow into contact with concentrated acid, water vapor is absorbed from the flow. After the step of contacting the concentrated acid containing sulfuric acid (H2SO4) and absorbing it, This includes recycling iodine(I2) vapor into an iodine(I2) drying process. , that is the method.

[0123] Embodiment 38 A method for recovering iodine(I2), wherein the iodine(I2) is flowed from the iodine(I2) drying process. The purpose is to provide a flow that includes iodine (I2) vapor, an inert gas, and water vapor. To provide, and to back sublimate or condense iodine (I2) vapor to produce solid or liquid iodine. This includes the formation of (I2), and the back sublimation or condensation of iodine (I2) vapor, which flows approximately Contacting with the surface at a temperature of 0 °C to about 100 °C to sublimate or condense iodine (I 2) without condensing water vapor, a method.

[0124] Aspect 39 A method for recovering iodine (I2), comprising providing a stream from an iodine I2 drying process, the stream comprising iodine (I2) vapor, an inert gas, and water vapor, providing, and sublimating or condensing the iodine (I2) vapor to form solid or liquid iodine ( I2), wherein the sublimation or condensation of the iodine (I2) vapor comprises contacting the stream with water at a temperature of about 9 0 °C to about 150 °C to condense the iodine (I2), a method.

[0125] Aspect 40 A method for recovering iodine (I2), comprising providing a stream from an iodine (I2) drying process, the stream comprising iodine (I2) vapor, an inert gas, and water vapor, providing, and sublimating or condensing the iodine (I2) vapor to form solid or liquid iodine (I2), wherein the sublimation or condensation of the iodine (I2) vapor comprises contacting the stream with liquid water to sublimate the iodine (I2), a method.<​​​​​​​​​​​​​​​​​ Iodine (I 2 ) To provide a flow containing steam, an inert gas, and at least one of water vapor, A method comprising contacting the aforementioned flow with an alkaline solution to form an iodide salt. [2] The alkaline solution may contain sodium hydroxide, potassium hydroxide, lithium hydroxide, magnesium hydroxide, or calcium hydroxide, or sodium bisulfite (NaHSO4). 3 ), sodium sulfite (Na 2 SO 3 ), potassium sulfite (K 2 SO 3 ), potassium bisulfite (KHSO 3 ), calcium sulfite (Ca(SO) 3 ), calcium bisulfite (Ca(HSO) 3 ) 2 Lithium sulfite (Li 2 SO 3 ), lithium bisulfite (LiHSO4) 3 ), magnesium sulfite (Mg(SO) 3 ), magnesium bisulfite (Mg(HSO4) 3 ) 2 The method according to item 1, wherein the aqueous solution is formed from a compound selected from the group consisting of ), and combinations thereof. [3] The iodide in the iodide salt is converted to iodine (I 2 The method according to item 1 or 2, further comprising converting to ). [4] In the steps provided above, the flow contains iodine (I 2 ) The method according to any one of claims 1 to 3, wherein the flow is provided from a drying process and the flow includes water vapor. [5] The method according to any one of items 1 to 4, wherein the flow includes an inert gas. [6] Iodine (I 2 A method for recovering ) and the said method Iodine (I 2 ) To provide a flow containing steam and water vapor, A method comprising bringing the flow into contact with an adsorbent to selectively adsorb water from the flow. [7] In the steps provided above, the flow contains iodine (I 2 The method according to item 6, provided from a drying process. [8] After the contact step, the iodine (I 2 ) vapor of the iodine (I 2 The method of paragraph 7, further comprising recycling into a drying process. [9] After the contact step, the iodine (I 2 ) By back sublimating the vapor, iodine (I 2 The method of item 6 or 7, further comprising recovering the )

[10] The method according to any one of claims 6 to 9, wherein the adsorbent is selected from the group consisting of molecular sieves of 3A, 4A, 5A, or XH-9, alumina, calcium sulfate, silica gel, calcium chloride, sodium sulfate, calcium iodide, magnesium chloride, magnesium iodide, or a combination thereof.

[11] The method according to any one of claims 6 to 10, further comprising heating the adsorbent to a temperature of 90°C to 120°C to vaporize the iodine attached to the adsorbent, and then heating the adsorbent to about 150°C to about 350°C to desorb water from the adsorbent to regenerate the adsorbent.

[12] The method according to any one of claims 6 to 11, wherein the flow further comprises an inert gas.

[13] Iodine (I 2 A method for recovering ) and the said method Iodine (I 2 ) To provide a flow containing steam and water vapor, A method comprising bringing the aforementioned flow into contact with a concentrated acid to absorb the water vapor from the aforementioned flow.

[14] In the steps provided above, the flow contains iodine (I 2 The method described in item 13, provided from a drying process.

[15] After the contact step, the iodine (I 2 ) vapor of the iodine (I 2 The method according to paragraph 14, further comprising recycling into a drying process.

Claims

1. Iodine (I ２ A method for recovering ) and the said method Iodine (I ２ ) To provide a flow containing steam and water vapor, The aforementioned flow is brought into contact with an adsorbent to selectively adsorb water from the flow. Includes, A method wherein the adsorbent is selected from the group consisting of molecular sieves of type 3A, 4A, 5A, or XH-9, alumina, calcium sulfate, silica gel, calcium chloride, sodium sulfate, calcium iodide, magnesium chloride, magnesium iodide, or combinations thereof.

2. In the steps provided above, the flow contains iodine (I ２ The method according to claim 1, provided from a drying process.

3. After the step of contacting, the iodine (I ２ ) vapor of the iodine (I ２ The method according to claim 2, further comprising recycling into a drying process.

4. After the step of contacting, the iodine (I ２ ) By back sublimating the steam, iodine (I ２ The method according to claim 1, further comprising recovering the following.

5. The method according to claim 1, further comprising heating the adsorbent to a temperature of 90°C to 120°C to vaporize the iodine attached to the adsorbent, and then heating the adsorbent to approximately 150°C to approximately 350°C to desorb water from the adsorbent to regenerate the adsorbent.

6. The method according to claim 1, wherein the flow further includes an inert gas.

7. The method according to claim 1, wherein the adsorbent comprises molecular sieve of 4A.

8. The method according to claim 1, wherein the adsorbent comprises molecular sieve of 3A.

9. The method according to claim 1, wherein the adsorbent comprises molecular sieve of 5A.

10. The method according to claim 1, wherein the adsorbent comprises an XH-9 molecular sieve.

11. The method according to claim 1, wherein the adsorbent comprises alumina.

12. The method according to claim 1, wherein the adsorbent comprises calcium sulfate.

13. The method according to claim 1, wherein the adsorbent includes silica gel.

14. The method according to claim 1, wherein the adsorbent comprises calcium chloride.

15. The method according to claim 1, wherein the adsorbent comprises sodium sulfate.

16. The method according to claim 1, wherein the adsorbent comprises calcium iodide.

17. The method according to claim 1, wherein the adsorbent comprises magnesium chloride.

18. The method according to claim 1, wherein the adsorbent comprises magnesium iodide.

19. The method according to claim 1, further comprising reacting iodine from the iodine (I₂) vapor with hydrogen to produce hydrogen iodide.

20. The method according to claim 19, further comprising using hydrogen iodide in the preparation of an iodoalkane.

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