WO2012041661A1 - A composition and method for treating substrates - Google Patents

A composition and method for treating substrates Download PDF

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Publication number
WO2012041661A1
WO2012041661A1 PCT/EP2011/065354 EP2011065354W WO2012041661A1 WO 2012041661 A1 WO2012041661 A1 WO 2012041661A1 EP 2011065354 W EP2011065354 W EP 2011065354W WO 2012041661 A1 WO2012041661 A1 WO 2012041661A1
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WO
WIPO (PCT)
Prior art keywords
water
composition
compositions
alkoxy silane
fluoro alkoxy
Prior art date
Application number
PCT/EP2011/065354
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English (en)
French (fr)
Inventor
Somnath Das
Kingshuk Dutta
Amitava Pramanik
Original Assignee
Unilever Nv
Unilever Plc
Hindustan Unilever 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
Application filed by Unilever Nv, Unilever Plc, Hindustan Unilever Limited filed Critical Unilever Nv
Priority to BR112013007235A priority Critical patent/BR112013007235A2/pt
Priority to CN2011800463084A priority patent/CN103119214A/zh
Priority to EP11752236.7A priority patent/EP2622124A1/en
Publication of WO2012041661A1 publication Critical patent/WO2012041661A1/en

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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/07Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D06M11/11Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
    • D06M11/155Halides of elements of Groups 2 or 12 of the Periodic Table
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/28Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
    • C03C17/30Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with silicon-containing compounds
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/07Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D06M11/11Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
    • D06M11/17Halides of elements of Groups 3 or 13 of the Periodic Table
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/07Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D06M11/11Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
    • D06M11/20Halides of elements of Groups 4 or 14 of the Periodic Table, e.g. zirconyl chloride
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/51Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/55Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
    • D06M11/56Sulfates or thiosulfates other than of elements of Groups 3 or 13 of the Periodic Table
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/51Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/55Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
    • D06M11/57Sulfates or thiosulfates of elements of Groups 3 or 13 of the Periodic Table, e.g. alums
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/58Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
    • D06M11/64Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
    • D06M11/65Salts of oxyacids of nitrogen
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/50Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
    • D06M13/51Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
    • D06M13/513Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10Repellency against liquids
    • D06M2200/11Oleophobic properties
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/10Repellency against liquids
    • D06M2200/12Hydrophobic properties

Definitions

  • the present invention relates to a composition and a method for treating substrates, such as fabrics; particularly to make the substrate stain repellent.
  • Fabrics and hard surfaces are generally cleaned with detergents.
  • Standard detergent compositions include surfactants and builders. Surfactants clean the fabrics.
  • Some detergent compositions also contain soda ash to enhance the cleaning action.
  • Many detergent compositions also include specialty polymers that help release stains. Such polymers are called soil release polymers (SRP).
  • SRP soil release polymers
  • Some detergent compositions also include additives that reduce re-deposition of dirt which is released in the wash liquor. Such additives are called Anti-redeposition agents (ARD).
  • Fabrics and hard surfaces tend to get stained during use. Stains are generally, either oily, or aqueous. Common sources of aqueous stains include tea, coffee, beverages and inks. Common sources of oily stains include pickles, sauces and ketchups, motor oil, and grease. People do prefer to wear clothes with lesser stains. This is particularly applicable to white fabrics, such as white shirts. People also prefer that kitchen, bathroom surfaces and windows surfaces are free of stains.
  • One of the ways to prevent fabrics and hard surfaces from getting stained is to treat them with compositions that form a film on the surface of the fabric or hard surface.
  • This film prevents, or at least reduces, the adhesion of stains.
  • the film also allows for facile removal of stains during washing, and it may be said to form a sacrificial layer. Salts of metals are generally present in such compositions. Surfaces get stained when stains spreads on it. In such cases, the stain wets the surface. When a stain wets a surface, the contact angle between the stain and the surface is very low, generally less than 10°. When a surface treatment composition forms a film, the film increases the contact angle. In other words, this film doesn't allow the stain to wet the surface.
  • water contact angle in the range of 90° to 170° is considered to be good for repelling aqueous stains.
  • oil contact angles greater than 60 are considered to be good for repelling oily stains.
  • Such treated surfaces may be termed as super-hydrophobic or super-oleophobic.
  • the contact angle is the angle at which a liquid/vapour (or two immiscible liquids) interface meets a solid surface.
  • the contact angle is specific for any given system and is determined by the interactions across the two interfaces. Most often, the concept is illustrated with a liquid droplet resting on a flat horizontal solid surface. The shape of the droplet is determined by Young-Laplace equation.
  • One of the ways to measure contact angle is to use a contact angle goniometer on a sessile drop of the liquid. This method is used to estimate wetting properties of a localized region on a solid surface. The angle between the baseline of the drop and the tangent at the drop boundary is the contact angle.
  • compositions help make substrates, particularly fabrics, repellent to hydrophilic stains.
  • the compositions include 25 to 50 wt% soap, 10 to 30 wt% a complex of zinc and triethanolamine, 30 to 65 wt% trivalent metal ion and/or tetravalent metal ion, and a solvent having a lower alcohol and water in a ratio of 99: 1 to 85: 15.
  • compositions are particularly effective against (i.e. they repel more of) aqueous stains, while some are effective only against oily stains.
  • Compositions that provide both oil and water repellant compositions with improved adhering properties are also disclosed in the art.
  • US6361871 discloses surface modifying coating composition with better adhering properties, a process for preparing the coating composition and method for its use.
  • the coating composition attaches to a polar substrate strongly and permanently providing improved coating.
  • the coating composition includes atleast one organo fluorine-functional silane and/or siloxane, atleast one mineral acid and atleast one metal salt of aluminium (III), tin (II), tin (IV), iron (III) or titanium (III). This application however does not disclose a composition for application as a sacrificial layer that temporarily adheres to the fabric surface, making it stain repellant.
  • US6426150 discloses a surface-modified insulator, method for modifying the surface of an insulator and a coating composition.
  • the surface-modified insulator includes an insulator body having a coating on atleast a portion of atleast one organo fluorine-functional silane, organo fluorine-functional siloxane, or a mixture thereof, atleast one mineral acid and atleast one metal salt selected from a group consisting of aluminium (III), tin (II), tin (IV), iron (III) or titanium (III).
  • This application teaches a coating composition that provides with a water oil and dirt repellant coating having improved adhesion properties and provides a homogeneous, highly cross linked coating on the insulator that remains fully and permanently bonded for long term.
  • aqueous-alcoholic compositions which include a water-soluble salt of a multivalent metal ion, and a fluoro alkoxy silane.
  • Such compositions have been found to provide higher repellence towards aqueous as well as oily stains.
  • the combination shows surprising synergistic effects that are an order of magnitude better than those shown individually by the water-soluble salt of the multivalent metal ion and the fluoro alkoxy silane.
  • the present invention provides a composition for treating a substrate, the composition including:
  • ratio of said water-soluble salt to said fluoro alkoxy silane is from 1 :5 to 5: 1.
  • the present invention provides a process for making a composition of the first aspect, the process including a step of mixing 0.05 parts by weight to 10 parts by weight water-soluble salt which includes a multivalent metal ion and 0.25 parts by weight to 5 parts by weight fluoro alkoxy silane with water and a Ci to C 4 alcohol to get 100 parts of the composition.
  • the present invention provides a method for treating a substrate which includes the steps of:
  • the present invention provides use of a composition of the first aspect for treating a substrate to make it hydrophobic and oleophobic.
  • weight percent, percent by weight, % by weight and wt% are synonyms that refer to the concentration of a substance as the weight of that substance divided by the weight of the composition and multiplied by 100.
  • the invention relates to a composition for treating a substrate.
  • the composition includes:
  • ratio of said water-soluble salt to said fluoro alkoxy silane is from 1 :5 to 5: 1.
  • the water-soluble salt includes a multivalent metal ion.
  • the multivalent metal ion may be divalent, trivalent, or may have higher valency, such as tetravalent.
  • Suitable metals may be selected from alkaline earth metals, transition metals, inner transition metals, Lanthanides and Actinides. Alkaline earth metals and transition metals are preferred over others, as they are safer to use. Simple salts such as nitrates or sulphates are preferred over compound salts, double salts and polymeric salts, but such compound, double and polymeric salts may also be used.
  • Preferred multivalent metal ions may be selected from Al 3+ , Ca 2+ , Zn 2+ , Cu 2+ , Ti 3+ or Fe 3+ .
  • Preferred trivalent metal ions are Al 3+ and Fe 3+ ; Al 3+ is particularly preferred.
  • Preferred divalent metal ions are Ca 2+ and Cu 2+ .
  • the water soluble salt may also be of any tetravalent metal ion.
  • the tetravalent metal ion is Ti 4+ .
  • salts of trivalent metal ions are preferred over salts of tetravalent metal ions.
  • Particularly preferred water-soluble salts include Aluminium nitrate, Calcium nitrate, Zinc nitrate, Copper nitrate, Ferric nitrate, Copper sulphate, Calcium chloride,
  • Aluminium sulphate Aluminium chloride and Titanium chloride.
  • the salt may be hydrated, or anhydrous.
  • the salt may be acidic or alkaline.
  • Preferred acidic salts include nitrates, chlorides and sulphates.
  • Alkaline compounds can be used provided that the pH is reduced by use of a pH modifier.
  • Preferred alkaline salts include aluminates. Sodium aluminate is one such salt. In this case, it is preferred that the molar ratio of Na 2 0 to Al 2 0 3 is from 1.5: 1 to 1 :1 , more preferably from 1.3:1 to 1 : 1 and most preferably from 1.25:1 to 1.1 : 1.
  • Some particularly preferred Aluminium salts include Polyaluminium chloride and Polyaluminium sulphate. Water-insoluble Aluminium compounds like clays, alumina and aluminium hydroxide may not be suitable. While it is preferred to use only one salt, a mixture of salts may also be used.
  • compositions include 0.05 wt% to 10 wt% of a water-soluble salt, more preferably 0.1 wt% to 5 wt%, and most preferably 0.5 wt% to 2 wt% water-soluble salt which includes a multivalent metal ion.
  • water-soluble implies solubility in water.
  • water-soluble salt means a salt whose solubility is at least 0.05 g/ 100 g water at 25 °C.
  • the solubility of the salt is preferably greater than 0.1 , more preferably greater than 1 and most preferably greater than 5.
  • fluoro alkoxy silanes may be selected from heptadecafluoro-1 ,1 ,2,2-tetrahydrodecyl trimethoxysilane (CAS: 83048-65-1); tridecafluoro-1 ,1 ,2,2-tetrahydrooctyl trimethoxysilane (CAS: 85857-16-5); heptadecafluoro-1 ,1 ,2,2-tetrahydrodecyl triethoxysilane (CAS: 101947-16-4 );
  • silanes may be purchased from any commercial vendor, such as Gelest Inc.
  • Heptadecafluoro-1 ,1 ,2,2-tetrahydrodecyl trimethoxysilane (CAS: 83048-65-1), and tridecafluoro-1 , 1 ,2, 2-tetrahydrooctyl trimethoxysilane (CAS: 85857-16-5) are particularly preferred.
  • the ratio of the water-soluble salt which includes the multivalent metal ion to the fluoro alkoxy silane is from 1 :5 to 5: 1 , preferably 1 : 1 to 2:3.
  • the compositions according to the invention include 0.25 wt% to 5 wt% fluoro alkoxy silane. It was observed that levels of 0.05 wt% showed insignificant repellence, particularly towards oily stains. Thus the compositions include 0.25 wt% to 5 wt% fluoro alkoxy silane, preferably 0.5 wt% to 2 wt%.
  • compositions according to the invention are hydro-alcoholic, meaning, that the compositions include water and a Ci to C 4 alcohol.
  • Preferred compositions may have from about 75 wt% to about 90 wt% alcohol.
  • Preferred alcohols include ethanol, n- propanol and iso-propanol. It is preferred that water is from 5 wt% to 15 wt%.
  • the ratio of water to the alcohol may vary from 1 :6 to 1 :9, without much change in performance.
  • compositions may also, preferably, include other common ingredients such as fluorescer, preservatives, perfume, and shading dyes.
  • the invention relates to a process for making a composition of the first aspect.
  • the process includes a step of mixing 0.05 parts by weight to 10 parts by weight water-soluble salt having a multivalent metal ion and 0.25 parts by weight to 5 parts by weight fluoro alkoxy silane, with water and a Ci to C 4 alcohol to get 100 parts of the composition.
  • the ingredients may be mixed in any suitable mixer, and they may be added in any order. It is preferred that water is added to the salt in a container, followed by alcohol, and then the fluoro alkoxy silane. After this, the mixture is preferably mixed in a vortex mixer at room temperature.
  • the invention relates to a method for treating a substrate.
  • the method includes the steps of:
  • composition or a solution thereof, may be sprayed onto the substrate, or the substrate, e.g. fabric may be dipped in the composition, or a solution thereof.
  • Other known methods not particularly mentioned here may also be used.
  • compositions of the present invention may be used to treat any given substrate.
  • Preferred substrates include metal, glass, ceramic, fabric and paper.
  • the substrate is a fabric, paper or glass. More preferably the substrate is a fabric or glass.
  • the fabric that can be treated includes synthetic as well as natural fabrics. Fabrics may be made of cotton, poly-cotton, polyester, silk or nylon. It is envisaged that the compositions of the present invention can be used to treat garments and other clothing and apparels that form a typical wash-load in household laundry.
  • the household materials that can be treated according to the method of the present invention include, but are not limited to, bedspreads, blankets, carpets, curtains and upholstery.
  • the compositions of the present invention are described primarily for treatment of fabrics, it is envisaged that the method may advantageously be used to treat jute, denim and canvass, shoes and jackets.
  • the method may take 15 to 90 minutes, preferably 20 minutes to an hour.
  • the method may be carried out without any heating or cooling e.g. from 15 °C to 40 °C.
  • fabrics may be squeezed before drying.
  • Treated fabrics may be air dried, sun dried, or dried in a drying machine. It is preferred that fabrics are ironed after drying.
  • liquid to cloth ratio or L/C ratio as used herein means the ratio of mass of the solution that is in contact with the fabrics to the mass of the fabrics.
  • the liquor to cloth ratio may be different in each step.
  • the liquor to cloth ratio is 2 to 100, more preferably 5 to 50, and most preferably from 5 to 20.
  • the term "area of the fabric contacted" as used herein refers to apparent surface area of any one side of the fabric that is contacted with a solution of the composition.
  • the invention provides use of a composition of the first aspect for treating a substrate to make it hydrophobic and oleophobic.
  • Use of the composition may help achieve water contact angle greater than 90° and oil contact angle greater than 60°.
  • the water contact angle is preferably 90° to 180°, more preferably at least 100°, still more preferably at least 1 10°, or even more preferably at least 120°.
  • the contact angle is measured using a sessile drop method immediately after droplet addition.
  • the invention provides a kit which includes a composition of the first aspect, along with instructions for use.
  • A.R Zinc nitrate hexahydrate A.R, Copper nitrate trihydrate A.R, Ferric nitrate nonahydrate A.R, Aluminium sulfate hexadecahydrate A.R, Aluminum chloride hexahydrate A.R - all procured from Merck.
  • silane 83048-65-1 tridecafluoro-1 ,1 ,2,2-tetrahydrooctyl
  • trimethoxysilane (CAS: 85857-16-5);
  • Substrate Desized cotton ex. Bombay dyeing
  • compositions were made by varying the ratio between the water-soluble salt (Al 3+ salt) and the fluoro alkoxy silane. All experiments were conducted with Tridecafluoro-(1 , 1 ,2,2-tetrahydrooctyl) trimethoxy silane. Seven ratios were tried; 1 : 1 , 1 :5, 5: 1 , 1 : 10, 3:5, 4:5 and 10: 1. The formulations were as follows.
  • compositions marked with * are comparative compositions.
  • g/l stands for "grams per litre", which indicates concentration of the silane or salt in the solution.
  • Table-4 Contact angles of water and oil on cotton fabric - synergistic effect of Al 3+ salt and silane in preferred compositions of table-2
  • compositions 17 to 20 showed relatively lower oil contact angles, as compared to 1-16, possibly due to the fact that they were done in a different experimental series. However the difference is small. Examples 5, 6, 15, 16, 17 and 20 are outside the claimed range, and show lower oil contact angles, except for 15, which is on the edge of the claimed range and still performs fairly well. For comparison, some glass slides were treated with only an aqueous solution of the Al 3+ salt.
  • Table-6 Contact angles of water and oil on glass slides - synergistic effect of the Al salt and the fluoro alkoxy silane in preferred compositions of table-2
  • compositions 6 and 16 show higher oil contact angles on glass, but the oil contact angles on fabrics were much lower as indicated in table-4. Therefore, the compositions 6 and 16 may be regarded as comparative compositions.
  • Example-2 Compositions with Fe 3+ salt and fluoro alkoxy silane
  • Example-1 The experiments conducted in Example-1 were repeated with a Fe 3+ salt (Ferric nitrate). Preferred compositions were made by varying the ratio between the Fe 3+ salt and the fluoro alkoxy silane (silane). All experiments were conducted with
  • Tridecafluoro-(1 , 1 ,2,2-tetrahydrooctyl) trimethoxy silane Table-7 describes the formulations.
  • Table-10 Contact angles of water and oil on glass slides - synergistic effect salt and fluoro alkoxy silane in compositions of table-7
  • Table-1 1 Contact angles of oil on cotton - synergistic effect of Fe salt and fluoro alkoxy silane in compositions of table-7
  • Example-1 and 2 were repeated with compositions containing Calcium chloride.
  • Preferred compositions were made by varying the ratio between the Ca 2+ salt and the fluoro alkoxy silane. All experiments were conducted with Tridecafluoro-1 ,1 ,2,2-tetrahydrooctyl) trimethoxy silane.
  • the formulations were as follows: Table-12
  • compositions containing Copper sulphate and a fluoro alkoxy silane were repeated with compositions containing Copper sulphate and a fluoro alkoxy silane.
  • Preferred compositions were made by varying the ratio between the Cu 2+ salt and the fluoro alkoxy silane. All experiments were conducted with Tridecafluoro-(1 , 1 ,2,2-tetrahydrooctyl) trimethoxy silane.
  • Table-15 shows the formulation of preferred compositions:
  • Table-17 Synergistic effect of compositions containing Copper sulphate and fluoro alkoxy silane (Compositions of table 15)
  • Example-5 Experiments with Aluminium chloride and Aluminium sulphate
  • compositions of Aluminium chloride and fluoro alkoxy silane were repeated with compositions of Aluminium chloride and fluoro alkoxy silane, and another set of compositions which had Aluminium sulphate and a fluoro alkoxy silane. Diluted solutions were used to treat glass surface. After the treatment, contact angles of water and oil were determined.
  • Table-20 Contact angles of water and oil on glass slides - synergistic effect of compositions table-18
  • Table-22 Contact angles of oil on cotton - synergistic effect of Al salts and silane of compositions of table-18
  • compositions and methods for treating substrates especially cotton and glass. Treated substrates show higher contact angles against both water and oil. It will also be appreciated that the illustrated examples explain the use of compositions for treating substrates to make it hydrophobic and oleophobic. The illustrated examples also explain that glass and cotton surface treated with preferred compositions show higher oil and water contact angles, as compared to glass and cotton surfaces treated with only a water-soluble salt comprising a multivalent metal ion, or only a fluoro alkoxy silane. It will also be appreciated that preferred compositions provide higher oil and water contact angles while containing lower quantities of a water-soluble salt comprising a multivalent metal ion and a fluoro alkoxy silane. Therefore, the compositions are capable of being effective against aqueous as well as oily stains.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Materials Applied To Surfaces To Minimize Adherence Of Mist Or Water (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
PCT/EP2011/065354 2010-09-27 2011-09-06 A composition and method for treating substrates WO2012041661A1 (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
BR112013007235A BR112013007235A2 (pt) 2010-09-27 2011-09-06 "composição para o tratamento de um substrato, processo para produzir uma composição, método para tratar um substrato e uso"
CN2011800463084A CN103119214A (zh) 2010-09-27 2011-09-06 用于处理基材的组合物和方法
EP11752236.7A EP2622124A1 (en) 2010-09-27 2011-09-06 A composition and method for treating substrates

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CN104276765B (zh) * 2013-07-08 2016-11-02 中国科学院重庆绿色智能技术研究院 超疏水透明玻璃的制备方法
CN104389163A (zh) * 2014-11-28 2015-03-04 杨帆 一种毛纺织物整理用印染前助剂
EP3421558A1 (en) * 2017-06-30 2019-01-02 3M Innovative Properties Company Amphiphilic copolymer-based protective coating composition for metal surfaces

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US6361871B1 (en) 1999-02-03 2002-03-26 Degussa Ag Composition of organofluorine-functional silanes and/or siloxanes, process for preparing it and its use
US6426150B1 (en) 1999-02-03 2002-07-30 Degussa Ag Surface-modified insulator and method of modifying the surface of an insulator

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US6426150B1 (en) 1999-02-03 2002-07-30 Degussa Ag Surface-modified insulator and method of modifying the surface of an insulator

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