Use of a liquid masker for the treatment of silicone rubber and method of preparation
By employing a dispensing and isolation technology and a gradient vulcanization process, combined with chitosan/sodium alginate microcapsules to encapsulate active ingredients, the shortcomings of traditional liquid silicone rubber in terms of skin care and mechanical properties have been overcome. This has enabled stable loading and controllable release of active ingredients, improving the material's adhesion and storage stability.
Patent Information
- Application Number
- CN202510467715.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-15
- Publication Date
- 2025-11-04
- Estimated Expiration
- 2045-04-15
AI Technical Summary
Traditional liquid silicone rubber lacks compatibility with skincare active ingredients in industrial applications, has insufficient mechanical properties and skin adhesion, and existing technologies pose risks of catalyst poisoning and storage stability issues for active ingredients.
Employing a separation technology (A/B glue system) and a gradient vulcanization process, skincare active ingredients are encapsulated in chitosan/sodium alginate composite microcapsules, combined with KH-560/vinyltriethoxysilane composite compatibilizer, to achieve stable loading and controllable release of skincare active ingredients. A highly elastic three-dimensional network is formed through two-stage gradient temperature vulcanization.
It achieves stable loading and controlled release of skincare active ingredients, avoids catalyst poisoning, improves the material's adhesion to the skin and storage stability, and significantly improves tensile strength and elongation at break.
Abstract
Description
TECHNICAL FIELD
[0001] The application relates to the technical field of liquid silicone rubber, in particular to application of liquid facial mask care silicone rubber and a preparation method thereof. BACKGROUND
[0002] Traditional liquid silicone rubber is mostly used in industrial fields, and lacks compatible design of skin care active ingredients in the formula, and the mechanical properties and skin adhesion are insufficient. Although the prior art (such as CN103351467A) attempts to add a tackifier, there is a risk of catalyst poisoning caused by direct contact between the platinum catalyst and the active ingredient; CN104559200B improves the mechanical properties, but does not solve the problems of skin care function integration and storage stability of the active ingredient. Therefore, a technical solution is urgently needed which can maintain the mechanical properties of silicone rubber and realize stable loading and controllable release of active ingredients. SUMMARY
[0003] The purpose of the application is to overcome the above-mentioned shortcomings, provide a preparation method of liquid facial mask care silicone rubber, realize stable loading and controllable release of skin care active ingredients in the process of forming a three-dimensional network of silicone rubber through the synergistic effect of separate packaging and isolation technology (A / B glue system) and gradient vulcanization process, and avoid catalyst poisoning problems, thereby improving the adhesion of the material to the skin.
[0004] To achieve the above-mentioned purpose, the specific scheme of the application is as follows:
[0005] The first aspect of the application provides a preparation method of liquid facial mask care silicone rubber, comprising the following steps:
[0006] (1) Base glue preparation: 50-80 parts by weight of vinyl-terminated polydimethylsiloxane, 5-15 parts by weight of modified white carbon black and 0.5-3 parts by weight of a compatibilizer are added to a kneader, and stirred at a vacuum degree of 0.05-0.1 MPa and a temperature of 120-150 DEG C for 2-4 hours;
[0007] (2) Separate packaging of A glue and B glue: the base glue obtained in step (1) is divided into two parts with equal mass; 2-5 parts by weight of hydrogen-containing silicone oil and 0.05-0.2 parts by weight of a platinum catalyst are added to one part of the base glue to form A glue containing a crosslinking agent; 0.005-0.02 parts by weight of an alkyne alcohol inhibitor and 1-5 parts by weight of a skin care active ingredient are added to the other part of the base glue to form B glue containing the active ingredient;
[0008] (3) Mixing and vulcanization: A glue and B glue are mixed in a mass ratio of 1:1, stirred at room temperature for 10-20 minutes, then injected into a mold, and vulcanized at 40-80 DEG C for 15-40 minutes, the vulcanization process including at least two temperature stages.
[0009] Preferably, the modified white carbon black in step (1) is a fumed white carbon black surface treated with hexamethyldisilazane and dimethyldiethoxysilane, with a specific surface area of 200-400 m² / g.
[0010] Preferably, the hydrogen-containing silicone oil in step (2) is a mixture of terminal hydrogen-containing polysiloxane and side hydrogen-containing polysiloxane, with a mass ratio of 1:2-4, and a hydrogen content of 0.3%-1.5%; the platinum catalyst is a chloroplatinic acid-vinylsiloxane complex, with a platinum content of 500-2000 ppm, and a mass ratio of 1:0.05-0.1 with respect to the alkyne alcohol inhibitor.
[0011] Preferably, the skin care active ingredient in step (2) is added in the form of microcapsules, and the microcapsule wall material is a complex of chitosan and sodium alginate in a mass ratio of 2:1-4:1.
[0012] The microcapsules are prepared by mixing 1-3 wt% chitosan solution with 0.5-2 wt% sodium alginate solution in a volume ratio of 1:1, crosslinking by dropwise addition of 5-10 wt% calcium chloride solution, centrifugal washing, and spray drying at an inlet temperature of 120-140°C.
[0013] Preferably, the compatibilizer in step (1) is composed of silane coupling agent KH-560 and vinyltriethoxysilane in a mass ratio of 1:1-3, and additionally 0.1-0.5 parts by weight of epoxy-modified polysiloxane is added.
[0014] Preferably, after the stirring process in step (1) is completed, the mixture is subjected to ultrasonic dispersion treatment, with an ultrasonic frequency of 40±5 kHz and a treatment time of 30-60 minutes.
[0015] Preferably, in step (2), the skin care active ingredient needs to be premixed with the compatibilizer under nitrogen protection for 10-15 minutes before the addition of B glue, with a premixing temperature of 25-40°C.
[0016] Preferably, the vulcanization process in step (3) uses gradient temperature vulcanization, specifically: the first stage is maintained at 40-50°C for 5-10 minutes to induce linear crosslinking of Si-H and vinyl groups, forming flexible segments; the second stage is maintained at 60-80°C for 15-30 minutes to promote deep reaction of side hydrogen, building a high-elasticity three-dimensional network; after vulcanization is completed, the product is aged at 25°C and a humidity of 50-70% for 24-48 hours.
[0017] Preferably, in step (3), the mixed rubber needs to be degassed under a vacuum of 0.05-0.08 MPa for 5-10 minutes before being injected into the mold for vulcanization.
[0018] The second aspect of the present application provides an application of the silicone rubber prepared by the preparation method in the field of liquid facial masks.
[0019] The present application has the following advantages: through the synergistic effect of the separate packaging and isolation technology (A / B glue system) and the gradient vulcanization process, the stable loading and controllable release of the skin care active ingredient are realized in the formation process of the three-dimensional network of the silicone rubber.
[0020] The skin care active ingredient is wrapped by chitosan / sodium alginate composite microcapsules, and the active substance is selectively released when it contacts the skin by using the pH responsiveness of the microcapsule wall material. This structure effectively isolates the direct contact between the platinum catalyst and the active ingredient, avoiding catalyst poisoning, and the barrier effect of the microcapsule significantly improves the storage stability and the reliability of the system.
[0021] Two-stage gradient temperature vulcanization is adopted, the first stage is low temperature induction of slow crosslinking of Si-H and vinyl group to form flexible chain segment, and the second stage is high temperature to promote the deep reaction of side group hydrogen to build high elasticity three-dimensional network. This process effectively balances the tensile strength and elongation at break, and significantly improves the dynamic fit of the material and the skin.
[0022] Through the synergistic effect of KH-560 / vinyl triethoxysilane composite compatibilizer and epoxy modified polysiloxane, the dispersibility of white carbon black in the silicone rubber matrix is improved. Ultrasonic treatment further breaks the white carbon black aggregate to form a nano-reinforced network, so that the tensile strength is improved. DETAILED DESCRIPTION
[0023] The present application will be further described in detail below in conjunction with specific examples, but the scope of the present application is not limited thereto.
[0024] Example 1: The preparation method of a liquid facial mask care silicone rubber described in this embodiment specifically includes the following steps:
[0025] (1) Base glue preparation: take 65 parts of ethenyl terminated polydimethylsiloxane (vinyl content 0.8%), 10 parts of white carbon black treated with hexamethyldisilazane / dimethyldiethoxysilane (3:1) (specific surface area 350 m² / g), 2 parts of KH-560 and vinyl triethoxysilane (1:2) mixed compatibilizer, 0.3 parts of epoxy modified polysiloxane, knead at 0.08 MPa and 135℃ for 3 hours, and ultrasonic treatment (40 kHz) for 45 minutes;
[0026] (2) Separate packaging treatment: after dividing the base glue, A glue is added with 3 parts of hydrogen-containing silicone oil (end group: side group = 1:3, hydrogen content 0.8%), 0.1 parts of chloroplatinic acid-vinylsiloxane complex (platinum content 1200 ppm);
[0027] The microcapsules were prepared by mixing 2 wt% chitosan acetic acid solution and 1 wt% sodium alginate solution at a volume ratio of 1:1, dropping into 8 wt% calcium chloride solution for crosslinking, and spray drying (inlet temperature 130°C) to obtain vitamin E microcapsules (chitosan / sodium alginate = 3:1), and premixing for 12 minutes (35°C) under nitrogen protection;
[0028] B glue added 0.01 parts of ethynyl cyclohexanol, 3 parts of vitamin E microcapsule (chitosan / sodium alginate = 3:1);
[0029] (3) vulcanization molding: A / B glue 1:1 mixed after vacuum degassing (0.06 MPa x 8 min), injection into the mask mold for gradient vulcanization: 45°C x 8 min→70°C x 25 min; After vulcanization, cure for 36 hours at 25°C and humidity of 60%.
[0030] Example 2: The preparation method of a liquid mask care silicone rubber described in this embodiment specifically includes the following steps:
[0031] (1) Base glue preparation: Take 75 parts of vinyl-terminated polydimethylsiloxane (vinyl content 1.2%), 8 parts of white carbon black treated with hexamethyldisilazane / dimethyldiethoxysilane (2:1) (specific surface area 280 m² / g), 1.5 parts of KH-560 and vinyltriethoxysilane (1:3) mixed compatibilizer, 0.5 parts of epoxy-modified polysiloxane, and add them to a kneader. Stir at a vacuum degree of 0.06 MPa and a temperature of 145°C for 2.5 hours, and then perform ultrasonic dispersion treatment (frequency 42 kHz, time 50 minutes).
[0032] (2) Subdivision treatment: Divide the base glue into two parts: add 4.5 parts of hydrogen-containing silicone oil (end group: side group = 1:4, hydrogen content 1.2%) to A glue, 0.15 parts of chloroplatinic acid-vinylsiloxane complex (platinum content 1800 ppm);
[0033] The microcapsules were prepared by mixing 1.5 wt% chitosan solution and 0.8 wt% sodium alginate solution at a volume ratio of 1:1, dropping into 10 wt% calcium chloride solution for crosslinking, and spray drying (inlet temperature 140°C) to obtain hyaluronic acid microcapsules (chitosan / sodium alginate = 4:1);
[0034] Add 0.015 parts of methylbutynol to B glue, and 4 parts of hyaluronic acid microcapsules (chitosan / sodium alginate = 4:1), and premix with the compatibilizer for 14 minutes (temperature 38°C) under nitrogen protection.
[0035] (3) Curing: Mix A and B at 1:1, vacuum degassing (0.07 MPa x 6 min), then inject into the mold; the curing process is divided into two stages: the first stage is 48°C x 10 min, and the second stage is 75°C x 28 min; after curing, cure at 25°C, humidity 65% for 42 hours.
[0036] Example 3: The preparation method of a liquid facial mask care silicone rubber described in this example specifically includes the following steps:
[0037] (1) Base rubber preparation: Take 50 parts of vinyl-terminated polydimethylsiloxane (vinyl content 0.5%), 13 parts of white carbon black treated with hexamethyldisilazane / dimethyldiethoxysilane (4:1) (specific surface area 380 m² / g), 3 parts of KH-560 and vinyl triethoxysilane (1:1) mixed compatibilizer, 0.2 parts of epoxy modified polysiloxane, under vacuum 0.09 MPa, temperature 125°C, stirring for 3.5 hours, ultrasonic treatment (frequency 38 kHz, time 35 minutes).
[0038] (2) Sub-packaging treatment: After the base rubber is evenly divided, it is treated as follows: 2.2 parts of hydrogen-containing silicone oil (end group: side group = 1:2, hydrogen content 0.5%) is added to A glue, 0.08 parts of chloroplatinic acid-vinylsiloxane complex (platinum content 800 ppm) is added to A glue;
[0039] The microcapsules are prepared by the following method: 3 wt% chitosan solution and 2 wt% sodium alginate solution are mixed at a volume ratio of 1:1, dropped into 5 wt% calcium chloride solution for crosslinking, and spray dried (inlet temperature 120°C) to obtain nicotinamide microcapsules (chitosan / sodium alginate = 2:1);
[0040] 0.008 parts of ethynylcyclohexanol and 2 parts of nicotinamide microcapsules (chitosan / sodium alginate = 2:1) are added to B glue, and the premixing is kept at 30°C for 10 minutes under nitrogen environment.
[0041] (3) Curing: After the mixed rubber is vacuum degassed at 0.05 MPa for 7 minutes, it is injected into the mold for gradient curing: the first stage is 43°C x 6 min, and the second stage is 68°C x 18 min; after curing, cure at 25°C, humidity 55% for 30 hours.
[0042] Example 4: The preparation method of a liquid facial mask care silicone rubber described in this example specifically includes the following steps:
[0043] (1) Base rubber preparation: Take 80 parts of end-vinyl polydimethylsiloxane (vinyl content 1.0%), 5 parts of white carbon black treated with hexamethyldisilazane / dimethyldiethoxysilane (1:1) (specific surface area 400 m² / g), 0.5 parts of KH-560 and vinyl triethoxysilane (1:3) mixed compatibilizer, 0.1 parts of epoxy modified polysiloxane, under vacuum degree 0.1 MPa, temperature 150°C, stirring for 4 hours, followed by ultrasonic treatment (frequency 45 kHz, time 60 minutes).
[0044] (2) Sub-packaging treatment: After the base rubber is evenly divided, 5 parts of hydrogen-containing silicone oil (end group: side group = 1:2.5, hydrogen content 1.5%), 0.2 parts of chloroplatinic acid-vinyl siloxane complex (platinum content 2000 ppm) are added to the A glue;
[0045] Microcapsules are prepared by the following method: mix 2.5 wt% chitosan solution with 0.7 wt% sodium alginate solution at a volume ratio of 1:1, drop into 7 wt% calcium chloride solution for crosslinking, spray drying (inlet temperature 135°C) to obtain ceramide microcapsules (chitosan / sodium alginate = 3.5:1);
[0046] 0.02 parts of diacetylene benzyl alcohol and 5 parts of ceramide microcapsules (chitosan / sodium alginate = 3.5:1) are added to the B glue and premixed under nitrogen protection at 40°C for 15 minutes.
[0047] (3) Vulcanization molding: After mixing, the rubber material is degassed at 0.08 MPa for 10 minutes, injected into the mold and subjected to two-stage vulcanization: first stage 50°C x 5 minutes, second stage 80°C x 30 minutes; After vulcanization is completed, it is cured at 25°C and humidity 70% for 48 hours.
[0048] In Examples 1 to 4, the pH responsiveness of the chitosan / sodium alginate composite microcapsules is based on the following chemical behavior:
[0049] pH sensitivity of chitosan:
[0050] Acidic environment (pH < 6.0): the amino groups (-NH2) in the chitosan molecules are protonated to form positively charged -NH3⁺, the molecular chains are relaxed due to electrostatic repulsion, and the carboxylate groups (-COO⁻) of sodium alginate are combined through ionic bonds to form stable polyelectrolyte complexes (PEC).
[0051] Neutral to alkaline environment (pH ≥ 6.0): the amino groups are deprotonated, the charge is reduced, the PEC structure is destroyed, the chitosan molecular chains are curled, the microcapsules are swollen or even dissolved, and the active ingredients are released.
[0052] Synergistic effect of sodium alginate:
[0053] Acidic condition: Carboxylate groups of sodium alginate dissociate and form ionic cross-linking network with positive charges of chitosan, which enhances the mechanical strength of microcapsules.
[0054] Basic condition: Carboxylate groups dissociate completely, sodium alginate molecular chains stretch out, which further weakens the PEC structure and accelerates the release.
[0055] Comparative Example 1: A method for preparing a liquid facial mask care silicone rubber, specifically comprising the following steps:
[0056] (1) Base rubber preparation: Take 65 parts of vinyl-terminated polydimethylsiloxane (vinyl content 0.8%), 10 parts of fumed silica treated with hexamethyldisilazane / dimethyldiethoxysilane (3:1) (specific surface area 350 m² / g), 2 parts of KH-560 and vinyltriethoxysilane (1:2) mixed compatibilizer, 0.3 parts of epoxy-modified polysiloxane, knead at 0.08 MPa and 135°C for 3 hours, and ultrasonic treatment (40 kHz) for 45 minutes.
[0057] (2) Sub-packaging treatment: After dividing the base rubber, add 3 parts of hydrogen-containing silicone oil (end group: side group = 1:3, hydrogen content 0.8%) to A rubber, and 0.1 parts of chloroplatinic acid-vinylsiloxane complex (Pt 1200 ppm); add 0.01 parts of ethynylcyclohexanol and 3 parts of liquid vitamin E (not microencapsulated) to B rubber, and pre-mix with the compatibilizer under nitrogen protection for 12 minutes (35°C).
[0058] (3) Vulcanization molding: After mixing A / B rubber at a ratio of 1:1, vacuum degassing (0.06 MPa x 8 min), inject into the facial mask mold for gradient vulcanization: 45°C x 8 min→70°C x 25 min; after vulcanization, cure at 25°C and humidity 60% for 36 hours.
[0059] Comparative Example 2: A method for preparing a liquid facial mask care silicone rubber, specifically comprising the following steps:
[0060] (1) Base rubber preparation: Take 58 parts of vinyl-terminated polydimethylsiloxane (vinyl content 0.5%), 13 parts of fumed silica treated with hexamethyldisilazane / dimethyldiethoxysilane (4:1) (specific surface area 380 m² / g), 3 parts of KH-560 and vinyltriethoxysilane (1:1) mixed compatibilizer, 0.2 parts of epoxy-modified polysiloxane, and add to a kneader. Stir at a vacuum degree of 0.09 MPa and a temperature of 125°C for 3.5 hours, and then perform ultrasonic dispersion treatment (frequency 38 kHz, time 35 minutes).
[0061] (2) Sub-packaging treatment: The base glue is evenly divided into two parts: 2.2 parts of hydrogen-containing silicone oil (end group: side group = 1:2, hydrogen content 0.5%) is added to A glue, 0.08 parts of platinum catalyst (platinum content 800 ppm); 0.008 parts of ethynylcyclohexanol and 2 parts of nicotinamide microcapsules (chitosan / sodium alginate = 2:1) are added to B glue, and the compatibilizer is premixed for 10 minutes under nitrogen protection (temperature 30°C).
[0062] (3) Vulcanization forming: After mixing A glue and B glue at a ratio of 1:1, vacuum degassing (0.05 MPa x 7 minutes); after injecting into the mask mold, it is directly placed in the constant temperature vulcanization box, and continuously vulcanized at 70°C for 33 minutes; after vulcanization is completed, it is cured at 25°C, humidity 55% for 30 hours.
[0063] The silicone rubber prepared by example 1, example 3, comparative example 1 and comparative example 2 is tested for tensile strength and elongation at break according to GB / T 528-2009 "Determination of tensile stress-strain properties of vulcanized or thermoplastic rubber", the retention rate of active ingredients is tested by high performance liquid chromatography (HPLC, C18 chromatographic column, mobile phase methanol: water = 80:20), the pH response release rate is tested by simulating the skin PH environment (medium: pH 5.5-7.0 phosphate buffer (PBS); temperature: 37±0.5°C; oscillation rate: 100 rpm; ) according to USP 724 "Dissolution Test", the stability is tested by measuring the viscosity change rate using a rotational viscometer after accelerated aging at 60°C for 7 days. The dumbbell-shaped standard test pieces (thickness 2.0±0.2mm) are respectively prepared, and the test is carried out after equilibration at 25±2°C, humidity 50±5% for 24 hours, and the results are shown in the following table:
[0064] Tensile strength (MPa) Elongation at break (%) Storage stability (viscosity change rate, 60°C x 7 days) Active ingredient retention rate (%) pH-responsive release rate (pH 6.5) Example 1 8.2±0.3 420±15 +8.5% 92.3±1.2 87.5±2.1% Example 3 7.8±0.2 380±12 +10.1% 89.7±1.5 84.6±2.0% Comparative Example 1 6.1±0.4 395±18 +28.7% 68.5±2.3 - Comparative Example 2 9.0±0.3 220±10 +15.4% 85.6±1.8 78.2±2.5%
[0065] From the above comparative test, it can be seen that the tensile strength of example 1 and example 3 is significantly higher than that of comparative example 1, but slightly lower than that of comparative example 2, and comparative example 2 adopts single-stage high temperature vulcanization, which improves the strength, but sacrifices the elongation at break. The elongation at break of example 1 and example 3 is much higher than that of comparative example 2, which shows that the gradient vulcanization process effectively balances the elasticity and rigidity of the material, that is, the gradient vulcanization process makes the material have high strength and high elasticity through step-by-step crosslinking, which is more suitable for the dynamic skin fitting requirement.
[0066] The active ingredient retention rates of Example 1 and Example 3 are significantly higher than those of Comparative Example 1 and Comparative Example 2, thereby embodying that the microcapsule wrapping effectively isolates the active ingredient from the external environment. Comparative Example 1 is not wrapped, and the active ingredient directly reacts with the silicone rubber matrix. Comparative Example 2 is wrapped with microcapsules, but the single-stage vulcanization causes damage to the microcapsule structure, and thus the chitosan / sodium alginate microcapsule is the key to improving the stability of the active ingredient.
[0067] The viscosity change rates of Example 1 and Example 3 are far lower than those of Comparative Example 1 and Comparative Example 2, that is, the barrier effect of the microcapsule reduces the plasticization of the active ingredient to the silicone rubber matrix, and the gradient vulcanization process optimizes the crosslinking network and inhibits structural relaxation at high temperatures. It can be seen that the synergistic effect of the microcapsule and the gradient vulcanization significantly improves the stability of the system.
[0068] The release rate of Example 1 and Example 3 at pH 6.5 is significantly higher than that of Comparative Example 2. Comparative Example 1 does not use microcapsule wrapping, so there is no pH-responsive release data. It is shown that the microcapsule wall material (chitosan / sodium alginate) swells at neutral pH, accelerating the release. The single-stage vulcanization of Comparative Example 2 may cause uneven particle size distribution of the microcapsule, reducing the release efficiency. Therefore, the combination of the gradient vulcanization process and the microcapsule technology realizes the efficient release of the active ingredient in the skin pH environment.
[0069] In this embodiment, the pH-responsive release mechanism is as follows:
[0070] The pH responsiveness of the chitosan / sodium alginate composite microcapsule is derived from the polyelectrolyte interaction between the two: when the environmental pH < 6.0, the chitosan amino group is protonated to form -NH3+, which is crosslinked with the -COO- of sodium alginate through ionic bonds to form a dense network structure, inhibiting the release of the active ingredient. When the pH ≥ 6.0, the amino group is deprotonated, the ionic bond is weakened, the microcapsule swells by absorbing water, the porosity increases, and the active ingredient is released by diffusion and network disintegration. The present application optimizes the release rate of the microcapsule at the skin pH (5.5-7.0) by controlling the degree of deacetylation of chitosan (≥90%) and the concentration of sodium alginate (0.5-2 wt%).
[0071] Scanning electron microscopy (SEM) can be used to observe the morphology of the microcapsule at different pH values: at pH 5.0, the microcapsule surface is smooth, and the particle size is uniform (10-20 μm); at pH 7.0, the microcapsule surface appears wrinkled, and the particle size increases to 30-40 μm, confirming the swelling behavior.
[0072] The embodiment also provides an application of the silicone rubber prepared by the preparation method in the field of liquid face masks.
[0073] The above merely describes preferred embodiments of the present application, and equivalent changes or modifications made according to the structure, features and principles described in the patent application scope of the present application are included in the protection scope of the patent application of the present application.
Claims
1. A process for the preparation of a liquid facial mask care silicone rubber, characterized in that, The method comprises the following steps: (1) Base glue preparation: 50-80 parts by weight of end-vinyl polydimethylsiloxane, 5-15 parts by weight of modified white carbon black, and 0.5-3 parts by weight of a compatibilizer are added to a kneader, and stirring is performed at a vacuum degree of 0.05-0.1 MPa and a temperature of 120-150°C for 2-4 hours; (2) A glue and B glue are separately stored: the base glue obtained in step (1) is divided into two parts of equal mass; 2-5 parts by weight of a hydrogen-containing silicone oil and 0.05-0.2 parts by weight of a platinum catalyst are added to one part of the base glue to form A glue containing a crosslinking agent; 0.005-0.02 parts by weight of an alkyne alcohol inhibitor and 1-5 parts by weight of a skin care active ingredient are added to the other part of the base glue to form B glue containing an active ingredient; (3) Mixing and vulcanization: A glue and B glue are mixed at a mass ratio of 1:1, stirred at room temperature for 10-20 minutes, and then injected into a mold, and vulcanized at 40-80°C for 15-40 minutes, the vulcanization process including at least two temperature stages; In step (1), the modified white carbon black is a fumed white carbon black treated with hexamethyldisilazane and dimethyldiethoxysilane, and has a specific surface area of 200-400 m² / g; In step (2), the hydrogen-containing silicone oil is a mixture of end-hydrogen-containing polysiloxane and side-hydrogen-containing polysiloxane at a mass ratio of 1:2-4, and has a hydrogen content of 0.3%-1.5%; the platinum catalyst is a chloroplatinic acid-vinylsiloxane complex, and has a platinum content of 500-2000 ppm, and a mass ratio of 1:0.05-0.1 with the alkyne alcohol inhibitor; In step (3), the vulcanization process adopts gradient temperature vulcanization, specifically: the first stage is kept at 40-50°C for 5-10 minutes to induce linear crosslinking of Si-H and vinyl groups to form flexible segments; the second stage is kept at 60-80°C for 15-30 minutes to promote deep reaction of side hydrogen and build a high-elasticity three-dimensional network; after the vulcanization is completed, the product is aged at 25°C and a humidity of 50-70% for 24-48 hours; In step (3), the mixed glue needs to be degassed at a vacuum degree of 0.05-0.08 MPa for 5-10 minutes before being injected into the mold for vulcanization.
2. A process for the preparation of a liquid facial mask silicone according to claim 1, characterized in that, In step (2), the skin care active ingredient is added in the form of microcapsules, and the microcapsule wall material is a complex of chitosan and sodium alginate at a mass ratio of 2:1-4:1; The microcapsules are prepared by the following method: 1-3 wt% chitosan solution and 0.5-2 wt% sodium alginate solution are mixed at a volume ratio of 1:1, 5-10 wt% calcium chloride solution is added dropwise for crosslinking, centrifugal washing is performed, and then spray drying is performed at an inlet temperature of 120-140°C.
3. A process for the preparation of a liquid facial mask silicone according to claim 1, characterized in that, In step (1), the compatibilizer is composed of silane coupling agent KH-560 and vinyl triethoxysilane at a mass ratio of 1:1-3, and additionally 0.1-0.5 parts by weight of epoxy-modified polysiloxane is added.
4. A process for the preparation of a liquid facial mask silicone according to claim 1, characterized in that, After the stirring process in step (1) is completed, the mixed material is subjected to ultrasonic dispersion treatment, the ultrasonic frequency is 40±5 kHz, and the treatment time is 30-60 minutes.
5. A process for the preparation of a liquid facial mask silicone according to claim 1, characterized in that, The skin care active ingredient in step (2) is premixed with the compatibilizer under nitrogen protection for 10-15 minutes before adding the B glue, and the premixing temperature is 25-40°C.
6. Use of a silicone rubber prepared according to the process of claim 1 in the field of liquid facial masks.
Citation Information
Patent Citations
Addition type liquid silicone rubber bonding accelerant and preparation method and application thereof
CN103351467A
A one-component addition-curable liquid silicone rubber and its preparation method
CN104559200B
Preparation method of composite microencapsulated anti-ultraviolet finishing agent
CN110063926A
Antistatic liquid silicone rubber and preparation method thereof
CN114479473A