Stable organic silicon emulsion as well as preparation method and application thereof

Abstract

The invention relates to the technical field of organic silicon emulsion preparation, and discloses stable organic silicon emulsion as well as a preparation method and application thereof. According to the method, hydroxyl-terminated polymethylsilicone oil is used as an organic silicon matrix, hydroxypropyl-beta-cyclodextrin is used as a biomass hydrophilic modifier, self-made glyceryl ether modified methylsilane is matched, a prepolymer is prepared through compound modification, then the prepolymer and a compound emulsifier aqueous solution are mixed and emulsified, and finally a finished product is obtained through crosslinking curing of an initiator. The problems that an existing organic silicon emulsion is prone to layering and demulsification, poor in compatibility and single in function are solved through a double stabilization mechanism of physical anchoring and chemical crosslinking, and the product keeps a uniform state in a complex environment and has the multiple functions of softness, lubrication, film forming and the like. The preparation process is simple and mild, raw materials are easy to obtain, complex purification is not needed, and the method is suitable for large-scale production and can be widely applied to the fields of textiles, cosmetics, personal care, medicine and industry.

Description

Technical Field

[0001] This invention relates to the field of organosilicon emulsion preparation technology, specifically to a stable organosilicon emulsion, its preparation method, and its application. Background Technology

[0002] Silicone emulsions are widely used in textiles, cosmetics, personal care, and pharmaceuticals, often serving as softeners, lubricants, or film-forming agents to enhance product performance. However, existing silicone emulsions suffer from significant instability. During temperature fluctuations or long-term storage, they are prone to stratification and demulsification, making it impossible to maintain a uniform system state. This affects the consistency of subsequent use and may even cause them to lose their intended function, posing challenges to practical applications.

[0003] Existing silicone emulsions have shortcomings in terms of compatibility. When used in combination with other additives or different substrates, they are prone to interacting with other systems, leading to problems such as aggregation and precipitation. This not only damages the performance of the silicone emulsion itself but also interferes with the stability of the overall formulation, increases the difficulty of debugging during application, and limits its compatibility in multi-component composite systems, making it difficult to meet the needs of use in complex scenarios.

[0004] As the requirements for material performance increase across various fields, the issue of the limited functionality of existing silicone emulsions is becoming increasingly prominent. Most products can only meet a single application need, such as providing only a softening effect or only having basic film-forming capabilities, and cannot simultaneously achieve multiple performance indicators. For example, in the textile industry, it is necessary to improve the softness of fabrics while ensuring their smoothness and durability. Existing silicone emulsions often cannot meet these diverse needs simultaneously, limiting their promotion in high-end application scenarios. Summary of the Invention

[0005] In view of this, the purpose of the present invention is to provide a stable organosilicon emulsion, its preparation method and application, which effectively solves the stability problems of existing organosilicon emulsions that are prone to stratification and demulsification when subjected to temperature fluctuations or long-term storage, the compatibility problems of easy aggregation and precipitation when combined with other systems, and the shortcomings of single function that makes it difficult to adapt to diverse application needs.

[0006] The objective of this invention can be achieved through the following technical solutions:

[0007] In a first aspect, the present invention provides a method for preparing a stable organosilicon emulsion, comprising the following preparation steps:

[0008] S1: Add the organosilicon matrix to the reaction apparatus, initially heat and stir, add biomass hydrophilic modifier and glycerol ether modified methylsilane, adjust the pH of the system, heat and keep the temperature for reaction, and obtain the composite modified organosilicon prepolymer.

[0009] S2: Mix deionized water with compound emulsifier, heat and stir to form a homogeneous aqueous phase, add the composite modified organosilicon prepolymer obtained in step S1 into the aqueous phase in portions, and disperse by high-speed shearing and stirring to obtain a preemulsion.

[0010] S3: Add an initiator to the pre-emulsion, adjust the stirring speed and heat up to maintain the reaction temperature. After cooling to room temperature, adjust the solid content of the emulsion and filter to obtain a stable organosilicon emulsion.

[0011] Further, the raw materials, by weight, include: 100-130 parts of organosilicon matrix, 7-11 parts of glycerol ether modified methylsilane, 3-5 parts of biomass hydrophilic modifier, 5-7 parts of compound emulsifier, 0.2-0.4 parts of initiator, and 180-220 parts of deionized water.

[0012] The organosilicon matrix is ​​hydroxyl-terminated polymethyl silicone oil;

[0013] The biomass hydrophilic modifier is hydroxypropyl-β-cyclodextrin;

[0014] Furthermore, the preparation method of the glycerol ether modified methylsilane is as follows:

[0015] Methyltrimethoxysilane, glycerol monoglycidyl ether, polyethylene glycol monomethyl ether, and triethanolamine were mixed, stirred, and heated to the initial temperature and kept at that temperature. Deionized water was added, and the temperature was raised to the first reaction temperature and kept at that temperature. Then the temperature was raised to the second reaction temperature and kept at that temperature. After the reaction was completed, the mixture was cooled to room temperature to obtain a pale yellow, transparent glycerol ether-modified methylsilane.

[0016] Further, the methyltrimethoxysilane, glyceryl monoglycidyl ether, polyethylene glycol monomethyl ether, and triethanolamine, by weight, are 5-7 parts of methyltrimethoxysilane, 5-6 parts of glyceryl monoglycidyl ether, 0.8-1 parts of polyethylene glycol monomethyl ether, and 0.5-0.7 parts of triethanolamine, respectively.

[0017] The stirring speed is 2800rpm-320rpm, the initial temperature is 32℃-40℃, and the corresponding holding and stirring time is 15min-25min; the first reaction temperature is 55-60℃, and the corresponding holding and reaction time is 50min-80min; the second reaction temperature is 65℃-70℃, and the corresponding holding and reaction time is 60min-80min.

[0018] Further, in step S1, the initial heating and stirring speed is 350 rpm-450 rpm, the temperature is raised to 52℃-58℃ and held for 10 min-15 min, the biomass hydrophilic modifier is added and dispersed for 15 min-20 min, the glycerol ether modified methylsilane is added and stirred for 20 min-30 min; the pH of the system is adjusted to 4.5-5.5, and the temperature is raised to 70℃-75℃ and held for 1 h-2.5 h.

[0019] Further, in step S2, the aqueous phase is stirred at 1000 rpm-1200 rpm, heated to 45℃-55℃ and stirred for 20 min-30 min; the composite modified organosilicon prepolymer is added in 2-3 batches, with an interval of 10 min-15 min between each batch, and high-speed shear stirring is maintained for 15 min-20 min after each addition, and high-speed stirring is continued for 30 min-40 min after all the prepolymer has been added.

[0020] Furthermore, the compound emulsifier is composed of anionic emulsifier and nonionic emulsifier, with a mass ratio of anionic emulsifier to nonionic emulsifier of 1:1-3. The anionic emulsifier is at least one of sodium dodecylbenzenesulfonate, sodium fatty alcohol polyoxyethylene ether sulfate, and sodium alkyl sulfonate. The nonionic emulsifier is polyoxyethylene sorbitan monooleate.

[0021] Further, in step S3, the stirring speed is 600rpm-800rpm, the temperature is raised to 85℃-90℃ and kept at that temperature for 2h-3h; after cooling to room temperature, the solid content of the emulsion is adjusted to 30%-35%, and the initiator is potassium persulfate.

[0022] Secondly, the present invention provides a stable organosilicon emulsion obtained by the above-described method for preparing a stable organosilicon emulsion.

[0023] Thirdly, the stable organosilicon emulsion provided by the present invention can be used in textiles, cosmetics, personal care products, pharmaceuticals or industrial fields as a softener, lubricant, film-forming agent or stabilizer.

[0024] The beneficial effects of this invention are:

[0025] This invention significantly improves the overall stability of silicone emulsions, effectively avoiding stratification, demulsification, and coagulation under complex environments such as long-term storage, temperature fluctuations, and the presence of electrolytes. It ensures that the emulsion always remains in a uniform state, extends the product's service life, and guarantees consistent performance.

[0026] The preparation process of this invention is simple and efficient. All raw materials used are common and readily available industrial-grade products. The self-made modified silane does not require complicated purification steps. The reaction conditions are mild and easy to control. No special equipment is required, which reduces the difficulty and cost of production and makes it suitable for large-scale industrial production.

[0027] The organosilicon emulsion prepared by this invention has both good compatibility and multifunctional adaptability. It can be efficiently matched with additives and substrates of different systems, and can simultaneously meet multiple application requirements such as softening, lubrication, and film formation. This broadens the scope of application in multiple fields such as textiles, daily chemicals, and industry, and solves the limitations of traditional products with single function and poor adaptability. Detailed Implementation

[0028] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0029] The polyethylene glycol monomethyl ether used in the following examples is MPEG-400, which was purchased from Haian Petrochemical Plant in Jiangsu Province.

[0030] The hydroxyl-terminated polymethyl silicone oil used in the following examples is hydroxyl-terminated polymethyl silicone oil MY 1203, purchased from Anhui Mingyi Silicon Industry Co., Ltd.

[0031] The tetramethyldiphenyltrisiloxane used in the following examples is tetramethyldiphenyltrisiloxane MY 232, which was purchased from Anhui Mingyi Silicon Industry Co., Ltd.

[0032] The hydroxypropyl-β-cyclodextrin used in the following examples had a dry basis content of 98% and an active ingredient content of 99.5%, and was purchased from Anhui Mingyi Silicon Industry Co., Ltd.

[0033] Example 1

[0034] A method for preparing a stable organosilicon emulsion includes the following preparation steps:

[0035] Preparation of glycerol ether modified methylsilane: 5 parts by weight of methyltrimethoxysilane, 5 parts by weight of glycerol monoglycidyl ether, 0.8 parts by weight of MPEG-400 and 0.5 parts by weight of triethanolamine were mixed. The mixture was stirred at 320 rpm and heated to 32°C for 25 min. Deionized water was added, and the mixture was heated to 55°C for 80 min. The temperature was then increased to 65°C and the mixture was kept at this temperature for another 80 min. After the reaction was completed, the mixture was cooled to room temperature to obtain glycerol ether modified methylsilane.

[0036] S1: Add 100 parts of hydroxyl-terminated polymethyl silicone oil MY 1203 to the reactor, turn on the stirrer and adjust the speed to 350 rpm, initially heat to 52℃ and keep warm for 15 min; add 3 parts of hydroxypropyl-β-cyclodextrin to the reactor and disperse at the current speed for 20 min; then add 7 parts of the glycerol ether modified methylsilane prepared above, and continue stirring for 30 min; adjust the pH of the system to 4.5 with 98% glacial acetic acid, heat to 70℃, and keep warm for 2.5 h to obtain the composite modified organosilicon prepolymer.

[0037] S2: Mix 180 parts of deionized water with 5 parts of compound emulsifier. The compound emulsifier is composed of 2.5 parts of sodium dodecylbenzenesulfonate and 2.5 parts of polyoxyethylene sorbitan monooleate in a mass ratio of 1:1. Turn on the stirrer and adjust the speed to 1000 rpm. Heat the mixture to 45°C and stir for 30 min to form a homogeneous aqueous phase. Add the composite modified organosilicon prepolymer to the aqueous phase in two portions, with an interval of 15 min between each addition. After each addition, maintain high-speed shear stirring for 20 min. After all the prepolymer has been added, continue high-speed stirring for 40 min to obtain the preemulsion.

[0038] S3: Add 0.2 parts of potassium persulfate to the pre-emulsion, adjust the stirring speed to 600 rpm, heat to 85℃ and keep the temperature for 3 hours; after the reaction is completed, cool to room temperature, add deionized water to adjust the solid content of the emulsion to 30%, filter with a 200-mesh filter to obtain a stable organosilicon emulsion.

[0039] Example 2

[0040] A method for preparing a stable organosilicon emulsion includes the following preparation steps:

[0041] Preparation of glycerol ether modified methylsilane: By weight, 6 parts of methyltrimethoxysilane, 5.5 parts of glycerol monoglycidyl ether, 0.9 parts of MPEG-400 and 0.6 parts of triethanolamine were mixed, stirred and adjusted to 300 rpm, heated to 36℃ and stirred for 20 min; deionized water was added, heated to 58℃ and reacted for 60 min, then heated to 68℃ and reacted for another 70 min; after the reaction was completed, the mixture was cooled to room temperature to obtain glycerol ether modified methylsilane.

[0042] S1: Add 115 parts of hydroxyl-terminated polymethyl silicone oil MY 1203 to the reactor, turn on the stirrer and adjust the speed to 400 rpm, initially heat to 55℃ and keep warm for 12 min; add 4 parts of hydroxypropyl-β-cyclodextrin to the reactor, maintain the current speed and disperse for 18 min; then add 9 parts of the glycerol ether modified methylsilane prepared above, and continue stirring for 25 min; adjust the pH of the system to 5.0 with 98% glacial acetic acid, heat to 72℃, keep warm and react for 1.8 h to obtain the composite modified organosilicon prepolymer.

[0043] S2: Mix 200 parts of deionized water with 6 parts of compound emulsifier. The compound emulsifier is composed of 2 parts of sodium fatty alcohol polyoxyethylene ether sulfate and 4 parts of polyoxyethylene sorbitan monooleate in a mass ratio of 1:2. Turn on the stirrer and adjust the speed to 1100 rpm. Heat the mixture to 50°C and stir for 25 min to form a homogeneous aqueous phase. Add the composite modified organosilicon prepolymer to the aqueous phase in 3 portions, with an interval of 12 min between each addition. After each addition, maintain high-speed shear stirring for 18 min. After all the prepolymers have been added, continue high-speed stirring for 35 min to obtain the preemulsion.

[0044] S3: Add 0.3 parts of potassium persulfate to the pre-emulsion, adjust the stirring speed to 700 rpm, heat to 88℃ and keep the temperature for 2.5 h; after the reaction is completed, cool to room temperature, add deionized water to adjust the solid content of the emulsion to 32%, filter with a 200 mesh filter to obtain a stable organosilicon emulsion.

[0045] Preparation of glycerol ether modified methylsilane: By weight, 5 parts of methyltrimethoxysilane, 5 parts of glycerol monoglycidyl ether, 0.8 parts of MPEG-400 and 0.5 parts of triethanolamine were mixed, stirred and adjusted to 320 rpm, heated to 32℃ and stirred for 25 min; deionized water was added, heated to 55℃ and reacted for 80 min, then heated to 65℃ and reacted for 1 h; after the reaction was completed, the mixture was cooled to room temperature to obtain glycerol ether modified methylsilane.

[0046] Example 3

[0047] A method for preparing a stable organosilicon emulsion includes the following preparation steps:

[0048] Preparation of glycerol ether modified methylsilane: By weight, 5 parts of methyltrimethoxysilane, 5 parts of glycerol monoglycidyl ether, 0.8 parts of MPEG-400 and 0.5 parts of triethanolamine were mixed, stirred and adjusted to 320 rpm, heated to 32℃ and stirred for 25 min; deionized water was added, heated to 55℃ and reacted for 50 min, then heated to 65℃ and reacted for another 60 min; after the reaction was completed, the mixture was cooled to room temperature to obtain glycerol ether modified methylsilane.

[0049] S1: Add 100 parts of hydroxyl-terminated polymethyl silicone oil MY 1203 to the reactor, turn on the stirrer and adjust the speed to 350 rpm, initially heat to 52℃ and keep warm for 15 min; add 3 parts of hydroxypropyl-β-cyclodextrin to the reactor and disperse at the current speed for 20 min; then add 7 parts of the glycerol ether modified methylsilane prepared above, and continue stirring for 30 min; adjust the pH of the system to 4.5 with 98% glacial acetic acid, heat to 70℃, and keep warm for 2.5 h to obtain the composite modified organosilicon prepolymer.

[0050] S2: Mix 180 parts of deionized water with 5 parts of compound emulsifier, which consists of 2.5 parts of sodium dodecylbenzenesulfonate and 2.5 parts of polyoxyethylene sorbitan monooleate; turn on the stirrer and adjust the speed to 1000 rpm, heat to 45℃ and stir for 30 min to form a homogeneous aqueous phase; add the composite modified organosilicon prepolymer to the aqueous phase in two batches, with an interval of 15 min between each batch. After each addition, maintain high-speed shear stirring for 20 min. After all the prepolymer has been added, continue high-speed stirring for 40 min to obtain the preemulsion.

[0051] S3: Add 0.2 parts of potassium persulfate to the pre-emulsion, adjust the stirring speed to 600 rpm, heat to 85℃ and keep the temperature for 3 hours; after the reaction is completed, cool to room temperature, add deionized water to adjust the solid content of the emulsion to 30%, filter with a 200-mesh filter to obtain a stable organosilicon emulsion.

[0052] Comparative Example 1

[0053] Compared with Example 1, this comparative example replaces "hydroxypropyl-β-cyclodextrin" with an equal mass of "polyethylene glycol PEG-400". All other steps and parameters are the same, and will not be repeated here. A stable silicone emulsion is finally obtained.

[0054] Comparative Example 2

[0055] Compared with Example 1, this comparative example replaces "glycerol ether modified methylsilane" with an equal mass of "methyltrimethoxysilane". All other steps and parameters are the same, and will not be repeated in this comparative example. Finally, a stable organosilicon emulsion is obtained.

[0056] Comparative Example 3

[0057] Compared with Example 1, this comparative example replaces "glycerol ether modified methylsilane" with an equal mass of "vinyltrimethoxysilane". All other steps and parameters are the same, and will not be repeated in this comparative example. Finally, a stable organosilicon emulsion is obtained.

[0058] Comparative Example 4

[0059] Compared with Example 1, this comparative example replaces "hydroxyl-terminated polymethyl silicone oil MY 1203" with an equal mass of "tetramethyldiphenyltrisiloxane MY 232". All other steps and parameters are the same, and will not be repeated in this comparative example. Finally, a stable organosilicon emulsion is obtained.

[0060] The stable organosilicon emulsions prepared in Examples 1-3 and Comparative Examples 1-4 were tested, and the results are recorded in Table 1.

[0061] 1. Static stability test:

[0062] Take 50 mL of each sample and place it in a transparent sealed container. Let it stand at room temperature (25±2℃) for 180 days. Observe whether layering, demulsification, or oil floating occurs and record the changes in state.

[0063] 2. Centrifugation stability test:

[0064] Take 10 mL of each sample and place it in a centrifuge tube. Centrifuge at 3000 rpm for 30 min using a high-speed centrifuge. After centrifugation, observe whether the emulsion remains homogeneous and whether there is any precipitation, layering, or demulsification.

[0065] 3. High and low temperature stability test:

[0066] Low temperature stability: The sample was frozen at -15℃ for 24 hours, then thawed naturally to room temperature and its condition was observed.

[0067] High temperature stability: The sample was placed in a 60℃ constant temperature oven for 30 days, then removed and cooled to room temperature to observe whether it separated into layers or broke emulsion.

[0068] 4. Electrolyte stability test:

[0069] Each sample was diluted to a solid content of 10%, and then mixed with an equal volume of 5% sodium chloride (NaCl) solution and 5% magnesium sulfate (MgSO4) solution. After stirring evenly, the mixture was allowed to stand for 24 hours to observe whether coagulation, precipitation or demulsification occurred.

[0070] 5. Particle size and particle size change detection:

[0071] The initial particle size (D) of the sample was determined using a laser particle size analyzer. 50 After standing at room temperature for 6 months, D was measured again after 6 months. 50 Calculate the particle size change rate.

[0072] Calculate using the following formula:

[0073]

[0074] Table 1 Experimental test data of stabilized silicone emulsion

[0075] Test item Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Standing stability Uniform milky white liquid, no delamination, emulsion breaking, oil floating Uniform milky white liquid, no delamination, emulsion breaking, oil floating Uniform milky white liquid, no delamination, emulsion breaking, oil floating Delamination after 117 days Complete delamination after 67 days Slight delamination after 123 days Slight delamination after 145 days Centrifugal stability Uniform dispersion, no precipitation, delamination and emulsion breaking Uniform dispersion, no precipitation, delamination and emulsion breaking Uniform dispersion, no precipitation, delamination and emulsion breaking White precipitate at the bottom, slight turbidity in the upper layer Complete emulsion breaking Fine particles at the bottom, uniform in the upper layer No emulsion breaking, a small amount of fine suspended particles appeared High and low temperature stability No delamination after low temperature thawing; no oil floating and stable viscosity after high temperature No delamination after low temperature thawing; no oil floating and stable viscosity after high temperature No delamination after low temperature thawing; no oil floating and stable viscosity after high temperature Delamination (oil phase floating up) after low temperature thawing; oil floating area expanded after high temperature Complete emulsion breaking after low temperature thawing; oil phase aggregated into drops after high temperature No delamination after low temperature thawing; no obvious viscosity change after high temperature No delamination after low temperature thawing; no obvious viscosity change after high temperature Electrolyte stability (5% NaCl) Uniform and transparent, no agglomeration and precipitation Uniform and transparent, no agglomeration and precipitation Uniform and transparent, no agglomeration and precipitation Slight turbidity, no obvious precipitation Severe precipitation (particle size 1-2 mm), solution delamination Uniform and transparent, no agglomeration and precipitation Uniform and transparent, no agglomeration and precipitation Electrolyte resistance stability (5% MgSO4) Uniform and transparent, no agglomeration and precipitation Uniform and transparent, no agglomeration and precipitation Uniform and transparent, no agglomeration and precipitation 0.5 mm fine agglomerates appeared, solution turbid Large agglomerates (particle size 5-8 mm), complete emulsion breaking Partial emulsion breaking, oil floating Uniform and transparent, no agglomeration and precipitation Initial D50 (μm) 0.35 0.42 0.38 0.85 0.92 0.76 0.51 D50 (μm) after 6 months 0.37 0.43 0.39 1.52 2.15 1.38 0.68 Particle size change rate (%) 5.71 2.38 2.63 78.82 133.70 81.58 33.33

[0076] The stable organosilicon emulsions prepared in Examples 1-3 have excellent overall stability and functional adaptability. They can maintain a uniform state under complex environments such as long-term storage, temperature fluctuations and the presence of electrolytes, and are not prone to stratification, demulsification or coagulation. They can also take into account core application performances such as softness and film formation.

[0077] A comparison of Example 1 and Comparative Example 1 shows that hydroxypropyl-β-cyclodextrin plays an irreplaceable and inventive role in the composite modification system of this invention. Unlike conventional hydrophilic modifiers that only improve compatibility by introducing hydrophilic groups, the "externally hydrophilic and internally hydrophobic" cavity structure of hydroxypropyl-β-cyclodextrin can enhance the affinity between organosilicon and the aqueous phase, and can also physically encapsulate emulsifier molecules to form a strong anchor, avoiding the decrease in stability caused by emulsifier desorption.

[0078] A comparison of Example 1 and Comparative Example 2 shows that the self-made glycerol ether-modified methylsilane has significant performance advantages and innovation compared to conventional silane coupling agents. Conventional silane coupling agents have limited functionality, providing only crosslinking sites or a small number of hydrophilic groups, making it difficult to simultaneously balance the crosslinking density and hydrophilicity of organosilicon, resulting in insufficient emulsion stability. In contrast, the glycerol ether-modified methylsilane of this invention, through synergistic modification with multiple raw materials, possesses multiple hydroxyl hydrophilic groups, siloxane crosslinking sites, and an ether-compatible structure. It can form a synergistic effect with hydroxypropyl-β-cyclodextrin, ensuring both the crosslinking strength of the organosilicon molecular chain and improving compatibility with the aqueous phase and emulsifier.

[0079] A comparison of Example 1 and Comparative Example 3 shows that the glycerol ether-modified methylsilane selected in this invention far surpasses ordinary functional silanes in terms of reactivity and performance compatibility. Ordinary silane coupling agents often suffer from insufficient reactivity and poor compatibility with other raw materials, easily leading to uneven crosslinking or localized aggregation, affecting emulsion stability. In contrast, this invention, through self-made modified silane, precisely controls the types of functional groups and reactivity, enabling it to efficiently crosslink with the organosilicon matrix and form a synergistic and stable system with hydroxypropyl-β-cyclodextrin and compound emulsifiers, avoiding the defects of ordinary silanes that are prone to failure under high temperature or electrolyte environments.

[0080] A comparison of Example 1 and Comparative Example 4 shows that the synergistic compatibility between the organosilicon matrix and the composite modification system is a crucial guarantee for the excellent performance of this invention. The hydroxyl-terminated polymethyl silicone oil selected in this invention has terminal hydroxyl groups that can efficiently condense with the silanol groups of glycerol ether-modified methylsilane, while simultaneously forming hydrogen bonds with hydroxypropyl-β-cyclodextrin, ensuring the uniformity and stability of the modification reaction. However, when other types of organosilicon matrices are used, the lack of active sites matching the composite modification system prevents the formation of a dense cross-linked network and stable interfacial interactions, leading to a decline in emulsion stability and functional performance.

[0081] The above description is merely an example and illustration of the concept of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described or use similar methods to replace them, as long as they do not deviate from the concept of the invention or exceed the scope defined in the claims, they should all fall within the protection scope of the present invention.

Claims

1. A method for preparing a stable organosilicon emulsion, characterized in that, The preparation steps include the following: S1: Add the organosilicon matrix to the reaction apparatus, initially heat and stir, add biomass hydrophilic modifier and glycerol ether modified methylsilane, adjust the pH of the system, heat and keep the temperature for reaction, and obtain the composite modified organosilicon prepolymer. S2: Mix deionized water with compound emulsifier, heat and stir to form a homogeneous aqueous phase, add the composite modified organosilicon prepolymer obtained in step S1 into the aqueous phase in portions, and disperse by high-speed shearing and stirring to obtain a preemulsion. S3: Add an initiator to the pre-emulsion, adjust the stirring speed and heat up to maintain the reaction temperature. After cooling to room temperature, adjust the solid content of the emulsion and filter to obtain a stable organosilicon emulsion.

2. The method for preparing a stable organosilicon emulsion according to claim 1, characterized in that, The raw materials, by weight, include: 100-130 parts of organosilicon matrix, 7-11 parts of glycerol ether modified methylsilane, 3-5 parts of biomass hydrophilic modifier, 5-7 parts of compound emulsifier, 0.2-0.4 parts of initiator, and 180-220 parts of deionized water; The organosilicon matrix is ​​hydroxyl-terminated polymethyl silicone oil; The biomass hydrophilic modifier is hydroxypropyl-β-cyclodextrin.

3. The method for preparing a stable organosilicon emulsion according to claim 2, characterized in that, The preparation method of the glycerol ether modified methylsilane is as follows: Methyltrimethoxysilane, glycerol monoglycidyl ether, polyethylene glycol monomethyl ether, and triethanolamine were mixed, stirred, and heated to the initial temperature and kept at that temperature. Deionized water was added, and the temperature was raised to the first reaction temperature and kept at that temperature. Then the temperature was raised to the second reaction temperature and kept at that temperature. After the reaction was completed, the mixture was cooled to room temperature to obtain a pale yellow, transparent glycerol ether-modified methylsilane.

4. The method for preparing a stable organosilicon emulsion according to claim 3, characterized in that, The methyltrimethoxysilane, glyceryl monoglycidyl ether, polyethylene glycol monomethyl ether, and triethanolamine are, by weight, 5-7 parts of methyltrimethoxysilane, 5-6 parts of glyceryl monoglycidyl ether, 0.8-1 parts of polyethylene glycol monomethyl ether, and 0.5-0.7 parts of triethanolamine. The stirring speed is 2800rpm-320rpm, the initial temperature is 32℃-40℃, and the corresponding holding and stirring time is 15min-25min; the first reaction temperature is 55-60℃, and the corresponding holding and reaction time is 50min-80min; the second reaction temperature is 65℃-70℃, and the corresponding holding and reaction time is 60min-80min.

5. The method for preparing a stable organosilicon emulsion according to claim 1, characterized in that, In step S1, the initial heating and stirring speed is 350 rpm-450 rpm, the temperature is raised to 52℃-58℃ and held for 10 min-15 min, the biomass hydrophilic modifier is added and dispersed for 15 min-20 min, the glycerol ether modified methylsilane is added and stirred for 20 min-30 min; the pH of the system is adjusted to 4.5-5.5, and the temperature is raised to 70℃-75℃ and held for 1 h-2.5 h.

6. The method for preparing a stable organosilicon emulsion according to claim 1, characterized in that, In step S2, the aqueous phase is stirred at 1000 rpm-1200 rpm and heated to 45℃-55℃ for 20 min-30 min. The composite modified organosilicon prepolymer is added in 2-3 batches, with an interval of 10 min-15 min between each batch. After each addition, high-speed shear stirring is maintained for 15 min-20 min. After all the prepolymer is added, high-speed stirring continues for 30 min-40 min.

7. The method for preparing a stable organosilicon emulsion according to claim 1, characterized in that, The compound emulsifier is composed of anionic emulsifier and nonionic emulsifier, with a mass ratio of anionic emulsifier to nonionic emulsifier of 1:1-3. The anionic emulsifier is at least one of sodium dodecylbenzenesulfonate, sodium fatty alcohol polyoxyethylene ether sulfate, and sodium alkyl sulfonate. The nonionic emulsifier is polyoxyethylene sorbitan monooleate.

8. The method for preparing a stable organosilicon emulsion according to claim 1, characterized in that, In step S3, the stirring speed is 600 rpm-800 rpm, the temperature is raised to 85℃-90℃ and kept at that temperature for 2-3 hours; after cooling to room temperature, the solid content of the emulsion is adjusted to 30%-35%; the initiator is potassium persulfate.

9. A stable organosilicon emulsion prepared by the method of any one of claims 1-8.

10. A stable silicone emulsion according to claim 9 can be used in the textile, cosmetic, personal care product, pharmaceutical or industrial fields as a softener, lubricant, film-forming agent or stabilizer.

Images