Butyl rubber composition, vulcanized butyl rubber and preparation method and application thereof

Abstract

The invention relates to the field of rubber, and discloses a butyl rubber composition and vulcanized butyl rubber as well as a preparation method and application thereof. The composition comprises the following components in parts by weight: 100 parts of butyl rubber, 10-40 parts of a reinforcing agent, 5-30 parts of tackifying resin, 3-10 parts of an activating agent, 0.5-3 parts of a vulcanizing agent and 0.5-3 parts of an accelerant, wherein the tackifying resin comprises tackifying resin A and tackifying resin B; the tackifying resin A is C5 resin; the tackifying resin B is selected from at least one of octyl phenolic vulcanized resin, brominated octyl phenolic resin, epoxy resin and aliphatic hydrocarbon resin. The rubber composition contains two specific types of tackifying resins and cooperates with a specific content of the reinforcing agent, so that the damping temperature range of a high-temperature region of butyl rubber can be widened on the premise of ensuring that vulcanized rubber prepared from the rubber composition has relatively good mechanical properties.

Description

Technical Field

[0001] The invention relates to the field of rubber, and in particular to a butyl rubber composition and vulcanized butyl rubber, and a preparation method and application thereof. Background Art

[0002] Butyl rubber is a high molecular polymer obtained by cationic polymerization of isobutylene and a small amount of isoprene. Its molecular structure contains dense side methyl groups. During the relaxation of the chain segments, the steric effect increases the internal friction between the rubber molecular chains, resulting in large energy loss, and thus exhibits excellent damping performance. The unique structure makes butyl rubber have excellent damping performance at low temperature and room temperature, but its damping performance is low in the high temperature zone. Therefore, the key to improving the damping performance of butyl rubber is to study and improve its damping performance in the high temperature zone.

[0003] The selection of appropriate polymer blends, the addition of small molecule fillers, special vulcanization methods and vulcanization systems are all important means to effectively broaden the damping temperature range of butyl rubber. Among them, adding resin to the rubber matrix has become a method for preparing new high-damping rubber composite materials. Strong van der Waals forces are formed between the resin and the rubber molecules, thereby limiting the movement of the rubber molecular chain, shifting the glass transition temperature to high temperature, and broadening its damping temperature range. Summary of the invention

[0004] The purpose of the present invention is to overcome the narrow damping temperature range of butyl rubber and the low damping performance in the high temperature zone, and to provide a butyl rubber composition and a vulcanized butyl rubber and a preparation method and application thereof. The rubber composition contains two specific types of tackifying resins and a specific content of reinforcing agent, which can ensure that the vulcanized rubber prepared from the rubber composition has good mechanical properties and broaden the damping temperature range of the butyl rubber in the high temperature zone.

[0005] In order to achieve the above object, the first aspect of the present invention provides a rubber composition, characterized in that, in parts by weight, the composition comprises: 100 parts of butyl rubber, 10-40 parts of reinforcing agent, 5-30 parts of tackifying resin, 3-10 parts of activator, 0.5-3 parts of vulcanizing agent and 0.5-3 parts of accelerator;

[0006] Wherein, the tackifying resin includes tackifying resin A and tackifying resin B;

[0007] The tackifying resin A is C5 resin; the tackifying resin B is at least one selected from octylphenolformaldehyde vulcanized resin, brominated octylphenolformaldehyde resin, epoxy resin and aliphatic hydrocarbon resin.

[0008] A second aspect of the present invention provides a method for preparing vulcanized rubber, characterized in that the rubber composition described in the first aspect is mixed and vulcanized.

[0009] The third aspect of the present invention provides a vulcanized rubber prepared by the method described in the second aspect.

[0010] The fourth aspect of the present invention provides a use of the vulcanized rubber described in the third aspect in a damping material.

[0011] Through the above technical scheme, the butyl rubber composition and vulcanized butyl rubber provided by the present invention and the preparation method and application thereof obtain the following beneficial effects:

[0012] The butyl rubber composition of the present invention contains two specific types of tackifying resins, which can form strong van der Waals forces with rubber molecules, thereby limiting the movement of rubber molecular chains, shifting the glass transition temperature to high temperature, and widening its damping temperature range; and at the same time, synergistically cooperating with a specific content of reinforcing agent, it can ensure that the mechanical properties of the vulcanized rubber prepared from the rubber composition meet the use requirements under the premise of a wider damping temperature range.

[0013] Furthermore, when two tackifying resins are mixed in a specific ratio, the damping performance of the vulcanized rubber prepared from the composition can be further improved. DETAILED DESCRIPTION

[0014] The endpoints and any values ​​of the ranges disclosed in this article are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of each range, the endpoint values ​​of each range and the individual point values, and the individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed in this article.

[0015] The first aspect of the present invention provides a butyl rubber composition, characterized in that the composition comprises, by weight: 100 parts of butyl rubber, 10-40 parts of reinforcing agent, 5-30 parts of tackifying resin, 3-10 parts of activator, 0.5-3 parts of vulcanizing agent and 0.5-3 parts of accelerator;

[0016] Wherein, the tackifying resin includes tackifying resin A and tackifying resin B;

[0017] The tackifying resin A is C5 resin; the tackifying resin B is at least one selected from octylphenolformaldehyde vulcanized resin, brominated octylphenolformaldehyde resin, epoxy resin and aliphatic hydrocarbon resin.

[0018] In the present invention, the butyl rubber composition contains two specific types of tackifying resins, which can form strong van der Waals forces with rubber molecules, thereby limiting the movement of rubber molecular chains, shifting the glass transition temperature to high temperature, and broadening its damping temperature range; and at the same time, synergistically cooperating with a specific content of reinforcing agent, it can ensure that the mechanical properties of the vulcanized rubber prepared from the rubber composition meet the use requirements under the premise of a wider damping temperature range.

[0019] Furthermore, the composition comprises, by weight: 100 parts of butyl rubber, 10-30 parts of reinforcing agent, 10-30 parts of tackifying resin, 4-8 parts of activator, 0.5-2 parts of vulcanizing agent and 1-2.5 parts of accelerator.

[0020] In a specific embodiment of the present invention, the tackifying resin A is C5 resin, preferably at least one selected from Wingtack 95 resin, Wingtack 10 resin and Wingtack 98 resin.

[0021] In a specific embodiment of the present invention, the octylphenol formaldehyde vulcanized resin is at least one of resin HY 2045, resin 1045 and resin 1055.

[0022] In a specific embodiment of the present invention, the brominated octylphenol-formaldehyde resin is resin 1055, resin 2055, etc.

[0023] In a specific embodiment of the present invention, the epoxy resin is resin 711, resin E51, resin 618, etc.

[0024] In a specific embodiment of the present invention, the aliphatic hydrocarbon resin is resin 1102, resin 1202, etc.

[0025] In the present invention, the inventors found that when the tackifying resin B is aliphatic hydrocarbon resin 1102, it can cooperate better with other components and further improve the comprehensive performance of the vulcanized rubber.

[0026] According to the present invention, the reinforcing agent is carbon black.

[0027] According to the present invention, the mass ratio of the tackifying resin A to the tackifying resin B is 1-5:1.

[0028] In the present invention, when the mass ratio of the tackifier resin A to the tackifier resin B satisfies the above range, the damping performance of the vulcanized rubber prepared from the composition can be further improved.

[0029] Furthermore, the mass ratio of the tackifying resin A to the tackifying resin B is 1-4:1.

[0030] According to the present invention, the total weight of the reinforcing agent and the tackifying resin is 15-70 parts relative to 100 parts by weight of the butyl rubber.

[0031] In the present invention, the inventors have found that the type of tackifying resin is closely related to the total amount of the reinforcing agent and the tackifying resin. When the relationship between them satisfies the above range, the mechanical properties of the prepared vulcanized rubber can be further improved under the premise of having a wide damping temperature range.

[0032] Furthermore, relative to 100 parts by weight of the butyl rubber, the total weight of the reinforcing agent and the tackifying resin is 20-60 parts.

[0033] According to the present invention, the unsaturation degree of the butyl rubber is 0.8-2.2 mol%, preferably 1-2 mol%.

[0034] According to the present invention, the number average molecular weight of the butyl rubber is 120,000-300,000, preferably 120,000-200,000.

[0035] According to the present invention, the Mooney viscosity ML (1+8min, 125°C) of the butyl rubber is 30-65.

[0036] In the present invention, the butyl rubber may be a halogenated butyl rubber, such as chlorinated butyl rubber and / or brominated butyl rubber.

[0037] According to the present invention, the CTAB adsorption specific surface area of ​​the carbon black is 10-600m 2 / g.

[0038] In the present invention, the CTAB adsorption specific surface area of ​​the carbon black satisfies the above range, which can effectively improve the tensile strength of the rubber.

[0039] In the present invention, the CTAB adsorption specific surface area of ​​the carbon black is 10-200m 2 / g.

[0040] According to the present invention, the activator is a mixture of metal oxides and fatty acids.

[0041] According to the present invention, the mass ratio of the metal oxide to the fatty acid is 2-5:1, preferably 3-5:1;

[0042] According to the present invention, the metal oxide is zinc oxide and / or magnesium oxide; the fatty acid is stearic acid.

[0043] According to the present invention, the vulcanizing agent is selected from sulfur donors.

[0044] According to the present invention, the vulcanizing agent is selected from at least one of sublimated sulfur, insoluble sulfur, soluble sulfur and oil-extended sulfur.

[0045] According to the present invention, the accelerator is selected from at least one of sulfenamide accelerators, thiazole accelerators, thiuram accelerators and guanidine accelerators.

[0046] According to some embodiments of the present invention, the accelerator is selected from at least one of N-cyclohexyl-2-benzothiazole sulfenamide (CZ), 2-mercaptobenzothiazole (M) and tetramethylthiuram disulfide (TMTD).

[0047] The second aspect of the present invention provides a method for preparing vulcanized butyl rubber, characterized in that the rubber composition described in the first aspect is mixed and vulcanized.

[0048] In the present invention, there is no particular limitation on the method for preparing vulcanized butyl rubber using the aforementioned composition, and the method can be carried out by various methods for preparing vulcanized rubber commonly used in the art, and the basic requirements of the present invention for the performance of the vulcanized rubber can be achieved.

[0049] However, the inventors have found through research that the following method can make the mixing components in the process more uniform, thereby making the vulcanized butyl rubber obtained after subsequent vulcanization have better mechanical properties and damping properties.

[0050] According to the present invention, the method comprises the following steps:

[0051] S1, mixing butyl rubber, tackifying resin, reinforcing agent and activator for the first time to obtain a rubber mixture;

[0052] S2, mixing the rubber mix, the vulcanizing agent and the accelerator for a second time to obtain a final rubber mix;

[0053] S3, vulcanizing the final rubber mixture to obtain the vulcanized rubber.

[0054] According to the present invention, the first mixing conditions include: the first mixing temperature is 40-160° C., preferably 50-160° C.; the time is 3-10 min, preferably 3-8 min.

[0055] According to the present invention, the second mixing conditions include: the second mixing temperature is ≤110°C, preferably 35-110°C; the mixing time is 3-5min, preferably 3-4min.

[0056] In the present invention, in order to obtain better effect, the discharge temperature of the final rubber mixing is ≤110°C.

[0057] According to the present invention, the vulcanization conditions include: temperature of 150-170° C., preferably 150-160° C.; pressure of 5-15 MPa, preferably 8-15 MPa; time of 15-35 min, preferably 15-30 min.

[0058] In the present invention, in order to further obtain vulcanized butyl rubber with better comprehensive performance, the method can also further refine the components in the composition by step mixing, specifically including:

[0059] S1, mixing butyl rubber and tackifying resin for the first time I to obtain a first mixed rubber;

[0060] S2, performing a first mixing II on the first rubber mixture, a reinforcing agent and an activator to obtain a second rubber mixture;

[0061] S3, mixing the second mixed rubber, the vulcanizing agent and the accelerator for the second time to obtain a final mixed rubber;

[0062] S4, vulcanizing the final rubber mixture to obtain the vulcanized rubber.

[0063] In the present invention, the conditions of the first mixing I include: the temperature of the first mixing I is 40-160° C., preferably 50-130° C.; the time is 0.5-5 min, preferably 0.5-3 min.

[0064] In the present invention, the conditions of the first mixing II include: the temperature of the first mixing II is 40-160° C., preferably 50-160° C.; the time is 1-10 min, preferably 3-8 min.

[0065] In the present invention, the sum of the mixing time of the first mixing I and the first mixing II is 3-15 min, preferably 5-15 min.

[0066] In the present invention, the conditions of the second mixing include: the temperature of the second mixing is ≤110°C, preferably 35-110°C; the time is 3-5min, preferably 3-4min.

[0067] In the present invention, in order to obtain better effect, the discharge temperature of the final rubber mixing is ≤110°C.

[0068] In the present invention, in a mixing device (such as an internal mixer), when each component is mixed, the temperature of the system will rise as the mixing proceeds, that is, the mixing temperature is a dynamic temperature increase process, and the mixing temperature in the present invention is a range value, as long as each mixing temperature does not exceed the above range. Specifically, the temperature of the first mixing I does not exceed 160°C, the temperature of the first mixing II does not exceed 160°C, and the temperature of the second mixing does not exceed 110°C.

[0069] In the present invention, the vulcanization conditions are consistent with the above-mentioned vulcanization conditions and will not be described in detail.

[0070] Unless otherwise specified, the pressures used in the present invention are gauge pressures.

[0071] The third aspect of the present invention provides a vulcanized butyl rubber prepared by the method described in the second aspect.

[0072] The fourth aspect of the present invention provides a use of the vulcanized butyl rubber described in the third aspect in a damping material.

[0073] Butyl rubber: brand 1751, unsaturation 1.74 mol%, Mooney viscosity ML (1+8min, 125°C) 51, number average molecular weight 236,000, Sinopec Beijing Yanshan Petrochemical Company;

[0074] Chlorobutyl rubber, brand 1066, unsaturation 1.7 mol%, Mooney viscosity ML (1+8 min, 125°C) 38, chlorine content 1.2±0.1, number average molecular weight 188,000, purchased from Exxon.

[0075] Reinforcement agent: carbon black N330, CTAB is 82m 2 / g, produced by Cabot Corporation.

[0076] Tackifying resin A: Wingtack95, produced by Cray Valley, USA, industrial grade.

[0077] Tackifying resin B1: Resin HY 2045, produced by Shanxi Chemical Research Institute, industrial grade.

[0078] Tackifying resin B2: Resin 1102, produced by ExxonMobil, industrial grade.

[0079] Tackifying resin B3: Resin 711, American Resinall Group, industrial grade.

[0080] Tackifying resin B4: Resin 2123, phenolic resin, purchased from Henan Zhongfan Dongsheng New Materials.

[0081] Resin 1045: thermally reactive octylphenol-formaldehyde resin, purchased from SI Group, USA.

[0082] Activator: zinc oxide (ZnO), stearic acid (SA), Weifang Hengfeng Chemical Co., Ltd.

[0083] Vulcanizing agent: sublimated sulfur, Weifang Zhongheng Chemical Co., Ltd.

[0084] Accelerator: N-cyclohexyl-2-benzothiazolesulfenamide (CZ), Tianjin Maofeng Rubber Additive Co., Ltd.

[0085] The equipment conditions of the vulcanized rubber prepared in the following examples and comparative examples are shown in Table 1.

[0086] The testing instruments of the vulcanized rubber prepared in the following examples and comparative examples are shown in Table 2.

[0087] The test conditions of the vulcanized rubbers prepared in the following examples and comparative examples are shown in Table 3.

[0088] Unless otherwise specified, the temperature ranges in the following examples represent the actual temperature changes displayed by the temperature monitor during the rubber mixing process.

[0089] Table 1

[0090] Serial number Device Name model Manufacturer 1 Internal Mixer BR1600 Farrar Corporation 2 Open Mixing Machine XK-160 Qingdao Xincheng Yiming Rubber Machinery Co., Ltd. 3 Plate vulcanizing press P-50-PCD-3L400×400\50T Taiwan Panshi Hydraulic Industry Co., Ltd.

[0091] Table 2

[0092] Serial number Test items Test instrument model Manufacturer 1 Tensile Strength GT-AT-3000 China Taiwan High Speed ​​Rail Corporation 2 Dynamic viscoelastic properties EPLEXOR500N GABO, Germany

[0093] Table 3

[0094]

[0095] Examples 1-6

[0096] The rubber composition was mixed according to the formulation in Table 4 as follows:

[0097] S1, adding butyl rubber and tackifying resin into an internal mixer for first mixing I, setting the speed of the internal mixer to 77 rpm, setting the initial temperature to 60° C., performing the first mixing I at 60° C. to 110° C. for 0.5 min, and obtaining a first mixed rubber;

[0098] S2, adding the first rubber mix, reinforcing agent and activator into an internal mixer for first mixing II, performing first mixing II at 70° C. to 130° C. for 5 min, discharging and standing for 4 h to obtain a second rubber mix;

[0099] S3, adding the second mixed rubber, accelerator and vulcanizing agent into an internal mixer for second mixing, the rotation speed is 60 rpm, the initial temperature is set to 35°C, the second mixing is carried out at 35°C to 110°C, the time is 4 minutes, the discharge temperature is 110°C, and the final mixed rubber is obtained;

[0100] S4, the final rubber is pressed and cut into pieces by an open mixer and then put into a flat vulcanizing press for vulcanization at a vulcanization temperature of 160°C, a vulcanization pressure of 15 MPa, and a vulcanization time of T. 90 -5min to T 90 +3min, and vulcanized rubber samples S1-S6 were obtained.

[0101] Table 4

[0102]

[0103]

[0104] Example 7

[0105] The method of Example 1 was followed, except that the 2045 resin was replaced by the Wingtack 95 resin, to obtain a vulcanized rubber sample S7.

[0106] Example 8

[0107] The method of Example 1 was followed, except that the butyl rubber was replaced by chlorinated butyl rubber 1066, to obtain a vulcanized rubber sample S8.

[0108] Example 9

[0109] The method of Example 1 was followed, except that the carbon black N330 was replaced by N660, to obtain a vulcanized rubber sample S9.

[0110] Example 10

[0111] The formulation in Example 1 in Table 4 was used to prepare a vulcanized rubber according to the following method.

[0112] S1, adding butyl rubber, tackifying resin, reinforcing agent and activator into an internal mixer for first mixing, setting the speed of the internal mixer to 77 rpm, setting the initial temperature to 60° C., performing the first mixing at 60° C. to 130° C. for 5 min, discharging and standing for 4 h, to obtain a first mixed rubber;

[0113] S2, adding the first mixed rubber, accelerator and vulcanizing agent into an internal mixer for second mixing, the rotation speed is 60 rpm, the initial temperature is set to 35°C, the second mixing is carried out at 35°C to 110°C, the time is 4 minutes, the discharge temperature is 110°C, and the final mixed rubber is obtained;

[0114] S3, the final rubber is pressed and cut into pieces by an open mixer and then put into a flat vulcanizing press for vulcanization at a vulcanization temperature of 160°C, a vulcanization pressure of 15 MPa, and a vulcanization time of T. 90 -5min to T 90 +3min, and obtain the vulcanized rubber sample S10.

[0115] Embodiment 11

[0116] The method of Example 1 was followed, except that the amount of carbon black was changed to 40 parts, to obtain a vulcanized rubber sample S11.

[0117] Example 12

[0118] The method of Example 1 was followed, except that the tackifier resin A was 20 parts and the tackifier resin B was 2 parts, to obtain a vulcanized rubber sample S12.

[0119] Embodiment 13

[0120] The method of Example 1 was followed, except that the tackifying resin B was 2123 resin, to obtain a vulcanized rubber sample S13.

[0121] Comparative Example 1

[0122] The method of Example 1 was followed, except that no tackifying resin was contained, to obtain a vulcanized rubber sample D1.

[0123] Comparative Example 2

[0124] The method of Example 1 was followed, except that tackifier resin B was not contained and tackifier resin A was changed to 5 parts, to obtain a vulcanized rubber sample D2.

[0125] Comparative Example 3

[0126] The method of Example 1 was followed, except that tackifying resin A and tackifying resin B were changed to 30% resin 1045, to obtain vulcanized rubber sample D3.

[0127] Comparative Example 4

[0128] The method of Example 1 was followed, except that tackifier resin B was not contained and tackifier resin A was changed to 50 parts, to obtain vulcanized rubber sample D4.

[0129] Test Case

[0130] The rubber samples prepared in the examples and comparative examples were subjected to performance tests, and the results are shown in Table 5.

[0131] Table 5

[0132]

[0133] It can be seen from the above results that the use of Examples 1-13 of the present invention has better effects. Under the premise of satisfying the tensile strength of not less than 10 MPa, it has a wider temperature range, wherein the temperature difference is not less than 104.6, and the loss factor is not less than 1.1, having a wider temperature range and good mechanical properties and damping properties.

[0134] The preferred embodiments of the present invention are described in detail above, but the present invention is not limited thereto. Within the technical concept of the present invention, the technical solution of the present invention can be subjected to a variety of simple modifications, including the combination of various technical features in any other suitable manner, and these simple modifications and combinations should also be regarded as the contents disclosed by the present invention and belong to the protection scope of the present invention.

Claims

1. A butyl rubber composition, It is characterized in that The composition comprises, by weight: 100 parts of butyl rubber, 10-40 parts of reinforcing agent, 5-30 parts of tackifying resin, 3-10 parts of activator, 0.5-3 parts of vulcanizing agent and 0.5-3 parts of accelerator; Wherein, the tackifying resin includes tackifying resin A and tackifying resin B; The tackifying resin A is C5 resin; the tackifying resin B is at least one selected from octylphenolformaldehyde vulcanized resin, brominated octylphenolformaldehyde resin, epoxy resin and aliphatic hydrocarbon resin.

2. The butyl rubber composition according to claim 1, in, The composition comprises, by weight: 100 parts of butyl rubber, 10-30 parts of reinforcing agent, 10-30 parts of tackifying resin, 4-8 parts of activator, 0.5-2 parts of vulcanizing agent and 1-2.5 parts of accelerator; Preferably, the reinforcing agent is carbon black; Preferably, the mass ratio of the tackifying resin A to the tackifying resin B is 1-5:1, preferably 1-4:

1.

3. The butyl rubber composition according to claim 1 or 2, in, Relative to 100 parts by weight of the butyl rubber, the total weight of the reinforcing agent and the tackifying resin is 15-70 parts, preferably 20-60 parts.

4. The butyl rubber composition according to any one of claims 1 to 3, in, The unsaturation degree of the butyl rubber is 0.8-2.2 mol%, preferably 1-2 mol%; Preferably, the Mooney viscosity ML (1+8min, 125°C) of the butyl rubber is 30-65; Preferably, the number average molecular weight of the butyl rubber is 120,000-300,000, preferably 120,000-200,000.

5. The butyl rubber composition according to any one of claims 1 to 4, in, The CTAB adsorption specific surface area of ​​the carbon black is 10-600m 2 / g, preferably 10-200m 2 / g; Preferably, the activator is a mixture of metal oxides and fatty acids; Preferably, the mass ratio of the metal oxide to the fatty acid is 2-5:1, preferably 3-5:1; Preferably, the metal oxide is zinc oxide and / or magnesium oxide; the fatty acid is stearic acid; Preferably, the vulcanizing agent is selected from sulfur donors; Preferably, the vulcanizing agent is selected from at least one of sublimated sulfur, insoluble sulfur, soluble sulfur and oil-extended sulfur; Preferably, the accelerator is selected from at least one of sulfenamide accelerators, thiazole accelerators, thiuram accelerators and guanidine accelerators.

6. A method for preparing vulcanized butyl rubber, It is characterized in that The butyl rubber composition according to any one of claims 1 to 5 is kneaded and vulcanized.

7. The method according to claim 6, in, The method comprises the following steps: S1, mixing butyl rubber, tackifying resin, reinforcing agent and activator for the first time to obtain a rubber mixture; S2, mixing the rubber mix, the vulcanizing agent and the accelerator for a second time to obtain a final rubber mix; S3, vulcanizing the final rubber mixture to obtain the vulcanized butyl rubber.

8. The method according to claim 7, in, The first mixing conditions include: the first mixing temperature is 40-160° C., preferably 50-160° C.; the time is 3-10 min, preferably 3-8 min; Preferably, the second mixing conditions include: the second mixing temperature is ≤110°C, preferably 35-110°C; the time is 3-5min, preferably 3-4min; Preferably, the vulcanization conditions include: temperature of 150-170° C., preferably 150-160° C.; pressure of 5-15 MPa, preferably 8-15 MPa; time of 15-35 min, preferably 15-30 min.

9. Vulcanized butyl rubber prepared by the method according to any one of claims 6 to 8.

10. Use of the vulcanized butyl rubber according to claim 9 in damping materials.

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