Preparation method of high-pressure hydrogen permeation resistant polymer rubber sealing product

Abstract

The application discloses a preparation method of high-pressure hydrogen permeation resistant polymer rubber sealing product, and relates to the technical field of rubber sealing, and comprises the following steps: S1, obtaining plasticated rubber; S2, obtaining mixed rubber; S3, placing the mixed rubber obtained in the step S2 on a vulcanizing machine to perform pre-vulcanization, passing through thin passages for three times, and performing secondary vulcanization, and the high-pressure hydrogen permeation resistant polymer rubber sealing product is obtained; the high-pressure hydrogen permeation resistant polymer rubber sealing product prepared by the application can be applied to various industrial fields, and plays an important role in high-temperature and high-pressure occasions. In the hydrogen energy field, due to the fact that hydrogen molecules are extremely small and highly active, hydrogen is easy to penetrate into many materials, therefore, the raw materials for preparing the rubber sealing product are greatly improved and the usage is optimized, so that the prepared rubber sealing product not only has excellent chemical resistance and high-temperature resistance, but also has good air tightness and high-pressure hydrogen permeation resistance in a high-pressure hydrogen medium environment.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of rubber sealing, in particular to a preparation method of high-molecular rubber sealing product with high-pressure hydrogen permeation resistance. BACKGROUND

[0002] In modern industry and life, there are many places with sealing needs, therefore, rubber sealing products are everywhere, and they have become an indispensable part of our daily life and industrial development with their unique performance and wide application field.

[0003] Rubber sealing products are mainly made of natural rubber or synthetic rubber, and have excellent elasticity, flex resistance and electrical insulation performance. Rubber sealing products can maintain good sealing effect in a wide temperature range, and have good resistance to various chemical media.

[0004] Rubber sealing products include: rotary shaft rubber seal, multi-lip reciprocating rubber seal, Y / M special-shaped section rubber seal, rubber gasket, V-shaped rubber seal and other products.

[0005] In order to cope with global climate change, the demand for energy saving and environmental protection is increasing, with the rapid development of new energy automobile industry, hydrogen energy automobile appears, and the hydrogen storage container of its device needs 90MPa superhigh pressure sealing system, and the rubber sealing product used in this sealing system needs to resist hydrogen permeation.

[0006] With the rapid development of hydrogen energy technology, hydrogen is gradually attracting global attention as a clean and efficient energy source. However, during the storage and transportation of hydrogen, how to ensure the safety and reliability of the system has become a problem to be solved. Among them, rubber sealing products, as an indispensable part of the hydrogen system, their high-pressure hydrogen permeation resistance is particularly important. This paper will conduct in-depth research on the high-pressure hydrogen permeation resistance of rubber sealing products.

[0007] Therefore, a preparation method of high-molecular rubber sealing product with high-pressure hydrogen permeation resistance is provided to solve the existing technical problems. SUMMARY

[0008] The purpose of the present application is to provide a preparation method of high-molecular rubber sealing product with high-pressure hydrogen permeation resistance to solve the deficiencies in the prior art.

[0009] The technical scheme adopted by the present application is as follows:

[0010] A preparation method of high-molecular rubber sealing product with high-pressure hydrogen permeation resistance, comprising the following steps:

[0011] S1 add ethylene propylene rubber, natural rubber into the internal mixer, heat to 92-95℃ at a rate of 3℃ / min, plasticize for 40min, to get plasticized rubber;

[0012] S2 add plasticized rubber, nano composite material, stearic acid, antioxidant, vulcanizing agent, accelerator into the internal mixer, heat to 98℃ at a rate of 5℃ / min, mix for 30-40min, to get mixed rubber;

[0013] S3 put the mixed rubber obtained in step S2 into the vulcanizing machine, pre-vulcanize at 120-128℃ for 12-16min, pass through the thin pass 3 times, and then secondarily vulcanize at 155-160℃ for 6-8min, to get the product.

[0014] As a further technical solution: the preparation method of nano composite material in S2 is:

[0015] Add zinc acetate and lanthanum chloride into ethylene glycol monomethyl ether, adjust the temperature to 60℃, and keep stirring for 30min;

[0016] Then add ethanolamine dropwise, continue to keep stirring and mixing for 2 hours, and stand for 20 hours to obtain a first reaction solution;

[0017] Disperse carbon nanotubes uniformly into ethylene glycol monomethyl ether to obtain a carbon nanotube dispersion solution;

[0018] Add the first reaction solution into the carbon nanotube dispersion solution, and then ultrasonic disperse for 10min to obtain a composite dispersion solution;

[0019] Dry the composite dispersion solution to constant weight to obtain a composite material;

[0020] Perform a first calcination treatment on the composite material in a muffle furnace, cool to room temperature, and obtain a calcined material;

[0021] Mix silicate and anhydrous ethanol, then add deionized water, continue to stir and disperse for 30min, add the calcined material, ultrasonic disperse, stand for 2 hours, then dry to constant weight, and finally perform a second calcination in a muffle furnace, cool to room temperature, to obtain a nano composite material.

[0022] As a further technical solution: the molar ratio of zinc acetate and lanthanum chloride is 2:1;

[0023] The mass ratio of zinc acetate, ethylene glycol monomethyl ether and ethanolamine is 1:20:3;

[0024] The mass fraction of the carbon nanotube dispersion solution is 10%;

[0025] The volume ratio of the first reaction solution and the carbon nanotube dispersion solution is 3:1-1.5.

[0026] As a further technical solution: the first calcination temperature is 500 DEG C, and the time is 40 min.

[0027] As a further technical solution: the mass ratio of the silicate, anhydrous ethanol and deionized water is 1:6:4.

[0028] The mass ratio of the silicate and the calcined material is 1:3.

[0029] The second calcination temperature is 550 DEG C, and the time is 45 min.

[0030] As a further technical solution: the stirring speed during plasticizing is 150 r / min.

[0031] The stirring speed during mixing is 300 r / min.

[0032] As a further technical solution: the high-pressure hydrogen permeation resistant polymer rubber sealing product comprises, by weight: 50-60 parts of ethylene-propylene-diene rubber, 25-28 parts of natural rubber, 12-15 parts of nano composite material, 1-2 parts of stearic acid, 1-3 parts of antioxidant, 1-1.5 parts of vulcanizing agent, and 0.5-0.8 parts of accelerator.

[0033] As a further technical solution: the antioxidant is antioxidant MB.

[0034] As a further technical solution: the vulcanizing agent is sulfur.

[0035] As a further technical solution, the accelerator is accelerator DTDM.

[0036] Beneficial effects:

[0037] The high-pressure hydrogen permeation resistant polymer rubber sealing product prepared by the application can be applied to various industrial fields, and plays an important role in high-temperature and high-pressure environments. In the hydrogen energy field, due to the small molecules and high activity of hydrogen, it is easy to penetrate into many materials. Therefore, the raw materials for preparing the rubber sealing product are greatly improved and optimized in quantity, so that the prepared rubber sealing product not only has excellent chemical resistance and high-temperature resistance, but also has good airtightness and high-pressure hydrogen permeation resistance in high-pressure hydrogen medium environment.

[0038] Improve the gas barrier properties: nanoparticles have extremely small size and high specific surface area, can form a dense network structure in the rubber matrix. The present application by introducing a special nano composite material, by the nano composite material can produce strong interaction with rubber molecules, this effect not only enhances the binding force between rubber molecules, but also makes the nano composite material particles can be uniformly dispersed in the rubber, forming a stable network structure, greatly improve the air tightness of rubber sealing products, thereby improving the performance of high pressure hydrogen permeability.

[0039] Because in the traditional rubber sealing products, the gas molecules permeate mainly through the gap between the rubber molecular chain, therefore, the present application by optimizing the raw material components of rubber sealing products, by introducing a special nano composite material, can prevent this process, by the introduction of nano composite material, can form a "barrier" in the rubber sealing products, so as to greatly block the hydrogen molecule permeation, and, because the nano composite material prepared by the present application is not a single nanoparticle, its structure is more complex, can increase the tortuosity of hydrogen molecule diffusion path, further reduce the hydrogen permeability. DETAILED DESCRIPTION

[0040] The technical solutions in the embodiments of the present application will be described below clearly and completely. Obviously, the described embodiments are only a part of the embodiments of the present application, not all. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the present application.

[0041] Embodiment 1

[0042] A preparation method of a high polymer rubber sealing product with high pressure hydrogen permeability resistance, comprising the following steps:

[0043] S1 add EPDM rubber and natural rubber into the internal mixer, heat to 92℃ at a heating rate of 3℃ / min, plasticize for 40min to obtain plasticized rubber;

[0044] S2 add the plasticized rubber in step S1, nano composite material, stearic acid, antioxidant, vulcanizing agent, accelerator into the mixer, heat to 98℃ at a heating rate of 5℃ / min, mix for 30min to obtain the mixed rubber;

[0045] S3 put the mixed rubber obtained in step S2 into the vulcanizing machine, pre-vulcanize at 120℃ for 12min, pass through the thin pass 3 times, and then secondarily vulcanize at 155℃ for 6min to obtain the product.

[0046] The preparation method of the nano composite material is:

[0047] Zinc acetate and lanthanum chloride are added into ethylene glycol monomethyl ether, the temperature is adjusted to 60 DEG C, and the mixture is stirred for 30 min;

[0048] Then, ethanolamine is added dropwise, the mixture is stirred and heated for 2 h, and then is left to stand for 20 h to obtain a first reaction solution;

[0049] Carbon nanotubes are uniformly dispersed in ethylene glycol monomethyl ether to obtain a carbon nanotube dispersion;

[0050] The first reaction solution is added into the carbon nanotube dispersion, and then is ultrasonically dispersed for 10 min to obtain a composite dispersion;

[0051] The composite dispersion is dried to constant weight to obtain a composite material;

[0052] The composite material is subjected to primary calcination in a muffle furnace, and then is cooled to room temperature to obtain a calcined material;

[0053] Silicate is mixed with anhydrous ethanol, and then deionized water is added, and the mixture is stirred and dispersed for 30 min, and then the calcined material is added, and the mixture is ultrasonically dispersed, and then is left to stand for 2 h, and then is dried to constant weight, and finally is subjected to secondary calcination in a muffle furnace, and then is cooled to room temperature to obtain a nanocomposite material.

[0054] The molar ratio of zinc acetate to lanthanum chloride is 2:1;

[0055] The mass ratio of zinc acetate to ethylene glycol monomethyl ether to ethanolamine is 1:20:3;

[0056] The mass fraction of the carbon nanotube dispersion is 10%;

[0057] The volume ratio of the first reaction solution to the carbon nanotube dispersion is 3:1.

[0058] The primary calcination temperature is 500 DEG C, and the time is 40 min.

[0059] The mass ratio of silicate to anhydrous ethanol to deionized water is 1:6:4;

[0060] The mass ratio of silicate to calcined material is 1:3;

[0061] The secondary calcination temperature is 550 DEG C, and the time is 45 min.

[0062] The stirring speed during plastication is 150 r / min;

[0063] The stirring speed during mixing is 300 r / min.

[0064] The high-pressure hydrogen permeation resistant polymer rubber sealing products, by weight, consist of: 50 parts EPDM rubber, 25 parts natural rubber, 12 parts nanocomposite material, 1 part stearic acid, 1 part antioxidant MB, 1 part sulfur, and 0.5 parts accelerator DTDM.

[0065] Example 2

[0066] A method for preparing a polymer rubber sealing product with high pressure hydrogen permeation resistance includes the following steps:

[0067] S1 mixes EPDM rubber and natural rubber and adds them to a mixer. The mixture is heated to 93°C at a heating rate of 3°C / min and then masticated for 40 minutes to obtain masticated rubber.

[0068] S2. The plasticized rubber, nanocomposite material, stearic acid, antioxidant, vulcanizing agent and accelerator from step S1 are mixed and added to the mixer. The mixture is heated to 98°C at a heating rate of 5°C / min and mixed for 30min to obtain the compounded rubber.

[0069] S3. The compound obtained in step S2 is placed on a vulcanizing machine and pre-vulcanized at 125°C for 15 minutes. After passing through a thin tube 3 times, it is vulcanized again at 158°C for 7 minutes to obtain the final product.

[0070] The preparation method of nanocomposite materials is as follows:

[0071] Add zinc acetate and lanthanum chloride to ethylene glycol monomethyl ether, adjust the temperature to 60°C, and stir for 30 minutes.

[0072] Add ethanolamine dropwise, continue stirring and mixing for 2 hours, and let stand for 20 hours to obtain the first reaction solution;

[0073] Carbon nanotubes were uniformly dispersed in ethylene glycol monomethyl ether to obtain a carbon nanotube dispersion.

[0074] The first reaction solution was added to the carbon nanotube dispersion, and then ultrasonically dispersed for 10 min to obtain the composite dispersion.

[0075] The composite dispersion was dried to constant weight to obtain the composite material;

[0076] The composite material was calcined once in a muffle furnace and then cooled to room temperature to obtain the calcined material.

[0077] The silicate ester was mixed with anhydrous ethanol, then deionized water was added, and the mixture was stirred and dispersed for 30 minutes. Then, calcined material was added, and after ultrasonic dispersion, it was allowed to stand for 2 hours. Then, it was dried to constant weight, and finally calcined again in a muffle furnace and cooled to room temperature to obtain nanocomposite material.

[0078] The molar ratio of zinc acetate to lanthanum chloride is 2:1;

[0079] The mass ratio of zinc acetate, ethylene glycol monomethyl ether and ethanolamine is 1:20:3;

[0080] The mass fraction of the carbon nanotube dispersion liquid is 10%;

[0081] The volume ratio of the first reaction liquid and the carbon nanotube dispersion liquid is 3:1.2.

[0082] The first calcination temperature is 500℃, and the time is 40min.

[0083] The mass ratio of silicate, anhydrous ethanol and deionized water is 1:6:4;

[0084] The mass ratio of silicate and calcined material is 1:3;

[0085] The second calcination temperature is 550℃, and the time is 45min.

[0086] The stirring speed during plasticizing is 150r / min;

[0087] The stirring speed during mixing is 300r / min.

[0088] The high polymer rubber sealing product with high pressure hydrogen permeation resistance comprises, by weight: 52 parts of ethylene-propylene-diene rubber, 26 parts of natural rubber, 13 parts of nano composite material, 1.5 parts of stearic acid, 2 parts of antioxidant MB, 1.2 parts of sulfur, and 0.6 parts of accelerator DTDM.

[0089] Example 3

[0090] A method for preparing a high polymer rubber sealing product with high pressure hydrogen permeation resistance, comprising the following steps:

[0091] S1: Add ethylene-propylene-diene rubber and natural rubber into a mixing mill, and heat to 94℃ at a heating rate of 3℃ / min, and plasticize for 40min to obtain plasticized rubber;

[0092] S2: Add the plasticized rubber in step S1, nano composite material, stearic acid, antioxidant, vulcanizing agent and accelerator into a mixing mill, and heat to 98℃ at a heating rate of 5℃ / min, and mix for 35min to obtain mixed rubber;

[0093] S3: Put the mixed rubber obtained in step S2 into a vulcanizing machine, and pre-vulcanize at 124℃ for 15min, then pass through thin pass 3 times, and secondarily vulcanize at 158℃ for 7min to obtain the product.

[0094] The preparation method of the nano composite material is:

[0095] Add zinc acetate and lanthanum chloride into ethylene glycol monomethyl ether, adjust the temperature to 60℃, and keep stirring for 30min.

[0096] Then, ethanolamine is added dropwise, and the mixture is continuously stirred and heated for 2 hours, and then left to stand for 20 hours to obtain a first reaction solution;

[0097] The carbon nanotubes are uniformly dispersed in ethylene glycol monomethyl ether to obtain a carbon nanotube dispersion liquid;

[0098] The first reaction solution is added to the carbon nanotube dispersion liquid, and then ultrasonic dispersion is performed for 10 minutes to obtain a composite dispersion liquid;

[0099] The composite dispersion liquid is dried to constant weight to obtain a composite material;

[0100] The composite material is subjected to primary calcination treatment in a muffle furnace, and then cooled to room temperature to obtain a calcined material;

[0101] The silicate is mixed with anhydrous ethanol, and then deionized water is added, and the mixture is continuously stirred and dispersed for 30 minutes, and then the calcined material is added, and ultrasonic dispersion is performed, and then the mixture is left to stand for 2 hours, and then dried to constant weight, and finally subjected to secondary calcination in a muffle furnace, and then cooled to room temperature to obtain a nanocomposite material.

[0102] The molar ratio of zinc acetate to lanthanum chloride is 2:1;

[0103] The mass ratio of zinc acetate to ethylene glycol monomethyl ether to ethanolamine is 1:20:3;

[0104] The mass fraction of the carbon nanotube dispersion liquid is 10%;

[0105] The volume ratio of the first reaction solution to the carbon nanotube dispersion liquid is 3:1.2.

[0106] The primary calcination temperature is 500°C, and the time is 40 minutes.

[0107] The mass ratio of the silicate to anhydrous ethanol to deionized water is 1:6:4;

[0108] The mass ratio of the silicate to the calcined material is 1:3;

[0109] The secondary calcination temperature is 550°C, and the time is 45 minutes.

[0110] The stirring speed during plastication is 150 r / min;

[0111] The stirring speed during mixing is 300 r / min.

[0112] The high-pressure hydrogen permeation resistant polymer rubber sealing product comprises, by weight parts: 55 parts of ethylene-propylene-diene rubber, 27 parts of natural rubber, 14 parts of nanocomposite material, 1.8 parts of stearic acid, 2 parts of antioxidant MB, 1.3 parts of sulfur, and 0.7 parts of accelerator DTDM.

[0113] Example 4

[0114] A method for preparing a high-pressure hydrogen permeation resistant polymer rubber sealing product, comprising the following steps:

[0115] S1. Add EPDM and natural rubber into a mixer, and heat to 93℃ at a heating rate of 3℃ / min, and plasticize for 40min to obtain plasticized rubber;

[0116] S2. Add the plasticized rubber in step S1, nano-composite material, stearic acid, antioxidant, vulcanizing agent, and accelerator into a mixer, and heat to 98℃ at a heating rate of 5℃ / min, and mix for 35min to obtain mixed rubber;

[0117] S3. Put the mixed rubber obtained in step S2 into a vulcanizing machine, and pre-vulcanize at 124℃ for 13min, then pass through thin pass 3 times, and secondarily vulcanize at 157℃ for 7min to obtain the product.

[0118] The method for preparing the nano-composite material is:

[0119] Add zinc acetate and lanthanum chloride into ethylene glycol monomethyl ether, adjust the temperature to 60℃, and keep stirring for 30min;

[0120] Then, add ethanolamine dropwise, continue to keep stirring for 2 hours, and stand for 20 hours to obtain a first reaction solution;

[0121] Disperse carbon nanotubes uniformly in ethylene glycol monomethyl ether to obtain a carbon nanotube dispersion solution;

[0122] Add the first reaction solution into the carbon nanotube dispersion solution, and then ultrasonically disperse for 10min to obtain a composite dispersion solution;

[0123] Dry the composite dispersion solution to constant weight to obtain a composite material;

[0124] Perform primary calcination treatment on the composite material in a muffle furnace, and cool to room temperature to obtain a calcined material;

[0125] Mix silicate and anhydrous ethanol, then add deionized water, continue to stir and disperse for 30min, add the calcined material, ultrasonically disperse, stand for 2 hours, then dry to constant weight, and finally perform secondary calcination in a muffle furnace, and cool to room temperature to obtain the nano-composite material.

[0126] The molar ratio of zinc acetate to lanthanum chloride is 2:1;

[0127] The mixed mass ratio of zinc acetate to ethylene glycol monomethyl ether and ethanolamine is 1:20:3;

[0128] The mass fraction of the carbon nanotube dispersion solution is 10%;

[0129] The first reaction liquid, carbon nanotube dispersion liquid mixed volume ratio is 3:1.2.

[0130] The first time calcination temperature is 500℃, and the time is 40min.

[0131] The mass ratio of silicate, anhydrous ethanol and deionized water is 1:6:4;

[0132] The mass ratio of silicate and calcined material is 1:3;

[0133] The second time calcination temperature is 550℃, and the time is 45min.

[0134] The stirring speed during plasticizing is 150r / min;

[0135] The stirring speed during mixing is 300r / min.

[0136] The high-pressure hydrogen permeation resistant polymer rubber sealing product includes, by weight: 54 parts of ethylene-propylene-diene rubber, 26 parts of natural rubber, 14 parts of nano composite material, 1.5 parts of stearic acid, 2 parts of antioxidant MB, 1.2 parts of sulfur, and 0.6 parts of accelerator DTDM.

[0137] Example 5

[0138] A high-pressure hydrogen permeation resistant polymer rubber sealing product preparation method, comprising the following steps:

[0139] S1: Add ethylene-propylene-diene rubber and natural rubber into a mixing mill, heat to 95℃ at a heating rate of 3℃ / min, plasticize for 40min to obtain plasticized rubber;

[0140] S2: Add the plasticized rubber in step S1, nano composite material, stearic acid, antioxidant, vulcanizing agent and accelerator into the mixing mill, heat to 98℃ at a heating rate of 5℃ / min, mix for 40min to obtain mixed rubber;

[0141] S3: Put the mixed rubber obtained in step S2 into a vulcanizing machine, pre-vulcanize at 128℃ for 16min, pass through thin pass 3 times, and then secondarily vulcanize at 160℃ for 8min to obtain the product.

[0142] The nano composite material preparation method is:

[0143] Add zinc acetate and lanthanum chloride into ethylene glycol monomethyl ether, adjust the temperature to 60℃, and keep stirring for 30min;

[0144] Then add ethanolamine dropwise, continue to keep stirring and mixing for 2 hours, stand for 20 hours to obtain the first reaction liquid;

[0145] The carbon nanotubes are uniformly dispersed into monomethyl ether of ethylene glycol to obtain a carbon nanotube dispersion liquid;

[0146] The first reaction liquid is added into the carbon nanotube dispersion liquid, and then ultrasonic dispersion is performed for 10 min to obtain a composite dispersion liquid;

[0147] The composite dispersion liquid is dried to constant weight to obtain a composite material;

[0148] The composite material is subjected to primary calcination treatment in a muffle furnace, and cooled to room temperature to obtain a calcined material;

[0149] The silicate is mixed with anhydrous ethanol, and then deionized water is added, and stirring and dispersion are continuously performed for 30 min, and then the calcined material is added, and after ultrasonic dispersion, standing is performed for 2 hours, and then drying to constant weight is performed, and finally secondary calcination in a muffle furnace is performed, and cooled to room temperature to obtain a nanocomposite material.

[0150] The molar ratio of zinc acetate to lanthanum chloride is 2:1;

[0151] The mass ratio of the zinc acetate to monomethyl ether of ethylene glycol and ethanolamine is 1:20:3;

[0152] The mass fraction of the carbon nanotube dispersion liquid is 10%;

[0153] The volume ratio of the first reaction liquid to the carbon nanotube dispersion liquid is 3:1.5.

[0154] The primary calcination temperature is 500 DEG C, and the time is 40 min.

[0155] The mass ratio of the silicate to anhydrous ethanol and deionized water is 1:6:4;

[0156] The mass ratio of the silicate to the calcined material is 1:3;

[0157] The secondary calcination temperature is 550 DEG C, and the time is 45 min.

[0158] The stirring speed during plastication is 150 r / min;

[0159] The stirring speed during mixing is 300 r / min.

[0160] The high-pressure hydrogen permeation resistant polymer rubber sealing product comprises, by weight parts: 60 parts of ethylene-propylene-diene rubber, 28 parts of natural rubber, 15 parts of nanocomposite material, 2 parts of stearic acid, 3 parts of antioxidant MB, 1.5 parts of sulfur, and 0.8 parts of accelerator DTDM.

[0161] Comparative Example 1:

[0162] On the basis of the technical solution of Example 1, the nanocomposite material is not added, and the remaining technical solutions remain unchanged.

[0163] Comparative Example 2

[0164] On the basis of the technical solution of Example 1, the nanocomposite material is replaced by equal amount of nano-zinc oxide, and the rest of the technical solution remains unchanged.

[0165] Test:

[0166] Test the samples of the same specification of the example and the comparative example:

[0167] Hardness detection: refer to the standard of GB / T531.1-2008;

[0168] Table 1

[0169] Shore hardness A Example 1 90 Example 2 92 Example 3 91 Example 4 90 Example 5 92 Comparative Example 1 78 Comparative Example 2 86

[0170] As shown in Table 1, the high polymer rubber sealing product prepared by the application has higher hardness.

[0171] High-pressure hydrogen permeation test (hydrogen medium, pressure 75 MPa, 88℃, 72 hours):

[0172] Table 2 hardness change

[0173] Hardness change rate % Example 1 -1.88 Example 2 -1.94 Example 3 -1.85 Example 4 -1.90 Example 5 -1.93 Comparative Example 1 -6.67 Comparative Example 2 -4.02

[0174] As shown in Table 2, the hardness change of the high polymer rubber sealing product prepared by the application is small under high-pressure hydrogen medium, indicating that it has good performance of resisting the influence of high-pressure hydrogen.

[0175] Table 3 volume change

[0176] Volume change rate % Example 1 +0.83 Example 2 +0.92 Example 3 +0.78 Example 4 +0.85 Example 5 +0.87 Comparative Example 1 +2.33 Comparative Example 2 +1.54

[0177] As shown in Table 3, the hardness change of the high polymer rubber sealing product prepared by the application is small under high-pressure hydrogen medium, indicating that it has good performance of resisting high-pressure hydrogen permeation. The above only describes the preferred embodiments of the application, but the application is not limited to the embodiments shown, any change or modification made according to the concept of the application, or equivalent embodiments with equivalent changes, as long as they are within the scope of the application.

Claims

1. A method for producing a high polymer rubber seal product resistant to high pressure hydrogen permeation, characterized by comprising the steps of: It comprises the following steps: ​ S1 add the ethylene propylene diene rubber and the natural rubber into a mixer, and heat to 92-95 DEG C at a heating rate of 3 DEG C / min, and plasticize for 40 min to obtain plasticized rubber; S2 add the plasticized rubber, the nano composite material, the stearic acid, the antioxidant, the vulcanizing agent and the accelerator into the mixer, and heat to 98 DEG C at a heating rate of 5 DEG C / min, and mix for 30-40 min to obtain mixed rubber; S3 place the mixed rubber obtained in S2 on a vulcanizing machine, and pre-vulcanize at 120-128 DEG C for 12-16 min, and then pass through the thin passage for 3 times, and then secondarily vulcanize at 155-160 DEG C for 6-8 min to obtain the high polymer rubber sealing product. Add zinc acetate and lanthanum chloride into ethylene glycol monomethyl ether, and adjust the temperature to 60 DEG C, and keep stirring for 30 min; Then add ethanolamine, and continue to keep stirring for 2 hours, and stand for 20 hours to obtain the first reaction liquid; Disperse the carbon nanotube into ethylene glycol monomethyl ether to obtain a carbon nanotube dispersion liquid; Add the first reaction liquid into the carbon nanotube dispersion liquid, and then ultrasonic disperse for 10 min to obtain a composite dispersion liquid; Dry the composite dispersion liquid to constant weight to obtain a composite material; Perform primary calcination treatment on the composite material in a muffle furnace, and cool to room temperature to obtain a calcined material; Mix silicate and anhydrous ethanol, and then add deionized water, and continue to stir and disperse for 30 min, and then add the calcined material, and ultrasonic disperse, and stand for 2 hours, and then dry to constant weight, and finally perform secondary calcination in a muffle furnace, and cool to room temperature to obtain the nano composite material.

2. The method of claim 1, wherein the method further comprises: (a) applying a primer layer to the surface of the polymer rubber article; and (b) applying a topcoat layer to the primer layer. The molar ratio of zinc acetate to lanthanum chloride is 2:1; The mass ratio of zinc acetate to ethylene glycol monomethyl ether and ethanolamine is 1:20:3; The mass fraction of the carbon nanotube dispersion liquid is 10%; The volume ratio of the first reaction liquid to the carbon nanotube dispersion liquid is 3:1-1.

5.

3. The method of claim 1, wherein the method further comprises: (a) applying a primer layer to the surface of the polymer rubber article; and (b) applying a topcoat layer to the primer layer. The primary calcination temperature is 500 DEG C, and the time is 40 min.

4. The method of claim 1, wherein the method further comprises: The mass ratio of silicate to anhydrous ethanol and deionized water is 1:6:4; ​ The mass ratio of silicate to calcined material is 1:3; The secondary calcination temperature is 550 DEG C, and the time is 45 min.

5. The method of claim 1, wherein the method further comprises: The stirring speed during plasticizing is 150 r / min; ​ The stirring speed during mixing is 300 r / min.

6. The method of claim 1, wherein the method further comprises: The high polymer rubber sealing product with high pressure hydrogen permeation resistance comprises, by weight parts, 50-60 parts of ethylene propylene diene rubber, 25-28 parts of natural rubber, 12-15 parts of nano composite material, 1-2 parts of stearic acid, 1-3 parts of antioxidant, 1-1.5 parts of vulcanizing agent, and 0.5-0.8 parts of accelerator. ​ 7. The method of claim 6, wherein the method further comprises: The antioxidant is antioxidant MB. ​ 8. The method of claim 1, wherein the method further comprises: The vulcanizing agent is sulfur. ​ 9. The method of claim 1, wherein the method further comprises the step of: The accelerator is accelerator DTDM. ​