Hydrogenated nitrile rubber composition, vulcanized rubber and preparation method and application thereof

Abstract

The invention relates to the field of rubber, and discloses a hydrogenated butadiene-acrylonitrile rubber composition, vulcanized rubber and a preparation method and application thereof. The hydrogenated butadiene-acrylonitrile rubber composition contains butadiene-acrylonitrile rubber, carbon nanotubes, carbon black, white carbon black, an activator, a plasticizer, an anti-aging agent, a peroxide vulcanizing agent and an auxiliary vulcanizing agent, based on 100 parts of nitrile rubber, 1 to 12 parts of carbon nanotube, 25 to 55 parts of carbon black, 5 to 20 parts of white carbon black, 4 to 12 parts of activator, 3 to 15 parts of plasticizer, 1 to 5 parts of anti-aging agent, 2 to 10 parts of peroxide vulcanizing agent and 1 to 6 parts of auxiliary vulcanizing agent are added; the nitrile rubber comprises 80-96 parts of hydrogenated nitrile rubber and 4-20 parts of hydrogenated carboxyl nitrile rubber. The vulcanized rubber prepared from the composition has relatively high mechanical strength, tear resistance and wear resistance, and meanwhile, the dynamic heat generation of the vulcanized rubber is reduced.

Description

Technical Field

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

[0002] The synchronous belt is a new type of conveyor belt developed by combining the advantages of belt drive, chain drive and gear drive. Since the transmission method of the synchronous belt is to mesh the teeth and grooves of the gear and the synchronous belt pulley, there will be no non-synchronous transmission between the belt and the pulley due to slip during the transmission process. Compared with chain and gear transmission, the synchronous belt transmission has smooth transmission, small impact, no need for lubrication, no pollution, and low noise. Due to the many advantages of synchronous belt transmission, it has developed very rapidly. Due to the increasing requirements of modern automobiles for energy saving, environmental protection, comfort, safety, etc., the entire engine room structure has become more complex and compact, and the working environment in the engine has become more harsh, so the synchronous belt is required to have excellent mechanical strength, tear resistance, wear resistance and low dynamic heat generation performance.

[0003] Therefore, how to improve the performance of synchronous belt materials has become an important research direction. Summary of the invention

[0004] The purpose of the present invention is to overcome the problem that the synchronous belt in the prior art cannot have high mechanical strength, high tear resistance, wear resistance and low dynamic heat generation performance, and to provide a hydrogenated nitrile rubber composition and vulcanized rubber and a preparation method and application thereof. The carbon nanotubes, carbon black and white carbon black in the hydrogenated nitrile rubber composition work together with a specific content of hydrogenated carboxyl nitrile rubber and other components in the composition, so that the vulcanized rubber prepared from the composition has high mechanical strength, tear resistance and wear resistance, and at the same time reduces the dynamic heat generation of the vulcanized rubber.

[0005] In order to achieve the above object, the first aspect of the present invention provides a hydrogenated nitrile rubber composition, wherein the hydrogenated nitrile rubber composition contains one or more of nitrile rubber, carbon nanotubes, carbon black, white carbon black, activator, plasticizer, antioxidant, peroxide vulcanizer and co-vulcanizing agent;

[0006] And relative to 100 parts by weight of nitrile rubber, the content of carbon nanotubes is 1-12 parts by weight, the content of carbon black is 25-55 parts by weight, the content of white carbon black is 5-20 parts by weight, the content of activator is 4-12 parts by weight, the content of plasticizer is 3-15 parts by weight, the content of antioxidant is 1-5 parts by weight, the content of peroxide vulcanizing agent is 2-10 parts by weight, and the content of co-vulcanizing agent is 1-6 parts by weight;

[0007] The nitrile rubber comprises 80-96 parts by weight of hydrogenated nitrile rubber and 4-20 parts by weight of hydrogenated carboxyl nitrile rubber.

[0008] A second aspect of the present invention provides a method for preparing vulcanized rubber from the aforementioned hydrogenated nitrile rubber composition, wherein the method comprises the following steps:

[0009] S1, mixing hydrogenated nitrile rubber, hydrogenated carboxyl nitrile rubber, carbon nanotubes, carbon black, white carbon black, antioxidant and plasticizer for the first time to prepare a masterbatch;

[0010] S2, mixing the activator, the peroxide vulcanizing agent, the co-vulcanizing agent and the first stage of the masterbatch for the second time to obtain a final rubber mix;

[0011] S3, vulcanizing the final rubber mixture to obtain vulcanized rubber.

[0012] The third aspect of the present invention provides a vulcanized rubber prepared by the above-mentioned method.

[0013] A fourth aspect of the present invention provides a use of the aforementioned vulcanized rubber in an automobile timing belt.

[0014] Through the above technical solution, the technical solution provided by the present invention has the following beneficial effects:

[0015] The carbon nanotubes, carbon black and white carbon black in the hydrogenated nitrile rubber composition provided by the present invention work together with a specific amount of hydrogenated carboxyl nitrile rubber and other components in the composition, so that the vulcanized rubber prepared from the composition has higher mechanical strength, tear resistance and wear resistance, and at the same time reduces the dynamic heat generation of the vulcanized rubber. DETAILED DESCRIPTION

[0016] 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.

[0017] As mentioned above, the first aspect of the present invention provides a hydrogenated nitrile rubber composition, wherein the hydrogenated nitrile rubber composition contains one or more of nitrile rubber, carbon nanotubes, carbon black, white carbon black, an activator, a plasticizer, an antioxidant, a peroxide vulcanizer, and a vulcanizing agent;

[0018] And relative to 100 parts by weight of nitrile rubber, the content of carbon nanotubes is 1-12 parts by weight, the content of carbon black is 25-55 parts by weight, the content of white carbon black is 5-20 parts by weight, the content of activator is 4-12 parts by weight, the content of plasticizer is 3-15 parts by weight, the content of antioxidant is 1-5 parts by weight, the content of peroxide vulcanizing agent is 2-10 parts by weight, and the content of co-vulcanizing agent is 1-6 parts by weight;

[0019] The nitrile rubber comprises 80-96 parts by weight of hydrogenated nitrile rubber and 4-20 parts by weight of hydrogenated carboxyl nitrile rubber.

[0020] In the present invention, the inventors of the present invention have found that carbon nanotubes, carbon black and white carbon black work together, synergistically with a specific content of hydrogenated carboxyl nitrile rubber and other components in the composition, and can maintain the vulcanized rubber prepared from the composition with high mechanical strength, reduce dynamic heat generation, and improve tear resistance and wear resistance.

[0021] Furthermore, the inventors of the present invention have found that when the hydrogenated nitrile rubber composition contains the above-mentioned specific types and specific contents of components under synergistic effect, the vulcanized rubber prepared from the composition can reduce dynamic heat generation and improve tear resistance and wear resistance while having high mechanical strength; if the carbon nanotube component is too high, the performance of the vulcanized rubber will deteriorate due to poor dispersion of the carbon nanotubes; if the white carbon black component is too low, the mechanical properties will be reduced and the heat generation will increase due to poor synergy with carbon black.

[0022] Further, in the present invention, preferably, relative to 100 parts by weight of nitrile rubber, the content of carbon nanotubes is 1-10 parts by weight, the content of carbon black is 30-50 parts by weight, the content of white carbon black is 7-15 parts by weight, the content of activator is 5-10 parts by weight, the content of plasticizer is 4-12 parts by weight, the content of antioxidant is 2-4 parts by weight, the content of peroxide vulcanizing agent is 3-7 parts by weight, and the content of co-vulcanizing agent is 1-4 parts by weight;

[0023] The nitrile rubber comprises 84-95 parts by weight of hydrogenated nitrile rubber and 5-16 parts by weight of hydrogenated carboxyl nitrile rubber.

[0024] According to the present invention, the Mooney viscosity ML of the hydrogenated nitrile rubber is 1+4 100℃ The content of acrylonitrile is not less than 30 wt %.

[0025] In the present invention, the Mooney viscosity, saturation and acrylonitrile content of the hydrogenated nitrile rubber meet the above ranges, and the mechanical strength of the vulcanized rubber prepared from the composition can be maintained without reducing the processing performance of the composition.

[0026] Furthermore, the Mooney viscosity ML of the hydrogenated nitrile rubber is 1+4 100℃ The content of acrylonitrile is 33-45wt%.

[0027] According to the present invention, in the hydrogenated carboxyl nitrile rubber, the mass fraction of carboxyl groups is 3-7wt%, and the Mooney viscosity ML 1+4 100℃ The content of acrylonitrile is not less than 30 wt %.

[0028] Furthermore, in the hydrogenated carboxyl nitrile rubber, the mass fraction of carboxyl groups is 4-6wt%, and the Mooney viscosity ML 1+4 100℃ The content of acrylonitrile is 33-45wt%.

[0029] In the present invention, the nitrile rubber comprises hydrogenated nitrile rubber and hydrogenated carboxyl nitrile rubber, and the combination of the two can improve the strength and wear resistance of the vulcanized rubber.

[0030] According to the present invention, the carbon black has an iodine absorption value of 20-90 g / kg and a DBP absorption value of (40-130)×10 -5 m 3 / kg.

[0031] In the present invention, the iodine absorption value and DBP absorption value of the carbon black meet the above ranges, and can generate lower heat generation.

[0032] Furthermore, in a preferred embodiment, the carbon black has an iodine absorption value of 30-90 g / kg and a DBP absorption value of (60-130)×10 -5 m 3 / kg.

[0033] According to the present invention, the specific surface area of ​​the white carbon black is 100-220m 2 / g, preferably 140-190m 2 / g.

[0034] According to the present invention, the carbon nanotubes have a diameter of 10-30 nm and a length of 3-20 μm, preferably a diameter of 10-20 nm and a length of 3-15 μm.

[0035] According to the present invention, the antioxidant is selected from at least one of amine antioxidants, phenol antioxidants, quinoline antioxidants and benzimidazole antioxidants.

[0036] In the present invention, preferably, the antioxidant is at least one selected from 4,4'-bis(α,α-dimethylbenzyl)diphenylamine, 2-thiolbenzimidazole zinc and 2,2,4-trimethyl-1,2-dihydroquinoline polymer.

[0037] According to the present invention, the plasticizer is selected from at least one of phthalate plasticizers, fatty dibasic acid ester plasticizers, partial phenyl ester plasticizers, ether ester plasticizers and polyester plasticizers.

[0038] In the present invention, preferably, the plasticizer is selected from at least one of trioctyl trimellitate, dioctyl phthalate and di[2-(2-butoxyethoxy)ethyl adipate].

[0039] According to the present invention, the activator is a combination of metal oxide and fatty acid.

[0040] Furthermore, preferably, the weight ratio of the metal oxide to the fatty acid is (3-8):1, preferably (4-6):1.

[0041] According to the present invention, the metal oxide is zinc oxide and / or magnesium oxide.

[0042] According to the present invention, the fatty acid is stearic acid.

[0043] According to the present invention, the peroxide curing agent is at least one selected from dicumyl peroxide, di-tert-butyl diisopropylbenzene peroxide and 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane.

[0044] According to the present invention, the co-vulcanizing agent is selected from at least one of triallyl isocyanurate, triallyl cyanurate, N,N'-m-phenylene bismaleimide, trimethylolpropane triacrylate and trimethylolpropane trimethacrylate.

[0045] A second aspect of the present invention provides a method for preparing vulcanized rubber from the aforementioned hydrogenated nitrile rubber composition, wherein the method comprises the following steps:

[0046] S1, mixing hydrogenated nitrile rubber, hydrogenated carboxyl nitrile rubber, carbon nanotubes, carbon black, white carbon black, antioxidant and plasticizer for the first time to prepare a masterbatch;

[0047] S2, mixing the activator, the peroxide vulcanizing agent, the co-vulcanizing agent and the first stage of the masterbatch for the second time to obtain a final rubber mix;

[0048] S3, vulcanizing the final rubber mixture to obtain vulcanized rubber.

[0049] According to the present invention, the method further comprises: performing a first mastication on the hydrogenated nitrile rubber and the hydrogenated carboxyl nitrile rubber.

[0050] In the present invention, after the hydrogenated nitrile rubber and the hydrogenated carboxyl nitrile rubber are first plasticized, their processing properties can be improved to meet the needs of further processing such as subsequent mixing.

[0051] According to the present invention, the temperature of the first mastication is 50-85° C.; the time of the first mastication is 0.5-2 min.

[0052] According to the present invention, the mixing temperature of the first mixing is 120-160° C., preferably 135-155° C.; the mixing time of the first mixing is 2-10 min, preferably 4-7 min.

[0053] In the present invention, after the first mixing is completed, in order to obtain a better effect, the product is allowed to stand for a period of time, and the standing time is not particularly limited, for example, it can be 2-24 hours in the present invention.

[0054] Furthermore, the method of the present invention further comprises: after the first mixing is completed, subjecting the masterbatch to a second mixing, wherein the temperature of the second mixing is 60-90° C. and the time of the second mixing is 0.5-2 min.

[0055] According to the present invention, the mixing temperature of the second mixing does not exceed 120°C, preferably 90-110°C.

[0056] According to the present invention, the mixing time of the second mixing is 2-6 minutes, preferably 3-5 minutes.

[0057] According to the present invention, the vulcanization conditions include: vulcanization time of 10-45 min, preferably 15-35 min; vulcanization temperature of 150-180° C., preferably 165-180° C.; vulcanization pressure of 3.5-40 MPa, preferably 10-20 MPa;

[0058] In the present invention, unless otherwise specified, all pressures used are gauge pressures.

[0059] The third aspect of the present invention provides a vulcanized rubber prepared by the above-mentioned method.

[0060] In the present invention, the tensile strength of the vulcanized rubber is not less than 22.5 MPa, the tear strength is not less than 46 kN / m, and the Akron abrasion is not higher than 0.19 cm 3 , compression heat is not higher than 25.6℃.

[0061] Furthermore, the tensile strength of the vulcanized rubber is 22.5-25.1 MPa, the tear strength is 46-51 kN / m, and the Akron abrasion is 0.09-0.19 cm 3 , compression heat generation is 21.3-25.6°C; preferably, the tensile strength of the vulcanized rubber is 23.7-25.1MPa, the tear strength is 48-51kN / m, and the Akron abrasion is 0.09-0.13cm 3 , compression heat is 21.3-22.1℃.

[0062] A fourth aspect of the present invention provides a use of the aforementioned vulcanized rubber in an automobile timing belt.

[0063] The present invention will be described in detail below through examples.

[0064] The equipment conditions for preparing the vulcanized rubber in the following examples and comparative examples are shown in Table 1.

[0065] The testing instruments of the vulcanized rubbers prepared in the examples and comparative examples are shown in Table 2, and the testing conditions are shown in Table 3.

[0066] The chemical reagents used in the embodiments and comparative examples are commercially available, as follows:

[0067] Table 1

[0068] Serial number Device Name model Manufacturer 1 Internal Mixer BR1600 Farrar 2 Open Mixing Machine XK-160 Qingdao Xincheng Yiming Machinery Co., Ltd. in China 3 Plate vulcanizing press XLB-D400*400*2 Shanghai No.1 Rubber Machinery Factory in China

[0069] Table 2

[0070]

[0071] Table 3

[0072]

[0073]

[0074] The following chemicals are used in the examples and comparative examples

[0075] Hydrogenated Nitrile Rubber (HNBR):

[0076] 4367, Mooney viscosity ML 1+4 100℃ 61, saturation 94.5%, acrylonitrile content 43wt%, ARLANXEO product;

[0077] 2020L, Mooney viscosity ML 1+4 100℃ 58, saturation 90%, acrylonitrile content 36wt%, Japan Zeon product;

[0078] Hydrogenated carboxyl nitrile rubber:

[0079] XT VP KA8889, carboxyl mass fraction is 5wt%, Mooney viscosity ML 1+4 100℃ The content of acrylonitrile is 33wt%, and the content of saturation is 96.5%, which is a product of ARLANXEO.

[0080] Carbon black N774, iodine absorption value is 29g / kg, DBP absorption value is 72×10 -5 m 3 / kg, Cabot Chemical (Tianjin) Co., Ltd.;

[0081] Carbon black N550, iodine absorption value is 43g / kg, DBP absorption value is 121×10 -5 m 3 / kg, Cabot Chemical (Tianjin) Co., Ltd.;

[0082] White carbon black 165N, specific surface area 165m 2 / g, Qingdao Rhodia Silica Co., Ltd.;

[0083] Carbon nanotubes: GT-300, average diameter 12.5 nm, average length 7.5 μm, Shandong Dazhan Nanomaterials Co., Ltd.

[0084] Plasticizer: trioctyl trimellitate (TOTM), Shandong Langtai Chemical Co., Ltd.;

[0085] Activators: zinc oxide and stearic acid, both purchased from Weifang Hengfeng Chemical Co., Ltd.

[0086] Antiaging agent: 2,2,4-trimethyl-1,2-dihydroquinoline polymer (RD), Hubei Xinkang Pharmaceutical Chemical Co., Ltd.; 2-mercaptobenzimidazole zinc (MBZ), Linhai Xinhua Chemical Plant;

[0087] Curing agent: dicumyl peroxide (DCP), Shanghai Fangruida Chemical Co., Ltd.;

[0088] Co-vulcanizing agent: triallyl isocyanurate (TAIC), Shanghai McLean Biochemical Technology Co., Ltd.

[0089] The amounts of components in the following examples and comparative examples are all parts by weight; in addition, "part" or "parts" all refer to "parts by weight".

[0090] Examples 1-9

[0091] S1, the internal mixer is set to a speed of 60rpm, an initial temperature of 70°C, and hydrogenated nitrile rubber (HNBR) and hydrogenated carboxyl nitrile rubber are placed in the internal mixer according to the formula in Table 4, and the first plasticization is performed for 0.5min, and carbon nanotubes, carbon black, white carbon black, antioxidant, and plasticizer are added. At the first mixing temperature of 145°C, the first mixing is performed for 5min, and the material is discharged. After the material is discharged, it is placed for 4h to obtain a masterbatch;

[0092] S2, the speed of the internal mixer is set to 40 rpm, the initial temperature is 40°C, the masterbatch is subjected to a second plasticizing for 0.5 min, and then an activator, a vulcanizing agent and a co-vulcanizing agent are added and a second mixing is carried out at 105°C for 4 min, and the final rubber is obtained;

[0093] S3. The final rubber mixture is subjected to flat plate vulcanization at 170° C., a pressure of 15 MPa, and a time of 20 min to obtain vulcanized rubbers of different experimental specifications, which are marked as S1-S9 respectively.

[0094] Comparative Examples 1-6

[0095] The method is consistent with that in the embodiment, except that the vulcanized rubbers obtained are prepared according to the formulation in Table 5 and are marked as D1-D6 respectively.

[0096] Table 4

[0097]

[0098] Table 5

[0099]

[0100]

[0101] Note: “-” in the table means that the component is 0 and the component is not used.

[0102] Test Case

[0103] The obtained vulcanized rubbers S1-S9 and D1-D6 were subjected to performance tests according to the methods in Table 2 and Table 3. The results are shown in Table 6.

[0104] Table 6

[0105]

[0106]

[0107] It can be seen from the above results that the vulcanized rubber made from the hydrogenated nitrile rubber composition of the present invention can have excellent comprehensive properties such as high mechanical strength, high tear resistance, low dynamic heat generation, and high wear resistance.

[0108] 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 hydrogenated nitrile rubber composition, characterized in that The hydrogenated nitrile rubber composition contains one or more of nitrile rubber, carbon nanotubes, carbon black, white carbon black, an activator, a plasticizer, an antioxidant, a peroxide vulcanizer and a vulcanizing agent; And relative to 100 parts by weight of nitrile rubber, the content of carbon nanotubes is 1-12 parts by weight, the content of carbon black is 25-55 parts by weight, the content of white carbon black is 5-20 parts by weight, the content of activator is 4-12 parts by weight, the content of plasticizer is 3-15 parts by weight, the content of antioxidant is 1-5 parts by weight, the content of peroxide vulcanizing agent is 2-10 parts by weight, and the content of co-vulcanizing agent is 1-6 parts by weight; The nitrile rubber comprises 80-96 parts by weight of hydrogenated nitrile rubber and 4-20 parts by weight of hydrogenated carboxyl nitrile rubber.

2. The hydrogenated nitrile rubber composition according to claim 1, wherein Relative to 100 parts by weight of nitrile rubber, the content of carbon nanotubes is 1-10 parts by weight, the content of carbon black is 30-50 parts by weight, the content of white carbon black is 7-15 parts by weight, the content of activator is 5-10 parts by weight, the content of plasticizer is 4-12 parts by weight, the content of antioxidant is 2-4 parts by weight, the content of peroxide vulcanizing agent is 3-7 parts by weight, and the content of co-vulcanizing agent is 1-4 parts by weight; The nitrile rubber comprises 84-95 parts by weight of hydrogenated nitrile rubber and 5-16 parts by weight of hydrogenated carboxyl nitrile rubber.

3. The hydrogenated nitrile rubber composition according to claim 1 or 2, wherein The Mooney viscosity ML of the hydrogenated nitrile rubber 1+4 100℃ is 50-85, the saturation is not less than 90%, and the acrylonitrile content is not less than 30wt%; Preferably, the mass fraction of carboxyl in the hydrogenated carboxyl nitrile rubber is 3-7wt%, and the Mooney viscosity ML 1+4 100℃ The content of acrylonitrile is not less than 30 wt %.

4. The hydrogenated nitrile rubber composition according to any one of claims 1 to 3, wherein The iodine absorption value of the carbon black is 20-90 g / kg, and the DBP absorption value is (40-130)×10 -5 m 3 / kg; Preferably, the specific surface area of ​​the white carbon black is 100-220m 2 / g; Preferably, the carbon nanotubes have a diameter of 10-30 nm and a length of 3-20 μm.

5. The hydrogenated nitrile rubber composition according to any one of claims 1 to 4, wherein The antioxidant is selected from at least one of amine antioxidants, phenol antioxidants, quinoline antioxidants and benzimidazole antioxidants; Preferably, the plasticizer is selected from at least one of phthalate plasticizers, fatty dibasic acid ester plasticizers, partial phenyl ester plasticizers, ether ester plasticizers and polyester plasticizers; Preferably, the activator is a combination of a metal oxide and a fatty acid; Preferably, the weight ratio of the metal oxide to the fatty acid is (3-8):1, preferably (4-6):1; Preferably, the metal oxide is zinc oxide and / or magnesium oxide; Preferably, the fatty acid is stearic acid; Preferably, the peroxide curing agent is selected from at least one of dicumyl peroxide, di-tert-butyl diisopropyl peroxide and 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane; Preferably, the co-vulcanizing agent is selected from at least one of triallyl isocyanurate, triallyl cyanurate, N,N'-m-phenylene bismaleimide, trimethylolpropane triacrylate and trimethylolpropane trimethacrylate.

6. A method for preparing vulcanized rubber from the hydrogenated nitrile rubber composition according to any one of claims 1 to 5, characterized in that: The method comprises the following steps: S1, mixing hydrogenated nitrile rubber, hydrogenated carboxyl nitrile rubber, carbon nanotubes, carbon black, white carbon black, antioxidant and plasticizer for the first time to prepare a masterbatch; S2, mixing the activator, the peroxide vulcanizing agent, the co-vulcanizing agent and the first stage of the masterbatch for the second time to obtain a final rubber mix; S3, vulcanizing the final rubber mixture to obtain vulcanized rubber.

7. The method according to claim 6, wherein: The method further comprises: performing a first mastication on the hydrogenated nitrile rubber and the hydrogenated carboxyl nitrile rubber; Preferably, the temperature of the first mastication is 50-85°C; the time of the first mastication is 0.5-2min; And / or, the mixing temperature of the first mixing is 120-160° C., preferably 135-155° C., and the mixing time of the first mixing is 2-10 min, preferably 4-7 min.

8. The method according to claim 6 or 7, wherein: The method further comprises: after the first mixing is completed, subjecting the masterbatch to a second plasticizing; Preferably, the second plasticizing temperature is 60-90°C; the second plasticizing time is 0.5-2min; And / or, the mixing temperature of the second mixing is not more than 120° C., and the mixing time of the second mixing is 2-6 min; And / or, the vulcanization conditions include: vulcanization time of 10-45 min, preferably 15-35 min; vulcanization temperature of 155-180° C., preferably 165-180° C.; vulcanization pressure of 3.5-40 MPa, preferably 10-20 MPa.

9. A vulcanized rubber prepared by the method according to any one of claims 6 to 8.

10. Use of the vulcanized rubber according to claim 9 in an automobile timing belt.

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