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WO2007017666A1 - Procédé pour traiter un matériau à base de noir d'os - Google Patents

Procédé pour traiter un matériau à base de noir d'os Download PDF

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Publication number
WO2007017666A1
WO2007017666A1 PCT/GB2006/002952 GB2006002952W WO2007017666A1 WO 2007017666 A1 WO2007017666 A1 WO 2007017666A1 GB 2006002952 W GB2006002952 W GB 2006002952W WO 2007017666 A1 WO2007017666 A1 WO 2007017666A1
Authority
WO
WIPO (PCT)
Prior art keywords
bone char
product
contaminant
carbon
bone
Prior art date
Application number
PCT/GB2006/002952
Other languages
English (en)
Inventor
James Russell
Original Assignee
Brimac Carbon Services Limited
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from GB0516283A external-priority patent/GB0516283D0/en
Application filed by Brimac Carbon Services Limited filed Critical Brimac Carbon Services Limited
Publication of WO2007017666A1 publication Critical patent/WO2007017666A1/fr

Links

Classifications

    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/04—Treating liquids
    • G21F9/06—Processing
    • G21F9/12—Processing by absorption; by adsorption; by ion-exchange
    • 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
    • C02F2101/006—Radioactive 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
    • C02F2101/20—Heavy metals or heavy metal 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
    • C02F2101/30—Organic compounds
    • C02F2101/305—Endocrine disruptive agents

Definitions

  • the present invention relates to an adsorbent product, to a process for the preparation of such a product, and to a plurality of uses of such a product.
  • groundwater forms the bulk of the potable water available to the local population. Any contaminants present in the groundwater therefore present a serious risk to health through ingestion.
  • the problem is further exacerbated by the fact that once pollutants have entered the groundwater, they tend to spread therein by various mechanisms including diffusion and tidal flow.
  • groundwater is extracted from below the water table, treated to remove contaminants, and the water returned;
  • Bone char also known as bone charcoal or bone black
  • Bone char is the product obtained from the calcining of animal bones. Its chemical constituents are principally apatite (or hydroxyapatite) and carbon. Bone char has a very high surface area to weight ratio, and for this reason it is a very good adsorbent of many materials present in aqueous systems. The principle use of bone char is the removal of coloured impurities in the sugar refining process.
  • Bone char has previously been shown to be effective in reducing the level of contaminants in water.
  • US4,902,427 discloses a filter cartridge for removing heavy metals from water, comprising a bone char impregnated filter. The cartridges are stated to be useful in the removal of cadmium, lead and mercury from water passed through them.
  • US6,428,695 discloses an in situ method for the removal of uranium from contaminated groundwater. Trenches are dug through the flow path of groundwater, and permeable reactive barriers are installed. A barrier consisting of bone char and iron oxide is shown to be superior to a barrier consiting of bone char alone in the removal of uranium from contaminated water near an abandoned uranium upgrader.
  • the present invention seeks to overcome / address the problems associated with the prior art.
  • the invention provides a process for the preparation of a bone char product of the invention comprising the steps of: a. converting at least an amount of the carbon present in bone char to give a volatile product; and b. separating said volatile product from the solid residue.
  • the invention relates to a bone char product having a reduced carbon content relative to virgin bone char. According to a third aspect, there is provided a product obtainable by the process of the invention.
  • a bone char product of the invention for removing a contaminant from a fluid.
  • a process for the removal of a contaminant from a fluid comprising bringing into association a bone char product of the invention with a contaminated fluid, to give a fluid having reduced level of contaminant and a bone char product loaded with contaminant.
  • the bone char products of the invention may be manufactured using any type of bone char.
  • Suitable bone chars are those made from animal bones. Particularly suitable bone chars are those made from cattle, sheep, pig, horse and fish. Bone char made from cattle bones is very highly preferred.
  • the bone char products of the invention may be prepared from virgin bone char (i.e. freshly manufactured bone char), or spent bone char (bone char that has been used previously for some other purpose, such as decolourising sugar).
  • bone char is produced by heating the animal bones in a reducing atmosphere.
  • a suitable method for producing bone char starting material is to heat bone grist in an oxygen-deficient atmosphere for 7 hours at a temperature of 700 0 C.
  • Bone char produced in this way has a carbon content of between 9.5 and 11.5 %.
  • virgin bone char has a carbon content of about 10 % w/w.
  • the particle size of the bone char starting material is not critical to the success of the process, and any commercially available grade may be employed.
  • the preferred particle size is "8/60 grade” (particle size 2.3mm to 0.25mm). More preferred is “20/60 grade” which has a particle size of 1 mm to 0.25 mm.
  • the bone char starting material is converted to the bone char product of the invention by converting at least an amount of the carbon present in the bone char starting material to a volatile product, and separating the volatile product from the bone char product.
  • volatile product means a chemical compound having a boiling point lower than that of elemental carbon.
  • Preferred volatile products include hydrocarbons, that is compounds of carbon and hydrogen. Particularly preferred volatile products are methane and ethane.
  • the volatile products are oxides of carbon.
  • Preferred oxides of carbon are carbon monoxide, carbon dioxide or a mixture of the two.
  • the conversion of the carbon present in the bone char starting material to the volatile product may be accomplished by any one of a number of means.
  • the bone char starting material is brought into association with a reducing agent.
  • reducing agent means a chemical compound or combination of compounds capable of reacting with elemental carbon present in the bone char starting material to give a product wherein the oxidation state of the carbon is negative.
  • a suitable reducing agent is hydrogen.
  • the volatile product will be a mixture of hydrocarbons.
  • the bone char starting material is brought into association with an oxidising agent.
  • oxidising agent means a chemical compound or combination of chemical compounds capable of reacting with the elemental carbon present in the bone char starting material to give a product wherein the oxidation state of the carbon is positive.
  • Suitable oxidising agents include halogens and their oxides, peroxides (especially hydrogen peroxide), and oxidising transition metal compounds, such as chromates (Vl) an manganates (VII).
  • a very highly preferred oxidising agent is oxygen. This may be used as pure oxygen, or may be mixed with other oxidising or diluent gases.
  • the term "diluent gas” refers to any gas which does not significantly participate in a reaction with the carbon present in the bone char starting material under conditions wherein the same carbon reacts with oxygen.
  • Typical diluent gases include nitrogen, the noble gases, carbon monoxide, carbon dioxide and water vapour.
  • a particularly preferred source of oxygen is air.
  • the volatile products will comprise carbon monoxide, carbon dioxide or a mixture of the two.
  • the conversion of the carbon present in the bone char starting material to the volatile product may be achieved in a number of ways.
  • the bone char starting material may be treated with a solution comprising an oxidising or reducing agent. It may be necessary to heat, agitate or otherwise stimulate the mixture so formed, so as to promote the conversion of the carbon to volatile product.
  • the bone char starting material may be treated by bringing it into association with a gaseous oxidising agent or reducing agent. Again, it may prove necessary to promote the reaction by means of heat and/or agitation.
  • the bone char starting material is heated in oxygen containing gas at above 300 0 C, more preferably at above 400 0 C, more preferably at above 500 0 C, more preferably at above 600 0 C, more preferably between 500 and 800 0 C, more preferably between 600 and 800 0 C, more preferably between 600 and 700 0 C.
  • the volatile products may be separated from the bone char products by any suitable physical separation method.
  • a suitable separation method is to allow the volatile products to diffuse out from the bone char product.
  • Such diffusion can be facilitated by heating, for example heating above the boiling point of the volatile product.
  • the passage of gas through the bone char product can also assist in freeing it from volatile product.
  • bone char starting material is heated in an oxygen-containing gas, to give bone char product and a volatile product comprising oxides of carbon.
  • the bone char product is separated from the volatile product by diffusion.
  • the bone char starting material is heated in a stream of oxygen containing gas.
  • the oxidising agent and carbon are effectively brought into contact, and the volatile products are swept out of the bone char product.
  • a particularly convenient means for conducting the process of the invention is in a rotary calciner.
  • a suitable apparatus is shown in Figure 1.
  • Oxygen containing gas (2) is passed through the rotating calciner (3) containing bone char starting material (6) fed continuously from a hopper heated by a vertical kiln (7).
  • the calciner (3) is held at a temperature appropriate to conducting the reaction at a reasonable rate.
  • the rotation of the calciner (3) ensures that the bone char starting material is evenly mixed, and ensures a more uniform product (1).
  • Flue gas is discharged at (5), and may be used to heat bone char feed (4).
  • Evolved gas (8) may be collected for recycling.
  • a particular advantage of using such a rotary calciner is that the process of the invention may be operated in a continuous fashion, with bone char starting material being introduced into one end of the calciner, and bone char product being discharged from the other.
  • the calciner may be inclined (as shown in Figure 1) so that the bone char particles proceed from inlet to outlet of the calciner under the influence of gravity.
  • the rotary calciner is inclined at an angle of less than 10 °. More preferably, the rotary calciner is inclined at an angle of less than 1 °. Most preferably, the rotary calciner is inclined at an angle of about 0.1 °.
  • the rotary calciner is rotated at a rate of less than 10 revolutions per minute. More preferably, the rotary calciner is rotated at a rate of less than 5 revolutions per minute. More preferably, the rotary calciner is rotated at a rate of about 3 revolutions per minute.
  • bone char is introduced into the calciner at a rate of less than 100 kg per hour. More preferably, bone char is introduced into the calciner at a rate of less than 50 kg per hour. More preferably, bone char is introduced into the calciner at a rate of about 30 kg per hour.
  • airflow through the calciner is maintained at less than 50 litres per second. More preferably, airflow through the calciner is maintained at less than 25 litres per second. Most preferably, airflow through the calciner is maintained at about 14 litres per second (0.5 cubic feet per second).
  • the rotary calciner is rotated at a rate of about 3 revolutions per minute and inclined at an angle of about 0.1 °, bone char is introduced into the calciner at a rate of about 30 kg per hour and airflow through the calciner is maintained at about 14 litres per second (0.5 cubic feet per second),
  • the calciner may be fired directly or indirectly. It is preferred that the rotary calciner is fired directly.
  • a convenient means for controlling the reaction is to adjust the speed of rotation and angle of incline of the rotary calciner such that average residence time of the bone char starting material in the calciner is constant.
  • the products of the invention are characterised in that they have a carbon content lower than that of virgin bone char.
  • the products of the invention have a ratio of apatite to carbon that is higher than the ratio of apatite to carbon in conventional virgin bone char.
  • the ratio of apatite to carbon in virgin bone char is typically 10:1.
  • the bone char of the invention has a ratio of apatite to carbon greater than 10:1. More preferably, the bone char of the invention has a ratio of apatite to carbon greater than 15:1. More preferably, the bone char of the invention has a ratio of apatite to carbon greater than 20:1.
  • the products of the invention have a carbon content of less than 8.5 % w/w. More preferably, the products of the invention have a carbon content of less than 8.0 % w/w. the products of the invention have a carbon content of less than 7.5 % w/w. More preferably the products of the invention have a carbon content of less than 7.0 % w/w. More preferably the products of the invention have a carbon content of less than 6.5 % w/w. More preferably the products of the invention have a carbon content of less than 6.0 % w/w. More preferably the products of the invention have a carbon content of less than 5.5 % w/w.
  • the products of the invention have a carbon content of less than 5.0 % w/w. More preferably the products of the invention have a carbon content of less than 4.5 % w/w. More preferably the products of the invention have a carbon content of less than 4.0 % w/w. More preferably the products of the invention have a carbon content of less than 3.5 % w/w. More preferably the products of the invention have a carbon content of less than 3.0 % w/w. More preferably the products of the invention have a carbon content of less than 2.5 % w/w. More preferably the products of the invention have a carbon content of less than 2.0 % w/w. More preferably the products of the invention have a carbon content of less than 1.5 % w/w.
  • the products of the invention have a carbon content of at least 0.5 % w/w. More preferably, the products of the invention have a carbon content of at least 1 % w/w. More preferably, the products of the invention have a carbon content of at least 1.5 % w/w. More preferably, the products of the invention have a carbon content of at least 2.0 % w/w. More preferably, the products of the invention have a carbon content of at least 2.5 % w/w. More preferably, the products of the invention have a carbon content of at least 3.0 % w/w. More preferably, the products of the invention have a carbon content of at least 3.5 % w/w. More preferably, the products of the invention have a carbon content of at least 4.0 % w/w. More preferably, the products of the invention have a carbon content of at least 4.5 % w/w.
  • the bone char products of the invention have a carbon content of between 1.5 and 6.5 % w/w, more preferably between 4.0 and 6.0 % w/w, most preferably between 3 and 5 % w/w.
  • the bone char products of the present invention are useful in the removal of the contaminant from a fluid.
  • Fluid refers to a gas or a liquid.
  • Contaminant refers to a material that it is desired to remove from the fluid, for example because it is toxic, or alternatively valuable.
  • the contaminant may be present in the fluid as a solution, suspension, emulsion, slurry or any other form.
  • a preferred fluid is sugar solution.
  • the contaminant is coloured impurities.
  • An alternative preferred fluid is water.
  • the bone char products of the invention show particular utility in this case, because of the diverse range of contaminants that can be removed. These include:
  • metals such as aluminium, arsenic, cadmium, chromium, copper, iron, lead, manganese, mercury, nickel, silver and zinc;
  • endocrine disrupters such as phthalates, bisphenol A, alkylphenols, parabens and phytoestrogens
  • radionuclides such as 241 Am, 109 Cd, 139 Ce, 60 Co, 137 Cs, 54 Mn, 113 Sn, 85 Sr, 99 Tc, 88 Y 65 Zn, and uranium especially 235 U.
  • endocrine disrupter refers to any material having the ability to mimic a hormone in an animal.
  • the products of the invention are particularly suitable for adsorption of radionuclides, and in particular are more effective than known bone chars.
  • the bone char products of the present invention find utility in the treatment of potable water, sewage, and the water used in aquaculture (fish farms).
  • the products of the invention once they have adsorbed contaminant, are referred to herein as "loaded".
  • the loaded products may be stored.
  • the products of the invention may be subjected to one or more subsequent treatment steps to render them in a form suitable for storage.
  • the loaded product may be encapsulated.
  • encapsulated refers to a process whereby loaded product is embedded, coated, or otherwise sealed within another material to prevent it interacting with the environment.
  • suitable encapsulating materials are glass, plastics materials, concrete, ceramics and metals.
  • a preferred method of encapsulation is vitrification, i.e. glass is used as the encapsulating material.
  • vitrification i.e. glass is used as the encapsulating material.
  • loaded product is mixed with frit and fused. Suitable methods are described in US5,873,675; US5,603,684; and US 5,662,579. A general summary is provided in the EPA Handbook entitled "Vitrification Technologies for Treatment of Hazardous and Radioactive Waste".
  • the contaminant may be a material that it is desirable to recover from the fluid, i.e. a valuable material.
  • the valuable material may be present in the fluid as a solution, suspension, emulsion, slurry or any other form.
  • Examples of valuable materials include:
  • precious metals particularly silver, gold, platinum, palladium and rhodium
  • fissile material particularly uranium (present e.g. in seawater).
  • contaminant and “valuable material” are not necessarily mutually exclusive, e.g. uranium may be both a contaminant and a valuable material.
  • the loaded products of the invention may be treated to recover valuable material.
  • loaded product may be washed with an aqueous medium to give a solution of valuable material.
  • Figure 1 is a diagram of an apparatus suitable for conducting a process of the invention.
  • Example 1 An indirect calciner was fitted with a paddle feeder, disturber cage and 2 inch open weir and air cooler for the test. The slope was set at 0.5 degrees and the revolution speed at 3 rpm. A feed rate of 30 kg per hour was maintained for the duration of the test.
  • the feed hood damper was fully opened.
  • the product hood and bypass dampers were closed.
  • Increasing the purge air by closing the burner inlet damper and the direct calciner exhaust had no effect on combustion indicating that airflow was adequate.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Inorganic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

L'invention fournit un procédé de traitement de noir d'os pour donner un nouveau produit à base de noir d'os, lequel est utile dans l’élimination des contaminants dans des fluides. Les produits sont plus particulièrement utiles dans l’élimination de radionucléides dans des déchets aqueux.
PCT/GB2006/002952 2005-08-08 2006-08-07 Procédé pour traiter un matériau à base de noir d'os WO2007017666A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
GB0516283A GB0516283D0 (en) 2005-08-08 2005-08-08 Process
GB0516283.9 2005-08-08
US70645105P 2005-08-09 2005-08-09
US60/706,451 2005-08-09

Publications (1)

Publication Number Publication Date
WO2007017666A1 true WO2007017666A1 (fr) 2007-02-15

Family

ID=37307334

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/GB2006/002952 WO2007017666A1 (fr) 2005-08-08 2006-08-07 Procédé pour traiter un matériau à base de noir d'os

Country Status (1)

Country Link
WO (1) WO2007017666A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012107022A3 (fr) * 2011-02-08 2012-10-11 Universität Rostock Procédé d'épuration du biogaz, des gaz de fumée ou des liquides, adsorbant à cet effet, filtres et utilisation de la substance adsorbante
CN109110757A (zh) * 2018-11-09 2019-01-01 青海民族大学 一种活性骨炭及其制备方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB541403A (en) * 1940-03-19 1941-11-26 Tate & Lyle Ltd Improvements in and relating to decolorising carbons or charcoals
GB643282A (en) * 1946-03-06 1950-09-15 Refined Syrups & Sugars Inc Improvements in or relating to methods and apparatus for reactivating bone-char
US4902427A (en) * 1988-04-25 1990-02-20 Ebonex Corporation Filter for removing heavy metals from drinking water
US20020117434A1 (en) * 2001-02-26 2002-08-29 Naftz David L. Aquifer remediation barrier for removal of inorganic contaminants
US20030196955A1 (en) * 2002-04-17 2003-10-23 Hughes Kenneth D. Membrane based fluid treatment systems

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB541403A (en) * 1940-03-19 1941-11-26 Tate & Lyle Ltd Improvements in and relating to decolorising carbons or charcoals
GB643282A (en) * 1946-03-06 1950-09-15 Refined Syrups & Sugars Inc Improvements in or relating to methods and apparatus for reactivating bone-char
US4902427A (en) * 1988-04-25 1990-02-20 Ebonex Corporation Filter for removing heavy metals from drinking water
US20020117434A1 (en) * 2001-02-26 2002-08-29 Naftz David L. Aquifer remediation barrier for removal of inorganic contaminants
US20030196955A1 (en) * 2002-04-17 2003-10-23 Hughes Kenneth D. Membrane based fluid treatment systems

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012107022A3 (fr) * 2011-02-08 2012-10-11 Universität Rostock Procédé d'épuration du biogaz, des gaz de fumée ou des liquides, adsorbant à cet effet, filtres et utilisation de la substance adsorbante
CN109110757A (zh) * 2018-11-09 2019-01-01 青海民族大学 一种活性骨炭及其制备方法

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