Diaphragm of diaphragm pump and preparation method thereof

Abstract

The invention discloses a diaphragm pump diaphragm and a preparation method thereof, and belongs to the technical field of diaphragms. The diaphragm of the diaphragm pump comprises the following raw materials in parts by weight: 40-60 parts of fluorinated silicone rubber, 15-35 parts of polyurethane elastomer, 5-10 parts of a modified nano reinforcing material, 5-10 parts of a sulfydryl-containing functionalized side chain monomer, 3-5 parts of a boric acid functional group-containing monomer, 3-8 parts of a plasticizer, 0.2-1 part of an antioxidant, 5-10 parts of a vulcanizing agent, 2-5 parts of an accelerant and 0.5-1 part of a cross-linking agent. The raw material components and the weight parts of the diaphragm of the diaphragm pump are limited, fluorosilicone rubber and a polyurethane elastomer are used as matrix raw materials, a modified nano reinforcing material is added, and the modified nano reinforcing material has good compatibility with the matrix raw materials, so that the mechanical property and the wear resistance of the diaphragm pump diaphragm can be improved; in addition, the diaphragm has certain self-repairing capacity, high resilience of the diaphragm is achieved, and the service life is prolonged.

Description

TECHNICAL FIELD

[0001] The application relates to a diaphragm pump membrane and a preparation method thereof, and belongs to the field of diaphragm pump membranes. BACKGROUND

[0002] The diaphragm pump is a special form of the volumetric pump, which changes the working chamber volume by back and forth driving of a diaphragm to suck and discharge liquid. The diaphragm pump membrane is installed in the middle of the hydraulic diaphragm pump cavity, and the edge is fixed on the pump body, and the diaphragm is driven back and forth by the power source (compressed air, steam, etc.) on one side. The space of the cavity on the other side of the diaphragm pump is changed through the reciprocating motion of the diaphragm, and the fluid is sucked from one end of the pump to the other end by means of two one-way valves.

[0003] The diaphragm is one of the most important core components of the diaphragm pump, and as an important component directly contacting and acting on the transported liquid, it needs to be periodically and quickly reciprocated, and is required to have good flexibility and excellent corrosion resistance. When the hydraulic diaphragm pump is working, the central diaphragm is continuously reciprocated back and forth, and is subjected to the test of flexural fatigue. However, the nature of the delivery medium of the diaphragm pump is usually very bad, which leads to the fact that the service life of the diaphragm in the actual use process is generally lower than the design life of the diaphragm pump.

[0004] In addition, the diaphragm pump is widely used, and sometimes it is used to transport fluid containing solid particles, which makes the diaphragm more prone to damage and increases the cost of loss. The diaphragm itself also has high requirements for elasticity and recovery. How to ensure the mechanical properties, high elasticity and high recovery of the diaphragm is a technical problem to be solved. SUMMARY

[0005] In order to solve the above problems, a diaphragm pump membrane and a preparation method thereof are provided. The raw material components and the weight fraction of the diaphragm pump membrane are limited, fluorosilicone rubber and polyurethane elastomer are used as the base raw material, and modified nano reinforcing materials are added. The modified nano reinforcing materials have good compatibility with the base raw material, can improve the mechanical properties and wear resistance of the diaphragm pump membrane, the functionalized side chain monomer containing mercapto and the monomer containing boric acid functional group interact to form a dynamic covalent bond. On the one hand, additional crosslinking points are introduced, which can effectively improve the mechanical strength and chemical corrosion resistance of the diaphragm; on the other hand, the existence of the dynamic chemical bond enables the diaphragm to have a certain self-repairing ability, realizes high recovery of the diaphragm, and prolongs the service life.

[0006] According to an aspect of the present application, the present application provides a diaphragm pump membrane, comprising the following raw materials in parts by weight: 40-60 parts of fluorosilicone rubber, 15-35 parts of polyurethane elastomer, 5-10 parts of modified nano reinforcing material, 5-10 parts of functionalized side chain monomer containing mercapto, 3-5 parts of monomer containing boric acid functional group, 3-8 parts of plasticizer, 0.2-1 part of antioxidant, 5-10 parts of vulcanizing agent, 2-5 parts of accelerator and 0.5-1 part of crosslinking agent.

[0007] Specifically, fluorosilicone rubber and polyurethane elastomer are used as base raw materials. On the one hand, fluorosilicone rubber has good corrosion resistance and high temperature resistance, and good flexibility and elasticity. Polyurethane elastomer has high elasticity, wear resistance and good mechanical properties. The modified nano reinforcing material and other components have good compatibility. Fluorosilicone rubber and polyurethane elastomer are used in a specific proportion and have a complementary effect.

[0008] Optionally, the modified nano reinforcing material comprises modified carbon nanotubes and modified nanosilica, and the mass ratio of the modified carbon nanotubes to the modified nanosilica is (2-4):1.

[0009] Optionally, the functionalized side chain monomer containing mercapto comprises bis(2-mercaptoethyl)amine and 3-mercaptopropionic acid; and the monomer containing boric acid functional group comprises 4-benzoic acid and N-(3-aminopropyl)-3-boronic acid propionamide.

[0010] Specifically, the functionalized side chain monomer containing mercapto and the monomer containing boric acid functional group interact to form dynamic covalent bonds. On the one hand, the introduction of additional crosslinking points can effectively improve the mechanical strength and chemical corrosion resistance of the membrane. On the other hand, the presence of dynamic chemical bonds enables the membrane to have certain self-repairing ability, thereby achieving high recovery and prolonging the service life.

[0011] Optionally, the modification method of the modified carbon nanotubes comprises the following steps:

[0012] S1 placing carbon nanotubes in a container, adding a mixed solution of concentrated sulfuric acid and concentrated nitric acid to obtain a mixture;

[0013] S2 cooling the mixture in an ice water bath, then heating to 80-90 DEG C, and refluxing for 3-5 hours;

[0014] S3 cooling to room temperature, centrifuging, washing and drying to obtain modified carbon nanotubes.

[0015] Specifically, the present application uses a mixed solution of concentrated sulfuric acid and concentrated nitric acid to modify the carbon nanotubes, and the acid is specifically limited. The surface of the carbon nanotubes is oxidized to introduce a large number of hydroxyl and carboxyl groups.

[0016] Optionally, the volume ratio of concentrated sulfuric acid and concentrated nitric acid is (2-4):1.

[0017] Optionally, the modification method of the modified nano-silica comprises the following steps:

[0018] S01 Put nano-silica into deionized water, stir uniformly, and adjust pH to 3-4 with hydrochloric acid;

[0019] S02 Dissolve amino silane coupling agent in ethanol, add pretreated nano-silica, stir uniformly, and react in a constant temperature water bath at 65-70℃ for 20-26h;

[0020] S03 Centrifuge, wash, and dry to obtain modified nano-silica.

[0021] Specifically, the application uses amino silane coupling agent to modify nano-silica, introduces amino groups on the surface of nano-silica, interacts with carboxyl groups on the surface of carbon nanotubes, forms amide bonds, effectively enhances the interfacial bonding strength of modified nano-silica and modified carbon nanotubes, and further enhances the mechanical properties of the membrane.

[0022] Optionally, the amino silane coupling agent is 3-aminopropyl triethoxysilane or N-(2-aminoethyl)-3-aminopropyl trimethoxysilane; the volume fraction of the amino silane coupling agent is 1.5%-3%.

[0023] Specifically, the application specifically limits the specific type and volume fraction of the amino silane coupling agent to obtain the required modified nano-silica.

[0024] Optionally, the plasticizer comprises dioctyl phthalate or diisononyl phthalate; the antioxidant comprises antioxidant 1010 or antioxidant 168; the vulcanizing agent is sulfur, the accelerator is one or more of accelerators DM, accelerator D, accelerator M, accelerator TT, and accelerator CE; and the crosslinking agent is an isocyanate crosslinking agent comprising HDI trimer or IPDI trimer.

[0025] According to another aspect of the application, a preparation method of a diaphragm pump membrane is also provided, comprising the following steps:

[0026] (1) Mix fluorosilicone rubber, polyurethane elastomer, functionalized side chain monomer containing mercapto group, monomer containing boric acid functional group, and crosslinking agent according to weight fraction, and stir uniformly;

[0027] (2) Continue to add modified nano-reinforcing material and stir until dispersed uniformly;

[0028] (3) Put the mixture obtained in step (2) into an open mill, add antioxidant and plasticizer, and perform mixing to obtain a first mixing product;

[0029] (4) adding a segment of the mixed material into a kneader, adding an accelerator and a vulcanizing agent to mix to obtain a second segment of the mixed material;

[0030] (5) loading the second segment of the mixed material into a vulcanization mold for vulcanization treatment, and then placing in an oven for baking to obtain the diaphragm pump membrane.

[0031] Optionally, in step (3), the mixing time is 1-2 h and the mixing temperature is 60-70°C; in step (4), the mixing time is 0.5-1 h and the mixing temperature is 65-75°C; in step (5), the vulcanization temperature is 150-170°C, the vulcanization time is 20-30 min, the oven baking temperature is 200-250°C, and the baking time is 1-2 h.

[0032] The beneficial effects of the present application include but are not limited to:

[0033] 1. The diaphragm pump membrane according to the present application, by limiting the raw material components and weight fractions of the diaphragm pump membrane, fluorosilicone rubber and polyurethane elastomer are used as base raw materials, modified nano reinforcing materials are added, which have good compatibility with the base raw materials and can improve the mechanical properties and wear resistance of the diaphragm pump membrane; the functionalized side chain monomer containing mercapto and the monomer containing boronic acid functional group interact to form a dynamic covalent bond, on the one hand, additional crosslinking points are introduced, which can effectively improve the mechanical strength and chemical corrosion resistance of the membrane; on the other hand, the existence of dynamic chemical bond makes it have certain self-repairing ability, realizes high recovery of the membrane, and prolongs the service life.

[0034] 2. The diaphragm pump membrane according to the present application, the composition of the nano reinforcing material is limited, including modified carbon nanotubes and modified nanosilica, and the ratio of the two is specifically limited, the modified carbon nanotubes and modified nanosilica in a specific ratio synergistically enhance the mechanical properties and wear resistance of the membrane, and the modified carbon nanotubes and nanosilica have better dispersibility and compatibility and better interfacial bonding strength.

[0035] 3. The diaphragm pump membrane according to the present application, the modification method of the modified carbon nanotubes and modified nanosilica is limited, wherein the modified carbon nanotubes are acid modified, and the acid is specifically limited, the surface of the carbon nanotubes is oxidized to introduce a large number of hydroxyl and carboxyl groups; amino groups are introduced on the surface of the nanosilica, which can undergo condensation reaction to form amide bonds, effectively enhancing the interfacial bonding strength of the modified nanosilica and the modified carbon nanotubes, and further enhancing the mechanical properties of the membrane.

[0036] 4. The method for preparing the diaphragm pump diaphragm according to the application, wherein the order of adding raw materials, process steps and process parameters are specifically limited to ensure the function of each component and the interaction between components, so that the diaphragm has good mechanical properties and high recovery. DETAILED DESCRIPTION

[0037] The application will be described in detail below with reference to examples, but the application is not limited to these examples.

[0038] Unless otherwise specified, the raw materials in the examples and comparative examples of the application are purchased through commercial channels.

[0039] Unless otherwise specified, the methods used in the examples and comparative examples of the application are conventional methods in the prior art.

[0040] Example 1

[0041] Preparation of modified carbon nanotubes

[0042] S1 Place the carbon nanotubes in a container, add a mixed solution of concentrated sulfuric acid and concentrated nitric acid, and the volume ratio of concentrated sulfuric acid and concentrated nitric acid is 4:1 to obtain a mixture;

[0043] S2 Cool the mixture in an ice water bath, then warm it to 90°C, and reflux for 5h;

[0044] S3 Cool to room temperature, centrifuge, wash and dry to obtain modified carbon nanotubes.

[0045] Preparation of modified nanosilica

[0046] S01 Place the nanosilica in deionized water, stir until uniform, and adjust the pH to 4 with hydrochloric acid;

[0047] S02 Dissolve the amino silane coupling agent in ethanol, add the pretreated nanosilica, stir until uniform, and react in a constant temperature water bath at 70°C for 26h;

[0048] S03 Centrifuge, wash and dry to obtain modified nanosilica.

[0049] The amino silane coupling agent is 3-aminopropyl triethoxysilane; the volume fraction of the amino silane coupling agent is 1.5%.

[0050] Preparation method of diaphragm pump diaphragm

[0051] (1) Mix 60 parts of fluorosilicone rubber, 35 parts of polyurethane elastomer, 10 parts of functionalized side chain monomer containing mercapto group 3-mercaptopropionic acid, 5 parts of monomer containing boric acid functional group 4-benzoic acid, and 1 part of crosslinking agent IPDI trimer according to weight fraction, and stir until uniform;

[0052] (2) continue to add modified nano-enhanced materials 9 parts, wherein, modified carbon nanotubes 6 parts, modified nanosilica 3 parts, stirring until evenly dispersed;

[0053] (3) the mixture obtained in step (2) is put into an open mill, 1 part of antioxidant 168 and 8 parts of plasticizer diisononyl phthalate are added, and mixing is carried out, the mixing time is 2 h, and the mixing temperature is 60-70℃, to obtain a first mixing product;

[0054] (4) the first mixing product is added to a kneader, 5 parts of accelerator D and 10 parts of vulcanizing agent sulfur are added and mixed, the mixing time is 1 h, and the mixing temperature is 75℃, to obtain a second mixing product;

[0055] (5) the second mixing product is loaded into a vulcanization mold for vulcanization treatment, the vulcanization temperature is 170℃, the vulcanization time is 30 min, and then it is placed in an oven for baking, the oven baking time is 250℃, and the baking time is 2 h to obtain a diaphragm pump membrane.

[0056] Example 2

[0057] Preparation of modified carbon nanotubes

[0058] S1 carbon nanotubes are placed in a container, a mixed solution of concentrated sulfuric acid and concentrated nitric acid is added, the volume ratio of concentrated sulfuric acid and concentrated nitric acid is 2:1, and a mixture is obtained;

[0059] S2 the mixture is placed in an ice water bath for cooling, and then warmed to 80℃, and refluxed for 3 h;

[0060] S3 cooling to room temperature, centrifugation, washing, and drying to obtain modified carbon nanotubes.

[0061] Preparation of modified nanosilica

[0062] S01 nanosilica is placed in deionized water and stirred uniformly, and the pH is adjusted to 3 with hydrochloric acid;

[0063] S02 amino silane coupling agent is dissolved in ethanol, and the pretreated nanosilica is added and stirred uniformly, and a constant temperature water bath reaction is carried out at 65℃ for 20 h;

[0064] S03 centrifugation, washing, and drying to obtain modified nanosilica.

[0065] The amino silane coupling agent is N-(2-aminoethyl)-3-aminopropyl trimethoxysilane; the volume fraction of the amino silane coupling agent is 3%.

[0066] Preparation method of diaphragm pump membrane

[0067] (1) Fluorosilicone rubber 40 parts, polyurethane elastomer 15 parts, functionalized side chain monomer containing mercapto group bis (2-mercaptoethyl) amine 5 parts, monomer containing boronic acid functional group N- (3-aminopropyl) -3-boronic acid propionamide 3 parts, crosslinking agent HDI trimer 0.5 parts are mixed according to the weight fraction, and stirred uniformly;

[0068] (2) Continue to add modified nano reinforcing material 5 parts, wherein modified carbon nanotube 4 parts, modified nanosilica 1 part, stir until dispersed uniformly;

[0069] (3) Put the mixture obtained in step (2) into an open mill, add antioxidant 1010 0.2 parts, plasticizer dioctyl phthalate 3 parts, and mix for 1 h at 60℃ to obtain a first mixing product;

[0070] (4) Put the first mixing product into a kneader, add accelerator DM 2 parts, vulcanizing agent sulfur 5 parts, mix for 0.5 h at 65℃ to obtain a second mixing product;

[0071] (5) Put the second mixing product into a vulcanization mold for vulcanization treatment at 150℃ for 20 min, then place it in an oven for baking at 200℃ for 1 h to obtain a diaphragm pump membrane.

[0072] Example 3

[0073] Preparation of modified carbon nanotubes

[0074] S1 Put the carbon nanotubes into a container, add a mixed solution of concentrated sulfuric acid and concentrated nitric acid, and the volume ratio of concentrated sulfuric acid and concentrated nitric acid is 3:1 to obtain a mixture;

[0075] S2 Cool the mixture in an ice water bath, then warm it to 85℃, and reflux for 4 h;

[0076] S3 Cool to room temperature, centrifuge, wash, and dry to obtain modified carbon nanotubes.

[0077] Preparation of modified nanosilica

[0078] S01 Put the nanosilica into deionized water, stir uniformly, and adjust the pH to 3 with hydrochloric acid;

[0079] S02 Dissolve the amino silane coupling agent in ethanol, add the pretreated nanosilica, stir uniformly, and react in a 70℃ constant temperature water bath for 23 h;

[0080] S03 Centrifuge, wash, and dry to obtain modified nanosilica.

[0081] The amino silane coupling agent is 3-aminopropyl triethoxysilane; the volume fraction of the amino silane coupling agent is 2%.

[0082] Method for preparing diaphragm pump membrane

[0083] (1) 50 parts of fluorosilicone rubber, 25 parts of polyurethane elastomer, 8 parts of functionalized side chain monomer containing mercapto group bis(2-mercaptoethyl) amine, 4 parts of monomer containing boronic acid functional group N-(3-aminopropyl)-3-boronic acid propionamide, 0.8 parts of crosslinking agent IPDI trimer are mixed according to the weight fraction, and stirred uniformly;

[0084] (2) Continue to add 8 parts of modified nano reinforcing material, wherein 6 parts of modified carbon nanotube and 2 parts of modified nanosilica, and stir until uniformly dispersed;

[0085] (3) Put the mixture obtained in step (2) into an open mill, add 0.5 parts of antioxidant 1010 and 5 parts of plasticizer diisononyl phthalate, and mix for 1.5 h at a mixing temperature of 65℃ to obtain a first mixing product;

[0086] (4) Put the first mixing product into a kneader, add 3 parts of accelerator M and 10 parts of vulcanizing agent sulfur, mix for 1 h at a mixing temperature of 70℃ to obtain a second mixing product;

[0087] (5) Put the second mixing product into a vulcanization mold for vulcanization treatment at a vulcanization temperature of 170℃ and a vulcanization time of 25℃, and then place it in an oven for baking at an oven baking temperature of 220℃ for a baking time of 1.5 h to obtain a diaphragm pump membrane.

[0088] Example 4

[0089] The difference between Example 4 and Example 3 is that the modified nano reinforcing material includes 8 parts of modified carbon nanotube, and the rest are the same.

[0090] Example 5

[0091] The difference between Example 5 and Example 3 is that the modified nano reinforcing material includes 8 parts of modified nanosilica, and the rest are the same.

[0092] Example 6

[0093] The difference between Example 6 and Example 3 is that the modified nano reinforcing material includes 4 parts of modified carbon nanotube and 4 parts of modified nanosilica, and the rest are the same.

[0094] Comparative Example 1

[0095] The difference between Comparative Example 1 and Example 3 is that it does not include polyurethane elastomer, and the rest are the same.

[0096] Comparative Example 2

[0097] The difference between Comparative Example 2 and Example 3 is that the antioxidant and plasticizer are added in step (2) in the preparation method of the diaphragm pump membrane, and the mixing of step (3) is not included, and the rest are the same.

[0098] Comparative Example 3

[0099] The difference between Comparative Example 3 and Example 3 is that the oven baking step in step (5) is not included, and the rest are the same.

[0100] Comparative Example 4

[0101] The difference between Comparative Example 4 and Example 3 is that the modified nano-reinforced material is not included, and the rest are the same.

[0102] Comparative Example 5

[0103] The difference between Comparative Example 5 and Example 3 is that the thiol-containing functional side chain monomer bis(2-mercaptoethyl) amine and the boronic acid functional group-containing monomer N-(3-aminopropyl)-3-boronic acid propionamide are not included, and the rest are the same.

[0104] Comparative Example 6

[0105] The difference between Comparative Example 6 and Example 3 is that methyl silicone rubber 50 parts is used instead of fluorosilicone rubber 50 parts, and the rest are the same.

[0106] Experimental Example 1

[0107] The diaphragm pump membrane prepared by Comparative Examples 1-6 and Comparative Examples 1-6 is tested for performance, and the test results are shown in Table 1.

[0108] Table 1 Performance test results

[0109]

[0110]

[0111]

[0112] The diaphragm pump membrane provided by the present application has mechanical properties and high recovery, and can adapt to various fluids, effectively prolonging the service life.

[0113] The above is only an embodiment of the present application, and the protection scope of the present application is not limited by these specific embodiments, but is determined by the claims of the present application. The present application can have various changes and variations for those skilled in the art. Any modification, equivalent replacement, improvement, etc. within the technical idea and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A diaphragm pump diaphragm, characterized in that: The invention comprises the following raw materials in proportion by weight: 40-60 parts of fluorosilicone rubber, 15-35 parts of polyurethane elastomer, 5-10 parts of modified nano-reinforced material, 5-10 parts of functionalized side chain monomer containing thiol group, 3-5 parts of monomer containing boric acid functional group, 3-8 parts of plasticizer, 0.2-1 part of antioxidant, 5-10 parts of vulcanizing agent, 2-5 parts of accelerator and 0.5-1 part of cross-linking agent.

2. The diaphragm pump diaphragm according to claim 1, characterized in that The modified nano-reinforced material comprises modified carbon nanotubes and modified nano-silicon dioxide, and the mass ratio of the modified carbon nanotubes to the modified nano-silicon dioxide is (2-4):

1.

3. The diaphragm pump diaphragm according to claim 2, characterized in that The functional side chain monomers containing mercapto groups include bis(2-mercaptoethyl)amine and 3-mercaptopropionic acid; the monomers containing boric acid functional groups include 4-boric acid benzoic acid and N-(3-aminopropyl)-3-boric acid propionamide.

4. The diaphragm pump diaphragm according to claim 1, characterized in that The modification method of the modified carbon nanotubes comprises the following steps: S1: placing carbon nanotubes in a container, and adding a mixed solution of concentrated sulfuric acid and concentrated nitric acid to obtain a mixture; S2: Cool the mixture in an ice-water bath, then heat to 80-90°C and reflux for 3-5 hours; S3 is cooled to room temperature, centrifuged, washed, and dried to obtain modified carbon nanotubes.

5. The diaphragm pump diaphragm according to claim 4, characterized in that The volume ratio of concentrated sulfuric acid to concentrated nitric acid is (2-4):

1.

6. The diaphragm pump diaphragm according to claim 1, characterized in that The modification method of the modified nano-silica comprises the following steps: S01 Place nano-silica in deionized water, stir evenly, and adjust the pH to 3-4 with hydrochloric acid; Dissolve S02 aminosilane coupling agent in ethanol, add pretreated nano-silica, stir evenly, and react in a constant temperature water bath at 65-70℃ for 20-26h; S03 is centrifuged, washed, and dried to obtain modified nano-silica.

7. The diaphragm pump diaphragm according to claim 6, characterized in that The aminosilane coupling agent is 3-aminopropyltriethoxysilane or N-(2-aminoethyl)-3-aminopropyltrimethoxysilane; and the volume fraction of the aminosilane coupling agent is 1.5% to 3%.

8. The diaphragm pump diaphragm according to claim 1, characterized in that The plasticizer includes dioctyl phthalate and diisononyl phthalate; the antioxidant includes antioxidant 1010 or antioxidant 168; the vulcanizing agent is sulfur, and the accelerator is one or more of accelerator DM, accelerator D, accelerator M, accelerator TT, and accelerator CE; the crosslinking agent is an isocyanate crosslinking agent including HDI trimer and IPDI trimer.

9. The method for preparing a diaphragm pump diaphragm according to any one of claims 1 to 8, characterized in that: The following steps are involved: (1) mixing fluorosilicone rubber, polyurethane elastomer, functional side chain monomer containing thiol group, monomer containing boric acid functional group, and crosslinking agent according to parts by weight and stirring uniformly; (2) Continue adding the modified nano-reinforced material and stirring until it is evenly dispersed; (3) putting the mixture obtained in step (2) into an open mill, adding an antioxidant and a plasticizer, and mixing to obtain a first-stage mixed material; (4) adding the first-stage mixture into a kneader, adding an accelerator and a vulcanizing agent and mixing to obtain a second-stage mixture; (5) The second-stage mixed product is placed in a vulcanization mold for vulcanization treatment, and then placed in an oven for baking to obtain a diaphragm pump diaphragm.

10. The method for preparing a diaphragm pump diaphragm according to claim 9, characterized in that: In step (3), the mixing time is 1 to 2 hours, and the mixing temperature is 60 to 70° C.; in step (4), the mixing time is 0.5 to 1 hour, and the mixing temperature is 65 to 75° C.; in step (5), the vulcanization temperature is 150 to 170° C., the vulcanization time is 20 to 30 minutes, the oven baking time is 200 to 250° C., and the baking time is 1 to 2 hours.

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