WO2005061099A1 - Adsorbents for removing heavy metals and methods for producing and using the same - Google Patents
Adsorbents for removing heavy metals and methods for producing and using the same Download PDFInfo
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- WO2005061099A1 WO2005061099A1 PCT/US2003/039925 US0339925W WO2005061099A1 WO 2005061099 A1 WO2005061099 A1 WO 2005061099A1 US 0339925 W US0339925 W US 0339925W WO 2005061099 A1 WO2005061099 A1 WO 2005061099A1
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- adsorbent
- metal
- carbon
- group
- oxygen
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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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
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- 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
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- 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
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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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- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B01J20/28042—Shaped bodies; Monolithic structures
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- B01J20/2808—Pore diameter being less than 2 nm, i.e. micropores or nanopores
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- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
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- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- 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
- B01J20/3204—Inorganic carriers, supports or substrates
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
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- C02F2307/00—Location of water treatment or water treatment device
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Definitions
- the present invention relates to adsorbents for removing heavy metals from a medium adjacent thereto and methods for producing and using the same.
- the present invention relates to adsorbents for removing arsenic and/or selenium from a medium adjacent thereto and methods for producing and using the same.
- MCL mellitus fibroblasts
- MCL melatonin-containing styrene-containing styrene-containing styrene-containing styrene-containing styrene-containing styrene-containing styrene-containing styrene-containing styrene-containing styrene-containing styrene-containing sta, liver, lung, kidney, and bladder cancer.
- Over exposure to selenium has been shown to have undesired effects on the nervous system and to contribute to the cause dyspnea, bronchitis, and gastrointestinal disturbance.
- adsorption of arsenic on alumina is seriously compromised when other ions are present, such as selenium, fluoride, chloride, and sulfate.
- ion exchange adsorbents can remove arsenic, but sulfate, total dissolved solids ("TDS"), selenium, fluoride, and nitrate also compete with arsenic for the ion exchange capacity, thus decreasing likely effectiveness.
- An adsorbent comprises a carbon adsorbent having at least one oxygen-containing compound incorporated therein wherein said oxygen-containing compound is of a metal selected from the group consisting of iron, copper, and aluminum.
- the oxygen-containing compound of a metal is selected from the group consisting of oxides and hydroxides.
- the oxygen-containing compound of a metal is inco ⁇ orated into the carbon adsorbent by a method of impregnating or dispersing at least a compound of said metal in the carbon adsorbent.
- Another embodiment of the present invention provides a method for producing a carbon adsorbent capable of removing heavy metals that exist as anions.
- the method comprises the steps of: (1) providing a carbon adsorbent; (2) impregnating the adsorbent with at least one compound of a metal selected from the group consisting of iron, copper, and aluminum or combinations thereof; and (3) converting said compound into at least one oxygen-containing compound.
- the method comprises 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, and aluminum or combinations thereof into the carbonaceous material to produce a mixture of said carbonaceous material and said metal; (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 said metal.
- a carbon adsorbent of the present invention for use in removing metal anions from a liquid or gas medium may be made by: (1) pulverizing a carbonaceous material, a binder, and at least one compound of a metal selected from the group consisting of iron, copper, and aluminum or combinations thereof to form a powdered mixture; (2) compacting said powdered mixture into shaped objects; and (3) crushing and screening the shaped objects into a metal-containing particulate material to produce said carbon adsorbent.
- the carbonaceous material, binder and metal compound is pulverized together or, alternatively, the carbonaceous material, binder and metal compound are pulverized separately before making the pulverized mixture.
- the compacting is accomplished by briquetting, pelletizing, densifying or extruding processes.
- the method may also have an additional step four comprising gasifying said metal containing particulate material to produce said carbon absorbent.
- the gasifying of step four is conducted under an atmosphere comprising an oxygen-containing gas at a temperature in a range from about 900° C to about 1100° C for a time sufficient to produce an adsorbent having a BET surface area of at least 100 m 2 /g.
- the method may also comprise the additional step of oxidizing said metal-containing particulate material before the step of gasifying.
- the method for removing heavy metals that exist as anions comprises the steps of: (1) providing a carbon adsorbent containing a metal selected from the group consisting of iron, copper, and aluminum; and (2) contacting said carbon adsorbent containing said metal with a medium containing the heavy metal anions.
- the medium may be a liquid or gas phase in which the metals exist as anions.
- the medium is drinking water.
- the present invention provides an adsorbent for removing heavy metal from a medium that comprises a carbon having at least one oxygen-containing compound of a metal incorporated therein, wherein said metal is selected from the group consisting of iron, copper, and aluminum.
- adsorbent for removing heavy metal from a medium that comprises a carbon having at least one oxygen-containing compound of a metal incorporated therein, wherein said metal is selected from the group consisting of iron, copper, and aluminum.
- the present invention provides carbon adsorbents that overcome this shortcoming of traditional carbon adsorbents by incorporating at least an oxygen-containing compound of a metal selected from the group consisting of iron, copper, and aluminum into a porous carbon. It is contemplated that these and similar metals having metal oxides or hydroxides which are stable in liquid phase would work in the present invention.
- the carbon adsorbents of the present invention retain a substantial amount of their microporosity enabling them to remove heavy metal anions such as arsenic and selenium anions as well as organic materials from the surrounding medium such as liquid or gas. In a preferred embodiment, the medium is drinking water.
- a metal-containing carbon adsorbent of the present invention is preferably a microporous carbon adsorbent, which has a large surface area as measured by the Brunauer-Emmett-Teller ("BET") method and has a substantial micropore volume for pores having diameter less than about 2 nm.
- BET Brunauer-Emmett-Teller
- micropore volume is the total volume of pores having diameter less than 2 nm.
- Suitable carbon adsorbents for use in the present invention are those having a BET surface area greater than about 100 m 2 /g, preferably greater than about 200 m 2 /g, more preferably greater than about 400 m 2 /g, and most preferably greater than about 600 m /g.
- the higher surface areas will capture metal anions and other contaminants, especially organics.
- These carbon adsorbents typically have a micropore volume greater than about 20 cm 3 /100g.
- the carbon adsorbents have a micropore volume greater than about 30 cm /100g, more preferably greater than about 40 cm /100g, and most preferably greater than about 50 cm 3 /100g.
- 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 incorporating the metal therein. They will inherently impart different surface areas and pore volumes.
- lignites can result in carbon having surface areas about 500-600 m 2 /g and, typically, fiber-based carbons areas are about 1200-1400 m 2 /g.
- Certain wood-based carbons may have areas in the range of about 200 m 2 /g, but tend to have a very large pore volume which is generally suitable for depositing large amounts of impregnates.
- Surface area and pore volume of coal based carbon may also be made to allow for some control of surface area and pore volumes.
- the carbon is an activated carbon adsorbent.
- at least one metal may be incorporated into the carbonaceous starting material, then the mixture may be processed into carbon adsorbents containing one or more of such metals.
- the carbon adsorbent contains metal at a concentration of up to about 50% by weight of the carbon.
- the metal is present at a concentration in the range from about 1% to about 40% or, more preferably, from about 2% to about 30% and, more preferably, from about 3% to about 20% by weight of the carbon.
- a microporous carbon adsorbent is impregnated with at least one salt of a metal selected from the group consisting of iron, copper, and aluminum.
- salts include halides, nitrates, sulfates, chlorates, carboxylates having from one to five carbon atoms such as formates, acetates, oxalates, malonates, succinates, or glutarates of iron, copper, or aluminum.
- the impregnated salts are then converted to oxygen-containing compounds of iron, copper, or aluminum by either thermal decomposition or chemical reaction.
- Preferred forms of the oxygen-containing compounds are hydroxides and oxides.
- the wet impregnated carbon was dried in an oven at 105° C for 2 hours based on the amount of ferric chloride solution used for the impregnation.
- the dried impregnated carbon had an iron content of about 7.9 % by weight of the carbon.
- the dried impregnated carbon was taken out of the oven and cooled down in a hood.
- a KOH solution was prepared by dissolving 12.47 g of KOH pellets in 60.02 g deionized water.
- the KOH solution was poured into the dried impregnated carbon. This amount of KOH was enough to completely wet the impregnated carbon without leaving an excess solution.
- the wet KOH-treated carbon was transferred into a 2000-ml beaker and the beaker was filled with deionized water.
- the water from the beaker was decanted and fresh deionized was added to wash potassium chloride from the impregnated carbon. This process of washing was repeated until the pH of the solution was about 7, as indicated by pH paper.
- the wet carbon was then dried in an oven at 105° C overnight. It was expected that the iron in the carbon would be in the form of ferric hydroxide.
- the dried ferric hydroxide-impregnated carbon was pulverized in a titanium vial containing tungsten abrading balls for testing of the removal of heavy metal anions. This impregnated carbon was identified as "3224-31-1.” Testing of Arsenic Removal:
- aqueous arsenic solution having an arsenic concentration of about 100 parts per billion (“ppb") by weight was prepared for testing by diluting into deionized water an appropriate amount of an arsenic standard solution of arsenic trioxide in 10 % (by weight) nitric acid.
- Polyethylene bottles having a nominal volume of 500 ml and magnetic stirring bars were cleaned with dilute nitric acid solution and dried.
- An appropriate amount of the pulverized impregnated carbon adsorbent 3224-31-1, as disclosed above, was put into a cleaned and dried polyethylene bottle containing a magnetic stirring bar.
- An amount of about 500 g of the arsenic solution prepared as disclosed above was put into the bottle.
- the bottle was then put on a multi-position stirring plate and the stirring continued for about 24 hours. At the end of the 24-hour period, a sample of the solution in the bottle was taken and filtered. The residual concentration of arsenic in the solution was analyzed by ICP/MS method. Many such bottles were prepared during the same experiment, each had a different amount of pulverized carbon adsorbent. In addition, a control bottle was also prepared in which no carbon adsorbent was added. The results of this testing are shown in Table 1 A below. The limit of detection for this method of analysis was 0.3 ppb. This carbon could reduce the level of arsenic to less than detection limit with a small dose of the carbon.
- activated carbons suitable for the present invention may be those made from wood chips in a chemical activation process employing phosphoric acid, or those made from phosphoric acid treatment of petroleum residue, or activated carbons made from gasification of carbonized polymeric materials, such as those derived from phenolic resins or polyesters.
- Activated carbons suitable for the present invention may have the form of powder, granule, sphere, pellet, honeycomb, woven or nonwoven fiber, mat, or felt.
- An iron (II) impregnated activated carbon was prepared similarly to the process disclosed in Example 1, except a ferrous chloride solution was prepared for impregnation, instead of ferric chloride. 1.778g of FeCl -4H O was dissolved into 40.0 g of deionized water. The ferrous chloride solution was impregnated into 50.0 g of oven-dried 12x30 mesh PCBTM activated carbon. The dried impregnated carbon had a nominal iron (II) loading of about 1% by weight. The dried impregnated carbon was reacted with a KOH solution consisting essentially of 1.27 g of KOH pellet dissolved in 70.16 g of deionized water. The washed and dried impregnated carbon was pulverized as above and labeled as "3224-32-1" for testing.
- Oven-dried 12x30 PCBTM activated carbon was impregnated with aluminum chloride in the same manner as disclosed in Example 1.
- the aluminum chloride solution was prepared by dissolving 89.48 g of AlCl 3 -6H O in 80.0 g of deionized water.
- the solution was impregnated into 100 g of oven-dried 12x30 PCBTM activated carbon.
- the impregnated carbon has an aluminum loading of about 10% by weight of the carbon.
- the aluminum chloride-impregnated carbon was reacted with a solution containing 63.17 g KOH in 120 g deionized water.
- the steps of washing, drying, and pulverizing were the same as those of Example 1.
- An arsenic solution having a targeted As concentration of about 1 ppm was prepared for testing.
- the arsenic removal testing was the same as that disclosed in Example 1 except different amounts of impregnated carbon were used. The results are shown in Table 4. Table 4
- the heating was conducted under a flow of nitrogen at substantially ambient pressure at about 300 cm 3 /minute.
- the tube with the carbon still inside was cooled down under nitrogen flow to ambient temperature. It was expected that ferric nitrate decomposed to ferric oxide under this treatment condition.
- a representative sample of the ferric oxide-loaded carbon was pulverized as described in Example 1 above for testing. The results of the testing are shown in Table 5. The results show that arsenic was removed even at low doses of carbon. Table 5
- the mixture also may be extruded into pellets instead of the above pressing to briquettes.
- the compaction pressure may be appropriately chosen for the particular coal used. It may be higher or lower than the pressure disclosed above, but typically is in the range from about 8 MPa to about 16 MPa.
- the briquettes were crushed and screened to produced particles having a mesh size of about 6x14. The produced particles were oxidized under an excess flow of air in an indirectly heated rotary kiln, the temperature of which was increased from ambient to about 250° C at a rate of 45° C per hour, and then from 250° C to about 450° C at a rate of 60° C per hour.
- oxidizing gases such as a mixture of oxygen and air or an inert gas, which mixture has an oxygen concentration greater than about 21% by volume, or a combustion product from a combustor containing oxygen, steam, and other gases.
- oxidizing gases such as a mixture of oxygen and air or an inert gas, which mixture has an oxygen concentration greater than about 21% by volume, or a combustion product from a combustor containing oxygen, steam, and other gases.
- the resulting oxidized iron-containing coal particulate material was gasified in steam at 925- 950° C for about 40-45 minutes to produce an iron-containing porous carbon adsorbent of the present invention.
- activation The step of gasifying the carbon precursor, such as this coal particulate, in an oxidizing atmosphere is usually termed "activation.”
- activation temperature and time are chosen to be appropriate for the type of coal, the compaction technique, the type of activation furnace used in the process of manufacture, and the desired microporosity of the activated product.
- higher-rank coals and higher compaction would require a higher temperature and/or a longer time.
- a longer activation time produces a more porous activated carbon.
- Activation furnace types that provide a very intimate contact between the solid and the gas phase and a well-mixed solid therein usually require a shorter activation time.
- Activation temperature is typically in the range from about 900° C to about 1100° C, and activation time is typically in the range from about 10 minutes to about 10 hours.
- other oxygen-containing gases may also be present.
- the steps of oxidizing the coal particles and of gasifying the oxidized coal particles were carried out in this example in a rotary kiln.
- furnaces or kilns may also be used in which an intimate contact between the solid and the gas phase can be maintained. Suitable furnaces or kilns are fluidized-bed kilns, belt furnaces, and Herreshoff furnaces. A representative sample of this adsorbent was pulverized in titanium vials using tungsten balls as disclosed above for testing.
- Example 1 The carbon of Example 1 was tested for selenium removal.
- a solution containing selenium was prepared as follows.
- aqueous selenium solution having a selenium concentration of about 300 parts per billion by weight was prepared for testing by diluting into Milli-Q water an appropriate amount of a 1000 ppm selenium standard reference solution.
- the reference solution was purchased from Fisher Scientific and is commonly used as the standard solution for atomic absorption spectroscopy.
- Example 5 The carbon of Example 5 was tested for selenium removal.
- the solution containing selenium was prepared as described in Example 7.
- Example 4 The carbon of Example 4 was tested for selenium removal.
- a solution containing selenium was prepared to have a target selenium concentration of about 300 ppb by diluting a selenium atomic absorption standard solution containing 100 ppm selenium dioxide in water.
- the adsorbents of the present invention may be used to remove heavy metal anions from a medium adjacent thereto in many arrangements.
- Granular particles of the adsorbents of the present invention may be installed in a fixed bed or a fluidized bed.
- Granular adsorbents are particularly suitable to be packaged in small cartridges for installation at the point of use.
- An adsorbent in powder form may be injected into a stirred tank and then removed by filtration or settling.
- Adsorbents in fiber form may be inserted in a section of the water supply piping.
- adsorbents are, for example, zeolites, ion exchange resins, silica gel, alumina, and unimpregnated activated carbons. While various embodiments are described herein, it will be appreciated from the specification that various combinations of elements, variations, equivalents, or improvements therein may be made by those skilled in the art, and are still within the scope of the invention as defined in the appended claims.
Abstract
Description
Claims
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AU2003300942A AU2003300942A1 (en) | 2003-12-16 | 2003-12-16 | Adsorbents for removing heavy metals and methods for producing and using the same |
PCT/US2003/039925 WO2005061099A1 (en) | 2003-12-16 | 2003-12-16 | Adsorbents for removing heavy metals and methods for producing and using the same |
PCT/US2004/042434 WO2005082524A1 (en) | 2003-12-16 | 2004-12-16 | Method for removing contaminants from fluid streams |
PCT/US2004/042191 WO2005058482A1 (en) | 2003-12-16 | 2004-12-16 | Adsorbents for removing heavy metals and methods for producing and using the same |
PCT/US2004/042201 WO2005082523A1 (en) | 2003-12-16 | 2004-12-16 | Adsorbents for removing heavy metal cations and methods for producing and using these adsorbents |
US11/014,892 US7429330B2 (en) | 2001-08-27 | 2004-12-16 | Method for removing contaminants from fluid streams |
US11/014,295 US20050247635A1 (en) | 2001-08-27 | 2004-12-16 | Adsorbents for removing heavy metal cations and methods for producing and using these adsorbents |
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US11/014,892 Continuation-In-Part US7429330B2 (en) | 2001-08-27 | 2004-12-16 | Method for removing contaminants from fluid streams |
US11/014,295 Continuation-In-Part US20050247635A1 (en) | 2001-08-27 | 2004-12-16 | Adsorbents for removing heavy metal cations and methods for producing and using these adsorbents |
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