Production and preparation method of novel silica gel elastomer material

Abstract

The invention discloses a production and preparation method of a novel silica gel elastomer material, and relates to the related field of silica gel elastomers. The novel silica gel elastomer material adopts a component A containing vinyl silicone oil and a nano silicon filler to construct a compact network structure so as to improve collapse resistance and rebound resilience, and through cooperation of polyether modified silicone oil and hydrophobic MQ resin, the anti-collapse performance and the rebound resilience of the novel silica gel elastomer material are improved. Meanwhile, modified chitosan-PLA particles and thermosensitive expansion microspheres are introduced, the material is endowed with excellent antibacterial, anti-mite and dynamic heat preservation performance, an efficient Pt catalyst, a slow-release inhibitor and a complexing and crosslinking auxiliary are introduced into the component B, the vulcanization reaction control precision and the structural stability are remarkably improved, and the mechanical property of the material is improved. A multi-stage vulcanization process is adopted in the process, shape stabilization is conducted firstly, deep vulcanization is conducted later, then stress is released, it is ensured that a spinning structure is formed completely, elasticity is stable, and a final product has the multiple excellent performance of being environmentally friendly, degradable, resistant to washing, resistant to aging, antibacterial and capable of preserving heat.

Description

Technical Field

[0001] This invention relates to the field of silicone elastomers, and more particularly to a method for producing and preparing a novel silicone elastomer material. Background Technology

[0002] Traditional elastic pillows often use polyurethane foam or latex elastomers, which, while possessing a certain degree of resilience and softness, suffer from problems such as easy aging, non-washability, poor antibacterial properties, and insufficient breathability. Furthermore, most materials are difficult to recycle, limiting their high-end applications in areas such as infant care and healthy sleep. To address these shortcomings, some companies have begun experimenting with silicone elastic materials. However, existing food-grade silicone materials are mostly homogeneous structures. For example, Chinese Patent Publication No. CN119752184A describes a slow-rebound silicone pillow and its preparation method, addressing the problems of existing slow-rebound pillows that easily produce odors, have difficulty adjusting firmness, and are prone to deformation, bacterial growth, and difficulty in cleaning and maintenance over long-term use. This pillow uses silicone as the slow-rebound material, does not produce odors, and has good pressure distribution. It has excellent ventilation, effectively relieving neck pressure, promoting blood circulation during sleep, improving sleep quality, and ensuring the durability and stability of the pillow core. It is not easily deformed or aged, and has a long service life. Adding modified organosilicon further enhances its softness, resilience, and comfort, while significantly improving its antibacterial and bacteriostatic properties, effectively inhibiting the growth of bacteria and mites, protecting the user's health. The pillowcase is removable, and the pillow core is washable and quick-drying, keeping the pillow clean. It is difficult to balance multiple functions such as elasticity, breathability, heat retention, and antibacterial properties. Moreover, it is prone to collapse and deformation during the complex shape molding process, making it impossible to form a stable appearance with a "powder-coated irregular cross structure," affecting comfort and aesthetics. In addition, conventional addition-curing vulcanization systems are extremely sensitive to temperature and time, with a narrow operating window, which can easily lead to premature vulcanization or structural instability, limiting large-scale molding and precise control. Summary of the Invention

[0003] Therefore, in order to overcome the above-mentioned shortcomings, the present invention provides a method for producing and preparing a novel silicone elastomer material.

[0004] To achieve the above objectives, the present invention adopts the following technical solution: a novel silicone elastomer material, comprising component A and component B;

[0005] Component A includes 75-85 parts of vinyl silicone oil, 6-12 parts of nano-silicone black, 3-6 parts of polyether-modified silicone oil, 3-6 parts of hydrophobic modified MQ resin, 2-5 parts of modified chitosan-PLA microparticles, 1.5-4 parts of thermosensitive hollow expansion microspheres, 0.5-2 parts of nano-silver-TiO2 composite antibacterial particles, and 0.2-0.5 parts of food-grade pearlescent pigment;

[0006] Component B includes 10 parts of methyl hydrosilicone oil + Pt catalyst mother liquor, 0.2-0.4 parts of slow-release platinum catalyst inhibitor, and 0.5-1.0 parts of cyclic silane crosslinking aid;

[0007] The specific synthesis steps for component A are as follows:

[0008] S1 Pour the vinyl silicone oil into the vacuum mixing vessel and start low-speed mixing;

[0009] S2 is gradually added to nano-silica, and high-shear emulsification dispersion is initiated for 7-9 minutes;

[0010] Add S3 to polyether-modified silicone oil and stir for 2-4 minutes to form a hydrophilic basic network;

[0011] Add S4 to hydrophobically modified MQ silicone resin and continue stirring for 4-6 minutes to improve molding strength;

[0012] S5 speed reduced to 150 rpm, modified chitosan-PLA microparticles and thermosensitive hollow expansion microspheres were added sequentially;

[0013] S6 is slowly mixed with nano-silver-TiO2 composite antibacterial particles while the temperature is controlled at ≤40℃.

[0014] Finally, food-grade pearlescent pigments are added to S7 for color adjustment, forming a complete component A system;

[0015] S8 performs a vacuum degassing process at a pressure of -0.08 MPa for 5 minutes to remove large air bubbles.

[0016] The specific synthesis steps for component B are as follows:

[0017] a. Pour the methyl hydrosilicone oil + Pt catalyst mother liquor into a clean container;

[0018] b. Add a sustained-release platinum catalytic inhibitor and stir slowly until homogeneous;

[0019] c. Add cyclic silane crosslinking aids to improve the efficiency of three-dimensional network crosslinking.

[0020] Preferably, the structure of the methylhydrosilicone oil + Pt catalyst mother liquor is: 95 parts of methylhydrosilicone oil and 2 parts of platinum catalyst, wherein the methylhydrosilicone oil contains about 0.8-1.2% Si–H and has a viscosity of 20-50 cSt, and the platinum catalyst has a platinum content of 1000-3000 ppm.

[0021] The production and preparation method of the novel silicone elastomer material, with specific preparation steps as follows:

[0022] ① Mix according to A:B = 10:1;

[0023] ② Mix for 3 minutes using a static mixer or a low-speed mechanical mixer;

[0024] ③ Perform pulsed vacuum degassing: Set the pumping time to 10 seconds → depressurize for 3 seconds → pump again for 10 seconds, repeat 3 to 4 times to remove microbubbles and prevent thermal particles from bursting.

[0025] ④ Place the degassed mixture into the screw pressurized feeding tank;

[0026] ⑤ The filaments are spun through a variable-diameter spiral nozzle in a cold water tank at a water temperature of 10℃;

[0027] ⑥ The nozzle movement trajectory is controlled by a six-axis servo system to simulate the following three-dimensional motion: X-axis horizontal sweep ±50mm, Y-axis forward and backward ±30mm, Z-axis vertical ±20mm, while the nozzle rotates 1 revolution per second.

[0028] ⑦ Electrolytic microbubbles are introduced into the bottom of the water tank, forming a bubble flow of 1μm to 10μm, which improves surface texture and molding adhesion;

[0029] ⑧ The molding and deposition time is 15-30 minutes per pillow core volume;

[0030] ⑨ Use a zoned temperature-controlled oven or tunnel furnace for step-by-step vulcanization. First stage: temperature 55-60℃, time 30min; Second stage: temperature 80-90℃, time 90min; Third stage: temperature 50℃, time 30min.

[0031] ⑩ Finally, use an ultrasonic cutting tool to cut and shape the pillow outline, and seal the edges to prevent fraying.

[0032] The beneficial effects of this invention are:

[0033] By employing food-grade silicone elastomer component A, which contains vinyl silicone oil, nano-silicone filler, and modified components, the mechanical properties are significantly improved: the nano-silicone filler forms a denser network structure in the vinyl silicone oil, enhancing the material's resistance to collapse, support, and compression rebound rate; the surface is controlled to be both hydrophilic and hydrophobic: the introduction of polyether-modified silicone oil and hydrophobic MQ resin enables the material to possess both washability and aging resistance, supporting long-term repeated cleaning and outdoor use; natural antibacterial and environmentally friendly functions are integrated: the combination of modified chitosan-PLA microparticles and thermosensitive microbubbles balances antibacterial and anti-mite properties with dynamic heat insulation, while achieving the ecological advantages of biodegradability and recyclability; the stability of irregular molding is enhanced: the internal viscoelasticity of the components is enhanced, which helps maintain the shape of the spinneret interlaced structure, ensuring that the finished product has a stable appearance and a powder-coated texture;

[0034] By employing a food-grade silicone elastomer B component containing a high-efficiency Pt catalyst, a sustained-release inhibitor, and a complexing agent, the reaction control precision and safety are improved: the sustained-release inhibitor effectively extends the operating window, prevents premature vulcanization, and enhances the controllability of material processing; crosslinking efficiency and stability are improved: the addition of a multi-toothed complexing crosslinking agent can construct a more stable three-dimensional crosslinking network, resulting in better overall structural strength and durability of the material; and the finished product is made more environmentally friendly and has low migration: the carefully selected platinum-based food-grade catalyst system exhibits extremely low migration rate under high-temperature aging, making it more suitable for skin-friendly and infant-grade products;

[0035] The process employs multi-stage vulcanization control to prevent thermal runaway and structural collapse: the initial vulcanization stage gently treats and locks the three-dimensional spinneret structure, effectively preventing deformation or adhesion collapse during the molding stage; it enhances elasticity and recovery performance: the main vulcanization stage achieves deep cross-linking within the optimal temperature range, improving material elasticity, fatigue resistance, and compression recovery rate; it releases residual stress and activates functional fillers: the final vulcanization stage promotes the expansion of heat-sensitive foam particles to form insulating cavities, while releasing the stress from the previous heat treatment, resulting in lower product deformation rate and longer service life; and it adapts to complex-shaped products: multi-stage vulcanization adapts to the molding of "powder-coated irregular cross-structures," ensuring structural uniformity and texture integrity, and improving appearance and comfort. Attached Figure Description

[0036] Figure 1 This is a schematic diagram of the pillow molded from the novel silicone elastomer material of the present invention. Detailed Implementation

[0037] To further explain the technical solution of the present invention, a detailed description is provided below through specific embodiments.

[0038] Table 1: Components and weight percentages of the novel silicone elastomer material;

[0039]

[0040]

[0041] Example 1

[0042] The raw materials were weighed according to the components and their weight percentages of the novel silicone elastomer material in Example 1 of Table 1. The specific synthesis steps for component A are as follows:

[0043] S1 Pour vinyl silicone oil into a vacuum mixing vessel and start low-speed stirring; S2 Gradually add nano-silica and start high-shear emulsification dispersion for 8 minutes; S3 Add polyether-modified silicone oil and stir for 3 minutes to form a hydrophilic basic network; S4 Add hydrophobic modified MQ silicone resin and continue stirring for 5 minutes to improve molding strength; S5 Reduce the speed to 150 rpm and add modified chitosan-PLA microparticles and thermosensitive hollow expansion microspheres in sequence; S6 Add nano-silver-TiO2 composite antibacterial particles and mix slowly while controlling the temperature at ≤40℃; S7 Finally, add food-grade pearlescent pigment for color adjustment to form a complete component A system; S8 Perform a vacuum degassing process at a pressure of -0.08 MPa for 5 minutes to remove large air bubbles;

[0044] The specific synthesis steps for component B are as follows:

[0045] a. Pour the methylhydrosilicone oil + Pt catalyst mother liquor into a clean container; b. Add a slow-release platinum catalyst inhibitor and stir slowly until homogeneous; c. Add a cyclic silane crosslinking aid to improve the efficiency of three-dimensional network crosslinking;

[0046] The structure of the methyl hydrosilicone oil + Pt catalyst mother liquor is: 95 parts of methyl hydrosilicone oil and 2 parts of platinum catalyst. The methyl hydrosilicone oil contains about 1% Si–H and has a viscosity of 35 cSt. The platinum catalyst has a platinum content of 2000 ppm.

[0047] The specific preparation steps for a novel silicone elastomer material are as follows:

[0048] ① Mix A:B = 10:1; ② Mix for 3 minutes using a static mixer or a low-speed mechanical mixer;

[0049] ③ Perform pulsed vacuum degassing: Set the pumping time to 10 seconds → depressurize for 3 seconds → pump again for 10 seconds, repeat 3-4 times to remove microbubbles and prevent the bursting of heat-sensitive particles; ④ Place the degassed mixture into the screw pressurized feeding tank; ⑤ Spin the mixture through a variable diameter spiral nozzle in a cold water tank at a water temperature of 10℃; ⑥ Control the nozzle movement trajectory using a six-axis servo system to simulate the following three-dimensional motion: X-axis horizontal sweep (±50mm), Y-axis forward and backward movement (±30mm), Z-axis vertical movement (±20mm), while simultaneously superimposing nozzle rotation (1 revolution per second); ⑦ Introduce electrolysis at the bottom of the water tank. Microbubbles, with a flow of 1μm to 10μm, enhance surface texture and molding adhesion; ⑧ Molding deposition time is 20 minutes per pillow core volume; ⑨ Step-by-step vulcanization is performed using a zoned temperature-controlled oven or tunnel furnace: First stage: temperature 60℃, time 30min; Second stage: temperature 85℃, time 90min; Third stage: temperature 50℃, time 30min. The multi-stage vulcanization process control record is shown in Table 2; ⑩ Finally, the pillow outline is cut and shaped using an ultrasonic cutting tool, and the edges are sealed to prevent fraying. The finished pillow is shown in the attached diagram. Figure 1 .

[0050] Table 2: Multi-stage vulcanization process control records

[0051]

[0052] Example 2

[0053] The raw materials were weighed according to the components and their weight percentages of the novel silicone elastomer material in Example 2 of Table 1, and the specific preparation method was the same as in Example 1.

[0054] Comparative Example 1

[0055] The raw materials were weighed according to the components and their weight percentages of the novel silicone elastomer material in Comparative Example 1 in Table 1, and the specific preparation method was a conventional preparation method in this field.

[0056] The comparison and summary are as follows:

[0057] Example 1:

[0058] This formula is a full-function design, using vinyl silicone oil as the main chain substrate, combined with highly dispersed nano-silica and hydrophobic MQ resin to construct a highly elastic support network. Modified chitosan-PLA microparticles and nano-silver-TiO2 composite particles are introduced to give the material excellent antibacterial, anti-mite, and anti-mildew properties. Meanwhile, hollow thermosensitive expansion microspheres effectively improve heat retention. Slow-release catalysts and cyclic silanes are used to achieve multi-stage deep vulcanization, improving the structural stability and lasting elasticity of the product. Performance characteristics: rebound rate >90%, antibacterial rate >99%, significantly enhanced thermal sensitivity, regular appearance, water-resistant and aging-resistant. Applications: high-end health pillows, baby products, functional bedding, breathable cushions.

[0059] Example 2:

[0060] The dosage of key functional components such as fillers, antibacterial particles, and hollow microspheres has been reduced, and some visual auxiliary components have not been added to control costs. Although there is a slight decrease in performance, it still maintains good elasticity, a certain degree of antibacterial and heat-insulating ability, and maintains the powder-coated texture structure. Performance characteristics: rebound rate of about 85%, good antibacterial effect, improved heat sensation, and balanced structure. Applicable fields: mass-market elastic pillows, home cushions, and general mid-range products.

[0061] Comparative Example 1:

[0062] As a control group, the basic silicone elastic network was retained, but no antibacterial particles, thermal insulation structure, or particulate functional components were included. The test results showed that its structure was prone to collapse, its elasticity retention rate was low, and its risk of bacterial and mite growth was high, which could not meet the needs of functional pillow products. Performance characteristics: low resilience <70%, no thermal insulation and antibacterial function, and the structural texture is prone to collapse.

[0063] Table 3: Test Report for Silicone Elastomer Materials;

[0064]

[0065] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A novel silicone elastomer material, characterized in that: Includes component A and component B; Component A includes 75-85 parts of vinyl silicone oil, 6-12 parts of nano-silicone black, 3-6 parts of polyether-modified silicone oil, 3-6 parts of hydrophobic modified MQ resin, 2-5 parts of modified chitosan-PLA microparticles, 1.5-4 parts of thermosensitive hollow expansion microspheres, 0.5-2 parts of nano-silver-TiO2 composite antibacterial particles, and 0.2-0.5 parts of food-grade pearlescent pigment; Component B includes 10 parts of methyl hydrosilicone oil + Pt catalyst mother liquor, 0.2-0.4 parts of slow-release platinum catalyst inhibitor, and 0.5-1.0 parts of cyclic silane crosslinking aid; The specific synthesis steps for component A are as follows: S1 Pour the vinyl silicone oil into the vacuum mixing vessel and start low-speed mixing; S2 is gradually added to nano-silica, and high-shear emulsification dispersion is initiated for 7-9 minutes; Add S3 to polyether-modified silicone oil and stir for 2-4 minutes to form a hydrophilic basic network; Add S4 to hydrophobically modified MQ silicone resin and continue stirring for 4-6 minutes to improve molding strength; S5 speed reduced to 150 rpm, modified chitosan-PLA microparticles and thermosensitive hollow expansion microspheres were added sequentially; S6 is slowly mixed with nano-silver-TiO2 composite antibacterial particles while the temperature is controlled at ≤40℃. Finally, food-grade pearlescent pigments are added to S7 for color adjustment, forming a complete component A system; S8 performs a vacuum degassing process at a pressure of -0.08 MPa for 5 minutes to remove large air bubbles. The specific synthesis steps for component B are as follows: a. Pour the methyl hydrosilicone oil + Pt catalyst mother liquor into a clean container; b. Add a sustained-release platinum catalytic inhibitor and stir slowly until homogeneous; c. Add cyclic silane crosslinking aids to improve the efficiency of three-dimensional network crosslinking.

2. The novel silicone elastomer material according to claim 1, characterized in that: The structure of the methylhydrosilicone oil + Pt catalyst mother liquor is: 95 parts methylhydrosilicone oil and 2 parts platinum catalyst. The methylhydrosilicone oil contains about 0.8-1.2% Si–H and has a viscosity of 20-50 cSt. The platinum catalyst has a platinum content of 1000-3000 ppm.

3. A method for producing and preparing a novel silicone elastomer material, used to prepare the novel silicone elastomer material as described in claim 1, characterized in that: The specific preparation steps are as follows: ① Mix according to A:B = 10:1; ② Mix for 3 minutes using a static mixer or a low-speed mechanical mixer; ③ Perform pulsed vacuum degassing: Set the pumping time to 10 seconds → depressurize for 3 seconds → pump again for 10 seconds, repeat 3 to 4 times to remove microbubbles and prevent thermal particles from bursting. ④ Place the degassed mixture into the screw pressurized feeding tank; ⑤ The filaments are spun through a variable-diameter spiral nozzle in a cold water tank at a water temperature of 10℃; ⑥ The nozzle movement trajectory is controlled by a six-axis servo system to simulate the following three-dimensional motion: X-axis horizontal sweep ±50mm, Y-axis forward and backward ±30mm, Z-axis vertical ±20mm, while the nozzle rotation is superimposed at 1 revolution per second. ⑦ Electrolytic microbubbles are introduced into the bottom of the water tank, forming a bubble flow of 1μm to 10μm; ⑧ The molding and deposition time is 15-30 minutes per pillow core volume; ⑨ Use a zoned temperature-controlled oven or tunnel furnace for step-by-step vulcanization. The first stage: temperature is 55-60℃, time is 30min. Second segment: temperature 80-90℃, time 90min; Third segment: temperature 50℃, time 30min; ⑩ Finally, use an ultrasonic cutting tool to cut and shape the pillow outline, and seal the edges to prevent fraying.

Images