WO2005082523A1 - Adsorbants pour eliminer les cations de metaux lourds et procedes de production et d'utilisation de ces adsorbants - Google Patents

Adsorbants pour eliminer les cations de metaux lourds et procedes de production et d'utilisation de ces adsorbants Download PDF

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Publication number
WO2005082523A1
WO2005082523A1 PCT/US2004/042201 US2004042201W WO2005082523A1 WO 2005082523 A1 WO2005082523 A1 WO 2005082523A1 US 2004042201 W US2004042201 W US 2004042201W WO 2005082523 A1 WO2005082523 A1 WO 2005082523A1
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WIPO (PCT)
Prior art keywords
adsorbent
metal
group
heavy metal
oxygen
Prior art date
Application number
PCT/US2004/042201
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English (en)
Inventor
Toan Phan Vo
Mark Randall Stouffer
Original Assignee
Calgon Carbon Corporation
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Filing date
Publication date
Priority claimed from PCT/US2003/039925 external-priority patent/WO2005061099A1/fr
Priority claimed from US11/006,084 external-priority patent/US7429551B2/en
Priority claimed from US11/005,825 external-priority patent/US20050093189A1/en
Application filed by Calgon Carbon Corporation filed Critical Calgon Carbon Corporation
Publication of WO2005082523A1 publication Critical patent/WO2005082523A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • 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
    • 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
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    • 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
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    • 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
    • B01J20/08—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 comprising aluminium oxide or hydroxide; comprising bauxite
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    • B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
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    • C—CHEMISTRY; METALLURGY
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Definitions

  • the present invention relates to adsorbents for removing lead from water and to methods for producing and using these adsorbents.
  • adsorbents for removing lead from water and to methods for producing and using these adsorbents.
  • heavy metals such as lead, nickel, chromium and mercury, cadmium, etc.
  • Lead is especially a problem in drinking water because piping in water distribution systems and in older plumbing fixtures often contains lead solder.
  • the current Action Level for lead established by the United States Environmental Protection Agency (“EPA") is 15 ppb and the maximum contaminant level (“MCL”) goal is zero.
  • MCL maximum contaminant level
  • the current screening level for soil on residential properties is 400 ppm.
  • Ion exchange resins can remove metal cations.
  • TDS total dissolved solids
  • ion exchange resin is not practical in many applications due to the change in size of the media with use.
  • the present invention provides adsorbents and methods for removing heavy metals that exist as cations from the environment.
  • heavy metals include, for example, lead, copper, nickel, cobalt, cadmium, zinc, mercury and combinations thereof.
  • An adsorbent of the present invention for removing heavy metals existing in a cationic form comprises a porous media such as a carbon adsorbent wherein at least one oxygen- containing compound of a metal has been inco ⁇ orated into the adsorbent.
  • the metal is selected from the group consisting of iron, copper, aluminum, zirconium, titanium and combinations thereof. Iron is the preferred metal.
  • a preferred class of oxygen compounds is metal hydroxides.
  • metal compound or compounds are inco ⁇ orated into the carbon adsorbent by a method consisting of impregnating and/or dispersing said metal(s) in the carbon adsorbent.
  • Another embodiment of the present invention provides a method for producing a carbon adsorbent capable of removing heavy metals that comprises the steps of: (1) providing a porous carbon adsorbent; (2) inco ⁇ orating at least one compound of a metal selected from the group consisting of iron, copper, aluminum, zirconium, titanium and combinations thereof into or onto the carbon adsorbent; and (3) converting the metal- containing compound into at least one oxygen-containing compound.
  • a method for producing a carbon adsorbent capable of removing heavy metals comprising the steps of: (1) providing a carbonaceous material; (2) mixing at least one compound of a metal selected from the group consisting of iron, copper, aluminum, zirconium, titanium and combinations thereof into the carbonaceous material; (3) forming the mixture into particles of a carbonaceous material containing said metal; and (4) converting the particles of said carbonaceous material containing said metal into particles of a carbon adsorbent containing oxygen compounds of said metal(s).
  • a method for removing heavy metals comprises the steps of: (1) providing a carbon adsorbent containing a metal selected from the group consisting of iron, copper, aluminum, zirconium, titanium and combinations thereof; and (2) contacting said carbon adsorbent containing said metal with a medium containing the heavy metal cations.
  • the medium contains heavy metal cations and heavy metal anions such as, for example, arsenic, antimony and selenium.
  • the present invention provides an adsorbent material and method for removing heavy metals existing in a cationic form in various media.
  • the adsorbent material comprises a porous material wherein at least one oxygen-containing compound of a metal has been inco ⁇ orated.
  • the adsorbents have been found to overcome shortcomings of traditional carbon adsorbents.
  • the adsorbents retain a substantial amount of their porosity so that they not only remove heavy metal cations such as lead, but the present adsorbents can also remove organic materials from a surrounding medium. Some heavy metals, such as lead, exist in the environment as cations.
  • the porous material of the present invention is selected from the group consisting of activated carbon, zeolites, activated alumina, ion exchange resins, zirconia, porous silica and combinations thereof. In a preferred embodiment of the invention the porous material is activated carbon.
  • the base carbon (before metal addition) has a large surface area as measured by the Brunauer-Emmett-Teller ("BET") method, and has a substantial micropore volume.
  • BET Brunauer-Emmett-Teller
  • micropore volume is the total volume of pores having diameter less than about 2 nm.
  • Suitable carbon adsorbents for use in the present invention are those having a BET surface areas greater than about 10 m /g or about 50 m 2 /g, preferably greater than about 200 m 2 /g, and more preferably greater than about 400 m 2 /g.
  • the adsorbent has a micropore volume of greater than about 5 c VlOOg.
  • the adsorbent has a micropore volume greater than about 20 c ⁇ rVlOOg.
  • Suitable carbon adsorbents for use in the present invention may be made from any of a variety of starting carbonaceous materials, such as, but not limited to, coals of various ranks such as anthracite, semianthracite, bituminous, subbituminous, brown coals, or lignites; nutshell; wood; vegetables such as rice hull or straw; residues or by-products from petroleum processing; and natural or synthetic polymeric materials.
  • the carbonaceous material may be processed into carbon adsorbents by any conventional thermal or chemical method known in the art before at least a metal selected from the group consisting of iron, copper, aluminum, zirconium, titanium and combinations thereof is inco ⁇ orated therein.
  • the metals may be inco ⁇ orated into the carbonaceous starting material, then the mixture may be processed into carbon adsorbents containing one or more of such metals.
  • the adsorbent is in the form of granule, pellet, sphere, powder, woven fabric, non- woven fabric, mat, felt, block, and honeycomb.
  • the metal compound in the present invention is selected from the group consisting of compounds of iron, copper, aluminum, zirconium, titanium and combinations thereof.
  • the compound is an oxygen-containing compound of iron, preferably iron hydroxide.
  • at least one metal is present at a concentration of about 0.01 to about 60% of the weight of the adsorbent material.
  • the adsorbent may be disposed in a fixed bed.
  • the bed may comprise a cartridge or the like that is disposed at the point of use, for example in at a water faucet.
  • the cartridge further comprises at least one adsorbent selected from the group consisting of zeolites, ion exchange resins, silica gel, alumina, and unimpregnated activated carbons.
  • the adsorbent can be disposed in a section of a water supply piping of a house.
  • a porous adsorbent is impregnated with at least one salt of a metal selected from the group consisting of iron, copper, aluminum, zirconium, titanium and combinations thereof.
  • salts are halides, nitrates, sulfates, chlorates, and carboxylates having from one to five carbon atoms such as formates, acetates, oxalates, malonates, succinates, or glutarates of iron, copper, aluminum, zirconium, and titanium.
  • the impregnated salts are then converted to oxygen- containing compounds of iron, copper, aluminum, zirconium, and titanium. In an example of an embodiment of the present invention conversion is conducted by either thermal decomposition or chemical reaction.
  • the oxygen-containing compounds are hydroxides.
  • the adsorbent material is prepared by providing a porous adsorbent material, impregnating the porous adsorbent with an aqueous solution comprising at least one compound of at least one metal selected from the group consisting of iron, copper, aluminum, zirconium, titanium and combinations thereof. Then the at least one compound is converted into an oxygen-containing compound of said metal to produce said adsorbent, for example, by thermal decomposition or chemical reaction.
  • the method may include the further step of activating the adsorbent.
  • an alternate preparation method includes: (a) pulverizing a carbonaceous material, a binder, and at least one compound of a metal selected from the group consisting of iron, copper, aluminum, zirconium, titanium and combinations thereof; (b) making a pulverized mixture comprising said carbonaceous material, said binder, and said at least one compound of said metal; (c) compacting the powdered mixture into shaped objects, such as briquettes or pellets; (d) crushing and screening the shaped objects into a metal- containing particulate material; and (e) gasifying said metal-containing particulate material to produce said adsorbent.
  • EXAMPLE 1 To prepare an iron impregnated carbon, 110 grams of anhydrous ferric chloride were dissolved in 73 ml of deionized water. This solution was added to 300 grams of 12x40 mesh (U.S. sieve series) coal based activated carbon identified as HIPUR (Barnebey Sutcliffe Co ⁇ oration, Columbus, Ohio). The carbon had a BET surface area of 1030 m /gram. The carbon was mixed thoroughly until all the solution was adsorbed completely. A 50% solution of NaOH was prepared with 110 grams of solid NaOH plus 110 ml of deionized water.
  • Example 2 To test the iron-impregnated carbon capability for lead removal, the carbon produced in Example 1 was placed in a 9" X 2.5" filter cartridge, such as used for household water purification. A 150 ppb solution of lead in water was prepared from lead nitrate according to NSF 53 protocol. The water characteristics were also adjusted to a pH of 8.5 + .25.
  • the inlet water flow was set at 0.5 gpm and remained constant through the duration of the experiment. Effluent samples were taken at various intervals and analyzed for lead content by GFAA. The detection limit for this method was below 1 ppb. The results of this filter test are shown in Table A below. As shown, the iron hydroxide impregnated carbon reduced lead to below the EPA action level for over 660 gallons of water treated. This result was su ⁇ risingly positive; standard granular activated carbon is not capable of removing lead to acceptable levels at the condition of this test. Commercially available adsorbents that can achieve similar performance (e.g, Engelhard ATC Granules) are very expensive. Table A
  • EXAMPLE 3 The same coal based activated carbon used in Example 1 was impregnated in the same manner except at an impregnation level of 10 g iron hydroxide per 100 g carbon. Lead removal capability of the impregnated carbon was tested following the same experimental procedure that was used in Example 2. Table B shows the results below. The data show that the carbon successfully removed lead to below the EPA action level for about 420 gallons water treated. However, the lead removal capability was not as great as for a carbon with more iron impregnant (Example 1). Table B
  • EXAMPLE 4 A coconut based activated carbon (1135 m /g surface area)was impregnated with iron using the same manner as Example 1 to achieve an impregnation level of 10% by weight (10 g iron hydroxide per 100 g virgin carbon). The same coconut carbon was impregnated at a level of 15% by weight following the same procedure. The test procedures and water characteristics were the same as in Examples 2 and 3 above. Tables C and D below show the results obtained. Table C represents the 10% loading while table D shows data for the 15% impregnation level. These data show that lead removal can be achieved with an activated carbon with a different base material. Again, the higher iron impregnation level yields an adsorbent with higher lead capacity. Table C
  • Example 5 A surface modified coconut base carbon identified as MCAT (Barnebey Sutcliffe Co ⁇ oration, Columbus, Ohio) was impregnated as in Example 1 but with an impregnation level of 15%. Another coconut base carbon was impregnated at the 7.5% by weight of carbon.
  • the test methods and water characteristics were the same Examples 2 and 3.
  • the tables below show the results obtained with Table E representing the 15% sample and Table F represents the 7.5%). Again, the data show an increase in capacity with a higher level of iron impregnation. Table E
  • EXAMPLE 7 Three separate 20x50 mesh (U.S. Sieve Series) iron impregnated samples were prepared the same as above with different impregnation levels or a different carbon base materials.
  • the comparison media for these experiments was Engelhard Co ⁇ oration' s lead removal media called ATC 20x50 mesh (U.S. Sieve Series). This material compared with the iron impregnated carbons because of its known and documented capability for lead removal in commercial applications. All variables of the experiment remained the same as above examples, except the filters were tested with a 15 minute on/off cycle with an 8 hour rest period for every 24 hours. This criterion was derived from NSF certification protocol for home water filters.
  • Table I shows the data gathered for the ATC material while Table J shows data for a 10% iron impregnated coconut based carbon.
  • Table K shows the data for a 20% impregnation by carbon weight with the base material identified as CPG (Calgon Carbon Co ⁇ oration, Pittsburgh, Pennsylvania).
  • Table L shows a 10% impregnation level with a base material previously identified as MCAT (Bamebey Sutcliffe Co ⁇ oration, Columbus, Ohio). The data demonstrate that the iron impregnated carbons can give lead removal performance similar to that of state-of-the art commercial media for lead removal. Table I
  • EXAMPLE 8 A sample of carbon identified as DCL 1240 (Bamebey Sutcliffe Co ⁇ oration, Columbus, Ohio) was impregnated with 50% FeOOH by carbon weight using the procedure of Example 1.
  • the DCL carbon had a high total pore volume (1200 Iodine Number, > 400 Molasses Number). This allowed inco ⁇ oration of high levels of iron hydroxide.
  • EXAMPLE 9 The media prepared in Example 8 was tested for removal of arsenic from water.
  • the challenge water was prepared per NSF 53 high pH protocol.
  • the arsenic concentration was obtained by adding sodium arsenate to the water for an approximate theoretical concentration of 100 ppb.
  • the analysis was performed by GFAA with a detection limit of less than 1 ppb.
  • Table M shows the data generated. The data demonstrate that the iron-impregnated media can be effective for removal of metal anions, as well as metal cations, thus providing a multi-pu ⁇ ose metal adsorbent. Table M
  • EXAMPLE 10 Testing was conducted to determine removal of metals other than lead and arsenic.
  • a carbon impregnated with 30% ferric hydroxide was prepared in the same manner as previous examples with ACL carbon used as the base material.
  • a 9" filter was filled with this material while another filter was filled with virgin (un-impregnated) 20x50 ACL for comparison.
  • the challenge solution was comprised of deionized water with the addition of sodium selenite, nickel chloride, zinc nitrate, mercury nitrate, cupric sulfate and sodium cobaltinitrite. The amount of each chemical added to the water to give ca. 100 ppb concentration of each metal in solution. Water flow was set at 0.25 gpm (continuous). Several effluent samples were taken and analyzed by ICP-MS with the results shown below. Table M gives the results for the impregnated carbon while Table N lists the results of the virgin ACL material. Table M (Iron-Impregnated Carbon)

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Abstract

La présente invention concerne des adsorbants et des procédés visant à éliminer des cations de métaux lourds d'un milieu. Ces adsorbants comprennent un support poreux auquel est incorporé au moins un composé oxygéné de fer, cuivre, aluminium, zirconium, titane, et certaines de leurs combinaisons. Ce composé oxygéné peut être incorporé au support poreux para imprégnation ou dispersion d'un précurseur approprié d'un tel composé. Le précurseur peut être traité plus avant pour donner le composé oxygéné. De tels adsorbants, qui conviennent particulièrement pour éliminer de l'environnement des cations de plomb et/ou d'autres métaux, conviennent pour traiter les sources d'eau potable.
PCT/US2004/042201 2003-12-16 2004-12-16 Adsorbants pour eliminer les cations de metaux lourds et procedes de production et d'utilisation de ces adsorbants WO2005082523A1 (fr)

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US11/006,084 US7429551B2 (en) 2001-08-27 2004-12-07 Adsorbents for removing heavy metals
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EP2127740A4 (fr) * 2007-01-09 2011-06-08 Badulin Nikolay Aleksandrovich Procédé de décontamination d'eau contenant des ions de métaux lourds
WO2009123725A1 (fr) * 2008-04-03 2009-10-08 Corning Incorporated Procédé et système permettant la sorption de contaminants en trace en phase liquide ou vapeur à partir d'un courant de fluide contenant une particule chargée électriquement
WO2011017768A1 (fr) * 2009-08-13 2011-02-17 Water Harvesting Technologies Pty Ltd Australia Système de filtration d'eau avec charbon actif et zéolithe
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US10336629B2 (en) 2011-12-16 2019-07-02 Helen Of Troy Limited Gravity filter
US9994461B2 (en) 2011-12-16 2018-06-12 Helen Of Troy Limited Gravity filter
JPWO2016199385A1 (ja) * 2015-06-09 2018-02-22 パナソニックＩｐマネジメント株式会社 金属材料凝集促進層、及びそれを用いた水処理装置
CN105384209A (zh) * 2015-10-30 2016-03-09 安徽炭之馨环保科技有限公司 一种活性炭水质净化复合材料及其制备方法和用途
CZ307602B6 (cs) * 2017-11-06 2019-01-02 Unipetrol výzkumně vzdělávací centrum, a.s. Nanoadsorbent na bázi hydratovaných oxidů hliníku, železa a manganu pro odstraňování arsenitanů a arseničnanů z vod, způsob jeho výroby a použití
CN109603745A (zh) * 2018-11-15 2019-04-12 西安建筑科技大学 一种强吸附型生物炭制备及用于含镍电镀废水处理的应用
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WO2023114807A1 (fr) * 2021-12-16 2023-06-22 Ionic Water Technologies, LLC Traitement de carbone pour l'élimination de contaminants

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