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WO2025125377A1 - Formulations huile dans l'eau à base d'huile végétale - Google Patents

Formulations huile dans l'eau à base d'huile végétale Download PDF

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Publication number
WO2025125377A1
WO2025125377A1 PCT/EP2024/085784 EP2024085784W WO2025125377A1 WO 2025125377 A1 WO2025125377 A1 WO 2025125377A1 EP 2024085784 W EP2024085784 W EP 2024085784W WO 2025125377 A1 WO2025125377 A1 WO 2025125377A1
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Prior art keywords
oil
formulation
surfactant
refined
vegetable oil
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English (en)
Inventor
Antía GONZÁLEZ BARRAL
Patricia VILLAVERDE DIOS
Luciano FERNÁNDEZ FONDEVILA
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Foresa Technologies SL
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Foresa Technologies SL
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Publication of WO2025125377A1 publication Critical patent/WO2025125377A1/fr
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/22—Materials not provided for elsewhere for dust-laying or dust-absorbing
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL 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
    • C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10—Coating
    • C03C25/24—Coatings containing organic materials
    • C03C25/255—Oils, waxes, fats or derivatives thereof
    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04B—GENERAL BUILDING CONSTRUCTIONS; WALLS, e.g. PARTITIONS; ROOFS; FLOORS; CEILINGS; INSULATION OR OTHER PROTECTION OF BUILDINGS
    • E04B1/00—Constructions in general; Structures which are not restricted either to walls, e.g. partitions, or floors or ceilings or roofs
    • E04B1/62—Insulation or other protection; Elements or use of specified material therefor
    • E04B1/74—Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls
    • E04B1/88—Insulating elements for both heat and sound
    • E04B1/90—Insulating elements for both heat and sound slab-shaped

Definitions

  • the present invention relates to vegetable oil-based O/W formulations, an environmentally friendly alternative to formulations based on mineral oil, which are obtainable from renewable resources instead of non-renewable resources. They comprise an O/W emulsion that contains refined vegetable oils with a flash point higher than 260°C and water, as well as specific surfactants and rheological additives which in combination result in a kinetically stable emulsion and formulation.
  • the vegetable oil-based formulations of the invention are kinetically stable and particularly useful for controlling dust typically generated in manufacturing, handling or installing fibre insulation products. More specifically, the invention provides an antidusting formulation for manufacturing fibreglass, rock wool or slag wool insulation products, so that the amount of dust generated during the manufacturing, handling or installing of those products can be significantly reduced.
  • formulations can also be used for other applications such as increasing the flexibility of polyflavonoid-based foams (i.e., tannin-based foams), or improving the release of boards from the molds used during manufacture, for example, but not limited to, of wood derived boards, fibreboards (including MDF and HDF boards, i.e., mediumdensity and high-density fibreboards), particleboards, chip boards, oriented strand boards, plywood, paperboards, and boards or insulations made from fibreglass, rock wool or slag wool.
  • polyflavonoid-based foams i.e., tannin-based foams
  • MDF and HDF boards i.e., mediumdensity and high-density fibreboards
  • particleboards chip boards
  • oriented strand boards plywood, paperboards, and boards or insulations made from fibreglass, rock wool or slag wool.
  • the invention also refers to articles treated or manufactured with the formulations of the invention, for example the insulation products, panels, foams or boards obtained by the use of said formulations.
  • the manufacture of said insulation products generally comprises a step of preparing the mineral fibres themselves, which can be performed by different procedures, for example according to the techniques known as rotary process (internal centrifuge), cascade process (external centrifuge), and flame attenuation process (pot & marble).
  • an adhesive resin generally a thermosetting resin
  • the mixture of fibres and resin is subjected to a thermal treatment, at a temperature generally higher than 150 °C, such as around 200 °C, for the polycondensation of the resin to take place and thus obtain a thermal and/or acoustic insulation product.
  • Commonly used adhesive compositions are, for example, acid or basic phenolic resins, sugar-based resins or starch-based resins.
  • Mineral oils in particular bright stock oils, have been extensively used as anti-dusting agents in the manufacture of the above-mentioned insulation products. However, they are based on non-renewable resources, cause environmental problems (e.g., air pollution) and, when mixed with the adhesive composition, tent to result in a rapid separation of phases despite the use of stirring mechanisms.
  • W02009/046521 A1 provides an aqueous anti-dusting emulsion formulation for use in the manufacture of fibre wool insulation, wherein the formulation may comprise a petroleum hydrocarbon, a triglyceride and a surfactant. Some of the embodiments disclosed therein, however, do not comprise the petroleum hydrocarbon component.
  • the petroleum hydrocarbon component may be mineral oil, bright stock oil, paraffinic slack wax or petrolatum.
  • the triglyceride may be palm oil, palm kernel oil, coconut oil, peanut oil, soybean oil, soy stearin, linseed oil, stearin oil, corn oil, cottonseed oil, rape seed oil, canola oil, sunflower oil, safflower oil, tung oil, castor oil, fish oil, lard, tallow, tall oil, animal fats and mixtures thereof.
  • the surfactant comprises a sodium or ammonium salt of a lignosulphonic acid.
  • W02009/046521 A1 discloses an anti-dusting emulsion formulation (sample 2) obtained by adding unmodified soy oil to a water solution comprising ammonium lignosulphonate under a high-speed mixer, followed by homogenization at 3000 psi, and then cooling to ambient temperature. According to the experimental data provided by this patent application, no separation was observed in sample 2 after 1 hour.
  • emulsion identified as sample 2 in W02009/046521 A1 also referred to as Walker's emulsion E2 in this document
  • One problem to be solved by the present invention thus is to provide an environmentally friendly alternative to formulations based on mineral oil, which are obtainable from renewable resources instead of non-renewable resources.
  • This is solved by the kinetically stable vegetable oil-based formulations according to the invention, which are O/W emulsions comprising refined vegetable oils with a flash point higher than 260 °C, low levels of specific surfactants and rheological additives, and water.
  • Said formulations can be manufactured on an industrial level, and completely or partially avoid the use of non-renewable resources, e.g., petroleum derived resources such as mineral oils. Due to their particular composition, viscosity and, preferably, particle size distribution, the formulations of the invention have a high kinetic stability (at least 1 month at normal conditions).
  • Said formulations are particularly useful for controlling dust generated in manufacturing, handling or installing fibre insulation products and, therefore, they can be used as anti-dusting agents in the manufacture of said articles, in particular fibreglass, rock wool or slag wool insulation products.
  • These vegetable oil-based formulations can also be used for other applications such as increasing the flexibility of polyflavonoid-based foams, or improving the release of boards from the molds used during manufacture, for example, but not limited to, of wood derived boards, fibreboards (including MDF and HDF boards, i.e., medium-density and high- density fibreboards), particleboards, chip boards, oriented strand boards, plywood, paperboards, and boards or insulations made from fibreglass, rock wool or slag wool.
  • wood derived boards including MDF and HDF boards, i.e., medium-density and high- density fibreboards
  • particleboards i.e., chip boards, oriented strand boards, plywood, paperboards, and boards or insulations made from fibreglass, rock wool or slag wool.
  • an object of the invention is a vegetable oil-based formulation which is an oil in water (O/W) emulsion comprising:
  • the anionic surfactant is selected from aryl sulfonate, >Ci2 alkyl sulfate, >Ci2 alkyl carboxylate, alkaline salt of C10-C15 alkyl-aryl sulfonic acid and a combination thereof, and
  • the non-ionic surfactant is selected from primary alcohol ethoxylate, secondary alcohol ethoxylate and a combination thereof, wherein said non-ionic surfactant has a HLB higher than 8;
  • rheological additive which is an ionic polysaccharide, preferably selected from the group consisting of gum ghatti, xanthan gum and a combination thereof;
  • the formulation has an active matter content of about 31 wt% and about 69 wt% and the rest of the formulation, until reaching 100 wt%, is water, the active matter content comprising all the components which are different from water; and wherein the viscosity of the formulation is of about 100 cP to about 1500 cP, preferably 150 cP to 1200 cP (25°C, Viscosimeter Brookfield HV, 20 rpm, preferably spindle 02).
  • the formulation of the invention is particularly useful for the intended uses, especially for controlling dust typically generated in manufacturing, handling or installing fibre insulation products, since it complies with the following features: 1. High active matter content: about 31 wt.% to about 69 wt. %, preferably about 45 wt.% to about 55 wt. %.
  • High stability at least 1 month (kinetic stability), preferably at least 2 months, more preferably at least 6 months, and even more preferably at least 12 months, at normal conditions of temperature and pressure.
  • Viscosity ranges and values specified in this document are expressed in cP, a well- known viscosity unit commonly used in the technical field of the invention. These viscosity ranges and values can be unambiguously converted to the corresponding ranges and values according to SI Units (Pa s), since that 1 cP is equal to 10' 3 Pa s.
  • the emulsion of the invention has a preferred viscosity of 150 cP to 1200 cP, i.e., of 0.15 Pa s to 1.2 Pa s.
  • the viscosity can be measured at 25°C using a Brookfield HV Viscometer, in particular DV-1 , preferably spindle 02, at 20 rpm.
  • An emulsion is a “fluid colloidal system in which liquid droplets and/or liquid crystals are dispersed in a liquid. The droplets often exceed the usual limits for colloids in size.
  • An emulsion is denoted by the symbol O/W if the continuous phase is an aqueous solution and by W/O if the continuous phase is an organic liquid (an 'oil'). More complicated emulsions such as O/W/O (i.e., oil droplets contained within aqueous droplets dispersed in a continuous oil phase) are also possible.”
  • a suspension according to the IUPAC, is “a liquid in which solid particles are dispersed”.
  • Vegetable oils comprised in the formulation of the invention are liquids at normal temperature and pressure conditions (i.e., at a temperature of 20°C and an absolute pressure of 1 atm (101 MPa)) and, therefore, they form O/W emulsions.
  • Glycerides are made up of fatty acids with a high molecular mass and trihydroxylated alcohols such as propanetriol, glycerol or glycerine.
  • Glycerides can have an esterified hydroxyl group, called monoglyceride, diglyceride when they have two esterified hydroxyl groups, and triglyceride when three hydroxyl groups were esterified.
  • glycerides When glycerides have saturated carbon chains, they are referred to as fats, all the carbon atoms exhibit sp3 hybridisation, except the carbon of the functional group (ester), from which it can be deduced that the fatty acids in these structures are saturate chains.
  • vegetable oils are characterised by the presence of double bonds in the fatty acid chains that form the glyceride structure, and therefore not all the carbon atoms exhibit sp3 hybridisation, a new functionality appears, where the carbon atoms exhibit sp2 hybridisation and different chemical reactivity, and the fatty acids present are not saturated.
  • the saturated fatty acids have a specific packing or order in the triglyceride molecules, which explains why the fats are solid substances, whereas the particular stereochemistry of the fatty acids that make up the oils (unsaturated fatty acids) with geometric isomers, the most abundant being cis isomer, provides a different spatial order, which can be seen in the figures below.
  • refined vegetable oils refers to crude oils obtained by mechanical or solvent extraction of vegetables, which have been chemically or physically refined to get a better quality, a more acceptable aspect (limpidity), a lighter odour and colour, longer stability and good safety through the elimination of pollutants.
  • Refined vegetable oils may be obtained by conventional processes as those described, for example, in Said Gharbi, The Scientific World Journal, Vol. 2022, Article ID 6627013 (2022). Those refined vegetable oils have not been subjected to any kind of hydrogenation and, therefore, they can also be referred to as non-hydrogenated oils or non-hydrogenated vegetable oils.
  • Refined vegetable oils comprised in the formulation of the invention are characterized by having a flash point higher than 260°C, preferably higher than 280°C, so that they can be used in the manufacturing of insulation products. Said high flash point is important in order to avoid fire in the manufacturing process of insulation product, which typically requires thermal treatment at temperatures higher than 150 °C, typically around 200°C.
  • flash point refers to the lowest temperature, measured to a barometric pressure of 101.3 kPa, at which application of an ignition source causes the vapour of the test portion to ignite momentarily and the flame to propagate across the surface of the liquid under the specified conditions of test.
  • the flash point may be determined following ASTM D92-18, Standard Test Method for Flash and Fire Points by Cleveland Open Cup Tester.
  • the refined vegetable oil is preferably selected from the group consisting of refined soybean oil, refined sunflower oil, refined rapeseed oil, refined corn oil, refined palm oil and mixtures thereof; more preferably refined soybean oil.
  • the flash point of the at least one refined vegetable oil comprised in the formulation of the invention is higher than 260°C, preferably higher than 280°C, more preferably of 300°C to 350°C and, even more preferably of 310°C to 330°C.
  • the at least one vegetable oil comprised in the formulation described herein is a nonhydrogenated oil (i.e. , it comprises a high proportion of unsaturated fatty acids) which is liquid in normal conditions (20 °C and 1 atm (101 MPa)).
  • said refined vegetable oil preferably has an iodine value higher of about 50 g iodine per 100 g of oil.
  • the iodine value may be determined following the standard LINE-EN ISO 3961 :2018 Animal and vegetable fats and oils. Determination of iodine value.
  • the iodine value of the at least one refined vegetable oil having a flash point higher than 260°C as defined in this document may be as follows:
  • the vegetable oil is refined soybean oil having a flash point higher than 260°C, preferably higher than 280°C, more preferably of about 300 °C to about 350°C, even more preferably of about 310 °C to about 330°C, wherein its iodine value preferably ranges from about 120 g to about 155 g iodine per 100 g of soy oil, both parameters measured as defined in this document.
  • the amount of vegetable oil in the formulation of the invention ranges from about 30 wt.% to about 60 wt.% of the total weight of the formulation. In preferred embodiments, this amount may range from about 40 wt.% to about 60 wt.%, more preferably from about 45 wt.% to about 55 wt.%, of the total weight of the formulation.
  • a lower content of vegetable oil would negatively affect dusting properties of the formulation. This reduced efficacy could be partially overcome by using a higher amount of formulation.
  • Oils have the difficulty that they have the property of occluding water inside their structure, normally between 2 and 6 times their weight. This property causes their emulsification to be very complicated, as it leads to the forming of semisolid creams, which makes it impossible to be properly applied to any material, e.g., by spraying, which is the preferred way of application, for which the product needs to be in a liquid state.
  • Emulsifiers are a group of substances of different origin and properties that may contribute to obtain a greater stabilization of the emulsions or suspensions; this is due mainly to its amphiphilic or double affinity character, which, from the physico-chemical point of view, is defined as a double polar and apolar property. Within this large group of compounds, we can find e.g., surfactants.
  • surfactant refers to a substance that possesses superficial or interfacial activity.
  • Surfactants are usually organic compounds that are akin to amphiphilic, which means that this molecule, being as double-agent, each contains a hydrophilic "water-seeking" group (the head), and a hydrophobic "water-avoiding” group (the tail).
  • a surfactant contains both a water-soluble component and a water-insoluble component. Surfactants diffuse in water and get adsorbed at interfaces between air and water, or at the interface between oil and water in the case where water is mixed with oil.
  • the waterinsoluble hydrophobic group may extend out of the bulk water phase into a non-water phase such as air or oil phase, while the water-soluble head group remains bound in the water phase. It should be noted that not all amphiphilic compounds possess such activity, so that it is required that the substance has relatively balanced properties, i.e., it must be neither too hydrophilic nor too hydrophobic.
  • surfactant does not have an exact translation in Spanish, where the generic term “tensioactivo” is used, which refers to an activity or an action on the surface or interfacial tension, i.e., on the Gibbs free energy. This term is equivalent to surfactant only if it is assumed that the surface or interfacial activity necessarily results in a decrease in tension, which is true in most cases of practical interest.
  • the formulation of the invention comprises about 1 wt.% to about 5 wt.%, preferably about 1.5 wt.% to about 3 wt.%, of at least one anionic surfactant, at least one non-ionic surfactant or a combination thereof, wherein the anionic surfactant is selected from aryl sulfonate, (higher than C12) alkyl sulfate, (equal to or higher than C12) alkyl carboxylate, alkaline salt of C10-C15 alkyl-aryl sulfonic acid and a combination thereof, and the nonionic surfactant is selected from primary alcohol ethoxylate, secondary alcohol ethoxylate and a combination thereof, wherein said surfactant has a hydrophilic lipophilic balance (HLB) higher than 8.
  • HLB hydrophilic lipophilic balance
  • surfactants in combination with the rheological additive as described in this document are particularly useful in providing the kinetically stable O/W emulsion in the formulation of the invention.
  • sulfate or carboxylate surfactants having an alkyl moiety lower than C12 typically generate a high amount of foam, which jeopardize the stability of the emulsion.
  • kinetically stable in the frame of the present invention means that the viscosity of formulations and emulsions to which the term refers to does not significantly change and, additionally, said formulations or emulsions do not separate into distinct phases within the indicated timeframe, for example, at least 1 months, preferably at least 2 months, more preferably at least 6 months, and even more preferably at least 12 months.
  • the allowed viscosity variation until it is considered that said formulation has lost its kinetically stability may be different.
  • Phase separation can be visually tested in a 100 ml test-tube. Formulations and emulsions are considered not stable if the % volume of phase separation is higher than 5 % of the total volume of the sample.
  • Non-ionic surfactants are surfactants that do not bear an electrical charge in aqueous solution since their hydrophilic groups are of the alcohol, phenol, ether o amide type. A high proportion of these surfactants can be rendered relatively hydrophilic by the presence of a polyether chain of the polyethylene oxide type.
  • alcohol ethoxylates are a class of non-ionic surfactants that contain a hydrophobic alkyl chain attached via an ether linkage to a hydrophilic ethylene oxide (EO) chain and have the general structure R(OCH2CH2) n OH, wherein R is the hydrophobic alkyl chain.
  • Non- anionic surfactant that can be comprised in the formulation of the invention is selected from primary alcohol ethoxylate, secondary alcohol ethoxylate and a combination thereof, wherein said surfactant has a hydrophilic lipophilic balance (HLB) higher than 8, preferably higher than 10, more preferably of 12 to 14.
  • Suitable non-ionic surfactants may be, for example, Tergitol® 15 S-9 (i.e., a secondary alcohol ethoxylate having a HLB of 12 to 14, and an EO content of 9), which is commercially available by Dow.
  • “Anionic surfactants” are surfactants that may be dissociated into an amphiphilic anion and a cation, usually an alkali metal or a quaternary ammonium.
  • Anionic surfactant comprised in the formulation of the invention is selected from aryl sulfonate, (higher than C12) alkyl sulfate, (equal to or higher than C12) alkyl carboxylate, alkaline salt of C10-C15 alkyl-aryl-sulfonic acid and a combination thereof.
  • said surfactants may be, in particular, alkaline or ethanolamine salts of the corresponding sulfonate, sulfate or carboxylate (fatty acid).
  • aryl sulfonates in particular naphthalene sulfonates such as sodium naphthalene sulfonate, are preferred because they are able to provide a high stability to the O/W emulsion over time (at least 6 months, preferably at least 12 months, at normal conditions), result in a stable vegetable oil-based formulation since the compatibility with other ingredients such as phenolic resins to be used as adhesive is higher in comparison to other surfactants, typically have a lower cost than alcohol ethoxylate and, additionally, they show a higher stability than sulfates and carboxylates in hard waters and pH changes.
  • Surfactants may either be added to the water or the oil phase.
  • the surfactant comprises a salt of a fatty acid, it may be obtained in situ, within the water phase, by a saponification reaction.
  • the weight percentages indicated refer to the final concentration of surfactants within the O/W emulsion formulation, independently of whether they were added as such or generated in situ by reaction of the fatty acids contained in the oils or waxes and an alkali, preferably an ethanolamine, which is added to the aqueous phase, before carrying out the emulsification.
  • an alkali preferably an ethanolamine
  • the ethanolamine may be selected for example, but not limited to, from monoethanolamine, diethanolamine and triethanolamine.
  • the ratio of surfactant vs. total amount of oil generally known as S/O ratio, preferably is of about 1 wt.% to about 10 wt.%, more preferably of about 2 wt.% to about 8 wt.%, even more preferably of about 3 wt.% to about 5 wt.%.
  • O/W emulsions comprising refined vegetable oils, in particular those comprising refined soybean oil, tent to separate into phases when they are not formulated with the proper surfactant or do not have the correct viscosity.
  • the present invention solves this problem by combining the required amount of specific surfactants as described herein with a very specific kind of rheological additives, i.e., an ionic polysaccharide such as gum ghatti, xanthan gum or mixtures thereof.
  • Rheology is the study of the principles that regulate the movement of fluids, i.e., substances that deform continuously when any kind of shear stress is applied to them. This branch of physics also studies the viscosity, elasticity, plasticity and spilling of fluids.
  • Rheology modifiers have the ability to modify the rheological characteristics of both aqueous and non-aqueous formulations. Among those, polysaccharide-type rheology modifiers typically have a high molecular weight, are colourless, tasteless and have the property of being hydrocolloid, whereby they retain water and swell, resulting in an increase in viscosity. It is worth noting that not all rheology modifiers are suitable to overcome the technical problem posed above. Thus, some of them increase the viscosity too much, which makes the use of the emulsion unfeasible in certain situations, whereas other additives may be incompatible with the resins used in the manufacturing of insulation products.
  • the vegetable oil-based formulation of the invention comprises about 0.2 wt.% to about 4 wt.%, preferably about 0.5 wt.% to about 1 .5 wt.%, of at least one rheological additive which is an ionic polysaccharide, preferably selected from the group consisting of gum ghatti, xanthan gum and a combination thereof, more preferably gum ghatti.
  • Gum ghatti (CAS Number 9000-28-6) is a complex polysaccharide gum of high molecular weight which may be extracted from Anogeissus latifolia, a tree originates from India. This ionic polysaccharide is mainly composed of the calcium and magnesium salts of L- arabinose, D-galactose, D-manose, D-xylose, D-glucuronic acids, in particular, in the approximate molar ratio of 10:6:2:1 :2.
  • gum ghatti disperses in cold water forming viscous solutions at concentrations of about equal to or higher than 5 wt.%, which show a no-Newtonian behavior. A maximum viscosity is achieved at a concentration between 5 wt.% and 7 wt.%.
  • Xanthan gum (CAS Number 11138-66-2) is a polysaccharide gum that can be produced from simple sugars using a fermentation process with bacteria from the specifies Xanthomonas campestris.
  • the primary structure of this ionic polysaccharide is mainly composed of D-glucose and D-mannose along with D-glucuronic acid.
  • the vegetable oil-based formulation of the invention comprises about 31 wt.% to about 69 wt.% of active matter content.
  • the active matter content is of about 45 wt.% to about 55 wt.%.
  • the active matter content refers to the total weight of the sum of all the components of the formulation which are different from water.
  • the formulation of the invention has a viscosity of about 100 cP to about 1500 cP, preferably about 150 cP to about 1200 cP, more preferably of about 300 cP to about 600 cP.
  • the viscosity can be measured at 25°C using a Brookfield HV Viscometer, in particular DV-1 , preferably spindle 02, at 20 rpm.
  • the vegetable oil-based formulation of the invention is also characterized in that the oil particles in the emulsion have a gaussian distribution with a Sauter mean diameter (D(3,2)) of about 0.5 pm to about 1.5 pm, preferably of about 0.5 pm to about 1.0 pm, measured by laser diffraction in a Mastersizer 300 equipment.
  • D(3,2) Sauter mean diameter
  • “Sauter mean diameter”, also designated as D(3,2), D32 or D(32) is the mean diameter with the same ratio of volume to surface area as the entire ensemble. It was originally developed by German scientist Josef Sauter in the late 1920s. The size of drops is determined based on the absorption/scattering of light. The technique depends on the fact that absorption/scattering is proportional to the surface area of the drops.
  • the small size and gaussian distribution of the oil particles in the O/W emulsion of the invention help to increase the stability of the emulsion and, at the same time, improve the effectivity of the vegetable oil-based formulation for controlling dust since the oil drops can be more effectively distributed in the fibre.
  • the formulation of the invention preferably has a density of about 0.94 g/m 3 to about 0.98 g/m 3 , measured by pycnometer according to the standard ISO 2811-1 :2023.
  • the vegetable oil-based formulations according to the invention are kinetically stable, which means that they do not significantly change its viscosity nor separate into distinct phases within the indicated timeframe, e.g., no oil particles appear throughout the formulation within a time frame.
  • the formulation of the invention is kinetically stable during at least 1 months at normal temperature and pressure conditions, preferably at least 2 months, more preferably at least 4 months, still more preferably at least 6 months, even more preferably at least 1 year, and the most preferably at least 2 years. This stability allows the formulation to be commercially distributed and offered, without the need of special conditions or equipment.
  • the timeframe of kinetical stability may be even further increased, to at least two years, by reducing the storing temperature, e.g., to temperatures lying between 5°C and 15°C, preferably between 5°C and 10°C.
  • the vegetable oil-based formulation of the invention may comprise other additives such as, for example, biocides which may be added to the formulation with the aim avoid the development of mildew, since it may negatively affect the applicability of the vegetable oil-based formulation of the invention.
  • said biocide may be present in the vegetable oil-based formulation of the invention in an amount of about 0.05 wt.% to about 0.3 wt.%, in particular, in an amount of 0.1 wt.% with respect to the total weight of the formulation.
  • Suitable biocides commercially available that can be used are, for example, Mergal® 758, Acticide® MBS, Mirecide® M 1 85.
  • the vegetable oil-based formulation according to the invention may be obtained by different methods of emulsification, including methods of emulsification well known in the art.
  • said O/W emulsion formulation may be obtained by direct emulsification method (sometimes herein referred to as direct O/W method), by slowly adding the oil phase to the water phase, both heated to temperatures equal to or higher than 70°C, preferably of about 70 °C to about 80 °C, under stirring or equivalent means of mixing.
  • the surfactant may be contained either in the oil phase or the water phase, normally, but not necessarily, an ionic surfactant is added to the water phase, and a nonionic surfactant to the oil phase.
  • the surfactant may be obtained in situ by reaction of corresponding reagents.
  • the invention also provides a method of manufacturing a vegetable oil-based formulation as described in this document, wherein the method comprises: a) obtaining a water phase comprising a rheological additive which is an ionic polysaccharide preferably selected from the group consisting of gum ghatti, xanthan gum and a combination thereof and, optionally, at least one anionic or non-ionic surfactant as defined in this document; b) obtaining an oil phase comprising at least one refined vegetable oil with a flash point higher than 260°C and, optionally, at least one anionic or non-ionic surfactant as defined in this document; wherein at least one of the water phase or the oil phase comprises at least one surfactant as defined above; c) heating the water phase and the oil phase at a temperature equal to or higher than about 70°C, preferably of about 70 to about 80°C; d) adding the heated oil phase to the heated water phase and stirring the mixture at a temperature equal to or higher than about 70°C, preferably of about
  • the refined vegetable oil may be selected from the group consisting of refined soybean oil, refined sunflower oil, refined rapeseed oil, refined corn oil, refined palm oil and mixtures thereof; and the surfactant may be selected from aryl sulfonates, fatty acid salts, alcohol ethoxylates and mixtures thereof.
  • the formulation comprises at least one anionic surfactant selected from aryl sulfonate, >Ci2 alkyl sulfate, >Ci2 alkyl carboxylate, alkaline salt of C10-C15 alkyl-aryl-sulfonic acid and a combination thereof, preferably an aryl sulfonate surfactant, preferably a naphthalene sulfonate surfactant, more preferably sodium naphthalene sulfonate; and said anionic surfactant is comprised in the aqueous phase obtained in step a).
  • anionic surfactants as described in this document can also be present in the oil phase obtained in step b), since the pre-mix time of step d) (at least 20 minutes) is enough to solubilize them.
  • the formulation comprises at least one non-ionic surfactant selected from primary alcohol ethoxylate, secondary alcohol ethoxylate and a combination thereof, wherein said non-ionic surfactant have a HLB higher than 8, preferably a HLB higher than 10, more preferably of 12 to 14; and said non-ionic surfactant is comprised in the oil phase obtained in step b).
  • non-ionic surfactants as described in this document can also be present in the aqueous phase obtained in step a), since the pre-mix time of step d) (at least 20 minutes) is enough to solubilize them.
  • the oil phase can be added to the water phase in a period of time of about 10 minutes to about 40 minutes, preferably of about 15 minutes to 30 minutes, the mixture obtained by addition of the heated oil phase to the heated water phase in step d) can be stirred at a rate of 30 rpm to 350 rpm for at least 20 minutes; the homogenization of step e) can be carried out in an homogenizer at a pressure of about 30 bar (3 MPa) to about 350 bar (35 MPa) preferably for a period of 1 min to 30 min; and/or the homogenized mixture can be gradually cold at a rate of 1 to 7 °C /min in step f), preferably of 4 to 7 °C/min.
  • the homogenization step in particular when it is carried out in an homogenizer at a pressure of about 30 bar (3 MPa) to about 350 bar (35 MPa), preferably for a period of 1 min to 30 min, allows the generation of the oil particles in the emulsion have a gaussian distribution with a Sauter mean diameter (D(3,2)) of about 0.5 pm to about 1.5 pm, preferably of about 0.5 pm to about 1.0 pm, measured by laser diffraction in a Mastersizer 300 equipment.
  • D(3,2) Sauter mean diameter
  • the particle diameter is inversely proportional to the applied pressure.
  • the homogenization may be carried out using a two-stage homogenizing valve assembly, also referred to as two-phase homogenizer in this document, which includes a first-stage valve and a second-stage valve that serves to exert a backpressure of the fluid moving through the first-stage valve.
  • the homogenization is carried out in two different homogenization sub-stages or phases, wherein different pressures are applied in each of these substages, in order to further reduce the particle diameter.
  • pressure applied in the second homogenization sub-stage i.e. , pressure applied to the second-stage valve
  • pressure applied to the second-stage valve is of about 10% to about 20% of the pressure of the first homogenization sub-stage.
  • the emulsification according to the method of the invention may be carried out either in a single reactor, by using mechanical dispersion, a rotor-stator, or with stirring and homogenizer.
  • the emulsification according to the invention may be carried out by using two differentiated reactors, an oil phase reactor and a water phase reactor.
  • the first reactor has a temperature regulating system and a stirrer, while the second mixing reactor or reactor in addition to the temperature control system has a disperser.
  • the emulsification may be carried out either with stirring, stirring and mechanical dispersion, stirring and rotor-stator (e.g., ULTRA TURRAX® type).
  • the formulations of the present invention may be applied to a variety of insulation products for controlling the generation of dust during its manufacture. Besides, they can also be used to improve flexibility of polyflavonoid-based foams.
  • a further object of the invention is the use of a formulation according to the present invention in the manufacture of articles selected from fibreglass insulations, rock wool insulations, slag wool insulations or polyflavonoid-based foams.
  • the invention refers to the use of the formulation herein described as anti-dust additive in the manufacture of insulations articles such as fibreglass insulations, rock wool insulations, slag wool insulations or a combination thereof.
  • the formulations may also be useful as internal mold release formulations.
  • the formulations may for example be used in the manufacture of molded items, such as boards or panels, to avoid the adherence of fibres or chips, agglomerated with synthetic resins, to the metal parts of the process, thus reducing the degree of soiling of the manufacturing process.
  • the vegetable oil-based O/W emulsion formulation of the invention may also be useful as external mold release formulations.
  • the formulations may for example be applied onto the surface of the layers or sandwich of fibres and/or chips and/ or particles and/or fibreglass or rock wool, for example, but not limited to, by spraying, before being pressed in a press, during the manufacture of cellulose-derived boards, wood derived boards, fibreboards, particleboards, chipboards, oriented strand boards, fibreglass or rock wool, or combinations thereof.
  • the formulation of the invention may be mixed with other additives commonly used for said uses.
  • the vegetable oil-based formulation herein described may be mixed with adhesive resins commonly used in the manufacture of insulation products such as those based on fibreglass, wool rock or slag wool fibres such as, for example but not limited to, phenolic resins, acrylic resina, starch-based resins, sugar-based resins or a combination thereof.
  • adhesive resins commonly used in the manufacture of insulation products such as those based on fibreglass, wool rock or slag wool fibres
  • Formulations of the invention provide a great advantage in the manufacturing of articles selected from fibreglass, rock wool insulations or slag wool insulations because, in addition to its kinetical stability and anti-dust efficiency, are able to show a great compatibility those adhesive resins.
  • the invention also refers to articles treated or manufactured by using the vegetable oilbased formulation described in this document, as well as articles treated or manufactured by using the vegetable oil-based formulation obtained or obtainable by the method according to the invention.
  • said articles are insulation products such as fibreglass, rock wool or slag wool insulation products, comprising the formulation as defined above and fibreglass, rock wool or slag wool fibres.
  • Figure 1a shows an image of an insulation fiberglass product manufactured with a formulation according to the invention, whereas figure 1b shows an image of another manufactured without said formulation.
  • Figure 2 shows a graph of the distribution of the Sauter diameter of the particles for the formulation E1 according to the invention, which were stored at normal conditions and tested at different points of time: months 1 , 2 and 6.
  • Figure 3 shows a graph of the distribution of the Sauter diameter of the particles for formulation E1 according to the invention and sample 2 of prior art reference W02009/046521 A1 (identified as Walker's emulsion E2), both samples were previously stored at normal conditions for 24 hours.
  • Figure 4 graphically represents the viscosity (triangles) and stress (squares) measured at different shear rates for the formulation according to the invention E1 , samples were previously stored at normal conditions for 24 hours.
  • Figure 5 graphically represents the viscosity (triangles) and stress (squares) measured at different shear rates for the formulation according to the invention E6, samples were previously stored at normal conditions for 24 hours.
  • Example 1 preparation of a soybean O/W emulsion according to the invention (E1)
  • the oil phase was slowly added to the water phase at a rate of 20 g/min.
  • the mixture was mixed at a stirring rate of 300 rpm for 20 min thus obtaining a pre-emulsion, which was then introduced in a singlephase homogenizer at a pressure of 300 bar (30 MPa). Subsequently the mixture was cooled, at a rate of 4.5°C per minute, until reaching a temperature of 20-25°C.
  • 1000 g of a liquid emulsion were obtained, having a viscosity of 300 cP (25°C, Viscosimeter Brookfield HV, spindle 02, 20 rpm) and 53 wt.% of active matter.
  • the particle size distribution was gaussian with a Sauter diameter of 0.62 pm, measured by laser diffraction in a Mastersizer 300 equipment.
  • the emulsion was kinetically stable for at least 10 months, at normal pressure and temperature conditions.
  • Example 2 preparation of a rapeseed O/W emulsion according to the invention (E2)
  • the oil phase was slowly added to the water phase at a rate of 15 g/min.
  • the mixture was mixed at a stirring rate of 250 rpm for 22 min. thus obtaining a pre-emulsion, which was then introduced in a singlephase homogenizer at 200 bar (20 MPa).
  • the mixture was cooled, at a rate of 6.0°C per minute, until reaching a temperature of 20-25°C.
  • 660 g of a liquid emulsion were obtained, having a viscosity of 390 cP (25°C, Viscosimeter Brookfield HV, spindle 02, 20 rpm) and 53 wt.% of active matter.
  • the particle size distribution was gaussian with a Sauter diameter of 0.71 pm, measured by laser diffraction in a Mastersizer 300 equipment.
  • the emulsion was kinetically stable for at least 10 months, at normal pressure and temperature conditions.
  • Example 3 preparation of a sunflower O/W emulsion according to the invention (E3)
  • the oil phase was slowly added to the water phase at a rate of 10 g/min.
  • the mixture was mixed at a stirring rate of 350 rpm for 30 minutes thus obtaining a pre-emulsion, which was then introduced in a homogenizer at a first phase of 150 bar (15 MPa) and a second phase of 30 bar (3 MPa). Subsequently the mixture was cooled, at a rate of 4.0 °C per minute, until reaching a temperature of 20-25°C.
  • 430 g of a liquid emulsion were obtained, having a viscosity of 360 cP (25°C, Viscosimeter Brookfield HV, spindle 02, 20 rpm) and 58 wt.% of active matter.
  • the particle size distribution was gaussian with a Sauter diameter of 0.68 pm, measured by laser diffraction in a Mastersizer 300 equipment.
  • the emulsion was kinetically stable for at least 10 months, at normal pressure and temperature conditions.
  • Example 4 preparation of a soybean O/W emulsion according to the invention (E4)
  • the mixture was mixed for 20 minutes at a stirring rate of 300 rpm and a temperature of 75 °C thus obtaining a pre-emulsion, which was then introduced in a single-phase homogenizer at 320 bar (32 MPa). Subsequently the mixture was cooled, at a rate of 7.0 °C per minute, until reaching a temperature of 20-25°C. 1250 g of a liquid emulsion were obtained, having a viscosity of 384 cP (25°C, Viscosimeter Brookfield HV, spindle 02, 20 rpm) and 54 wt.% of active matter. The particle size distribution was gaussian with a Sauter diameter of 0.60 pm, measured by laser diffraction in a Mastersizer 300 equipment. The emulsion was kinetically stable for at least 10 months, at normal pressure and temperature conditions. to the invention
  • the mixture was mixed at a stirring rate of 300 rpm for 25 minutes thus obtaining a preemulsion, which was then introduced in a single-phase homogenizer at 300 bar (30 MPa). Subsequently the mixture was cooled, at a rate of 5.0 °C per minute, until reaching a temperature of 20-25°C. 1350 g of a liquid emulsion were obtained, having a viscosity of 710 cP (25°C, Viscosimeter Brookfield HV, spindle 02, 20 rpm) and 49 wt.% of active matter.
  • the particle size distribution was gaussian with a Sauter diameter of 0.60 pm, measured by laser diffraction in a Mastersizer 300 equipment.
  • the emulsion was kinetically stable for at least 10 months, at normal pressure and temperature conditions. to the invention
  • the oil phase was slowly added to the water phase at a rate of 9 g/min.
  • the mixture was mixed at a stirring rate of 300 rpm for 40 minutes thus obtaining a pre-emulsion, which was then introduced in a single-phase homogenizer at a homogenizer pressure of 300 bar (30 MPa). Subsequently the mixture was cooled, at a rate of 5.0°C per minute, until reaching a temperature of 20-25°C. 692.58 g of a liquid emulsion were obtained, having a viscosity of 120 cP (25°C, Viscosimeter Brookfield HV, spindle 02, 20 rpm) and 33 wt.% of active matter.
  • the particle size distribution was gaussian with a Sauter diameter of 0.53 pm, measured by laser diffraction in a Mastersizer 300 equipment.
  • the emulsion was kinetically stable for at least 10 months, at normal pressure and temperature conditions.
  • 315.11 g water, 20.64 g of sodium naphthalene-2-sulfonate (Tamol® NN-3501 from BASF, a solution having a 38 wt. % solid content, the amount expressed is referred to sodium naphthalene-2-sulfonate on dry matter basis) and 8.26 g of ghatti gum (N°CAS: 9000-28-6) were mixed, introduced in a water phase reactor and heated at 80°C.
  • a liquid emulsion 860 g of a liquid emulsion were obtained, having a viscosity of 1500 cP (25°C, Viscosimeter Brookfield HV, spindle 02, 20 rpm) and 63 wt.% of active matter.
  • the particle size distribution was gaussian with a Sauter diameter of 0.62 pm, measured by laser diffraction in a Mastersizer 300 equipment.
  • the emulsion was kinetically stable for at least 10 months, at normal pressure and temperature conditions.
  • Example 8 preparation of a soybean O/W emulsion accordinq to the invention (E8)
  • the mixture was mixed at a stirring rate of 300 rpm for 35 minutes thus obtaining a pre-emulsion, which was then introduced in a single-phase homogenizer at a pressure of 300 bar (30 MPa). Subsequently the mixture was cooled, at a rate of 5.0°C per minute, until reaching a temperature of 20- 25°C. 802,40 g of a liquid emulsion were obtained, having a viscosity of 780 cP (25°C, Viscosimeter Brookfield HV, spindle 02) and 47 wt.% of active matter. The particle size distribution was gaussian with a Sauter diameter of 0.64 pm, measured by laser diffraction in a Mastersizer 300 equipment. The emulsion was kinetically stable for at least 10 months, at normal pressure and temperature conditions. O/W emulsion maleic as surfactant bv direct O/W method
  • the mixture was mixed at a stirring rate of 300 rpm for 20 minutes thus obtaining a pre-emulsion, which was then introduced in a single-phase homogenizer at a pressure of 300 bar (30 MPa). Subsequently the mixture was cooled, at a rate of 4.0°C per minute, until reaching a temperature of 20-25°C. 780 g of a liquid emulsion were obtained, having a viscosity of 180 cP (25°C, Viscosimeter Brookfield HV, spindle 02, 20 rpm) and 49 wt.% of active matter. The particle size distribution was not gaussian with a Sauter diameter of 4.77 pm, measured by laser diffraction in a Mastersizer 300 equipment. The emulsion was kinetically stable for less than 1 week, at normal pressure and temperature conditions. O/W emulsion sulfate as surfactant bv direct O/W method
  • the mixture was cooled, at a rate of 6.5°C per minute, until reaching a temperature of 20- 25°C.
  • 1150 g of a liquid emulsion were obtained, having a viscosity of 930 cP (25°C, Viscosimeter Brookfield HV, spindle 02, 20 rpm) and 51 wt.% of active matter.
  • the particle size distribution was gaussian with a Sauter diameter of 0.46 pm, measured by laser diffraction in a Mastersizer 300 equipment.
  • the emulsion was kinetically stable for less than 1 week, at normal pressure and temperature conditions.
  • Comparative Example 3 preparation of a soybean O/W emulsion using cellulose as rheological additive bv direct O/W method (CE3)
  • the oil phase was slowly added to the water phase at a rate of 25 g/min.
  • the mixture was mixed at a stirring rate of 300 rpm for 30 minutes thus obtaining a pre-emulsion, which was then introduced in a single-phase homogenizer at a pressure of 300 bar (30 MPa). Subsequently the mixture was cooled, at a rate of 4.0°C per minute, until reaching a temperature of 20-25°C. 1460 g of a creamy emulsion were obtained, having 55 wt.% of active matter.
  • the emulsion was kinetically unstable since it became creamy in the homogenizer.
  • Comparative Example 4 preparation of a soybean O/W emulsion using an acrylic thickener as rheological additive by direct O/W method (CE4)
  • the oil phase was slowly added to the water phase at a rate of 25 g/min.
  • the mixture was mixed at a stirring rate of 300 rpm for 25 minutes thus obtaining a pre-emulsion, which was then introduced in a single-phase homogenizer at a pressure of 300 bar (30 MPa). Subsequently the mixture was cooled, at a rate of 6.0°C per minute, until reaching a temperature of 20-25°C. 966 g of a liquid emulsion were obtained, having a viscosity of 50 cP (25°C, Viscosimeter Brookfield HV, spindle 02, 20 rpm) and 55 wt.% of active matter.
  • the particle size distribution was not gaussian with a Sauter diameter of 6.34 pm, measured by laser diffraction in a Mastersizer 300 equipment.
  • the emulsion was kinetically stable for less than 24 hours, at normal pressure and temperature conditions. O/W emulsion with low
  • the oil phase was slowly added to the water phase at a rate of 23 g/min.
  • the mixture was mixed at a stirring rate of 300 rpm thus for 22 minutes obtaining a pre-emulsion, which was then introduced in a singlephase homogenizer at a pressure of 300 bar (30 MPa). Subsequently the mixture was cooled, at a rate of 6.0°C per minute, until reaching a temperature of 20-25°C. 659 g of a liquid emulsion were obtained, having a viscosity of 18 cP (25°C, Viscosimeter Brookfield HV, spindle 02, 20 rpm) and 32 wt.% of active matter.
  • the particle size distribution was gaussian with a Sauter diameter of 0.59 pm, measured by laser diffraction in a Mastersizer 300 equipment.
  • the emulsion was kinetically stable for less than 24 hours, at normal pressure and temperature conditions.
  • a basic phenolic resin (FORESA RES 3169) was adjusted to a temperature of 20 °C ⁇ 1 °C and diluted until a 20 wt.% solid content. Then, 20 parts, on a dry basis, of the vegetable oil-based emulsion were added to the diluted resin solution and the mixture was stirred for 1 min with a magnetic stirring bar. Subsequently, the mixture was transferred to a test-tube of 100 ml and visually observed to determine if there was phase separation. If so, the separation percentage volume after 1 h, 24 h and 48 h was measured. There was also visually observed if the emulsion was broken down, i.e. , if small particles could be distinguished.
  • formulations according to the invention are compatible with phenolic resins conventionally used in the manufacture of insulation products.
  • molds were manufactured weighting 100 g of fiberglass, adding 6 g of a binder agent and, in the manufacture of mold (A), adding 2 g of the vegetable-oil based formulation of the invention. Mixing these ingredients and heating at 220°C for 5 minutes.
  • the thermal insulation product according to the invention is a more compacted piece, without dust in the surface thereof.
  • the anti-dust effect can also be appreciated by touch, since mold A (according to the invention) does not release dust and, therefore, it does not scratch when touched, whereas mold A (without the formulation of the invention) does.

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Abstract

L'invention concerne une formulation à base d'huile végétale qui est une émulsion huile dans l'eau (O/W) comprenant au moins une huile végétale raffinée ayant un point d'éclair supérieur à 260 °C ; au moins un tensioactif anionique, au moins un tensioactif non ionique ou une combinaison de ceux-ci ; au moins un additif rhéologique qui est un polysaccharide ionique ; et de l'eau ; la formulation ayant une teneur en matière active d'environ 31% en poids et d'environ 69% en poids et le reste de la formulation, jusqu'à atteindre 100% en poids, étant de l'eau ; et la viscosité de la formulation étant d'environ 100 cP à environ 1500 cP (25 °C, viscosimètre Brookfield HV, 20 tr/min). L'invention concerne également un procédé de fabrication de ladite formulation et ses utilisations.
PCT/EP2024/085784 2023-12-13 2024-12-11 Formulations huile dans l'eau à base d'huile végétale Pending WO2025125377A1 (fr)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3861895A (en) 1971-04-13 1975-01-21 Withrow Arthur C Co Method for reducing smoke and dust in the process for manufacturing mineral wool
WO1995006013A1 (fr) 1993-08-25 1995-03-02 Rockwool Aktiebolaget Procede de liaison de la poussiere de laine minerale
WO2009046521A1 (fr) 2007-10-10 2009-04-16 Walker Industries Holdings Limited Formulation et procédé de lutte contre la poussière d'une isolation en fibre
CN103651380A (zh) * 2012-09-14 2014-03-26 青岛星牌作物科学有限公司 一种唑虫酰胺增效悬浮剂及其制备方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3861895A (en) 1971-04-13 1975-01-21 Withrow Arthur C Co Method for reducing smoke and dust in the process for manufacturing mineral wool
WO1995006013A1 (fr) 1993-08-25 1995-03-02 Rockwool Aktiebolaget Procede de liaison de la poussiere de laine minerale
WO2009046521A1 (fr) 2007-10-10 2009-04-16 Walker Industries Holdings Limited Formulation et procédé de lutte contre la poussière d'une isolation en fibre
US20100279573A1 (en) * 2007-10-10 2010-11-04 Laurence Sinnige Formulation and method for dust control of fibre insulation
CN103651380A (zh) * 2012-09-14 2014-03-26 青岛星牌作物科学有限公司 一种唑虫酰胺增效悬浮剂及其制备方法

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
no. 11138-66-2
SAID GHARBI, THE SCIENTIFIC WORLD JOURNAL, vol. 2022, no. 6627013, 2022

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