WO2022047504A1 - Copper, iron, and nitrogen treated sorbent and method for making same - Google Patents

Copper, iron, and nitrogen treated sorbent and method for making same Download PDF

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Publication number
WO2022047504A1
WO2022047504A1 PCT/US2021/071328 US2021071328W WO2022047504A1 WO 2022047504 A1 WO2022047504 A1 WO 2022047504A1 US 2021071328 W US2021071328 W US 2021071328W WO 2022047504 A1 WO2022047504 A1 WO 2022047504A1
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WIPO (PCT)
Prior art keywords
copper
activated carbon
iron
source
precursor activated
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.)
Ceased
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PCT/US2021/071328
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English (en)
French (fr)
Inventor
Jason P. Mazzoccoli
Ryan W. WALKER
Walter G. Tramposch
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Calgon Carbon Corp
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Calgon Carbon Corp
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Publication date
Application filed by Calgon Carbon Corp filed Critical Calgon Carbon Corp
Priority to CA3188226A priority Critical patent/CA3188226A1/en
Priority to KR1020237010898A priority patent/KR20230062593A/ko
Priority to EP21863031.7A priority patent/EP4204127A4/en
Priority to CN202180053096.6A priority patent/CN116096478A/zh
Priority to JP2023509859A priority patent/JP7828707B2/ja
Priority to MX2023002245A priority patent/MX2023002245A/es
Publication of WO2022047504A1 publication Critical patent/WO2022047504A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • B01J20/28011—Other properties, e.g. density, crush strength
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
    • B01J20/0229—Compounds of Fe
    • 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
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0233—Compounds of Cu, Ag, Au
    • B01J20/0237—Compounds of Cu
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0259—Compounds of N, P, As, Sb, Bi
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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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
    • 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
    • B01J20/20—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
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • 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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    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3234—Inorganic material layers
    • B01J20/3236—Inorganic material layers containing metal, other than zeolites, e.g. oxides, hydroxides, sulphides or salts
    • 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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/18—Carbon
    • 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
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24—Nitrogen compounds
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0201—Impregnation
    • B01J37/0203—Impregnation the impregnation liquid containing organic compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/082—Decomposition and pyrolysis
    • B01J37/088—Decomposition of a metal salt
    • 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
    • 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
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/42—Materials comprising a mixture of inorganic materials
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4881—Residues from shells, e.g. eggshells, mollusk shells
    • C—CHEMISTRY; METALLURGY
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    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/12—Halogens or halogen-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/16—Nitrogen compounds, e.g. ammonia
    • C—CHEMISTRY; METALLURGY
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    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
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    • C02F2101/322—Volatile compounds, e.g. benzene
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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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
    • C02F2303/00—Specific treatment goals
    • C02F2303/04—Disinfection
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2303/00—Specific treatment goals
    • C02F2303/18—Removal of treatment agents after treatment
    • C02F2303/185—The treatment agent being halogen or a halogenated compound

Definitions

  • Fluids such as water are routinely disinfected by adding oxidizing compounds, irradiating the water with ultraviolet radiation, or both. While these techniques are effective at disinfecting the water, the disinfected water will often include the oxidizing compounds themselves, products of the oxidizing compounds as they dissolve in the water, or reaction compounds that result from the irradiation of the water that contains various constituent compounds.
  • these various compounds include chlorine, chloramines, chloroform, trihalomethanes, haloacetic acids, organic peroxides, and hydrogen peroxides. These compounds are undesired because they alter the smell and taste of the water, cause health problems, and can cause corrosion of mains and service lines. [0003] To remove these compounds, sorbents have been used. The sorbents absorb and adsorb the various compounds. In particular, the pores of sorbents permit the adsorption of the compounds. However, pure sorbents are inefficient and only adsorb a fraction of the compounds that must be removed. To increase their effectiveness, the sorbents are sometimes treated with compounds to form catalytic sorbent.
  • Catalytic species are usually present on the surface of the sorbent particles and function by catalyzing the chemical decomposition of those undesired compounds that adsorb or absorb poorly on the sorbent.
  • a catalytic sorbent is significantly more efficient than a pure, untreated sorbent.
  • Catalytic sorbents have proven effective for removing chlorine, chloramines, chloroform, trihalomethanes, haloacetic acids, organic peroxides, and hydrogen peroxides from water and other fluids. Even so, there remains a continued need to improve the various steps of forming such catalytic sorbents, and thereby improve overall sorbent performance.
  • a sorbent material formed from a carbonaceous material that is activated to form a precursor activated carbon comprising: about 2 wt.% to about 20 wt.% nitrogen as measured on a dry precursor activated carbon basis; about 0.1 wt.% to about 4 wt.% iron and copper as measured on a dry precursor activated carbon basis; wherein the sorbent material has a chloramine destruction number (CDN) of about 5 to about 75.
  • CDN chloramine destruction number
  • the chloramine destruction number is about 20 to about 75.
  • the sorbent material has a peroxide number of less than about 20 minutes.
  • the sorbent material has a peroxide number of about 1 minute to about 10 minutes.
  • the amount of nitrogen is about 2.5 wt.% to about 5 wt.%.
  • the amount of nitrogen is about 1.4 wt.% to about 3.0 wt.%.
  • the sorbent material is formed from a carbonaceous material that is formed from one or more of coal, wood, and coconut.
  • At least part of the carbonaceous material is formed from coconut.
  • the weight ratio of iron and copper is about 25:75 to about 75:25.
  • the weight ratio of iron and copper is about 50:50.
  • a method of manufacturing a sorbent material comprising: providing a carbonaceous material; activating the carbonaceous material to form a precursor activated carbon; optionally oxidizing the precursor activated carbon; doping the precursor activated carbon by contacting the precursor activated carbon with one or more compounds that are a copper source, an iron source, and a nitrogen source to thereby form a doped precursor activated carbon; calcining the doped precursor activated carbon by heating to a temperature of at least about 950°C in a calcining atmosphere that does not cause any substantial oxidation or activation of the doped precursor activated carbon to thereby form a sorbent material.
  • a single compound is the copper source, the iron source, and the nitrogen source.
  • a first compound is the copper source and the iron source, and a second compound is the nitrogen source.
  • a first compound is the copper source and the nitrogen source, and a second compound is the iron source.
  • a first compound is the iron source and the nitrogen source, and a second compound is the copper source.
  • a first compound is the copper source, a second compound is the iron source, and a third compound is the nitrogen source.
  • doping the precursor activated carbon is performed in a single stage process, the single stage process including contacting the precursor activated carbon in an aqueous solution that contains the copper source, the iron source, and the nitrogen source.
  • the copper source is one or more of copper(II) sulfate pentahydrate (CuSO 4 . 5H 2 O), copper(II) chloride (CuCl 2 ), copper(II) chloride dihydrate (CuCl 2 . 2H 2 O), copper(II) nitrate (Cu(NO 3 ) 2 ), copper(II) nitrate monohydrate (Cu(NO 3 ) 2 .
  • the iron source is one or more of iron(III) chloride hexahydrate (FeCl 3 ⁇ 6H 2 O), iron(II) chloride tetrahydrate (FeCl 2 ⁇ 4H 2 O), ammonium iron(III) sulfate dodecahydrate (NH 4 Fe(SO 4 ) ⁇ 12H 2 O), iron(II) sulfate heptahydrate (Fe 2 SO 4 ⁇ 7H 2 O), ammonium
  • calcining is performed at a temperature of about 800°C to about 1050°C in a N 2 atmosphere.
  • the oxidizing is required and is performed.
  • the oxidizing is not performed.
  • the copper source is copper(II) sulfate pentahydrate (CuSO 4 . 5H 2 O)
  • the iron source is iron(III) chloride hexahydrate (FeCl 3 ⁇ 6H 2 O)
  • the nitrogen source is one or more of urea or dicyandiamide (DCD).
  • calcining is performed at a temperature of about 400°C to about 1050°C in a N 2 atmosphere. [0028] In another embodiment, calcining is performed at a temperature of about 925°C to about 975°C in a N 2 atmosphere.
  • a method of removing chlorine, chloramine, or both chlorine and chloramine from a fluid comprising: providing a sorbent material, the sorbent material being formed from a carbonaceous material that is activated to form a precursor activated carbon, said sorbent material comprising about 2 wt.% to about 20 wt.% nitrogen as measured on a dry precursor activated carbon basis, about 0.1 wt.% to about 4 wt.% iron and copper as measured on a dry precursor activated carbon basis, and wherein the sorbent material has a chloramine destruction number (CDN) of about 5 to about 75; and contacting the sorbent material with a fluid.
  • the fluid is liquid water.
  • FIG.1 depicts a process in accordance with an embodiment.
  • FIG.2 depicts a process in accordance with an embodiment.
  • FIG.3 depicts a process in accordance with an embodiment.
  • FIG.4 depicts the CDN and peroxide number versus varying nitrogen content for Cu-Fe-N doped OLC.
  • FIG.5 depicts the CDN versus added metal loading with oxidized OLC.
  • FIG.6 depicts the peroxide number versus added metal loading with oxidized OLC.
  • FIG.7 depicts the CDN of Cu-N, Fe-N, or Cu-Fe-N doped oxidized OLC versus added nitrogen content.
  • FIG.8 depicts the CDN and peroxide number versus varying nitrogen content for Cu-Fe-N doped unoxidized OLC.
  • FIG.9 depicts the CDN versus added metal loading with unoxidized OLC.
  • FIG.10 depicts the peroxide number versus added metal loading with unoxidized OLC. DETAILED DESCRIPTION [0043] This disclosure is not limited to the particular systems, devices and methods described, as these may vary.
  • the term “comprising” means “including, but not limited to.” [0045] As used herein, the term “about” means plus or minus 10% of the numerical value of the number with which it is being used. Therefore, about 50% means in the range of 45%-55%. [0046] As used herein, the term “sorbent material” means any material that exhibits adsorbent properties, absorbent properties, or a combination of adsorbent properties and absorbent properties. Adsorbent properties mean that atoms, ions, or molecules physically adhere to the surface of the material. Absorbent properties means that atoms, ions, or molecule enter and are retained by a bulk phase of the material.
  • sorbent materials include activated carbon, reactivated carbon, natural and synthetic zeolite, silica, silica gel, alumina, zirconia, and diatomaceous earths.
  • sorbent material is a material whose constituent components are substantially adsorbent and/or absorbent, with only minimal components that are not adsorbent and/or absorbent (for example, the minimal amount of binder that is required for activated carbon pellets to maintain their shape).
  • the term “sorbent” means any composition or composite that includes a sorbent material in a blend, mixture, composite, or compound with one or more additional materials that do not exhibit adsorbent properties.
  • one embodiment of sorbent includes an activated carbon sorbent material mixed with a thermally conductive filler.
  • carbonaceous material means a material that contains carbon that has not been thermally activated or chemically activated. Carbonaceous material may have been mechanically treated, thermally treated, or chemically treated, and can even have weakly sorbent properties, but carbonaceous material does not adsorb compounds in substantial amounts as would be expected of a material such as activated carbon.
  • carbonaceous material examples include but are not limited to bituminous coal, sub-bituminous coal, lignite coal, anthracite coal, wood, wood chips, sawdust, peat, nut shells, pits, coconut shell, babassu nut, macadamia nut, dende nut, peach pit, cherry pit, olive pit, walnut shell, wood, lignin, polymers, nitrogen-containing polymers, resins, petroleum pitches, bagasse, rice hulls, corn husks, wheat hulls and chaff, graphenes, carbon nanotubes, or polymer fibers.
  • the term “disinfection byproduct” means a compound that is formed as a result of chemical reactions between organic and inorganic matter found in water and the chemical compounds that are used during the disinfection process, or a compound that is formed as a result of the irradiation of organic and inorganic matter found in water by ultraviolet radiation.
  • disinfection byproducts include one or more of chlorine, chloramines, chloroform, trihalomethanes, haloacetic acids, organic peroxides, and hydrogen peroxides. It should be noted, however, that it is possible for compounds that are disinfection byproducts to be present in water that has not undergone a disinfection process.
  • the term “macropores” means pores within a sorbent that are greater than about 50 nm in diameter.
  • the term “mesopores” means pores within a sorbent that have a diameter of about 2 nm to about 50 nm.
  • the term “micropores” means pores within a sorbent that have a diameter of less than about 2 nm.
  • chloramine means one or more of mono-chloramine (NH 2 Cl), di-chloramine (NHCl 2 ), or tri-chloramine (NCl 3 ).
  • the sorbents or sorbent materials described herein are useful for removing chloroforms and other similar volatile organic chemical compounds (VOC) from fluids such as water.
  • VOC volatile organic chemical compounds
  • the VOC are not limited and include one or more of styrene, alachlor, atrazine, benzene, carbofuran, carbon tetrachloride, chlorobenzene, chloropicrin, 2,4- dichlorophenoxyacetic acid (2,4-D), dibromochloropropane (DBCP), o-dichlorobenzene, p- dichlorobenzene, 1,2-dichloroethane, 1,1-dichloroethylene, cis-1,2-dichloroethylene, trans- 1,2-dichloroethylene, 1,2-dichloropropane, cis-1,3-dichloropropylene, dinoseb, endrin, ethylbenzene, ethylene dibromide (EDB), halo
  • VOC that are relevant in the field of drinking water are known in the industry and are described, for example, in NSF/ANSI 53-2019, which was designated a standard on May 6, 2019 and which is incorporated by reference in its entirety.
  • the removal of VOC by sorbents or sorbent materials is measured by the removal of the individual VOC species themselves.
  • the removal of VOC by sorbents or sorbent materials is measured by the removal of surrogate compounds.
  • Surrogates are compounds that are similar in chemical composition to the analytes of interest and which are present in sample prior to preparation and analysis. For example, chloroform is one example of a surrogate for the compounds of this paragraph.
  • the sorbents or sorbent materials described herein are also useful for removing other contaminants from water or other fluids such as perfluoroalkyl and polyfluoroalkyl substances (PFAS).
  • PFAS compounds include one or more of perfluorooctanoic acid (PFOA), perfluorooctanesulfonic acid (PFOS), and compounds produced by the GENX process such as 2,3,3,3,-tetrafluoro-2-(heptafluoropropoxy)propanoate and heptafluoropropyl 1,2,2,2-tetrafluoroethyl ether.
  • the sorbents or sorbent materials are also useful in removing a wide variety of emerging contaminants from water or other fluids.
  • emerging contaminants include one or more of meprobamate, phenytoin, atenolol, carbamazepine, tris(2-chloroethyl) phosphate (TCEP), tris(1-chloro-2-propyl) phosphate (TCPP), N,N-diethyl-meta-toluamide (DEET), metolachlor, trimethoprim, ibuprofen, naproxen, estrone, bisphenol A, linuron, or nonyl phenol.
  • TCEP tris(2-chloroethyl) phosphate
  • TCPP tris(1-chloro-2-propyl) phosphate
  • DEET N,N-diethyl-meta-toluamide
  • metolachlor trimethoprim, ibuprofen, naproxen
  • a carbonaceous material is provided 20, followed by activating 30 the carbonaceous material to form a precursor activated carbon.
  • the precursor activated carbon is optionally oxidized 40, which means that in certain embodiments oxidation 40 is performed, but in certain other embodiments oxidation 40 is not performed.
  • the precursor activated carbon is doped 50 which imparts a quantity of copper dopants, iron dopants, and nitrogen dopants to the precursor activated carbon and thereby produce a doped precursor activated carbon.
  • the doped precursor activated carbon is then calcined 60 by heating under at specified temperatures and under a specified atmosphere and cooled 70 in an inert atmosphere so as not to substantially alter the pore structure or cause any substantial oxidation or activation of the doped precursor activated carbon.
  • the completion of calcination 60 and cooling 70 produces the sorbent material of the disclosure.
  • Carbonaceous Material Processing [0058] The disclosure provides one or more carbonaceous materials that are precursors to the final sorbents. Carbonaceous material may have been mechanically treated, thermally treated, or chemically treated, and can even have weakly sorbent properties, but carbonaceous material does not adsorb compounds in substantial amounts as would be expected of a material such as activated carbon.
  • carbonaceous materials may have been mechanically treated, thermally treated, or chemically treated, they have not been treated in ways that activate the carbon.
  • Examples of carbonaceous material include but are not limited to bituminous coal, sub-bituminous coal, lignite coal, anthracite coal, wood, wood chips, sawdust, peat, nut shells, pits, coconut shell, babassu nut, macadamia nut, dende nut, peach pit, cherry pit, olive pit, walnut shell, wood, lignin, polymers, nitrogen-containing polymers, resins, petroleum pitches, bagasse, rice hulls, corn husks, wheat hulls and chaff, graphenes, carbon nanotubes, or polymer fibers.
  • the carbonaceous material is coconut.
  • coconut carbonaceous materials are particularly useful because when coconut is activated to form activated carbon, it has excellent adsorption of chloroform and other organic compounds.
  • the carbonaceous material is provided, it is processed. Certain processing steps are not limited.
  • steps that are not limited and depend on the kind of the carbonaceous material and also the desired form of the final activated carbon, and the steps include one or more of pyrolysis of the carbonaceous material to form a charcoal, pulverizing the charcoal, mixing a binder with the pulverized charcoal, briquetting the pulverized charcoal and binder, crushing the briquettes, sizing the crushed briquettes, and baking the sized briquettes or the briquettes themselves to carbonize, cure, or remove the binder.
  • the carbonaceous material in the form of baked briquettes or sized particles is thermally activated, chemically activated, or thermally and chemically activated.
  • Thermal activation is performed by heating the baked briquettes or sized particles in the presence of one or more of water, oxygen, and carbon dioxide. Chemical activation is performed by impregnating the baked briquettes or sized particles in the presence of a strong acid, strong base, or a salt. It should be noted that whether each of the above steps are included in the processing sometimes depends on the provided carbonaceous material. For example, when the carbonaceous material is coconut, process steps do not include “reagglomeration,” which is the steps of mixing a binder with the pulverized charcoal, briquetting the pulverized charcoal and binder, crushing the briquettes, and sizing the crushed briquettes. [0061] The result of processing the carbonaceous material is that activated carbon is formed.
  • this activated carbon will be referred to as “precursor activated carbon” as subsequent disclosure describes additional steps that will be applied to the precursor activated carbon to further improve its performance.
  • the performance of the precursor activated carbon depends on several factors, including the kind and amount of one or more carbonaceous materials that are included, the type of activation including chemical or thermal activation, and the level of activation that is imparted on the carbonaceous material to thereby form the precursor activated carbon. Performance of the precursor activated carbon is also affected by other processing steps such as the crushing and sizing of reagglomerated carbonaceous material particles, the level of residual binder, and the final size of the precursor activated carbon.
  • the precursor activated carbon is not separately treated or oxidized beyond the steps outlined above.
  • the sorbent capacity with respect to different disinfection byproducts or other contaminant species is substantial because the adsorptive capacity of the precursor activated carbon itself is maintained and is not particularly dependent on catalytic effects.
  • the precursor activated carbon retains substantially all organic compound adsorption capability including adsorption of chloroform, VOCs, PFAS, and emerging contaminants because of the internal pore structure of the precursor activated carbon.
  • Oxidation of Precursor Activated Carbon [0063] The disclosure contemplates optional oxidation of the precursor activated carbon. In certain embodiments, the precursor activated carbon is oxidized after it is activated.
  • the precursor activated carbon is not oxidized after it is activated.
  • Oxidation of the precursor activated carbon means that the precursor activated carbon is exposed to oxygen molecules at temperatures sufficient to impart oxygen species or complexes on the surface of the activated carbon. Oxidation does not contemplate substantial modification of the pore structure of the precursor activated carbon.
  • oxidation is performed by exposing the feedstock to an oxygen containing environment and heating the feedstock to a temperature of about 150°C to about 1050°C.
  • the temperature of oxidizing can be about 150°C to about 250°C, about 250°C to about 350°C, about 350°C to about 450°C, about 450°C to about 550°C, about 550°C to about 650°C, about 650°C to about 750°C, or about 750°C to about 850°C, or any of those disclosed endpoints, or any range that is made of a combination of any of the above ranges or values within those ranges.
  • the oxygen containing environment is one or more of atmospheric air, oxygen gas (O 2 ), oxygen plasma, hydrogen peroxide (H 2 O 2 ), ozone (O 3 ), nitrous oxide (N 2 O), or carbon dioxide (CO 2 ).
  • the oxygen containing environment is dry, and includes no moisture or substantially no measurable moisture.
  • the selection of the oxidizing temperature and the oxidant and oxidizing process does not substantially modify the pore structure of the precursor activated carbon. Thus, if a more oxidizing oxygen containing environment is selected, temperatures must be lowered to reduce the potential that additional activation will occur. Alternatively, if a higher temperature is selected, a less oxidizing oxygen containing environment must be selected to reduce the potential that additional activation will occur.
  • Oxidation can also be accomplished electrochemically. It should be noted that carbons slowly oxidize in the presence of air with or without moisture at room temperature and this oxidation, although slow, would eventually be sufficient to produce an oxidized carbon precursor.
  • the carbon may be oxidized in a non-thermal process using hydrogen peroxide, ozone, chlorine, persulfates, percarbonates, oxidizing acids such as nitric acid, air, pure oxygen or any combination thereof in the liquid or vapor phase at temperatures less than about 100°C.
  • the oxidizing step is omitted, i.e., the sorbent feedstock is not oxidized by any step faster than the above described slow oxidation that takes place naturally at room temperature under normal conditions.
  • Cu-Fe-N Doping [0067] After the precursor activated carbon is prepared and optionally oxidized, the precursor activated carbon is further treated by doping with copper-iron-nitrogen (Cu-Fe-N) compounds.
  • Doping with Cu-Fe-N imparts Cu-Fe-N complexes on the surface of the precursor activated carbon, thereby serving to catalyze disinfection byproducts.
  • Doping is achieved by contacting the precursor activated carbon with at least one copper source, at least one iron source, and at least one nitrogen source.
  • a single compound is the source of all three of copper, iron, and nitrogen.
  • a first compound is the source of copper and iron
  • a second compound is the source of nitrogen.
  • a single compound is the source of the copper and nitrogen
  • a second compound is the source of the iron.
  • a single compound is the source of the iron and the nitrogen, and a second compounds is a source of the copper.
  • the copper source is not limited, and includes one or more of copper(II) sulfate pentahydrate (CuSO 4 . 5H 2 O), copper(II) chloride (CuCl 2 ), copper(II) chloride dihydrate (CuCl 2 . 2H 2 O), copper(II) nitrate (Cu(NO 3 ) 2 ), copper(II) nitrate monohydrate (Cu(NO 3 ) 2 . H 2 O), copper(II) nitrate sesquihydrate (Cu(NO 3 ) 2 .
  • the copper source is provided as part of an aqueous solution.
  • the iron source is not limited, and includes one or more of iron(III) chloride hexahydrate (FeCl 3 ⁇ 6H 2 O), iron(II) chloride tetrahydrate (FeCl 2 ⁇ 4H 2 O), ammonium iron(III) sulfate dodecahydrate (NH 4 Fe(SO 4 ) ⁇ 12H 2 O), iron(II) sulfate heptahydrate (Fe 2 SO 4 ⁇ 7H 2 O), ammonium iron(III) oxalate trihydrate ((NH 4 ) 3 Fe(C 2 O 4 ) 3 ⁇ 3H 2 O), ammonium hexacyanoferrate(II) hydrate ((NH 4 ) 4 [Fe(CN) 6 ] ⁇ xH 2 O), ammonium iron(III) citrate ((NH 4 ) 5 [Fe(C 6 H 4 O 7 ) 2 ]), sodium ferro
  • the iron source is provided as part of an aqueous solution.
  • the nitrogen source is not limited and in some embodiments includes any source of nitrogen with a -3 oxidation state.
  • nitrogen sources that have a -3 oxidation state include one or more of urea which has the formula CO(NH 2 ) 2 or dicyandiamide (DCD) or compounds thereof, mixtures thereof, or combinations thereof.
  • the nitrogen source is provided as part of an aqueous solution. It should be noted that anhydrous copper salt or iron salt precursors, including CuCl 2 , FeCl 3 , and FeCl 2 , are analogous to hydrated counterparts including CuCl 2 .
  • the nitrogen source or the single source of iron or copper combined with nitrogen or the single source of iron, copper, and nitrogen includes several listed compounds, such compounds of combinations of compounds are not so limited. In particular Applicants discovered that those nitrogen compounds that have an oxidation state of -3 provided resulted in excellent performance. Therefore, in some embodiments, the nitrogen source is not limited so long as the nitrogen source has an oxidation state of -3. It is not believed that the oxidation state of the copper or iron is important to the results.
  • the doping process is not limited. In some embodiments, doping is performed in a single stage.
  • the precursor activated carbon is treated by contacting it with a single solution, and that single solution includes the copper compounds, the iron compounds and the nitrogen compounds.
  • the doping is performed in a single stage by contacting the precursor activated carbon with an aqueous solution containing copper(II) sulfate pentahydrate, iron(III) chloride hexahydrate, and urea.
  • the doping is performed in a single stage by contacting the precursor activated carbon with an aqueous solution containing copper(II) sulfate pentahydrate, iron(III) chloride hexahydrate, and dicyandiamide.
  • the amount of copper compounds, the amount of iron compounds, and the amount of nitrogen compounds that are doped can be controlled by one or more of varying the concentration of the copper compound in solution, varying the concentration of the iron compound in solution, varying the concentration of nitrogen concentration in solution, varying the amount of time that the solution contacts the precursor activated carbon, or varying the temperature of the solution.
  • the precursor activated carbon is dried to remove water or other solvent, with the copper, iron, and nitrogen compounds thereby remaining on the precursor activated carbon. The process of drying is not limited and is performed by drying in air at about 100°C to about 150°C for up to 2 hours.
  • the resultant doped and dried precursor activated carbon includes copper, iron, and nitrogen in various amounts.
  • the amount of copper that is added when measured on a dry precursor activated carbon basis is about 0.1 wt.%, about 0.2 wt.%, 0.3 wt.%, about 0.4 wt.%, about 0.5 wt.%, about 0.6 wt.%, about 0.7 wt.%, about 0.8 wt.%, about 0.9 wt.%, about 1.0 wt.%, about 1.1 wt.%, about 1.2 wt.%, about 1.3 wt.%, about 1.4 wt.%, about 1.5 wt.%, about 1.6 wt.%, about 1.7 wt.%, about 1.8 wt.%, about 1.9 wt.%, about 2.0 wt.%, about 2.1 wt.%, about 2.2 wt.%, about 2.3 wt
  • the amount of iron that is added when measured on a dry precursor activated carbon basis is about 0.1 wt.%, about 0.2 wt.%, 0.3 wt.%, about 0.4 wt.%, about 0.5 wt.%, about 0.6 wt.%, about 0.7 wt.%, about 0.8 wt.%, about 0.9 wt.%, about 1.0 wt.%, about 1.1 wt.%, about 1.2 wt.%, about 1.3 wt.%, about 1.4 wt.%, about 1.5 wt.%, about 1.6 wt.%, about 1.7 wt.%, about 1.8 wt.%, about 1.9 wt.%, about 2.0 wt.%, about 2.1 wt.%, about 2.2 wt.%, about 2.3 wt.%, about 2.4 wt.%, about 2.5 wt.%, about 2.6 wt.%, about 2.7 w
  • the amount of nitrogen when measured on a dry precursor activated carbon basis is about 1.5 wt.%, about 2.0 wt.%, about 2.2 wt.%, about 2.5 wt.%, about 3.0 wt.%, about 3.5 wt.%, about 4.0 wt.%, about 4.5 wt.%, about 5.0 wt.%, about 5.5 wt.%, about 6.0 wt.%, about 6.5 wt.%, about 7.0 wt.%, about 7.5 wt.%, about 8.0 wt.%, about 8.3 wt.%, about 8.5 wt.%, about 9.0 wt.%, about 9.5 wt.%, about 10.0 wt.%, about 10.5 wt.%, about 11.0 wt.%, about 11.5 wt.%, about 12.0 wt.%, about 12.5 wt.%, about 13.0 wt.%, about 13.5 wt.
  • FIG.2 shows one embodiment of the doping process 50 in a single stage configuration.
  • the precursor activated carbon is contacted with an aqueous solution containing a copper source, an iron source, and a nitrogen source, shown by box 51.
  • the contacted precursor activated carbon is dried 52.
  • doped precursor activated carbon is ready for calcining.
  • the precursor activated carbon is provided and subsequently sprayed with an aqueous solution that includes dissolved copper(II) sulfate pentahydrate, urea, and dissolved iron(III) chloride hexahydrate dopants. The precursor activated carbon then stands for a predetermined period of time.
  • the precursor activated carbon is dried for a predetermined period of time and at a predetermined temperature.
  • the aqueous solution adds about 0.19 wt.% Cu, about 12.1 wt.% N, and about 0.19 wt.% Fe, with each measured by the weight of the dry precursor activated carbon.
  • the standing time can be about 40 minutes, about 50 minutes, about 60 minutes, about 70 minutes, or about 80 minutes. Drying is performed at a temperature of about 100°C for about 4 hours, though the drying is not limited and these times and temperatures can vary.
  • the doped precursor activated carbon is ready for calcining. [0076]
  • doping is performed in a two-stages.
  • the precursor activated carbon is treated by first contacting it with a solution that contains copper and iron, optionally drying the precursor activated carbon containing copper and iron, second contacting the precursor activated carbon containing copper and iron with a solution that contains nitrogen, and drying the precursor activated carbon that contains copper, iron, and nitrogen.
  • the precursor activated carbon is treated by first contacting it with a solution that contains copper and nitrogen, optionally drying the precursor activated carbon containing copper and nitrogen, second contacting the precursor activated carbon containing copper and nitrogen with a solution that contains iron, and drying the precursor activated carbon that contains copper, iron, and nitrogen.
  • the precursor activated carbon is treated by first contacting it with a solution that contains copper and nitrogen, optionally drying the precursor activated carbon containing copper and nitrogen, second contacting the precursor activated carbon containing copper and nitrogen with a solution that contains iron, and drying the precursor activated carbon that contains copper, iron, and nitrogen.
  • the precursor activated carbon is treated by first contacting it with a solution that contains iron and nitrogen, optionally drying the precursor activated carbon containing iron and nitrogen, second contacting the precursor activated carbon containing iron and nitrogen with a solution that contains copper, and drying the precursor activated carbon that contains copper, iron, and nitrogen.
  • the doping is performed in two stages by first contacting the precursor activated carbon with an aqueous solution containing dissolved copper(II) sulfate pentahydrate and an aqueous solution containing dissolved iron(III) chloride hexahydrate and second contacting the precursor activated carbon with an aqueous solution of urea. In one such embodiment, the doping is performed in two stages by first contacting the precursor activated carbon with an aqueous solution containing dissolved copper(II) sulfate pentahydrate and an aqueous solution of urea and second contacting the precursor activated carbon with an aqueous solution containing dissolved iron(III) chloride hexahydrate.
  • the doping is performed in two stages by first contacting the precursor activated carbon with an aqueous solution containing dissolved iron(III) chloride hexahydrate and an aqueous solution of urea and second contacting the precursor activated carbon with an aqueous solution containing dissolved copper(II) sulfate pentahydrate.
  • the two stage doping is performed by contacting the precursor activated carbon with an aqueous solution containing dissolved copper(II) sulfate pentahydrate and an aqueous solution containing dissolved iron(III) chloride hexahydrate and second contacting the precursor activated carbon with an aqueous solution of dicyandiamide.
  • the doping is performed in two stages by first contacting the precursor activated carbon with an aqueous solution containing dissolved copper(II) sulfate pentahydrate and an aqueous solution of dicyandiamide and second contacting the precursor activated carbon with an aqueous solution containing dissolved iron(III) chloride hexahydrate.
  • the doping is performed in two stages by first contacting the precursor activated carbon with an aqueous solution containing dissolved iron(III) chloride hexahydrate and an aqueous solution of dicyandiamide and second contacting the precursor activated carbon with an aqueous solution containing dissolved copper(II) sulfate pentahydrate.
  • the amount of copper compounds, the amount of iron compounds, and the amount of nitrogen compounds that are doped can be controlled by one or more of varying the concentration of the copper compound in solution, varying the concentration of the iron compound in solution, varying the concentration of nitrogen concentration in solution, varying the amount of time that one or more of the solution containing copper, solution containing iron, or the solution containing nitrogen contacts the precursor activated carbon, or varying the temperature of one or more of the solution containing copper, solution containing iron, or the solution containing nitrogen.
  • the resultant doped and dried precursor activated carbon includes copper, iron, and nitrogen in specified amounts.
  • the amount of copper when measured on a dry precursor activated carbon basis is about 0.1 wt.%, about 0.2 wt.%, 0.3 wt.%, about 0.4 wt.%, about 0.5 wt.%, about 0.6 wt.%, about 0.7 wt.%, about 0.8 wt.%, about 0.9 wt.%, about 1.0 wt.%, about 1.1 wt.%, about 1.2 wt.%, about 1.3 wt.%, about 1.4 wt.%, about 1.5 wt.%, about 1.6 wt.%, about 1.7 wt.%, about 1.8 wt.%, about 1.9 wt.%, about 2.0 wt.%, about 2.1 wt.%, about 2.2 wt.%, about 2.3 wt.%, about 2.4 wt.%, about 2.5 wt.%, about 2.6 wt.%, about 2.7 wt
  • the amount of iron when measured on a dry precursor activated carbon basis is about 0.1 wt.%, about 0.2 wt.%, 0.3 wt.%, about 0.4 wt.%, about 0.5 wt.%, about 0.6 wt.%, about 0.7 wt.%, about 0.8 wt.%, about 0.9 wt.%, about 1.0 wt.%, about 1.1 wt.%, about 1.2 wt.%, about 1.3 wt.%, about 1.4 wt.%, about 1.5 wt.%, about 1.6 wt.%, about 1.7 wt.%, about 1.8 wt.%, about 1.9 wt.%, about 2.0 wt.%, about 2.1 wt.%, about 2.2 wt.%, about 2.3 wt.%, about 2.4 wt.%, about 2.5 wt.%, about 2.6 wt.%, about 2.7 wt.%
  • the amount of nitrogen when measured on a dry precursor activated carbon basis is about 1.5 wt.%, about 2.0 wt.%, about 2.2 wt.%, about 2.5 wt.%, about 3.0 wt.%, about 3.5 wt.%, about 4.0 wt.%, about 4.5 wt.%, about 5.0 wt.%, about 5.5 wt.%, about 6.0 wt.%, about 6.5 wt.%, about 7.0 wt.%, about 7.5 wt.%, about 8.0 wt.%, about 8.3 wt.%, about 8.5 wt.%, about 9.0 wt.%, about 9.5 wt.%, about 10.0 wt.%, about 10.5 wt.%, about 11.0 wt.%, about 11.5 wt.%, about 12.0 wt.%, about 12.5 wt.%, about 13.0 wt.%, about 13.5 wt.
  • FIG.3 shows one embodiment of the doping process 50 in a two stage configuration.
  • the precursor activated carbon is contacted with an aqueous solution containing a copper source and an iron source, shown by box 51.
  • precursor activated carbon is dried 52.
  • the precursor activated carbon is contacted with an aqueous solution containing a nitrogen source, shown by box 53.
  • the precursor activated carbon is dried 54.
  • the doped precursor activated carbon is ready for calcining.
  • doping is performed in three-stages.
  • the precursor activated carbon is treated by first contacting it with a solution that contains copper, optionally drying the precursor activated carbon containing copper, second contacting the precursor activated carbon containing copper with a solution that contains iron, optionally drying the precursor activated carbon containing copper and iron, third contacting the precursor activated carbon containing copper and iron with a solution that contains nitrogen, and drying the precursor activated carbon that contains copper, iron, and nitrogen.
  • the precursor activated carbon is treated by first contacting it with a solution that contains iron, optionally drying the precursor activated carbon containing iron, second contacting the precursor activated carbon containing iron with a solution that contains copper, optionally drying the precursor activated carbon containing iron and copper, third contacting the precursor activated carbon containing iron and copper with a solution that contains nitrogen, and drying the precursor activated carbon that contains copper, iron, and nitrogen.
  • the precursor activated carbon is treated by first contacting it with a solution that contains copper, optionally drying the precursor activated carbon containing copper, second contacting the precursor activated carbon containing copper with a solution that contains nitrogen, optionally drying the precursor activated carbon containing copper and nitrogen, third contacting the precursor activated carbon containing copper and nitrogen with a solution that contains iron, and drying the precursor activated carbon that contains copper, iron, and nitrogen.
  • the precursor activated carbon is treated by first contacting it with a solution that contains iron, optionally drying the precursor activated carbon containing iron, second contacting the precursor activated carbon containing copper with a solution that contains nitrogen, optionally drying the precursor activated carbon containing iron and nitrogen, third contacting the precursor activated carbon containing iron and nitrogen with a solution that contains copper, and drying the precursor activated carbon that contains copper, iron, and nitrogen.
  • the precursor activated carbon is treated by first contacting it with a solution that contains nitrogen, optionally drying the precursor activated carbon containing nitrogen, second contacting the precursor activated carbon containing nitrogen with a solution that contains copper, optionally drying the precursor activated carbon containing nitrogen and copper, third contacting the precursor activated carbon containing nitrogen and copper with a solution that contains iron, and drying the precursor activated carbon that contains copper, iron, and nitrogen.
  • the precursor activated carbon is treated by first contacting it with a solution that contains nitrogen, optionally drying the precursor activated carbon containing nitrogen, second contacting the precursor activated carbon containing nitrogen with a solution that contains iron, optionally drying the precursor activated carbon containing nitrogen and iron, third contacting the precursor activated carbon containing nitrogen and iron with a solution that contains copper, and drying the precursor activated carbon that contains copper, iron, and nitrogen.
  • the doping is performed in three stages by first contacting the precursor activated carbon with an aqueous solution containing dissolved copper(II) sulfate pentahydrate, second contacting the precursor activated carbon with an aqueous solution containing dissolved iron(III) chloride hexahydrate, and third contacting the precursor activated carbon with an aqueous solution of urea.
  • the doping is performed in three stages by first contacting the precursor activated carbon with an aqueous solution containing dissolved iron(III) chloride hexahydrate, second contacting the precursor activated carbon with an aqueous solution containing dissolved copper(II) sulfate pentahydrate, and third contacting the precursor activated carbon with an aqueous solution of urea.
  • the doping is performed in three stages by first contacting the precursor activated carbon with an aqueous solution containing dissolved copper(II) sulfate pentahydrate, second contacting the precursor activated carbon with an aqueous solution of urea, and third contacting the precursor activated carbon with an aqueous solution containing dissolved iron(III) chloride hexahydrate.
  • the doping is performed in three stages by first contacting the precursor activated carbon with an aqueous solution containing dissolved iron(III) chloride hexahydrate, second contacting the precursor activated carbon with an aqueous solution of urea, and third contacting the precursor activated carbon with an aqueous solution of dissolved copper(II) sulfate pentahydrate.
  • the doping is performed in three stages by first contacting the precursor activated carbon with an aqueous solution of urea, second contacting the precursor activated carbon with an aqueous solution containing dissolved copper(II) sulfate pentahydrate, and third contacting the precursor activated carbon with an aqueous solution containing dissolved iron(III) chloride hexahydrate.
  • the doping is performed in three stages by first contacting the precursor activated carbon with an aqueous solution of urea, second contacting the precursor activated carbon with an aqueous solution containing dissolved iron(III) chloride hexahydrate, and third contacting the precursor activated carbon with an aqueous solution of dissolved copper(II) sulfate pentahydrate.
  • the three stage doping is performed by first contacting the precursor activated carbon with an aqueous solution of dissolved copper(II) sulfate pentahydrate, second contacting the precursor activated carbon with an aqueous solution containing dissolved iron(III) chloride hexahydrate, and third contacting the precursor activated carbon with an aqueous solution of dicyandiamide.
  • the doping is performed in three stages by first contacting the precursor activated carbon with an aqueous solution containing dissolved iron(III) chloride hexahydrate, second contacting the precursor activated carbon with an aqueous solution containing dissolved copper(II) sulfate pentahydrate, and third contacting the precursor activated carbon with an aqueous solution of dicyandiamide.
  • the doping is performed in three stages by first contacting the precursor activated carbon with an aqueous solution containing dissolved copper(II) sulfate pentahydrate, second contacting the precursor activated carbon with an aqueous solution of dicyandiamide, and third contacting the precursor activated carbon with an aqueous solution containing dissolved iron(III) chloride hexahydrate.
  • the doping is performed in three stages by first contacting the precursor activated carbon with an aqueous solution containing dissolved iron(III) chloride hexahydrate, second contacting the precursor activated carbon with an aqueous solution of dicyandiamide, and third contacting the precursor activated carbon with an aqueous solution containing dissolved copper(II) sulfate pentahydrate.
  • the doping is performed in three stages by first contacting the precursor activated carbon with an aqueous solution of dicyandiamide, second contacting the precursor activated carbon with an aqueous solution containing dissolved copper(II) sulfate pentahydrate, and third contacting the precursor activated carbon with an aqueous solution containing dissolved iron(III) chloride hexahydrate.
  • the doping is performed in three stages by first contacting the precursor activated carbon with an aqueous solution of dicyandiamide, second contacting the precursor activated carbon with an aqueous solution containing dissolved iron(III) chloride hexahydrate, and third contacting the precursor activated carbon with an aqueous solution containing dissolved copper(II) sulfate pentahydrate.
  • the amount of copper compounds, the amount of iron compounds, and the amount of nitrogen compounds that are doped can be controlled by one or more of varying the concentration of the copper compound in solution, varying the concentration of the iron compound in solution, varying the concentration of nitrogen concentration in solution, varying the amount of time that one or more of the solution containing copper, solution containing iron, or the solution containing nitrogen contacts the precursor activated carbon, or varying the temperature of one or more of the solution containing copper, solution containing iron, or the solution containing nitrogen.
  • the resultant doped and dried precursor activated carbon includes copper, iron, and nitrogen in specified amounts.
  • the amount of copper that is added when measured on a dry precursor activated carbon basis is about 0.1 wt.%, about 0.2 wt.%, 0.3 wt.%, about 0.4 wt.%, about 0.5 wt.%, about 0.6 wt.%, about 0.7 wt.%, about 0.8 wt.%, about 0.9 wt.%, about 1.0 wt.%, about 1.1 wt.%, about 1.2 wt.%, about 1.3 wt.%, about 1.4 wt.%, about 1.5 wt.%, about 1.6 wt.%, about 1.7 wt.%, about 1.8 wt.%, about 1.9 wt.%, about 2.0 wt.%, about 2.1 wt.%, about 2.2 wt.%, about 2.3 wt.%, about 2.4 wt.%, about 2.5 wt.%, about 2.6 wt.%, about 2.7
  • the amount of iron that is added when measured on a dry precursor activated carbon basis is about 0.1 wt.%, about 0.2 wt.%, 0.3 wt.%, about 0.4 wt.%, about 0.5 wt.%, about 0.6 wt.%, about 0.7 wt.%, about 0.8 wt.%, about 0.9 wt.%, about 1.0 wt.%, about 1.1 wt.%, about 1.2 wt.%, about 1.3 wt.%, about 1.4 wt.%, about 1.5 wt.%, about 1.6 wt.%, about 1.7 wt.%, about 1.8 wt.%, about 1.9 wt.%, about 2.0 wt.%, about 2.1 wt.%, about 2.2 wt.%, about 2.3 wt.%, about 2.4 wt.%, about 2.5 wt.%, about 2.6 wt.%, about 2.7 w
  • the amount of nitrogen when measured on a dry precursor activated carbon basis is about 1.5 wt.%, about 2.0 wt.%, about 2.2 wt.%, about 2.5 wt.%, about 3.0 wt.%, about 3.5 wt.%, about 4.0 wt.%, about 4.5 wt.%, about 5.0 wt.%, about 5.5 wt.%, about 6.0 wt.%, about 6.5 wt.%, about 7.0 wt.%, about 7.5 wt.%, about 8.0 wt.%, about 8.3 wt.%, about 8.5 wt.%, about 9.0 wt.%, about 9.5 wt.%, about 10.0 wt.%, about 10.5 wt.%, about 11.0 wt.%, about 11.5 wt.%, about 12.0 wt.%, about 12.5 wt.%, about 13.0 wt.%, about 13.5 wt.
  • the processes are not so limited.
  • additional dopants can be applied in additional stages or as part of any of the solutions that contact the precursor activated carbon.
  • the ratio of iron and copper is not limited. In some embodiments, the ratio of iron to copper is about 10:90 to about 90:10, about 30:70 to about 70:30, about 60:40 to about 40:60, about 50:50, or any range that includes that falls within the preceding listed ranges.
  • the doped precursor activated carbon is ready for thermal processing, which is also referred to as calcination.
  • the doped precursor activated carbon is heated in the presence of an inert atmosphere to achieve additional changes in the doped precursor activated carbon.
  • the temperature of calcination of the doped precursor activated carbon is not limited.
  • calcination takes place at a temperature of about 400°C, about 450°C, about 500°C, about 550°C, about 600°C, about 650°C, about 700°C, about 750°C, about 800°C, about 850°C, about 900°C, about 950°C, about 1000°C, about 1050°C, or any range that includes one or more of the above values as endpoints.
  • the temperature of calcination is about 900°C to about 1000°C.
  • the inert atmosphere for calcination is one that does not cause any substantial oxidation or activation of the doped precursor activated carbon at the specified temperatures so as not to alter the pore structure of the doped precursor activated carbon.
  • the atmosphere contains no oxygen, carbon dioxide, or water, or the atmosphere contains amounts of oxygen, carbon dioxide, or water that are so small as to not cause any oxidation or activation.
  • atmospheres for calcination include one or more of nitrogen gas (N 2 ), helium, neon, argon, krypton, xenon, and combinations thereof.
  • N 2 nitrogen gas
  • sorbent material is granular activated carbon (GAC), which is defined as activated carbon particles sized to be retained on a 50-mesh sieve (holes of about 0.300 mm).
  • the sorbent material is powdered activated carbon (PAC), which is defined as particles that pass through an 80-mesh sieve (holes of about 0.180 mm). While these particle size ranges are mentioned for activated carbon sorbent materials, it is also contemplated that any of the disclosed sorbent materials may be measured by the above 50-mesh and 80-mesh sieve sizes. In still other embodiments, the sorbent material is pelletized activated carbon. Performance Measurement / Sorbent Characterization [0093] The performance of the sorbent materials of the disclosure is measured in various ways, including the “chloramine destruction number” (CDN) which defined below. The chloramine destruction number quantifies the amount of chloramine that can be removed from a fluid by the sorbent materials of the disclosure.
  • CDN chloramine destruction number
  • the measurement of the CDN is known in the art, for example in U.S. Patent No.10,702,853 patented on July 7, 2020 and titled “CHLORAMINE AND CHLORINE REMOVAL MATERIAL AND METHODS FOR MAKING THE SAME,” which is incorporated by reference herein in its entirety.
  • the CDN is the absolute value of the first order linear kinetic fit, multiplied by 1000, that is applied to a natural log of a concentration of chloramine in water versus time, where the initial concentration of chloramine is decreased over a period of 150 minutes. When ammonia is in equilibrium with chlorine in solution the form of chloramine is pH dependent.
  • the chloramine solution comprised ammonium chloride; sodium hypochlorite and deionized water were mixed to obtain a 1 L solution of 300 ppm chloramine at a pH of 9.0. At a pH value of 9.0, the chloramine species that is present at equilibrium is the mono- chloramine form, which is the most difficult to destroy.
  • the solution was buffered using sodium carbonate to maintain the solution pH during evaluation.
  • the chlorine solution comprised sodium hyprochlorite and deionized water to obtain 1 L of a 300 ppm chlorine solution.
  • One liter of the 300 ppm respective solution was added to an Erlenmeyer flask that was placed in a water bath controlled to 20°C.
  • a constant volume of 2.0 mL activated carbon (sized at 80 ⁇ 325 mesh) was added to the agitated 1 L chloramine or chlorine solution for each sample analysis.
  • the volume of the carbon used was determined from the apparent density of the 80 ⁇ 325 carbon as determined by ASTM Method D-2854.
  • the concentration of total chlorine in solution was measured at various time points over a 150 min period by taking aliquots and then analyzing using a standard HACH colorimetric EPA accepted method 10070 for total chlorine.
  • concentration versus time data for each sorbent material sample is replotted as the natural log of total chlorine concentration versus time to linearize the data according to first order kinetic theory.
  • a linear fit is then applied to the data and the slope of the linear fit is determined.
  • the slope is always negative because the initial concentration of total chlorine decreases over the 150 min period.
  • the absolute value of the slope multiplied by 1000 is used quantify the rate of chloramine and chlorine destruction (removal). The larger the absolute slope, the more effective the sorbent material is at removing chlorine and chloramine.
  • the slope resulting from the linear fit of the first order kinetic experimental data is referred to as the “chloramine destruction number” or CDN. In the case of chlorine destruction this rate is referred to as the “chlorine destruction number” of Cl-DN.
  • the disclosure contemplates values of about 3.0, about 3.5, about 4.0, about 4.5, about 5.0, about 5.5, about 6.0, about 6.5, about 7.0, about 7.5, about 8.0, about 8.5, about 9.0, about 9.5, about 10.0, about 10.5, about 11.0, about 12.0, about 12.5, about 13.0, about 13.5, about 14.0, about 14.5, about 15.0, about 15.5, about 16.0, about 16.5, about 17.0, about 17.5, about 18.0, about, 18.5, about 19.0, about 19.5, about 20.0, about 20.5, about 21.0, about 21.5, about 22.0, about 22.5, about 23.0, about 23.5, about 24.0, about 24.5, about 25.0, about 25.5, about 26.0, about 26.5, about 27.5, about 28.0, about 28.5, about 29.0, about 29.5, about 30.0, about 35.0, about 40.0, about 45.0, about 50.0, about 55.0, about 60.0, about 65.0, about 70.0, about 3.0, about 9.5,
  • the CDN can be a range with these numbers as a lower performance bound, such as at least about 4.0, at least about 4.5, at least about 5.0, at least about 10.0, at least about 15.0, at least about 20.0, at least about 23.0, at least about 50.0, at least about 75.0, or at least about 100.0.
  • the chloramine destruction number is measured with respect to mono-chloramine.
  • the “peroxide destruction number” which is also referred to as the “peroxide number” is also measured.
  • the peroxide number is a volumetric test, which means that performance is measured and normalized to a specified volume of sorbent material.
  • the test for the peroxide number is well known in the art, and is described for example by U.S. Patent No.5,470,748, which is incorporated by reference herein in its entirety.
  • the sorbent material is first pulverized to a fine mesh size fraction where at least 90 wt.%, and in certain tests at least 95 wt.%, of the sorbent will pass through a 325 mesh U.S. Standard Series sieve (44 ⁇ m opening size).
  • a specified amount of the pulverized sorbent material is placed in a vacuum flask (Dewar), and 100 mL of deionized water is added to the vacuum flask.
  • the addition of the deionized water is performed such that any pulverized sorbent material clinging to the sides of the vacuum flask is carried into the main body of water at the bottom of the vacuum flask.
  • a 50 mL aliquot of aqueous buffer solution is added to the vacuum flask.
  • the aqueous buffer solution is 0.5 molar in K 2 HPO 4 and 0.5 molar in KH 2 PO 4 .
  • a magnetic stir bar is added into the vacuum flask and energized to begin stirring. Stirring speed is increased until a vortex greater than about 0.5 inches (1.27 cm) deep is formed in the mixture and the optimum stir bar speed is achieved.
  • the optimum stir bar speed is selected so that additional increases in stir bar speed do not significantly affect the peroxide decomposition time.
  • a specified amount of the sorbent material is added to a buffered hydrogen peroxide solution. Because the test is a volumetric test, the specified amount of sorbent material that is added to the buffered hydrogen peroxide solution is based on one half (1/2) of the apparent density of the sorbent material. In particular, the mass of sorbent material in grams that is added to the solution is equal to one half (1/2) of the measured apparent density of the sorbent material, when the apparent density of the sorbent material is reported in g/cm 3 .
  • the catalytic properties of the sorbent material cause the peroxide to be catalyzed and thereby destroyed (i.e., the hydrogen peroxide decomposes into water and oxygen gas).
  • the catalysis of hydrogen peroxide is exothermic.
  • the rated of decomposition by way of the sorbent material can be approximated over time by measuring the temperature of the buffered solution.
  • the “peroxide number” is the length of time in minutes that is required for the buffered solution containing the sorbent material sample to reach 75% of the recorded maximum temperature. Faster times and therefore smaller values of the peroxide number indicate more catalytic activity and thus a higher performance sorbent material.
  • the peroxide destruction number measured in minutes is about 1.0, about, about 1.5, about 2.0, about 2.1, about 2.2, about 2.3, about 2.4, about 2.5, about 2.6, about 2.7, about 2.8, about 2.9, about 3.0, about 3.1, about 3.2, about 3.3, about 3.4, about 3.5, about 3.6, about 3.7, about 3.8, about 3.9, about 4.0, about 4.1, about 4.2, about 4.3, about 4.4, about 4.5, about 4.6, about 4.7, about 4.8, about 4.9, about 5.0, about 5.1, about 5.2, about 5.3, about 5.4, about 5.5, about 5.6, about 5.7, about 5.8, about 5.9, about 6.0, about 6.1, about 6.2, about 6.3, about 6.4, about 6.5, about 6.6, about 6.7, about 6.8, about 6.9, about 7.0, about 7.1, about 7.2, about 7.3, about 7.4, about 7.5, about 7.6, about 7.7, about 7.8, about 7.
  • the peroxide destruction number measured in minutes is about 10, about 15, about 20, about 25, about 30, about 35, about 40, about 45, or any range that is formed from two or more of the above values as endpoints of the range.
  • the peroxide number is related to and has some correlation with the CDN and C1-DN, in that each are measures of the catalytic activity of the sorbent material. However, the correlation is not always exact, because each represents a different aspect of the catalytic activity of a sorbent material. Still further, the catalytic activity is useful only for those compounds that are catalyzed, but other compounds must be adsorbed to be effectively removed from a fluid stream.
  • a superior sorbent material therefore must have good performance in more than one of the CDN, C1-DN, peroxide number, and adsorption tests so that it is effective at removing a broad range of compounds from fluid streams.
  • Fluid Treatment [0103] Further embodiments are directed to methods for purifying fluids such as water by using the chlorine and chloramine destroying sorbent materials described above.
  • a fluid is treated by flowing the fluid over a bed of sorbent material, introducing fluid onto a filter including sorbent material, introducing sorbent material into a container for holding fluid, and the like.
  • the above steps are combined in parallel or subsequently in series.
  • the fluid is water.
  • the fluid is water that is for human, plant, animal, or marine life consumption. In some embodiments, the fluid is in liquid form.
  • the methods of purifying fluids includes additional steps. For example, in some embodiments, methods for purifying includes the steps of filtering the fluid using, for example, a screen or sand filter before, after, or both before and after contacting with sorbent material to remove particulates. In further embodiments, the methods include a step of disinfecting the water to remove biological contaminants such as bacteria or other microorganisms, and in some embodiments, the methods include the step of introducing a disinfectant into the fluid or irradiating the fluid with ultraviolet radiation.
  • the methods include the step of clarifying the fluid, adjusting the pH of the fluid, and the like and combinations thereof.
  • the fluid can be water.
  • EXAMPLES [0105] The following experimental examples are intended to better illustrate specific embodiments, and they are not intended to limit the disclosure.
  • Single Stage Process Examples [0106] Coconut carbonaceous material was provided, processed and activated. The resultant coconut activated carbon is available from Calgon Carbon Corporation under the product name OLC and is referred to as precursor activated carbon. The coconut activated carbon is a granular activated carbon and tested in the size of 12 ⁇ 40. The precursor activated carbon is oxidized for some tests but is not oxidized for other tests.
  • the precursor activated carbon is ready for doping with Cu, Fe, and N.
  • a single stage doping process is performed. The single stage doping process dopes the oxidized or the unoxidized precursor activated carbon with copper, iron, and nitrogen.
  • an aqueous solution containing CuSO 4 ⁇ 5H 2 O, FeCl 3 ⁇ 6H 2 O, and urea contacts the oxidized or unoxidized precursor activated carbon to achieve 0.2 wt.% to 1.0 wt.% Cu, achieve 0.2 wt.% to 1.0 wt.% Fe, and 2.2 wt.% to 8.3 wt.% N, to 15 wt.% N on the carbon, measured on a dry precursor activated carbon basis.
  • the aqueous solution contacts the precursor activated carbon for up to 30 minutes at 25°C. After the aqueous solution contacts the precursor activated carbon, the precursor activated carbon is dried to thereby produce a doped precursor activated carbon.
  • FIG.4 shows the effect on CDN and peroxide number of varying the amount of nitrogen that is doped on the precursor activated carbon while maintaining the total metal level at about 0.5 wt.%.
  • the results shown in FIG.4 are for precursor activated carbon that was formed from coconut carbonaceous material and subsequently oxidized. Doping added Cu, Fe and N to the this oxidized activated carbon.
  • FIG.4 shows that, for a 0.5 wt.% total metals loading level, CDN and peroxide destruction numbers do not substantially increase after about 4 wt.% nitrogen is doped.
  • FIG.5 and FIG.6 demonstrate the effect of metal doping of the precursor activated carbon on both CDN and peroxide destruction numbers for Cu, Fe, and N doped oxidized precursor activated carbon that is prepared from coconut carbonaceous material. Doping such activated carbon precursor with Cu, Fe, and N achieves higher CDN values versus doping with Cu and N or Fe and N precursor activated carbon that is formed from coconut carbonaceous material. Such doping with Cu, Fe, and N also achieves faster (and therefore superior) peroxide destruction numbers versus Cu and N or Fe and N doping.
  • FIG.7 shows a comparison of the effect on CDN and peroxide destruction numbers of varying the amount of nitrogen added to the oxidized precursor activated carbon while keeping the total metal level at about 0.5 wt.% for Cu-N, Fe-N, and Cu-Fe-N.
  • FIG.8 shows the effect of varying the amount of nitrogen added to the unoxidized precursor activated carbon while maintaining the total metal level at about 0.5 wt.% on both CDN and peroxide destruction numbers for Cu, Fe, and N doped unoxidized precursor activated carbon formed from coconut carbonaceous material.
  • FIG.8 shows that, for a 0.5 wt.% total metals loading level, there is a linear increase in CDN as more nitrogen is added to the carbon.
  • FIG.9 and FIG.10 show the effect of added metal loading to the carbon on both CDN and peroxide destruction numbers, respectively, for Cu, Fe, and N doped precursor activated carbon formed from coconut and that has not been oxidized. Doping such unoxidized precursor activated carbon with Cu, Fe, and N achieves higher CDN values versus unoxidized precursor activated carbon that is only doped with Cu and N or Fe and N. Doping unoxidized precursor activated carbon formed from coconut carbonaceous material with Cu, Fe, and N achieves faster peroxide destruction number versus only doping with Cu and N, or only Fe and N.
  • Table 1 shows a comparison between Cu-N, Fe-N, and Cu-Fe-N doped unoxidized activated carbon formed from wood carbonaceous material.
  • peroxide number is listed as “> 60”, it means that no temperature peak was observed after 60 minutes of testing duration and that the true peroxide number is a duration greater than 60 minutes. This is an indicator of poor performance for this metric.
  • BGE is a granular wood-based, activated carbon available from Calgon Carbon Corporation.
  • AquaGuard® is a wood-based catalytic activated carbon for chlorine and chloramine removal in drinking water applications and is available from Ingevity Corporation of North Charleston, South Carolina.
  • compositions, methods, and devices are described in terms of “comprising” various components or steps (interpreted as meaning “including, but not limited to”), the compositions, methods, and devices can also “consist essentially of” or “consist of” the various components and steps, and such terminology should be interpreted as defining essentially closed-member groups. It will be further understood by those within the art that if a specific number of an introduced claim recitation is intended, such an intent will be explicitly recited in the claim, and in the absence of such recitation no such intent is present. [0119] For example, as an aid to understanding, the following appended claims may contain usage of the introductory phrases "at least one" and "one or more” to introduce claim recitations.
  • each range discussed herein can be readily broken down into a lower third, middle third and upper third, et cetera.
  • all language such as “up to,” “at least,” and the like include the number recited and refer to ranges that can be subsequently broken down into subranges as discussed above.
  • a range includes each individual member.
  • a group having 1-3 components refers to groups having 1, 2, or 3 components.
  • a group having 1-5 components refers to groups having 1, 2, 3, 4, or 5 components, and so forth.

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