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WO2018108700A1 - Tamis revêtus et leur utilisation, specialement pour la séparation huile-eau - Google Patents

Tamis revêtus et leur utilisation, specialement pour la séparation huile-eau Download PDF

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Publication number
WO2018108700A1
WO2018108700A1 PCT/EP2017/081878 EP2017081878W WO2018108700A1 WO 2018108700 A1 WO2018108700 A1 WO 2018108700A1 EP 2017081878 W EP2017081878 W EP 2017081878W WO 2018108700 A1 WO2018108700 A1 WO 2018108700A1
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WO
WIPO (PCT)
Prior art keywords
mesh
water
oil
separation
threads
Prior art date
Application number
PCT/EP2017/081878
Other languages
English (en)
Inventor
Friederike Fleischhaker
Sung Yeun Choi
Kai BERGNER
Stefanie RUNCK
Aron WOSYLUS
Original Assignee
Basf Se
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
Application filed by Basf Se filed Critical Basf Se
Priority to EP17811296.7A priority Critical patent/EP3554666A1/fr
Priority to EA201991326A priority patent/EA201991326A1/ru
Publication of WO2018108700A1 publication Critical patent/WO2018108700A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02—Separation of non-miscible liquids
    • B01D17/04—Breaking emulsions
    • B01D17/045—Breaking emulsions with coalescers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/08—Thickening liquid suspensions by filtration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/10—Filter screens essentially made of metal
    • B01D39/12—Filter screens essentially made of metal of wire gauze; of knitted wire; of expanded metal
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G33/00—Dewatering or demulsification of hydrocarbon oils
    • C10G33/06—Dewatering or demulsification of hydrocarbon oils with mechanical means, e.g. by filtration
    • D—TEXTILES; PAPER
    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D1/00—Woven fabrics designed to make specified articles
    • D—TEXTILES; PAPER
    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/40—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the structure of the yarns or threads
    • D03D15/43—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the structure of the yarns or threads with differing diameters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/04—Additives and treatments of the filtering material
    • B01D2239/0414—Surface modifiers, e.g. comprising ion exchange groups
    • B01D2239/0421—Rendering the filter material hydrophilic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/12—Special parameters characterising the filtering material
    • B01D2239/1216—Pore size
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2101/00—Inorganic fibres
    • D10B2101/20—Metallic fibres
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00—Physical properties
    • D10B2401/06—Load-responsive characteristics
    • D10B2401/062—Load-responsive characteristics stiff, shape retention
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2505/00—Industrial
    • D10B2505/04—Filters

Definitions

  • the present invention relates to methods for the separation of a liquid mixture comprising water, especially for oil-water separation, comprising the step of contacting a liquid mixture comprising at least one hydrophobic liquid and water with a hydrophilically coated mesh allowing water to pass through the mesh while at least part of the hydrophobic liquid remains on the mesh as well as such hydrophilically coated meshes and their use.
  • Oil-water separation is a worldwide challenge.
  • Typical separation problems comprise the sepa- ration emulsions of crude oil and (formation) water, the separation of industrial oily waste water or separation in connection with the removal of oil spills.
  • materials which are capable of selectively absorbing organic solvents including but not limited to oils.
  • examples comprise open-cell foams based on a mela- mine-formaldehyde modified with a hydrophobic coating such as disclosed in
  • J. K. Yuan, X. G. Liu, O. Akbulut, J. Q. Hu, S. L. Suib, J. Kong, F. Stellacci, Nat. Nanotechnol. 2008, 3, 332 disclose superwetting nanowire membranes for selective absorption. Such membranes are obtained by coating nanowire membranes with silicones. It has also been suggested to use meshes for separation of oil and water. Meshes are widely known for various applications. Especially wire weaves can be used as suitable meshes.
  • the coating is performed by using a homogeneous emulsion comprising 50 % by wt. of water, 30 % by wt. of polytetrafluoro- ethylene (teflon), 10 % by wt. of polyvinylacetate as adhesive, 8 % by wt. of polyvinylalcohol as dispersant 2% dodecylbenzenesulfonate as surfactant.
  • teflon polytetrafluoro- ethylene
  • dispersant 2% dodecylbenzenesulfonate as surfactant.
  • the netting described has the opposite separation characteristics than the netting described by L. Feng et al. A drop of water can pass through the netting while oil remains on the netting. Such materials have the advantage that they are easy to clean, the equipment is reusable, the oil-phase can be processed after separation and the equipment is protected from oil-fouling.
  • an object of the present invention is to provide such methods and separation means.
  • the object is also achieved by a hydrophilically coated mesh as defined herein.
  • the coated mesh of the present invention can be used for the separation of water from a liquid mixture comprising water, especially for oil-water separation.
  • Another aspect of the present invention is the use of the coated mesh of the present invention for the separation of water from a liquid mixture comprising water and a hydrophobic liquid, especially for oil-water separation.
  • Another aspect of the present invention is a device for cross-flow filtration comprising a hydrophilically coated mesh of the present invention. Surprisingly it has been found that improvement of the aforementioned separation is possible by using a coated mesh with specific weaving characteristics.
  • the liquid mixture to be separated comprises water and a hydrophobic liquid.
  • hydrophobic liquid as used herein encompasses any kind of organic liquids which is immiscible or only partially miscible with water. Accordingly a hydrophobic liquid is a single hydrophobic liquid substance or a mixture of two or more hydrophobic liquid substances.
  • hydrophobic liquids examples include hydrocarbons, such as aliphatic and/or aromatic hydrocarbons, like n-hexane or n-dodecane, in particular hydrocarbons having a boiling point of more than 150 °C, and oil, like crude oil, mineral oils such as diesel oil, gasoline, heavy fuel oil, engine oil, like motor oil, vege- table oils such as coconut oil, tall oil or rape oil, or synthetic oils such as silicone oils.
  • hydrocarbons such as aliphatic and/or aromatic hydrocarbons, like n-hexane or n-dodecane, in particular hydrocarbons having a boiling point of more than 150 °C
  • oil like crude oil, mineral oils such as diesel oil, gasoline, heavy fuel oil, engine oil, like motor oil, vege- table oils such as coconut oil, tall oil or rape oil, or synthetic oils such as silicone oils.
  • the hydrophobic liquid is oil, especially crude or refined oil.
  • the liquid mixture of water and the hydrophobic liquid shall include any kind of mixtures of the hydrophobic liquid (HL) and water comprising a HL phase and a water phase, including but not limited to HL-water emulsions or water-HL emulsions, in particular emulsions of oil, especially crude oil and water such as formation water or sea water.
  • the liquid mixture to be separated is a mixture of crude oil and water, in particular a mixture of crude oil and water.
  • Examples of specific water-oil separation processes include separation processes in course of oil production and oil refining, such as the separation of crude oil and water produced from an oil bearing formation, the separation of heavy oil from oil sands tailings or heavy oil obtained from steam assisted gravity drainage (SAGD) techniques, de-oiling of water, oil sludge dewater- ing or the removal of hydrocarbons from drilling fluids. Further examples comprise the separation of oil-water mixtures from tank bottoms at refineries or other storage facilities, collection points for disposable waste oils, waste from chemical factories, ballast water or the removal of oil spills.
  • SAGD steam assisted gravity drainage
  • the method according to the present invention for the separation of the liquid mixture comprises the step of contacting the liquid mixture with a hydrophilically coated mesh allowing water to pass through the mesh while at least part of the hydrophobic liquid remains on the mesh.
  • water is at least partly separated off from the mixture resulting in a remaining mixture with increased fraction of hydrophobic liquid.
  • separation includes partial and full separation of water.
  • water is separated off to at least 50 % (v/v), more preferred to at least 60 %(v/v), even more preferred to at least 70 % (v/v), even more preferred to at least 75 % (v/v), even more preferred to at least 80 % (v/v), even more preferred to at least 85 % (v/v), even more preferred to at least 90 % (v/v), even more preferred to at least 95 % (v/v), even more preferred to at least 96 % (v/v), even more preferred to at least 97 % (v/v), even more preferred to at least 98 % (v/v), even more preferred to at least 99 % (v/v), even more preferred to at least 99.5 % (v/v), even more preferred to at least 99.9 % (v/v).
  • the mixture may be pressed against the mesh.
  • the force applied may simply be gravity forces but of course also elevated pressure may be applied. Due to the hydrophilic surface properties of the coated mesh, water may pass through the mesh while the passage of oil through the mesh is impeded so that at least part of the oil is retained on the mesh and may be removed from the mesh.
  • a separating device which at least comprises: a first chamber at least comprising an inlet for fluids and an outlet for fluids, wherein the first chamber is connected with a second chamber at least comprising an outlet for fluids and wherein furthermore the coated mesh according to this invention separates the first chamber from the second chamber.
  • the device is a device for cross-flow filtration.
  • another aspect of the present invention is a device for cross-flow filtration comprising a hydrophilically coated mesh according to the present invention.
  • the mixture to be separated is allowed to flow into the first chamber.
  • a suitable pressure selected by the skilled artisan may be applied.
  • Water or at least part of the water of the oil-water mixture passes through the mesh into the second chamber and may be recovered from the second chamber from the outlet of the second chamber.
  • the hydrophobic liquid, like oil, or a mixture with decreased water content may be recovered from the outlet of the first chamber.
  • the process may be continuous or discontinu- ous. In a preferred embodiment the process is a continuous cross-flow filtration. If one separating step is not sufficient to separate oil and water completely the separation step may be repeated using the same or another device. For example for separating a cascade of two or more of the devices described successively assembled may be used.
  • a separator for the separation of the hydrophobic liquid, e.g. crude oil, and water may be used as described in WO 2015/180 872 A1 and which is equipped with meshes according to the present invention.
  • a schematic representation of such a separator is shown in Fig. 1 .
  • the separator is a cylinder shaped hollow body which at least comprises an inlet for an oil-water mixture, an oil bucket for separated oil, outlets for separated water and separated oil and furthermore a mist extractor and an outlet for separated gas.
  • Meshes may be incorporated vertically (1 a) or almost vertically (1 b) into the separator at a location close to the inlet for the oil-water emulsion.
  • a mesh (1 c) may also be incorporated horizontally.
  • the inlet for the oil-water emulsion is located above the mesh so that the mixture may be separated into oil and water under the influence of gravity.
  • a mesh may fur- thermore be used as water weir (3) and/or in the mist extractor (2).
  • the skilled artisan may use meshes in an oil-water separator in another manner.
  • the mesh used in the separation of the mixture is a weave with a geometric pore size of less than 100 ⁇ having warp threads, the warp threads having a diameter d w , and shute threads, the shute threads having a diameter d s , wherein d s and d w differ by at least a factor of 1 .1 and wherein the surface of the mesh is at least partly covered by a hydrophilic coating, the hydro- philic coating having a contact angle for water of less than 10°
  • the threads are preferably made of metals such as steel, stainless steel, bronze, brass, or alu- minum or polymeric materials such as polyethylene, polypropylene, polyacrylamide, or polyeth- ersulfone or natural fibers such as cotton, cellulose or mixtures thereof, preferably made of metals (wires), more preferably stainless steel.
  • metals such as steel, stainless steel, bronze, brass, or alu- minum or polymeric materials such as polyethylene, polypropylene, polyacrylamide, or polyeth- ersulfone or natural fibers such as cotton, cellulose or mixtures thereof, preferably made of metals (wires), more preferably stainless steel.
  • the weave is a woven wire cloth, especially a zero aperture filter cloth.
  • the shute and warp threads are shute and warp wires.
  • wire cloths are known in the art.
  • plain weave with single wires of same diameter forming apertures, typically forming rectangular apertures the wires are pressed closely together in zero aperture filter cloths (D.B. Purchas, K. Sutherland, Handbook of Filter Media, second edition (2002), chapter 6.2, Elsevier Sience Ltd., Oxford).
  • the weave according to the present invention is characterized by warp threads, the warp threads having a diameter d w , and shute threads, also known as weft threads, the shute threads having a diameter d s .
  • warp threads the warp threads having a diameter d w
  • shute threads also known as weft threads
  • the shute threads having a diameter d s .
  • meshes have warp and shute threads of same diameter, which are woven by alternating the shute thread over and under the warp threat (Plain weave).
  • the weave according to the present invention has different diameters ds/dw (Dutch type weave).
  • the diameters d s and d w differ by at least a factor of 1 .1. More preferable the diameters differ by at least a factor of 1 .3, even more preferably by at least 1.5, even more pref- erably at least 1 .8, even more preferably at least 2.0, even more preferably at least 2.2 and even more preferably at least 2.4.
  • the diameter d w is greater than ds.
  • ds is greater than d w (Reverse Dutch weave). Reversed Dutch type weave is preferred.
  • each shute thread crosses the warp threads by going over one and then under the next (Plain Dutch weave) or the shute thread passes over one or more warp threads and then under two or more warp threads (Twilled Dutch weave). Plain Dutch weave is more preferred.
  • Such weaves are commercially available.
  • filter clothes such as filter clothes of Haver & Boecker, Oelde, Germany.
  • Minimesh SPW single plain Dutch weave
  • Minimesh HIFLO single plain Dutch weave
  • RPD HIFLO-S reverse plain Dutch weave
  • DTW twilled Dutch weave
  • BMT twilled Dutch weave
  • BMT-ZZ twilled Dutch weave
  • RPD reverse plain Dutch weave
  • TRC twilled reverse plain Dutch weave
  • SPW single plain Dutch weave
  • Preference is given to RPD HIFLO-S and RPD, even more preferred is RPD HIFLO-S.
  • the warp and shute threads may have different pattern. All patterns can be used as long as warp and shute threads are different in size as described herein. In case different warp and shute threads are used, diameters refer to the average diameter. It is clear to the practitioner in the art that due to the weaving process diameter of the threads can be changed slightly. Thus the diameters refer to the thread diameters used before weaving. Technical requirements and testing are described in DIN ISO 9044:2001 -09.
  • a wire cloth can be used comprising warp wires and shute (weft) wires crossing each other and interwoven by a weave pattern, said warp wires being formed in at least two different configurations to define warp wires of first and second types, wherein a length of the first type of warp wires deviates from a length of the second type of warp wires in relation to a particular length unit, wherein pores are formed in interstices between sections of two neighboring warp wires and crossing sections of two neighboring weft wires.
  • a longer one of the first and second types of the warp wires loops around the weft wires by substantially 360°, with confronting sections of two spaced-apart warp wires touching one another.
  • the wire cloth can be treated by at least one process consisting of compacting and stabilization by thermal treatment, like calendaring or sintering.
  • the first and second types of warp wires can have a waved configuration of different degrees to define warp wires of low waviness and warp wires of high waviness.
  • the wave height of the warp wires of high waviness is a multiple of a wave height of the warp wires of low waviness.
  • the warp wires of first and second types of warp wires can define an alternating pattern of low waviness and high waviness.
  • the warp wires of first and second types of warp wires define in direction of the weft wires a pattern in which a number of warp wires of low waviness follow one another and a number of warp wires of high waviness follow one another.
  • the warp wires of first and second types of warp wires can define in direction of the weft wires a pattern in which a number of warp wires of low waviness is different than a number of warp wires of high waviness.
  • the weft wires can be placed in alternating vertically offset rela- tionship.
  • the warp wires of first and second types of warp wires can have a same or different diameter.
  • the warp wires of first and second types of warp wires can define a pattern in which the number of warp wires of first and second types of warp wires varies, with the weft wires woven substantially planar.
  • the thread with the larger diameter has a diameter in the range from 0.02 mm to 0.3 mm, more preferably 0.03 mm to 0.2 mm, even more preferably 0.04 mm to 0.1 mm, even more preferably 0.05 mm to 0.09 mm, even more preferably 0.06 mm to 0.08 mm.
  • the thread with the smaller diameter has a diameter in the range from 0.01 mm to 0.2 mm, more preferably 0.01 mm to 0.1 mm, even more preferably 0.01 mm to 0.08 mm, even more preferably 0.01 mm to 0.05 mm.
  • the geometric pore size is less than 50 ⁇ , more preferably in the range of 1 ⁇ to ⁇ 50 ⁇ , even more preferably the pore size is in the range of 5 ⁇ to ⁇ 50 ⁇ , even more pref- erably from 5 to 40 ⁇ .
  • the geometric pore size can be determined using the so called glass bead test. Accordingly the pore size represents the largest geometrical determined pore size verified by the glass bead test, typically with a tolerance of 5%. In said test a suspension containing glass beads is passed through the mesh - the diameter of the largest bead passing through is considered as the geometric pore size.
  • the mesh count is 1 15 to 380 MESH in one direction (warp or shute direction) and 325 to 850 MESH in the other direction (shute or warp direction).
  • the dimension MESH refers to the number of apertures per English inch.
  • Exemplary mesh counts are 850x380 (5, 10 or 15 ⁇ pore size), 640x200 (20 ⁇ pore size), 425x150 (25 or 30 ⁇ pore size), 325x1 15 (40 ⁇ pore size). Due to the different diameter of the shute and warp threads the number of meshes are also different with regard to warp and shute direction.
  • the hydrophilic coating has a contact angle for water of less than 10°, preferably less than 5°.
  • the hydrophilic coatings described in the following are considered to fulfill this requirement.
  • the contact angle can be measured by a contact angle goniometer. Surfaces with contact angles greater than 90° are typically designated as hydrophobic.
  • the hydrophilic coating having a contact angle for water of less than 10° comprises hydrated aluminum oxide or a hydrophilic polymer crosslinked by heat or radiation curing, pref- erably comprising hydrated aluminium oxide.
  • the hydrophilic coating has a thickness of 50 nm to 5000 nm, more preferably 50 nm to 2000 nm, even more preferably 50 nm to 500 nm, even more preferably 50 nm to 200 nm, even more preferably 100 nm to 200 nm or 50 nm to 150 nm.
  • the hydrophilic coating having a contact angle for water of less than 10° comprising, preferably consisting of, hydrated aluminum oxide is described in WO 2015/180 872 A1 .
  • the mesh to be used for the separation according to this invention comprises preferably a surface comprising hydrated aluminumoxide.
  • “Hydrated aluminium oxides” include al- uminiumoxyhydroxides, such as a-AIOOH or y-AIOOH having a defined crystalline structure but also aluminumoxyhydroxides having a less defined structure, i.e. products being amorphous or having at least amorphous portions.
  • “Hydrated aluminum oxides” may comprise besides aluminium ions also other metal ions such as for instance ferric ions being understood that usually at least 90 mol % of the metal ions present are aluminum ions.
  • the surface of the mesh comprises ⁇ - ⁇ which is also known as Boehmite.
  • the thickness of layer of hydrated aluminum oxides on the surface of the mesh typically may be 50 nm to 500 nm, preferably 100 nm to 200 nm.
  • the mesh according to the invention may be made by converting the surface of an aluminum mesh to a surface comprising hydrated aluminum oxides or by coating a mesh of another material, for instance a mesh of stainless steel with aluminum or aluminum compounds such as aluminum oxides and converting the coating to hydrated aluminum oxides.
  • a surface-modified mesh comprising a surface comprising hydrated aluminumoxide, preferably ⁇ - ⁇ can be obtained.
  • the modified surface provides hydrophilic, preferably superhydrophilic properties to the mesh thereby rendering it suitable for separation of a mixture of water with a hydrophobic liquid, such as oil.
  • a hydrophobic liquid such as oil.
  • the term "superhydrophilic” means that the contact angle for oil is preferably > 150° while the contact angle for water is below ⁇ 5°.
  • Such coating is suitable to provide a hydrophilic surface with a contact angle of less than 10°.
  • a mesh as described above is coated with aluminum or aluminum oxide.
  • Any technology for coating may be used.
  • suitable coating tech- nologies include physical vapor deposition methods such as thermal evaporation, sputtering, electron beam evaporation techniques, or CVD technologies. Such techniques are known to the skilled artisan and are for example disclosed in Mahan, John E. "Physical Vapor Deposition of Thin Films” New York: John Wiley & Sons, 2000; Dobkin and Zuraw (2003) “Principles of Chemical Vapor Deposition”; or or Kluwer, Smith, Donald (1995) "Thin-Film Deposition: Princi- pies and Practice” McGraw-Hill.
  • aluminum layer can be deposited on the mesh using thin aluminum flakes.
  • the thickness of aluminum flakes may be 5 nm to 500 nm, preferably 5 nm to 50 nm.
  • the flakes wrap the thread and bind on the thread surface.
  • the thickness of the layer of aluminum or aluminum oxide is selected by the skilled artisan ac- cording to his/her needs and usually is from 50 nm to 500 nm, preferably 100 nm to 200 nm.
  • Layers of aluminum /aluminum oxide may also be coated onto the mesh by sol-gel methods followed by thermal treatment. Also such techniques are known to the skilled artisan and are for example disclosed in C. Jeffrey Brinker, George W. Scherer (Hrsg.) "Sol Gel Science. The Physics and Chemistry of Sol-Gel Processing. The Physics and Chemistry of Sol-gel Processing", Academic Press, Boston (1990) or Kim, Philseok; Kreder, Michael J.; Alvarenga, Jack; et al. NANO LETTERS Volume: 13 Issue: 4 Pages: 1793-1799 Published: APR 2013.
  • the uncoated mesh may be precoated with an adhesion layer.
  • an adhesion layer may be a layer of Cr or Ti which also may be applied by using by physical vapor deposition methods but also layers of other oxides may be possible.
  • the thickness of such an additional coating may be from 1 to 20 nm, for example 3 to 10 nm.
  • the coating is con- verted into hydrated aluminum oxides, preferably ⁇ - ⁇ , by treating the coating with water, preferably deionized water, or water vapor at a temperature above room temperature, preferably more than 50°C and more preferably more than 95°C.
  • the coated mesh may be put into boiling water.
  • the duration of the treatment with water is selected by the skilled artisan according to his/her needs and may be from 10 to 40 min, preferably 15 to 30 min.
  • hydrated aluminum oxides can be directly formed on the mesh starting from soluble aluminum sources. Under the controlled pH and temperature, hydrated aluminum oxides can be deposited on the mesh by precipitation from the solution of such aluminum sources, like aluminates or aluminum salts. Said method is further described in B. Dash, I. N. Bhattacharya B. K. Mishra ..Precipitation and Dehydration of Hydrated Alumina", Lambert Academic Publishing (2014), or US 2 935 376 A.
  • the thickness of the layer of hydrated aluminum oxides on the surface of the mesh usually is from 50 nm to 1 ⁇ , preferably 100 nm to 500 nm.
  • the present invention also relates to a mesh comprising a surface comprising hydrated aluminum oxides, in particular a surface comprising ⁇ - ⁇ which is available by the methods of the first embodiment described above.
  • a mesh comprising a surface comprising hydrated aluminum oxides, in particular a surface comprising ⁇ - ⁇ which is available by the methods of the first embodiment described above.
  • an aluminum mesh is used as starting material.
  • the mesh size may be chosen by the skilled artisan according to his/her needs.
  • the mesh size may be from 10 ⁇ to 100 ⁇ , for example 40 ⁇ to 60 ⁇ . Further details of unmodified meshes to be used have been described above and we explicitly refer to the description.
  • the surface of the mesh is converted into hydrated aluminum oxides, preferably ⁇ - AIOOH by treating the mesh with water at a temperature above room temperature, preferably more than 50°C.
  • the aluminum mesh may be put into boiling water for about 10 to 40 min, preferably 15 to 30 min.
  • the present invention also relates to a mesh comprising a surface comprising hydrated aluminum oxides, in particular a surface comprising ⁇ - ⁇ which is available by the method of the second embodiment described above.
  • hydrophilic coating having a contact angle for water of less than 10° comprising, preferably consisting of, a hydrophilic polymer crosslinked by heat or radiation curing is described in WO 2015/180 873 A1. Accordingly in a first aspect a method of manufacturing a coated mesh is described in
  • the method comprises coating a mesh with a curable coating composition and curing the coating by irradiation with UV comprising radiation and/or by annealing wherein the coating composition comprises at least ⁇ a polar solvent or solvent mixture,
  • the method comprises coating a mesh with a photochemically curable coating composition and curing the coating by irradiation with UV comprising radiation wherein the coating composition comprises at least
  • a polar solvent or solvent mixture comprising at least 70 % by wt. of water relating to the total of all solvents used
  • hydrophilic crosslinker comprising at least two ethylenically unsaturated groups, ⁇ a hydrophilic photoinitiator, and
  • a hydrophilic polymeric adhesion agent comprising acrylic acid.
  • the coated mesh is available by coating an uncoated mesh with a curable coating composition followed by thermally and/or photochemically curing the coating.
  • the coating provides hydrophilic surface properties to the mesh.
  • a suitable pre-coating may be applied before coating the mesh.
  • the curable coating composition may be a thermally and/or photocurable composition, preferably a photocurable composition. It provides hydrophilic, preferably superhydrophilic properties to the mesh coated with the formulation so that it may be suitable for oil-water separation.
  • hydrophilic means that the contact angle for an oil is > 150° while the contact angle for water is ⁇ 5°.
  • Such coating is suitable to provide a hydrophilic surface with a contact angle of less than 10°.
  • the curable coating composition comprises at least a polar solvent, a hydrophilic coating precursor, a hydrophilic crosslinker, a hydrophilic initiator and a hydrophilic, polymeric adhesive agent.
  • the curable coating composition comprises at least a polar solvent.
  • the polar solvent may be water or an organic solvent miscible with water.
  • Examples of polar organic solvents miscible with water comprise alcohols such as methanol, ethanol, propanol, isopropanol or ketones such as acetone.
  • the solvent at least comprises water. Besides water one or more than one additional polar organic solvents solvent miscible with water as defined above may be used.
  • the solvent comprises at least 50 % by wt. of water relating to the total of all solvents, preferably at least 70 % by wt. of water, more preferably at least 85 % by wt., and most preferably only water is used as solvent.
  • the amount of polar solvent(s) in the curable coating composition may be selected by the skilled artisan according to his/her needs. Generally, the amount of polar solvent(s) is from 20 % by. wt. to 90 by wt., preferably 40 % by wt. to 60 by wt. % relating to the total of all components of the curable coating composition.
  • the coating precursors are hydrophilic components and are selected from the group of hydrophilic, polymerizable monomers, preformed hydrophilic oligomers and polymers. Oligomers and polymers themselves may also comprise polymerizable group.
  • the crosslinkable composition comprises at least one monoethylenically unsaturated, hydrophilic monomer with the proviso that at least one of the monomers is (meth)acrylamide, preferably acrylamide.
  • the hydrophilic monomers, oligomers or polymers used are miscible with water in any ratio, but it is sufficient for execution of the invention that the components dissolve in the coating composition.
  • the solubility of the hydrophilic monomers in water at room temperature should be at least 50 g/l, preferably at least 100 g/l.
  • acrylamide preferably acrylamide other monoethylenically unsaturated mono- mers may be used as comonomers.
  • further monomers comprise monomers comprising COOH-groups such as (meth)acrylic acid, fumaric acid, itaconic acid, crotonic acid, or maleic acid, monomers comprising other acid groups such as vinylphosphonic acid, esters of hydroxyethyl or hydroxypropyl(meth)acrylate with (poly)phosphoric acid, allylphosphonic acid, 2- acrylamido-2-methylpropanesulfonicacid, or vinylsulfonic acid, hydrophilic (meth)acrylates, for instance amino(meth)acrylates or such as dimethylaminoethyl(meth)acrylate, dimethyla- minopropyl(meth)acrylate, 2-(2-dimethylaminoethyloxy)ethyl (meth)acrylate or ami- no(meth)acrylamides
  • a monomer mixture comprising at least 50 % by wt. of (meth)acrylamide, preferably acrylamide, more preferably at least 75 % by wt. of (meth)acryl amide, preferably acrylamide may be used.
  • (meth)acrylamide preferably acrylamide is used as monomer.
  • preformed hydrophilic oligomers or hydrophilic polymers may be used.
  • preformed polymers or oligomers comprise homopolymers or copolymers of the monomers mentioned above such as polyacrylamide or polyvinylpyrrolidone. Further examples comprise polyethyleneglycol or polyethyleneimine.
  • the amount of monomers and/or oligomers and/or polymers in the curable coating composition may be from 2 % by wt. to 80 % by wt., preferably from 40 % by wt. to 60 % by wt. with respect to the total of all components of the coating composition.
  • monomers are used as coating precursor.
  • the curing coating composition furthermore comprises at least one hydrophilic crosslinker, i.e. components comprising at least two polymerizable groups.
  • the precursor For reacting with monoethylenically unsaturated monomers the precursor comprises at least two ethylenically unsaturated groups.
  • the crosslinkers used are miscible with water in any ratio, but it is sufficient for execution of the invention that the components dissolve in the coating composition.
  • the solubility of the crosslinkers in water at room temperature should be at least 50 g/l, preferably at least 100 g/l.
  • hydrophilic crosslinkers comprise water soluble multifunctional acrylates, - acrylamides such as oligoethyleneglycoldiacrylat.es or ⁇ , ⁇ '- methylene bis acrylamide. Such crosslinkers are particularly preferred if monomers are used in the coating composition.
  • oligomeric or polymeric precursors are used also such crosslinkers may be used. In one embodiment they are used together with additional monomers.
  • the amount of crosslinkers in the coating composition may be selected by the skilled artisan according to his/her needs. Generally, the amount may be from 0.5 to 10 % by wt, preferably 0.5 to 5 % by wt. with respect to the total of all components of the coating composition.
  • Hydrophilic initiators for initiating curing may be initiators for thermally initiating polymerization and/or photoinitiators. Preferably, photoiniators are used.
  • the initiators used are miscible with water in any ratio, but it is sufficient for execution of the invention that the components dissolve in the coating composition.
  • photoinitiators comprise 2,2'-diethoxyacetophenone, mixtures of benzophenone and 2,2'-diethoxyacetophenone, oxy-phenyl-acetic acid 2-[2 oxo-2 phenyl-acetoxy-ethoxy]-ethyl ester and oxy-phenyl-acetic 2-[2-hydroxy-ethoxy]-ethyl ester, or phosphine oxides such as phenyl bis (2, 4, 6-trimethyl benzoyl) phosphine oxide.
  • phosphine oxides such as phenyl bis (2, 4, 6-trimethyl benzoyl) phosphine oxide.
  • a mixture of two or more initiators may be used.
  • thermal initiators comprise water soluble azo initiators or peroxo initiators.
  • the amount of initiators in the coating composition may be selected by the skilled artisan ac- cording to his/her needs. Generally, the amount may be from 0.5 to 7 % by wt., preferably 1 to 5 % by wt. with respect to the total of all components of the coating composition.
  • the curing composition furthermore comprises at least one hydrophilic polymeric adhesion agent.
  • the polymeric adhesion agent comprises acidic groups.
  • the adhesion agents used are miscible with water in any ratio, but it is sufficient for execution of the invention that the components dissolve in the coating composition.
  • the polymeric adhesion agent comprises at least carboxylate -COOH groups.
  • the polymeric adhesion agent may in particular comprise monoethylenically unsaturated monomers comprising acidic groups, preferably -COOH groups.
  • suitable polymeric adhesion agents comprise polyacrylic acid or homopolymers or copolymers of fumaric acid, itaconic acid, crotonic acid, maleic acid, methacrylic acid and acrylic acid.
  • the adhe- sion agent comprises at least (meth)acrylic acid, preferably acrylic acid.
  • polyacrylic acid is used, preferably polyacrylic acid having a weight average molecular weight M w of more than 1 ,000,000 g/mol, for example 1 ,000,000 g/mol to 5,000,000 g/mol.
  • the amount of adhesion agents in the coating composition may be selected by the skilled artisan according to his/her needs. Generally, the amount may be from 0.1 to 5% by wt., preferably 0.2 to 2 % by wt. with respect to the total of all components of the coating composition.
  • the curing composition may of course comprise further components. Such further components may be used modifying and/or fine-tuning the properties of the coating.
  • the coating components are made by mixing all components of coating composition.
  • an uncoated mesh which optionally might have been precoated is coated with the curing coating composition described above.
  • Such coating may be performed by dipping an uncoated mesh into the coating composition.
  • the coating composition may be sprayed onto the uncoated mesh.
  • the thickness of the coating may be selected by the skilled artisan according to his/her needs. In one embodiment it may be from 0.5 ⁇ to 2 ⁇ .
  • compositions comprising photoinitiators crosslinking is started by irradiating the meshs comprising an uncured coating with UV- or UV/VIS - radiation, for instance with a radia- tion of about 365 nm.
  • compositions comprising thermal initiators crosslinking is started by annealing the mesh coated with an uncured coating.
  • the process of coating the uncoated mesh may comprise additional steps.
  • the mesh may be cleaned in an additional step before coating.
  • Such a cleaning step may comprise removing organic impurities from a metal mesh using organic solvents such as acetone.
  • the mesh may be precoated with adhesion agents before coating it with the curable composition.
  • suitable adhesion agents comprise in particular the polymeric adhesion agents as described above.
  • the curing coating composition comprises at least a polar solvent or solvent mixture comprising water in an amount of at least 70 % by wt. of water relating to the total of all solvents used.
  • the amount of water is at least 85 % by wt., and more preferably only water is used as solvent.
  • the preferred curing coating composition comprises at least one hydro- philic, monoethylenically unsaturated monomer, with the proviso that at least 50 % by wt. relating to the total amount of all monomers used is (meth)acryl amide, preferably acrylamide.
  • (meth)acryl amide preferably acrylamide.
  • Suitable hydro- philic comonomers which may be used besides (meth)acrylamide have already been described above.
  • the preferred curing coating composition comprises at least a hydro- philic crosslinker comprising at least two ethylenically unsaturated groups. Examples of such crosslinkers have already been described above.
  • the preferred curing coating composition comprises at least a hydro- philic photoinitiator. Examples of such photoinitiators have already been described above.
  • the preferred curing coating composition comprises at least one hydro- philic polymeric adhesion agent comprising (meth)acrylic acid, preferably acrylic acid.
  • the adhesion agent comprises polyacrylic acid, preferably polyacrylic acid having a weight average molecular weight M w of more than 1 ,000,000 g/mol, for example 1 ,000,000 g/mol to 5,000,000 g/mol.
  • the thickness of the curing coating may be selected by the skilled artisan according to his/her needs. In one embodiment it may be from 0.5 ⁇ to 2 ⁇ .
  • the coated meshes can be used for the separation of water from a liquid mixture comprising water and a hydrophobic liquid, especially for oil-water separation.
  • the coated meshes may be used waste in water treatment, water purification, or in oil/gas industry.
  • Fig. 1 Schematic representation of an oil-water separator equipped with meshes
  • Fig. 2 Schematic representation of the testing device for the meshes
  • Pore size 50 ⁇ , MESH 325, d s :d w * 1
  • the meshes as specified in item 1 were cut into pieces with a size 6 cm x 6 cm.
  • the resulting metal grid pieces were cleaned with acetone, deionized water and again acetone and dried with air.
  • the Al layer was converted into aluminum oxyhydroxide by putting the coated grids into boiling deionized water for 30 min. All contact angles of the hydrophilically coated meshes are below 10°.
  • test mixtures of water and hydrophobic liquid (all Vol-%A/ol.-%) were used:
  • the water phase was colored blue for better visibility with methylene blue.
  • the percentage of oil phase (vol-% relating to the total volume of oil used for the test) that is not held back by the mesh and passes through the mesh is listed in Tables 1 and 2. Since at least three reproduction experiments were performed per mesh and mixture a range may be provided.
  • a stainless steel (1 .4404) mesh, Minimesh ® RPD HIFLO-S (Haver & Boecker) with 20 ⁇ , 10 ⁇ and 5 ⁇ of pore size were cleaned as described in Example 1 .
  • the cleaned filter cloth was immersed in 0.2 wt.-% aluminum flake dispersion made of Metasheen® 41 (BASF) and /- propanol for 1 minute. After 3 times immersion, the coated filter clothes were dried at room temperature on the bench for overnight.
  • the Al layer was converted into aluminum oxyhydroxide by putting the coated filter clothes into boiling deionized water for 30 min. Separation test was carried out as described in Example 1.
  • a stainless steel (1 .4404) mesh, Minimesh ® RPD HIFLO-S (Haver & Boecker) with 20 ⁇ , 15 ⁇ and 10 ⁇ m of pore size were cleaned as described in Example 1.
  • the cleaned filter cloth was immersed in 1 L of Dl water. Using 0.5M NaOH solution, pH raised to 9.7. Hydrated alumina precipitation was carried out at 60°C and pH 9.7 using 4.6w% Sodium Aluminate solution and 7w% HCI solution.
  • the coated filter cloth was washed with Dl water in a sonication bath for 10 s and dried at room temperature.
  • a stainless steel (1 .4404) mesh, Minimesh ® RPD HIFLO-S (Haver & Boecker) with 20 ⁇ , 10 ⁇ and DTW-S, and RPD-S (Haver & Boecker) with 20 ⁇ m of pore size were cleaned as de- scribed in Example 1 .
  • the cleaned meshes were damped with the hydrogel precursor, then cured under UV-light (365 nm).

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  • Thermal Sciences (AREA)
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Abstract

La présente invention concerne un procédé de séparation d'un mélange liquide comprenant de l'eau et un liquide hydrophobe. Particulièrement, l'invention concerne un procédé de séparation huile-eau, comprenant une étape consistant à mettre en contact le mélange liquide comprenant le liquide hydrophobe et de l'eau avec un tamis à revêtement hydrophile permettant à l'eau de passer à travers le tamis tandis qu'au moins une partie du liquide hydrophobe reste sur le tamis. Le tamis est une armure ayant une taille de pore géométrique inférieure à 100 μm ayant des fils de chaîne de diamètre dw, et des fils de trame de diamètre ds, les ds et dw différant d'au moins un facteur de 1,1 et la surface du tamis étant au moins partiellement recouverte par un revêtement hydrophile, le revêtement hydrophile ayant un angle de contact pour l'eau inférieur à 10°. L'invention concerne, en outre, un tamis à revêtement hydrophobe et son utilisation.
PCT/EP2017/081878 2016-12-16 2017-12-07 Tamis revêtus et leur utilisation, specialement pour la séparation huile-eau WO2018108700A1 (fr)

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EP17811296.7A EP3554666A1 (fr) 2016-12-16 2017-12-07 Tamis revêtus et leur utilisation, specialement pour la séparation huile-eau
EA201991326A EA201991326A1 (ru) 2016-12-16 2017-12-07 Сито с покрытием и его применение, в частности, для сепарации воды от нефти

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IT201800010762A1 (it) * 2018-12-03 2020-06-03 Saati Spa Tessuto ad alta prestazione per filtri di separazione acqua/gasolio.
EP3988194A4 (fr) * 2019-06-21 2022-08-10 Asada Mesh Co.,Ltd. Coalesceur et dispositif de séparation huile-eau

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
IT201800010762A1 (it) * 2018-12-03 2020-06-03 Saati Spa Tessuto ad alta prestazione per filtri di separazione acqua/gasolio.
WO2020115625A1 (fr) * 2018-12-03 2020-06-11 Saati S.P.A. Tissu haute performance pour filtres de séparation eau/diesel
KR20210090169A (ko) * 2018-12-03 2021-07-19 사아티 에스.피.에이. 물/디젤 분리 필터들을 위한 고성능 직물
KR102695057B1 (ko) * 2018-12-03 2024-08-12 사아티 에스.피.에이. 물/디젤 분리 필터들을 위한 고성능 직물
EP3988194A4 (fr) * 2019-06-21 2022-08-10 Asada Mesh Co.,Ltd. Coalesceur et dispositif de séparation huile-eau

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