WO2019182513A1 - Formulation d'imperméabilisation - Google Patents

Formulation d'imperméabilisation Download PDF

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Publication number
WO2019182513A1
WO2019182513A1 PCT/SG2019/050148 SG2019050148W WO2019182513A1 WO 2019182513 A1 WO2019182513 A1 WO 2019182513A1 SG 2019050148 W SG2019050148 W SG 2019050148W WO 2019182513 A1 WO2019182513 A1 WO 2019182513A1
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Prior art keywords
silane
propyl
methyl
composition according
alkyl
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PCT/SG2019/050148
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English (en)
Inventor
Hong Yan
Jianwei Xu
Ching Mui CHO
Angeline Yan Xuan TAN
Hui Ning ZENG
Debbie Xiang Yun SOO
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Agency For Science, Technology And Research
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Publication of WO2019182513A1 publication Critical patent/WO2019182513A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/60—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only artificial stone
    • C04B41/61—Coating or impregnation
    • C04B41/62—Coating or impregnation with organic materials
    • C04B41/64—Compounds having one or more carbon-to-metal of carbon-to-silicon linkages
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
    • C04B41/49—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes
    • C04B41/4905—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon
    • C04B41/4922—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon applied to the substrate as monomers, i.e. as organosilanes RnSiX4-n, e.g. alkyltrialkoxysilane, dialkyldialkoxysilane
    • C04B41/4927—Alkali metal or ammonium salts
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/63—Additives non-macromolecular organic

Definitions

  • the present invention generally relates to a composition and a liquid mixture.
  • the present invention also relates to a method of preparing the liquid mixture, the uses and the methods of uses thereof.
  • organic polymers are commonly used in mixing with cement to improve the impermeability and resistance to cracking of concrete.
  • this will increase shrinkage, resulting in many examples of application failure.
  • the more commonly used waterproofing compacting agents are mainly the higher fatty acids, triethanolamine, ferric chloride and many others.
  • Such compounds can make the concrete capillary water absorption to decrease, but increase the amount of incorporation where the intensity will be reduced, and circumstances under which the long-term impregnation water resistance is reduced.
  • specific organic polymers like siliconates have played an important role as hydrophobizing agents for building materials.
  • the organic silicon has stronger hydrophobicity, and a tight network structure can be formed in concrete which can simultaneously block or obstruct capillary orifices in the concrete, thereby achieving the purpose of bleeding resistance and water prevention.
  • a composition comprising an alkyl siliconate and at least one additional compound selected from an alkyl silane or a geopolymer.
  • the disclosed composition may be prepared as a water based composition and thus, may be environmental friendly.
  • the disclosed composition may provide unexpectedly superior water proofing properties and anti-fungal properties to surfaces to which the composition has been applied.
  • the disclosed composition may also provide superior water repellent properties on surfaces.
  • the disclosed composition may be effective for water-proofing surfaces and inhibiting fungal growth thereon, even when the alkyl siliconate is provided in amounts of 10 wt. % or less based on the total weight of the composition.
  • the disclosed composition may be cost-effective to prepare in view that only two chemical components are required to achieve the technical effects.
  • the disclosed composition may exhibit unexpectedly superior water-proofing properties and fungal inhibitory effects, while remaining cost-effective to produce due to the relatively low concentrations of the alkyl siliconate present.
  • a liquid mixture comprising an alkyl siliconate and at least one additional compound selected from a silane or a geopolymer.
  • a method of providing water-repellency and fungal resistance to a surface comprising a step of applying a composition as defined herein to the surface to form a coating thereon; and optionally drying or curing the coating.
  • composition as defined herein for coating a surface to thereby provide water-repellency and fungal resistance thereon the surface.
  • the disclosed composition may be compatible for applications onto a variety of surfaces.
  • the disclosed composition may be particularly suited for application onto porous surfaces to reduce the water permeability and/or water absorption property of the surface.
  • the alkyl siliconate (silicone) may be useful for improving the adhesion between the composition and the surface to which it is applied. This may advantageously allow the disclosed composition to readily penetrate pores, cover crevices or even smooth uneven surfaces to result in uniform application of the composition.
  • hydrophobic refers to or relates to an act or process of making something hydrophobic, such as the surface of a particle. This may involve the use of a “hydrophobizing agent” that alters adhesives and/or sealants to make them more hydrophobic.
  • the hydrophobizing agent may impart instantaneous hydrophobicity to material when applied or coated onto a surface.
  • water repellent refers to a surface or material having a property of not being easily penetrated by water, especially as a result of being treated for such a purpose with a surface coating.
  • the surface or material may have a finish that resists the absorption of water or is resistant to the absorption or passage of water.
  • the surface or material may be porous.
  • the term“water-repellency” may also be used interchangeably with the term“water repellent”.
  • water permeability refers to an action that allows water to permeate or pass through (either in or out) its structure.
  • A“bond” is a linkage between atoms in a compound or molecule.
  • the bond may be a single bond, a double bond, or a triple bond.
  • Alkyl as a group or part of a group refers to a straight or branched aliphatic hydrocarbon group to be interpreted broadly, having from 1 to 16 carbon atoms, e.g., 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15 or 16 carbon atoms, preferably a Ci C i6 alkyl, C 4 -C 12 alkyl, more preferably a CV o alkyl, most preferably C ! -C 6 alkyl unless otherwise noted.
  • Suitable straight and branched alkyl substituents include but is not limited to, methyl, ethyl, 1 -propyl, isopropyl, 1 -butyl, 2-butyl, isobutyl, tert-butyl, amyl, 1 ,2-dimethylpropyl, 1,1- dimethylpropyl, pentyl, isopentyl, hexyl, 4-methylpentyl, 1-methylpentyl, 2-methylpentyl, 3-methylpentyl, 2,2-dimethylbutyl, 3,3-dimethylbutyl, 1,2-dimethylbutyl, 1,3- dimethylbutyl, 5-methylheptyl, 1 -methylheptyl, octyl, nonyl, decyl, undecyl, 2,2,3- trimethyl-undecyl, dodecyl, 2,2-dimethyl-dodecyl, tridecyl, 2-methyl-tride
  • Halide or“halogen” represents chlorine, fluorine, bromine or iodine.
  • Silane refers to an inorganic acyclic compound with chemical formula, Si sauceH 2 consult + 2 and is saturated chemical compound consisting of one or multiple silicon atoms linked to each other, or one or multiple atoms of other chemical elements as the tetrahedral centers of multiple single bonds.
  • the term“silane” may be used as a group or part of a group, where the hydride (H) is replaced with other functional groups (e.g. Si or a halogen) or is optionally substituted as defined herein, to be interpreted broadly.
  • the group may be a terminal group or a bridging group.
  • Siliconol as used herein, refers to a functional group in silicon chemistry with the connectivity
  • Si-O-H to be interpreted broadly, having at least one hydroxyl (OH) group.
  • the functional group in silicon chemistry has two hydroxyl (OH) groups, the term is known as
  • silanediol When the functional group in silicon chemistry has three hydroxyl (OH) groups,
  • the term is known as “silanetriol” with a chemical structure HO R , whereby the R substituent can be any functional group, preferably an alkyl group.
  • Silicon as used herein also refers to silicon dioxide (Si0 2 ).
  • the term“silicate” is also used for any salt of such anions.
  • Siliconate refers to an organic modified alkali silicate. Siliconate is generally applied in aqueous solution to harden and/or protect masonry substrates.
  • Silicon-oxygen backbone chain -Si-O-Si-O- Si-O- ⁇
  • organic side groups attached to the silicon atoms to be interpreted broadly, more precisely called polymerized siloxane or polysiloxane.
  • the term“silicone” as used herein, may be used interchangeably with the term“siliconate”.
  • optionally substituted means the group to which this term refers may be unsubstituted, or may be substituted with one or more groups independently selected from alkyl, alkenyl, alkynyl, thioalkyl, cycloalkyl, cycloalkylalkyl, cycloalkenyl, cycloalkylalkenyl, heterocycloalkyl, cycloalkylheteroalkyl, cycloalkyloxy, cycloalkenyloxy, cycloamino, halo, carboxyl, haloalkyl, haloalkynyl, alkynyloxy, heteroalkyl, heteroalkyloxy, hydroxyl, hydroxyalkyl, alkoxy, thioalkoxy, alkenyloxy, haloalkoxy, haloalkenyl, haloalkynyl, haloalkenyloxy, nitro, amino, nitroalkyl, cycloal
  • the term "about”, in the context of concentrations of components of the formulations, typically means +/- 5% of the stated value, more typically +/- 4% of the stated value, more typically +/- 3% of the stated value, more typically, +/- 2% of the stated value, even more typically +/- 1% of the stated value, and even more typically +/- 0.5% of the stated value.
  • range format is merely for convenience and brevity and should not be construed as an inflexible limitation on the scope of the disclosed ranges. Accordingly, the description of a range should be considered to have specifically disclosed all the possible sub-ranges as well as individual numerical values within that range. For example, description of a range such as from 1 to 6 should be considered to have specifically disclosed sub-ranges such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6 etc., as well as individual numbers within that range, for example, 1, 2, 3, 4, 5, and 6. This applies regardless of the breadth of the range.
  • the composition may comprise an alkyl siliconate and at least one additional compound selected from an alkyl silane or a geopolymer.
  • alkyl siliconate of the composition as defined herein may have the general formula:
  • R is C
  • R substituent of the alkyl siliconate as defined above may be selected from the group consisting of methyl, ethyl, propyl, butyl, pentyl and hexyl.
  • R may be methyl.
  • the metal ion or M of the alkyl siliconate as defined above may be an alkali metal ion or a Group I metal ion.
  • M of the alkyl siliconate as defined above may be selected from the group consisting of Li + , Na + and K + .
  • M may be Li + .
  • the alkyl siliconate of the composition may be selected from methyl lithium silicate, methyl sodium silicate, methyl potassium silicate, or mixtures thereof.
  • the alkyl siliconate may be an alkali metal methylsiliconate.
  • exceptionally good water-proofing properties may be achieved, such as water penetration ⁇ 13 mm, water absorption ⁇ 0.8%, coefficient of permeability to water 3.7334e-l3 m/s.
  • the additional compound of the composition as defined above may be a silane compound.
  • the alkyl silane may be selected from the group consisting of: l l-acetateundecyltriethoxysilane, 11- acetateundecyltrimethoxysilane, allyltrichlorosilane, allyltriethoxysilane, allyltrimethoxysilane, [3-(2-aminoethylamino)propyl]trimethoxysilane, 3-aminopropyl(diethoxy)methylsilane, (3- aminopropyljtrimethoxysilane, azidotrimethylsilane, 11 -azidoundecyltriethoxysilane, 11- azidoundecyltrimethoxysilane, 3 - [bis(2 -hydroxyethyl) amino] propyl -triethoxysilane
  • the geopolymer may be an organic geopolymer or an inorganic geopolymer.
  • the geopolymer may contain metal ion in the framework.
  • the metal may be a Group I metal.
  • the metal may be a Group III metal.
  • the geopolymer may comprise of a polymeric Si-O-Al framework.
  • the geopolymer may have a repeating unit comprising the following formula:
  • the additional compound of the composition as defined above may also act as a promoter for the reaction.
  • the volume ratio between the alkyl siliconate and the additional compound of the composition as defined above may be from 10: 1 to 1 : 1 , 9: 1 to 1 : 1, 8: 1 to 1 : 1, 7:1 to 1 : 1, 6: 1 to 1 :1, 5: 1 to 1 : 1, 4: 1 to 1: 1, 3: 1 to 1 : 1, 2: 1 to 1 : 1, 10: 1 to 2: 1, 10: 1 to 3: 1, 10: 1 to 4: 1, 10: 1 to 5: 1, 10: 1 to 6: 1, 10: 1 to 7: 1, 10: 1 to 8:1 or 10: 1 to 9:1.
  • the additional compound is a silane, more preferably an triethoxyalkylsilane, and even more preferably a triethoxyoctylsilane; wherein the molar concentration of the silane may be provided from around 1 to 5 mM, 2 to 5 mM, 3 to 5 mM, 4 to 5 mM, 1 to 2 mM, 1 to 3 mM or 1 to 4 mM.
  • the alkali metal methylsiliconate as defined above may be mixed or reacted with the silane compound as defined above, wherein the alkali metal methylsiliconate may be provided in molar concentrations of from 8 to 14 mM, 9 to 14 mM, 10 to 14 mM, 11 to 14 mM, 12 to 14 mM, 13 to 14 mM, 8 to 13 mM, 8 to 12 mM, 8 to 11 mM, 8 to 10 mM or 8 to 9 mM.
  • the alkali metal methylsiliconate may preferably be provided in molar concentrations selected from 8.2 mM, 8.4 mM, 8.6 mM, 8.8 mM, 9 mM, 9.2 mM, 9.4 mM, 9.6 mM, 9.8 mM, 10 mM, 10.2 mM, 10.4 mM, 10.6 mM, 10.8 mM, 11 mM, 11.2 mM, 11.4 mM, 11.6 mM, 11.8 mM, 12 mM, 12.2 mM, 12.4 mM, 12.6 mM, 12.8 mM, 13 mM, 13.2 mM, 13.4 mM, 13.6 mM, 13.8 mM or 14 mM.
  • the hydrolyzing molar ratio (defined as the mole ratio of reactants used in the hydrolysis reaction) between the triethoxyoctylsilane and alkali metal methylsiliconate may be from 1 - 20 : 300 - 370.
  • the molar ratio of the silane compound and the alkali metal methylsiliconate may be from 0.1 mol% to 10 mol%, 0.1 mol% to 0.5 mol%, 0.5 mol% to 1 mol%, 0.1 mol% to 1 mol%, 1 mol% to 10 mol%, 1 mol% to 9 mol%, 1 mol% to 8 mol%, 1 mol% to 7 mol%, 1 mol% to 6 mol%, 1 mol% to 5 mol%, 1 mol% to 4 mol%, 1 mol% to 3 mol%, 1 mol% to 2 mol%, 2 mol% to 10 mol%, 3 mol% to 10 mol%, 4 mol% to 10 mol%, 5 mol% to 10 mol%, 6 mol% to 10 mol% , 7 mol% to 10 mol%, 8 mol% to 10 mol%, 9 mol% to 10 mol%, e.g.
  • compositions comprising such ratios may be particularly useful for providing waterproofing properties and/or microbial resistance, whilst exhibiting optimal compatibility and good adhesive qualities with surfaces e.g. concrete.
  • the disclosed composition may comprise or consist essentially of potassium methyl siliconate and triethoxyoctylsilane. Such a combination has been found to be particularly useful in achieving superior water-proofing properties and/or anti-fungal properties.
  • the alkyl silane group may be mixed into silicone as a hydrophobic agent.
  • the silicone may be selected from methyl lithium silicate, methyl sodium silicate, methyl potassium silicate, or mixtures thereof.
  • the composition as defined above may comprise a solvent.
  • the solvent may be an aqueous solution.
  • the aqueous solution may preferably be water.
  • the water may be tap water or deionized water.
  • the disclosed composition may be prepared as a water-borne (water-based) coating composition.
  • the solvent may be provided in an amount of from 90 to 97 parts, 90 to 96 parts, 90 to 95 parts, 90 to 94 parts, 90 to 93 parts, 90 to 92 parts, 90 to 91 parts, 91 to 97 parts, 92 to 97 parts, 93 to 97 parts, 94 to 97 parts, 95 to 97 parts, 96 to 97 parts by weight of the composition.
  • the composition may comprise around 95 parts by weight solvent and 5 parts by weight of a mixture comprising the alkyl siliconate and the additional compound.
  • the disclosed composition may be cost-effective to prepare in view that only two chemical components are required to achieve the technical effects.
  • the disclosed composition may be unexpectedly effective for water proofing surfaces and inhibiting fungal growth thereon, even when the alkyl siliconate is provided in amounts of 10 wt. % or less, based on the total weight of the composition.
  • the disclosed composition may be found to be effective when provided in amounts of from 1 wt.
  • % to 10 wt.%. or the concentration of the alkyl siliconate is provided in amounts of from 2 wt.% to 9 wt.%, 2 wt.% to 8 wt.%, 2 wt.% to 7 wt.%, 2 wt.% to 6 wt.%, 3 wt.% to 9 wt.%, 3 wt.% to 8 wt.%, 3 wt.% to 7 wt.%, 3 wt.% to 6 wt.%, or from 3 wt.% to 5 wt.%.
  • the alkyl siliconate may be provided in an amount of from around 3 wt.% to 5 wt.% based on the total weight of the disclosed composition. Such a composition may exhibit unexpectedly superior water-proofing properties and fungal inhibitory effects, while remaining cost-effective to produce due to the relatively low concentrations of the alkyl siliconate present.
  • the alkyl siliconate may be the active ingredient of the formulation.
  • the disclosed composition may be obtained by hydrolysing triethoxyoctylsilane in alkali metal methyl siliconate.
  • the alkyl siliconate compound may be obtained by reacting 10 to 200 mL of 97.5 wt.% of triethoxyoctylsilane with 1000 mL of 50 to 55 wt.% alkali metal methylsiliconate.
  • the disclosed composition has been surprisingly found to provide unexpectedly superior water proofing properties and anti-fungal properties to surfaces to which the composition has been applied. The effectiveness can be observed from the data provided herein.
  • Water-proofing may also be interpreted as providing water repellency to surfaces to which the disclosed composition has been applied. For instance, water repellency may be empirically measured by experimentally determining the coefficient of permeability to water.
  • the disclosed compositions may be able to provide water-repellency to coated concrete surfaces, wherein the coefficient of permeability to water is smaller than 1x10 12 , or smaller than 1x10 13 .
  • the water permeability tests may be conducted in accordance with an industrial standard, e.g. DIN 1048-5. Exemplary, non-limiting embodiments of a liquid mixture and method of preparing a liquid mixture will now be disclosed.
  • the liquid mixture may comprise an alkyl siliconate and at least one additional compound selected from a silane or a geopolymer.
  • the alkyl siliconate of the liquid mixture may have the formula:
  • R is C 1 6 alkyl
  • M is a metal ion
  • n is an integer from 1 to 3.
  • R substituent of the alkyl siliconate as defined above may be selected from the group consisting of methyl, ethyl, propyl, butyl, pentyl and hexyl.
  • R may be methyl.
  • the metal ion or M of the alkyl siliconate as defined above may be an alkali metal ion or a Group I metal ion.
  • M of the alkyl siliconate as defined above may be selected from the group consisting of Li + , Na + and K + .
  • M may be Li + .
  • the liquid mixture may be prepared by dissolving silane with a reaction product that is obtained from reacting a metal hydroxide with an alkyl silanetriol.
  • the silane compound as defined above may be an alkyl silane.
  • the reaction product may be an alkali metal methylsiliconate as defined above.
  • the metal hydroxide may be alkali metal hydroxide.
  • the alkali metal hydroxide may be selected from lithium hydroxide, potassium hydroxide and sodium hydroxide.
  • the alkyl silanetriol may be Ci_ 6 alkyl silanetriol.
  • the alkyl silanetriol may preferably be methyl silanetriol.
  • the liquid mixture may be prepared by dissolving silane with the reaction product at ambient conditions or at elevated temperature.
  • the liquid mixture may preferably be prepared at room temperature.
  • the hydrolysis polycondensation reaction between a silane and an acid may preferably be prepared at room temperature.
  • the reaction between a metal hydroxide and an alkyl silanetriol may preferably be prepared at room temperature.
  • the room temperature may be from 20 °C to 25 °C, 21 °C to 25 °C, 22 °C to 25 °C, 23 °C to 25 °C or 24 °C to 25 °C.
  • the hydrolysis polycondensation reaction between a silane and an acid may be stirred for a period of time in the range of 1 to 6 hours, 1 to 5 hours, 1 to 4 hours, 1 to 3 hours, 1 to 2 hours, 2 to 6 hours, 3 to 6 hours, 4 to 6 hours or 5 to 6 hours.
  • the stirring may preferably be for 1 to 2 hours.
  • the reaction between a metal hydroxide and an alkyl silanetriol may be stirred for a period of time in the range of 1 to 6 hours, 1 to 5 hours, 1 to 4 hours, 1 to 3 hours, 1 to 2 hours, 2 to 6 hours, 3 to 6 hours, 4 to 6 hours or 5 to 6 hours.
  • the stirring may preferably be for 4 hours.
  • the solvent used for the reaction may be an organic solvent.
  • the organic solvent may be polar solvent.
  • the polar solvent may be selected from the group consisting of acetone, N,N- dimethylformamide (DMF), dimethyl sulfoxide (DMSO), ethanol and methanol
  • the method of providing water-repellency and fungal resistance to a surface may comprise a step of applying a composition as defined above to the surface to form a coating thereon; and optionally drying or curing the coating.
  • the disclosed method may comprise an additional curing step, wherein the curing may be undertaken under ambient conditions in the presence of carbon dioxide.
  • the ambient conditions may be at room temperature.
  • the room temperature may be from about 20 °C to about 25 °C, about 21 °C to about 25 °C, about 22 °C to about 25 °C, about 23 °C to about 25 °C or about 24 °C to about 25 °C.
  • the ambient conditions may be in a dry and clean environment.
  • the disclosed method may comprise an additional drying step, wherein the drying is under the standard drying methods, particularly, under vacuum conditions or anhydrous conditions.
  • the drying step may comprise of the adjustment or reduced of moisture levels on the coated surface.
  • the surface where the composition as defined above is applied to may be selected from concrete, brick, masonry, ceramics, stones, cloth, or wood.
  • the disclosed composition may be compatible for application onto a variety of surfaces.
  • the disclosed composition may be particularly suited for application onto porous surfaces to reduce the water permeability and/or water absorption property of the surface.
  • the alkyl siliconate silicone
  • This may advantageously allow the disclosed composition to readily penetrate pores, cover crevices or even smooth uneven surfaces to result in uniform application of the composition.
  • composition as defined above may be for coating a surface, to thereby provide water-repellency and fungal resistance thereon the surface.
  • the composition as defined above may be in a liquid mixture.
  • the liquid mixture may comprise an aqueous solution.
  • the composition may be applied or coated onto the surface and dried thereafter to form a hydrophobic coating thereon.
  • FIG. 1 shows two images of antifungal treatments on wood: Fig. 1A shows the“before coating” occurs and Fig. 1B shows the“after coating for more than four years”.
  • FIG. 2 shows a series of images of the fungal test on the positive control and the test item (PMS): Fig. 2A shows the positive control strips, Fig. 2B shows the front view of the test item (PMS), Fig. 2C shows the back view of the test item (PMS), Fig. 2D shows the left view of the test item (PMS), and Fig. 2E shows the right view of the test item (PMS).
  • Fig. 2A shows the positive control strips where there is massive microbial growth at the end of the 28-day incubation period.
  • Fig. 2B shows the front view of the test item (PMS) where there is no fungal growth at the end of the 28-day incubation period.
  • Fig. 2C shows the back view of the test item (PMS) where there is no fungal growth at the end of the 28-day incubation period,
  • Fig. 2D shows the left view of the test item (PMS) where there is no fungal growth at the end of the 28-day incubation period, and
  • Fig. 2E shows the right view of the test item (PMS) where there is no fungal growth at the end of the 28-day incubation period.
  • the concrete at the end of the 28-day incubation period does not have any fungal growth,
  • F1C1 hydrochloric acid
  • LiOFl lithium hydroxide
  • TEOS tetraethyl orthosilicate
  • Methyl trichlorosilane, hydrochloric acid, lithium hydroxide, sodium hydroxide, potassium hydroxide, silicone and silane (if different from methyl trichlorosilane) were purchased from Sigma-Aldrich Corp. (St. Louis, Missouri, U.S.A.) and were used as received. Concrete was purchased and/or obtained from Admaterials Technologies Pte Ltd. All other reagents were used as received, except where otherwise noted in the experimental text below. All anhydrous solvents were also purchased from Sigma-Aldrich Corp. (St. Louis, Missouri, U.S.A.) and used without further purification.
  • the various waterproof tests include concrete density, coefficient of water permeability, static modulus of elasticity, water absorption, tensile splitting strength, water penetration, flexural strength and antifungal testing method.
  • the standard is based on British Standards Institution. The method of each specific test is provided below, in Example 3.
  • methyl trichlorosilane and concentrated hydrochloric acid (volume ratio of 1 to 7 respectively) are added to a flask and stirred for 1 to 2 hours (h) at room temperature (hydrolysis polycondensation reaction was conducted). The solid obtained was then filtered and washed with water. With the silanetriol solid on hand, an equal amount of lithium hydroxide, sodium hydroxide or potassium hydroxide was added at room temperature, and stirred for 4 hours (h). The final products of this reaction are methyl lithium silicate, methyl sodium silicate or methyl potassium silicate solution, respectively (Scheme 1).
  • Scheme 1 Schematic illustration showing the preparation process of the various methyl metal silicates.
  • a catalyst is present, particularly an alkaline -reacting catalyst such as an alkali metal methylsiliconate or, where an alkali metal hydroxide is the hydrolyzing agent.
  • the preferred hydrolyzing agent is a solution of potassium hydroxide, or of sodium hydroxide, or of lithium hydroxide in alkali metal methylsiliconate.
  • this is preferably present in an amount up to 5% by weight of the octyltriethoxysilane (w.t. % >97.5%) in alkali metal methylsiliconate (w.t. % 50-55%).
  • the resulting suspension was stirred to dissolve the silane completely at room temperature to thereby obtain the concrete comprising the waterproofing agent.
  • the as-prepared concentrated solution was diluted with tap water before mixing into cement. Five parts of the concentrated solution are typically diluted with 95 parts of water.
  • the diluted waterproofing agent was then mixed into concrete for the various concrete tests: concrete density, coefficient of water permeability, static modulus of elasticity, water absorption, tensile splitting strength, water penetration, flexural strength and antifungal testing method.
  • BS EN 12390 - 7: 2009 specifies a method for determining the density of hardened concrete. It applies to lightweight, normal-weight and heavy-weight concrete. It differentiates between hardened concrete in the following states: 1) as-received 2) water saturated and 3) oven-dried. The mass and volume of the specimen of hardened concrete are determined and the density calculated.
  • the range of density is between 1750 to 2400 kg/m 3 for lightweight concrete to normal concrete.
  • our product 1 being tested three times falls within the acceptable range of densities.
  • Test method In-House Method: ADM/CE/017:2013.
  • product 1 typically has a low coefficient of permeability to water.
  • product 1 being tested three times and indicated as 1/1 to 1/3, has an average compressive strength of 25.5 M/mm 2 .
  • BS 1881-122: 2011 provides a way to test the water absorption of concrete. It specifies a method for determining the water absorption of concrete specimens cored from a structure or a precast component. The method may also be used to determine the water absorption of concrete cast into prisms or cylinders where the surface to volume ratio can be calculated and where no point in the specimen is more than 50 mm from a free surface. The measured water absorption of the specimen is corrected to that equivalent to a surface to volume ratio of a core 75 mm long with a diameter of 75 mm. Absorption values for cast specimens are normally slightly lower than those for a core from the same concrete but the difference can be more significant if the aggregate is absorbent.
  • product 1 being tested three times and indicated as 1/1 to 1/3 has a typically low percentage of water absorption, as indicated in Table 11 as well.
  • BS EN 12390-6 2000 provides a way to test the tensile splitting strength of test specimens.
  • product 1 was tested three times and indicated as 1/1 to 1/3, has an average tensile splitting strength of 3.37 N/mm 2 . When compared with other grades of hardened concrete, it falls within the acceptable allowance limit.
  • DIN 1048: Pt5: 1991 provides a way to determine the depth of penetration of water under pressure.
  • BS EN 12390-5 specifies a method for testing the flexural strength of specimens of hardened concrete. This is a test on concrete beams or slabs to resist failure in bending.
  • product 1 was tested three times and indicated as 1/1 to 1/3, has an average flexural strength of 5.1 N/mm 2 . When compared with other grades of hardened concrete, it falls within the acceptable allowance limit.
  • product PMS-SIL also known as product 1 in other tests, was tested multiple times and has an average density of 1.012+0.0016 g/cm 3 .
  • MIL-STD-810 addresses a broad range of environmental conditions that include: low pressure for altitude testing; exposure to high and low temperatures plus temperature shock (both operating and in storage); rain (including wind-blown and freezing rain); humidity, fungus, salt fog for rust testing; sand and dust exposure; explosive atmosphere; leakage; acceleration; shock and transport shock; gunfire vibration; and random vibration.
  • Test fungi used Aspergillus flavus (ATCC 9643), Aspergillus versicolor (ATCC 11730), Penicillium funiculosum (ATCC 11797), Chaetomium globosum (ATCC 6205), Aspergillus niger (ATCC 9642).
  • Test result the rating based on the above evaluation scheme for visible effects.
  • test items PMS or also known as product 1
  • results reported relate to the sample as received. The observations can be seen from the photos that are taken after the 28-day incubation period as indicated in Fig. 2A to Fig. 2E.
  • the hardened concrete or test item is devoid of microbial growth at the end of the 28-day incubation period.
  • test specimen of “IMRE” as compared to the“LTA specs” and“no treated concrete” has the lowest percentage for the water absorption test.
  • test specimen of“IMRE” has the lowest measurement.
  • composition as defined above may be applied onto a variety of surfaces and may be suited for application onto porous surfaces to reduce the water permeability and/or water absorption property of the surface.
  • the liquid mixture as defined above may also be applied onto a variety of surfaces and may be suited for application onto porous surfaces to reduce the water permeability and/or water absorption property of the surface.
  • the composition and/or liquid mixture may be used to reduce the water permeability and/or water absorption property of the surface, or to increase the water-repellency properties of the surface.
  • composition and/or liquid mixture may be used to improve the impermeability and resistance to cracking of surface, specifically hardened concrete. Further, the composition and/or liquid mixture may be used to protect surfaces (e.g. concrete surface) and transform it from hydrophilic to superhydrophobic as well as to provide antifungal functions on the surfaces.
  • the alkyl siliconate (silicone) of the composition as defined above may also be useful for improving the adhesion between the composition and the surface to which it is applied. This may advantageously allow the disclosed composition to readily penetrate pores, cover crevices or even smooth uneven surfaces to result in uniform application of the composition.
  • composition and liquid mixture relate to multiple functional agents (such as waterproofing, water repellent and antifungal) that are able to protect various types of porous substrates from deterioration due to water absorption and thus, extend their useful lives.
  • functional agents such as waterproofing, water repellent and antifungal
  • the treatment reduces the rate of water absorption considerably, thereby, preventing water related damages.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Paints Or Removers (AREA)

Abstract

La présente invention concerne une composition comprenant un siliconate d'alkyle et au moins un composé supplémentaire choisi parmi un alkylsilane ou un géopolymère. L'invention concerne également un mélange liquide et un procédé de préparation du mélange liquide. La présente invention concerne en outre un procédé pour conférer une résistance hydrophobe et fongique à une surface et des utilisations de la composition associée.
PCT/SG2019/050148 2018-03-20 2019-03-20 Formulation d'imperméabilisation WO2019182513A1 (fr)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111269024A (zh) * 2020-04-12 2020-06-12 长沙汇泉环境科技有限公司 一种防污抗油的表面渗透防护剂及其制备方法
CN111607233A (zh) * 2020-06-29 2020-09-01 南京大学 一种含硅高透明阻燃eva转光膜及其制备方法
CN113801501A (zh) * 2021-09-07 2021-12-17 浙江大学杭州国际科创中心 一种双组份复合型地坪硬化材料及其制备方法
CN116042181A (zh) * 2022-11-08 2023-05-02 安徽上氟表面处理技术有限公司 一种无机非金属建材防水防油防污处理剂及其制备方法
CN116396029A (zh) * 2023-03-27 2023-07-07 重庆科顺新材料科技有限公司 用于填充水泥基瓷砖缝隙的双组份组合物及建筑墙体

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FR2528818A1 (fr) * 1982-06-22 1983-12-23 Joseph Davidovits Procede de fabrication de revetements de sols ou de murs par polycondensation de geopolymeres
WO1998007793A1 (fr) * 1996-08-16 1998-02-26 Fmc Corporation Compositions protectrices hybrides inorganiques-organiques resistant aux degradations causees par l'environnement
WO2008113609A2 (fr) * 2007-03-22 2008-09-25 Xuhong, Turella-Yuan Composition de géopolymère, revêtement pouvant être obtenu à partir de celle-ci et procédés
WO2012145659A1 (fr) * 2011-04-20 2012-10-26 Dow Corning Corporation Compositions aqueuses stables d'alkyl siliconates de métal alcalin avec alkylsilanes fluorés et aminosilanes, et procédés de traitement de surface à l'aide des compositions
US8299151B1 (en) * 2010-01-29 2012-10-30 Advanced Concrete Technologies Llc Protective coatings for inorganic substrates and associated methods
CN104829161B (zh) * 2015-04-02 2016-09-28 安徽建筑大学 一种建筑石膏用防水剂及其制备方法
KR101736146B1 (ko) * 2016-10-25 2017-05-16 전혜란 친환경 보호 코팅제 조성물 및 이를 이용한 시공방법

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Publication number Priority date Publication date Assignee Title
FR2528818A1 (fr) * 1982-06-22 1983-12-23 Joseph Davidovits Procede de fabrication de revetements de sols ou de murs par polycondensation de geopolymeres
WO1998007793A1 (fr) * 1996-08-16 1998-02-26 Fmc Corporation Compositions protectrices hybrides inorganiques-organiques resistant aux degradations causees par l'environnement
WO2008113609A2 (fr) * 2007-03-22 2008-09-25 Xuhong, Turella-Yuan Composition de géopolymère, revêtement pouvant être obtenu à partir de celle-ci et procédés
US8299151B1 (en) * 2010-01-29 2012-10-30 Advanced Concrete Technologies Llc Protective coatings for inorganic substrates and associated methods
WO2012145659A1 (fr) * 2011-04-20 2012-10-26 Dow Corning Corporation Compositions aqueuses stables d'alkyl siliconates de métal alcalin avec alkylsilanes fluorés et aminosilanes, et procédés de traitement de surface à l'aide des compositions
CN104829161B (zh) * 2015-04-02 2016-09-28 安徽建筑大学 一种建筑石膏用防水剂及其制备方法
KR101736146B1 (ko) * 2016-10-25 2017-05-16 전혜란 친환경 보호 코팅제 조성물 및 이를 이용한 시공방법

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111269024A (zh) * 2020-04-12 2020-06-12 长沙汇泉环境科技有限公司 一种防污抗油的表面渗透防护剂及其制备方法
CN111607233A (zh) * 2020-06-29 2020-09-01 南京大学 一种含硅高透明阻燃eva转光膜及其制备方法
CN113801501A (zh) * 2021-09-07 2021-12-17 浙江大学杭州国际科创中心 一种双组份复合型地坪硬化材料及其制备方法
CN116042181A (zh) * 2022-11-08 2023-05-02 安徽上氟表面处理技术有限公司 一种无机非金属建材防水防油防污处理剂及其制备方法
CN116396029A (zh) * 2023-03-27 2023-07-07 重庆科顺新材料科技有限公司 用于填充水泥基瓷砖缝隙的双组份组合物及建筑墙体

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