Silicone rubber foam material as well as preparation method and application thereof
By using modified base glue and activators A and B in silicone rubber foam materials, the problems of uneven bubble cells and insufficient waterproofness are solved, and the silicone rubber foam materials with high resilience and waterproofness are achieved, which meets the needs of the The sealing and buffering requirements of new energy battery cells ensure the safe and reliable operation of the battery.
Patent Information
- Application Number
- CN202411528668.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-30
- Publication Date
- 2025-01-07
AI Technical Summary
The existing silicon foam materials have problems such as uneven cell cells, poor resilience and low waterproofness in the field of new energy storage, making it difficult to ensure the safe and reliable long-term operation of the battery.
Modified base glue and specific activators A and B are formulated in silicone rubber foam materials. Through stirring and foaming processes, uniform and highly resilient silicone rubber foam materials are formed to improve their cross-linking density and waterproof properties. .
It realizes silicone rubber foam material with uniform bubble cells, excellent compression elasticity and high waterproofness, which meets the sealing and buffering needs of new energy battery cells and ensures the safe and reliable operation of the battery.
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Figure BDA0005109929270000161
Abstract
Description
Technical Field
[0001] The present invention relates to the field of energy storage technology, and in particular to a silicone rubber foam material and a preparation method and application thereof. Background Art
[0002] Green travel has been a hot topic in recent years. As new energy continues to break through technical difficulties and battery energy density continues to increase, timely and effective maintenance of the internal structure of battery cells, environmental stability control, and ensuring the normal operation of equipment are issues that need to be focused on. However, how to ensure the safe and reliable operation of batteries has always been a pain point in the development of the industry.
[0003] Silicone foam has excellent resilience and anti-aging properties and is widely used in many fields. With the development of new energy, the application of silicone foam has been further expanded. Silicone foam sealing materials mainly play the role of sealing and buffering in battery cells. The density of its network structure is an important indicator for judging the sealing and buffering performance of the foam. However, the foam products currently used for new energy storage on the market generally have poor product stability, inconsistent foam pore uniformity, poor resilience, and low sealing and waterproof grades. They cannot meet the use requirements of new energy battery cells and it is difficult to ensure the safe and reliable operation of the battery for a long time.
[0004] Therefore, there is an urgent need to develop a silicone foam material with uniform pores, high resilience and strong waterproofness to ensure that it can maintain safe and reliable operation of batteries for a long time in the new energy storage industry. Summary of the invention
[0005] In view of the defects in the prior art, the present invention provides a silicone rubber foam material and a preparation method and application thereof.
[0006] The present invention provides a silicone rubber foam material, which comprises the following components in parts by weight:
[0007] A glue: vinyl silicone oil 30-35 parts, such as 30, 31, 32, 33, 34, 35 parts, modified base glue 15-25 parts, such as 15, 16, 18, 20, 22, 24, 25 parts, activator A 0.5-2 parts, such as 0.5, 1, 1.5, 2 parts, activator B 0.05-0.25 parts, such as 0.05, 0.1, 0.15, 0.2, 0.25 parts, flame retardant 10-25 parts, such as 10, 15, 20, 25 parts, structure control agent 6-7 parts, such as 6, 6.5, 7 parts, platinum catalyst 1-3 parts, such as 1, 2, 3 parts;
[0008] B glue: vinyl silicone oil 30-35 parts, such as 30, 31, 32, 33, 34, 35 parts, modified base glue 15-25 parts, such as 15, 16, 18, 20, 22, 24, 25 parts, activator A 0.5-2 parts, such as 0.5, 1, 1.5, 2 parts, activator B 0.05-0.25 parts, such as 0.05, 0.1, 0.15, 0.2, 0.25 parts, flame retardant 10-25 parts, such as 10, 15, 20, 25 parts, structure control agent 6-7 parts, such as 6, 6.5, 7 parts, hydrogen-containing silicone oil 1-2 parts, such as 1, 1.5, 2 parts, inhibitor 0.06-0.10 parts, such as 0.06, 0.07, 0.08, 0.09, 0.10 parts, color paste 0.10-0.20 parts, such as 0.10, 0.12, 0.14, 0.16, 0.18, 0.20 parts;
[0009] The vinyl silicone oil in the A and B glues is any one or more of double-terminal vinyl silicone oil, single-terminal vinyl silicone oil, and end-side vinyl silicone oil, with a viscosity of 2000-20000cps and a vinyl content of 0.10-0.26wt%, such as 0.10wt%, 0.15wt%, 0.20wt%, 0.22wt%, 0.24wt%, and 0.26wt%;
[0010] The mass ratio of the A glue to the B glue is 1: (0.9-1.1). If the amount of the A glue added is too little, the foaming time will increase and thus affect the production efficiency, and it will also cause problems such as uneven foaming holes. If the amount of the B material added is too little, it will also cause uneven foaming. The modified base glue comprises the following components by weight: 68-72 parts of vinyl silicone oil, 3-6 parts of diphenylsilanediol, 28-32 parts of silicon dioxide, and 0.5-0.8 parts of a coupling agent; wherein the vinyl silicone oil is a double-terminated The vinyl silicone oil has a viscosity of 2000cps, 5000cps or both. The double-end vinyl silicone oil has a good crosslinking density and is more conducive to the formation of foaming than the single-end vinyl silicone oil or the polyvinyl silicone oil. The inventors also found that in the system of the present invention, if the vinyl silicone oil in the modified base rubber is a single-end vinyl silicone oil, the foam cells of the foam product will be uneven. The silicon dioxide is any one of fumed silicon dioxide or precipitated silicon dioxide, with a specific surface area of 200m 2 / g or more; the coupling agent is preferably a silane coupling agent, and adding diphenylsilanediol to the base rubber can also control the compression rebound of the foam within a better range.
[0011] By modifying the base rubber and adding modified base rubber, activator A and activator B to the A and B rubber components, the silicone rubber foam material can achieve uniform pores, high resilience and high waterproof performance. The modified base rubber mainly improves the compression resilience of the foam product and maintains a good compression permanent deformation. In this system, adding special activators A and B can activate the overall performance of the rubber, reduce the viscosity of the rubber, and lubricate it, so that the reaction can react quickly under certain conditions, thereby reducing other side reactions. At the same time, the specific activator can also activate the surface energy of silica, making it easier to form cross-linking points during foaming and forming a dense structure. The mutual coordination of each component greatly improves the activity of the mixed rubber, increases the base points of foaming cross-linking, and improves the cross-linking degree of the foam, ultimately achieving the purpose of improving the uniformity and resilience of the foam, so that the material can quickly foam at a suitable temperature to form a uniform and highly dense foam product.
[0012] Furthermore, the activator A is one or more of zinc oxide, magnesium oxide, zinc stearate, and calcium stearate, preferably in micrometer or nanometer level.
[0013] Furthermore, the activator B is any one or more of alcohols, amines, and alkanes, including but not limited to any one of anhydrous ethanol, alkane white oil, triethanolamine, and the like.
[0014] Furthermore, the flame retardant is selected from one or more of magnesium hydroxide, aluminum hydroxide, talcum powder, clay, and calcium carbonate, and has a particle size of 50 nm-10 μm.
[0015] Furthermore, the structure control agent is hydroxy silicone oil, preferably with a hydroxy content of more than 3%.
[0016] Furthermore, the inhibitor is one or more of 1-ethynylcyclohexanol, 2-methyl-3-butyn-2-ol and 3,5-dimethyl-1-hexyn-3-ol.
[0017] Furthermore, the hydrogen-containing silicone oil is selected from one or more of hydrogen-containing silicone oils having a hydrogen content of 0.75wt%, 1.2wt%, and 1.6wt%. If the hydrogen content is too low, uneven foaming will result.
[0018] Furthermore, the melting point of the diphenylsilanediol is 132°C-155°C.
[0019] Furthermore, the platinum catalyst is preferably a 3000 PPM chloroplatinic acid catalyst.
[0020] Furthermore, the preparation method of the modified rubber base comprises the following steps:
[0021] S1. Take 68-72 parts of vinyl silicone oil and 3-6 parts of diphenylsilanediol and stir them at 160-170°C, then add 28-32 parts of silica powder in 2-3 times, and then stir at a speed of 30-45r / min for 30-60min to mix the rubber evenly, and let it cool;
[0022] S2. Add 0.5-0.8 parts of silane coupling agent to the cooled rubber material, raise the temperature to 105-125°C, stir at a speed of 30-45r / min for 30-60min to mix evenly, and obtain the modified base rubber after cooling.
[0023] The present invention also provides a method for preparing the silicone rubber foam material, comprising the following steps:
[0024] S1. Weigh each component according to the formula ratio of A and B glue and mix them evenly at room temperature to obtain A glue and B glue;
[0025] S2. The rubber materials A and B are conveyed to the mixing and stirring head in proportion through the feeding system and mixed evenly to obtain a mixed rubber material;
[0026] S3. The mixed rubber material is calendered, foamed, de-filmed and rolled to obtain a sulfurized silicone rubber foam material;
[0027] S4. The silicone rubber foam material after sulfurization is baked and matured at high temperature to obtain the silicone rubber foam material;
[0028] Wherein, in step S1, both glue A and glue B are stirred in a dynamic mixer at a temperature of 20-40° C. at a speed of 30-45 r / min for 60-90 min to obtain;
[0029] When preparing rubber materials A and B, the temperature is effectively controlled. At the same time, a specific rotation speed and stirring time are used to mix the various components in rubber materials A and B evenly. At the same time, side reactions of the rubber materials caused by excessive stirring speed and time during processing, or the accelerated volatilization of the inhibitor due to increased temperature, can be avoided.
[0030] In step S2, the rubber materials A and B are mixed uniformly under high-speed stirring of a stirring blade at 800-1000 r / min.
[0031] The present invention also provides the application of the silicone rubber foam material as a sealing and buffering material, especially as a sealing and buffering material for new energy battery cells.
[0032] In summary, compared with the prior art, the present invention achieves the following technical effects:
[0033] (1) The pores of the silicone rubber foam material provided by the present invention are small and uniform;
[0034] (2) The silicone rubber foam material provided by the present invention has excellent compression resilience;
[0035] (3) The silicone rubber foam material provided by the present invention has high waterproofness;
[0036] (4) The silicone rubber foam material formula provided by the present invention has relatively low raw material prices, a simple preparation process, no side reactions during the production process, and no waste gas is generated, which has the advantages of being environmentally friendly and safe. DETAILED DESCRIPTION
[0037] In order to enable those skilled in the art to better understand the solutions of the present invention, the technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only embodiments of a part of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work should fall within the scope of protection of the present invention.
[0038] Example
[0039] The present invention is further described below in conjunction with specific examples and comparative examples. The following specific examples are all preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the following examples, and are particularly not limited to the types of the various component raw materials used in the following specific examples.
[0040] 1. The sources of raw materials for the embodiments and comparative examples are as follows:
[0041] Unless otherwise specified, the raw materials used in the examples and comparative examples of the present invention are commercially available.
[0042] 2. Various performance test methods
[0043] (1) Appearance test: Through visual inspection, the number of obvious large holes in the cross section of a sample with a thickness of 10 mm and a length of 10 cm is required to be less than 3;
[0044] (2) Compression set test: The test is conducted in accordance with GB / T 7759.1-2015 "Determination of compression set of vulcanized rubber or thermoplastic rubber", and the compression set of a 5.0 mm thick silicone rubber foam sample at 150°C is tested;
[0045] (3) Test of vacuum water absorption rate: weigh the silicone rubber foam sample to obtain m1, then immerse it in distilled water 50 mm below the surface, and reduce the water surface pressure to (-85) KPa for 3 minutes, then release the vacuum, leave the sample in distilled water for 3 minutes, take it out, wipe off the surface water and weigh it to obtain m2, then calculate the mass increase percentage, the calculation formula is [(m2-m1) / m1]×100%;
[0046] (4) Sealing and waterproofing test: According to GB / T 4208-2017 enclosure protection grade (IP code) test, the test sample is immersed in water at a depth of 2 meters and the waterproof performance is measured after 48 hours.
[0047] Example 1
[0048] The silicone rubber foam material provided in this embodiment is prepared as follows:
[0049] S1. Preparation of glue A: 30 parts of vinyl silicone oil, 25 parts of modified base glue, 0.5 parts of activator A, 0.05 parts of activator B, 25 parts of flame retardant, 6 parts of structure control agent, and 1 part of platinum catalyst were weighed and put into a power mixer, the temperature was controlled at 20-40°C, the stirring speed was set to 30-40r / min, the stirring time was 60-90min, and after stirring evenly, it was taken out for use;
[0050] Preparation of B glue: weigh 30 parts of vinyl silicone oil, 25 parts of modified base glue, 0.5 parts of activator A, 0.05 parts of activator B, 25 parts of flame retardant, 6 parts of structure control agent, 1 part of hydrogenated silicone oil, 0.06 parts of inhibitor, and 0.1 parts of color paste according to mass parts, put them into a power mixer, control the temperature at 20-40°C, set the stirring speed to 30-40r / min, and stir for 60-90min. After stirring evenly, take out for use;
[0051] Among them, the vinyl silicone oil used in A and B glue is double-ended vinyl silicone oil, the viscosity is 20000cps, and the vinyl content is 0.12wt%; the activator A is zinc oxide, and the particle size is 2-5μm; the activator B is anhydrous ethanol; the flame retardant is a mixed flame retardant of magnesium hydroxide and aluminum hydroxide, and the particle size is 2-10μm, and the structure control agent is hydroxyl silicone oil, and the hydroxyl content is 4%; the platinum catalyst is 3000PPM chloroplatinic acid catalyst; the hydrogen content of the hydrogen-containing silicone oil is 1.6wt%; the inhibitor is 1-ethynyl cyclohexanol; the color paste is: a color paste in the 39 series provided by Guangzhou Hongyu Technology Candle Paint Co., Ltd., and the color is not limited;
[0052] S2. The rubber material A and rubber material B produced in step S1 are poured into the material cylinders A and B of the feeding system respectively, and the rubber materials A and B are delivered to the mixing and stirring head at a mass ratio of 1:1 through the feeding system, and the stirring speed is set to 1000r / min, and the rubber materials A and B are stirred evenly, and then ejected from the glue outlet;
[0053] S3. coating the mixed rubber material sprayed out in step S2 on the PET film, and then compounding a layer of PET film on the upper surface through a calender to form a slurry layer of a certain thickness, and heating and foaming through a tunnel furnace, the foaming temperature is gradually increased from 120°C to 160°C in a gradient with a temperature difference of 10°C, each section is 4 meters long, and a total of five sections are foamed. After the foaming is completed, the upper and lower PET films are peeled off, and the silicone rubber foam after sulfurization is obtained by winding;
[0054] S4. The silicone rubber foam obtained in S3 was baked at high temperature in a disulfide baking furnace for 30 min, and the silicone rubber foam material was obtained by winding;
[0055] The modified base rubbers are all homemade, and the preparation method is as follows:
[0056] S1. Weigh 70 parts of vinyl silicone oil and 3 parts of diphenylsilanediol by mass and stir them evenly at 160-170°C, then add 30 parts of silica powder in 2-3 times, and then stir at a speed of 30-45r / min for 30-60min to mix the rubber evenly and let it cool;
[0057] S2. Add 0.5 parts of a silane coupling agent to the cooled rubber, raise the temperature to 120°C, stir at a speed of 30-45r / min for 30-60min to mix evenly, and after cooling, obtain the modified rubber base;
[0058] The viscosity of vinyl silicone oil is 2000cps; the specific surface area of fumed silica is 200m 2 / g; the silane coupling agent is silane coupling agent KH560.
[0059] Example 2
[0060] The silicone rubber foam material provided in this embodiment is different from that in Embodiment 1 only in the step S1 of material preparation:
[0061] S1. Preparation of glue A: 30 parts of vinyl silicone oil, 15 parts of modified base glue, 0.5 parts of activator A, 0.05 parts of activator B, 25 parts of flame retardant, 6 parts of structure control agent, and 1 part of platinum catalyst were weighed and put into a power mixer, the temperature was controlled at 20-40°C, the stirring speed was set to 30-40r / min, the stirring time was 60-90min, and after stirring evenly, it was taken out for use;
[0062] Preparation of B glue: weigh 30 parts of vinyl silicone oil, 15 parts of modified base glue, 0.5 parts of activator A, 0.05 parts of activator B, 25 parts of flame retardant, 6 parts of structure control agent, 1 part of hydrogenated silicone oil, 0.06 parts of inhibitor, and 0.1 parts of color paste according to mass parts, put them into a power mixer, control the temperature at 20-40°C, set the stirring speed to 30-40r / min, and stir for 60-90min. After stirring evenly, take out for use;
[0063] Among them, the vinyl silicone oil used in A and B glues is a double-ended vinyl silicone oil with a viscosity of 2000cps and a vinyl content of 0.22wt%; the activator A is magnesium oxide with a particle size of 2-5μm; the activator B is alkane white oil; the flame retardant is a mixed flame retardant of magnesium hydroxide and aluminum hydroxide with a particle size of 2-10μm; the structure control agent is hydroxyl silicone oil with a hydroxyl content of 4%; the platinum catalyst is a 3000PPM chloroplatinic acid catalyst; the hydrogen content of the hydrogen-containing silicone oil is 1.6wt%; the inhibitor is 1-ethynylcyclohexanol; the color paste is: a color paste in the 39 series provided by Guangzhou Hongyu Craft Candle Paint Co., Ltd., and the color is not restricted.
[0064] Example 3
[0065] The silicone rubber foam material provided in this embodiment is different from that in Embodiment 1 only in the steps S1 and S2 of material preparation and the preparation method of the modified base rubber:
[0066] S1. Prepare glue A: weigh 30 parts of vinyl silicone oil, 15 parts of modified base glue, 2 parts of activator A, 0.25 parts of activator B, 25 parts of flame retardant, 6 parts of structure control agent, and 1 part of platinum catalyst into a power mixer, control the temperature at 20-40°C, set the stirring speed to 30-40r / min, and stir for 60-90min. Stir evenly and take out for use;
[0067] Preparation of B glue: weigh 30 parts of vinyl silicone oil, 15 parts of modified base glue, 2 parts of activator A, 0.25 parts of activator B, 25 parts of flame retardant, 6 parts of structure control agent, 1 part of hydrogenated silicone oil, 0.06 parts of inhibitor, and 0.1 parts of color paste according to mass parts, put them into a power mixer, control the temperature at 20-40°C, set the stirring speed to 30-40r / min, and stir for 60-90min. After stirring evenly, take out for use;
[0068] Among them, the vinyl silicone oil used in A and B glue is double-ended vinyl silicone oil, with a viscosity of 5000cps and a vinyl content of 0.18wt%; the activator A is zinc stearate with a particle size of 2-5μm; the activator B is triethanolamine; the flame retardant is a mixed flame retardant of magnesium hydroxide and aluminum hydroxide with a particle size of 2-10μm; the structure control agent is hydroxyl silicone oil with a hydroxyl content of 9%; the platinum catalyst is a 3000PPM chloroplatinic acid catalyst; the hydrogen content of the hydrogen-containing silicone oil is 1.6wt%; the inhibitor is 1-ethynylcyclohexanol; the color paste is: a color paste in the 39 series provided by Guangzhou Hongyu Technology Candle Paint Co., Ltd., and the color is not limited;
[0069] S2. The rubber material A and rubber material B produced in step S1 are poured into the material cylinders A and B of the feeding system respectively, and the rubber materials A and B are delivered to the mixing and stirring head at a mass ratio of 1:1 through the feeding system, and the stirring speed is set to 800r / min, and the rubber materials A and B are stirred evenly, and then ejected from the glue outlet;
[0070] The modified base rubbers are all homemade, and the preparation method is as follows:
[0071] S1. Weigh 70 parts of vinyl silicone oil and 3 parts of diphenylsilanediol by mass and stir them evenly at 160-170°C, then add 30 parts of silica powder in 2-3 times, and then stir at a speed of 30-45r / min for 30-60min to mix the rubber evenly and let it cool;
[0072] S2. Add 0.5 parts of a silane coupling agent to the cooled rubber, raise the temperature to 120°C, stir at a speed of 30-45r / min for 30-60min to mix evenly, and after cooling, obtain the modified rubber base;
[0073] The viscosity of vinyl silicone oil is 5000cps; the specific surface area of fumed silica is 200m 2 / g; the silane coupling agent is silane coupling agent KH560.
[0074] Example 4
[0075] The silicone rubber foam material provided in this embodiment is different from that in Embodiment 3 only in the steps S1 and S2 of material preparation:
[0076] S1. Preparation of glue A: 35 parts of vinyl silicone oil, 15 parts of modified base glue, 2 parts of activator A, 0.05 parts of activator B, 25 parts of flame retardant, 7 parts of structure control agent, and 1 part of platinum catalyst were weighed and put into a power mixer, the temperature was controlled at 20-40°C, the stirring speed was set to 30-40r / min, the stirring time was 60-90min, and after stirring evenly, it was taken out for use;
[0077] Preparation of B glue: weigh 35 parts of vinyl silicone oil, 15 parts of modified base glue, 2 parts of activator A, 0.05 parts of activator B, 25 parts of flame retardant, 7 parts of structure control agent, 2 parts of hydrogenated silicone oil, 0.06 parts of inhibitor, and 0.2 parts of color paste according to mass parts, put them into a power mixer, control the temperature at 20-40°C, set the stirring speed to 30-40r / min, and stir for 60-90min. After stirring evenly, take out for use;
[0078] Among them, the vinyl silicone oil used in A and B glue is double-terminal vinyl silicone oil, with a viscosity of 20000cps and a vinyl content of 0.12wt%; the activator A is zinc oxide with a particle size of 2-5μm; the activator B is alkane white oil; the flame retardant is a mixed flame retardant of magnesium hydroxide and aluminum hydroxide with a particle size of 2-10μm; the structure control agent is hydroxyl silicone oil with a hydroxyl content of 9%; the platinum catalyst is a 3000PPM chloroplatinic acid catalyst; the hydrogen content of the hydrogen-containing silicone oil is 0.75wt%; the inhibitor is 1-ethynylcyclohexanol; the color paste is: a color paste in the 39 series provided by Guangzhou Hongyu Technology Candle Paint Co., Ltd., and the color is not limited;
[0079] S2. Pour the A rubber material and B rubber material produced in step S1 into the A and B material cylinders of the feeding system respectively. Through the feeding system, transfer the A and B rubber materials to the mixing and stirring head in a mass ratio of 1:1. Set the stirring speed to 900r / min, stir the A and B rubber materials evenly, and then spray them out from the glue outlet.
[0080] Example 5
[0081] The silicone rubber foam material provided in this embodiment is different from that in Embodiment 1 only in the step S1 of material preparation:
[0082] S1. Preparation of glue A: 35 parts of vinyl silicone oil, 25 parts of modified base glue, 2 parts of activator A, 0.05 parts of activator B, 25 parts of flame retardant, 7 parts of structure control agent, and 3 parts of platinum catalyst were weighed and put into a power mixer, the temperature was controlled at 20-40°C, the stirring speed was set to 30-40r / min, the stirring time was 60-90min, and after stirring evenly, it was taken out for use;
[0083] Preparation of B glue: according to the mass parts, 35 parts of vinyl silicone oil, 25 parts of modified base glue, 2 parts of activator A, 0.05 parts of activator B, 25 parts of flame retardant, 7 parts of structure control agent, 2 parts of hydrogenated silicone oil, 0.1 parts of inhibitor, and 0.1 parts of color paste are weighed and put into a power mixer, the temperature is controlled at 20-40°C, the stirring speed is set to 30-40r / min, the stirring time is 60-90min, and after stirring evenly, take out for use;
[0084] Among them, the vinyl silicone oil used in A and B glue is a double-ended vinyl silicone oil with a viscosity of 2000cps and a vinyl content of 0.24wt%; the activator A is zinc oxide with a particle size of 2-5μm; the activator B is alkane anhydrous ethanol; the flame retardant is a mixed flame retardant of magnesium hydroxide and aluminum hydroxide with a particle size of 2-10μm; the structure control is hydroxyl silicone oil with a hydroxyl content of 4%; the platinum catalyst is a 3000PPM chloroplatinic acid catalyst; the hydrogen content of the hydrogen-containing silicone oil is 1.2wt%; the inhibitor is 1-ethynylcyclohexanol; the color paste is: a color paste in the 39 series provided by Guangzhou Hongyu Technology Candle Paint Co., Ltd., and the color is not restricted.
[0085] Comparative Example 1
[0086] A silicone rubber foam material, which differs from Example 1 only in the step S1 of material preparation (the added base rubber is not modified, and no activators A and B are added):
[0087] S1. Preparation of glue A: Weigh 30 parts of vinyl silicone oil, 25 parts of base glue, 25 parts of flame retardant, 6 parts of structure control agent, and 1 part of platinum catalyst into a power mixer according to mass, control the temperature at 20-40 ° C, set the stirring speed to 30-40r / min, and stir for 60-90min. Stir well and take out for use;
[0088] Preparation of B glue: weigh 30 parts of vinyl silicone oil, 25 parts of base glue, 25 parts of flame retardant, 6 parts of structure control agent, 1 part of hydrogenated silicone oil, 0.06 parts of inhibitor, and 0.1 parts of color paste according to mass parts, put them into a power mixer, control the temperature at 20-40°C, set the stirring speed to 30-40r / min, and stir for 60-90min. After stirring evenly, take out for use;
[0089] Among them, the vinyl silicone oil used in A and B glue is double-terminal vinyl silicone oil, the viscosity is 20000cps, and the vinyl content is 0.12wt%; the flame retardant is a mixed flame retardant of magnesium hydroxide and aluminum hydroxide, and the particle size is 2-10μm; the structure control agent is hydroxyl silicone oil, and the hydroxyl content is 4%; the platinum catalyst is 3000PPM chloroplatinic acid catalyst; the hydrogen content of the hydrogen-containing silicone oil is 1.6wt%; the inhibitor is 1-ethynylcyclohexanol; the color paste is: a color paste in the 39 series provided by Guangzhou Hongyu Technology Candle Paint Co., Ltd., and the color is not limited;
[0090] The base rubber is homemade, and the preparation method is as follows: S1. Weigh 70 parts of vinyl silicone oil and 30 parts of silica powder by mass, stir them evenly at 160-170°C, and then stir them at a speed of 30-45r / min for 30-60min to mix the rubber evenly, and let it cool;
[0091] S2. Add 0.5 parts of silane coupling agent to the cooled rubber, raise the temperature to 120 ° C, stir at a speed of 30-45r / min for 30-60min to mix evenly, and obtain the base rubber after cooling;
[0092] The viscosity of vinyl silicone oil is 2000cps; the specific surface area of fumed silica is 200m 2 / g; the silane coupling agent is silane coupling agent KH560.
[0093] Comparative Example 2
[0094] A silicone rubber foam material, which differs from Example 2 only in the step S1 of material preparation (the added base rubber is not modified, and no activators A and B are added):
[0095] S1. Preparation of glue A: Weigh 30 parts of vinyl silicone oil, 15 parts of base glue, 25 parts of flame retardant, 6 parts of structure control agent, and 1 part of platinum catalyst into a power mixer, control the temperature at 20-40 ° C, set the stirring speed to 30-40r / min, and stir for 60-90min. Stir well and take out for use;
[0096] Preparation of B glue: weigh 30 parts of vinyl silicone oil, 15 parts of base glue, 25 parts of flame retardant, 6 parts of structure control agent, 1 part of hydrogenated silicone oil, 0.06 parts of inhibitor, and 0.1 parts of color paste according to mass parts, put them into a power mixer, control the temperature at 20-40°C, set the stirring speed to 30-40r / min, and stir for 60-90min. After stirring evenly, take out for use;
[0097] Among them, the vinyl silicone oil used in A and B glue is double-terminal vinyl silicone oil, the viscosity is 2000cps, and the vinyl content is 0.22wt%; the flame retardant is a mixed flame retardant of magnesium hydroxide and aluminum hydroxide, and the particle size is 2-10μm; the structure control agent is hydroxyl silicone oil, and the hydroxyl content is 4%; the platinum catalyst is 3000PPM chloroplatinic acid catalyst; the hydrogen content of the hydrogen-containing silicone oil is 1.6wt%; the inhibitor is 1-ethynylcyclohexanol; the color paste is: a color paste in the 39 series provided by Guangzhou Hongyu Technology Candle Paint Co., Ltd., and the color is not limited;
[0098] The base rubber is homemade, and the preparation method is as follows: S1. Weigh 70 parts of vinyl silicone oil and 30 parts of silica powder by mass, stir them evenly at 160-170°C, and then stir them at a speed of 30-45r / min for 30-60min to mix the rubber evenly, and let it cool;
[0099] S2. Add 0.5 parts of silane coupling agent to the cooled rubber material, raise the temperature to 120°C, stir at a speed of 30-45 r / min for 30-60 min to mix evenly, and obtain the base rubber after cooling.
[0100] Comparative Example 3
[0101] A silicone rubber foam material, which differs from Example 5 only in the step S1 of material preparation (the added base rubber is not modified, and no activators A and B are added):
[0102] S1. Preparation of glue A: 35 parts of vinyl silicone oil, 25 parts of base glue, 25 parts of flame retardant, 7 parts of structure control agent, and 3 parts of platinum catalyst were weighed in parts by mass and put into a power mixer, the temperature was controlled at 20-40 ° C, the stirring speed was set to 30-40 r / min, the stirring time was 60-90 min, and the mixture was stirred evenly and then taken out for use;
[0103] Preparation of B glue: weigh 35 parts of vinyl silicone oil, 25 parts of base glue, 25 parts of flame retardant, 7 parts of structure control agent, 2 parts of hydrogenated silicone oil, 0.1 parts of inhibitor, and 0.1 parts of color paste according to mass parts, put them into a power mixer, control the temperature at 20-40°C, set the stirring speed to 30-40r / min, and stir for 60-90min. After stirring evenly, take out for use;
[0104] Among them, the vinyl silicone oil used in A and B glue is double-terminal vinyl silicone oil, the viscosity is 2000cps, and the vinyl content is 0.24wt%; the flame retardant is a mixed flame retardant of magnesium hydroxide and aluminum hydroxide, and the particle size is 2-10μm; the structure control is hydroxy silicone oil, and the hydroxyl content is 4%; the platinum catalyst is 3000PPM chloroplatinic acid catalyst; the hydrogen content of the hydrogen-containing silicone oil is 1.2wt%; the inhibitor is 1-ethynylcyclohexanol; the color paste is: a color paste in the 39 series provided by Guangzhou Hongyu Technology Candle Paint Co., Ltd., and the color is not limited;
[0105] The base rubber is homemade, and the preparation method is as follows: S1. Weigh 70 parts of vinyl silicone oil and 30 parts of silica powder by mass, stir them evenly at 160-170°C, and then stir them at a speed of 30-45r / min for 30-60min to mix the rubber evenly, and let it cool;
[0106] S2. Add 0.5 parts of silane coupling agent to the cooled rubber material, raise the temperature to 120°C, stir at a speed of 30-45 r / min for 30-60 min to mix evenly, and obtain the base rubber after cooling.
[0107] Comparative Example 4
[0108] A silicone rubber foam material, which differs from Example 2 only in the step S1 of material preparation (the added base rubber is not modified):
[0109] S1. Prepare glue A: weigh 30 parts of vinyl silicone oil, 15 parts of base glue, 0.5 parts of activator A, 0.05 parts of activator B, 25 parts of flame retardant, 6 parts of structure control agent, and 1 part of platinum catalyst into a power mixer, control the temperature at 20-40°C, set the stirring speed to 30-40r / min, and stir for 60-90min. Stir well and take out for use;
[0110] Preparation of glue B: weigh 30 parts of vinyl silicone oil, 15 parts of base glue, 0.5 parts of activator A, 0.05 parts of activator B, 25 parts of flame retardant, 6 parts of structure control agent, 1 part of hydrogenated silicone oil, 0.06 parts of inhibitor, and 0.1 parts of color paste according to mass parts, put them into a power mixer, control the temperature at 20-40°C, set the stirring speed to 30-40r / min, and stir for 60-90min. After stirring evenly, take out for use;
[0111] Among them, the vinyl silicone oil used in A and B glue is double-terminal vinyl silicone oil, with a viscosity of 2000cps and a vinyl content of 0.22wt%; the activator A is magnesium oxide with a particle size of 2-5μm; the activator B is alkane white oil; the flame retardant is a mixed flame retardant of magnesium hydroxide and aluminum hydroxide with a particle size of 2-10μm; the structure control agent is hydroxyl silicone oil with a hydroxyl content of 4%; the platinum catalyst is a 3000PPM chloroplatinic acid catalyst; the hydrogen content of the hydrogen-containing silicone oil is 1.6wt%; the inhibitor is 1-ethynylcyclohexanol; the color paste is: a color paste in the 39 series provided by Guangzhou Hongyu Technology Candle Paint Co., Ltd., and the color is not limited;
[0112] The base rubber is homemade, and the preparation method is as follows: S1. Weigh 70 parts of vinyl silicone oil and 30 parts of silica powder by mass, stir them evenly at 160-170°C, and then stir them at a speed of 30-45r / min for 30-60min to mix the rubber evenly, and let it cool;
[0113] S2. Add 0.5 parts of silane coupling agent to the cooled rubber material, raise the temperature to 120°C, stir at a speed of 30-45 r / min for 30-60 min to mix evenly, and obtain the base rubber after cooling.
[0114] Comparative Example 5
[0115] A silicone rubber foam material, which differs from Example 2 only in the step S1 of material preparation (active agent A and active agent B are not added):
[0116] S1. Preparation of glue A: 30 parts of vinyl silicone oil, 15 parts of modified base rubber, 25 parts of flame retardant, 6 parts of structure control agent, and 1 part of platinum catalyst were weighed and put into a power mixer, the temperature was controlled at 20-40 ° C, the stirring speed was set to 30-40r / min, the stirring time was 60-90min, and the mixture was stirred evenly and then taken out for use;
[0117] Preparation of B glue: weigh 30 parts of vinyl silicone oil, 15 parts of modified base glue, 25 parts of flame retardant, 6 parts of structure control agent, 1 part of hydrogenated silicone oil, 0.06 parts of inhibitor, and 0.1 parts of color paste according to mass parts, put them into a power mixer, control the temperature at 20-40°C, set the stirring speed to 30-40r / min, and stir for 60-90min. After stirring evenly, take out for use;
[0118] Among them, the vinyl silicone oil used in A and B glues is a double-ended vinyl silicone oil with a viscosity of 2000cps and a vinyl content of 0.22wt%; the activator A is magnesium oxide with a particle size of 2-5μm; the activator B is alkane white oil; the flame retardant is a mixed flame retardant of magnesium hydroxide and aluminum hydroxide with a particle size of 2-10μm; the structure control agent is hydroxyl silicone oil with a hydroxyl content of 4%; the platinum catalyst is a 3000PPM chloroplatinic acid catalyst; the hydrogen content of the hydrogen-containing silicone oil is 1.6wt%; the inhibitor is 1-ethynylcyclohexanol; the color paste is: a color paste in the 39 series provided by Guangzhou Hongyu Craft Candle Paint Co., Ltd., and the color is not restricted.
[0119] Table 1 Performance test results of embodiments and comparative examples
[0120]
[0121] In Examples 1-5, modified base rubber, activator A and activator B are introduced into the system at the same time, and the silicone rubber foam materials obtained can achieve small and uniform pores while having high resilience and high waterproofness. Among them, the compression permanent deformation is less than 3%, the vacuum water absorption rate is less than 4.0%, and they can pass the sealing and waterproofing test, achieving a significant improvement in the overall performance of the silicone rubber foam material.
[0122] In Comparative Examples 1-3, the base rubber was not modified, and activator A and activator B were not added. The obtained silicone rubber foam material could not obtain uniform and fine pores, and the resilience and waterproof properties were significantly reduced. It can be seen that modifying the base rubber and adding activators A and B can improve the activity of A and B rubber materials, and ultimately improve the overall performance of the silicone rubber foam.
[0123] Compared with Example 2, Comparative Example 4 does not add modified base glue, and Comparative Example 5 does not add activator A and activator B compared with Example 2. According to the test results of the two groups of comparative examples, the appearance of the bubbles is large and uneven, and the sealing and waterproof part fails the test. It can be seen that the simultaneous use of modified base glue and activator is beneficial to improving the comprehensive performance of the foam.
[0124] Based on the test data of appearance performance, compression permanent deformation, vacuum water absorption rate and sealing waterproofness in Table 1, the silicone rubber foam material prepared by Examples 1-5 has obvious advantages over the comparative example and can effectively meet the high standards of customers and the market.
[0125] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims
1. A silicone rubber foam material, characterized in that: By weight, it includes the following components: Glue A: 30-35 parts of vinyl silicone oil, 15-25 parts of modified base glue, 0.5-2 parts of activator A, 0.05-0.25 parts of activator B, 10-25 parts of flame retardant, 6-7 parts of structure control agent, 1-3 parts of platinum catalyst; B glue: vinyl silicone oil 30-35 parts, modified base glue 15-25 parts, activator A 0.5-2 parts, activator B 0.05-0.25 parts, flame retardant 10-25 parts, structure control agent 6-7 parts, hydrogen-containing silicone oil 1-2 parts, inhibitor 0.06-0.10 parts, color paste 0.10-0.20 parts; Among them, the mass ratio of the A glue to the B glue is 1: (0.9-1.1); the modified base glue includes the following components by weight: 68-72 parts of vinyl silicone oil, 3-6 parts of diphenylsilanediol, 28-32 parts of silicon dioxide, and 0.5-0.8 parts of coupling agent.
2. The silicone rubber foam material according to claim 1, characterized in that: The activator A is one or more of zinc oxide, magnesium oxide, zinc stearate and calcium stearate.
3. The silicone rubber foam material according to claim 1, characterized in that: The activator B is any one or more of alcohols, amines and alkanes.
4. The silicone rubber foam material according to claim 1, characterized in that: The flame retardant is selected from one or more of magnesium hydroxide, aluminum hydroxide, talcum powder, clay, and calcium carbonate.
5. The silicone rubber foam material according to claim 1, characterized in that: The structure control agent is hydroxy silicone oil.
6. The silicone rubber foam material according to claim 1, characterized in that: The inhibitor is one or more of 1-ethynylcyclohexanol, 2-methyl-3-butyn-2-ol and 3,5-dimethyl-1-hexyn-3-ol.
7. The silicone rubber foam material according to claim 1, characterized in that: The hydrogen-containing silicone oil is selected from one or more of hydrogen-containing silicone oils having a hydrogen content of 0.75wt%, 1.2wt%, and 1.6wt%.
8. The silicone rubber foam material according to claim 1, characterized in that: The preparation method of the modified rubber base comprises the following steps: S1. Take 68-72 parts of vinyl silicone oil and 3-6 parts of diphenylsilanediol and stir them at 160-170°C, then add 28-32 parts of silica powder in 2-3 times, and then stir at a speed of 30-45r / min for 30-60min to mix the rubber evenly, and let it cool; S2. Add 0.5-0.8 parts of silane coupling agent to the cooled rubber material, raise the temperature to 105-125°C, stir at a speed of 30-45r / min for 30-60min to mix evenly, and obtain the modified base rubber after cooling.
9. The method for preparing the silicone rubber foam material according to any one of claims 1 to 8, characterized in that: The steps include: S1. Weigh each component according to the formula ratio of A and B glue and mix them evenly to obtain A glue and B glue; S2. The rubber materials A and B are transferred to the mixing and stirring head in proportion and mixed evenly to obtain a mixed rubber material; S3. The mixed rubber material is calendered, foamed, de-filmed and rolled to obtain a sulfurized silicone rubber foam material; S4. The silicone rubber foam material after sulfurization is baked and matured at high temperature to obtain the silicone rubber foam material.
10. Use of the silicone rubber foam material according to any one of claims 1 to 8 as a sealing or buffering material.