Method for synthesizing elastomer emulsion by emulsion phase inversion method

Abstract

The invention mainly relates to the field of organosilicon chemistry, the technical field of emulsion preparation and the field of high polymer materials, and discloses a method for synthesizing an elastomer emulsion by an emulsion phase inversion method, which is soft and fluffy, improves the combing property and glossiness of hair and endows the hair with various skin feelings such as silky feeling. According to the preparation method, the organic silicon emulsion is prepared from elastomer powder under the emulsification of modified polyether silicone oil. The organic silicon emulsion provided by the invention adopts a phase inversion method, is few in preparation steps, simple to operate, low in cost and high in safety, greatly improves the use safety, can be directly added into hair care products for blending and use, and is suitable for various daily chemical products.

Description

Technical Field

[0001] The present invention mainly relates to the "field of organosilicon chemistry", "field of emulsion preparation technology" and "field of polymer materials", and specifically to a method for synthesizing an elastomer emulsion by an emulsion phase inversion method. Background Art

[0002] Silicone material is a new type of polymer material, which has been widely used in various fields due to its excellent performance. Silicone elastomer is based on high molecular weight linear polysiloxane and is obtained by cross-linking to form a flexible grid. Due to its good swelling and application feeling, its application in daily cosmetics is developing rapidly. In the daily chemical industry, silicone elastomer is also called silicone elastomer gel. Silicone elastomer is generally made by dispersing and swelling high molecular weight cross-linked silicone powder in low viscosity oil. Commonly used oils include cyclopentasiloxane, low viscosity dimethyl silicone oil, cyclohexane, isododecane, etc. Silicone elastomer gel can only be added to the pure oil system or to the oil phase of the emulsified system. Pure water system and emulsified system with a small proportion of oil phase cannot obtain the soft and smooth skin feel of silicone elastomer because it cannot add enough silicone elastomer gel.

[0003] As a new type of green material, silicone emulsion is one of the most important secondary processed silicone products. Usually, silicone emulsion is emulsified by silicone compounds, water, emulsifiers and other additives. If silicone emulsion is to be truly used in industrial production, it needs to have high emulsion stability. The structure and stability of the emulsion are the basis of its application performance. Since the emulsion is a multiphase dispersion system, the droplets tend to coalesce automatically, so it has thermodynamic instability. In order to obtain a stable silicone emulsion, a suitable emulsifier system should be selected to reduce the interfacial tension. Usually, silicone emulsion is obtained by emulsifying silicone oil with a compound emulsifier under heating conditions, but the emulsification process is relatively complicated and is not conducive to energy saving and environmental protection. In addition, the existing hair care products on the market are mostly not ideal for repairing damaged hair after use. Because the formula adds more oil components such as acetylated lanolin, the product is easy to cause greasy hair after use, and the use feeling is poor.

[0004] In view of this, the present invention provides a method for synthesizing an elastomer emulsion by an emulsion phase inversion method. Summary of the invention

[0005] The purpose of the present invention is to provide a method for synthesizing an elastomer emulsion by an emulsion phase inversion method in view of the deficiencies of the prior art.

[0006] In order to solve the above technical problems, the following technical solutions are adopted:

[0007] A method for synthesizing an elastomer emulsion by an emulsion phase inversion method comprises the following steps:

[0008] S1. First take the emulsifier and bake it completely;

[0009] S2. The polyether silicone oil and elastomer powder are slowly added to the completely baked emulsifier, stirred and homogenized to obtain a semi-paste;

[0010] S3. Add primary phase water to make the semi-paste change phase into oil or water emulsion under shearing action, observe the phase change of the semi-paste, then add the remaining water and preservative with stirring, adjust the pH value of the emulsion, and obtain a milky white emulsion.

[0011] A further improvement based on the technical solution is that the elastomer powder is prepared by cross-linking divinyl-terminated silicone oil and hydrogen-containing silicone oil.

[0012] A further improvement based on the technical solution is that the vinyl mass fraction of the divinyl-terminated silicone oil is 2.97% and the viscosity is 23 mm 2 / s.

[0013] A further improvement made on the basis of the technical solution is that the hydrogen value of the side chain hydrogen-containing silicone oil of the divinyl-terminated silicone oil is 1.4%.

[0014] A further improvement based on the technical solution is that the polyether silicone oil is a synthetic self-made PEG series polyether silicone oil, and the PEG series polyether silicone oil includes hydroxyl-terminated PEG-8 polyether silicone oil, PEG-10 polyether silicone oil and PEG-12 series polyether silicone oil; the structure of the PEG series polyether silicone oil is as follows:

[0015]

[0016] Among them, m=65-90; n=6-10; x is 8, 10, 12.

[0017] A further improvement based on the technical solution is that the emulsifier includes isomeric tridecyl alcohol polyether-12 and PEG series polyether silicone oil, wherein, calculated according to the metering method, the ratio of the input amount of the emulsifier to the elastomer powder is (2-4): (55-60).

[0018] A further improvement based on the technical solution is that in step S1, a composite surfactant needs to be added when baking the emulsifier. The composite surfactant is a non-ionic surfactant. The ratio of the composite surfactant to the emulsifier is 100:(2-10) by weight.

[0019] A further improvement based on the technical solution is that the nonionic surfactant is at least one of the silicone surfactants suitable for water-in-oil systems, including isomeric alcohol polyoxyethylene ether, fatty acid methyl ester polyoxyethylene ether, trimethyl nonanol polyoxyethylene ether, glycerol monostearate, fatty acid polyoxyethylene ester, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, glycerol fatty acid ester, polyglycerol fatty acid ester, propylene glycol fatty acid ester, polyoxyethylene hardened castor oil fatty acid ester, sorbitan tristearate polyoxyethylene ether ester, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene ether and PEG-55 stearate.

[0020] A further improvement based on the technical solution is that in step S3, the shear homogenization emulsification rate is 100-200 rpm / min.

[0021] A further improvement based on the technical solution is that in step S3, the water is the continuous phase of the emulsion, the water is deionized water or purified water, and the amount of the water is 30-35% of the total formula amount. A further improvement based on the technical solution is that the mercaptosilane is one of 3-mercaptopropylmethyldimethoxysilane and 3-mercaptopropyltrimethoxysilane.

[0022] The above technical solution has the following beneficial effects:

[0023] The invention discloses a method for synthesizing an elastomer emulsion by an emulsion phase inversion method, which is smooth, fluffy, improves the combing property and glossiness of hair, and gives hair various skin feelings such as a silky feeling. The preparation method prepares an organosilicon emulsion by emulsifying an elastomer powder with a modified polyether silicone oil. The organosilicon emulsion of the invention adopts a phase inversion method, has a small number of preparation steps, is simple to operate, has a low cost, and is highly safe, greatly improving the safety of use, can be directly added to hair care products for preparation and use, and is suitable for various daily chemical products.

[0024] PEG series polyether silicone oil (INCI name: Polyether Modified polysiloxane) has good hydrophilicity. In hair care products, it can improve the combing and glossiness of hair and give hair a silky feel. It can also reduce the irritation of components such as surfactants to the eyes. It is physiologically inert and very safe to add to daily chemical systems. It can promote chemical degradation under the action of clay and nitrate ions or under ultraviolet irradiation, and it does not pollute the environment.

[0025] Emulsifiers can absorb polar and non-polar oils and fats, and can be used as thickeners in W / O systems or pure oil systems. They have good compatibility with oil systems and can reduce the viscosity of the formula system, making the product refreshing and non-greasy, with a long-lasting silky feel. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] The present invention will be further described below in conjunction with the accompanying drawings:

[0027] Figure 1 The improvement graphs of the dry / wet combing performance of Example 1, Example 2, Example 3 and the blank sample of the present invention are shown in FIG.

[0028] Figure 2 This is a visual comparison chart of hair bundles before and after the emulsion shampoo test in Example 1 of the present invention.

[0029] Figure 3 This is a visual comparison chart of hair bundles before and after the emulsion shampoo test in Example 2 of the present invention.

[0030] Figure 4 This is a visual comparison chart of hair bundles before and after the emulsion shampoo test in Example 3 of the present invention.

[0031] Figure 5 The following are sensory evaluation graphs of hair tresses treated with emulsions of different embodiments of the present invention. DETAILED DESCRIPTION

[0032] In order to make the purpose, technical scheme and advantages of the present invention clearer, the present invention is further described in detail below through the accompanying drawings and embodiments. However, it should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the scope of the present invention. In addition, in the following description, the description of known structures and technologies is omitted to avoid unnecessary confusion of the concept of the present invention.

[0033] A method for synthesizing an elastomer emulsion by an emulsion phase inversion method comprises the following steps:

[0034] S1. First, take the emulsifier and bake it completely; the emulsifier includes isotridecyl alcohol polyether-12 and PEG series polyether silicone oil. Specific isotridecyl alcohol polyether-12 emulsifier and PEG series polyether silicone oil are used, and through precise measurement and control, they are baked at a specific temperature to ensure reaction stability and effectiveness.

[0035] S2. Slowly add the polyether silicone oil and the elastomer powder to the completely baked emulsifier, stir and homogenize to obtain a semi-paste. In this process, the stirring time and speed need to be strictly controlled to ensure that the dispersion state of the elastomer powder in the liquid is stable and to avoid precipitation, stratification and other problems.

[0036] S3. Add primary phase water to the semi-paste, adjust the shear rate so that the semi-paste changes phase into oil or water emulsion under shear, and observe the phase change of the semi-paste. In this process, it is necessary to closely observe the phase change of the semi-paste and adjust the shear rate in time to ensure the quality of the emulsion. Adjust the pH value of the emulsion through precise metering and control to ensure the stability and safety of the emulsion. Finally, stir at high speed to make the emulsion milky white, thereby obtaining the final elastomer emulsion. In this process, the stirring speed and time need to be strictly controlled to ensure the uniformity and stability of the emulsion.

[0037] As a further illustration of this embodiment, the elastomer powder is prepared by cross-linking divinyl-terminated silicone oil and hydrogen-containing silicone oil.

[0038] As a further illustration of this embodiment, the vinyl mass fraction of the divinyl-terminated silicone oil is 2.97%, and the viscosity is 23 mm 2 / s.

[0039] As a further illustration of this embodiment, the hydrogen value of the side chain hydrogen-containing silicone oil of the divinyl-terminated silicone oil is 1.4%.

[0040] As a further illustration of this embodiment, the polyether silicone oil is a synthetic self-made PEG series polyether silicone oil, and the PEG series polyether silicone oil includes hydroxyl-terminated PEG-8 polyether silicone oil, PEG-10 polyether silicone oil and PEG-12 series polyether silicone oil; the structure of the PEG series polyether silicone oil is as follows:

[0041]

[0042] Among them, m=65-90; n=6-10; x is 8, 10, 12.

[0043] As a further illustration of this embodiment, according to the metering method, the ratio of the input amount of the emulsifier to the elastomer powder is (2-4): (55-60).

[0044] As a further illustration of this embodiment, in step S1, a composite surfactant needs to be added when baking the emulsifier. The composite surfactant is a nonionic surfactant. In terms of weight, the ratio of the composite surfactant to the emulsifier is 100:(2-10).

[0045] As a further illustration of this embodiment, the nonionic surfactant is at least one of the silicone surfactants selected from isomeric alcohol polyoxyethylene ether, fatty acid methyl ester polyoxyethylene ether, trimethyl nonanol polyoxyethylene ether, glycerol monostearate, fatty acid polyoxyethylene ester, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, glycerol fatty acid ester, polyglycerol fatty acid ester, propylene glycol fatty acid ester, polyoxyethylene hardened castor oil fatty acid ester, sorbitan tristearate polyoxyethylene ether ester, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene ether and PEG-55 stearate adapted to the water-in-oil system.

[0046] As a further illustration of this embodiment, in step S3, the shear homogenization emulsification rate is 100-200 rpm / min.

[0047] As a further illustration of this embodiment, in step S3, the water is the continuous phase of the emulsion, the water is deionized water or purified water, and the amount of the water is 30-35% of the total formula amount. As a further illustration of this embodiment, the mercaptosilane is one of 3-mercaptopropylmethyldimethoxysilane and 3-mercaptopropyltrimethoxysilane.

[0048] The beneficial effects of this technical solution are as follows:

[0049] 1. Optimizing the dispersion effect: The present invention mixes the elastomer powder and a specific emulsifier (such as isotridecyl alcohol polyether-12, PEG-55 stearate, etc.) through specific steps and proportions to form a semi-paste, and then transforms the phase into an oil / water emulsion under a certain shearing action. This method can make the dispersion state of the elastomer powder in the liquid more stable and is less prone to problems such as precipitation and stratification.

[0050] 2. Reduce irritation: In the preparation process of the present invention, less emulsifiers and other substances are used, and they are added only in the final stage, which can effectively reduce the irritation of these substances to the skin, eyes, etc., and have less impact on human health.

[0051] 3. Energy saving and environmental protection: The preparation process of the present invention is simple and does not require excessive energy consumption, which is beneficial to environmental protection and resource conservation.

[0052] 4. Improve product quality: The elastomer emulsion prepared by the present invention can effectively maintain the softness and moisturization of hair and keep it smooth for a long time, improve the combing property of hair and give hair a silky feel, and can also reduce the irritation of components such as surfactants to the eyes. It has physiological inertness and is very safe to be added to the daily chemical system.

[0053] Through the above steps, the present invention can obtain a stable elastomer emulsion, which can be used to prepare hair care products, can effectively maintain the softness and moisturizing degree of hair and keep it smooth for a long time, can improve the combing property of hair and give hair a silky feeling, can also reduce the irritation of components such as surfactants to the eyes, has physiological inertness, and is very safe to be added to daily chemical systems.

[0054] In order to further understand the present invention, the self-leveling high bonding strength electronic adhesive and the preparation method thereof provided by the present invention are described below in conjunction with embodiments. The protection scope of the present invention is not limited by the following embodiments.

[0055] Example 1

[0056] Weigh 4 parts by weight of isotridecyl alcohol polyether-12 and 3 parts by weight of PEG-55 stearate, and bake them completely in a 60°C water bath in advance; slowly add 60 parts by weight of elastomer powder and 2 parts by weight of PEG-8 polyether silicone oil in small amounts and multiple times, stir evenly, and beat into a semi-paste; (maintain time is 20 minutes, 100-150rpm / min.) Adjust the speed to about 200rpm / min, add initial phase water (50% of the total amount) water to prevent the emulsion from foaming; observe the phase transition of the semi-paste, take a sample to measure the emulsion particle size after 20-30 minutes, and the particle size is 3.0μm; then add the remaining water phase and preservative, adjust the pH value of the emulsion, and stir at about 200rpm / min for 30 minutes to obtain a milky white elastomer emulsion.

[0057] Example 2

[0058] Weigh 4.5 parts by weight of isotridecyl alcohol polyether-12 and 2.5 parts by weight of PEG-55 stearate, and bake them completely in a 60°C water bath in advance; slowly add 55 parts by weight of elastomer powder and 1.5 parts by weight of PEG-10 polyether silicone oil, in small amounts and multiple times, stir evenly, and beat into a semi-paste; (maintain time is 20 minutes, 100-150rpm / min.) Adjust the speed to about 200rpm / min, add initial phase water (50% of the total amount) water to prevent the emulsion from foaming; observe the phase transition of the semi-paste, take a sample to measure the emulsion particle size after 20-30 minutes, and the particle size is 4.9μm; then add the remaining water phase and preservative, adjust the pH value of the emulsion, and stir at about 200rpm / min for 30 minutes to obtain a milky white elastomer emulsion.

[0059] Example 3

[0060] Weigh 4.2 parts by weight of isotridecyl alcohol polyether-12 and 3 parts by weight of PEG-55 stearate, and bake them completely in a 60°C water bath in advance; slowly add 58 parts by weight of elastomer powder and 1.5 parts by weight of PEG-12 polyether silicone oil, in small amounts and multiple times, stir evenly, and beat into a semi-paste; (maintain time is 20 minutes, 100-150rpm / min.) Adjust the speed to about 200rpm / min, add initial phase water (50% of the total amount) water to prevent the emulsion from foaming; observe the phase transition of the semi-paste, take a sample to measure the emulsion particle size after 20-30 minutes, and the particle size is 4.1μm; then add the remaining water phase and preservative, adjust the pH value of the emulsion, and stir at about 200rpm / min for 30 minutes to obtain a milky white elastomer emulsion.

[0061] The above embodiments were investigated for stability and application performance, and the results are as follows:

[0062] 1. Stability test results

[0063] Table 1 Stability investigation

[0064]

[0065]

[0066] 2. Application performance evaluation

[0067] 2.1 Conditioning performance - dry / wet combing of hair

[0068] See also Figure 1 , tested on healthy hair bundles: adding the example emulsion to shampoo can effectively improve wet combing and dry combing performance.

[0069] Table 2 Shampoo formula

[0070] Formula ingredients Blank Comparison sample 1 Comparison sample 2 Comparison sample 3 water To 100 To 100 To 100 To 100 Sodium Laureth Sulfate (70%) 15 15 15 15 Cocamidopropyl Betaine (35%) 8 8 8 8 Cocamide MEA 1 1 1 1 Ethylene glycol distearate (13%) 7 7 7 7 Guar Hydroxypropyltrimonium Chloride 0.5 0.5 0.5 0.5 Example 1 Emulsion - 3.7 - - Example 2 Emulsion - - 3.7 - Example 3 Emulsion - - - 3.7 Disodium EDTA 0.05 0.05 0.05 0.05 Sodium chloride 0.7 0.7 0.7 0.7 Citric acid qs qs qs qs

[0071] The results show that the dry and wet combing forces of hair bundles can be significantly reduced by shampoo treatment containing 3.7% of the example emulsion. The improvement of dry combing performance of healthy hair bundles by elastomer emulsions prepared with PEG of different structures shows that the polyether of PEG-8 structure has a significant improvement effect.

[0072] 2.2 Adjustment performance - fluffy and airy feeling of hair

[0073] PEG series polyether modified polysiloxane has good hydrophilicity. In hair care products, it can improve the combing and glossiness of hair and give hair a silky feel. Its special structure effectively improves the spread of silicone chain segments on hair bundles, making the hair care effect significant;

[0074] 2.2.1 Fluffiness test

[0075] The hair bundles before treatment were naturally fixed vertically on the rack and left to stand for 30 minutes to remove static electricity. The hair bundles were combed 5 times and the state of the samples was recorded with a camera at a fixed position.

[0076] The treated hair strands were placed in the same position for 30 minutes, combed 5 times, and photographed at the same position.

[0077] Extract the hair bundle outline through Ps and calculate the area according to the trapezoidal formula. S = (upper + lower) * height / 2

[0078] Calculate the volume percentage of a hair clump:

[0079]

[0080] Table 3 Shampoo Fluffiness Test Results

[0081] Sample name Integral area Fluffy feeling / % Containing Example 1 emulsion shampoo Front 66.099 / Rear 77.080 16.6 Containing Example 2 emulsion shampoo Front 65.275 / Rear 66.704 2.19 Containing Example 3 emulsion shampoo Front 59.953 / Rear 65.450 9.17

[0082] The results show that Figure 2 , Figure 3 and Figure 4 , after being treated with shampoo containing 3.7% of the emulsion of the embodiment, the fluffiness of healthy hair can be significantly improved, giving the hair a silky feel; for the improvement of the fluffiness of healthy hair by the elastomer emulsions prepared with PEG of different structures, it can be concluded that the polyether of PEG-8 structure has a significant improvement effect.

[0083] 2.3 Human sensory evaluation

[0084] The hair bundles are renumbered and hung straight and parallel on a rack. A skin sensory evaluation team directly touches the hair bundles with their hands and conducts a sensory evaluation of the hair bundles, including smoothness, softness, suppleness, stickiness, fluffiness, etc.

[0085] Very poor: 1 point, Poor: 2 points, Average: 3 points, Good: 4 points, Excellent: 5 points.

[0086] The above results show that Figure 5 , after being treated with shampoo containing 3.7% of the emulsion of Example 1, the fluffiness of healthy hair bundles can be significantly improved, giving the hair a silky feel.

[0087] From the comprehensive results, it can be seen that when the modified elastomer emulsion of the present invention is used to prepare hair care products, it can effectively maintain the softness and moisturization of hair and keep it smooth for a long time, can improve the combing properties of hair and give hair a silky feel, can also reduce the irritation of components such as surfactants to the eyes, has physiological inertness, and is very safe to be added to daily chemical systems.

[0088] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solution of the present invention can be modified or replaced by equivalents without departing from the essence and scope of the technical solution of the present invention.

Claims

1. A method for synthesizing an elastomer emulsion by an emulsion phase inversion method, characterized in that The following steps are involved: S1. First take the emulsifier and bake it completely; S2. The polyether silicone oil and elastomer powder are slowly added to the completely baked emulsifier, stirred and homogenized to obtain a semi-paste; S3. Add primary phase water to make the semi-paste change phase into oil or water emulsion under shearing action, observe the phase change of the semi-paste, then add the remaining water and preservative with stirring, adjust the pH value of the emulsion, and obtain a milky white emulsion.

2. The method for synthesizing an elastomer emulsion by an emulsion phase inversion method according to claim 1, characterized in that: The elastomer powder is prepared by cross-linking divinyl-terminated silicone oil and hydrogen-containing silicone oil.

3. The method for synthesizing an elastomer emulsion by an emulsion phase inversion method according to claim 2, characterized in that: The vinyl mass fraction of the divinyl-terminated silicone oil is 2.97%, and the viscosity is 23 mm 2 / s.

4. The method for synthesizing an elastomer emulsion by an emulsion phase inversion method according to claim 2, characterized in that: The side chain hydrogen-containing silicone oil of the divinyl-terminated silicone oil has a hydrogen value of 1.4%.

5. The method for synthesizing an elastomer emulsion by an emulsion phase inversion method according to claim 1, characterized in that: The polyether silicone oil is a synthetic self-made PEG series polyether silicone oil, and the PEG series polyether silicone oil includes hydroxyl-terminated PEG-8 polyether silicone oil, PEG-10 polyether silicone oil and PEG-12 series polyether silicone oil; the structure of the PEG series polyether silicone oil is as follows: Among them, m=65-90; n=6-10; x is 8, 10, 12.

6. The method for synthesizing an elastomer emulsion by an emulsion phase inversion method according to claim 5, characterized in that: The emulsifier includes isomeric tridecyl alcohol polyether-12 and PEG series polyether silicone oil, wherein, calculated according to the metering method, the ratio of the input amount of the emulsifier to the elastomer powder is (2-4): (55-60).

7. The method for synthesizing an elastomer emulsion by an emulsion phase inversion method according to claim 1, characterized in that: In step S1, a composite surfactant needs to be added when baking the emulsifier. The composite surfactant is a nonionic surfactant. The ratio of the composite surfactant to the emulsifier is 100:(2-10) by weight.

8. The method for synthesizing an elastomer emulsion by an emulsion phase inversion method according to claim 1, characterized in that: The nonionic surfactant is at least one of isomeric alcohol polyoxyethylene ether, fatty acid methyl ester polyoxyethylene ether, trimethyl nonanol polyoxyethylene ether, glycerol monostearate, fatty acid polyoxyethylene ester, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, glycerol fatty acid ester, polyglycerol fatty acid ester, propylene glycol fatty acid ester, polyoxyethylene hardened castor oil fatty acid ester, sorbitan tristearate polyoxyethylene ether ester, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene ether and PEG-55 stearate, which is suitable for silicone surfactants in water-in-oil systems.

9. The method for synthesizing an elastomer emulsion by an emulsion phase inversion method according to claim 1, characterized in that: In step S3, the shear homogenization emulsification rate is 100-200 rpm / min.

10. The method for synthesizing an elastomer emulsion by an emulsion phase inversion method according to claim 1, characterized in that: In step S3, the water is the continuous phase of the emulsion, the water is deionized water or purified water, and the amount of the water is 30-35% of the total formula.

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