Method for preparing wide-temperature-range damping silicone rubber by dissolving and blending, product and application

Abstract

The invention belongs to the field of organic silicon damping materials, and particularly relates to a method for preparing wide-temperature-range damping silicon rubber through dissolving and blending, a product and application. The preparation method comprises the following steps: dissolving phenyl silicone rubber and MQ resin in a solvent, stirring and mixing, removing the solvent, mixing with a reinforcing filler, standing, adding a vulcanizing agent, mixing, and vulcanizing the obtained mixture to obtain the wide-temperature-range damping silicone rubber. The MQ resin is doped into the phenyl silicone rubber through dissolving and blending, so that formation of larger molecular interpenetration and entanglement between the phenyl silicone rubber and the MQ resin is promoted, more interface areas are formed in a phenyl silicone rubber matrix, and the damping performance and mechanical strength of the composite material are improved.

Description

Technical Field

[0001] The present invention belongs to the field of organic silicon damping materials, and specifically relates to a method for preparing wide-temperature-range damping silicone rubber by dissolution and blending, a product and an application thereof. Background Art

[0002] The information disclosed in this background technology section is only intended to enhance the understanding of the overall background of the invention, and should not necessarily be regarded as an admission or any form of suggestion that the information constitutes the prior art already known to a person skilled in the art.

[0003] Vibration is a ubiquitous challenge in various fields such as mechanical engineering, construction, transportation, and aerospace, with potentially significant impacts. In the aerospace field in particular, vibrations occurring during launch and orbital operation can severely compromise structural stability, disrupt the functionality of critical instruments, and ultimately lead to a shortened spacecraft service life. Damping materials can effectively absorb and dissipate vibration energy, reduce noise, and minimize structural resonances, providing critical protection for spacecraft and their internal systems. Due to the urgent need for long-term functional stability and reliability under harsh environmental conditions, damping materials for aerospace applications must be lightweight, mechanically robust, and have excellent resistance to extreme temperatures, corrosion, and aging. Compared with traditional alloy-based damping materials, viscoelastic damping materials exhibit superior performance over a wider frequency range, while having lower density, better processing performance, stronger corrosion resistance, and lower cost. As a result, viscoelastic damping materials have become the first choice for vibration control in aerospace applications.

[0004] Among viscoelastic damping materials, silicone rubber has obvious advantages over traditional rubber due to its -Si-O-Si- skeleton. On the one hand, the bond energy of Si-O-Si bond (460 kJ / mol) is significantly higher than that of CC bond (346 kJ / mol), and on the other hand, Si-O-Si bond has longer bonding length and larger bonding angle. This unique structure gives silicone rubber extraordinary resistance to extreme temperatures, weather resistance, aging resistance and excellent elasticity retention, making it particularly suitable for applications in harsh environments. However, the inherent flexibility of silicone rubber and its weak intermolecular interactions limit its damping performance. In order to improve the damping performance, the introduction of phenyl groups into silicone rubber can improve the damping characteristics, but it is still difficult to meet the effective damping requirements under a wide temperature range.

[0005] Damping fillers (damping additives) include particles, flakes, fibers and nanoscale fillers, which can be introduced into the silicone rubber matrix by mechanical blending to improve the damping performance of silicone rubber. The previous patent 202410078263.8 synthesized MQ resin as a silicone rubber damping additive and incorporated it into phenyl silicone rubber by mechanical blending. Although the phenyl silicone rubber composite material prepared by mechanical blending exhibits excellent damping properties, the mechanical blending method can only ensure that the MQ resin is evenly dispersed in the silicone rubber due to the presence of only mechanical shear force. Only the surface hydroxyl and phenyl groups of the MQ resin can interact with the phenyl silicone rubber, making it difficult to achieve effective damping in high temperature environments, which is not conducive to application in harsh environments. Summary of the invention

[0006] In order to solve the deficiencies of the prior art, the present invention provides a method, product and application for preparing wide temperature range damping silicone rubber by dissolution blending. The present invention incorporates MQ resin into phenyl silicone rubber by dissolution blending, which promotes the formation of greater molecular interpenetration and entanglement between phenyl silicone rubber and MQ resin, thereby forming more interface areas in the phenyl silicone rubber matrix, and improving the damping performance and mechanical strength of the composite material.

[0007] In order to achieve the above object, the present invention is implemented through the following technical solutions: In a first aspect, the present invention provides a method for preparing a wide temperature range damping silicone rubber by dissolution blending, comprising the following steps: The phenyl silicone rubber and the MQ resin are dissolved in a solvent, stirred and mixed, and then the solvent is removed, mixed with a reinforcing filler, and then allowed to stand, and then a vulcanizing agent is added and mixed, and the obtained mixture is vulcanized to obtain a wide temperature range damping silicone rubber; The molar ratio of M / Q of the MQ resin is 0.5 to 0.9, and the structure of the M unit is , wherein R1, R2, and R3 are independently selected from one of an alkyl group and an aryl group, and at least one of R1, R2, and R3 is an aryl group.

[0008] Preferably, the mass ratio of the MQ resin to the silicone rubber is (0.2-0.4):1.

[0009] Preferably, the alkyl group is an alkyl group having 1 to 6 carbon atoms, and the aryl group is a phenyl group or a biphenyl group.

[0010] Preferably, the preparation method of the MQ resin comprises the following steps: Tetraethyl orthosilicate, water, an acid catalyst and a solubilizer are stirred and mixed, and then the M monomer is added dropwise to react. After the reaction is completed, toluene is added, and the obtained MQ resin toluene solution is washed with deionized water, the solvent is removed, washed with ethanol, and dried to obtain MQ resin.

[0011] Further preferably, the acid catalyst comprises hydrochloric acid, and the solubilizer comprises ethanol.

[0012] More preferably, the reaction temperature is 60-80° C. and the reaction time is 3-5 h.

[0013] Preferably, the phenyl silicone rubber comprises monophenyl silicone rubber, and the phenyl content of the phenyl silicone rubber is 20-40 mol%.

[0014] Preferably, the reinforcing filler includes fumed silica, the vulcanizing agent includes bis(2,4-dimethylsiloxane), and the mass ratio of the reinforcing filler, the vulcanizing agent and the silicone rubber is (0.4-0.6):(0.01-0.03):1.

[0015] Preferably, the solvent comprises dichloromethane.

[0016] Preferably, the silicone rubber and MQ resin are dissolved in a solvent, stirred and mixed at room temperature for 12 to 36 hours; and after being mixed with the reinforcing filler, the mixture is allowed to stand at room temperature for 12 to 36 hours.

[0017] Preferably, the vulcanization includes primary vulcanization and secondary vulcanization; the temperature of the primary vulcanization is 100-120°C, the pressure is 5-15 MPa, and the time is 5-15 min; the temperature of the secondary vulcanization is 170-190°C, and the time is 3-5 h.

[0018] In a second aspect, the present invention provides a wide temperature range damping silicone rubber obtained by the method described in the first aspect.

[0019] In a third aspect, the present invention provides use of the wide temperature range damping silicone rubber as described in the second aspect in preparing a damping material and / or a damping device.

[0020] The beneficial effects achieved by one or more technical solutions of the present invention are as follows: The present invention incorporates MQ resin into phenyl silicone rubber by dissolving and blending, thereby avoiding the aggregation of MQ resin caused by mechanical blending, promoting more significant molecular interpenetration and entanglement between phenyl silicone rubber and MQ resin, so that thicker tightly bound rubber layers and loosely bound rubber layers are formed in the composite material, thereby expanding the interface area and generating more interface effects, and improving the damping performance and mechanical strength of the composite material.

[0021] The invention prepares wide temperature range damping silicone rubber by dissolution blending. Compared with the damping silicone rubber prepared by mechanical blending, the wide temperature range damping silicone rubber has a wider Tanδ>0.3 damping temperature range and Tanδ>0.2 damping temperature range, can effectively buffer the impact of a falling steel ball, and has better mechanical properties, meets the anti-vibration needs in harsh environments, and broadens the application field of silicone rubber materials.

[0022] The present invention further regulates the M / Q molar ratio in the MQ resin, proves the universality of dissolution blending for different MQ resins, and points out the direction for further modification of high-damping silicone rubber in a wide temperature range. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] The accompanying drawings in the specification, which constitute a part of the present invention, are used to provide a further understanding of the present invention. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute improper limitations on the present invention.

[0024] Figure 1 DMA curves of the wide temperature range high damping silicone rubber in Examples 1 to 5, the MBDC in Comparative Example 1, and the blank silicone rubber in Comparative Example 2; Figure 2 : The stress-strain curves of the wide temperature range high damping silicone rubber in Examples 1 to 5, the MBDC in Comparative Example 1, and the blank silicone rubber in Comparative Example 2; Figure 3 is the cross-linking chain density of the wide temperature range high damping silicone rubber in Examples 1 to 5, the MBDC in Comparative Example 1, and the blank silicone rubber in Comparative Example 2; Figure 4 AFM modulus images of (a) DBDC in Example 1, (b) MBDC in Comparative Example 1, and (c) blank silicone rubber in Comparative Example 2; Figure 5 DSC curves of (a) uncured DBDC in Example 1, (b) uncured MBDC in Comparative Example 1, and (c) phenyl silicone rubber; Figure 6 AFM-QNM modulus images of (a) DBDC in Example 1, (b) MBDC in Comparative Example 1, and (c) blank silicone rubber in Comparative Example 2, and modulus displacement curves of the interface region marked by dashed lines in the AFM-QNM modulus images of (d) DBDC in Example 1, (e) MBDC in Comparative Example 1, and (f) blank silicone rubber in Comparative Example 2; Figure 7 Schematic diagram of the damping enhancement mechanism of DBDC. DETAILED DESCRIPTION

[0025] In order to enable those skilled in the art to more clearly understand the technical solution of the present invention, the technical solution of the present invention will be described in detail below in combination with specific embodiments and comparative examples.

[0026] Example 1 208 g of tetraethyl orthosilicate, 120 mL of water, 12 mL of concentrated hydrochloric acid (mass fraction of 36%) and 50 g of ethanol were stirred and mixed, and then 185.6 g (molar weight of 80% of tetraethyl orthosilicate) of diphenylmethylsilyl chloride was added dropwise, and the mixture was stirred at 70°C for 4 hours for reaction. After the reaction, toluene was added to promote the extraction of MQ resin. The MQ resin toluene solution was washed with deionized water until it reached a natural pH value. The toluene solvent was removed by a rotary evaporator, and then washed three times with anhydrous ethanol and then dried in an oven to obtain MQ resin, which was recorded as 0.8M / Q.

[0027] 100 parts by weight of phenyl silicone rubber (phenyl content of 30 mol%) and 30 parts by weight of MQ resin (0.8M / Q) were dissolved in dichloromethane, stirred and mixed at room temperature for 24 hours, and then the solvent dichloromethane was removed in an oven; the above mixture and 50 parts by weight of fumed silica were added to a dense refiner, fully mixed at room temperature, and then passed through a hole opener for 5 minutes and allowed to stand for 24 hours; finally, 2 parts by weight of double 2,4 were added using a double-roll open grinder at 25°C to obtain a mixture. The mixture was transferred to a metal mold, vacuum vulcanized at 110°C and 10 MPa for 10 minutes using a vacuum plate vulcanizer, and then secondary vulcanized in a blast furnace at 180°C for 4 hours to obtain a wide temperature range high damping silicone rubber, recorded as DBDC.

[0028] Example 2 Different from Example 1, 116 g (molar weight is 50% of tetraethyl orthosilicate) of diphenylmethylchlorosilane was added dropwise, and the obtained MQ resin was recorded as 0.5M / Q. 0.5M / Q was used to prepare high-damping silicone rubber with a wide temperature range.

[0029] Example 3 Different from Example 1, 139.2 g (molar weight is 60% of tetraethyl orthosilicate) of diphenylmethylchlorosilane was added dropwise, and the obtained MQ resin was recorded as 0.6M / Q. 0.6M / Q was used to prepare high-damping silicone rubber with a wide temperature range.

[0030] Example 4 Different from Example 1, 162.4 g (molar weight is 70% of tetraethyl orthosilicate) of diphenylmethylchlorosilane was added dropwise, and the obtained MQ resin was recorded as 0.7M / Q. 0.7M / Q was used to prepare high-damping silicone rubber with a wide temperature range.

[0031] Example 5 Different from Example 1, 208.8 g (molar weight is 90% of tetraethyl orthosilicate) of diphenylmethylchlorosilane was added dropwise, and the obtained MQ resin was recorded as 0.9M / Q. 0.9M / Q was used to prepare high-damping silicone rubber with a wide temperature range.

[0032] MQ resins with different M / Q molar ratios were characterized, and the results are shown in Table 1. As the M / Q molar ratio increases, the molecular weight and particle size of the MQ resin decrease.

[0033] Table 1 Parameters of different MQ resins

[0034] Dynamic mechanical tests were performed on the wide temperature range high damping silicone rubber obtained in Examples 1 to 5 under tensile mode, 1 Hz and different temperatures. Figure 1 As shown in the figure, the damping coefficient of the wide temperature range high damping silicone rubber prepared from different MQ resins has the same trend of changing with temperature. The damping performance shows a trend of first increasing and then decreasing with the increase of M / Q molar ratio, and reaches a peak value when the M / Q molar ratio is 0.8. Further stress-strain tests were conducted on the wide temperature range high damping silicone rubber, such as Figure 2 As shown in the figure, the mechanical properties also show a trend of first increasing and then decreasing with the increase of M / Q molar ratio and reach a peak value at an M / Q molar ratio of 0.8. M monomer (such as diphenylmethylchlorosilane) is used as a capping agent. Increasing M monomer will reduce the molecular weight and particle size of MQ resin, and also reduce its crosslinking density, so that MQ resin has higher solubility and can achieve greater interpenetration and entanglement with phenyl silicone rubber chains during solvent blending. In addition, as the M / Q molar ratio increases, the phenyl content in MQ resin will also increase, thereby enhancing the π-π interaction between MQ resin and phenyl silicone rubber. The stronger interaction significantly improves the damping and mechanical properties of wide temperature range high damping silicone rubber. However, when the M / Q molar ratio becomes too high, the molecular weight of MQ resin decreases too much, resulting in a resin core that is too small to provide sufficient mechanical strength, and the damping performance at high temperature may be impaired, thereby limiting the effectiveness of wide temperature range high damping silicone rubber.

[0035] Comparative Example 1 100 parts by weight of phenyl silicone rubber (phenyl content of 30 mol%) and 50 parts by weight of fumed silica were mixed in an internal mixer, then transferred to a two-roll open mill, and 30 parts by weight of MQ resin (0.8M / Q) and 2 parts by weight of double 2,4 were added and mixed at 25°C. The mixed rubber was transferred to a metal mold, and vacuum cured at 110°C and 10 MPa for 10 minutes using a vacuum flat vulcanizer, and then secondary vulcanized in a blast oven at 180°C for 4 hours to obtain a mechanically blended damping silicone rubber, recorded as MBDC.

[0036] Comparative Example 2 100 parts by weight of phenyl silicone rubber (phenyl content of 30 mol%) and 50 parts by weight of fumed silica were added to an internal mixer, fully mixed at room temperature, and then thinned for 5 minutes using an open mixer, and allowed to stand for 24 hours; finally, 2 parts by weight of bis-2,4 was added using an open mixer at 25°C to obtain a mixed rubber. The mixed rubber was transferred to a metal mold, and vacuum vulcanized at 110°C and 10 MPa for 10 minutes using a vacuum plate vulcanizer, and then secondary vulcanized in a blast oven at 180°C for 4 hours to obtain a blank silicone rubber.

[0037] Dynamic mechanical tests were performed on MBDC and blank silicone rubber and compared with DBDC. The results are as follows: Figure 1 As shown. Near the glass transition temperature (Tg), the order of tanδ is: blank silicone rubber>MBDC>DBDC. However, at higher temperatures, the order is DBDC>MBDC>blank silicone rubber. When the temperature is below Tg, phenyl silicone rubber is still in a glassy state, and the movement of its molecular chains is significantly restricted. As the temperature increases, the chain segments gradually change from a frozen state to an active state. The movement of the molecular chain needs to overcome the cohesive force between molecules, resulting in the absorption and dissipation of energy. The addition of MQ resin introduces bulky phenyl groups, which further hinders the segmental movement of phenyl silicone rubber, so the tanδ of MBDC and DBDC near Tg is lower than that of the blank sample. Among them, DBDC is the lowest, which is attributed to the stronger molecular interpenetration and entanglement between MQ resin and phenyl silicone rubber, which imposes greater restrictions on chain movement. Above Tg, the mobility of the phenyl silicone rubber chain increases, and the phenyl groups in the MQ resin produce π-π interactions and hydrogen bonds with the phenyl silicone rubber molecules, which can significantly improve the damping properties of the composite material. These interactions significantly improve the damping properties of the composite material. In addition, the mutual penetration and entanglement between molecular chains produce more interfacial interactions, further improving the damping performance. The greater molecular interpenetration and entanglement between MQ resin and phenyl silicone rubber chains in DBDC improves its high-temperature tanδ. The damping temperature range of Tanδ>0.3 and Tanδ>0.2 are 139℃ and 235℃, respectively, which are significantly wider than 110℃ and 207℃ of MBDC.

[0038] like Figure 2 As shown, the blank silicone rubber exhibits the highest tensile strength and Young's modulus, with a tensile strength of 10.1 MPa and an elongation at break of 340%. In contrast, MBDC has the lowest tensile strength of 6.5 MPa and an elongation at break of 380%. The mechanical properties of DBDC are improved compared to MBDC, with a tensile strength of 7 MPa and an elongation at break of 448%. Low-field nuclear magnetic resonance tests were performed on the blank silicone rubber, MBDC, and the wide temperature range high damping silicone rubber of Examples 1 to 5, and the cross-linking chain density was calculated, as shown in FIG. Figure 3MBDC and wide temperature range high damping silicone rubber have similar crosslinking density and are lower than blank silicone rubber. Since MQ resin does not participate in crosslinking, the mechanical properties of MBDC and wide temperature range high damping silicone rubber are lower than those of blank silicone rubber. However, wide temperature range high damping silicone rubber contains more bound rubber and thus produces more interface effects, which makes it have better mechanical properties than MBDC.

[0039] AFM modulus image ( Figure 4 ) shows that the low modulus region corresponds to the silicone rubber matrix, while the high modulus region corresponds to the filler. The smaller aggregates in the high modulus region are SiO2, and the larger aggregates are MQ resin. The distribution of SiO2 and MQ resin in phenyl silicone rubber forms a characteristic "island" structure. Both DBDC and MBDC show that the distribution of MQ resin in phenyl silicone rubber is relatively uniform. The aggregates in MBDC are larger and more numerous, while the aggregates in DBDC are smaller and more uniformly distributed. This difference is attributed to the solvent blending process, which allows the MQ resin molecular chains to interpenetrate and entangle with the phenyl silicone rubber chains, effectively dissolving part of the MQ resin in the matrix and reducing the number of aggregates. In contrast, the mechanical blending process does not involve a solvent, resulting in larger MQ resin aggregates in MBDC.

[0040] Differential scanning calorimetry (DSC) was used to measure the heat capacity jump (ΔCp) of pure phenyl silicone rubber (unvulcanized phenyl silicone rubber raw rubber), MBDC (unvulcanized compound rubber) and DBDC (unvulcanized compound rubber) (DSC curves are shown in Figure 5 The Tg and ΔCp values ​​of each sample were obtained from the DSC curves, and the normalized heat capacity jump (ΔC pn ), the mass fraction of polymer segments in the interface region (χ im ): ΔC pn =ΔC p / (1- )(1) χ im =(ΔC p0 -ΔC pn ) / ΔC p0 (2) In the formula, ω represents the mass fraction of filler in the composite material, and ΔC p0 It indicates the heat capacity jump of pure phenyl silicone rubber near Tg.

[0041] Table 2 Tg and ΔC of pure phenyl silicone rubber, MBDC and DBDC p , ΔC pn and χ im

[0042] As shown in Table 2, DBDC contains a higher proportion of polymer segments in the interfacial region. This indicates that the solution blending method helps to form more bonded rubber between MQ resin and phenyl silicone rubber, thereby forming more interfacial regions in DBDC. Figure 6 As shown in Figure 2, the AFM-QNM modulus images of blank silicone rubber, MBDC, and DBDC were obtained, and then the interface area marked by the dashed line was quantitatively analyzed. The filler in the rubber can form a bound rubber (BR) layer with the rubber molecules, and this bound rubber layer can be divided into a tightly bound rubber (TBR) layer formed by chemical adsorption and a loosely bound rubber (LBR) layer formed by physical adsorption and mechanical entanglement. In summary, the damping enhancement mechanism of DBDC is as follows: Figure 7 As shown in Figure 2, DBDC prepared by solution blending exhibits a thicker bound rubber layer compared to MBDC. During the preparation of DBDC, MQ resin and phenyl silicone rubber are dissolved in an organic solvent to allow their molecular chains to move freely. Under stirring, the interpenetration and entanglement of the molecular chains are promoted, while the aggregation of MQ resin is reduced. As a result, more interactions and hydrogen bonds occur between MQ resin and phenyl silicone rubber. After the solvent is removed, a thicker TBR layer is formed in DBDC, and this thicker TBR layer facilitates additional physical adsorption and mechanical entanglement with the external rubber matrix, resulting in a thicker LBR layer. In contrast, only mechanical forces are involved in the preparation of MBDC. Although MQ resin is uniformly dispersed in the phenyl silicone rubber matrix, it aggregates during the mixing process. In this case, π-π interactions and hydrogen bonds are limited to the surface of MQ aggregates, while the phenyl groups and hydrogen bonds within the aggregates cannot interact with the phenyl silicone rubber, resulting in a significantly thinner bonded rubber layer. In DBDC, the higher bound rubber content increases the interfacial area within the composite, and the rubber molecules in these interfacial areas undergo nonlinear deformation under the action of external forces, enhancing energy dissipation and improving complex damping performance.

[0043] Example 6 100 parts by weight of phenyl silicone rubber (phenyl content is 20 mol%) and 20 parts by weight of MQ resin (0.8M / Q) were dissolved in dichloromethane, stirred and mixed at room temperature for 24 hours, and then the solvent dichloromethane was removed in an oven; the above mixture and 40 parts by weight of fumed silica were added to an internal mixer, fully mixed at room temperature, and then thinly passed through an open mixer for 5 minutes and allowed to stand for 24 hours; finally, 1 part by weight of double 2,4 was added to the open mixer at 25°C to obtain a mixed rubber. The mixed rubber was transferred to a metal mold, vacuum vulcanized at 110°C and 10 MPa for 10 minutes using a vacuum flat vulcanizer, and then secondary vulcanized in a blast oven at 180°C for 4 hours to obtain a wide temperature range high damping silicone rubber.

[0044] Example 7 100 parts by weight of phenyl silicone rubber (phenyl content of 40 mol%) and 40 parts by weight of MQ resin (0.8M / Q) were dissolved in dichloromethane, stirred and mixed at room temperature for 24 hours, and then the solvent dichloromethane was removed in an oven; the above mixture and 60 parts by weight of fumed silica were added to an internal mixer, fully mixed at room temperature, and then thinly passed through an open mixer for 5 minutes and allowed to stand for 24 hours; finally, 3 parts by weight of double 2,4 were added to an open mixer at 25°C to obtain a rubber compound. The rubber compound was transferred to a metal mold, vacuum vulcanized at 110°C and 10 MPa for 10 minutes using a vacuum flat vulcanizer, and then secondary vulcanized in a blast oven at 180°C for 4 hours to obtain a high-damping silicone rubber with a wide temperature range.

[0045] Example 8 100 parts by weight of phenyl silicone rubber (phenyl content of 30 mol%) and 30 parts by weight of MQ resin (0.8M / Q) were dissolved in dichloromethane, stirred and mixed at room temperature for 24 hours, and then the solvent dichloromethane was removed in an oven; the above mixture and 50 parts by weight of fumed silica were added to an internal mixer, fully mixed at room temperature, and then thinly passed through an open mixer for 5 minutes, and allowed to stand for 24 hours; finally, 2 parts by weight of double 2,4 were added to an open mixer at 25°C to obtain a rubber compound. The rubber compound was transferred to a metal mold, vacuum vulcanized at 120°C and 15 MPa for 5 minutes using a vacuum flat vulcanizer, and then secondary vulcanized in a blast oven at 170°C for 3 hours to obtain a high-damping silicone rubber with a wide temperature range.

[0046] Example 9 100 parts by weight of phenyl silicone rubber (phenyl content is 30 mol%) and 30 parts by weight of MQ resin (0.8M / Q) were dissolved in dichloromethane, stirred and mixed at room temperature for 24 hours, and then the solvent dichloromethane was removed in an oven; the above mixture and 50 parts by weight of fumed silica were added to an internal mixer, fully mixed at room temperature, and then thinly passed through an open mixer for 5 minutes and allowed to stand for 24 hours; finally, 2 parts by weight of double 2,4 were added to an open mixer at 25°C to obtain a rubber compound. The rubber compound was transferred to a metal mold, vacuum vulcanized at 100°C and 5 MPa for 15 minutes using a vacuum flat vulcanizer, and then secondary vulcanized in a blast oven at 190°C for 5 hours to obtain a high-damping silicone rubber with a wide temperature range.

[0047] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for preparing a wide temperature range damping silicone rubber by dissolving and blending, characterized in that: The following steps are involved: The phenyl silicone rubber and the MQ resin are dissolved in a solvent, stirred and mixed, and then the solvent is removed, mixed with a reinforcing filler, and then allowed to stand, and then a vulcanizing agent is added and mixed, and the obtained mixture is vulcanized to obtain a wide temperature range damping silicone rubber; The molar ratio of M / Q of the MQ resin is 0.5 to 0.9, and the structure of the M unit is , wherein R1, R2, and R3 are independently selected from one of an alkyl group and an aryl group, and at least one of R1, R2, and R3 is an aryl group.

2. The method according to claim 1, characterized in that The mass ratio of the MQ resin to the silicone rubber is (0.2-0.4):

1.

3. The method according to claim 1, characterized in that The alkyl group is an alkyl group having 1 to 6 carbon atoms, and the aryl group is a phenyl group or a biphenyl group.

4. The method according to claim 1, characterized in that The phenyl silicone rubber includes monophenyl silicone rubber, and the phenyl content of the phenyl silicone rubber is 20-40 mol%.

5. The method according to claim 1, characterized in that The reinforcing filler includes fumed silica, the vulcanizing agent includes di-2,4, and the mass ratio of the reinforcing filler, the vulcanizing agent and the silicone rubber is (0.4-0.6):(0.01-0.03):

1.

6. The method according to claim 1, characterized in that The solvent includes dichloromethane.

7. The method according to claim 1, characterized in that Dissolve silicone rubber and MQ resin in a solvent, stir and mix at room temperature for 12 to 36 hours; after mixing with reinforcing fillers, let stand at room temperature for 12 to 36 hours.

8. The method according to claim 1, characterized in that Vulcanization includes primary vulcanization and secondary vulcanization; the temperature of primary vulcanization is 100~120℃, the pressure is 5~15 MPa, and the time is 5~15 min; the temperature of secondary vulcanization is 170~190℃, and the time is 3~5 h.

9. A wide temperature range damping silicone rubber, characterized in that: Obtained by the method according to any one of claims 1 to 7.

10. Use of the wide temperature range damping silicone rubber according to claim 8 in preparing damping materials and / or damping devices.

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