Silicone emulsions

By using a combination of polar additives and liquid crystal surfactants in silicone emulsions, the stability problem of silicone oil emulsions is solved, and the smaller droplet size and better fluidity are achieved, which expands the application range of silicone oil emulsions.

CN119301181APending Publication Date: 2025-01-10BASF SE
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Patent Information

Application Number
CN202380043978.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Priority Date
2022-05-31
Filing Date
2023-05-09
Publication Date
2025-01-10

AI Technical Summary

Technical Problem

The prior art is difficult to effectively stabilize the silicone oil emulsion, resulting in droplet coalescence or emulsion, limiting the application range and stability of the silicone oil emulsion.

Method used

By using a combination of polar additives and surfactants in the form of liquid crystals in silicone emulsions, the effective filling parameters of the surfactants are changed to form a liquid crystal structure to stabilize the silicone oil emulsions, reduce interfacial tension and improve rheological characteristics.

Benefits of technology

The surfactant species for stabilizing silicone oil emulsions are expanded to achieve silicone oil emulsions with smaller droplet sizes and better fluidity, providing resistance to particle settlement and emulsion, allowing flow under high pressure conditions.

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Abstract

Silicone emulsions, methods of making silicone emulsions, and methods of using silicone emulsions are described herein. The silicone emulsion is stabilized by a combination of a polar additive and a surfactant in liquid crystal form. The silicone emulsions can be used in a variety of industrial applications.
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Description

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS

[0002] This application claims priority to U.S. Provisional Application No. 63 / 365,513, filed on May 31, 2022, which is hereby incorporated by reference herein. Technical Field

[0003] The present disclosure relates to silicone emulsions, methods of making silicone emulsions, and methods of using silicone emulsions. Silicone emulsions are stabilized by a combination of polar additives and surfactants in liquid crystal form. Silicone emulsions can be used in a variety of industrial applications. Background Art

[0004] Silicone oil is a wide range of fluids, including linear chains of poly (dimethylsiloxane) with different degrees of polymerization and viscosities. Depending on the degree of polymerization, the viscosity can range from 0.65-1,000,000s cSt. For ease of use in fields including sealants, coatings and defoamers, silicone oil is emulsified into an aqueous dispersion with micron-sized droplets and a reduced viscosity. Aqueous silicone emulsions require stabilizers, such as surfactants, polymers or solid particles, to prevent silicone oil droplets from coalescing and emulsifying to maintain uniform dispersion of particle size and droplets throughout the emulsion. Conventional silicone oil emulsions are therefore composed of an aqueous phase, a silicone oil phase and a stabilizer.

[0005] While many surfactants can disperse silicone oil into a continuous aqueous phase, not all surfactants can maintain the required stability. Surfactants reduce the interfacial tension between the silicone oil and the aqueous phase in silicone emulsions, thereby helping to reduce droplet size. During the catastrophe inversion process used to produce oil-in-water (o / w) emulsions, some surfactants also produce lyotropic liquid crystals in the aqueous phase as water is gradually added to the surfactant-silicone oil mixture. The highly viscous structure of the lyotropic liquid crystals reduces the viscosity ratio between the aqueous phase and the silicone oil, enabling better transfer of stresses toward deformation of the silicone oil droplets and resulting in rupture. This liquid crystal phase is typically formed at high surfactant concentrations (usually over 40% surfactant in water), so it is a temporary structure that exists during catastrophe inversion and, depending on the surfactant, may disappear after all the water has been added.

[0006] Although the presence of surfactants and an intermediate liquid crystal phase during the mutation inversion is necessary to achieve small droplet sizes, these silicone oil emulsions may or may not remain stable. Some silicone oil emulsions coalesce and undergo bulk phase separation. Other silicone oil emulsions may be stable to coalescence but undergo creaming. It is hypothesized that this difference arises from the fact that at the final surfactant concentration (less than about 20% surfactant in water), some surfactants continue to exist in liquid crystal form, while other surfactants form micelles. Liquid crystals are known to provide three mechanisms that contribute to emulsion stability: 1) a protective sticky skin at the oil-water interface, 2) a three-dimensional network that reduces droplet mobility, and 3) steric repulsion. Therefore, the ability to formulate liquid crystals at the final concentration is necessary to achieve stable silicone oil emulsions.

[0007] According to the critical packing parameter of the surfactant, the cross-sectional area ratio between the head group and the tail determines the structure formed. Surfactants with a much larger head relative to the tail tend to form spherical micelles, while surfactants with roughly equal areas of the head and tail tend to form lamellar structures. Compared with surfactants that tend to form spherical micelles, surfactants that tend to form lamellar structures also tend to form liquid crystals at lower surfactant concentrations. However, this natural limitation often hinders the use of surfactants that tend to form spherical micelles, and therefore limits the number and type of surfactants that can be used to stabilize silicone oil emulsions.

[0008] Therefore, the present application seeks to expand the available surfactants that form liquid crystals for stabilizing silicone oil emulsions.

[0009] Silicone emulsions, methods of making silicone emulsions, and methods of using silicone emulsions are described herein.Silicone emulsions are stabilized by a combination of polar additives and surfactants in liquid crystal form. Summary of the invention

[0010] In one aspect, provided herein is an emulsion comprising: silicone oil; and liquid crystal, the liquid crystal comprising: an aqueous solvent; a polar additive; and a surfactant; wherein the surfactant is present in an amount less than about 20 wt. % of the emulsion.

[0011] On the other hand, the present invention provides a method for making an emulsion, the emulsion comprising: silicone oil; and liquid crystal, the liquid crystal comprising: an aqueous solvent; a polar additive; and a surfactant; wherein the surfactant is present in an amount less than about 20 wt.% of the emulsion, the method comprising: (i) forming a mixture, the mixture comprising: a first amount of the aqueous solvent; optionally a first amount of the silicone oil; the polar additive; and the surfactant, wherein the surfactant is optionally in the form of a liquid crystal; (ii) mixing the mixture; (iii) optionally adding a second amount of the silicone oil; and (iv) optionally adding a second amount of the aqueous solvent.

[0012] In yet another aspect, provided herein is a method of using an emulsion comprising: silicone oil; and a liquid crystal, the liquid crystal comprising: an aqueous solvent; a polar additive; and a surfactant; wherein the surfactant is present in an amount less than about 20 wt.% of the emulsion, the method comprising using the emulsion to form a product selected from the group consisting of a sealant composition, a coating composition, an adhesive composition, an elastomeric composition, a release agent composition, a texture enhancing composition, a lubricant composition, a defoaming composition, a gloss providing composition, a construction composition, a building material composition, a clay composition, a concrete composition, a concrete composition for improving water repellency, and a personal care composition. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Figure 1 is a photograph of an exemplary embodiment of the present disclosure depicting silicone emulsions containing different amounts of silicone oil, surfactant, and polar additive.

[0014] Figure 2 is a photograph of an exemplary embodiment of the present disclosure depicting silicone emulsions containing different amounts of silicone oil, surfactant, and polar additive.

[0015] Figure 3 is a photograph of an exemplary embodiment of the present disclosure depicting a silicone emulsion including a polar additive to address creaming issues.

[0016] Figure 4A is a 40x microscope image of a silicone oil emulsion containing 12,500 cSt silicone oil according to an exemplary embodiment of the present disclosure.

[0017] Figure 4B is a photograph of an exemplary embodiment according to the present disclosure, depicting a silicone oil emulsion containing 12,500 cSt silicone oil.

[0018] Figure 5A is a 40x microscope image of a silicone oil emulsion containing 1,000,000 cSt silicone oil according to an exemplary embodiment of the present disclosure.

[0019] Figure 5B is a photograph of an exemplary embodiment according to the present disclosure, depicting a silicone oil emulsion containing 1,000,000 cSt silicone oil.

[0020] Figure 6 is a photograph of an exemplary embodiment of the present disclosure depicting silicone emulsions containing different amounts of silicone oil, surfactant, and polar additive.

[0021] Fig. 7A is a 40x microscope image of a silicone oil emulsion containing 1,000,000 cSt silicone oil according to an exemplary embodiment of the present disclosure.

[0022] Figure 7B is a photograph of an exemplary embodiment according to the present disclosure, depicting a silicone oil emulsion containing 1,000,000 cSt silicone oil.

[0023] 8 is a photograph depicting silicone emulsions containing different amounts of silicone oil, surfactant, and polar additive according to an exemplary embodiment of the present disclosure.

[0024] 9 is a photograph depicting silicone emulsions containing different amounts of silicone oil, surfactant, stabilizer, and polar additive, according to an exemplary embodiment of the present disclosure. DETAILED DESCRIPTION

[0025] The present disclosure relates to silicone emulsions, methods of making silicone emulsions, and methods of using silicone emulsions. The silicone emulsions include silicone oil; and liquid crystals, the liquid crystals including: an aqueous solvent; a polar additive; and a surfactant. The surfactant is present in the emulsion in an amount less than about 20 wt.% of the emulsion.

[0026] The present application seeks to expand the available surfactants that form liquid crystals in order to stabilize silicone oil emulsions. In the absence of additional components, the surfactants demonstrated do not produce liquid crystals at the final surfactant concentration. On the contrary, this goal is achieved with polar additives (such as polar oils or alcohols), which change the effective filling parameters of the surfactant. When these additives are gradually introduced into the surfactant-water solution that forms micellar solutions, the micellar structure becomes liquid crystal. This produces a significant viscosity difference, and provides yield stress and shear-thinning behavior that are conducive to resisting particle sedimentation and emulsification for the solution. When observing the sample under crossed polarized light, birefringence can also be observed.

[0027] The present application provides several advantages. First, the use of additives to produce liquid crystals expands the number of surfactants that can be used to make stable silicone oil emulsions. New classes of surfactants can be explored in this way. Second, these additives can contribute to a further reduction in interfacial tension, resulting in smaller droplet sizes when undergoing a sudden reversal. Third, these additives can provide more favorable rheological characteristics for the fluid. The yield point provides good stability at rest, and the shear-thinning behavior allows flow in the absence of high pressure. Fourth, these additives can be added at multiple stages of the method (including at the beginning) or as post-emulsification additives.

[0028] Typically, the emulsion can be in the form of any suitable emulsion form known in the art. In some embodiments, the emulsion is an oil-in-water emulsion or a water-in-oil emulsion. In some embodiments, the emulsion is an oil-in-water emulsion.

[0029] In many embodiments, the surfactant can be any suitable surfactant known in the art. In some embodiments, the surfactant is selected from the group consisting of ionic surfactants, cationic surfactants, anionic surfactants, amphoteric surfactants, zwitterionic surfactants, nonionic surfactants, alcohol ethoxylates, alcohol alkoxylates, alkyl polyglycosides, alkyl polyglucosides, extended surfactants, surfactants containing an intermediate propoxylate group between the head group and the tail, and combinations thereof. Examples of suitable surfactants include alcohol ethoxylates, such as XL79 and / or TO8; alkyl polyglucosides, such as 625; or an extending surfactant, such as S8310.

[0030] In many embodiments, the surfactant can be present in the emulsion in any suitable amount known in the art. Typically, the surfactant is present in an amount less than the amount required to form liquid crystals in the absence of the polar additive.

[0031] In some embodiments, the surfactant is present in an amount less than or equal to about 20 wt.%, about 19 wt.%, about 18 wt.%, about 17 wt.%, about 16 wt.%, about 15 wt.%, about 14 wt.%, about 13 wt.%, about 12 wt.%, about 11 wt.%, about 10 wt.%, about 9 wt.%, about 8 wt.%, about 7 wt.%, about 6 wt.%, about 5 wt.%, about 4 wt.%, about 3 wt.%, about 2 wt.%, or about 1 wt.% of the emulsion. In some embodiments, the surfactant is present in an amount greater than or equal to about 0.1 wt.%, about 1 wt.%, about 2 wt.%, about 3 wt.%, about 4 wt.%, about 5 wt.%, about 6 wt.%, about 7 wt.%, about 8 wt.%, about 9 wt.%, about 10 wt.%, about 11 wt.%, about 12 wt.%, about 13 wt.%, about 14 wt.%, about 15 wt.%, about 16 wt.%, about 17 wt.%, about 18 wt.%, or about 19 wt.% of the emulsion.

[0032] In some embodiments, the surfactant comprises a surfactant that is not originally in the form of a liquid crystal when present in an amount less than about 20 wt.% of the emulsion in the absence of a polar additive. In some embodiments, the surfactant comprises a surfactant that is originally in the form of a micellar structure, a spherical structure, a rod-like structure, a worm-like micellar structure, or a combination thereof when present in an amount less than about 20 wt.% of the emulsion in the absence of a polar additive.

[0033] In many embodiments, the liquid crystal can be selected from any type of suitable liquid crystal known in the art. In some embodiments, the liquid crystal is a lyotropic liquid crystal.

[0034] In many embodiments, the polar additive can be any suitable polar additive known in the art. In some embodiments, the polar additive is selected from the group consisting of polar oils, alcohols, surfactants, polar surfactants, and combinations thereof. Examples of suitable polar additives include fatty alcohols, such as C10; polar oils, such as AE 3-2EH; and polar surfactants such as EVM 70 / 2E.

[0035] In many embodiments, the polar additive can be any suitable polar additive known in the art. In certain embodiments, the polar additive can be any suitable polar oil known in the art. Polar oils are usually slightly soluble in water and do not include alkanes. In certain embodiments, the polar additive is a polar oil selected from the group of: alkyl esters, fatty acids, polar aromatic compounds, and combinations thereof.

[0036] In some embodiments, the polar additive is a surfactant. In some embodiments, the surfactant is selected from the group consisting of ionic surfactants, cationic surfactants, anionic surfactants, amphoteric surfactants, zwitterionic surfactants, nonionic surfactants, alcohol ethoxylates, alcohol alkoxylates, alkyl polyglycosides, alkyl polyglucosides, extended surfactants, surfactants comprising an intermediate propoxylate group between the head group and the tail, and combinations thereof.

[0037] In many embodiments, the polar additive can be present in the emulsion in any suitable amount known in the art. In some embodiments, the polar additive is present in an amount less than or equal to about 20 wt.%, about 19 wt.%, about 18 wt.%, about 17 wt.%, about 16 wt.%, about 15 wt.%, about 14 wt.%, about 13 wt.%, about 12 wt.%, about 11 wt.%, about 10 wt.%, about 9 wt.%, about 8 wt.%, about 7 wt.%, about 6 wt.%, about 5 wt.%, about 4 wt.%, about 3 wt.%, about 2 wt.%, or about 1 wt.% of the emulsion. In some embodiments, the polar additive is present in an amount greater than or equal to about 0.1 wt.%, about 1 wt.%, about 2 wt.%, about 3 wt.%, about 4 wt.%, about 5 wt.%, about 6 wt.%, about 7 wt.%, about 8 wt.%, about 9 wt.%, about 10 wt.%, about 11 wt.%, about 12 wt.%, about 13 wt.%, about 14 wt.%, about 15 wt.%, about 16 wt.%, about 17 wt.%, about 18 wt.%, or about 19 wt.% of the emulsion.

[0038] In many embodiments, the polar additive can be present in the emulsion in any suitable amount relative to the amount of surfactant known in the art. In some embodiments, the polar additive is present in a weight fraction (wt. fraction) relative to the surfactant of less than or equal to about 5.0, about 4.5, about 4.0, about 3.5, about 3.0, about 2.5, about 2.0, about 1.5, about 1.0, about 0.95, about 0.90, about 0.85, about 0.80, about 0.75, about 0.70, about 0.65, about 0.60, about 0.55, about 0.50, about 0.45, about 0.40, about 0.35, about 0.30, about 0.25, about 0.20, about 0.15, about 0.10, or about 0.05. In some embodiments, the polar additive is present at a wt. fraction relative to the surfactant of greater than or equal to about 0.05, about 0.10, about 0.15, about 0.20, about 0.25, about 0.30, about 0.35, about 0.40, about 0.45, about 0.50, about 0.55, about 0.60, about 0.65, about 0.70, about 0.75, about 0.80, about 0.85, about 0.90, about 0.95, about 1.0, about 1.5, about 2.0, about 2.5, about 3.0, about 3.5, about 4.0, about 4.5, or about 5.0.

[0039] In some embodiments, the polar additive is present at a weight fraction (wt. fraction) relative to the surfactant of less than or equal to about 0.50, about 0.45, about 0.40, about 0.35, about 0.30, about 0.25, about 0.20, about 0.15, about 0.10, or about 0.05. In some embodiments, the polar additive is present at a wt. fraction relative to the surfactant of greater than or equal to about 0.05, about 0.10, about 0.15, about 0.20, about 0.25, about 0.30, about 0.35, about 0.40, about 0.45, or about 0.50.

[0040] In many embodiments, the aqueous solvent can be any suitable aqueous solvent known in the art. In some embodiments, the aqueous solvent comprises water. In some embodiments, the aqueous solvent comprises deionized water. In some embodiments, the aqueous solvent is substantially free of salt.

[0041] In some embodiments, the aqueous solvent comprises a salt. When the emulsion comprises an anionic surfactant, the presence of the salt is particularly beneficial. When the emulsion comprises a cationic surfactant, the presence of the salt is also particularly beneficial. These salts can be inorganic or organic salts. Examples of suitable salts include those containing cations (such as Na + and Ca 2+ ) and anions (such as Cl - Br - 、CO3 2-or salicylate).

[0042] In many embodiments, the silicone oil can be any suitable silicone oil known in the art. In some embodiments, the silicone oil is from the category of silicone oil selected from the group consisting of epoxy silicone oil, mercapto silicone oil, phenyl silicone oil, reactive silicone oil, and combinations thereof. In some embodiments, the silicone oil is selected from the group consisting of polydimethylsiloxane, organically modified silicone, amino-modified silicone, methyl silicone resin, MQ resin, and combinations thereof.

[0043] In some embodiments, the silicone oil has a viscosity in a range of about 0.65 cSt to about 1,500,000 cSt. In some embodiments, the silicone oil has a viscosity in a range of about 0.65 cSt to about 1,000,000 cSt.

[0044] In many embodiments, the emulsified silicone oil droplets can have any suitable size known in the art. In some embodiments, the emulsified silicone oil droplets include size dimensions in the order of microns. In some embodiments, the emulsified silicone oil droplets have a diameter in the range of about 0.5 microns to about 100 microns. In some embodiments, the emulsified silicone oil droplets have a diameter in the range of about 0.5 microns to about 10 microns.

[0045] In many embodiments, the emulsion may further comprise any suitable emulsion component known in the art. In some embodiments, the emulsion comprises a stabilizer selected from the group consisting of surfactants, polymers, solid particles, surface active proteins, fibers, clays, temperature stabilizers, and combinations thereof. In some embodiments, the stabilizer comprises an alkoxylated polymer. In some embodiments, the stabilizer comprises an alkoxylated block copolymer. In some embodiments, the stabilizer comprises an ethoxylated / propoxylated (EO / PO) block copolymer. In some embodiments, the stabilizer comprises P105.

[0046] In many embodiments, the emulsion is storage stable. In some embodiments, the emulsion is storage stable for at least one month. In some embodiments, the emulsion is storage stable at elevated temperatures. In some embodiments, the emulsion is storage stable at temperatures up to about 80° C. Storage at elevated temperatures is particularly useful when the emulsion comprises a temperature-insensitive surfactant or a temperature-insensitive surfactant blend.

[0047] In general, the emulsion can be made according to any suitable method known in the art. In some embodiments, the emulsion is made according to a method comprising the following steps: (i) forming a mixture comprising an optionally first amount of an aqueous solvent; optionally a first amount of a silicone oil; a polar additive; and a surfactant, wherein the surfactant is optionally in the form of a liquid crystal; (ii) mixing the mixture; (iii) optionally adding a second amount of the silicone oil; and (iv) optionally adding a second amount of the aqueous solvent.

[0048] In many embodiments, the polar additive can be added at any stage of the method. In some embodiments, the polar additive is added to the surfactant to form a blend. The blend can be added to the silicone oil or the silicone oil can be added to the blend. In some embodiments, the polar additive is added to a mixture comprising an aqueous solvent and a surfactant. In some embodiments, the polar additive is added to a mixture comprising silicone oil and a surfactant.

[0049] In some embodiments, the method steps of forming a mixture include (i) forming a first mixture comprising, optionally, a first amount of an aqueous solvent, a silicone oil, and a surfactant; and (ii) adding a polar additive to the first mixture to form a second mixture.

[0050] In some embodiments, the emulsion is made according to a method comprising the steps of: (i) forming a first mixture comprising a first amount of an aqueous solvent, a silicone oil, and a surfactant; (ii) mixing the first mixture; and (iii) adding a polar additive to the first mixture to form a second mixture.

[0051] In some embodiments, the method steps of forming a mixture include (i) forming a first mixture comprising, optionally, a first amount of an aqueous solvent, a polar additive, and a surfactant; and (ii) adding the first mixture to silicone oil to form a second mixture.

[0052] In some embodiments, the emulsion is made according to a method comprising the steps of: (i) forming a first mixture comprising, optionally, a first amount of an aqueous solvent, a polar additive, and a surfactant; (ii) adding the first mixture to silicone oil to form a second mixture, (iii) mixing the second mixture, and (iv) adding a second amount of the aqueous solvent.

[0053] In many embodiments, during the method step of forming the mixture, the surfactant can be in any suitable form. In some embodiments, during the method step of forming the mixture, the surfactant is not in the form of a liquid crystal. In some embodiments, during the method step of forming the mixture, the surfactant is in the form of a micellar structure, a spherical structure, a rod-like structure, a worm-like micellar structure, or a combination thereof.

[0054] In many embodiments, the method step of mixing this mixture includes mixing this mixture at a suitable speed. Generally, it is desired that a higher speed produces a smaller droplet size, while it is desired that a lower speed produces a larger droplet size and / or limits the shear rate. In certain embodiments, the method step of mixing this mixture includes mixing this mixture at a speed less than or equal to about 10000rpm. In certain embodiments, the method step of mixing this mixture includes mixing this mixture at a speed less than or equal to about 1000rpm. In certain embodiments, the method step of mixing this mixture includes mixing this mixture at a speed less than or equal to about 300rpm.

[0055] In many embodiments, the method step of mixing the mixture comprises mixing the mixture according to any suitable mixing procedure known in the art. In some embodiments, the method step of mixing the mixture comprises mixing the mixture with a mixer (such as an overhead mixer or a static mixer).

[0056] Typically, the emulsion undergoes mutational reversal during the manufacturing method. In some embodiments, the method step of adding a first amount of an aqueous solvent induces mutational reversal of the emulsion. In some embodiments, the method step of adding a second amount of an aqueous solvent induces mutational reversal of the emulsion. In some embodiments, the method includes the method step of adding a first amount of an aqueous solvent to induce mutational reversal of the emulsion, followed by the method step of adding a second amount of an aqueous solvent after mutational reversal has occurred.

[0057] In some embodiments, the emulsion does not undergo a catastrophe reversal during the manufacturing method. In some embodiments, wherein the emulsion does not undergo a catastrophe reversal during the manufacturing method, the manufacturing method comprises direct emulsification, whereby the desired components of the emulsion are mixed together simultaneously. In some embodiments, wherein the emulsion does not undergo a catastrophe reversal during the manufacturing method, the manufacturing method comprises adding silicone oil after liquid crystal formation.

[0058] In these embodiments, a sudden reversal describes the change of the emulsion from oil continuous to water continuous. In some embodiments, a sudden reversal can be detected by a sharp increase in the conductivity of the fluid. In some embodiments, when oil continuous, the conductivity is less than about 5-10 μS, and the conductivity increases sharply by several orders of magnitude during the reversal to water continuous.

[0059] Generally, a number of compositions can include silicone emulsions according to the present disclosure. These silicone emulsions can also be used in a number of compositions.

[0060] In many embodiments, the composition is a composition that can be used in industrial applications. In some embodiments, the composition is selected from the group consisting of a sealant composition, a coating composition, an adhesive composition, an elastomeric composition, a release agent composition, a texture enhancing composition, a lubricant composition, a defoaming composition, a gloss providing composition, a construction composition, a building material composition, a clay composition, a concrete composition, a concrete composition for improving water repellency, and a personal care composition.

[0061] Further aspects of the disclosure are provided by the subject matter of the following clauses:

[0062] 1. An emulsion comprising:

[0063] Silicone oil; and

[0064] A liquid crystal, the liquid crystal comprising:

[0065] Aqueous solvents;

[0066] Polar additives; and

[0067] Surfactants;

[0068] wherein the surfactant is present in an amount less than about 20 wt. % of the emulsion.

[0069] 2. An emulsion as described in the preceding clause, wherein the surfactant is selected from the group consisting of ionic surfactants, cationic surfactants, anionic surfactants, amphoteric surfactants, zwitterionic surfactants, nonionic surfactants, alcohol ethoxylates, alcohol alkoxylates, alkyl polyglycosides, alkyl polyglucosides, extending surfactants, surfactants comprising an intermediate propoxylate group between the head group and the tail, and combinations thereof.

[0070] 3. The emulsion of any preceding clause, wherein the surfactant is present in an amount less than about 15 wt. % of the emulsion.

[0071] 4. The emulsion of any preceding clause, wherein the surfactant comprises a surfactant that is not originally in liquid crystal form when present in an amount less than about 20 wt. % of the emulsion in the absence of the polar additive.

[0072] 5. An emulsion as described in any preceding clause, wherein the liquid crystal is a lyotropic liquid crystal.

[0073] 6. The emulsion of any preceding clause, wherein the polar additive is selected from the group consisting of polar oils, alcohols, alkyl esters, fatty acids, polar aromatic compounds, surfactants, polar surfactants, and combinations thereof.

[0074] 7. The emulsion of any preceding clause, the polar additive being present in a wt. fraction relative to the surfactant in the range of about 0.25 to about 5.0.

[0075] 8. An emulsion as described in any preceding clause, wherein the aqueous solvent comprises water.

[0076] 9. The emulsion of any preceding clause, wherein the silicone oil is selected from the group consisting of polydimethylsiloxanes, organomodified silicones, amino-modified silicones, methyl silicone resins, MQ resins, and combinations thereof.

[0077] 10. The emulsion of any preceding clause, wherein the silicone oil has a viscosity in the range of about 0.65 cSt to about 1,500,000 cSt.

[0078] 11. The emulsion of any preceding clause, further comprising a stabilizer selected from the group consisting of surfactants, polymers, solid particles, surface active proteins, fibers, clays, temperature stabilizers, and combinations thereof.

[0079] 12. An emulsion as claimed in any preceding clause, wherein the emulsion is an oil-in-water emulsion.

[0080] 13. An emulsion as described in any preceding clause, wherein the composition is selected from the group consisting of a sealant composition, a coating composition, an adhesive composition, an elastomeric composition, a release agent composition, a texture enhancing composition, a lubricant composition, a defoaming composition, a gloss providing composition, a construction composition, a building material composition, a clay composition, a concrete composition, a concrete composition for improving water repellency, and a personal care composition.

[0081] 14. A method for producing an emulsion, the emulsion comprising:

[0082] Silicone oil; and

[0083] A liquid crystal, the liquid crystal comprising:

[0084] Aqueous solvents;

[0085] Polar additives; and

[0086] Surfactants;

[0087] wherein the surfactant is present in an amount less than about 20 wt. % of the emulsion,

[0088] The method includes:

[0089] A mixture is formed, the mixture comprising:

[0090] optionally a first amount of the aqueous solvent;

[0091] optionally a first amount of the silicone oil;

[0092] the polar additive; and

[0093] the surfactant, wherein the surfactant is optionally in the form of a liquid crystal;

[0094] mixing the mixture;

[0095] optionally adding a second amount of the silicone oil; and

[0096] A second amount of the aqueous solvent is optionally added.

[0097] 15. The emulsion of the preceding clause, wherein the method step of forming the mixture comprises:

[0098] forming a first mixture comprising the first amount of the silicone oil and the surfactant; and

[0099] The polar additive is added to the first mixture to form a second mixture.

[0100] 16. An emulsion as described in any preceding clause, wherein the method step of forming the mixture comprises:

[0101] forming a first mixture comprising the first amount of the aqueous solvent, the polar additive, and the surfactant; and

[0102] The first amount of the silicone oil is added to the first mixture to form a second mixture.

[0103] 17. The emulsion of any preceding clause, wherein the method step of mixing the mixture comprises mixing the mixture at a rate of less than or equal to about 300 rpm.

[0104] 18. An emulsion as described in any preceding clause, wherein the method step of adding a second amount of the aqueous solvent induces a catastrophe reversal of the emulsion.

[0105] 19. An emulsion as claimed in any preceding clause, wherein, during the method step of forming the mixture, the surfactant is not in liquid crystal form.

[0106] 20. A method of using an emulsion comprising:

[0107] Silicone oil; and

[0108] A liquid crystal, the liquid crystal comprising:

[0109] Aqueous solvents;

[0110] Polar additives; and

[0111] Surfactants;

[0112] wherein the surfactant is present in an amount less than about 20 wt. % of the emulsion,

[0113] The method comprises using the emulsion to form a product selected from the group consisting of a sealant composition, a coating composition, an adhesive composition, an elastomeric composition, a release agent composition, a texture enhancing composition, a lubricant composition, a defoaming composition, a gloss providing composition, a construction composition, a building material composition, a clay composition, a concrete composition, a concrete composition for improving water repellency, and a personal care composition.

[0114] Examples

[0115] Without further elaboration, it is believed that one skilled in the art can, using the preceding description, utilize the present invention to its fullest extent.Therefore, the following examples should be construed as merely illustrative, and not limiting of the present disclosure in any way.

[0116] Material.

[0117] XL79: Nonionic alkyl polyglycol ether surfactant.

[0118] TO 8: Based on saturated iso-C 13 - Alcohol nonionic surfactant.

[0119] 625UP: Alkyl polyglycoside surfactant.

[0120] C10: 1-Decanol.

[0121] AE 3-2EH: 2-ethylhexyl lactate.

[0122] Aspiro S8310: Anionic spreading surfactant.

[0123] XL70: Nonionic alkyl polyglycol ether surfactant.

[0124] EVM 70 / 2E: linear dodecylbenzenesulfonic acid calcium salt in 2-ethylhexanol / propylene glycol solvent.

[0125] P105: nonionic EO / PO block copolymer, 50% EO.

[0126] Example 1. Silicone emulsions with 8.5 wt.% surfactant and varying amounts of polar additives.

[0127] With water, silicone oil, 8.5wt.% active surfactant ( XL79) and different amounts of polar additives ( C10) to form a silicone emulsion. The emulsion was formed by direct emulsification followed by vortex mixing for two minutes. This process was repeated twice with a four-hour interval between each mixing. The relevant composition is shown in Figure 1 In. Figure 1 In the top image of , a composition comprising water, a surfactant, and a polar additive is shown under normal light. Figure 1 In the middle image of , a composition comprising water, a surfactant and a polar additive is shown under cross-polarized light. Figure 1 In the bottom image of , a composition comprising water, a surfactant, a polar additive, and silicone oil is shown under normal light.

[0128] As from Figure 1 As can be seen in the middle image of , birefringence is readily seen for compositions having at least 2 wt.% of polar additive, indicating that these compositions contain liquid crystals. Figure 1 In the bottom image of , the composition having at least 2 wt. % polar additive is homogeneous, while the composition having less than 2 wt. % polar additive is phase separated.

[0129] Example 2. Silicone emulsions with 5 wt.% surfactant and different weight fractions of polar additives.

[0130] With water, silicone oil and a constant 5 wt.% active surfactant ( XL79) and polar additives ( C10) to form a silicone emulsion. The emulsion was formed by direct emulsification followed by vortex mixing for two minutes. This process was repeated twice with a four-hour interval between each mixing. The relative weight fractions of the polar additives were varied. The relevant compositions are shown in Figure 2 In. Figure 2 In the top image of , a composition comprising water, a surfactant, and a polar additive is shown under normal light. Figure 2 In the middle image of , a composition comprising water, a surfactant and a polar additive is shown under cross-polarized light. Figure 2 In the bottom image of , a composition comprising water, a surfactant, a polar additive, and silicone oil is shown under normal light.

[0131] As from Figure 2 As can be seen in the middle image of , birefringence is readily seen for compositions having at least 0.25 wt. fraction of polar additive, indicating that these compositions contain liquid crystals. Figure 2 In the bottom image of , the composition having at least 0.25 wt. fraction of the polar additive is homogeneous, while the composition having less than 0.25 wt. fraction of the polar additive is phase separated.

[0132] Example 3. Silicone emulsion with polar additive as post-emulsion additive.

[0133] By forming a surfactant containing 10 g ( XL79 or A base formulation of 45 g of TO 8), 45 g of deionized water and 45 g of silicone oil (350 cSt PDMS) formed a comparative silicone emulsion. The comparative silicone emulsion is shown in Figure 3 As can be seen, the comparative emulsion phase separated after one day.

[0134] By adding 5 mL of polar additive ( AE 3-2EH) was added to the comparative silicone emulsion and the resulting mixture was shaken for about one minute to form the silicone emulsion of the present invention. The silicone emulsion of the present invention is shown in Figure 3 As can be seen, the emulsion of the invention remains stable and homogeneous after one month.

[0135] Example 4. Mutation reversal of a silicone emulsion containing 12,500 cSt silicone oil.

[0136] 46.53 wt.% water, 47.19 wt.% silicone oil with a viscosity of 12,500 cSt, 4.38 wt.% active surfactant ( XL79) and 1.24wt.% polar additive ( C10) forming a silicone emulsion. The blend is formed by forming a mixture comprising a surfactant and a polar additive. The blend is added to the silicone oil, and the resulting mixture is then mixed at 250 rpm. Water is then added at a progressive rate of 1 g / min until a sudden change occurs. After the sudden change is reversed, water is further added at a rate of 2 g / min.

[0137] A microscope image of the resulting silicone oil emulsion containing 12,500 cSt silicone oil is shown in Figure 4A The silicone oil droplets are relatively small and evenly dispersed. A photograph of the resulting silicone oil emulsion containing 12,500 cSt silicone oil is shown in Figure 4B Medium. The emulsion is clearly homogeneous.

[0138] Example 5. Mutation reversal of a silicone emulsion containing 1,000,000 cSt silicone oil.

[0139] 46.53 wt.% water, 47.19 wt.% silicone oil with a viscosity of 1,000,000 cSt, 4.38 wt.% active surfactant ( XL79) and 1.24wt.% polar additive ( C10) forms a silicone emulsion. A blend is formed by forming a mixture comprising a surfactant and a polar additive. The blend is added to the silicone oil, and the resulting mixture is then mixed at 60 rpm. Water is then added at a progressive rate of 1 g / min until a sudden change occurs. After the sudden change occurs, the mixture is further mixed at 60-250 rpm. After mixing, water is further added at a rate of 2 g / min.

[0140] A microscope image of the resulting silicone oil emulsion containing 1,000,000 cSt silicone oil is shown in Figure 5A The silicone oil droplets are relatively large and are not uniformly dispersed. A photograph of the resulting silicone oil emulsion containing 1,000,000 cSt silicone oil is shown in Figure 5B Medium. The emulsion is clearly homogeneous.

[0141] Example 6. Silicone emulsions with 5 wt.% surfactant and varying amounts of polar additives.

[0142] Water, silicone oil, 5wt.% active surfactant ( 625UP) and different amounts of polar additives ( C10) to form a silicone emulsion. The emulsion was formed by direct emulsification followed by vortex mixing for two minutes. This process was repeated twice with a four-hour interval between each mixing. The relevant composition is shown in Figure 6 In. Figure 6 In the top image of , a composition comprising water, a surfactant, and a polar additive is shown under normal light. Figure 6 In the middle image of , a composition comprising water, a surfactant and a polar additive is shown under cross-polarized light. Figure 6 In the bottom image of , a composition comprising water, a surfactant, a polar additive, and silicone oil is shown under normal light.

[0143] As from Figure 6 As can be seen in the middle image of , birefringence is seen for the composition with 2 wt.% polar additive, indicating that this composition contains liquid crystals. Figure 6 In the bottom image of , the composition with 2 wt.% polar additive is homogeneous, while the composition with less than 2 wt.% polar additive is phase separated.

[0144] Example 7. Mutation reversal of a silicone emulsion containing 1,000,000 cSt silicone oil.

[0145] Water, silicone oil with a viscosity of 1,000,000 cSt, 5 wt.% active surfactant ( 625UP) and 2wt.% polar additive ( C10) forms a silicone emulsion. A blend is formed by forming a mixture comprising a surfactant and a polar additive. The blend is added to the silicone oil, and the resulting mixture is then mixed at 60 rpm. Water is then added at a progressive rate of 1 g / min until a sudden change occurs. After the sudden change occurs, the mixture is further mixed at 60-250 rpm. After mixing, water is further added at a rate of 2 g / min.

[0146] The microscope image of the resulting silicone oil emulsion containing 1,000,000 cSt silicone oil after dilution 10 times is shown in Fig. 7A The silicone oil droplets are a mixture of relatively small droplets and relatively large droplets dispersed uniformly. A photograph of the resulting silicone oil emulsion containing 1,000,000 cSt silicone oil is shown in Figure 7B Medium. The emulsion is clearly homogeneous.

[0147] These examples demonstrate the benefits of using a combination of surfactants and polar additives to stabilize aqueous silicone emulsions. Liquid crystals are necessary to stabilize the droplets after emulsification. Liquid crystals can be formed from a variety of surfactants. Silicones with a wide range of viscosities can be emulsified.

[0148] Example 8. Silicone emulsions with 4 wt.% surfactant and varying amounts of polar additives.

[0149] With water, silicone oil, 4wt.% active surfactant ( XL70) and different amounts of polar additives ( EVM 70 / 2E) to form a silicone emulsion. The emulsion was formed as described above. The amount of the component that causes the formation of liquid crystals is 4 wt.% XL 70, 4wt.%NANSA 70 / 2E and appropriate amount of water. The amounts of these components are not determined before mixing and required experiments.

[0150] The corresponding compositions are shown in FIG8 . In the top image of FIG8 , the composition comprising water, a surfactant and a polar additive is shown under normal light. In the middle image of FIG8 , the composition comprising water, a surfactant and a polar additive is shown under cross-polarized light. The middle image of FIG8 was taken two weeks later to improve the visualization of the birefringence. In the bottom image of FIG8 , the composition comprising water, a surfactant, a polar additive and silicone oil is shown under normal light.

[0151] In each image of FIG. 8 , the concentration of the polar additive increases from left to right as follows: 0 wt.% in the first vial, 2 wt.% in the second vial, 4 wt.% in the third vial, and 6 wt.% in the fourth vial.

[0152] As can be seen from the middle image of Figure 8, birefringence is seen for the composition with 4 wt.% polar additive, indicating that this composition contains liquid crystals. In the bottom image of Figure 8, the composition with 4 wt.% polar additive is homogeneous, while the composition with less than 4 wt.% polar additive is phase separated.

[0153] use One advantage of EVM 70 / 2E or other polar surfactants as polar additives is that the silicone emulsion is temperature stable.

[0154] Example 9. Silicone emulsions with 4 wt.% surfactant, 3 wt.% stabilizer, and varying amounts of polar additives.

[0155] With water, silicone oil, 4wt.% active surfactant ( XL70), 3wt.% stabilizer ( P105) and different amounts of polar additives ( EVM 70 / 2E) to form a silicone emulsion. The emulsion was formed as described above. The amount of the component that causes the formation of liquid crystals is 4 wt.% XL 70, 8wt.%NANSA 70 / 2E, 3wt.% P105 and appropriate amount of water. The amounts of these components are not determined until mixing and required experiments.

[0156] The corresponding compositions are shown in FIG9 . In the top image of FIG9 , a composition comprising water, a surfactant, a stabilizer, and a polar additive is shown under normal light. In the middle image of FIG9 , a composition comprising water, a surfactant, a stabilizer, and a polar additive is shown under cross-polarized light. The middle image of FIG9 was taken two weeks later to improve the visualization of the birefringence. In the bottom image of FIG9 , a composition comprising water, a surfactant, a stabilizer, a polar additive, and silicone oil is shown under normal light.

[0157] In each image of FIG. 9 , the concentration of the polar additive increases from left to right as follows: 0 wt.% in the first vial, 2 wt.% in the second vial, 4 wt.% in the third vial, 6 wt.% in the fourth vial, 8 wt.% in the fifth vial, and 10 wt.% in the sixth vial.

[0158] As can be seen from the middle image of Figure 9, birefringence is seen for the composition with 8 wt.% polar additive, indicating that this composition contains liquid crystals. In the bottom image of Figure 9, the composition with 8 wt.% polar additive is homogeneous, while the composition with less than 8 wt.% polar additive is phase separated.

[0159] use EVM 70 / 2E or other polar surfactants as polar additives and stabilizers (e.g. One advantage of the combination of P105) is that the silicone emulsion is temperature stable.

[0160] This written description uses examples to illustrate the disclosure, including the best mode, and also to enable any person skilled in the art to practice the disclosure, including making and using any compositions or systems and performing any combined methods. The patentable scope of the disclosure is defined by the claims, and may include other examples that occur to those skilled in the art. Such other embodiments are intended to be within the scope of the claims if they have elements that do not depart from the literal language of the claims, or if they include equivalent elements that do not differ significantly from the literal language of the claims.

[0161] As used herein, the terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," "characterized by," or any other variation thereof, are intended to cover a non-exclusive inclusion, subject to any limitation expressly stated. For example, a composition, mixture, process, or method that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, mixture, process, or method.

[0162] The transitional phrase "consisting of" excludes any unspecified element, step, or ingredient. If in a claim, this phrase will make the claim closed-ended, excluding materials other than those recited, except for impurities normally associated therewith. When the phrase "consisting of" appears in a clause of the body of a claim, rather than immediately following the preamble, the phrase is limited only to the elements set forth in that clause; other elements are not excluded from the claim as a whole.

[0163] The transitional phrase "consisting essentially of is used to define compositions or methods that include materials, steps, features, components, or elements in addition to those literally disclosed, provided that such additional materials, steps, features, components, or elements do not materially affect one or more of the basic and novel characteristics of the claimed invention. The term "consisting essentially of is a middle ground between "comprising" and "consisting of."

[0164] When an invention or a portion thereof is defined using an open-ended term such as "comprising", it should be readily understood that (unless otherwise indicated) the specification should be interpreted as also describing the invention using the term "consisting essentially of" or "consisting of".

[0165] In addition, unless expressly stated to the contrary, "or" refers to an inclusive or rather than an exclusive or. For example, condition A or B is satisfied by any of the following: A is true (or exists) and B is false (or does not exist), A is false (or does not exist) and B is true (or exists), and both A and B are true (or exist).

[0166] In addition, the indefinite articles "a" and "an" before the elements or components of the present invention are intended to have no restriction on the number of instances (i.e., occurrences) of the elements or components. Therefore, "a" and "an" should be interpreted as including one or at least one, and the singular word form of the elements or components also includes the plural, unless the number obviously means the singular.

[0167] As used herein, the term "about" means plus or minus 10% of the value.

Claims

1. An emulsion comprising: Silicone oil; and A liquid crystal, the liquid crystal comprising: Aqueous solvents; Polar additives; and Surfactants; wherein the surfactant is present in an amount less than about 20 wt. % of the emulsion.

2. The emulsion according to claim 1, wherein The surfactant is selected from the group consisting of ionic surfactants, cationic surfactants, anionic surfactants, amphoteric surfactants, zwitterionic surfactants, nonionic surfactants, alcohol ethoxylates, alcohol alkoxylates, alkyl polyglycosides, alkyl polyglucosides, extending surfactants, surfactants comprising an intermediate propoxylate group between the head group and the tail, and combinations thereof.

3. The emulsion according to claim 1, wherein The surfactant is present in an amount less than about 15 wt. % of the emulsion.

4. The emulsion according to claim 1, wherein The surfactant comprises a surfactant that is not originally in liquid crystal form when present in an amount less than about 20 wt. % of the emulsion in the absence of the polar additive.

5. The emulsion according to claim 1, wherein The liquid crystal is a lyotropic liquid crystal.

6. The emulsion according to claim 1, wherein The polar additive is selected from the group consisting of polar oils, alcohols, alkyl esters, fatty acids, polar aromatic compounds, surfactants, polar surfactants, and combinations thereof.

7. The emulsion according to claim 1, wherein The polar additive is present in a wt. fraction relative to the surfactant in the range of about 0.25 to about 5.

0.

8. The emulsion according to claim 1, wherein The aqueous solvent includes water.

9. The emulsion according to claim 1, wherein The silicone oil is selected from the group consisting of polydimethylsiloxane, organic modified silicone, amino modified silicone, methyl silicone resin, MQ resin, and combinations thereof.

10. The emulsion according to claim 1, wherein The silicone oil has a viscosity in the range of about 0.65 cSt to about 1,500,000 cSt.

11. The emulsion of claim 1, further comprising a stabilizer selected from the group consisting of surfactants, polymers, solid particles, surface active proteins, fibers, clays, temperature stabilizers, and combinations thereof.

12. The emulsion according to claim 1, wherein The emulsion is an oil-in-water emulsion.

13. A composition comprising the emulsion according to claim 1, wherein: The composition is selected from the group consisting of a sealant composition, a coating composition, an adhesive composition, an elastomeric composition, a release agent composition, a texture enhancing composition, a lubricant composition, a defoaming composition, a gloss providing composition, a construction composition, a building material composition, a clay composition, a concrete composition, a concrete composition for improving water repellency, and a personal care composition.

14. A method for producing an emulsion, the emulsion comprising: Silicone oil; and A liquid crystal, the liquid crystal comprising: Aqueous solvents; Polar additives; and Surfactants; wherein the surfactant is present in an amount less than about 20 wt. % of the emulsion, The method includes: A mixture is formed, the mixture comprising: optionally a first amount of the aqueous solvent; optionally a first amount of the silicone oil; the polar additive; and the surfactant, wherein the surfactant is optionally in the form of a liquid crystal; mixing the mixture; optionally adding a second amount of the silicone oil; as well as A second amount of the aqueous solvent is optionally added.

15. The method of claim 14, wherein: The method steps of forming the mixture include: forming a first mixture comprising the first amount of the silicone oil and the surfactant; and The polar additive is added to the first mixture to form a second mixture.

16. The method of claim 14, wherein: The method steps of forming the mixture include: forming a first mixture comprising the first amount of the aqueous solvent, the polar additive, and the surfactant; and The first amount of the silicone oil is added to the first mixture to form a second mixture.

17. The method of claim 14, wherein: The method step of mixing the mixture includes mixing the mixture at a rate of less than or equal to about 300 rpm.

18. The method of claim 14, wherein: The method step of adding a second amount of the aqueous solvent induces a catastrophe reversal of the emulsion.

19. The method of claim 14, wherein: During this process step of forming the mixture, the surfactant is not in liquid crystal form.

20. A method of using an emulsion comprising: Silicone oil; and A liquid crystal, the liquid crystal comprising: Aqueous solvents; Polar additives; and Surfactants; wherein the surfactant is present in an amount less than about 20 wt. % of the emulsion, The method comprises using the emulsion to form a product selected from the group consisting of a sealant composition, a coating composition, an adhesive composition, an elastomeric composition, a release agent composition, a texture enhancing composition, a lubricant composition, a defoaming composition, a gloss providing composition, a construction composition, a building material composition, a clay composition, a concrete composition, a concrete composition for improving water repellency, and a personal care composition.