Oil-resistant dynamically vulcanized thermoplastic elastomer material and preparation method thereof

Abstract

The invention discloses an oil-resistant dynamically vulcanized thermoplastic elastomer material, comprising the following raw materials in parts by weight: 35-45 parts of EPDM rubber, 25-30 parts of polyvinyl chloride resin, 1-4 parts of a vulcanizing agent, 5-10 parts of a nano-silica-co-modified graphene body, 3-7 parts of a coupling agent conditioning fluid, 1-3 parts of a lubricant, and 1-2 parts of an antioxidant. The thermoplastic elastomer material of the invention uses EPDM rubber and polyvinyl chloride resin as a matrix, and the vulcanizing agent, vulcanizing agent, and antioxidant as additives. The nano-silica-co-modified graphene body and the coupling agent conditioning fluid are synergistically coordinated to enhance the mechanical strength and fracture properties of the product, thereby improving the performance of both.

Description

Technical Field

[0001] The present invention relates to the technical field of thermoplastic elastomers, and in particular to an oil-resistant dynamically vulcanized thermoplastic elastomer material and a preparation method thereof. Background Art

[0002] Thermoplastic elastomers are a class of elastomeric materials that exhibit the elasticity of rubber at room temperature and the ability to be plasticized and molded at high temperatures. They can be repeatedly processed and recycled using similar processing techniques to thermoplastic resins. Thermoplastic elastomers are typically produced by dynamic vulcanization of thermoplastic resin and rubber. During the melt processing, the rubber vulcanizes and becomes uniformly dispersed as dispersed particles within the continuous phase of the thermoplastic resin.

[0003] Existing vulcanized thermoplastic elastomer materials have poor oil resistance, and the strength and fracture properties of the products are average. The strength and fracture properties of the mechanical properties are not coordinated. At the same time, under oil-resistant conditions, the performance deteriorates significantly. Based on this, the present invention further improves it. Summary of the Invention

[0004] In view of the defects of the prior art, the purpose of the present invention is to provide an oil-resistant dynamically vulcanized thermoplastic elastomer material and a preparation method thereof, so as to solve the problems raised in the above background technology.

[0005] The present invention solves the technical problem by adopting the following technical solutions:

[0006] The present invention provides an oil-resistant dynamically vulcanized thermoplastic elastomer material, comprising the following raw materials in parts by weight:

[0007] 35-45 parts of EPDM rubber, 25-30 parts of polyvinyl chloride resin, 1-4 parts of vulcanizing agent, 5-10 parts of nano-silica modified graphene, 3-7 parts of coupling agent regulating liquid, 1-3 parts of lubricant and 1-2 parts of antioxidant.

[0008] Preferably, the dynamically vulcanized thermoplastic elastomer material comprises the following raw materials in parts by weight:

[0009] 40 parts of EPDM rubber, 27.5 parts of polyvinyl chloride resin, 2.5 parts of vulcanizing agent, 7.5 parts of nano-silica modified graphene, 5 parts of coupling agent regulating liquid, 2 parts of lubricant and 1.5 parts of antioxidant.

[0010] Preferably, the preparation method of the nano-silica modified graphene body is:

[0011] S01: placing the graphene in a ball mill for 10-20 min at a ball milling speed of 1000-1500 r / min, and then finishing the ball milling;

[0012] S02: The product of S01 is placed in 3-5 times the volume of chitosan modification liquid and stirred for modification. After the modification is completed, a modified graphene agent is obtained;

[0013] S03: Place the nano-silica in a 3-5 times hydrochloric acid solution and stir evenly, then add 10-20% of lanthanum sulfate and 1-5% of sodium oxalate to the total amount of nano-silica, stir evenly, wash with water, and dry to obtain pre-conditioned nano-silica;

[0014] S04: Add the pre-adjusted nano-silica to 5-10 times the modified graphene agent and stir thoroughly, then wash with water and dry to obtain the nano-silica coordinated modified graphene body.

[0015] Preferably, the mass fraction of the hydrochloric acid solution is 2-5%.

[0016] Preferably, the stirring modification speed is 550-650 r / min, the stirring time is 20-30 min, and the stirring temperature is 35-40°C.

[0017] Preferably, the chitosan modified liquid comprises the following raw materials in parts by weight:

[0018] 10-20 parts of chitosan, 45-55 parts of deionized water, 1-4 parts of oxalic acid, 0.2-0.5 parts of titanate coupling agent and 1-3 parts of sodium alkyl sulfonate.

[0019] Preferably, the preparation method of the coupling agent regulating solution is:

[0020] The coupling agent KH560 was added to the ethanol solvent at a weight ratio of 1:4, and then 5-10% of the total amount of the coupling agent KH560 sodium alginate and 1-4% of the phosphate buffer solution were added and stirred evenly to obtain a coupling agent adjustment solution.

[0021] Preferably, the pH value of the phosphate buffer solution is 5.5.

[0022] Preferably, the vulcanizing agent is dicumyl peroxide;

[0023] The lubricant is one or more combinations of calcium stearate, stearic acid, and polyethylene wax;

[0024] The present invention provides a method for preparing an oil-resistant dynamically vulcanized thermoplastic elastomer material, comprising the following steps:

[0025] Step 1) EPDM rubber, polyvinyl chloride resin, vulcanizing agent, lubricant and antioxidant are stirred and mixed;

[0026] Step 2) adding nano-silica modified graphene and coupling agent regulating solution to the mixture of step 1) and continuing to stir and mix thoroughly, then washing with water, drying, and then melt mixing, the melt mixing temperature is 100-110° C., and the melt blending time is 10-15 minutes;

[0027] Step 3) Finally, dynamic vulcanization is performed at a temperature of 180-185° C. and a vulcanization time of 5-10 minutes to obtain the thermoplastic elastomer material of the present invention.

[0028] Compared with the prior art, the present invention has the following beneficial effects:

[0029] The thermoplastic elastomer material of the present invention is based on EPDM rubber and polyvinyl chloride resin, and vulcanizing agent, curing agent and antioxidant are added as auxiliary agents. The modified graphene body and coupling agent regulating liquid are coordinated and coordinated by nano-silica to enhance the synergy, thereby enhancing the mechanical strength and fracture performance of the product, and improving the performance of the two in a coordinated manner. At the same time, the stability of the product under oil-resistant conditions is optimized. The modified graphene agent obtained by ball milling and stirring and modifying the graphene in a chitosan modifying liquid is coordinated with the pre-adjusted nano-silica. The toughness of the graphene is optimized by the nano-silica with a high specific surface area. At the same time, under specific optimized conditions, the mechanical strength and fracture performance of the product can be improved in a coordinated manner. The coupling agent regulating liquid adopts a coupling agent in combination with other auxiliary raw materials to improve the interface between the nano-silica modified graphene body and the product raw materials of the thermoplastic elastomer material, thereby achieving a synergistic effect. The performance of the prepared product is coordinated and perfect, and it also has excellent stability under oil-resistant conditions. DETAILED DESCRIPTION

[0030] The following is a clear and complete description of the technical solutions in the embodiments of the present invention in conjunction with specific embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0031] The oil-resistant dynamically vulcanized thermoplastic elastomer material of this embodiment includes the following raw materials in parts by weight:

[0032] 35-45 parts of EPDM rubber, 25-30 parts of polyvinyl chloride resin, 1-4 parts of vulcanizing agent, 5-10 parts of nano-silica modified graphene, 3-7 parts of coupling agent regulating liquid, 1-3 parts of lubricant and 1-2 parts of antioxidant.

[0033] The dynamically vulcanized thermoplastic elastomer material of this embodiment includes the following raw materials in parts by weight:

[0034] 40 parts of EPDM rubber, 27.5 parts of polyvinyl chloride resin, 2.5 parts of vulcanizing agent, 7.5 parts of nano-silica modified graphene, 5 parts of coupling agent regulating liquid, 2 parts of lubricant and 1.5 parts of antioxidant.

[0035] The preparation method of the nano-silicon dioxide modified graphene body in this embodiment is:

[0036] S01: placing the graphene in a ball mill for 10-20 min at a ball milling speed of 1000-1500 r / min, and then finishing the ball milling;

[0037] S02: The product of S01 is placed in 3-5 times the volume of chitosan modification liquid and stirred for modification. After the modification is completed, a modified graphene agent is obtained;

[0038] S03: Place the nano-silica in a 3-5 times hydrochloric acid solution and stir evenly, then add 10-20% of lanthanum sulfate and 1-5% of sodium oxalate to the total amount of nano-silica, stir evenly, wash with water, and dry to obtain pre-conditioned nano-silica;

[0039] S04: Add the pre-adjusted nano-silica to 5-10 times the modified graphene agent and stir thoroughly, then wash with water and dry to obtain the nano-silica coordinated modified graphene body.

[0040] The mass fraction of the hydrochloric acid solution in this embodiment is 2-5%.

[0041] The stirring and modification in this embodiment has a rotation speed of 550-650 r / min, a stirring time of 20-30 min, and a stirring temperature of 35-40°C.

[0042] The chitosan modified solution of this embodiment includes the following raw materials in parts by weight:

[0043] 10-20 parts of chitosan, 45-55 parts of deionized water, 1-4 parts of oxalic acid, 0.2-0.5 parts of titanate coupling agent and 1-3 parts of sodium alkyl sulfonate.

[0044] The preparation method of the coupling agent regulating solution of this embodiment is:

[0045] The coupling agent KH560 was added to the ethanol solvent at a weight ratio of 1:4, and then 5-10% of the total amount of the coupling agent KH560 sodium alginate and 1-4% of the phosphate buffer solution were added and stirred evenly to obtain a coupling agent adjustment solution.

[0046] The pH value of the phosphate buffer solution in this example is 5.5.

[0047] The curing agent in this embodiment is dicumyl peroxide;

[0048] The lubricant is one or more combinations of calcium stearate, stearic acid, and polyethylene wax;

[0049] A method for preparing an oil-resistant dynamically vulcanized thermoplastic elastomer material according to this embodiment includes the following steps:

[0050] Step 1) EPDM rubber, polyvinyl chloride resin, vulcanizing agent, lubricant and antioxidant are stirred and mixed;

[0051] Step 2) adding nano-silica modified graphene and coupling agent regulating solution to the mixture of step 1) and continuing to stir and mix thoroughly, then washing with water, drying, and then melt mixing, the melt mixing temperature is 100-110° C., and the melt blending time is 10-15 minutes;

[0052] Step 3) Finally, dynamic vulcanization is performed at a temperature of 180-185° C. and a vulcanization time of 5-10 minutes to obtain the thermoplastic elastomer material of the present invention.

[0053] Example 1

[0054] The oil-resistant dynamically vulcanized thermoplastic elastomer material of this embodiment includes the following raw materials in parts by weight:

[0055] 35 parts of EPDM rubber, 25 parts of polyvinyl chloride resin, 1 part of vulcanizing agent, 5 parts of nano-silica modified graphene, 3 parts of coupling agent regulating liquid, 1 part of lubricant and 1 part of antioxidant.

[0056] The preparation method of the nano-silicon dioxide modified graphene body in this embodiment is:

[0057] S01: The graphene is first placed in a ball mill and ball milled for 10 minutes at a ball milling speed of 1000 r / min, and the ball milling is completed;

[0058] S02: The product of S01 is placed in 3 times the amount of chitosan modification liquid and stirred for modification. After the modification is completed, a modified graphene agent is obtained;

[0059] S03: Place nano-silica in a 3-fold hydrochloric acid solution and stir evenly, then add 10% lanthanum sulfate and 1% sodium oxalate of the total amount of nano-silica, stir evenly, wash with water, and dry to obtain pre-conditioned nano-silica;

[0060] S04: Add the pre-adjusted nano-silica to 5 times the modified graphene agent and stir thoroughly, then wash with water and dry to obtain the nano-silica coordinated modified graphene body.

[0061] The mass fraction of the hydrochloric acid solution in this embodiment is 2%.

[0062] The stirring and modification in this embodiment has a rotation speed of 550 r / min, a stirring time of 20 min, and a stirring temperature of 35°C.

[0063] The chitosan modified solution of this embodiment includes the following raw materials in parts by weight:

[0064] 10 parts of chitosan, 45 parts of deionized water, 1 part of oxalic acid, 0.2 parts of titanate coupling agent and 1 part of sodium alkyl sulfonate.

[0065] The preparation method of the coupling agent regulating solution of this embodiment is:

[0066] The coupling agent KH560 was added to the ethanol solvent at a weight ratio of 1:4, and then 5% of the total amount of the coupling agent KH560, sodium alginate, and 1% of phosphate buffer solution were added and stirred evenly to obtain a coupling agent adjustment solution.

[0067] The pH value of the phosphate buffer solution in this example is 5.5.

[0068] The curing agent in this embodiment is dicumyl peroxide;

[0069] The lubricant is calcium stearate;

[0070] A method for preparing an oil-resistant dynamically vulcanized thermoplastic elastomer material according to this embodiment includes the following steps:

[0071] Step 1) EPDM rubber, polyvinyl chloride resin, vulcanizing agent, lubricant and antioxidant are stirred and mixed;

[0072] Step 2) adding nano-silica modified graphene and coupling agent regulating solution to the mixture of step 1) and continuing to stir and mix thoroughly, then washing with water, drying, and then melt mixing, the melt mixing temperature is 100° C., and the melt blending time is 10 min;

[0073] Step 3) Finally, dynamic vulcanization is performed at a temperature of 180° C. and a vulcanization time of 5 minutes to obtain the thermoplastic elastomer material of the present invention.

[0074] Example 2.

[0075] The oil-resistant dynamically vulcanized thermoplastic elastomer material of this embodiment includes the following raw materials in parts by weight:

[0076] 45 parts of EPDM rubber, 30 parts of polyvinyl chloride resin, 4 parts of vulcanizing agent, 10 parts of nano-silica co-modified graphene body, 7 parts of coupling agent regulating liquid, 3 parts of lubricant and 2 parts of antioxidant.

[0077] The preparation method of the nano-silicon dioxide modified graphene body in this embodiment is:

[0078] S01: The graphene was first placed in a ball mill and ball milled for 20 min at a speed of 1500 r / min, and the ball milling was completed;

[0079] S02: The product of S01 is placed in a 5-fold chitosan modification solution and stirred for modification. After the modification is completed, a modified graphene agent is obtained;

[0080] S03: Place the nano-silica in a 5-fold hydrochloric acid solution and stir evenly, then add 20% of the total amount of nano-silica lanthanum sulfate and 5% of sodium oxalate, stir evenly, wash with water, and dry to obtain pre-conditioned nano-silica;

[0081] S04: Add the pre-adjusted nano-silica to 10 times the modified graphene agent and stir thoroughly, then wash with water and dry to obtain the nano-silica coordinated modified graphene body.

[0082] The mass fraction of the hydrochloric acid solution in this embodiment is 5%.

[0083] The stirring and modification in this embodiment has a rotation speed of 650 r / min, a stirring time of 30 min, and a stirring temperature of 40°C.

[0084] The chitosan modified solution of this embodiment includes the following raw materials in parts by weight:

[0085] 20 parts of chitosan, 55 parts of deionized water, 4 parts of oxalic acid, 0.5 parts of titanate coupling agent and 3 parts of sodium alkyl sulfonate.

[0086] The preparation method of the coupling agent regulating solution of this embodiment is:

[0087] The coupling agent KH560 was added to the ethanol solvent at a weight ratio of 1:4, and then 10% of the total amount of the coupling agent KH560, sodium alginate, and 4% of phosphate buffer solution were added and stirred evenly to obtain a coupling agent adjustment solution.

[0088] The pH value of the phosphate buffer solution in this example is 5.5.

[0089] The curing agent in this embodiment is dicumyl peroxide;

[0090] The lubricant is stearic acid;

[0091] A method for preparing an oil-resistant dynamically vulcanized thermoplastic elastomer material according to this embodiment includes the following steps:

[0092] Step 1) EPDM rubber, polyvinyl chloride resin, vulcanizing agent, lubricant and antioxidant are stirred and mixed;

[0093] Step 2) adding nano-silica modified graphene and coupling agent regulating solution to the mixture of step 1) and continuing to stir and mix thoroughly, then washing with water, drying, and then melt mixing, the melt mixing temperature is 110° C., and the melt blending time is 15 min;

[0094] Step 3) Finally, dynamic vulcanization is performed at a temperature of 185° C. and a vulcanization time of 10 min to obtain the thermoplastic elastomer material of the present invention.

[0095] Example 3.

[0096] The oil-resistant dynamically vulcanized thermoplastic elastomer material of this embodiment includes the following raw materials in parts by weight:

[0097] 40 parts of EPDM rubber, 27.5 parts of polyvinyl chloride resin, 2.5 parts of vulcanizing agent, 7.5 parts of nano-silica modified graphene, 5 parts of coupling agent regulating liquid, 2 parts of lubricant and 1.5 parts of antioxidant.

[0098] The preparation method of the nano-silicon dioxide modified graphene body in this embodiment is:

[0099] S01: The graphene was first placed in a ball mill and ball milled for 15 min at a speed of 1250 r / min, and the ball milling was completed;

[0100] S02: The product of S01 is placed in 4 times the amount of chitosan modification liquid and stirred for modification. After the modification is completed, a modified graphene agent is obtained;

[0101] S03: Place nano-silica in a 4-fold hydrochloric acid solution and stir evenly, then add 15% lanthanum sulfate and 3% sodium oxalate of the total amount of nano-silica, stir evenly, wash with water, and dry to obtain pre-conditioned nano-silica;

[0102] S04: Add the pre-adjusted nano-silica to 7.5 times the modified graphene agent and stir thoroughly, then wash with water and dry to obtain the nano-silica coordinated modified graphene body.

[0103] The mass fraction of the hydrochloric acid solution in this embodiment is 3.5%.

[0104] The stirring and modification speed of this embodiment is 600 r / min, the stirring time is 25 min, and the stirring temperature is 37°C.

[0105] The chitosan modified solution of this embodiment includes the following raw materials in parts by weight:

[0106] 150 parts of chitosan, 50 parts of deionized water, 2.5 parts of oxalic acid, 0.35 parts of titanate coupling agent and 2 parts of sodium alkyl sulfonate.

[0107] The preparation method of the coupling agent regulating solution of this embodiment is:

[0108] The coupling agent KH560 was added to the ethanol solvent at a weight ratio of 1:4, and then 7.5% of sodium alginate and 2.5% of phosphate buffer solution were added, and the mixture was stirred evenly to obtain a coupling agent adjustment solution.

[0109] The pH value of the phosphate buffer solution in this example is 5.5.

[0110] The curing agent in this embodiment is dicumyl peroxide;

[0111] The lubricant is calcium stearate;

[0112] A method for preparing an oil-resistant dynamically vulcanized thermoplastic elastomer material according to this embodiment includes the following steps:

[0113] Step 1) EPDM rubber, polyvinyl chloride resin, vulcanizing agent, lubricant and antioxidant are stirred and mixed;

[0114] Step 2) adding nano-silica modified graphene and coupling agent regulating solution to the mixture of step 1) and continuing to stir and mix thoroughly, then washing with water, drying, and then melt mixing, the melt mixing temperature is 105° C., and the melt blending time is 12 min;

[0115] Step 3) Finally, dynamic vulcanization is performed at a temperature of 182° C. and a vulcanization time of 6 minutes to obtain the thermoplastic elastomer material of the present invention.

[0116] Comparative Example 1.

[0117] The difference from Optimization Example 3 is that nano-silica is not added to coordinately modify the graphene.

[0118] Comparative Example 2.

[0119] The difference from Optimization Example 3 is that the nano-silica co-modified graphene body is replaced by a mixture of nano-silica and graphene in a weight ratio of 1:7.

[0120] Comparative Example 3.

[0121] The difference from Optimization Example 3 is that the preparation method of the nano-silica co-modified graphene body is different; the pre-adjusted nano-silica is directly replaced by nano-silica raw material.

[0122] Comparative Example 4.

[0123] The difference from Optimization Example 3 is that the preparation method of nano-silica co-modified graphene is different; chitosan modification liquid treatment is not used.

[0124] Comparative Example 5.

[0125] The difference from Optimization Example 3 is that no sodium alkyl sulfonate is added to the chitosan modification solution.

[0126] Comparative Example 6.

[0127] The difference from Optimization Example 3 is that no titanate coupling agent is added to the chitosan modified liquid.

[0128] Comparative Example 7.

[0129] The difference from Optimization Example 3 is that no coupling agent regulating liquid is added.

[0130] The performance measurement results of Examples 1-3 and Comparative Examples 1-7 are as follows

[0131]

[0132]

[0133] From Examples 1-3 and Comparative Examples 1-7, it can be concluded that the product of the present invention has excellent strength and elongation at break properties, the two of which can be improved in a coordinated manner, and has excellent stability in an oil environment;

[0134] As can be seen from Comparative Examples 1-4 and Example 3, without adding nano-silica co-modified graphene bodies, the performance of the product is significantly reduced, the strength and fracture properties are significantly reduced in an oil environment, and the oil resistance stability has a significant deterioration trend; in addition, the nano-silica co-modified graphene bodies are replaced by nano-silica and graphene in a weight ratio of 1:7, and the performance improvement of the product is not obvious; in the preparation method of the nano-silica co-modified graphene bodies, the pre-adjusted nano-silica is directly replaced by nano-silica raw materials and is not treated with chitosan modification liquid. The performance of the product has a deterioration trend. Only the nano-silica co-modified graphene bodies prepared by the method of the present invention have the most significant performance effect of the product;

[0135] As can be seen from Comparative Examples 5-6, the performance of the products is different when the raw materials of the chitosan modified liquid are different. Only when the chitosan modified liquid of the present invention is combined with the other conditions for preparing the modified graphene body with nano-silica, the performance of the prepared product is the most significant.

[0136] It can be seen from Comparative Example 1, Comparative Example 7 and Example 3 that without adding the coupling agent regulating liquid, the performance stability of the product has a significant deterioration trend. By co-combining the coupling agent regulating liquid with the nano-silica modified graphene body, the two synergistically enhance the performance of the product.

[0137] The preparation method of the coupling agent regulating solution is as follows:

[0138] The coupling agent KH560 was added to the ethanol solvent at a weight ratio of 1:4, and then 7.5% of sodium alginate and 2.5% of phosphate buffer solution were added, and the mixture was stirred evenly to obtain a coupling agent adjustment solution.

[0139] The present invention further explores the product performance through the coupling agent regulating liquid

[0140] Experimental Example 1.

[0141] The same as Example 3, except that no phosphate buffer solution was added to the coupling agent adjustment solution.

[0142] Experimental Example 2.

[0143] The same as Example 3, except that sodium alginate is not added to the coupling agent adjustment solution.

[0144] Experimental Example 3.

[0145] The same as Example 3, the only difference is that the coupling agent KH560 is a titanate coupling agent.

[0146]

[0147] As can be seen from Experimental Examples 1-3, the phosphate buffer solution, sodium alginate, and coupling agent KH560 in the coupling agent conditioning solution have an optimized improvement effect on the strength, fracture performance, and oil resistance stability of the product. At the same time, when the coupling agent KH560 is replaced by a titanate coupling agent, the performance change of the product is most obvious. The preparation of the coupling agent conditioning solution is proprietary, and only the coupling agent conditioning solution prepared by the method of the present invention can significantly improve the performance and stability of the product.

[0148] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations that come within the meaning and range of equivalents of the claims be embraced therein.

[0149] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. An oil-resistant dynamically vulcanized thermoplastic elastomer material, characterized in that: It includes the following raw materials in parts by weight: 35-45 parts of EPDM rubber, 25-30 parts of polyvinyl chloride resin, 1-4 parts of vulcanizing agent, 5-10 parts of nano-silica modified graphene, 3-7 parts of coupling agent regulating liquid, 1-3 parts of lubricant and 1-2 parts of antioxidant; The preparation method of the nano-silicon dioxide coordinated modified graphene body is: S01: placing the graphene in a ball mill for 10-20 min at a ball milling speed of 1000-1500 r / min, and then finishing the ball milling; S02: The product of S01 is placed in 3-5 times the volume of chitosan modification liquid and stirred for modification. After the modification is completed, a modified graphene agent is obtained; S03: Place nano-silica in a 3-5 times hydrochloric acid solution and stir evenly, then add 10-20% of lanthanum sulfate and 1-5% of sodium oxalate to the total amount of nano-silica, stir evenly, wash with water, and dry to obtain pre-conditioned nano-silica; S04: adding the pre-adjusted nano-silica to 5-10 times the modified graphene agent and stirring thoroughly, then washing with water and drying to obtain nano-silica coordinated modified graphene bodies; The chitosan modified liquid comprises the following raw materials in parts by weight: 10-20 parts of chitosan, 45-55 parts of deionized water, 1-4 parts of oxalic acid, 0.2-0.5 parts of titanate coupling agent and 1-3 parts of sodium alkyl sulfonate; the preparation method of the coupling agent regulating solution is as follows: The coupling agent KH560 was added to the ethanol solvent at a weight ratio of 1:4, and then 5-10% of the total amount of the coupling agent KH560 sodium alginate and 1-4% of the phosphate buffer solution were added and stirred evenly to obtain a coupling agent adjustment solution.

2. The oil-resistant dynamically vulcanized thermoplastic elastomer material according to claim 1, characterized in that: The dynamically vulcanized thermoplastic elastomer material comprises the following raw materials in parts by weight: 40 parts of EPDM rubber, 27.5 parts of polyvinyl chloride resin, 2.5 parts of vulcanizing agent, 7.5 parts of nano-silica modified graphene, 5 parts of coupling agent regulating liquid, 2 parts of lubricant and 1.5 parts of antioxidant.

3. The oil-resistant dynamically vulcanized thermoplastic elastomer material according to claim 1, characterized in that: The mass fraction of the hydrochloric acid solution is 2-5%.

4. The oil-resistant dynamically vulcanized thermoplastic elastomer material according to claim 1, characterized in that: The stirring modification has a rotation speed of 550-650 r / min, a stirring time of 20-30 min, and a stirring temperature of 35-40°C.

5. The oil-resistant dynamically vulcanized thermoplastic elastomer material according to claim 1, characterized in that: The pH value of the phosphate buffer solution is 5.

5.

6. The oil-resistant dynamically vulcanized thermoplastic elastomer material according to claim 1, characterized in that: The vulcanizing agent is dicumyl peroxide; The lubricant is one or more combinations of calcium stearate, stearic acid, and polyethylene wax; The antioxidant is the antioxidant DLTP.

7. The method for preparing an oil-resistant dynamically vulcanized thermoplastic elastomer material according to any one of claims 1 to 6, characterized in that: The following steps are involved: Step 1) Stirring and mixing EPDM rubber, polyvinyl chloride resin, vulcanizing agent, lubricant and antioxidant; Step 2) Adding nano-silica modified graphene and coupling agent regulating solution to the mixture of step 1) and continuing to stir and mix thoroughly, then washing with water, drying, and then melt mixing, the melt mixing temperature is 100-110°C, and the melt blending time is 10-15 minutes; Step 3) Finally, dynamic vulcanization is performed at a temperature of 180-185°C and a vulcanization time of 5-10 minutes to obtain a thermoplastic elastomer material.

Images