Sound-insulation rubber synthetic material as well as preparation method and application thereof

Abstract

The invention provides a sound insulation rubber synthetic material and a preparation method and application thereof, and belongs to the technical field of rubber.The preparation method comprises the following steps that butyl rubber and ethylene propylene diene monomer are added into an internal mixer for plastication, then carbon black, a metal oxide compound, a modification auxiliary agent, a vulcanization activator and an anti-aging agent are added for mixing, and the sound insulation rubber synthetic material is obtained. Adding a vulcanization accelerator and a vulcanizing agent, continuously mixing, and discharging rubber to obtain a rubber material; putting the rubber material into an open mill for thin-passing and standing to obtain a rubber compound; and vulcanizing the rubber compound on a flat vulcanizing machine to obtain the sound insulation rubber synthetic material. Wherein the metal oxide compound is prepared by calcining and fragmenting cerium dioxide, titanium dioxide and silicon dioxide; the modification additive is prepared from a functional polymer and modified hollow glass beads. The sound insulation rubber synthetic material is good in sound insulation performance and durability, and the preparation process is simple and convenient.

Description

Technical Field

[0001] The invention belongs to the technical field of rubber, and in particular relates to a sound insulation rubber synthetic material and a preparation method and application thereof. Background Art

[0002] As an important industrial raw material, rubber materials have been widely used in many fields due to their good elasticity, wear resistance and anti-aging properties. Natural rubber comes from the latex of rubber trees, while synthetic rubber is made by chemical methods. Both have excellent physical and mechanical properties and are suitable for manufacturing tires, seals, etc. With the development of science and technology and changes in market demand, rubber materials with specific functional improvements continue to emerge, and sound insulation rubber materials are one of them. This special rubber not only inherits the advantages of traditional rubber, but also optimizes its molecular structure to enhance the sound barrier effect, making it an ideal sound insulation material in fields such as building decoration and automobile manufacturing. The main advantages of sound insulation rubber materials include good sound insulation effect, flexibility and easy processing and molding. They can effectively reduce external noise interference. They are widely used in sound insulation treatment of building walls, floors and ceilings, as well as sound insulation of car interiors, improving people's quality of life.

[0003] However, the shortcomings of existing sound insulation rubber materials cannot be ignored. For example, in order to achieve good sound insulation effect, sound insulation rubber often requires a certain thickness, which increases the weight of the overall structure and is not applicable to application scenarios such as automobile manufacturing; in extreme environments such as high or low temperatures, the performance of sound insulation rubber may decline, affecting its service life and sound insulation effect; some sound insulation rubbers may contain chemicals that are harmful to the human body or the environment, and there are environmental and safety risks during production, use and disposal; in addition, due to the complex production process of sound insulation rubber and the expensive raw materials, the overall cost is high, which increases the cost of use.

[0004] In order to overcome the above-mentioned shortcomings of sound insulation rubber materials, the weight of sound insulation rubber materials can be reduced by adding other lightweight and high-strength materials or nanomaterials to rubber; the weather resistance of sound insulation rubber can be improved by adding specific anti-aging agents, heat stabilizers and other additives to solve the problem of performance degradation in extreme environments; by developing green and environmentally friendly sound insulation rubber, traditional petroleum-based raw materials can be replaced by green and non-toxic raw materials, thereby reducing the use of harmful chemicals. However, these methods will increase the difficulty of the production process and the cost of raw materials, making it difficult to achieve large-scale commercial use. Therefore, it is urgent to develop a preparation method for sound insulation rubber synthetic materials that not only has good sound insulation effect and durability, but also has a simple process and is suitable for promotion and application. Summary of the invention

[0005] The purpose of the present invention is to provide a sound insulation rubber synthetic material, by adding a metal oxide complex and a specific modification aid to the rubber raw material, the sound insulation performance and durability of the rubber material are further improved. The present invention also provides a preparation method of the above-mentioned sound insulation rubber synthetic material, which has a simple process.

[0006] In order to achieve the above object, the present invention provides the following technical solutions:

[0007] The present invention provides a sound insulation rubber synthetic material, comprising the following raw materials in parts by weight:

[0008] 60-80 parts by weight of butyl rubber, 20-40 parts by weight of EPDM rubber, 20-30 parts by weight of carbon black, 3-7 parts by weight of metal oxide composite, 7-13 parts by weight of modifying aid, 10-15 parts by weight of vulcanization activator, 2-4 parts by weight of vulcanization accelerator, 1-3 parts by weight of vulcanizing agent, and 2-5 parts by weight of antioxidant.

[0009] Preferably, the vulcanization activator is a mixture of stearic acid and zinc oxide in a weight ratio of 3-5:3.

[0010] Preferably, the vulcanization accelerator is one or a mixture of two or more of N-tert-butyl-2-benzothiazole sulfenamide, N-cyclohexyl-2-benzothiazole sulfenamide, dibenzothiazyl disulfide, zinc dimethyldithiocarbamate, and zinc diethyldithiocarbamate.

[0011] Preferably, the vulcanization accelerator is a mixture of N-tert-butyl-2-benzothiazolesulfenamide and zinc diethyldithiocarbamate in a weight ratio of 1:1-3.

[0012] Preferably, the vulcanizing agent is sulfur.

[0013] Preferably, the antioxidant is one of antioxidant RD, antioxidant MB, antioxidant 4010, antioxidant D, and antioxidant BLE, or a mixture of two or more thereof.

[0014] Preferably, the antioxidant is a mixture of antioxidant RD and antioxidant MB in a weight ratio of 3:1-3.

[0015] Preferably, the method for preparing the metal oxide composite comprises the following steps:

[0016] 1-3 parts by weight of cerium dioxide, 2-4 parts by weight of titanium dioxide and 8-12 parts by weight of silicon dioxide are uniformly mixed and then pressed into a cylindrical sample. The cylindrical sample is then calcined, crushed, pulverized and sieved to obtain a metal oxide composite.

[0017] The present invention can effectively improve the sound insulation performance of the sound insulation rubber synthetic material by adding the metal oxide composite prepared by the above method. The metal oxide composite is composed of cerium dioxide, titanium dioxide and silicon dioxide, each of which has unique physical and chemical properties and plays an important role in enhancing the overall performance of the rubber material.

[0018] First, silica as a matrix material provides the necessary physical support to ensure the structural integrity of the composite material. Its porosity promotes multiple reflections and scattering of sound waves on its internal surface, increasing the propagation path length of sound waves within the material, thereby improving the sound absorption efficiency. In addition, the high stability and durability of silica help maintain the performance stability of the composite material during long-term use.

[0019] Secondly, due to its good thermal and chemical stability, cerium dioxide can maintain the structural stability of the material at high temperatures. More importantly, its catalytic activity can promote the conversion of sound wave energy into heat energy. Part of the sound energy is absorbed and converted into other forms of energy, such as heat energy, further enhancing the sound absorption performance of the material. At the same time, cerium dioxide can also capture free radicals during the combustion process, inhibiting the occurrence of chain reactions, thereby delaying or preventing the spread of flames and improving the flame retardant properties of the material.

[0020] Thirdly, titanium dioxide not only has excellent chemical stability and photocatalytic activity, but also due to its special crystal structure can effectively increase the reflection path of sound waves inside the material, which increases the propagation distance of sound waves within the material, enhances the absorption and scattering efficiency of sound waves, and improves the overall sound insulation effect. The addition of titanium dioxide also helps promote the formation of a carbon layer, which can play a role in heat insulation and oxygen isolation during the combustion process, thereby further improving the flame retardant properties of the material.

[0021] The metal oxide composite of the present invention can form a loose pore structure through the process of calcination, rapid cooling and fragmentation, which is conducive to the absorption and scattering of sound waves, and also provides a certain degree of elasticity for the material, which helps to attenuate vibration.

[0022] Furthermore, the method for preparing the metal oxide composite comprises the following steps:

[0023] 1-3 parts by weight of cerium dioxide, 2-4 parts by weight of titanium dioxide and 8-12 parts by weight of silicon dioxide are mixed evenly, and then pressed into a cylindrical sample under 0.1-0.5MPa conditions, wherein the diameter of the cylindrical sample is 0.5-1cm and the height is 1-2cm. The cylindrical sample is then calcined at 1100-1400°C for 100-200min. After calcination, the cylindrical sample is placed under -160 to -140°C liquid nitrogen conditions for 30-40min of crushing treatment, and then sieved through a 120-180 mesh sieve to obtain a metal oxide composite.

[0024] Preferably, the preparation method of the modification aid comprises the following steps:

[0025] 5-10 parts by weight of hollow glass microspheres are added to 60-80 parts by weight of sodium hydroxide aqueous solution, stirred, filtered, washed with water, and dried to obtain activated hollow glass microspheres; 4-6 parts by weight of N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane and 40-50 parts by weight of ethanol aqueous solution are uniformly mixed, and then 2-5 parts by weight of activated hollow glass microspheres are added, heated and stirred, filtered, and dried to obtain modified hollow glass microspheres;

[0026] 1-4 parts by weight of phenylphosphonyl dichloride and 5-10 parts by weight of N-(4-aminophenyl)maleimide are added to 70-90 parts by weight of dimethyl sulfoxide, stirred, then 1-2 parts by weight of potassium hydroxide are added, heated for reaction, distilled under reduced pressure, and dried to obtain an intermediate containing maleimide; 3-5 parts by weight of the intermediate containing maleimide, 1-2 parts by weight of maleic anhydride and 40-60 parts by weight of xylene are uniformly mixed, heated under a nitrogen atmosphere, then 0.04-0.06 parts by weight of azobisisobutyronitrile are added for reaction, distilled under reduced pressure, and dried to obtain a functional polymer;

[0027] 2-4 parts by weight of functional polymer are added to 40-60 parts by weight of dimethyl sulfoxide, stirred, and then 1-2 parts by weight of modified hollow glass microspheres are added, heated and stirred, filtered, and dried to obtain a modified auxiliary agent.

[0028] The present invention also adds a modification aid to cooperate with other components, further improving the sound insulation performance and aging resistance of the sound insulation rubber synthetic material. In the preparation process of the modification aid, the hollow glass microspheres are activated by surface treating the hollow glass microspheres in a sodium hydroxide solution. This process increases the active sites on the surface of the microspheres, improves the interface compatibility and bonding strength between them and other materials, and the activated hollow glass microspheres not only retain the original dense shell layer and hollow internal structure, but also enhance the ability of sound waves to reflect inside them due to the change in surface properties, increase the length of the sound wave propagation path, thereby consuming more sound wave energy and effectively improving the sound insulation effect. In addition, the dispersion of these microspheres in the rubber matrix can form a vibration loss mechanism at the microscopic level, further enhancing the sound insulation performance of the damping silicone rubber.

[0029] Furthermore, the grafting reaction of N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane with activated hollow glass microspheres makes the silane molecules firmly attached to the surface of the microspheres, which not only enhances the reactivity between the microspheres and subsequent polymers, but also gives the microspheres additional functional properties, such as improving their dispersibility and stability. The modified hollow glass microspheres can be evenly distributed in the rubber matrix, avoiding the occurrence of agglomeration, ensuring that each microsphere can play the best sound insulation and reinforcement role.

[0030] The intermediate generated by the substitution reaction between phenylphosphonyl dichloride and N-(4-aminophenyl) maleimide has a phosphorus-containing group, which gives the modified auxiliary agent excellent flame retardant properties. The functional polymer introduces maleic anhydride through copolymerization, which not only enhances the mechanical properties of the material, but also helps to capture free radicals in the combustion process due to its special chemical structure, inhibits the spread of flames, and improves the overall flame retardant level. The functional polymer is combined with the modified hollow glass microspheres to form a modified auxiliary agent with a high synergistic effect. After the auxiliary agent is added to the rubber matrix, it can not only significantly improve the sound insulation effect, but also further enhance the flame retardant properties through the presence of the phosphorus-containing group. At the same time, due to the good dispersibility and stability brought by silane grafting, the aging resistance of the material is improved.

[0031] Furthermore, the preparation method of the modification aid comprises the following steps:

[0032] 5-10 parts by weight of hollow glass microspheres are added to 60-80 parts by weight of 2-5wt% sodium hydroxide aqueous solution, stirred at room temperature and 400-600rpm for 20-30min, filtered, washed with water until neutral, and dried to obtain activated hollow glass microspheres; 4-6 parts by weight of N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane and 40-50 parts by weight of 60-70wt% ethanol aqueous solution are mixed uniformly, and then 2-5 parts by weight of activated hollow glass microspheres are added, stirred at 70-80°C and 100-300rpm for 5-10h, filtered, and dried to obtain modified hollow glass microspheres;

[0033] 1-4 parts by weight of phenylphosphonyl dichloride and 5-10 parts by weight of N-(4-aminophenyl)maleimide are added to 70-90 parts by weight of dimethyl sulfoxide, stirred at room temperature and 400-600 rpm for 7-15 minutes, then 1-2 parts by weight of potassium hydroxide are added, heated to 55-70° C. for reaction for 7-12 hours, dimethyl sulfoxide is removed by reduced pressure distillation, and dried to obtain an intermediate containing maleimide; 3-5 parts by weight of the intermediate containing maleimide, 1-2 parts by weight of maleic anhydride and 40-60 parts by weight of xylene are uniformly mixed, heated to 90-95° C. under a nitrogen atmosphere, then 0.04-0.06 parts by weight of azobisisobutyronitrile are added to react for 3-5 hours, xylene is removed by reduced pressure distillation, and dried to obtain a functional polymer;

[0034] Add 2-4 parts by weight of functional polymer to 40-60 parts by weight of dimethyl sulfoxide, stir at room temperature and 400-600 rpm for 10-20 minutes, then add 1-2 parts by weight of modified hollow glass microspheres, stir at 65-75°C and 100-300 rpm for 5-8 hours, filter, and dry to obtain a modified auxiliary agent.

[0035] The present invention also provides a method for preparing a sound insulation rubber synthetic material, comprising the following steps:

[0036] According to the raw material formula, butyl rubber and EPDM rubber are added to an internal mixer for plasticization for 1-3 minutes, and then carbon black, metal oxide composite, modification aid, vulcanization activator and antioxidant are added and mixed for 2-5 minutes, and then vulcanization accelerator and vulcanizer are added and mixed for 2-5 minutes, and the rubber is discharged to obtain a rubber compound; the rubber compound is placed in an open mixer and thinned for 3-5 times, and then parked for 20-25 hours to obtain a mixed rubber; the mixed rubber is placed on a flat vulcanizer for vulcanization for 20-40 minutes to obtain the sound insulation rubber synthetic material.

[0037] Preferably, the temperature of the internal mixer is 65-75° C. and the rotation speed is 70-90 rpm.

[0038] Preferably, the roller distance of the mixing mill is 0.5-1.0 mm and the temperature is 55-65°C.

[0039] Preferably, the temperature of the plate vulcanizer is 150-170° C. and the pressure is 8-12 MPa.

[0040] The present invention also provides application of the sound insulation rubber synthetic material in preparing building materials and automobile materials.

[0041] Compared with the prior art, the advantages and beneficial effects of the present invention are:

[0042] 1. The present invention provides a sound-insulating rubber synthetic material and a preparation method thereof, wherein a metal oxide composite and a specific modifying agent are added to the raw material formula, and act together with butyl rubber, EPDM rubber, carbon black, etc., wherein the metal oxide composite is made of cerium dioxide, titanium dioxide and silicon dioxide after calcination and crushing, and the modifying agent is made of functional polymer and modified hollow glass microspheres, which further improves the sound insulation performance and durability of the rubber material. The present invention also provides a preparation method of the above-mentioned sound-insulating rubber synthetic material, which has a simple process and is suitable for popularization and application.

[0043] 2. The metal oxide composite prepared by the present invention can effectively improve the sound insulation performance of the sound insulation rubber synthetic material. Among them, silicon dioxide as a matrix material provides the necessary physical support to ensure the structural integrity of the composite material. Its porosity promotes multiple reflections and scattering of sound waves on its internal surface, increasing the propagation path length of sound waves in the material. The catalytic activity of cerium dioxide can promote the conversion of sound wave energy into heat energy. Part of the sound energy is absorbed and converted into other forms of energy, such as heat energy, further enhancing the sound absorption performance of the material. Titanium dioxide can effectively increase the reflection path of sound waves in the material due to its special crystal structure, which increases the propagation distance of sound waves in the material, enhances the absorption and scattering efficiency of sound waves, and improves the overall sound insulation effect.

[0044] 3. The present invention also adds a modification agent to synergize with other components to further improve the sound insulation performance and aging resistance of the sound insulation rubber synthetic material. The modification agent uses surface activated and silane-grafted hollow glass microspheres to enhance sound wave reflection and energy dissipation. At the same time, the phosphorus-containing groups in the functional polymer provide excellent flame retardancy, and silane improves dispersibility and interface bonding. The synergistic effect of these components not only prolongs the sound wave propagation path and improves the sound insulation effect, but also enhances the aging resistance of the material, ensuring long-term stability and high-efficiency sound insulation. DETAILED DESCRIPTION

[0045] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0046] Butyl rubber, brand: 268, specific gravity: 0.92, Mooney viscosity: 51MU (ML1+8, 125°C), unsaturation: 1.7 mol%, manufacturer: ExxonMobil Chemical Company, USA.

[0047] EPDM rubber, brand: 4045M, Mooney viscosity: 45MU (ML1+4, 125°C), ethylene content: 44.5wt%, manufacturer: Mitsui Chemicals, Japan.

[0048] Carbon black, brand: N550, manufacturer: Jinneng Technology Co., Ltd.

[0049] Hollow glass microspheres, model: HL60S, particle size D50: 35μm, manufacturer: Zhengzhou Shenglait Hollow Microsphere New Materials Co., Ltd.

[0050] Example 1

[0051] This embodiment provides a sound insulation rubber synthetic material, comprising the following raw materials in parts by weight:

[0052] 70 parts by weight of butyl rubber, 30 parts by weight of EPDM rubber, 25 parts by weight of carbon black, 5 parts by weight of metal oxide composite, 10 parts by weight of modification aid, 12 parts by weight of vulcanization activator, 3 parts by weight of vulcanization accelerator, 2 parts by weight of vulcanizing agent, and 3.5 parts by weight of antioxidant.

[0053] The vulcanization activator is a mixture of stearic acid and zinc oxide in a weight ratio of 4:3;

[0054] The vulcanization accelerator is a mixture of N-tert-butyl-2-benzothiazole sulfenamide and zinc diethyldithiocarbamate in a weight ratio of 1:2;

[0055] The vulcanizing agent is sulfur;

[0056] The antioxidant is a mixture of antioxidant RD and antioxidant MB in a weight ratio of 3:2.

[0057] The method for preparing the metal oxide composite comprises the following steps:

[0058] 2 parts by weight of cerium dioxide, 3 parts by weight of titanium dioxide and 10 parts by weight of silicon dioxide are mixed evenly, and then pressed into a cylindrical sample under 0.2 MPa conditions. The cylindrical sample has a diameter of 1 cm and a height of 1.5 cm. The cylindrical sample is then calcined at 1250°C for 150 min. After calcination, the cylindrical sample is placed under -150°C liquid nitrogen conditions for crushing for 35 min. After crushing, the sample is sieved through a 150-mesh screen to obtain a metal oxide composite.

[0059] The preparation method of the modified auxiliary agent comprises the following steps:

[0060] 8 parts by weight of hollow glass microspheres are added to 70 parts by weight of a 3 wt% sodium hydroxide aqueous solution, stirred at room temperature and 500 rpm for 25 min, filtered, washed with water until neutral, and dried to obtain activated hollow glass microspheres; 5 parts by weight of N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane and 45 parts by weight of a 65 wt% ethanol aqueous solution are uniformly mixed, and then 3 parts by weight of activated hollow glass microspheres are added, stirred at 75° C. and 200 rpm for 8 h, filtered, and dried to obtain modified hollow glass microspheres;

[0061] 2.5 parts by weight of phenylphosphonyl dichloride and 7 parts by weight of N-(4-aminophenyl)maleimide are added to 80 parts by weight of dimethyl sulfoxide, stirred at room temperature and 500 rpm for 10 minutes, then 1.5 parts by weight of potassium hydroxide are added, heated to 60°C for reaction for 10 hours, dimethyl sulfoxide is removed by vacuum distillation, and dried to obtain an intermediate containing maleimide; 4 parts by weight of the intermediate containing maleimide, 1.5 parts by weight of maleic anhydride and 50 parts by weight of xylene are uniformly mixed, heated to 92°C under a nitrogen atmosphere, then 0.05 parts by weight of azobisisobutyronitrile are added to react for 4 hours, xylene is removed by vacuum distillation, and dried to obtain a functional polymer;

[0062] 3.2 parts by weight of functional polymer were added to 50 parts by weight of dimethyl sulfoxide, stirred at room temperature and 500 rpm for 15 minutes, then 1.6 parts by weight of modified hollow glass microspheres were added, stirred at 70°C and 200 rpm for 6 hours, filtered, and dried to obtain a modified auxiliary agent.

[0063] This embodiment provides a method for preparing a sound insulation rubber synthetic material, comprising the following steps:

[0064] According to the raw material formula, butyl rubber and EPDM rubber are added to an internal mixer for plasticization for 2 minutes, then carbon black, metal oxide composite, modification aid, vulcanization activator, and antioxidant are added for mixing for 3 minutes, and then vulcanization accelerator and vulcanizer are added for mixing for 3 minutes, and the rubber is discharged to obtain a rubber compound; the rubber compound is placed in an open mixer and thinned for 4 times, and then parked for 24 hours to obtain a mixed rubber; the mixed rubber is placed on a flat vulcanizer for vulcanization for 30 minutes to obtain the sound insulation rubber synthetic material. Among them, the temperature of the internal mixer is 70°C and the speed is 80rpm; the roller distance of the open mixer is 1.0mm, the temperature is 60°C, and the temperature of the flat vulcanizer is 160°C and the pressure is 10MPa.

[0065] Example 2

[0066] This embodiment provides a sound insulation rubber synthetic material, comprising the following raw materials in parts by weight:

[0067] 60 parts by weight of butyl rubber, 20 parts by weight of EPDM rubber, 20 parts by weight of carbon black, 3 parts by weight of metal oxide composite, 7 parts by weight of modifying aid, 10 parts by weight of vulcanization activator, 2 parts by weight of vulcanization accelerator, 1 part by weight of vulcanizing agent, and 2 parts by weight of antioxidant. The vulcanization activator is a mixture of stearic acid and zinc oxide in a weight ratio of 3:3; the vulcanization accelerator is a mixture of N-tert-butyl-2-benzothiazole sulfenamide and zinc diethyl dithiocarbamate in a weight ratio of 1:1; the vulcanizing agent is sulfur; and the antioxidant is a mixture of antioxidant RD and antioxidant MB in a weight ratio of 3:1.

[0068] The preparation method of the metal oxide composite is the same as that of Example 1.

[0069] The preparation method of the modification aid is the same as that in Example 1.

[0070] This embodiment provides a method for preparing a sound insulation rubber synthetic material, comprising the following steps:

[0071] According to the raw material formula, butyl rubber and EPDM rubber are added to an internal mixer for plasticization for 1 minute, and then carbon black, metal oxide composite, modification aid, vulcanization activator, and antioxidant are added for mixing for 2 minutes, and then vulcanization accelerator and vulcanizer are added for mixing for 5 minutes, and the rubber is discharged to obtain a rubber compound; the rubber compound is placed in an open mixer and thinned for 3 times, and then parked for 20 hours to obtain a mixed rubber; the mixed rubber is placed on a flat vulcanizer for vulcanization for 20 minutes to obtain the sound insulation rubber synthetic material. Among them, the temperature of the internal mixer is 65°C and the speed is 70rpm; the roller distance of the open mixer is 0.5mm, the temperature is 55°C, and the temperature of the flat vulcanizer is 150°C and the pressure is 8MPa.

[0072] Example 3

[0073] This embodiment provides a sound insulation rubber synthetic material, comprising the following raw materials in parts by weight:

[0074] 80 parts by weight of butyl rubber, 40 parts by weight of EPDM rubber, 30 parts by weight of carbon black, 7 parts by weight of metal oxide composite, 13 parts by weight of modifying aid, 15 parts by weight of vulcanization activator, 4 parts by weight of vulcanization accelerator, 3 parts by weight of vulcanizing agent, and 5 parts by weight of antioxidant. The vulcanization activator is a mixture of stearic acid and zinc oxide in a weight ratio of 5:3; the vulcanization accelerator is a mixture of N-tert-butyl-2-benzothiazole sulfenamide and zinc diethyl dithiocarbamate in a weight ratio of 1:3; the vulcanizing agent is sulfur; and the antioxidant is a mixture of antioxidant RD and antioxidant MB in a weight ratio of 3:3.

[0075] The preparation method of the metal oxide composite is the same as that of Example 1.

[0076] The preparation method of the modification aid is the same as that in Example 1.

[0077] This embodiment provides a method for preparing a sound insulation rubber synthetic material, comprising the following steps:

[0078] According to the raw material formula, butyl rubber and EPDM rubber are added to an internal mixer for plasticization for 3 minutes, then carbon black, metal oxide composite, modification aid, vulcanization activator, and antioxidant are added for mixing for 5 minutes, and then vulcanization accelerator and vulcanizer are added for mixing for 2 minutes, and the rubber is discharged to obtain a rubber compound; the rubber compound is placed in an open mixer for thinning 5 times, and then parked for 25 hours to obtain a mixed rubber; the mixed rubber is placed on a flat vulcanizer for vulcanization for 40 minutes to obtain the sound insulation rubber synthetic material. Among them, the temperature of the internal mixer is 75°C and the speed is 90rpm; the roller distance of the open mixer is 1.0mm, the temperature is 65°C, and the temperature of the flat vulcanizer is 170°C and the pressure is 12MPa.

[0079] Comparative Example 1

[0080] The difference between this comparative example and Example 1 is that the preparation method of the metal oxide composite is different, which is as follows: the preparation method of the metal oxide composite comprises the following steps: 3 parts by weight of titanium dioxide and 10 parts by weight of silicon dioxide are mixed evenly, and then pressed into a cylindrical sample under 0.2 MPa conditions, wherein the diameter of the cylindrical sample is 1 cm and the height is 1.5 cm, and then the cylindrical sample is calcined at 1250°C for 150 min. After the calcination, the cylindrical sample is placed under -150°C liquid nitrogen conditions for crushing treatment for 35 min, and then crushed through a 150-mesh sieve to obtain a metal oxide composite.

[0081] Comparative Example 2

[0082] The difference between this comparative example and Example 1 is that the preparation method of the metal oxide composite is different, specifically as follows: the preparation method of the metal oxide composite comprises the following steps: 2 parts by weight of cerium dioxide and 10 parts by weight of silicon dioxide are mixed evenly, and then pressed into a cylindrical sample under 0.2 MPa conditions, wherein the diameter of the cylindrical sample is 1 cm and the height is 1.5 cm, and then the cylindrical sample is calcined at 1250°C for 150 min. After the calcination, the cylindrical sample is placed under -150°C liquid nitrogen conditions for crushing treatment for 35 min, and then crushed through a 150-mesh sieve to obtain a metal oxide composite.

[0083] Comparative Example 3

[0084] The difference between this comparative example and Example 1 is that the preparation method of the modification aid is different, which is as follows: The preparation method of the modification aid comprises the following steps:

[0085] 2.5 parts by weight of phenylphosphonyl dichloride and 7 parts by weight of N-(4-aminophenyl)maleimide are added to 80 parts by weight of dimethyl sulfoxide, stirred at room temperature and 500 rpm for 10 minutes, then 1.5 parts by weight of potassium hydroxide are added, heated to 60°C for reaction for 10 hours, dimethyl sulfoxide is removed by vacuum distillation, and dried to obtain an intermediate containing maleimide; 4 parts by weight of the intermediate containing maleimide, 1.5 parts by weight of maleic anhydride and 50 parts by weight of xylene are uniformly mixed, heated to 92°C under a nitrogen atmosphere, then 0.05 parts by weight of azobisisobutyronitrile are added to react for 4 hours, xylene is removed by vacuum distillation, and dried to obtain a functional polymer;

[0086] 3.2 parts by weight of functional polymer were added to 50 parts by weight of dimethyl sulfoxide, stirred at room temperature and 500 rpm for 15 minutes, then 1.6 parts by weight of hollow glass microspheres were added, stirred at 70°C and 200 rpm for 6 hours, filtered, and dried to obtain a modified auxiliary agent.

[0087] Comparative Example 4

[0088] The difference between this comparative example and Example 1 is that the preparation method of the modification aid is different, which is as follows: The preparation method of the modification aid comprises the following steps:

[0089] 8 parts by weight of hollow glass microspheres were added to 70 parts by weight of a 3 wt% sodium hydroxide aqueous solution, stirred at room temperature and 500 rpm for 25 min, filtered, washed with water until neutral, and dried to obtain activated hollow glass microspheres; 5 parts by weight of 3-aminopropyltriethoxysilane was uniformly mixed with 45 parts by weight of a 65 wt% ethanol aqueous solution, and then 3 parts by weight of activated hollow glass microspheres were added, stirred at 75° C. and 200 rpm for 8 h, filtered, and dried to obtain modified hollow glass microspheres;

[0090] 2.5 parts by weight of phenylphosphonyl dichloride and 7 parts by weight of N-(4-aminophenyl)maleimide are added to 80 parts by weight of dimethyl sulfoxide, stirred at room temperature and 500 rpm for 10 minutes, then 1.5 parts by weight of potassium hydroxide are added, heated to 60°C for reaction for 10 hours, dimethyl sulfoxide is removed by vacuum distillation, and dried to obtain an intermediate containing maleimide; 4 parts by weight of the intermediate containing maleimide, 1.5 parts by weight of maleic anhydride and 50 parts by weight of xylene are uniformly mixed, heated to 92°C under a nitrogen atmosphere, then 0.05 parts by weight of azobisisobutyronitrile are added to react for 4 hours, xylene is removed by vacuum distillation, and dried to obtain a functional polymer;

[0091] 3.2 parts by weight of functional polymer were added to 50 parts by weight of dimethyl sulfoxide, stirred at room temperature and 500 rpm for 15 minutes, then 1.6 parts by weight of modified hollow glass microspheres were added, stirred at 70°C and 200 rpm for 6 hours, filtered, and dried to obtain a modified auxiliary agent.

[0092] Comparative Example 5

[0093] The difference between this comparative example and Example 1 is that the preparation method of the modification aid is different, which is as follows: The preparation method of the modification aid comprises the following steps:

[0094] 8 parts by weight of hollow glass microspheres are added to 70 parts by weight of a 3wt% sodium hydroxide aqueous solution, stirred at room temperature and 500 rpm for 25 minutes, filtered, washed with water until neutral, and dried to obtain activated hollow glass microspheres; 5 parts by weight of N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane and 45 parts by weight of a 65wt% ethanol aqueous solution are mixed evenly, and then 3 parts by weight of activated hollow glass microspheres are added, stirred at 75°C and 200 rpm for 8 hours, filtered, and dried to obtain a modified auxiliary agent.

[0095] Comparative Example 6

[0096] The difference between this comparative example and Example 1 is that the preparation method of the modification aid is different, which is as follows: The preparation method of the modification aid comprises the following steps:

[0097] 8 parts by weight of hollow glass microspheres are added to 70 parts by weight of a 3 wt% sodium hydroxide aqueous solution, stirred at room temperature and 500 rpm for 25 min, filtered, washed with water until neutral, and dried to obtain activated hollow glass microspheres; 5 parts by weight of N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane and 45 parts by weight of a 65 wt% ethanol aqueous solution are uniformly mixed, and then 3 parts by weight of activated hollow glass microspheres are added, stirred at 75° C. and 200 rpm for 8 h, filtered, and dried to obtain modified hollow glass microspheres;

[0098] 4 parts by weight of N-(4-aminophenyl)maleimide, 1.5 parts by weight of maleic anhydride and 50 parts by weight of xylene were uniformly mixed, heated to 92° C. under a nitrogen atmosphere, then 0.05 parts by weight of azobisisobutyronitrile was added to react for 4 hours, xylene was removed by vacuum distillation, and dried to obtain a functional polymer;

[0099] 3.2 parts by weight of functional polymer were added to 50 parts by weight of dimethyl sulfoxide, stirred at room temperature and 500 rpm for 15 minutes, then 1.6 parts by weight of modified hollow glass microspheres were added, stirred at 70°C and 200 rpm for 6 hours, filtered, and dried to obtain a modified auxiliary agent.

[0100] Performance Testing

[0101] The performance of the sound insulation rubber synthetic material obtained in Examples 1-3 and Comparative Examples 1-6 of the present application was tested. Among them, the sound insulation performance was measured at room temperature using a 7758 four-microphone standing wave tube (B&K Company of Denmark) (standing wave tube method), the test frequency was 50-1600HZ, and the data of 1000Hz was taken to compare the sound insulation performance. The sample size was: 100mm in diameter and 3mm in thickness. The flame retardant performance (oxygen index) was measured with reference to the standard GB / T2406.2-2009. The aging resistance was measured with reference to the standard GB / T3512-2014, the test conditions were: aging at 100℃ for 168h, the tensile strength and elongation at break of the material before and after aging were measured (GB / T528-2009), and the retention rate was calculated, the retention rate % = mechanical properties after aging / performance before aging × 100%. The results are shown in Table 1.

[0102] Table 1: Performance test results of sound insulation rubber synthetic materials

[0103]

[0104]

[0105] It can be seen from the above performance test results that the sound insulation rubber synthetic materials prepared in Examples 1-3 have excellent sound insulation performance, flame retardant performance and aging resistance, especially the comprehensive performance of the sound insulation rubber synthetic material of Example 1 is the most outstanding. This is because the present invention significantly improves the sound insulation performance, flame retardant performance and aging resistance of the sound insulation rubber synthetic material by adopting specific modification additives and metal oxide composites.

[0106] In comparison, since Comparative Examples 1-6 did not adopt the necessary technical solutions, their corresponding performance tests were significantly worse than those of Examples 1-3. No specific metal oxide composite was used in Comparative Examples 1-2, and no homemade modification additive was used in Comparative Examples 5-6. It can be seen from the results that the sound insulation performance, flame retardancy and aging resistance of the sound insulation rubber synthetic material decreased. The above experimental results further prove the importance of the technical solutions defined in the present invention for its technical effects.

[0107] The above is a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A sound insulation rubber synthetic material, characterized in that: It includes the following raw materials in parts by weight: 60-80 parts by weight of butyl rubber, 20-40 parts by weight of EPDM rubber, 20-30 parts by weight of carbon black, 3-7 parts by weight of metal oxide composite, 7-13 parts by weight of modifying aid, 10-15 parts by weight of vulcanization activator, 2-4 parts by weight of vulcanizing accelerator, 1-3 parts by weight of vulcanizing agent, and 2-5 parts by weight of antioxidant; the metal oxide composite is prepared by calcining and crushing cerium dioxide, titanium dioxide and silicon dioxide; the modifying aid is prepared by functional polymer and modified hollow glass microspheres.

2. The sound insulation rubber synthetic material according to claim 1, characterized in that: The method for preparing the metal oxide composite comprises the following steps: 1-3 parts by weight of cerium dioxide, 2-4 parts by weight of titanium dioxide and 8-12 parts by weight of silicon dioxide are uniformly mixed and then pressed into a cylindrical sample. The cylindrical sample is then calcined, crushed, pulverized and sieved to obtain a metal oxide composite.

3. The sound insulation rubber synthetic material according to claim 2, characterized in that: The method for preparing the metal oxide composite comprises the following steps: 1-3 parts by weight of cerium dioxide, 2-4 parts by weight of titanium dioxide and 8-12 parts by weight of silicon dioxide are mixed evenly, and then pressed into a cylindrical sample under 0.1-0.5MPa conditions, wherein the diameter of the cylindrical sample is 0.5-1cm and the height is 1-2cm. The cylindrical sample is then calcined at 1100-1400°C for 100-200min. After calcination, the cylindrical sample is placed under -160 to -140°C liquid nitrogen conditions for 30-40min of crushing treatment, and then sieved through a 120-180 mesh sieve to obtain a metal oxide composite.

4. The sound insulation rubber synthetic material according to claim 1, characterized in that: The preparation method of the modified auxiliary agent comprises the following steps: 5-10 parts by weight of hollow glass microspheres are added to 60-80 parts by weight of sodium hydroxide aqueous solution, stirred, filtered, washed with water, and dried to obtain activated hollow glass microspheres; 4-6 parts by weight of N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane and 40-50 parts by weight of ethanol aqueous solution are uniformly mixed, and then 2-5 parts by weight of activated hollow glass microspheres are added, heated and stirred, filtered, and dried to obtain modified hollow glass microspheres; 1-4 parts by weight of phenylphosphonyl dichloride and 5-10 parts by weight of N-(4-aminophenyl)maleimide are added to 70-90 parts by weight of dimethyl sulfoxide, stirred, then 1-2 parts by weight of potassium hydroxide are added, heated for reaction, distilled under reduced pressure, and dried to obtain an intermediate containing maleimide; 3-5 parts by weight of the intermediate containing maleimide, 1-2 parts by weight of maleic anhydride and 40-60 parts by weight of xylene are uniformly mixed, heated under a nitrogen atmosphere, then 0.04-0.06 parts by weight of azobisisobutyronitrile are added for reaction, distilled under reduced pressure, and dried to obtain a functional polymer; 2-4 parts by weight of functional polymer are added to 40-60 parts by weight of dimethyl sulfoxide, stirred, and then 1-2 parts by weight of modified hollow glass microspheres are added, heated and stirred, filtered, and dried to obtain a modified auxiliary agent.

5. The sound insulation rubber synthetic material according to claim 4, characterized in that: The preparation method of the modified auxiliary agent comprises the following steps: 5-10 parts by weight of hollow glass microspheres are added to 60-80 parts by weight of 2-5wt% sodium hydroxide aqueous solution, stirred at room temperature and 400-600rpm for 20-30min, filtered, washed with water until neutral, and dried to obtain activated hollow glass microspheres; 4-6 parts by weight of N-(β-aminoethyl)-γ-aminopropylmethyldimethoxysilane and 40-50 parts by weight of 60-70wt% ethanol aqueous solution are mixed uniformly, and then 2-5 parts by weight of activated hollow glass microspheres are added, stirred at 70-80°C and 100-300rpm for 5-10h, filtered, and dried to obtain modified hollow glass microspheres; 1-4 parts by weight of phenylphosphonyl dichloride and 5-10 parts by weight of N-(4-aminophenyl)maleimide are added to 70-90 parts by weight of dimethyl sulfoxide, stirred at room temperature and 400-600 rpm for 7-15 minutes, then 1-2 parts by weight of potassium hydroxide are added, heated to 55-70° C. for reaction for 7-12 hours, dimethyl sulfoxide is removed by reduced pressure distillation, and dried to obtain an intermediate containing maleimide; 3-5 parts by weight of the intermediate containing maleimide, 1-2 parts by weight of maleic anhydride and 40-60 parts by weight of xylene are uniformly mixed, heated to 90-95° C. under a nitrogen atmosphere, then 0.04-0.06 parts by weight of azobisisobutyronitrile are added to react for 3-5 hours, xylene is removed by reduced pressure distillation, and dried to obtain a functional polymer; Add 2-4 parts by weight of functional polymer to 40-60 parts by weight of dimethyl sulfoxide, stir at room temperature and 400-600 rpm for 10-20 minutes, then add 1-2 parts by weight of modified hollow glass microspheres, stir at 65-75°C and 100-300 rpm for 5-8 hours, filter, and dry to obtain a modified auxiliary agent.

6. The sound insulation rubber synthetic material according to claim 1, characterized in that: The vulcanization activator is a mixture of stearic acid and zinc oxide in a weight ratio of 3-5:3; and the vulcanizing agent is sulfur.

7. The sound insulation rubber synthetic material according to claim 1, characterized in that: The vulcanization accelerator is one or a mixture of two or more of N-tert-butyl-2-benzothiazole sulfenamide, N-cyclohexyl-2-benzothiazole sulfenamide, dibenzothiazole disulfide, zinc dimethyldithiocarbamate, and zinc diethyldithiocarbamate; the antioxidant is one or a mixture of two or more of antioxidant RD, antioxidant MB, antioxidant 4010, antioxidant D, and antioxidant BLE.

8. The sound insulation rubber composite material according to claim 7, characterized in that: The vulcanization accelerator is a mixture of N-tert-butyl-2-benzothiazole sulfenamide and zinc diethyldithiocarbamate in a weight ratio of 1:1-3; the antioxidant is a mixture of antioxidant RD and antioxidant MB in a weight ratio of 3:1-3.

9. The method for preparing the sound insulation rubber synthetic material according to any one of claims 1 to 8, characterized in that: The following steps are involved: According to the raw material formula, butyl rubber and EPDM rubber are added to an internal mixer for plasticization for 1-3 minutes, and then carbon black, metal oxide composite, modification aid, vulcanization activator and antioxidant are added and mixed for 2-5 minutes, and then vulcanization accelerator and vulcanizer are added and mixed for 2-5 minutes, and the rubber is discharged to obtain a rubber compound; the rubber compound is placed in an open mixer and thinned for 3-5 times, and then parked for 20-25 hours to obtain a mixed rubber; the mixed rubber is placed on a flat vulcanizer for vulcanization for 20-40 minutes to obtain the sound insulation rubber synthetic material.

10. Use of the sound insulation rubber synthetic material according to any one of claims 1 to 8 in the preparation of building materials and automobile materials.

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