EP2861322A1 - Adsorbants magnétiques, procédés pour fabriquer un adsorbant magnétique, et procédés d'élimination de contaminants de flux de fluide - Google Patents

Adsorbants magnétiques, procédés pour fabriquer un adsorbant magnétique, et procédés d'élimination de contaminants de flux de fluide

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Publication number
EP2861322A1
EP2861322A1 EP20130804938 EP13804938A EP2861322A1 EP 2861322 A1 EP2861322 A1 EP 2861322A1 EP 20130804938 EP20130804938 EP 20130804938 EP 13804938 A EP13804938 A EP 13804938A EP 2861322 A1 EP2861322 A1 EP 2861322A1
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EP
European Patent Office
Prior art keywords
adsorbent
magnetic
activated carbon
iron oxide
magnetic adsorbent
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP20130804938
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German (de)
English (en)
Other versions
EP2861322A4 (fr
Inventor
Heather BYRNE
Ameena KHAN
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Carbonxt Group Ltd
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Carbonxt Group Ltd
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Publication date
Application filed by Carbonxt Group Ltd filed Critical Carbonxt Group Ltd
Publication of EP2861322A1 publication Critical patent/EP2861322A1/fr
Publication of EP2861322A4 publication Critical patent/EP2861322A4/fr
Withdrawn legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—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
    • 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
    • B01D53/06—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 moving adsorbents, e.g. rotating beds
    • B01D53/10—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 moving adsorbents, e.g. rotating beds with dispersed adsorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—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
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/64—Heavy metals or compounds thereof, e.g. mercury
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—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
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/81—Solid phase processes
    • B01D53/83—Solid phase processes with moving reactants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28009—Magnetic properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3021—Milling, crushing or grinding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/10—Oxidants
    • B01D2251/108—Halogens or halogen compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/102—Carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/20707—Titanium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/80—Type of catalytic reaction
    • B01D2255/802—Photocatalytic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/60—Heavy metals or heavy metal compounds
    • B01D2257/602—Mercury or mercury compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/02—Other waste gases
    • B01D2258/0283—Flue gases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/80—Employing electric, magnetic, electromagnetic or wave energy, or particle radiation
    • B01D2259/814—Magnetic fields

Definitions

  • HAPs hazardous air pollutants
  • mercury and mercury -containing compounds have been a source of significant concern due to their increasing rate of release and the lack of adequate control technologies.
  • the resulting quantity in the environment is usually low, it can transfer to various organisms, and then magnify up the food chain.
  • concentration of accumulated mercury in some fish can reach levels that are millions of times greater than that in the water.
  • the consumption of such fish by humans, and the resulting buildup of mercury in various tissues may lead to serious neurological and developmental effects such as losses of sensory or cognitive ability, tremors, inability to walk, convulsions, and even death.
  • Methylmercury the most common form of organic mercury, is almost completely incorporated into the blood stream, and can be transferred through the placenta and into all of the tissues of the fetus, including that of the brain. Because of the health concerns related to eating mercury contaminated fish, bans on fishing in certain regions such as in the Great Lakes have resulted in considerable losses to the economy.
  • brominated activated carbons have been shown to have the highest mercury removal rate per pound of product.
  • these products have a higher cost margin - and therefore would increase the economic impact - and may cause corrosion of plant equipment.
  • PAC's generally low mercury adsorption efficiency and lack of adequate regeneration technologies have sparked an interest in modifying the material to either decrease costs or improve performance.
  • Such fly ash cannot be resold for beneficial reuse and must, instead, be landfilled.
  • Current research geared towards separation technologies has yet to find an adequate method to isolate the PAC from the fly ash. Therefore, a method that can easily separate PAC from the fly ash is desirable. Such a method will (a) maintain the quality of the fly ash for subsequent sale and reuse, and (b) permit the reuse of the PAC for additional mercury capture.
  • U.S. Patent No. 7,879,136 teaches a method to recover PAC from fly ash by creating a magnetic activated carbon through a wet precipitation method. This method is similar to US Patents 2,479,930, 6,914,034, and 8,097, 185B2, which also teach wet methods using iron precursors to make a magnetic activated carbon. Others have created magnetic adsorbents by: combining the sorbent with a magnetic material using a binder (US Patent No. 7,429,330), mixing a sorbent with a magnetic material (US Patent No. 4,260,523), or mixing a magnetic material with an organic material, followed by activation (US Patents 4,260,523, 4,201,831, and 7,429,330).
  • Disclosed herein are processes to manufacture a magnetic adsorbent, a method using the magnetic adsorbent for the removal of contaminants from fluid streams, and the recovery of the magnetic adsorbent after use.
  • a magnetic adsorbent with sufficient oxidizing power, affinity, and surface area for the capture of mercury from the flue gas of coal combustion devices is provided. This material may also be applied for the capture of other target contaminants such as arsenic and selenium. The magnetic adsorbent can then be recovered from the coal combustion flyash, and re-injected into the flue gas for additional mercury capture.
  • a method of manufacturing the magnetic adsorbent involves combining the selected adsorbent with a magnetic additive and in some cases an oxidizing additive.
  • the precursor adsorbent may be an activated carbon, reactivated carbon, silica gel, zeolite, alumina clay, or other solid material with sufficient surface area for mercury capture.
  • the magnetic additive is preferably one of the following: magnetite, hematite, goethite, or maghemite.
  • the oxidizing additives may include, but are not limited to halides of alkali metals, alkaline earth metals, and ammonium (i.e., NH 4 Br, KBr, LiBr, NaBr, NaCl, KC1, LiCl, I, Lil, Nal), and semiconductors (T1O2, ZnO, Sn0 2 , V0 2 , and CdS).
  • halides of alkali metals, alkaline earth metals, and ammonium i.e., NH 4 Br, KBr, LiBr, NaBr, NaCl, KC1, LiCl, I, Lil, Nal
  • semiconductors T1O2, ZnO, Sn0 2 , V0 2 , and CdS.
  • a method to manufacture the magnetic adsorbent involves combining the selected adsorbent with a magnetic additive and in some cases additional additives to improve the oxidation capacity.
  • the additives may be implanted on the adsorbent using a variety of means, including but not limited to: mixing, milling, or grinding the adsorbent and the additives together until some fraction of the material is physically implanted on the surface of the activated carbon.
  • a method for removing a contaminant or contaminants from a fluid stream is provided (Contaminant Removal Method).
  • the method includes contacting the fluid stream with the magnetic adsorbent whereby the contaminant is adsorbed on the magnetic adsorbent, and then removing the magnetic adsorbent having the contaminant adsorbed thereon from the fluid stream. Also provided is a method to recycle the collected composite back into contact with the fluid stream for further contaminant removal (Composite Recycling Method).
  • a magnetic adsorbent in one embodiment, includes an adsorbent and iron oxide implanted onto a surface of the adsorbent, wherein a total surface area of the magnetic adsorbent is not substantially less than a total surface area of the adsorbent.
  • the adsorbent is activated carbon.
  • an additive selected from the group consisting of a halogen, a photocatalyst, and a binder is added.
  • the magnetic adsorbent does not include secondary deposits.
  • a ratio of the weight of the iron oxide to a total weight of the magnetic adsorbent is between 1% to 20%.
  • a ratio of the weight of the iron oxide to a total weight of the magnetic adsorbent is between 5% to 15%.
  • a ratio of the weight of the iron oxide to a total weight of the magnetic adsorbent is 10%.
  • the iron oxide is highly crystalline after implantation. In one configuration, a crystalline nature of the iron oxide is maintained after implantation.
  • a magnetic adsorbent consists essentially of an adsorbent; and an iron oxide implanted onto the surface of the adsorbent, wherein a surface area of the magnetic adsorbent is not substantially less than the surface area of the adsorbent.
  • the adsorbent is activated carbon.
  • a method of making a magnetic adsorbent includes combining an adsorbent and a magnetic material using mechanical mixing equipment.
  • the adsorbent is activated carbon and the magnetic material is iron oxide.
  • the mechanical mixing equipment is selected from the group consisting of a ball mill, a jet mill, and a conical mill.
  • the mechanical mixing equipment encourages friction and collision between particles.
  • the method includes implanting the magnetic material on the surface of the adsorbent.
  • the combining includes grinding and is performed until the magnetic adsorbent will pass through a 325- mesh sieve.
  • a method of treating an effluent stream includes treating the effluent stream by injecting magnetic adsorbent particles and using magnetic field to recover the magnetic adsorbent particles.
  • the magnetic adsorbent particles are re-injected into the effluent stream with additional magnetic adsorbent particles after recovery.
  • the magnetic adsorbent particles remove mercury from the effluent stream.
  • high quality fly ash is recovered from a stream treated by a magnetic adsorbent.
  • the method includes capturing the magnetic adsorbent from fly ash in the effluent stream using a magnetic field to generate two products: (1) high quality fly ash, and (2) recovered magnetic adsorbent.
  • a system for removing mercury from an effluent system includes an activated carbon injection system, injecting an activated carbon product into an effluent.
  • the system further includes a first electrostatic precipitator positioned after the activated carbon injection system, receiving the effluent.
  • the first electrostatic precipitator is positioned immediately following the activated carbon injection system, without any intervening treatments.
  • the activated carbon product is magnetic.
  • the activated carbon product includes a photocatalyst.
  • the first electrostatic precipitator activates the photocatalyst.
  • a second electrostatic precipitator immediately precedes the activated carbon injection system.
  • the activated carbon product has iron oxide implanted on the surface and has a surface area that is not substantially less than the surface area without the iron oxide.
  • an adsorbent in another embodiment, includes an activated carbon portion and a magnetic portion joined with the activated carbon portion, wherein magnetic activity of the magnetic portion is not shielded by the activated carbon portion.
  • the magnetic portion is implanted on the surface of the activated carbon portion.
  • a total surface area of the activated carbon portion without the magnetic portion is substantially at least the same as a total surface area of the adsorbent.
  • Figure 1 shows an SEM image and EDS map of the titania and iron signals of the activated carbon adsorbent, demonstrating the absence of additives on the adsorbent surface
  • Figure 2 shows an SEM image and an EDS map of the iron signal of a magnetic adsorbent prepared by milling an activated carbon material with magnetite at a loading of 10% by weight, demonstrating the distribution of magnetite throughout the sample, on its surface;
  • Figure 3 represents a spot EDS analysis on a particle isolated in Figure 2, demonstrating the clear presence of iron on the adsorbent;
  • Figure 4 represents an SEM image and an EDS map of the iron and titania signal of a magnetic adsorbent prepared through ball-milling an activated carbon adsorbent with T1O2 and magnetite at 1% and 10% loading by weight, respectively.
  • the image demonstrates the wide distribution of magnetite, as well as the presence of titania, on the adsorbent surface;
  • Figure 5 represents a spot EDS analysis on a particle isolated in Figure 4, demonstrating the clear presence of iron on the adsorbent
  • Figure 6 represents a spot EDS analysis on a particle isolated in Figure 4, demonstrating the clear presence of titania on the adsorbent
  • Figure 7 represents an SEM image and an EDS map of the iron signal of a magnetic adsorbent prepared with magnetite, at a loading of 10% by weight, via mechano fusion. The figure demonstrates the distribution of magnetite throughout the sample, on its surface;
  • Figure 8 represents a schematic of the bench scale apparatus used to collect the fixed bed data presented herein;
  • Figure 9 represents the mercury removal curve during a fixed bed evaluation with various magnetic adsorbent materials, demonstrating the benefit of additives for mercury removal;
  • Figure 10 represents the mercury removal curve during actual flue gas conditions with the base activated carbon and the produced magnetic adsorbent, demonstrating the benefit for mercury removal;
  • Fig. 1 1a and l ib show embodiments of an activate carbon injection system up stream of an electrostatic precipitator (ESP);
  • ESP electrostatic precipitator
  • Fig. 12 shows Mercury removal curve for activated carbon injection in a 5 MW slip stream flue gas for a PAC readily available for commercial purchase in the industry (Industry Carbon), a MPAC coated with 10% Fe 3 0 4 (MPAC), with 10% Fe 3 0 4 and 1% Ti0 2 (MPAC- Ti0 2 ), and another with 10% Fe 3 0 4 and 2.5% NaBr (MPAC-Na-Br) by weight.
  • MPAC MPAC coated with 10% Fe 3 0 4
  • MPAC- Ti0 2 MPAC- Ti0 2
  • MPAC-Na-Br 10% Fe 3 0 4 and 2.5% NaBr
  • magnetic adsorbent composites are prepared, whereby a magnetic material is physically implanted onto the exposed surface of an adsorbent.
  • the implantation may be achieved by simultaneously combining the adsorbent and iron oxide together and using mechanical mixing equipment such as a ball mill, jet mill, conical mill, etc. This mixing environment encourages friction and collision between the particles to promote implantation.
  • Forces for implantation may include Van der Waals Forces, capillary forces, electrical forces and electrostatic coulomb forces. These forces may be promoted during the mixing process.
  • Magnetic adsorbent is an important feature of the magnetic adsorbent created, in contrast to some prior art adsorbents where the magnetic material is implanted within the adsorbent; implantation on the surface does not shield or block the magnetic forces from acting on the magnetic material. This feature provides for the recapture and recycling of magnetic adsorbent since magnetic forces may be applied to recapture it after treatment. This greatly improves the cost effectiveness of the methods and materials described herein. In various places herein the implantation of magnetic materials is discussed. Significant variation of the amount and type of magnetic material implanted is contemplated and may be related to the implantation techniques used and described herein.
  • the adsorbent material for the creation of a magnetic adsorbent will have an appreciable surface area and developed porosity.
  • activated carbon It can be: activated carbon, reactivated carbon, zeolite, alumina clays, silica gels, etc.
  • the adsorbent is activated carbon.
  • the term "activated carbon” as used herein is meant to reference powdered or granular carbon used for purification by adsorption. In many configurations the activated carbon used has a surface area between 200 and l,000m 2 /g, more preferably between 300 and 700m 2 /g, and most preferably between 400 and 600m /g. In some alternatives, powder activated carbon (PAC) is used.
  • PAC powder activated carbon
  • the term "Powdered Activated Carbon” refers to an activated carbon, 90% of which passes through a 352-mesh sieve (45 ⁇ ) (i.e., at least 90% passes through a 352 mesh). Also, the following abbreviations may be used herein: Activated Carbon: AC; Powdered Activated Carbon: PAC; and Magnetic Powdered Activated Carbon: MPAC.
  • the magnetic material may be at least one of the following: magnetite (Fe304), maghemite (y-Fe 2 0 3 ), hematite (a-Fe 2 0 3 ) and goethite (FeO(OH)); and in many embodiments magnetite.
  • the amount of magnetic material in the composite is preferably between at least 1% and less than 20% by weight based on the total weight of the final composite; more preferably between 5% and 15% by weight based on the total weight of the final composite; most preferably 5% by weight based on the total weight of the final composite.
  • Figs. 1-3 show the results of a composite made as described above.
  • Fig. 1 shows an SEM image and EDS map of the titania and iron signals of the activated carbon adsorbent at 500 times magnification, demonstrating the absence of additives on the adsorbent surface according to one embodiment.
  • an SEM image and an EDS (Energy-dispersive X- ray spectroscopy) map show the iron signals appearing on the activated carbon.
  • Fig. 2 shows a sample created according to the milling with activated carbon described above.
  • Fig. 1 shows an SEM image and EDS map of the titania and iron signals of the activated carbon adsorbent at 500 times magnification, demonstrating the absence of additives on the adsorbent surface according to one embodiment.
  • an SEM image and an EDS (Energy-dispersive X- ray spectroscopy) map show the iron signals appearing on the activated carbon.
  • Fig. 2 shows a sample created
  • FIG. 2 shows an SEM image and an EDS map of the iron signal of a magnetic adsorbent at 500 times magnification prepared by milling an activated carbon material with magnetite at a loading of 10% by weight, demonstrating the distribution of magnetite throughout the sample, on its surface.
  • a graph showing the occurrence of primarily Fe 330 on the activated carbon is shown as compared to other contaminates.
  • Fig. 3 represents a spot EDS analysis on a particle isolated on Fe-particle in ball milled sample (FeOx), demonstrating the clear presence of iron on the adsorbent.
  • the graph shows the counts 310 vs. energy (keV) 320.
  • Fig. 1 shows an SEM image and EDS map of the titania and iron signals of the activated carbon adsorbent at 500 times magnification, demonstrating the absence of additives on the adsorbent surface according to one embodiment;
  • Oxidizing additives may be selected from halides of alkali metals, alkaline earth metals, and ammonium (i.e., NH 4 Br, Br, LiBr, NaBr, NaCl, KC1, LiCl, KI, Lil, Nal) and photocatalysts (i.e., T1O2, ZnO, VO2, SnCh, and CdS).
  • Some oxidizing additives and photocatalyts may also act as a binder, encouraging the magnetic additives to adhere to the adsorbent surface.
  • Binders Other separate binders may also be applied (i.e., Binders).
  • the adsorbent is activated carbon
  • the magnetic material is magnetite
  • the oxidizing and/or binding additives are NaBr and/or Ti0 2 .
  • the amount of additional additive material in the composite is preferably between at least 0.1% and less than 10% by weight based on the total weight of the final composite; more preferably between 0.5% and 5% by weight based on the total weight of the final composite.
  • Additional features of embodiments of magnetic adsorbent created include unique iron oxide concentration, the crystalline nature of the iron oxide included, the absence of secondary deposits or byproducts on the surface, the impact on the physical characteristics of the magnetic adsorbent, and the additives that may be added.
  • the iron oxide concentration of the magnetic adsorbent produced is between 1% and 20% by weight, more preferably between 5% and 15% by weight, most preferably 10% by weight.
  • the Magnetic Adsorbent Creation Method produces an adsorbent that maintains the crystalline structure of the magnetic material. This crystallinity is likely greater than that of materials produced via wet chemistry methods. Further, since heat treatments are not necessary in the Magnetic Adsorbent Creation Method, the crystalline nature is not degraded.
  • Magnetic Adsorbent Creation Method The occurrence of secondary deposits is also reduced or eliminated by the Magnetic Adsorbent Creation Method.
  • wet chemistry methodologies may include reactants that leave byproducts and interact with the adsorbent or iron oxide.
  • the Magnetic Adsorbent Creation Method further does not erode the pore volume or pore size of the magnetic adsorbent and may result in a slight measurable increase in total surface area caused by interstitial spaces created by the adhered particles on the surface of the activated carbon adding to the available surface area.
  • the deposition of iron oxides may degrade the surface area, pore size, and pore volume.
  • the magnetic adsorbent can be treated with a halogen, a photocatalyst, or a binder to further enhance the mercury oxidation and therefore adsorption and removal from the contaminated stream.
  • a known magnetic species By adding a known magnetic species, the magnetic strength is controlled and deposited on the surface of the adsorbent. Surface-deposition of the magnetic material allows magnetic forces for recovery to be maximized. Further, the speciation and crystallinity of the magnetic material is not altered by production, thereby protecting its magnetic properties. This is in contrast to those methods that deposit the magnetic material within the sorbent, where the sorbent material itself can mask the magnetic forces and hinder recovery.
  • the material can be applied for contaminant removal in a fluid stream. While the said material has the potential to be effective for various contaminants in a myriad of fluid streams, it is known to be effective for the contaminant mercury and the fluid stream of flue gas. In this representation, the material is removed from the flue gas by typical particle collection devices in operation, such as electrostatic precipitators, fabric filters, cyclones, and even scrubbers.
  • the composite After the composite is separated from the fluid stream and collected, it can be recovered and reused.
  • the recovery utilizes the magnetic properties of the material.
  • the magnetic material is collected in an electrostatic precipitator with other flue gas particles (fly ash).
  • a magnetic recovery system is applied after the electrostatic precipitator collection to separate the magnetic material from the fly ash.
  • the magnetic material is then stored for reuse. Additionally, before reuse, the material may be regenerated using chemical or thermal techniques. The material may then be reapplied for further contaminant removal from the fluid stream. Utilizing this technique results in significant cost savings for the user and reduces the quantity of waste materials.
  • the composite is treated with a halogen known for oxidizing Hg.
  • the halogenated composite may be formed by (i) mechanically mixing a halogen compound, a magnetic material and adsorbent; (ii) exposing the composite of adsorbent and magnetic material to a halogen gas; or (iii) reacting the magnetic material and a halogen, then co-milling the resultant with adsorbent.
  • a photocatalyst for example, titanium dioxide (Ti0 2 ) is included in the magnetic adsorbent.
  • Hydroxyl radicals can be generated on the surface of Ti0 2 in an excited state; these powerful oxidants enhance mercury capture by oxidizing elemental Hg to form, for example, HgO.
  • the oxidized mercury e.g., HgO
  • HgO oxidized mercury
  • the gradual buildup of HgO on the sorbent may improve mercury uptake over the injection cycles.
  • UV lamps generating wavelengths less than about 365 nm would be required to provide the required energy for Ti0 2 excitation.
  • UV radiation includes invisible radiation wavelengths from about 4 nanometers, on the border of the x-ray region, to about 380 nanometers, just beyond the violet in the visible spectrum.
  • Figs. 4-6 show the results from preparing a ball milled sample as described above with TiCVFeOx.
  • Fig. 4 represents an SEM (Scanning Electron Microscope) image and an EDS map of the iron and titania signal of a magnetic adsorbent (at 500 times magnification) prepared through ball- milling an activated carbon adsorbent with Ti0 2 and magnetite at 1% and 10% loading by weight, respectively, demonstrating the wide distribution of magnetite, as well as the presence of titana, on the adsorbent surface.
  • SEM Sccanning Electron Microscope
  • FIG. 5 represents a spot EDS analysis on a particle isolated on Fe-particle in ball milled sample (Ti0 2 /FeO x ), demonstrating the clear presence of iron on the adsorbent.
  • Fig. 5 demonstrates the existence of iron with peak 530.
  • the graph shows the counts 510 vs. energy (keV) 520.
  • Fig. 6 represents a spot EDS analysis on a particle isolated on Ti-particle in ball milled sample (Ti0 2 /FeO x ), demonstrating the clear presence of titania on the adsorbent.
  • Fig. 6 demonstrates the existence of Ti with peak 630.
  • the graph shows the counts 610 vs. energy (keV) 620.
  • the magnetic adsorbent will have a specific fraction of magnetized particles depending on the manufacturing technique. In some embodiments, this fraction is recoverable from fly ash or other non-magnetic particles from fluid streams (such as air and water). The magnetic recovery is achieved by passing a mixed particle stream through a magnetic recovery device.
  • ESP electrostatic precipitator
  • electromagnets to collect the magnetic adsorbent while allowing the other particles to pass through the collection device.
  • the recovered magnetic adsorbent can then be regenerated or reused, depending on the application.
  • magnetic adsorbent In flue gas treatment for mercury, magnetic adsorbent is separated from the other particles (fly ash) in the flue gas airflow.
  • the recovered, used magnetic adsorbent would be mingled with fresh magnetic adsorbent, and then injected again for in-flight mercury capture. This has the added benefit of improving the quality of the flyash for potential salability.
  • Fig. 11a and l ib show two embodiments of an activated carbon injection system positioned before and between an ESP. Boiler 1110 feeds to a selective catalytic reduction system 1 115. Then the effluent flows to an air heater 1120.
  • activated carbon is injected from ACI 1 125.
  • the activated carbon then passes through the ESP 1130 which produces an electrostatic discharge, which, in some embodiments, can excite the properties of the activated carbon to result in enhanced mercury removal.
  • the flue gas passes through the flue gas desulfurization 1 135 and out of exhaust stack 1 140.
  • a first ESP 1130 precedes the injection of activated carbon and a second ESP 1 132 follows. The injection may also occur before both ESPs. Other instances would exclude the use of a selective catalytic reduction system 1 115 or a flue gas desulfurization 1 135.
  • the activated carbon in many of these cases, as described above, includes a photocatalyst.
  • this system is that similar results may be achieved as compared to an activated carbon system with a fabric filter, without the same pressure drop as would be experienced with a fabric filter.
  • an ACI system and an added ESP system may be used to retrofit existing plants.
  • this system may provide synergy with the magnetic adsorbent for mercury removal but be less costly than other well established retrofits known by those skilled in the art, such as a fabric filter installation for ACI, and may be easily integrated into existing systems.
  • the positioning of the ESP in a typical system may enhance the activity of the activated carbon as compared to systems injecting activated carbon at an earlier point in the system.
  • ESP systems are located near the end of an effluent cleaning system as shown in Figs. 11a and l ib. Therefore, activated carbon may be injected immediately before the ESP and may have higher effectiveness since the effluent will have cooled significantly by that point in the system. Also, fewer other constituents may exist in the effluent immediately before the ESP, therefore allowing the activated carbon to work primarily to remove Mercury. The specific configuration of the system will determined the exact operating parameters and removal capabilities. In some embodiments halogens may be substituted for the photocatalyst.
  • a magnetic activated carbon sample with a 10% by weight concentration of magnetite (Fe 3 0 4 ) was prepared by simultaneously grinding 9g of activated carbon with lg of magnetite in a ball mill. Grinding continued until 90% of the final product would pass through a 325- mesh sieve.
  • a virgin product was also prepared using the same activated carbon, but with no additive, milled to the same specification.
  • Figure 8 presents the bench-scale test stand that was used to quantify the adsorption capacity of the inventive MPAC.
  • Air 815 and High-grade nitrogen gas 815 were passed through mass flow controllers 820, to control the flow of air representing effluent into the system.
  • the nitrogen gas 815 from reservoir was passed through an elemental mercury permeation tube 825 to create a mercury vapor laden air with 10 ug/m 3 of Hg.
  • the mercury vapor was then transported through a heating tube 830 to the fixed-bed reaction column.
  • the temperature of the Hg gas was monitored and maintained at 150°C upstream of the MPAC 835.
  • the sorbent was evenly dispersed within a matrix of silica sand, and supported on a quartz frit. The temperature of the sorbent bed was monitored and maintained at 110 °C using heating tape.
  • Effluent gas from the sorbent bed was cooled using a series of impingers 840, 845 in a water bath prior to monitoring elemental Hg by an inline RA-915 Zeeman Mercury Spectrometer (Ohio Lumex) 855. Effluent concentrations of mercury from the stand were recorded for comparison of composite PAC samples. A carbon trap and exhaust system 860 collected remaining waste from the system.
  • Hg adsorption capacities of the composite and the virgin counterpart were quantified using the test stand shown in Figure 8.
  • Table 1 summarizes the test results. As shown, the addition of iron oxide produced a sorbent with greater Hg removal capacity.
  • Table 2 shows the characteristics of the virgin AC and the composite product.
  • a magnetic activated carbon sample with a 10% by weight concentration of magnetite (Fe 3 0 4 ) was prepared by simultaneously milling 18 lbs. of activated carbon with 2 lbs. of magnetite in a ball mill. Grinding continued until 95% of the final product would pass through a 325-mesh sieve. Two additional sorbents were made by adding additional oxidants. The first was prepared by simultaneously milling 18 lbs. of activated carbon with 2 lbs. of magnetite and 0.2 lb. of T1O2 in a ball mill to the same size specification as the first. The second was prepared by simultaneously milling 18 lbs, of activated carbon with 2 lbs. of magnetite and 0.5 lb. of NaBr in a ball mill to the same size specification as the first. A fourth carbon was procured from a commercial activated carbon supplier designed for the mercury removal from flue gas application.
  • Fig. 9 represents the mercury removal curve during a fixed bed evaluation with various magnetic adsorbent materials, demonstrating the benefit of additives for mercury removal.
  • the y-axis 910 shows the normalized mercury concentration in C/Co.
  • the x-axis 920 represents time in minutes.
  • the results for various additives are shown including PAC 920, MPAC 930, PAC-Br 935, MPAC-Br 940, and MPAC-Ti0 2 945 in accordance with the various embodiments described herein.
  • Fig. 10 represents the mercury removal curve during actual flue gas conditions with the base activated carbon (injection in a 5 MW slip stream flue gas for a Base AC (PAC) 1030 and a MPAC 1040 coated with 5% Fe304 by weight) and the produced magnetic adsorbent, demonstrating the benefit for mercury removal.
  • the y-axis 1010 shows the total percentage of mercury removal and the x-axis shows the injection rate in lb/MMacf.
  • the four products were tested at the Mercury Research Center (MRC).
  • the MRC removes a constant flow of approximately 20,500 acfm of flue gas (representative of a 5 MW boiler) from the Southern Company Plant Christ Boiler (78 MW).
  • the boiler runs on low-sulfur bituminous coal blend from varying sources. While typical S03 concentrations of previous fuel blends resulted in less than 1 ppm of S03, the current coal blend lead to S03 concentrations between 2 - 3 ppm downstream of the air heater (AH).
  • the products were pneumatically injected at 3, 5, and 7 lb/MMacf injection rates upstream of the electrostatic precipitator (ESP). Particulate removal was achieved with the ESP.
  • ESP electrostatic precipitator
  • Mercury concentrations were monitored at the MRC inlet and just downstream of the ESP and the observed concentrations were adjusted to 3% oxygen concentration for the purpose of standardization for comparison.
  • Total mercury removal was calculated as the inlet mercury concentration (in ug/m3 at STP and 3% 02) minus the outlet mercury concentration (in ug/m 3 at STP and 3% O2) divided by the inlet and is illustrated in Figure 12.
  • the MPAC carbons 1241, 1242, 1243, 1251, 1252, 1253, 1261, 1262, 1263 show significant advantage in higher mercury removal percentages.
  • a PAC 1231, 1232, 1233 readily available for commercial purchase in the industry (Industry Carbon), a MPAC coated with 10% Fe 3 0 4 (MPAC) 1241, 1242, 1243, with 10% Fe 3 0 4 and 1% Ti0 2 (MPAC-Ti0 2 ) 1251, 152, 1253, and another with 10% Fe 3 0 4 and 2.5% NaBr (MPAC-Na-Br) 1261, 1262, 1263 by weight.

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Abstract

La présente invention concerne un adsorbant magnétique qui comprend un adsorbant et de l'oxyde de fer implanté sur une surface de l'adsorbant, la surface totale de l'adsorbant magnétique n'étant pas sensiblement inférieure à une surface totale de l'adsorbant. Éventuellement, l'adsorbant est du charbon actif.
EP13804938.2A 2012-06-15 2013-02-20 Adsorbants magnétiques, procédés pour fabriquer un adsorbant magnétique, et procédés d'élimination de contaminants de flux de fluide Withdrawn EP2861322A4 (fr)

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CN106731388A (zh) * 2016-12-27 2017-05-31 盐城工学院 一种角型管道式超细颗粒凝并器
CN106622661B (zh) * 2016-12-27 2019-02-01 盐城工学院 一种交汇式波形变速管道凝并器
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CN106693579A (zh) * 2016-12-27 2017-05-24 盐城工学院 一种横置锚型管道式超细颗粒凝并器
CN106731432A (zh) * 2016-12-27 2017-05-31 盐城工学院 组合型管式凝并器
CN106621682A (zh) * 2016-12-27 2017-05-10 盐城工学院 一种波形变速超细颗粒凝并箱
CN106731392A (zh) * 2016-12-27 2017-05-31 盐城工学院 一种新型超细颗粒凝并器
CN107138272B (zh) * 2017-04-24 2019-08-13 航天凯天环保科技股份有限公司 一种喷涂废气磁化净化方法及装置
CN107930390B (zh) * 2017-12-15 2021-05-28 中南大学 一种光催化氧化烟气中单质汞的方法
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CA2876164A1 (fr) 2013-12-19
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