WO2004101142A1 - Method of preparing a water treatment product - Google Patents
Method of preparing a water treatment productInfo
- Publication number
- WO2004101142A1 WO2004101142A1 PCT/GB2004/002041 GB2004002041W WO2004101142A1 WO 2004101142 A1 WO2004101142 A1 WO 2004101142A1 GB 2004002041 W GB2004002041 W GB 2004002041W WO 2004101142 A1 WO2004101142 A1 WO 2004101142A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- surface area
- water treatment
- water
- high surface
- iron salt
- Prior art date
Links
Classifications
-
- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
-
- 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
- B01J20/28014—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 form
- B01J20/28016—Particle form
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/32—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
-
- 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
- B01J20/32—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
-
- 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
-
- 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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- C02F2101/103—Arsenic 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
Definitions
- This invention relates to a method of preparing a water treatment product, particularly one that is capable of adsorbing arsenic, fluoride, selenium or other contaminants including other heavy metals, or organic materials.
- Adsorption is capable of removing many metals over a wider pH range and to much lower levels than precipitation. Additionally, adsorption can often remove complexed metals which would not be checked by conventional treatment processes.
- ferrihydrite An adsorbent commonly present in metal treatment processes is an amorphous iron oxide called ferrihydrite.
- a disadvantage of such treatment is that ferrihydrite forms a sludge product from which it is difficult to recover purified water.
- a water treatment product has been described which consists of washed sand coated with ferrihydrite (M Edwards and M Benjamin, Jnl. Water Poll Control Fed, Vol 61 , Part 9, 1989, pages 1523-1533). That product has also been tested for removal of arsenic from drinking water (F G A Vagliasindi et al, Proceedings Water Quality Technology Conference, Part 2, New La, 12-16 November 1995, pages 1829-1853).
- WO-A-99/50182 discloses a water treatment product and method in which a water treatment product is coated with an insoluble ferric iron coating.
- a method of preparing a water treatment product which method comprises the steps of:
- the high surface area material is preferably selected from alumina, silica, and/or phosphate containing materials such as natural or synthetic zeolites (e.g. chabazite, Faujasite or the like), zeotype materials such as ALPO's (synthetic aluminophosphates) or SAPO's (silica containing aluminophosphates), felspathoids (e.g. sodalite), melanophlogite, imogolite, chalcogenides, zirconium phosphate, zeolite, clay or hydrotalcite. Alumina is particularly preferred.
- Other examples of high surface area materials are disclosed in US 5322641 , which is incorporated herein by reference. For example, this document discloses the use of a porous inorganic solid wherein at least some of its pores are micropores comprising holes, cages or channels which are essentially of molecular dimensions and which are formed by the structure of the solid.
- the high surface area material is activated, a particularly preferred example being activated alumina. It should be noted that not all high surface area materials need to be activated; zeolites are naturally high surface area materials and do not need to be activated.
- the method of the invention has been found to produce a product which is not wet or clumpy as it is not completely saturated with water. Furthermore, no forced drying step is required because the product is still in a free-flowing state at the end of the production process, as such lumps and/or agglomerates tend not to be produced. In particular, the process allows the product to be removed from the equipment in which it is produced immediately after completion of the process without lumps or agglomerates being present. Furthermore, the method has been found to provide a simple, economical process for the production of the water treatment product.
- the high surface material is alumina
- an activated alumina product a product formed by heating alumina trihydrate at 300-1100°C.
- Activated alumina has the advantage of having a large specific surface area.
- the commercial product AA400G has a specific surface area of 260 - 380 m 2 /g.
- the material may be of bauxite.
- the non-volatile content of bauxite preferably comprises from 40 - 95 wt% of AI 2 O 3 together with from 3 - 25 wt% of iron oxide.
- Activated bauxite is a preferred material which may be formed by heating the mineral at a temperature in the range 300 - 800°C, and may typically have a specific surface area of from 100 - 200 m 2 /g. Because the iron content of bauxite is present in, rather than on, the particle surface, it is generally not counted as part of the coating of this invention.
- Any suitable grade of activated alumina can be used, for example AA400G.
- any mesh size of the high surface area material for example activated alumina may be used; preferred are smaller particles that increase the capacity of the adsorbent for arsenic removal. Examples are 14 x 28 mesh, more preferably 28 x 48 mesh.
- the high surface area material is impregnated with the iron salt solution using spray impregnation. It is preferred that the material and iron salt solution are agitated during the impregnating step. This agitation can be periodic or continuous.
- the impregnation step can occur in any suitable apparatus, one example being a rotating drum or the like, such as a pelletising drum or pan.
- the rotating drum preferably comprises internal vanes.
- the iron salt is preferably in the form of a solution and may be either a ferrous or ferric salt. Any suitable iron salt solution can be used, examples being the chloride and sulphate solutions.
- the optional oxidising step (ii) is used when the material is impregnated with a ferrous salt and is used to oxidise it to the ferric salt. The oxidation may simply be oxidation in air.
- the concentration of the iron solution is important in order to obtain the desired level of coating with the desired level of iron. In general, higher concentration strengths are preferred in order to obtain higher levels of iron coatings, for example 1 - 9% Fe, preferably 2 - 7% Fe, most preferably 3 - 5% Fe.
- the base is added until a pH of 5 - 9 is reached, preferably 6 - 8, more preferably 6.5 - 7.5.
- This treatment provides a hydrated ferric oxide coating by conversion of the iron salt to the hydrated ferric oxide coated over the material.
- the product resulting from the process of the invention comprises exposed material, that is material (for example alumina) which is not entirely covered by the hydrated ferric oxide coating.
- the base itself can be any suitable base, examples being sodium hydroxide or sodium carbonate solutions. Typical strengths are about 50% solutions.
- a water treatment method which method comprises contacting water to be treated with a water treatment product formed by the above method, and thereafter recovering treated water containing a reduced concentration of organic or inorganic materials.
- Batch treatment typically involves agitating the water to be treated with an aliquot of the water treatment product, the amount of which is chosen in order to achieve a desired degree of water purification in a desired time, typically more than 1 hour, generally 24-28 hours.
- Continuous methods are also possible as well known in the art.
- the water to be treated is passed through a column, bed, cartridge or the like which contains the water treatment product with Empty Bed Contact Time (EBCT) of typically 1-12 minutes depending on the size of the column.
- EBCT Empty Bed Contact Time
- the treated water has a reduced As concentration of not more than 20 ⁇ g/l, even more preferably not more than 10 ⁇ g/l, even more preferably not more than 3 ⁇ g/l.
- Optimum conditions for removal of organic materials and of inorganic materials are generally different. Depending on the nature of the contaminant to be removed, it may be advantageous to adjust the pH of the water in order to improve the performance of the water treatment product. Thus, for example, arsenic is best removed at a pH of 5 to 7 preferably 5.5, while fluoride is best removed at a pH of 6 to 8, preferably 7.
- Particulate materials having a high specific surface area show a high capacity for adsorbing contaminants and removing them from water.
- the high surface area materials used in this invention preferably have a specific surface area of at least 10m 2 /g, more preferably at least 50m 2 /g, and even more preferably at least 150m 2 /g.
- An upper limit may be, for example, 800 m 2 /g.
- the water treatment product produced by the method of this invention has a combination of useful properties including excellent capacity and avidity for rapidly adsorbing inorganic contaminants from water being treated, it is a robust material which is easily separable from treated water and can be treated to recover inorganic contaminants and so permit reuse without losing its structure.
- the solution pH of the ferric chloride treated granules was determined by mixing 1.0 g of the granules in 100 ml of water for 10 minutes. The pH of the ferric chloride treated granules was measured as 2.8 before NaOH addition.
- each adsorbent was pre-weighed into a 25 ml glass vial and adsorbent was washed with 20 ml of RO/DI water (reverse osmosis/deionized water). The washing was discarded. The washed adsorbent was quantitatively transferred to nalgene bottles containing 1 I of prepared NSF challenge water. The bottles were tightly closed and mixed for at least 72 h at room temperature on a laboratory shaker set at -150 rpm. The equilibrium arsenic concentration of each solution was measured by continuous hydride generation/inductively coupled plasma spectroscopy [Varian VGA-76P Vapor Generation Accessory with Varian Liberty 220 spectrometry system].
- NSF Challenge Water As (V) 0.3 mg/l, S0 4 50 mg/l, NQ 3 2.0 mg/l, F 1 mg/l, Si0 2 20 mg/l, PG 4 0.04 mg/l, Total alkalinity 160 mg/l)
- Table 2 shows an improved arsenic (V) adsorption capacity for adsorbents according to the invention over AA400G.
- results show that it may be preferred to adjust the pH of the water to be treated to achieve optimal results, in terms of unwanted materials from water.
- a further advantage is that the water treatment products prepared according to the invention do not need to be dried and do not form lumps or agglomerates.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Water Treatment By Sorption (AREA)
Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
NZ543609A NZ543609A (en) | 2003-05-15 | 2004-05-12 | Method of preparing a water treatment product |
AU2004238612A AU2004238612B2 (en) | 2003-05-15 | 2004-05-12 | Method of preparing a water treatment product |
EP04732355.5A EP1622716B1 (en) | 2003-05-15 | 2004-05-12 | Method of preparing a water treatment product |
ES04732355T ES2703816T3 (en) | 2003-05-15 | 2004-05-12 | Method to prepare a product for water treatment |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB0311154A GB0311154D0 (en) | 2003-05-15 | 2003-05-15 | Method of preparing a water treatment product |
GB0311154.9 | 2003-05-15 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2004101142A1 true WO2004101142A1 (en) | 2004-11-25 |
Family
ID=9958115
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/GB2004/002041 WO2004101142A1 (en) | 2003-05-15 | 2004-05-12 | Method of preparing a water treatment product |
Country Status (6)
Country | Link |
---|---|
EP (1) | EP1622716B1 (en) |
AU (1) | AU2004238612B2 (en) |
ES (1) | ES2703816T3 (en) |
GB (1) | GB0311154D0 (en) |
NZ (1) | NZ543609A (en) |
WO (1) | WO2004101142A1 (en) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2010029034A2 (en) * | 2008-09-12 | 2010-03-18 | Siemens Aktiengesellschaft | Method and device for removing impurities from water |
WO2014030080A1 (en) * | 2012-06-13 | 2014-02-27 | Universidad De Santiago De Chile | Inorganic nanoparticle, ferro-imogolite, and preparation process of said nanoparticle, for removing trace elements |
EP2666539A4 (en) * | 2011-01-21 | 2016-07-13 | Kyungpook Nat Univ Ind Acad | Method for manufacturing an organic-inorganic composite hybrid sorbent by impregnating an oxide into nanopores of activated carbon and method for using the method in water treatment |
US10525415B2 (en) | 2017-06-15 | 2020-01-07 | Saudi Arabian Oil Company | Processing systems for produced water and methods for recovering organic compounds from the produced water |
US11944952B2 (en) | 2021-05-28 | 2024-04-02 | Fuel Tech, Inc. | Removing contaminants from water with adsorbents |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA1067627A (en) * | 1976-08-20 | 1979-12-04 | Gerald D. Lutwick | Removal of arsenic from water |
JPS5916590A (en) * | 1982-07-20 | 1984-01-27 | Nippon Denki Kankyo Eng Kk | Treatment of waste water containing heavy metal |
WO1994006717A1 (en) * | 1992-09-18 | 1994-03-31 | I. Krüger Systems As | Method for the purification of metal-containing aqueous media and method of preparing an adsorbent |
WO1999050182A1 (en) * | 1998-04-01 | 1999-10-07 | Alcan International Limited | Water treatment product and method |
US6200482B1 (en) * | 1997-08-12 | 2001-03-13 | Adi International Inc. | Arsenic filtering media |
-
2003
- 2003-05-15 GB GB0311154A patent/GB0311154D0/en not_active Ceased
-
2004
- 2004-05-12 NZ NZ543609A patent/NZ543609A/en not_active IP Right Cessation
- 2004-05-12 EP EP04732355.5A patent/EP1622716B1/en not_active Expired - Lifetime
- 2004-05-12 WO PCT/GB2004/002041 patent/WO2004101142A1/en active Application Filing
- 2004-05-12 AU AU2004238612A patent/AU2004238612B2/en not_active Ceased
- 2004-05-12 ES ES04732355T patent/ES2703816T3/en not_active Expired - Lifetime
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA1067627A (en) * | 1976-08-20 | 1979-12-04 | Gerald D. Lutwick | Removal of arsenic from water |
JPS5916590A (en) * | 1982-07-20 | 1984-01-27 | Nippon Denki Kankyo Eng Kk | Treatment of waste water containing heavy metal |
WO1994006717A1 (en) * | 1992-09-18 | 1994-03-31 | I. Krüger Systems As | Method for the purification of metal-containing aqueous media and method of preparing an adsorbent |
US6200482B1 (en) * | 1997-08-12 | 2001-03-13 | Adi International Inc. | Arsenic filtering media |
WO1999050182A1 (en) * | 1998-04-01 | 1999-10-07 | Alcan International Limited | Water treatment product and method |
US6599429B1 (en) * | 1998-04-01 | 2003-07-29 | Alcan International Limited | Water treatment product and method |
Non-Patent Citations (2)
Title |
---|
DATABASE WPI Section Ch Week 198410, Derwent World Patents Index; Class D15, AN 1984-059133, XP002294812 * |
EDWARDS M; BENJAMIN M M: "ADSORPTIVE FILTRATION USING COATED SAND: A NEW APPROACH FOR TREATMENT OF METAL-BEARING WASTES", JOURNAL OF THE WATER POLLUTION CONTROL FEDERATION, vol. 61, no. 9/10, 1 September 1989 (1989-09-01), WASHINGTON, US, pages 1523 - 1533, XP000173147 * |
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2010029034A2 (en) * | 2008-09-12 | 2010-03-18 | Siemens Aktiengesellschaft | Method and device for removing impurities from water |
WO2010029034A3 (en) * | 2008-09-12 | 2010-05-27 | Siemens Aktiengesellschaft | Method and device for removing impurities from water |
EP2666539A4 (en) * | 2011-01-21 | 2016-07-13 | Kyungpook Nat Univ Ind Acad | Method for manufacturing an organic-inorganic composite hybrid sorbent by impregnating an oxide into nanopores of activated carbon and method for using the method in water treatment |
WO2014030080A1 (en) * | 2012-06-13 | 2014-02-27 | Universidad De Santiago De Chile | Inorganic nanoparticle, ferro-imogolite, and preparation process of said nanoparticle, for removing trace elements |
US20150166366A1 (en) * | 2012-06-13 | 2015-06-18 | Universidad De Santiago De Chile | Inorganic Nanoparticle, Ferro-Imogolite, and Preparation Process of Said Nanoparticle, for Removing Trace Elements |
JP2015527281A (en) * | 2012-06-13 | 2015-09-17 | ウニベルシダッド デ サンティアゴ デ チリ | Inorganic nanoparticles that are ferro-imogolites for removing trace elements from contaminated water and methods for preparing the nanoparticles |
US9670073B2 (en) * | 2012-06-13 | 2017-06-06 | Universidad De Santiago De Chile | Inorganic nanoparticle of magnetic ferro-imogolite for removing trace elements |
US10525415B2 (en) | 2017-06-15 | 2020-01-07 | Saudi Arabian Oil Company | Processing systems for produced water and methods for recovering organic compounds from the produced water |
US11944952B2 (en) | 2021-05-28 | 2024-04-02 | Fuel Tech, Inc. | Removing contaminants from water with adsorbents |
Also Published As
Publication number | Publication date |
---|---|
EP1622716A1 (en) | 2006-02-08 |
ES2703816T3 (en) | 2019-03-12 |
AU2004238612A1 (en) | 2004-11-25 |
EP1622716B1 (en) | 2018-10-03 |
GB0311154D0 (en) | 2003-06-18 |
NZ543609A (en) | 2009-03-31 |
AU2004238612B2 (en) | 2009-02-19 |
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