A renewable epdm material based on reversible ionic crosslinking and a method for its preparation

By introducing reversible ion cross-linking technology into EPDM rubber, the problem of difficult recycling of traditional EPDM products has been solved, efficient regeneration and performance retention of the material have been achieved, and environmental pollution has been reduced.

CN118725203BActive Publication Date: 2025-10-10QINGDAO UNIV OF SCI & TECH
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Patent Information

Application Number
CN202410602862.5
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-05-15
Publication Date
2025-10-10
Estimated Expiration
2044-05-15

AI Technical Summary

Technical Problem

Traditional EPDM products are difficult to recycle and reuse. Existing processing technologies have low efficiency, high costs, and severe performance loss, leading to environmental pollution and waste of resources.

Method used

Reversible ionic cross-linking technology is used to prepare renewable EPDM rubber materials by introducing maleic anhydride and zinc phytate into EPDM to form reversible metal coordination bonds, thereby achieving reversible deconstruction and reconstruction of the cross-linked structure.

Benefits of technology

The mechanical properties and recycling rate of rubber have been significantly improved. The material can still maintain excellent mechanical properties after multiple cycles of processing, realizing true material recycling.

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Abstract

The application discloses a renewable EPDM material based on reversible ion crosslinking and a preparation method thereof, relates to the technical field of renewable rubber materials, and the preparation method is as follows: 100-150 phr EPDM matrix is added into a torque rheometer for mixing; 1-3 phr maleic anhydride and 0.05-0.2 phr peroxide are added into the mixture for continuous mixing to graft the maleic anhydride; 1-3 phr ammonia water and 1-3 phr zinc phytate mixed solution are added into the mixture for uniform mixing; and the mixture is subjected to degassing and thinning treatment to obtain the rubber material. The ZDMA is used to form an ion crosslinking network, so that the mechanical properties of the rubber material are significantly improved, the tensile strength and the elongation at break are respectively improved, after three cycles, the tensile strength recovery rate is maintained at 78%, and the elongation at break is maintained at 107.4%, and the rubber material exhibits excellent recyclability and reusability.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of renewable rubber materials, in particular to a renewable ethylene propylene diene monomer material based on reversible ionic crosslinking and a preparation method thereof. BACKGROUND

[0002] In modern industrial applications, ethylene propylene diene monomer (EPDM) is widely used in various fields such as automobile parts, building sealing materials and cable insulation due to its excellent temperature resistance, chemical resistance and electrical insulation performance. However, with the increasing demand for environmental protection and resource recycling, the recycling of EPDM products has become the focus of research and industry. Traditional vulcanized rubber, through the irreversible crosslinking process initiated by sulfur or peroxide, although it gives the rubber excellent physical properties, but this irreversibility also leads to the difficulty in processing waste through reprocessing or recycling once the rubber product reaches the end of its service life, thereby causing serious environmental problems.

[0003] Currently, the treatment of waste EPDM rubber mainly relies on physical crushing and chemical devulcanization technology. Physical crushing can convert waste rubber into renewable rubber particles, but this method cannot restore the original performance of the rubber, limiting the application range of the renewable material. The chemical devulcanization process can disassemble the vulcanized network to some extent, but often accompanied by the rupture of the rubber chain, resulting in a significant decrease in the mechanical properties of the renewable rubber. These traditional technologies, although to some extent, recover the rubber material, but have low processing efficiency, high cost, and great damage to the rubber, and cannot fully restore the performance of the material, thereby limiting the further application of the recycled material.

[0004] In view of the many shortcomings of the prior art, the present application aims to develop a new type of ethylene propylene diene monomer material by introducing a dynamic crosslinking network based on reversible ionic crosslinking to solve the recycling problem caused by the irreversible crosslinking of traditional rubber. The goal of the present application is to improve the recycling rate and reusability of waste rubber, reduce environmental pollution, and at the same time maintain or even improve the mechanical and physical properties of the rubber. By developing reversible chemical crosslinking technology, the crosslinking structure of the rubber material can be reversibly disassembled and reconstructed through simple chemical or thermal treatment after the end of its service life, thereby realizing the true recycling of the material. SUMMARY

[0005] In order to achieve the above-mentioned application purpose, in view of the above technical problems,

[0006] The present application provides a preparation method of a renewable ethylene propylene diene monomer material based on reversible ionic crosslinking, comprising the following steps:

[0007] a1 adding 100 - 150 phr of ethylene propylene diene monomer matrix into a torque rheometer for mixing;

[0008] a2. Add 1-3 phr of maleic anhydride and 0.05-0.2 phr of peroxide to the mixture of a1 and continue mixing to graft the maleic anhydride;

[0009] a3. Add 1-3 phr of ammonia water and 1-3 phr of zinc phytate to the mixture in a2 and mix well.

[0010] a4 The mixture of a3 is subjected to debinding and thin-pass treatment to obtain EPDM-g-MAH@ZnPA.

[0011] Preferably, the peroxide is dicumyl peroxide (DCP).

[0012] Preferably, the mixing temperature in step a1 is 160°C and the rotor speed is 40-45 r / min; and the binder removal temperature in step a4 is 170°C.

[0013] The present invention also provides a renewable EPDM rubber material based on reversible ionic crosslinking, which is prepared by the above-mentioned preparation method.

[0014] The present invention also provides a method for preparing a renewable EPDM rubber composite material based on reversible ionic crosslinking, comprising the following steps:

[0015] A1: Add 100-150 phr of EPDM rubber matrix into the torque rheometer and mix;

[0016] A2 adds 1-3 phr of maleic anhydride and 0.05-0.2 phr of peroxide to the mixture of A1 and continues mixing to graft the maleic anhydride;

[0017] A3 adds 1-3 phr of a mixed solution of ammonia water and 1-3 phr of zinc phytate to the mixture in A2, and mixes evenly;

[0018] A4 debinds and thins the mixture of A3 to obtain EPDM-g-MAH@ZnPA;

[0019] A5: The EPDM-g-MAH@ZnPA masterbatch of A4 is put into a double-roller mill for milling, 10 phr to 50 phr of filler is added and fully mixed, and the mixture is allowed to stand after mixing to obtain a composite material.

[0020] Preferably, the peroxide is dicumyl peroxide (DCP).

[0021] Preferably, the filler is one of zinc methacrylate (ZDMA), modified aluminum silicate (SW), and carbon black (CB).

[0022] Preferably, the mixing temperature in step A1 is 160° C. and the rotor speed is 40-45 r / min; and the binder removal temperature in step A4 is 170° C.

[0023] Preferably, in step A5, the temperature of the open mill is 35-45° C., the roller speed is 20-25 r / min, and the roller distance is adjusted to 0.8-1.2 mm.

[0024] The present invention also provides a renewable EPDM rubber composite material based on reversible ionic crosslinking, and the material is prepared by the above-mentioned preparation method.

[0025] Zinc phytate (ZnPA) is a phytate form of zinc, formed by the combination of phytic acid (PA) and zinc ions. Phytic acid is a natural organophosphate compound found in plant seeds, particularly in the shells of grains, legumes, and seeds. Zinc phytate primarily acts as a chelating agent, effectively forming stable complexes with metal ions (such as zinc, iron, and calcium), and is widely used in food, feed, medicine, and cosmetics. More importantly, as a green reagent, zinc phytate possesses numerous ion exchange reaction sites, capable of generating ionic bond interactions under certain conditions, thereby promoting the formation of dynamic networks.

[0026] Zinc phytate structure

[0027] First, maleic anhydride (MAH) was grafted onto the EPDM backbone using peroxide as a free radical initiator. Because MAH has a carbon-carbon double bond (C=C), it reacts with the double bond of the third monomer in EPDM, resulting in grafting onto the EPDM molecular chain. During the melt reaction, MAH undergoes ring opening under the action of ammonia, generating carboxyl groups. The zinc ions on ZnPA form metal coordination bonds with the carboxyl groups formed after the ring opening of MAH, achieving EPDM crosslinking. Reversible and exchangeable COOH@ZnPA@HOOC metal coordination bonds exist within the crosslinked EPDM rubber. Therefore, the reversibility and exchangeability of the COOH@ZnPA@HOOC metal coordination bonds make it feasible for the recycling of EPDM.

[0028]

[0029] Figure 1 Reaction process and Zn2+-carboxyl ion cross-linking exchange process for the preparation of EPDM-g-MAH@ZnPA rubber

[0030] The technical solutions provided by the embodiments of the present invention have the following beneficial effects:

[0031] Significantly Improved Mechanical Properties: The addition of ZDMA to EPDM creates an ionically crosslinked network that significantly enhances the rubber's mechanical properties. Experimental data show that the tensile strength and elongation at break of EPDM-g-MAH@ZnPA increase by 108% and 188%, respectively, compared to unmodified EPDM. This demonstrates that ionic crosslinking enhances the rubber's overall mechanical properties to a certain extent.

[0032] Excellent strength retention: EPDM-g-MAH@ZnPA maintains excellent mechanical properties after recycling. Experimental results show that after three recycling cycles, the tensile strength recovery rate can still reach 78%, and the elongation at break retention rate is as high as 107.4%, demonstrating its strong reprocessing and recycling capabilities.

[0033] Excellent recyclability: EPDM-g-MAH@ZnPA rubber is recyclable through Zn 2+ The exchangeable ion crosslinking between the anhydride groups changes the crosslinked network structure, and the initial mechanical properties can be effectively restored after re-hot pressing at 150°C. Even after multiple cycles of processing, the composite material can still maintain a high recovery rate of mechanical properties.

[0034] Excellent recyclability: Compared to traditional covalently cross-linked rubber, EPDM-g-MAH@ZnPA enables high-temperature recyclability through dynamic ionic cross-linking. Compared to other self-healing composites, EPDM-g-MAH@ZnPA exhibits superior performance retention of tensile strength and elongation at break after one and three cycles. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] Figure 1 The figures show the effects of different fillers on the vulcanization characteristic curve (a), stress-strain curve (b), tensile strength and elongation at break (c), and 100% modulus stress and tear strength (d) of the EPDM composite material of the present invention.

[0036] Figure 2 The stress-strain curves (a) and tensile strength and elongation at break (b) of EPDM, EPDM-g-MAH and EPDM-g-MAH@ZnPA of the present invention are shown.

[0037] Figure 3 This is a flow chart of the recycling process of EPDM-g-MAH@ZnPA of the present invention.

[0038] Figure 4 The stress-strain curve (b), tensile strength (c) and elongation at break (d) of the EPDM-g-MAH@ZnPA of the present invention after multiple cycles of processing.

[0039] Figure 5 Recovery rate of EPDM-g-MAH@ZnPA and self-healing composite reported in the literature under 1 and 3 times of repair. DETAILED DESCRIPTION

[0040] In order to make the objects, technical solutions and advantages of the present application clearer, the present application will be further described in detail below with reference to the embodiments. Of course, the specific embodiments described herein are only used to explain the present application and not used to limit the present application.

[0041] Example 1

[0042] A renewable EPDM material based on reversible ionic crosslinking, the preparation method comprising the following steps:

[0043] a1 100 phr of EPDM base was added into a torque rheometer for mixing, the mixing temperature was 160℃, and the rotor speed was 45 r / min;

[0044] a2 2.5 phr of maleic anhydride and 0.1 phr of dicumyl peroxide (DCP) were added into the mixture of a1, and the mixing was continued to graft maleic anhydride;

[0045] a3 a mixed solution of 1.5 phr of ammonia water and 1.5 phr of zinc phytate was added into the mixture of a2, and the mixing was uniform;

[0046] a4 the mixture of a3 was subjected to discharge and thin pass treatment, the discharge temperature was 170℃, and EPDM-g-MAH@ZnPA was obtained.

[0047] Example 2

[0048] A renewable EPDM composite material based on reversible ionic crosslinking, prepared by the following steps:

[0049] A1 100 phr of EPDM base was added into a torque rheometer for mixing, the mixing temperature was 160℃, and the rotor speed was 45 r / min;

[0050] A2 2.5 phr of maleic anhydride and 0.1 phr of dicumyl peroxide (DCP) were added into the mixture of A1, and the mixing was continued to graft maleic anhydride;

[0051] A3 a mixed solution of 1.5 phr of ammonia water and 1.5 phr of zinc phytate was added into the mixture of A2, and the mixing was uniform;

[0052] A4 the mixture of A3 was subjected to discharge and thin pass treatment, the discharge temperature was 170℃, and EPDM-g-MAH@ZnPA was obtained.

[0053] A5: The EPDM-g-MAH@ZnPA masterbatch of A4 was placed in a double-roller mill for milling. The mill temperature was 40°C, the roller speed was 25 r / min, and the roller gap was adjusted to 1 mm. 30 phr of zinc methacrylate (ZDMA) was added and fully mixed. After mixing, the mixture was allowed to stand to obtain a composite material. Zinc methacrylate (ZDMA) was produced by Shanghai Anaiji Chemical Co., Ltd.

[0054] Example 3

[0055] A composite material was prepared according to the same preparation method as in Example 2, except that the added filler was modified aluminum silicate (SW), and the modified aluminum silicate (SW) model was T1000, produced by Jiangsu Qixiang High-tech Materials Co., Ltd.

[0056] Example 4

[0057] A composite material was prepared according to the same preparation method as in Example 2, except that the added filler was carbon black N330 (CB), produced by Cabot Corporation of the United States.

[0058] Example 5

[0059] A renewable EPDM rubber material based on reversible ionic crosslinking, the preparation method of which comprises the following steps:

[0060] a1 Add 100phr EPDM rubber matrix into the torque rheometer and mix it at a mixing temperature of 160℃ and a rotor speed of 40 r / min;

[0061] a2: Add 1 phr of maleic anhydride and 0.05 phr of dicumyl peroxide (DCP) to the mixture of a1 and continue mixing to graft the maleic anhydride;

[0062] a3: Add 1phr of ammonia water and 1phr of zinc phytate to the mixture in a2 and mix well;

[0063] a4 The mixture of a3 is subjected to debinding and thin-pass treatment at a debinding temperature of 170°C to obtain EPDM-g-MAH@ZnPA.

[0064] Example 6

[0065] A renewable EPDM rubber material based on reversible ionic crosslinking, the preparation method of which comprises the following steps:

[0066] a1. Add 150phr EPDM rubber matrix into the torque rheometer and mix it. The mixing temperature is 160℃ and the rotor speed is 45 r / min.

[0067] a2: Add 3 phr of maleic anhydride and 0.2 phr of dicumyl peroxide (DCP) to the mixture of a1 and continue mixing to graft the maleic anhydride;

[0068] a3: Add 3 phr of ammonia water and 3 phr of zinc phytate to the mixture in a2, and mix well;

[0069] a4 The mixture of a3 is subjected to debinding and thin-pass treatment at a debinding temperature of 170°C to obtain EPDM-g-MAH@ZnPA.

[0070] Example 7

[0071] A renewable EPDM rubber composite material based on reversible ionic crosslinking is prepared by the following steps:

[0072] A1: 100 phr of EPDM matrix was added to the torque rheometer and mixed at a mixing temperature of 160°C and a rotor speed of 40 r / min.

[0073] A2 adds 1 phr of maleic anhydride and 0.05 phr of dicumyl peroxide (DCP) to the mixture of A1 and continues mixing to graft the maleic anhydride;

[0074] A3 adds 1 phr of ammonia water and 1 phr of zinc phytate to the mixture in A2 and mixes evenly;

[0075] A4 subjected the mixture of A3 to debinding and thin-pass treatment at a debinding temperature of 170°C to obtain EPDM-g-MAH@ZnPA;

[0076] A5: The EPDM-g-MAH@ZnPA masterbatch of A4 was placed in a double-roller mill for milling. The mill temperature was 35°C, the roller speed was 20 r / min, and the roller gap was adjusted to 0.8 mm. 10 phr of zinc methacrylate (ZDMA) was added and fully mixed. After mixing, the mixture was allowed to stand to obtain a composite material. Zinc methacrylate (ZDMA) was produced by Shanghai Anaiji Chemical Co., Ltd.

[0077] Example 8

[0078] A renewable EPDM rubber composite material based on reversible ionic crosslinking is prepared by the following steps:

[0079] A1: 150 phr of EPDM matrix was added to the torque rheometer and mixed at a mixing temperature of 160°C and a rotor speed of 45 r / min.

[0080] A2 adds 3 phr of maleic anhydride and 0.2 phr of dicumyl peroxide (DCP) to the mixture of A1 and continues mixing to graft the maleic anhydride;

[0081] A3 adds 3 phr of ammonia water and 3 phr of zinc phytate to the mixture of A2 and mixes evenly;

[0082] A4 subjected the mixture of A3 to debinding and thin-pass treatment at a debinding temperature of 170°C to obtain EPDM-g-MAH@ZnPA;

[0083] A5 put the EPDM-g-MAH@ZnPA masterbatch of A4 into a double-roller mill for milling. The mill temperature was 45°C, the roller speed was 25 r / min, and the roller gap was adjusted to 1.2 mm. 50 phr of zinc methacrylate (ZDMA) was added and fully mixed. After mixing, the mixture was allowed to stand to obtain a composite material. Zinc methacrylate (ZDMA) was produced by Shanghai Anaiji Chemical Co., Ltd.

[0084] Comparative Example 1

[0085] Use an open mill to process the EPDM thin film.

[0086] Comparative Example 2

[0087] a1 Add 100phr EPDM rubber matrix into the torque rheometer and mix it at a mixing temperature of 160℃ and a rotor speed of 45 r / min;

[0088] a2: Add 2.5 phr of maleic anhydride and 0.1 phr of dicumyl peroxide (DCP) to the mixture of a1, and continue mixing to graft maleic anhydride to obtain EPDM-g-MAH.

[0089] Experimental test:

[0090] 1. Tensile test: A Z005 universal electronic tensile testing machine was used to conduct tensile tests on dumbbell-shaped specimens of EPDM composite materials in accordance with the GB / T 528-2009 test standard. The tensile rate was 500 mm / min, the temperature was room temperature, and the curing conditions were: 150°C × 30 min, 10 MPa.

[0091] 2. Tear test: Tear test was conducted on trouser-shaped specimens of EPDM composite materials in accordance with GB / T 529-2008, with a tensile rate of 500 mm / min, room temperature, and vulcanization conditions: 150°C × 30 min, 10 MPa.

[0092] Figure 1 The following are the vulcanization characteristic curves, stress-strain curves, and tensile and tearing properties of EPDM composite materials with different reinforcing fillers. Figure 1As can be seen in (a), compared with EPDM, the COOH@ZnPA crosslinking in EPDM-g-MAH@ZnPA increases the torque value of the rubber. After adding SW and CB, the torque values ​​of EPDM-g-MAH@ZnPA / SW and EPDM-g-MAH@ZnPA / CB further increase, but the torque difference does not increase significantly, indicating that the addition of SW and CB does not increase the crosslinking density of the rubber. However, after filling with ZDMA, the torque difference of the rubber increases significantly, which is due to the increase in the ionic crosslinking network inside the rubber. Figure 1 (bd) As can be seen, the addition of reinforcing fillers significantly improves the tensile strength, 100% modulus of elongation, and tear strength of the composite. The addition of ZDMA forms a more ionically crosslinked network within the rubber, further enhancing the overall performance of the composite. Furthermore, EPDM-g-MAH@ZnPA exhibits the highest elongation at break. This is because the addition of ZDMA, SW, and CB hinders the rearrangement of Zn2+ and carboxyl groups in the rubber, thereby reducing the composite's elongation at break. In summary, the addition of ZDMA to rubber, without the addition of a vulcanizer, creates an ionically crosslinked network that significantly improves the rubber's mechanical properties.

[0093] Figure 2 As shown in (ab), it is clear that EPDM exhibits weak strength, while the tensile strength and elongation at break of EPDM-g-MAH and EPDM-g-MAH@ZnPA after grafting modification are significantly improved. EPDM-g-MAH@ZnPA has the best mechanical properties, with a tensile strength and elongation at break reaching 1.23 MPa and 470%, respectively. Compared with EPDM, the tensile strength and elongation at break of EPDM-g-MAH@ZnPA increase by 108% and 188%, respectively, indicating that ionic crosslinking improves the mechanical properties of rubber to a certain extent.

[0094] Traditional covalent cross-linked rubber cannot be reprocessed once cured, while dynamic ionic cross-linking bonds can give rubber the ability to be recycled at high temperatures. 2+ Exchangeable ionic crosslinks between the anhydride groups can change the crosslinked network structure and release stress. Figure 3 As shown in Figure 2, the EPDM-g-MAH@ZnPA rubber was cut into small pieces, reprocessed, and then remolded by hot pressing at 150 °C for 30 minutes to verify the recyclability of the EPDM-g-MAH@ZnPA rubber.

[0095] Figure 4(b) and (d) show the stress-strain curves, tensile strength, and elongation at break of EPDM-g-MAH@ZnPA after three cycles of processing. As shown in the figures, after one remolding at 150°C, the EPDM-g-MAH@ZnPA retained 87.0% of its tensile strength and 99.6% of its elongation at break, respectively. This demonstrates excellent performance retention, and even after three cycles, it regained most of its initial mechanical properties, demonstrating a 78% tensile strength recovery rate. Furthermore, without the restriction of reinforcing fillers, the EPDM-g-MAH@ZnPA maintained its initial elongation at break after three cycles, with the elongation retention reaching 107.4%.

[0096] Figure 5 (ad) Retention of tensile strength and elongation at break for EPDM-g-MAH@ZnPA and polymer composites from the literature after one and three cycles. The figures clearly show that EPDM-g-MAH@ZnPA maintains superior mechanical property retention after the first and third cycles compared to previously published self-healing composites. These results demonstrate that EPDM-g-MAH@ZnPA retains most of its mechanical properties after recycling, and that EPDM rubber cross-linked with COOH@ZnPA exchangeable bonds exhibits excellent reprocessing and recycling capabilities.

[0097] Note: References for comparative polymers Ref1-12

[0098] Ref.1: Han H, Zhang X, Kuang W, et al. Self-healing and recyclableelastomer based on epoxidized natural rubber and carboxylated-chitosan[J]. Composites Communications, 2023, 40: 101594.

[0099] Ref.2: Zhang G, Zhou

[0100] Ref.3:Yang L, Wu M, Yang X, et al. Healable, recyclable, and adhesiverubber composites equipped with ester linkages, zinc ionic bonds, andhydrogen bonds[J]. Composites Part A: Applied Science and Manufacturing,2022, 155: 106816.

[0101] Ref.4:Li C, Wang Y, Yuan Z, et al. Construction of sacrificial bondsand hybrid networks in EPDM rubber towards mechanical performance enhancement[J]. Applied Surface Science, 2019, 484: 616-627.

[0102] Ref.5:Gong C, Cao J, Guo M, et al. A facile strategy for highmechanical performance and recyclable EPDM rubber enabled by exchangeable ioncrosslinking[J]. European Polymer Journal, 2022, 175: 111339.

[0103] Ref.6:Utrera-Barrios S, Manzanares R V, Grande A M, et al. Newinsights into the molecular structure and dynamics of a recyclable andionically crosslinked carboxylated nitrile rubber (XNBR)[J]. Materials&Design, 2023, 233: 112273.

[0104] Ref.7:Wang Q, Shi Y, Li Q, et al. Toughening, recyclable and healablenitrile rubber based on multi-coordination crosslink networks after“tetrazine click” reaction[J]. European Polymer Journal, 2021, 150: 110415.

[0105] Ref.8:Dong H, Zhang Y. Robust, thermally conductive and dampingrubbers with recyclable and self-healable capability[J]. Composites Part A:Applied Science and Manufacturing, 2023, 175: 107783.

[0106] Ref.9:Dong H, Zhang G, Zhang Y. Green self-vulcanizable rubbers withrecyclable, self-healable capabilities and excellent damping performance[J].Composites Science and Technology, 2023, 238: 110025.

[0107] Ref.10:Li C, Yuan Z, Ye L. Facile Construction of Zn2+‐Carboxyl Salt‐Bonding as Sacrificial Unit in EPDM Rubber toward Mechanical and SealingResilience Performance Enhancement[J]. Macromolecular Materials andEngineering, 2021, 306(8).

[0108] Ref.11:蒋业华. 自修复及可回收乙丙橡胶的制备和性能研究[D]. 青岛科技大学, 2021.

[0109] Ref.12: Yan Wenqiang. Preparation and performance research of self-repairing shape memory composite materials[D]. Beijing University of Chemical Technology, 2022.

[0110] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A method for preparing a renewable EPDM rubber material based on reversible ionic crosslinking, characterized in that: The following steps are involved: a1. Add 100-150 phr of EPDM matrix into the torque rheometer and mix at a mixing temperature of 160°C and a rotor speed of 40-45 r / min. a2. Add 1-3 phr of maleic anhydride and 0.05-0.2 phr of peroxide to the mixture of a1, and continue mixing to graft the maleic anhydride. The peroxide is dicumyl peroxide; a3. Add 1-3 phr of ammonia water and 1-3 phr of zinc phytate to the mixture in a2 and mix well. a4 The mixture of a3 is subjected to debinding and thin-pass treatment to obtain EPDM-g-MAH@ZnPA, and the debinding temperature is 170℃.

2. A renewable EPDM rubber material based on reversible ionic crosslinking, characterized in that: The material is prepared by the preparation method according to claim 1.

3. A method for preparing a renewable EPDM rubber composite material based on reversible ionic crosslinking, characterized in that: The following steps are involved: A1: Add 100-150 phr of EPDM matrix into the torque rheometer and mix at a mixing temperature of 160°C and a rotor speed of 40-45 r / min. A2 adds 1-3 phr of maleic anhydride and 0.05-0.2 phr of peroxide to the mixture of A1, and continues mixing to graft the maleic anhydride. The peroxide is dicumyl peroxide; A3 adds 1-3 phr of a mixed solution of ammonia water and 1-3 phr of zinc phytate to the mixture in A2, and mixes evenly; A4 debinds and thins the mixture of A3 to obtain EPDM-g-MAH@ZnPA at a debinding temperature of 170°C. A5: The EPDM-g-MAH@ZnPA masterbatch of A4 is placed in a double-roller mill for milling, 10 phr to 50 phr of filler is added and fully mixed, and the mixture is allowed to stand after mixing to obtain a composite material. The filler is one of zinc methacrylate, modified aluminum silicate, and carbon black. The mill temperature is 35-45°C, the roller speed is 20-25 r / min, and the roller gap is adjusted to 0.8-1.2 mm.

4. A renewable EPDM rubber composite material based on reversible ionic crosslinking, characterized in that: The material is prepared by the preparation method of claim 3.

Citation Information

Patent Citations

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