Silicone emulsion

By employing a combination of a polar additive and a surfactant in the form of a liquid crystal in silicone oil emulsions, the stability and rheological properties of these emulsions are enhanced, addressing the limitations of existing surfactants and achieving improved stability and droplet size reduction.

JP2025518166AInactive Publication Date: 2025-06-12BASF SE
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Patent Information

Application Number
JP2024570437
Authority / Receiving Office
JP · JP
Patent Type
Applications
Current Assignee / Owner
Priority Date
2022-05-31
Filing Date
2023-05-09
Publication Date
2025-06-12
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

The existing surfactants used to stabilize silicone oil emulsions are limited in their ability to form liquid crystals at the final surfactant concentration, leading to instability issues such as coalescence and creaming.

Method used

The use of a combination of a polar additive and a surfactant in the form of a liquid crystal, where the surfactant is present in an amount of less than about 20% by weight of the emulsion, to stabilize silicone oil emulsions and enhance their stability and rheological properties.

Benefits of technology

This approach expands the range of surfactants that can be used to produce stable silicone oil emulsions, reduces droplet size, and imparts favorable rheological properties such as yield stress and shear-thinning behavior, which improve stability against sedimentation and creaming.

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Abstract

This specification describes a silicone emulsion, a method for producing a silicone emulsion, and a method for using a silicone emulsion. The silicone emulsion is stabilized by a combination of a polar additive and a surfactant in the form of a liquid crystal. The silicone emulsion is useful in various industrial applications.
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Description

Technical Field

[0001] Cross - Reference to Related Applications This application claims priority from U.S. Provisional Patent Application No. 63 / 365,513, filed on May 31, 2022, which is incorporated herein by reference.

[0002] The present disclosure relates to silicone emulsions, methods of making silicone emulsions, and methods of using silicone emulsions. The silicone emulsions are stabilized by a combination of a polar additive and a surfactant in the form of a liquid crystal. The silicone emulsions are useful in a variety of industrial applications.

Background Art

[0003] Silicone oils are a wide range of fluids that include straight - chains of polydimethylsiloxane with various degrees of polymerization and viscosities. The viscosity can range from 0.65 to 1,000,000 cSt of s depending on the degree of polymerization. To make them more useful in fields such as sealants, coatings, and defoamers, silicone oils are emulsified into aqueous dispersions with micron - sized droplets and a reduced viscosity. Aqueous silicone emulsions require stabilizers such as surfactants, polymers, or solid particles to prevent coalescence and creaming of the silicone oil droplets and to maintain particle size and uniform dispersion of the droplets throughout the emulsion. Therefore, conventional silicone oil emulsions are composed of an aqueous phase, a silicone oil phase, and a stabilizer.

[0004] Although many surfactants can disperse silicone oil in 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 the silicone emulsion, thereby promoting the reduction of droplet size. During the catastrophic phase inversion process to produce an oil-in-water (o / w) emulsion, when water is gradually added to the surfactant-silicone oil mixture, some surfactants also form lyotropic liquid crystals in the aqueous phase. The highly viscous structure of the lyotropic liquid crystals reduces the viscosity ratio between the aqueous phase and the silicone oil, thereby enabling better stress transmission against the deformation of the silicone oil droplets, resulting in destruction. This liquid crystal phase is typically a temporary structure that exists during the catastrophic phase inversion, usually when the surfactant concentration is high (often exceeding 40% surfactant in water), and may disappear after all the water has been added, depending on the surfactant.

[0005] The presence of surfactants and intermediate liquid crystal phases during catastrophic phase inversion is essential to achieve small droplet sizes, but these silicone oil emulsions can be either stable or unstable. Some silicone oil emulsions coalesce to cause bulk phase separation. There are also those that are stable against coalescence but exhibit creaming. This difference is hypothesized to arise from the fact that at the final surfactant concentration (less than about 20% surfactant in water), certain surfactants continue to exist as liquid crystals while another surfactant forms micelles. Liquid crystals are known to provide three mechanisms beneficial to the stability of emulsions: 1) a viscous protective film at the oil-water interface, 2) a three-dimensional network that reduces droplet mobility, and 3) steric repulsion. Therefore, the ability to form liquid crystals at the final concentration is essential to achieve stable silicone oil emulsions.

[0006] According to the critical packing parameter of the surfactant, the structure formed is determined by the ratio between the cross-sectional areas of the head group and the tail. Surfactants with a much larger head compared to the tail tend to form spherical micelles, while surfactants with approximately equal head and tail areas tend to form lamellar structures. Surfactants that tend to form lamellar structures also tend to form liquid crystals at lower surfactant concentrations compared to surfactants that tend to form spherical micelles. However, due to this natural constraint, the use of surfactants that tend to form spherical micelles is often hindered, and as a result, the number and types of surfactants that can be used to stabilize silicone oil emulsions are limited.

Summary of the Invention

Problems to be Solved by the Invention

[0007] Therefore, the present application attempts to expand the available surfactants that form liquid crystals to stabilize silicone oil emulsions.

Means for Solving the Problems

[0008] This specification describes a silicone emulsion, a method for producing a silicone emulsion, and a method for using a silicone emulsion. The silicone emulsion is stabilized by a combination of a polar additive and a surfactant in the form of a liquid crystal.

[0009] In one aspect, this specification provides an emulsion comprising silicone oil and a liquid crystal comprising an aqueous solvent, a polar additive, and a surfactant, wherein the surfactant is present in an amount of less than about 20% by weight of the emulsion.

[0010] In another aspect, provided herein is a method for producing an emulsion comprising silicone oil and a liquid crystal comprising an aqueous solvent, a polar additive, and a surfactant, wherein the surfactant is present in an amount of less than about 20% by weight of the emulsion, the method comprising: (i) forming a mixture comprising a first amount of the aqueous solvent, optionally a first amount of the silicone oil, the polar additive, and optionally a surfactant 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.

[0011] In yet another aspect, provided herein is a method for using an emulsion comprising silicone oil and a liquid crystal comprising an aqueous solvent, a polar additive, and a surfactant, wherein the surfactant is present in an amount of less than about 20% by weight 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 elastomer composition, a release agent composition, a texture enhancing composition, a lubricant composition, an anti-foaming composition, a gloss imparting 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

[0012]

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Mode for Carrying Out the Invention

[0013] The present disclosure relates to silicone emulsions, methods of manufacturing silicone emulsions, and methods of using silicone emulsions. The silicone emulsion includes a silicone oil and a liquid crystal including an aqueous solvent, a polar additive, and a surfactant. The surfactant is present in the emulsion in an amount of less than about 20% by weight of the emulsion.

[0014] This application seeks to expand the available surfactants that form liquid crystals to stabilize silicone oil emulsions. The demonstrated surfactants do not produce liquid crystals at the final surfactant concentration without additional components. Rather, this goal is achieved by polar additives (such as polar oils or alcohols) that change the effective packing parameter of the surfactant. As these additives are gradually introduced into an aqueous surfactant solution that forms a micelle solution, the micelle structure changes to a liquid crystal. This results in a distinct difference in viscosity and gives the solution a yield stress and shear-thinning behavior that are advantageous for resisting particle sedimentation and creaming. When samples are observed under cross-polarized light, birefringence can also be observed.

[0015] This application provides several advantages. First, the use of additives to produce liquid crystals increases the number of surfactants that can be used to produce stable silicone oil emulsions. This approach allows for the exploration of new classes of surfactants. Second, these additives contribute to a further reduction in surface tension, and as a result, the droplet size can be reduced when catastrophic phase inversion occurs. Third, these additives can impart more favorable rheological properties to the fluid. The yield point provides good stability at rest, and the shear-thinning behavior allows for flow without high pressure. Fourth, these additives can be added at multiple stages of the process, such as at the start or as an additive after emulsification.

[0016] Typically, the emulsion can be in 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.

[0017] 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 an ionic surfactant, a cationic surfactant, an anionic surfactant, an amphoteric surfactant, a zwitterionic surfactant, a nonionic surfactant, an alcohol ethoxylate, an alcohol alkoxylate, an alkyl polyglycoside, an alkyl polyglucoside, an extended surfactant, a surfactant containing an intermediate propoxylate group between the head group and the tail, and combinations thereof. Examples of suitable surfactants include alcohol ethoxylates such as Lutensol® XL79 and / or Lutensol® TO8, alkyl polyglucosides such as Glucopon® 625, or extended surfactants such as Aspiro® S8310.

[0018] 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 a liquid crystal in the absence of polar additives.

[0019] In some embodiments, the surfactant is present in an amount of about 20 wt% or less, about 19 wt% or less, about 18 wt% or less, about 17 wt% or less, about 16 wt% or less, about 15 wt% or less, about 14 wt% or less, about 13 wt% or less, about 12 wt% or less, about 11 wt% or less, about 10 wt% or less, about 9 wt% or less, about 8 wt% or less, about 7 wt% or less, about 6 wt% or less, about 5 wt% or less, about 4 wt% or less, about 3 wt% or less, about 2 wt% or less, or about 1 wt% or less of the emulsion. In some embodiments, the surfactant is present in an amount of about 0.1 wt% or more, about 1 wt% or more, about 2 wt% or more, about 3 wt% or more, about 4 wt% or more, about 5 wt% or more, about 6 wt% or more, about 7 wt% or more, about 8 wt% or more, about 9 wt% or more, about 10 wt% or more, about 11 wt% or more, about 12 wt% or more, about 13 wt% or more, about 14 wt% or more, about 15 wt% or more, about 16 wt% or more, about 17 wt% or more, about 18 wt% or more, or about 19 wt% or more of the emulsion.

[0020] In some embodiments, when the surfactant is present in an amount of less than about 20% by weight of the emulsion without a polar additive, it includes a surfactant that is not in the form of a liquid crystal separately. In some embodiments, when the surfactant is present in an amount of less than about 20% by weight of the emulsion without a polar additive, it includes a surfactant in the form of a micelle structure, a spherical structure, a rod-like structure, a string-like micelle structure, or a combination thereof.

[0021] In many embodiments, the liquid crystal can be selected from any suitable type of liquid crystal known in the art. In some embodiments, the liquid crystal is a lyotropic liquid crystal.

[0022] 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 Lorol® C10, polar oils such as Agnique® AE3-2EH, and polar surfactants such as NANSA® EVM70 / 2E.

[0023] In many embodiments, the polar additive can be any suitable polar additive known in the art. In some embodiments, the polar additive can be any suitable polar oil known in the art. Polar oils are usually poorly soluble in water and do not contain alkanes. In some embodiments, the polar additive is a polar oil selected from the group consisting of alkyl esters, fatty acids, polar aromatics, and combinations thereof.

[0024] In some embodiments, the polar additive is a surfactant. In some embodiments, the surfactant is selected from the group consisting of an ionic surfactant, a cationic surfactant, an anionic surfactant, an amphoteric surfactant, a zwitterionic surfactant, a nonionic surfactant, an alcohol ethoxylate, an alcohol alkoxylate, an alkyl polyglycoside, an alkyl polyglucoside, an extended surfactant, a surfactant containing an intermediate propoxylate group between the head group and the tail, and combinations thereof.

[0025] In many embodiments, the polar additive may be present in the emulsion in any suitable amount known in the art. In some embodiments, the polar additive is present in an amount of about 20 wt% or less, about 19 wt% or less, about 18 wt% or less, about 17 wt% or less, about 16 wt% or less, about 15 wt% or less, about 14 wt% or less, about 13 wt% or less, about 12 wt% or less, about 11 wt% or less, about 10 wt% or less, about 9 wt% or less, about 8 wt% or less, about 7 wt% or less, about 6 wt% or less, about 5 wt% or less, about 4 wt% or less, about 3 wt% or less, about 2 wt% or less, or about 1 wt% or less of the emulsion. In some embodiments, the polar additive is present in an amount of about 0.1 wt% or more, about 1 wt% or more, about 2 wt% or more, about 3 wt% or more, about 4 wt% or more, about 5 wt% or more, about 6 wt% or more, about 7 wt% or more, about 8 wt% or more, about 9 wt% or more, about 10 wt% or more, about 11 wt% or more, about 12 wt% or more, about 13 wt% or more, about 14 wt% or more, about 15 wt% or more, about 16 wt% or more, about 17 wt% or more, about 18 wt% or more, or about 19 wt% or more of the emulsion.

[0026] In many embodiments, the polar additive may be present in the emulsion in any suitable amount known in the art relative to the amount of surfactant. In some embodiments, the polar additive is present at a weight fraction (wt. fraction) relative to the surfactant of about 5.0 or less, about 4.5 or less, about 4.0 or less, about 3.5 or less, about 3.0 or less, about 2.5 or less, about 2.0 or less, about 1.5 or less, about 1.0 or less, about 0.95 or less, about 0.90 or less, about 0.85 or less, about 0.80 or less, about 0.75 or less, about 0.70 or less, about 0.65 or less, about 0.60 or less, about 0.55 or less, about 0.50 or less, about 0.45 or less, about 0.40 or less, about 0.35 or less, about 0.30 or less, about 0.25 or less, about 0.20 or less, about 0.15 or less, about 0.10 or less, or about 0.05 or less. In some embodiments, the polar additive is present at a weight fraction relative to the surfactant of about 0.05 or more, about 0.10 or more, about 0.15 or more, about 0.20 or more, about 0.25 or more, about 0.30 or more, about 0.35 or more, about 0.40 or more, about 0.45 or more, about 0.50 or more, about 0.55 or more, about 0.60 or more, about 0.65 or more, about 0.70 or more, about 0.75 or more, about 0.80 or more, about 0.85 or more, about 0.90 or more, about 0.95 or more, about 1.0 or more, about 1.5 or more, about 2.0 or more, about 2.5 or more, about 3.0 or more, about 3.5 or more, about 4.0 or more, about 4.5 or more, or about 5.0 or more.

[0027] In some embodiments, the polar additive is present at a weight fraction (wt. fraction) relative to the surfactant of about 0.50 or less, about 0.45 or less, about 0.40 or less, about 0.35 or less, about 0.30 or less, about 0.25 or less, about 0.20 or less, about 0.15 or less, about 0.10 or less, or about 0.05 or less. In some embodiments, the polar additive is present at a weight fraction relative to the surfactant of about 0.05 or more, about 0.10 or more, about 0.15 or more, about 0.20 or more, about 0.25 or more, about 0.30 or more, about 0.35 or more, about 0.40 or more, about 0.45 or more, or about 0.50 or more.

[0028] In many embodiments, the aqueous solvent can be any suitable aqueous solvent known in the art. In some embodiments, the aqueous solvent includes water. In some embodiments, the aqueous solvent includes deionized water. In some embodiments, the aqueous solvent is substantially salt-free.

[0029] In some embodiments, the aqueous solvent includes salt. The presence of salt is particularly beneficial when the emulsion includes an anionic surfactant. The presence of salt is also particularly beneficial when the emulsion includes a cationic surfactant. The salt can be an inorganic salt or an organic salt. Examples of suitable salts include salts containing combinations of cations such as Na + and Ca 2+ and anions such as Cl - , Br - , CO 3 2- or salicylate.

[0030] In many embodiments, the silicone oil can be any suitable silicone oil known in the art. In some embodiments, the silicone oil is of a classification of silicone oils selected from the group consisting of epoxy, mercapto, phenyl, reactive, 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.

[0031] In some embodiments, the silicone oil has a viscosity in the range of about 0.65 to about 1,500,000 cSt. In some embodiments, the silicone oil has a viscosity in the range of about 0.65 to about 1,000,000 cSt.

[0032] In many embodiments, the emulsified silicone oil droplets can be of any suitable size known in the art. In some embodiments, the emulsified silicone oil droplets have dimensions on the micron order. In some embodiments, the emulsified silicone oil droplets have a diameter in the range of about 0.5 to about 100 micrometers. In some embodiments, the emulsified silicone oil droplets have a diameter in the range of about 0.5 to about 10 micrometers.

[0033] In many embodiments, the emulsion can further include any suitable emulsion components known in the art. In some embodiments, the emulsion includes 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 includes an alkoxylated polymer. In some embodiments, the stabilizer includes an alkoxylated block copolymer. In some embodiments, the stabilizer includes an ethoxylated / propoxylated (EO / PO) block copolymer. In some embodiments, the stabilizer includes Pluronic® P105.

[0034] In many embodiments, the emulsion has storage stability. In some embodiments, the emulsion has storage stability for at least one month. In some embodiments, the emulsion has storage stability at elevated temperatures. In some embodiments, the emulsion has storage stability at temperatures up to about 80°C. Storage at elevated temperatures is particularly useful when the emulsion includes a surfactant that is less affected by temperature or a blend of surfactants that are less affected by temperature.

[0035] Typically, emulsions can be manufactured according to any suitable method known in the art. In some embodiments, the emulsion is manufactured according to a method comprising: (i) optionally forming a mixture comprising a first amount of an aqueous solvent, optionally a first amount of silicone oil, a polar additive, and optionally a surfactant in the form of a liquid crystal; (ii) mixing the mixture; (iii) optionally adding a second amount of silicone oil; and (iv) optionally adding a second amount of an aqueous solvent.

[0036] 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 the aqueous solvent and the surfactant. In some embodiments, the polar additive is added to a mixture comprising the silicone oil and the surfactant.

[0037] In some embodiments, the steps of the method of forming the mixture comprise: (i) optionally forming a first mixture comprising a first amount of an aqueous solvent, silicone oil, and a surfactant; and (ii) adding a polar additive to the first mixture to form a second mixture.

[0038] In some embodiments, the emulsion is manufactured according to a method comprising: (i) forming a first mixture comprising a first amount of an aqueous solvent, 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.

[0039] In some embodiments, the steps of the method of forming the mixture comprise: (i) optionally forming a first mixture comprising 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.

[0040] In some embodiments, the emulsion is produced according to a method that includes: (i) optionally, forming a first mixture that includes 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 an aqueous solvent.

[0041] In many embodiments, the surfactant can be in any suitable form during the steps of the method of forming the mixture. In some embodiments, the surfactant is not in the form of a liquid crystal during the steps of the method of forming the mixture. In some embodiments, the surfactant is in the form of a micelle structure, a spherical structure, a rod-like structure, a string-like micelle structure, or a combination thereof during the steps of the method of forming the mixture.

[0042] In many embodiments, the step of mixing the mixture includes mixing the mixture at a suitable rate. Generally, a higher speed is desirable to produce smaller droplet sizes, while a lower speed is desirable to produce larger droplet sizes and / or limit the shear rate. In some embodiments, the step of mixing the mixture includes mixing the mixture at a speed of about 10,000 rpm or less. In some embodiments, the step of mixing the mixture includes mixing the mixture at a speed of about 1,000 rpm or less. In some embodiments, the step of mixing the mixture includes mixing the mixture at a speed of about 300 rpm or less.

[0043] In many embodiments, the step of mixing the mixture includes mixing the mixture according to any suitable mixing procedure known in the art. In some embodiments, the step of mixing the mixture includes mixing the mixture with a mixer such as an overhead mixer or a static mixer.

[0044] Typically, an emulsion undergoes a catastrophic phase inversion during the manufacturing process. In some embodiments, the step of the method of adding a first amount of an aqueous solvent induces a catastrophic phase inversion of the emulsion. In some embodiments, the step of the method of adding a second amount of an aqueous solvent induces a catastrophic phase inversion of the emulsion. In some embodiments, the method includes the step of the method of adding a first amount of an aqueous solvent to induce a catastrophic phase inversion of the emulsion, followed by the step of the method of adding a second amount of the aqueous solvent after the catastrophic phase inversion has occurred.

[0045] In some embodiments, the emulsion does not undergo a catastrophic phase inversion during the manufacturing process. In some embodiments where the emulsion does not undergo a catastrophic phase inversion during the manufacturing process, the manufacturing method includes direct emulsification, whereby the desired components of the emulsion are mixed together simultaneously. In some embodiments where the emulsion does not undergo a catastrophic phase inversion during the manufacturing process, the manufacturing method includes adding silicone oil after the formation of a liquid crystal.

[0046] In these embodiments, the catastrophic phase inversion represents a change of the emulsion from an oil-continuous type to a water-continuous type. In some embodiments, the catastrophic phase inversion is detectable by a sharp increase in the conductivity of the fluid. In some embodiments, the conductivity is less than about 5-10 μS in the case of the oil-continuous type and increases several orders of magnitude sharply during the phase inversion to the water-continuous type.

[0047] Generally, a number of compositions can include the silicone emulsion according to the present disclosure. The silicone emulsion can also be used in a number of compositions.

[0048] In many embodiments, the composition is a composition useful for industrial applications. In some embodiments, the composition is selected from the group consisting of a sealant composition, a coating composition, an adhesive composition, an elastomer composition, a release agent composition, a texture enhancing composition, a lubricant composition, an antifoaming composition, a gloss imparting 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.

[0049] Further aspects of the present disclosure are provided by the subject matter of the following clauses.

[0050] 1. A silicone oil and a liquid crystal, an aqueous solvent, a polar additive, and a surfactant wherein the liquid crystal contains An emulsion comprising, wherein the surfactant is present in an amount of less than about 20% by weight of the emulsion.

[0051] 2. The emulsion of the preceding clause, wherein the surfactant is selected from the group consisting of an ionic surfactant, a cationic surfactant, an anionic surfactant, an amphoteric surfactant, a zwitterionic surfactant, a nonionic surfactant, an alcohol ethoxylate, an alcohol alkoxylate, an alkyl polyglycoside, an alkyl polyglucoside, an extended surfactant, a surfactant containing an intermediate propoxylate group between the head group and the tail, and combinations thereof.

[0052] 3. The emulsion of any of the preceding clauses, wherein the surfactant is present in an amount of less than about 15% by weight of the emulsion.

[0053] 4. The emulsion of any of the preceding clauses, wherein when the surfactant is present in an amount of less than about 20% by weight of the emulsion without a polar additive, the surfactant is included which is not in the form of a liquid crystal separately.

[0054] 5. The emulsion of any of the preceding clauses, wherein the liquid crystal is a lyotropic liquid crystal.

[0055] 6. The polar additive is an emulsion of any of the preceding clauses selected from the group consisting of polar oils, alcohols, alkyl esters, fatty acids, polar aromatics, surfactants, polar surfactants, and combinations thereof.

[0056] 7. The polar additive is present in a weight fraction relative to the surfactant in the range of about 0.25 to about 5.0 in the emulsion of any of the preceding clauses.

[0057] 8. The aqueous solvent is an emulsion of any of the preceding clauses containing water.

[0058] 9. The silicone oil is an emulsion of any of the preceding clauses selected from the group consisting of polydimethylsiloxane, organically modified silicone, amino-modified silicone, methyl silicone resin, MQ resin, and combinations thereof.

[0059] 10. The silicone oil has a viscosity in the range of about 0.65 to about 1,500,000 cSt in the emulsion of any of the preceding clauses.

[0060] 11. The emulsion of any of the preceding clauses further comprises a stabilizer selected from the group consisting of surfactants, polymers, solid particles, surface-active proteins, fibers, clays, temperature stabilizers, and combinations thereof.

[0061] 12. The emulsion is an oil-in-water emulsion in the emulsion of any of the preceding clauses.

[0062] 13. The composition is an emulsion of any of the preceding clauses selected from the group consisting of sealant compositions, coating compositions, adhesive compositions, elastomer compositions, release agent compositions, texture-improving compositions, lubricant compositions, defoaming compositions, gloss-imparting compositions, construction compositions, building material compositions, clay compositions, concrete compositions, concrete compositions for improving water repellency, and personal care compositions.

[0063] 14. A silicone oil, a liquid crystal, an aqueous solvent, a polar additive, and a surfactant to form an emulsion containing a liquid crystal and wherein the surfactant is present in an amount of less than about 20% by weight of the emulsion, the method for producing an emulsion comprising: optionally, a first amount of an aqueous solvent, and optionally, a first amount of a silicone oil, and a polar additive, and optionally, a surfactant in the form of a liquid crystal to form a mixture; mixing the mixture; optionally, adding a second amount of a silicone oil; and optionally, adding a second amount of an aqueous solvent comprising.

[0064] 15. The steps of the method for forming a mixture include: forming a first mixture comprising a first amount of a silicone oil and a surfactant; adding a polar additive to the first mixture to form a second mixture and an emulsion according to the preceding clause.

[0065] 16. The steps of the method for forming a mixture include: forming a first mixture comprising a first amount of an aqueous solvent, a polar additive, and a surfactant; adding a first amount of a silicone oil to the first mixture to form a second mixture and an emulsion according to any of the preceding clauses.

[0066] 17. The steps of the method for mixing a mixture include mixing the mixture at a speed of about 300 rpm or less, and an emulsion according to any of the preceding clauses.

[0067] 18. An emulsion of any preceding clause, wherein the method step of adding a second amount of aqueous solvent induces a catastrophic phase inversion of the emulsion.

[0068] 19. An emulsion of any of the preceding clauses, wherein the surfactant is not in the form of a liquid crystal during the process step of forming the mixture.

[0069] 20. Silicone oil, A liquid crystal, Aqueous solvents, Polar additives, and Liquid crystal containing surfactant wherein the surfactant is present in an amount of less than about 20% by weight of the emulsion. A method of using the emulsion comprising using the emulsion to form a product selected from the group of a sealant composition, a coating composition, an adhesive composition, an elastomeric composition, a release agent composition, a texturing composition, a lubricant composition, an antifoam composition, a gloss imparting 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. EXAMPLES

[0070] Without further elaboration, it is believed that one skilled in the art using the preceding description can utilize the present invention to its fullest extent. Accordingly, the following examples are to be construed as merely illustrative and not limiting of the present disclosure in any way.

[0071] material Lutensol® XL79: A nonionic alkyl polyethylene glycol ether surfactant. Lutensol® TO8: Saturated iso-C 13 -Non-ionic surfactants based on alcohol. Glucopon® 625UP: Alkyl polyglycoside surfactant. Lorol® C10: 1-Decanol. Agnique® AE3-2EH: 2-Ethylhexyl lactate. Aspiro S8310: Anionic extended surfactant. Lutensol® XL70: Nonionic alkyl polyethylene glycol ether surfactant. NANSA® EVM70 / 2E: Calcium linear dodecylbenzene sulfonate in 2-ethylhexanol / propylene glycol solvent. Pluronic® P105: Nonionic EO / PO block copolymer, 50% EO.

[0072] Example 1. A silicone emulsion containing 8.5 wt% surfactant and various amounts of polar additives. A silicone emulsion was formed using water, silicone oil, 8.5 wt% active surfactant (Lutensol® XL79), and different amounts of polar additive (Lorol® C10). The emulsion was formed by direct emulsification and then vortex mixed for 2 minutes. This process was carried out twice with a 4-hour interval between each mixing. The related compositions are shown in Figure 1. In the upper image of Figure 1, the composition containing water, surfactant, and polar additive is shown under normal light. In the middle image of Figure 1, the composition containing water, surfactant, and polar additive is shown under cross-polarized light. In the lower image of Figure 1, the composition containing water, surfactant, polar additive, and silicone oil is shown under normal light.

[0073] As seen in the middle image of Figure 1, the birefringence of the compositions containing at least 2 wt% polar additive is readily visible, suggesting that these compositions contain liquid crystals. In the lower image of Figure 1, the compositions containing at least 2 wt% polar additive are homogeneous, while the compositions containing less than 2 wt% polar additive are phase-separated.

[0074] Example 2. A silicone emulsion containing 5 wt% surfactant and various weight fractions of polar additives. A silicone emulsion was formed using water, silicone oil, a certain amount of 5 wt% active surfactant (Lutensol® XL79), and a polar additive (Lorol® C10). The emulsion was formed by direct emulsification and then vortex mixed for 2 minutes. This process was carried out twice with a 4-hour interval between each mixing. The relative weight fraction of the polar additive was varied. The related compositions are shown in Figure 2. In the upper image of Figure 2, the composition containing water, surfactant, and polar additive is shown under normal light. In the middle image of Figure 2, the composition containing water, surfactant, and polar additive is shown under cross-polarized light. In the lower image of Figure 2, the composition containing water, surfactant, polar additive, and silicone oil is shown under normal light.

[0075] As seen in the middle image of Figure 2, the birefringence of the composition containing at least 0.25 weight fraction of the polar additive is readily visible, suggesting that these compositions contain liquid crystals. In the lower image of Figure 2, the composition containing at least 0.25 weight fraction of the polar additive is homogeneous, while the composition containing less than 0.25 weight fraction of the polar additive is phase-separated.

[0076] Example 3. Polar Additive of Silicone Emulsion as an Additive after Emulsification. The comparative silicone emulsion was formed by forming a base formulation containing 10 g of surfactant (Lutensol® XL79 or Lutensol® TO8), 45 g of deionized water, and 45 g of silicone oil (350 cSt PDMS). The comparative silicone emulsion is shown in the left image of Figure 3. As can be seen, the comparative emulsion phase-separates after 1 day.

[0077] The silicone emulsion of the present invention was formed by adding 5 mL of a polar additive (Agnique® AE3-2EH) to a comparative silicone emulsion and shaking the resulting mixture for about 1 minute. The silicone emulsion of the present invention is shown in the image on the right side of Figure 3. As can be seen, the emulsion of the present invention remains stable and uniform even after one month.

[0078] Example 4. Catastrophic phase inversion of a silicone emulsion containing 12,500 cSt silicone oil. A silicone emulsion was formed using 46.53 wt% water, 47.19 wt% silicone oil with a viscosity of 12,500 cSt, 4.38 wt% active surfactant (Lutensol® XL79), and 1.24 wt% polar additive (Lorol® C10). A blend was formed by creating a mixture containing the surfactant and the polar additive. This blend was added to the silicone oil, and then the resulting mixture was mixed at 250 rpm. Subsequently, water was gradually added at a rate of 1 g / min until catastrophic phase inversion occurred. After catastrophic phase inversion, water was further added at a rate of 2 g / min.

[0079] A microscopic 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 uniformly dispersed. A photograph of the resulting silicone oil emulsion containing 12,500 cSt silicone oil is shown in Figure 4B. The emulsion is clearly uniform.

[0080] Example 5. Catastrophic phase inversion of a silicone emulsion containing 1,000,000 cSt silicone oil. A silicone emulsion was formed using 46.53 wt% water, 47.19 wt% silicone oil with a viscosity of 1,000,000 cSt, 4.38 wt% active surfactant (Lutensol® XL79), and 1.24 wt% polar additive (Lorol® C10). A blend was formed by creating a mixture containing the surfactant and the polar additive. This blend was added to the silicone oil, and then the resulting mixture was mixed at 60 rpm. Thereafter, water was gradually added at a rate of 1 g / min until catastrophic phase inversion occurred. After catastrophic phase inversion, the mixture was further mixed at 60 - 250 rpm. After mixing, water was further added at a rate of 2 g / min.

[0081] A microscopic image of the silicone oil emulsion containing the resulting 1,000,000 cSt silicone oil is shown in Figure 5A. The silicone oil droplets are relatively large and not uniformly dispersed. A photograph of the silicone oil emulsion containing the resulting 1,000,000 cSt silicone oil is shown in Figure 5B. The emulsion is clearly uniform.

[0082] Example 6. A silicone emulsion containing 6.5 wt% surfactant and various amounts of polar additive. A silicone emulsion was formed using water, silicone oil, 5 wt% active surfactant (Glucopon® 625UP), and different amounts of polar additive (Lorol® C10). The emulsion was formed by direct emulsification and then vortex mixed for 2 minutes. This process was performed twice with a 4 - hour interval between each mixing. The related compositions are shown in Figure 6. In the upper image of Figure 6, the composition containing water, surfactant, and polar additive is shown under normal light. In the middle image of Figure 6, the composition containing water, surfactant, and polar additive is shown under cross - polarized light. In the lower image of Figure 6, the composition containing water, surfactant, polar additive, and silicone oil is shown under normal light.

[0083] As can be seen in the middle image of FIG. 6, the birefringence of the composition containing 2 wt% of the polar additive is visible, suggesting that these compositions contain liquid crystals. In the lower image of FIG. 6, the composition containing 2 wt% of the polar additive is uniform, while the composition containing less than 2 wt% of the polar additive is phase-separated.

[0084] Example 7. Catastrophic phase inversion of a silicone emulsion containing 1,000,000 cSt silicone oil. A silicone emulsion was formed using water, 1,000,000 cSt silicone oil, 5 wt% active surfactant (Glucopon® 625UP), and 2 wt% polar additive (Lorol® C10). A blend was formed by creating a mixture containing the surfactant and the polar additive. This blend was added to the silicone oil, and the resulting mixture was then mixed at 60 rpm. Subsequently, water was gradually added at a rate of 1 g / min until catastrophic phase inversion occurred. After catastrophic phase inversion, the mixture was further mixed at 60 - 250 rpm. After mixing, water was added further at a rate of 2 g / min.

[0085] A microscopic image of the resulting silicone oil emulsion containing 1,000,000 cSt silicone oil after being diluted 10-fold is shown in FIG. 7A. The silicone oil droplets are a mixture of relatively small droplets that are uniformly dispersed and relatively large droplets. A photograph of the resulting silicone oil emulsion containing 1,000,000 cSt silicone oil is shown in FIG. 7B. The emulsion is clearly uniform.

[0086] These examples demonstrate the advantage of using a combination of surfactant and polar additive to stabilize aqueous silicone emulsions. Liquid crystals are essential for stabilizing the droplets after emulsification. Liquid crystals can be formed from various surfactants. Silicones with a wide range of viscosities can be emulsified.

[0087] Example 8. Silicone emulsions containing 4 wt% surfactant and various amounts of polar additive. A silicone emulsion was formed using water, silicone oil, 4 wt% of an active surfactant (Lutensol® XL70), and different amounts of a polar additive (NANSA® EVM70 / 2E). The emulsion was formed as described above. The amounts of the components that brought about the formation of the liquid crystal were 4 wt% of Lutensol® XL70, 4 wt% of NANSA EVM® 70 / 2E, and an appropriate amount of water. The amounts of these components were unknown before mixing and experiments were required.

[0088] The corresponding compositions are shown in Figure 8. In the upper image of Figure 8, the composition containing water, surfactant, and polar additive is shown under normal light. In the middle image of Figure 8, the composition containing water, surfactant, and polar additive is shown under cross-polarized light. The middle image of Figure 8 was taken two weeks later to improve the visibility of birefringence. In the lower image of Figure 8, the composition containing water, surfactant, polar additive, and silicone oil is shown under normal light.

[0089] In each image of Figure 8, the concentration of the polar additive increases as follows from left to right: 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.

[0090] As seen in the middle image of Figure 8, the birefringence of the composition containing 4 wt% of the polar additive is visible, suggesting that this composition contains liquid crystals. In the lower image of Figure 8, the composition containing 4 wt% of the polar additive is homogeneous, while the compositions containing less than 4 wt% of the polar additive are phase-separated.

[0091] One of the advantages of using NANSA® EVM70 / 2E or other polar surfactants as the polar additive is that the silicone emulsion has temperature stability.

[0092] Example 9. A silicone emulsion containing 4 wt% of a surfactant, 3 wt% of a stabilizer, and different amounts of a polar additive. A silicone emulsion was formed using water, silicone oil, 4 wt% of an active surfactant (Lutensol® XL70), 3 wt% of a stabilizer (Pluronic® P105), and different amounts of a polar additive (NANSA® EVM70 / 2E). The emulsion was formed as described above. The amounts of the components that brought about the formation of the liquid crystal were 4 wt% of Lutensol® XL70, 8 wt% of NANSA EVM® 70 / 2E, 3 wt% of Pluronic® P105, and an appropriate amount of water. The amounts of these components were unknown before mixing and experiments were required.

[0093] The corresponding compositions are shown in Figure 9. In the upper image of Figure 9, a composition containing water, a surfactant, a stabilizer, and a polar additive is shown under normal light. In the middle image of Figure 9, a composition containing water, a surfactant, a stabilizer, and a polar additive is shown under cross-polarized light. The middle image of Figure 9 was taken two weeks later to improve the visibility of birefringence. In the lower image of Figure 9, a composition containing water, a surfactant, a stabilizer, a polar additive, and silicone oil is shown under normal light.

[0094] In each image of Figure 9, the concentration of the polar additive increases as follows from left to right: 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.

[0095] As seen in the middle image of Figure 9, the birefringence of the composition containing 8 wt% of the polar additive is visible, suggesting that this composition contains liquid crystals. In the lower image of Figure 9, the composition containing 8 wt% of the polar additive is homogeneous, while the compositions containing less than 8 wt% of the polar additive are phase-separated.

[0096] One advantage of using NANSA® EVM70 / 2E or other polar surfactants in combination with a stabilizer (e.g., Pluronic® P105) as a polar additive is that the silicone emulsion has temperature stability.

[0097] The description herein explains the present disclosure, including the best mode, and also uses examples to enable those skilled in the art to practice the present disclosure, such as manufacturing and using a composition or system and performing incorporated methods. The scope of patentability of the present disclosure is defined by the claims and may include other examples that occur to those skilled in the art. Such other examples are intended to be within the scope of the claims if they have elements that do not differ from the language of the claims or include equivalent elements that have no substantial difference from the language of the claims.

[0098] As used herein, the terms "comprising," "including," "containing," "having," "characterized by," or any other variation thereof are intended to cover non-exclusive inclusion subject to the explicitly stated limitations. For example, a composition, mixture, process, or method that includes a list of elements is not necessarily limited to only those elements, but may include other elements not explicitly listed or other elements inherent to such composition, mixture, process, or method.

[0099] The transitional phrase "consisting of" excludes elements, steps, or components not specified. If such a phrase appears in a claim, materials other than those described are not included in the claim, except for the usual accompanying impurities. When the phrase "consisting of" appears in a clause of the body of the claim rather than immediately following the preamble, only the elements specified in that clause are limited, and other elements are not excluded from the entire claim.

[0100] The transitional phrase "consisting essentially of" is used to define a composition or method that includes materials, steps, features, components, or elements in addition to what is literally disclosed, provided that these additional materials, steps, features, components, or elements do not materially affect the basic and novel features recited in the claims of the invention. The term "consisting essentially of" lies between "comprising" and "consisting of".

[0101] It should be readily understood that when an invention or a part thereof is defined by a non-limiting term such as "comprising", the description should (absent a contrary indication) also be construed as describing such an invention using the terms "consisting essentially of" or "consisting of".

[0102] Furthermore, unless expressly stated to the contrary, "or" means an inclusive or and not an exclusive or. For example, the condition A or B is satisfied by any one of the following: A is true (or present) and B is false (or absent), A is false (or absent) and B is true (or present), and both A and B are true (or present).

[0103] The indefinite articles "a" and "an" preceding an element or component of the invention are also intended to be non-limiting with respect to the number of occurrences of the element or component. Thus, "a" or "an" should be construed to include one or at least one, and the singular form of an element or component includes the plural unless the number is clearly intended to be singular.

[0104] As used herein, the term "about" means plus or minus 10% of a value.

Claims

1. A silicone oil, a liquid crystal, an aqueous solvent, a polar additive, and a surfactant an emulsion containing a liquid crystal and wherein the surfactant is present in an amount of less than about 20% by weight of the emulsion.

2. The emulsion according to claim 1, wherein the surfactant is selected from the group consisting of an ionic surfactant, a cationic surfactant, an anionic surfactant, an amphoteric surfactant, a zwitterionic surfactant, a nonionic surfactant, an alcohol ethoxylate, an alcohol alkoxylate, an alkyl polyglycoside, an alkyl polyglucoside, an extended surfactant, a surfactant containing 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 of less than about 15% by weight of the emulsion.

4. The emulsion according to claim 1, wherein when the surfactant is present in an amount of less than about 20% by weight of the emulsion without the polar additive, it contains a surfactant that is not in the form of a liquid crystal separately.

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 a polar oil, an alcohol, an alkyl ester, a fatty acid, a polar aromatic, a surfactant, a polar surfactant, and combinations thereof.

7. The emulsion according to claim 1, wherein the polar additive is present in a weight fraction range of about 0.25 to about 5.0 with respect to the surfactant.

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

9. The emulsion according to claim 1, wherein the silicone oil is selected from the group consisting of polydimethylsiloxane, an organically modified silicone, an amino-modified silicone, a methyl silicone resin, an 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 to about 1,500,000 cSt.

11. The emulsion according to claim 1, further comprising a stabilizer selected from the group consisting of a surfactant, a polymer, solid particles, a surface-active protein, a fiber, a clay, a temperature stabilizer, and combinations thereof.

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

13. A composition comprising the emulsion according to claim 1, selected from the group consisting of a sealant composition, a coating composition, an adhesive composition, an elastomer composition, a release agent composition, a texture improving composition, a lubricant composition, an antifoaming composition, a gloss imparting 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 silicone oil, a liquid crystal, an aqueous solvent, a polar additive, and a surfactant and a liquid crystal containing An emulsion, wherein the surfactant is present in an amount of less than about 20% by weight of the emulsion, a method for producing an emulsion, Optionally, a first amount of the aqueous solvent, Optionally, a first amount of the silicone oil, the polar additive, Optionally, the surfactant in the form of a liquid crystal to form a mixture comprising mixing the mixture, Optionally, adding a second amount of the silicone oil, Optionally, adding a second amount of the aqueous solvent A method comprising

15. The step of forming the mixture in the method is forming a first mixture comprising the first amount of the silicone oil and the surfactant, adding the polar additive to the first mixture to form a second mixture The method according to claim 14, comprising

16. The step of forming the mixture in the method is forming a first mixture comprising the first amount of the aqueous solvent, the polar additive, and the surfactant, adding the first amount of the silicone oil to the first mixture to form a second mixture The method according to claim 14, comprising

17. The step of mixing the mixture in the method comprises mixing the mixture at a speed of about 300 rpm or less. The method according to claim 14.

18. The step of adding the second amount of the aqueous solvent in the method induces a catastrophic phase inversion of the emulsion. The method according to claim 14.

19. The surfactant is not in the form of a liquid crystal during the step of forming the mixture. The method according to claim 14.

20. A silicone oil, a liquid crystal, an aqueous solvent, a polar additive, and a surfactant and a liquid crystal containing A method of using an emulsion comprising a surfactant present in an amount of less than about 20% by weight 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 elastomer composition, a release agent composition, a texture enhancing composition, a lubricant composition, an antifoaming composition, a gloss imparting 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.