阅读说明：本技术 一种耐油防撕裂密封件材料及其制备方法 (Oil-resistant anti-tearing sealing element material and preparation method thereof ) 是由 张茂刚 于 2020-12-22 设计创作，主要内容包括：本发明公开了一种耐油防撕裂密封件材料,其特征在于,由如下重量份的各组分制备而成：端乙烯基液体丁腈橡胶15-20份、2,3-二巯基丁二酸/端氨基液体丁腈橡胶缩聚物10-20份、丁腈橡胶40-60份、乙烯基氟硅油5-10份、三氟氯菊酸改性端氨基液体丁腈橡胶4-8份、偶联剂2-3份、纳米硼纤维3-6份、填充料20-30份、光引发剂1-3份。本发明还提供了一种所述耐油防撕裂密封件材料的制备方法。本发明公开的耐油防撕裂密封件材料耐油防撕裂效果好,耐热、耐老化性能佳,耐磨、气密性、阻燃和耐用性优异,综合性能和性能稳定性足。(The invention discloses an oil-resistant and tear-resistant sealing element material which is characterized by being prepared from the following components in parts by weight: 15-20 parts of vinyl-terminated liquid nitrile rubber, 10-20 parts of 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate, 40-60 parts of nitrile rubber, 5-10 parts of vinyl fluorosilicone oil, 4-8 parts of trifluoro-chloro-chrysanthemic acid modified amino-terminated liquid nitrile rubber, 2-3 parts of coupling agent, 3-6 parts of nano boron fiber, 20-30 parts of filler and 1-3 parts of photoinitiator. The invention also provides a preparation method of the oil-resistant and tear-resistant sealing element material. The oil-resistant and anti-tearing sealing element material disclosed by the invention has the advantages of good oil-resistant and anti-tearing effect, good heat resistance and aging resistance, excellent wear resistance, air tightness, flame retardance and durability, and sufficient comprehensive performance and performance stability.)

1. The oil-resistant and tear-resistant sealing element material is characterized by being prepared from the following components in parts by weight: 15-20 parts of vinyl-terminated liquid nitrile rubber, 10-20 parts of 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate, 40-60 parts of nitrile rubber, 5-10 parts of vinyl fluorosilicone oil, 4-8 parts of trifluoro-chloro-chrysanthemic acid modified amino-terminated liquid nitrile rubber, 2-3 parts of coupling agent, 3-6 parts of nano boron fiber, 20-30 parts of filler and 1-3 parts of photoinitiator.

2. The oil resistant, tear resistant seal material of claim 1 wherein the photoinitiator is at least one of 2-hydroxy-2-methyl-1-phenyl acetone, benzoin ethyl ether, benzoin isopropyl ether; the filler is at least one of ordinary portland cement PO42.5, glass fiber powder, white carbon black and walnut shell powder; the particle size of the filler is 400-800 meshes.

3. The oil-resistant and tear-resistant sealing member material as claimed in claim 1, wherein the nano boron fiber has a diameter of 300-500nm, an aspect ratio (12-16): 1; the coupling agent is at least one of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.

4. The oil-resistant tear-resistant sealing member material according to claim 1, wherein the preparation method of the amino-terminated liquid nitrile rubber modified by trichloro-chrysanthemic acid comprises the following steps: adding the chlorotrifluoro chrysanthemic acid and the amino-terminated liquid nitrile rubber into an organic solvent, stirring and reacting for 6-8 hours at the temperature of 30-40 ℃, and after the reaction is finished, removing the solvent by rotary evaporation to obtain the chlorotrifluoro chrysanthemic acid modified amino-terminated liquid nitrile rubber.

5. The oil-resistant tear-resistant seal material according to claim 4, wherein the mass ratio of the trichloro-chrysanthemic acid, the amino-terminated liquid nitrile rubber and the organic solvent is (0.1-0.3): (3-5): (15-25); the organic solvent is any one of ethyl acetate, butyl acetate, chlorobenzene, methyl ethyl ketone and dichloromethane.

6. The oil-resistant and tear-resistant sealing member material according to claim 1, wherein the amino-terminated liquid nitrile rubber is a liquid nitrile polymer containing amino groups at the chain end, the number average molecular weight is 3500, and the amino group content is 17%; the vinyl fluorosilicone oil is KX-205 vinyl fluorosilicone oil; the grade of the nitrile rubber is N41; the grade of the vinyl-terminated liquid nitrile rubber is any one of VTBN1300X3 and VTBN1300X 43.

7. The oil-resistant tear-resistant seal material according to claim 1, wherein the preparation method of the 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate comprises the following steps: adding 2, 3-dimercaptosuccinic acid and amino-terminated liquid nitrile rubber into chlorobenzene, uniformly mixing, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 4-dimethylaminopyridine into the chlorobenzene, carrying out reflux stirring reaction for 6-8 hours at the temperature of 110-150 ℃ in an inert gas atmosphere, carrying out rotary evaporation to remove a solvent and a by-product after the reaction is finished, precipitating the solvent and the by-product in water, washing the precipitate with ethanol for 3-6 times, and finally carrying out rotary evaporation to remove the ethanol to obtain the 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate.

8. The oil-resistant tear-resistant seal material of claim 7 wherein the molar ratio of 2, 3-dimercaptosuccinic acid, amino terminated liquid nitrile rubber, chlorobenzene, 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, 4-dimethylaminopyridine is 1:1 (6-10) to (0.8-1.2) to 0.5.

9. The oil resistant, tear resistant seal material of claim 7 wherein said inert gas is any one of nitrogen, helium, neon, argon.

10. A method of making an oil resistant tear resistant seal material according to any one of claims 1 to 9, comprising the steps of: according to the weight ratio, the components are put into an internal mixer for mixing for 7-10 minutes, then the mixture is discharged to a cutting machine for discharging, then the mixture is quickly placed in a die and is die-pressed for 9-12 minutes at the temperature of 160-180 ℃ and under the pressure of 8-15MPa, and finally the oil-resistant anti-tearing sealing element material is prepared by irradiating under the ultraviolet light with the wavelength of 280-380nm for 30-40 minutes at room temperature.

Technical Field

The invention relates to the technical field of sealing element materials, in particular to an oil-resistant anti-tearing sealing element material and a preparation method thereof.

Background

The seal is a material or a part that prevents fluid or solid particles from leaking from between adjacent bonding surfaces and prevents foreign substances such as dust and moisture from intruding into parts inside the machine equipment. Although the sealing element is small, the sealing element has the function of becoming a basic part and a fitting in the main national economy industries such as national defense, chemical engineering, petroleum, coal, transportation, mechanical manufacturing and the like, and plays a very important role in the development of the national economy.

The ideal seal is required to have not only oil and heat resistance, but also high gas tightness and tear resistance. However, the existing sealing element materials have the defects of low tearing strength, poor sealing effect, insufficient oil resistance, heat resistance, wear resistance and flame retardance, and further improvement of durability.

For example, the chinese patent document "ethylene propylene diene monomer rubber material for automotive cooling system seal and preparation method thereof (grant publication No. CN 102304255B)" discloses an ethylene propylene diene monomer rubber material for automotive cooling system seal and preparation method thereof, which comprises the following raw materials by weight: 53-58 parts of ethylene propylene diene monomer raw rubber, 20-25 parts of high-wear-resistance carbon black, 5-10 parts of semi-reinforcing carbon black, 3-5 parts of zinc oxide, 0.5-1.0 part of stearic acid, 1.0-1.5 parts of 4,4 '-bis (phenylisopropyl) diphenylamine, 0.5-1.0 part of 2-mercaptomethylbenzimidazole zinc salt, 2.0-2.5 parts of alpha, alpha' -di-tert-butyl peroxide diisopropylbenzene and 1.5-2.0 parts of triallyl isocyanurate. The rubber sealing element material prepared by the invention has the advantages of high temperature resistance, overheating coolant soaking resistance and excellent low compression permanent deformation performance, but has the problems of insufficient oil resistance and insufficient tear resistance.

Therefore, a more effective method is sought, and the oil-resistant and tear-resistant sealing element material which has good oil-resistant and tear-resistant effects, good heat resistance and aging resistance, excellent wear resistance, flame retardance and excellent durability is very important.

Disclosure of Invention

In order to overcome the defects in the prior art, the invention provides the oil-resistant anti-tearing sealing element material which has good oil-resistant anti-tearing effect, good heat resistance and aging resistance, excellent wear resistance, flame retardance, air tightness and durability and sufficient comprehensive performance and performance stability. Meanwhile, the invention also provides a preparation method of the oil-resistant and tear-resistant sealing element material, which is simple in process, convenient to operate and control, high in preparation efficiency and suitable for industrial popularization and application.

In order to achieve the aim, the invention adopts the technical scheme that the oil-resistant anti-tearing sealing element material is characterized by being prepared from the following components in parts by weight: 15-20 parts of vinyl-terminated liquid nitrile rubber, 10-20 parts of 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate, 40-60 parts of nitrile rubber, 5-10 parts of vinyl fluorosilicone oil, 4-8 parts of trifluoro-chloro-chrysanthemic acid modified amino-terminated liquid nitrile rubber, 2-3 parts of coupling agent, 3-6 parts of nano boron fiber, 20-30 parts of filler and 1-3 parts of photoinitiator.

Preferably, the photoinitiator is at least one of 2-hydroxy-2-methyl-1-phenyl acetone, benzoin ethyl ether and benzoin isopropyl ether.

Preferably, the filler is at least one of ordinary portland cement PO42.5, glass fiber powder, white carbon black and walnut shell powder; the particle size of the filler is 400-800 meshes.

Preferably, the diameter of the nano boron fiber is 300-500nm, and the length-diameter ratio is (12-16): 1.

Preferably, the coupling agent is at least one of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.

Preferably, the preparation method of the trifluoro-chloro-chrysanthemic acid modified amino-terminated liquid nitrile rubber comprises the following steps: adding the chlorotrifluoro chrysanthemic acid and the amino-terminated liquid nitrile rubber into an organic solvent, stirring and reacting for 6-8 hours at the temperature of 30-40 ℃, and after the reaction is finished, removing the solvent by rotary evaporation to obtain the chlorotrifluoro chrysanthemic acid modified amino-terminated liquid nitrile rubber.

Preferably, the mass ratio of the trifluoro-chloro chrysanthemic acid to the amino-terminated liquid nitrile rubber to the organic solvent is (0.1-0.3) to (3-5) to (15-25); the organic solvent is any one of ethyl acetate, butyl acetate, chlorobenzene, methyl ethyl ketone and dichloromethane.

Preferably, the amino-terminated liquid nitrile rubber refers to a nitrile rubber containing amino (-NH) at the chain end₂) The liquid nitrile polymer of (1) is abbreviated as ATBN, and the number average molecular weight is 3500. The amino group content was about 17% and was purchased from Citeron industries, Inc. of Shanghai.

Preferably, the vinyl fluorosilicone oil is KX-205 vinyl fluorosilicone oil.

Preferably, the nitrile rubber is N41; the grade of the vinyl-terminated liquid nitrile rubber is any one of VTBN1300X3 and VTBN1300X 43.

Preferably, the preparation method of the 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate comprises the following steps: adding 2, 3-dimercaptosuccinic acid and amino-terminated liquid nitrile rubber into chlorobenzene, uniformly mixing, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 4-dimethylaminopyridine into the chlorobenzene, carrying out reflux stirring reaction for 6-8 hours at the temperature of 110-150 ℃ in an inert gas atmosphere, carrying out rotary evaporation to remove a solvent and a by-product after the reaction is finished, precipitating the solvent and the by-product in water, washing the precipitate with ethanol for 3-6 times, and finally carrying out rotary evaporation to remove the ethanol to obtain the 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate.

Preferably, the molar ratio of the 2, 3-dimercaptosuccinic acid to the amino-terminated liquid nitrile rubber to the chlorobenzene to the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the 4-dimethylaminopyridine is 1:1 (6-10) to 0.8-1.2) to 0.5.

Preferably, the inert gas is any one of nitrogen, helium, neon and argon.

Another object of the present invention is to provide a method for preparing the oil-resistant and tear-resistant sealing material, which is characterized by comprising the following steps: according to the weight ratio, the components are put into an internal mixer for mixing for 7-10 minutes, then the mixture is discharged to a cutting machine for discharging, then the mixture is quickly placed in a die and is die-pressed for 9-12 minutes at the temperature of 160-180 ℃ and under the pressure of 8-15MPa, and finally the oil-resistant anti-tearing sealing element material is prepared by irradiating under the ultraviolet light with the wavelength of 280-380nm for 30-40 minutes at room temperature.

Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:

1) the preparation method of the oil-resistant anti-tearing sealing element material provided by the invention is simple in process, convenient to operate and control, high in preparation efficiency and suitable for industrial popularization and application.

2) The oil-resistant and tear-resistant sealing element material provided by the invention overcomes the defects that the existing sealing element material is low in tear strength, poor in sealing effect, insufficient in oil resistance, heat resistance, wear resistance and flame retardance, and the durability needs to be further improved; through the synergistic effect of the components, the prepared oil-resistant anti-tearing sealing element material has good oil-resistant anti-tearing effect, good heat resistance and aging resistance, excellent wear resistance, flame retardance and durability, and sufficient comprehensive performance and performance stability.

3) The oil-resistant anti-tearing sealing element material provided by the invention takes the vinyl-terminated liquid nitrile rubber, the 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate, the nitrile rubber, the vinyl fluorosilicone oil and the trifluoro-chloro-chrysanthemic acid modified amino-terminated liquid nitrile rubber as the rubber base material, and combines the advantages of the nitrile rubber and the fluorosilicone, so that the prepared rubber material has good oil resistance, obvious anti-tearing effect, and good comprehensive performance and performance stability; unsaturated bonds on the vinyl-terminated liquid nitrile rubber, the vinyl fluorosilicone oil and the trifluoro chloro chrysanthemic acid modified amino-terminated liquid nitrile rubber are subjected to click reaction with sulfydryl on 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate in a rubber forming stage to form a three-dimensional network structure, so that the comprehensive performance of the material is effectively improved, the ageing resistance is better, and the mechanical property, the oil resistance and the tear resistance are better; the introduction of sulfur radicals into the molecular chain of the sealing element makes it simultaneously advantageous for polysulfide rubbers.

4) According to the oil-resistant anti-tearing sealing element material provided by the invention, the vinyl-terminated liquid nitrile rubber, the 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate and the trifluoro-chloro-chrysanthemic acid modified amino-terminated liquid nitrile rubber all contain nitrile rubber structures, so that the compatibility is good; the 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate and the trifluoro-chloro-chrysanthemic acid modified amino-terminated liquid nitrile rubber are matched, so that the polycondensate has excellent adhesiveness and compatibility with a nitrile rubber substrate, and a stable structure is formed by matching the polycondensate with the nitrile rubber, so that the tear resistance and the oil resistance of the product are improved. The sulfydryl in the 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate is on a polymer side chain, so that the polycondensate is more easily contacted with other components to generate a crosslinking curing reaction, the sulfydryl which does not participate in the reaction is also linked on a molecular chain, the influence of the traditional unreacted micromolecule substance in the polymer on the comprehensive performance and the performance stability of a polymer material is avoided, in addition, through polycondensation, an amido group is also introduced on the molecular chain, the synergistic effect of other groups is realized, under the multiple effects of an electronic effect, a steric effect and a conjugation effect, the performance stability and the comprehensive performance are better, in addition, the film forming property can be improved through polycondensation, and the oil resistance and the anti-tearing performance are further improved.

5) According to the oil-resistant anti-tearing sealing element material, the trifluoro-cloxacillin modified amino-terminated liquid nitrile rubber is modified by trifluoro-cloxacillin, so that the film forming property is improved, the oil resistance and the anti-tearing property are further improved, and the compatibility with vinyl fluorosilicone oil can be enhanced; the nano boron fiber is used as a filler among rubber particles to enhance the bonding strength between each rubber particle and a phase state in the rubber sealing element, so that the tear resistance is improved; the added filler is at least one of ordinary portland cement PO42.5, glass fiber powder, white carbon black and walnut shell powder, and the fillers can improve the mechanical strength of the material and reduce the cost through a dispersion strengthening mechanism.

Detailed Description

In order to make the technical solutions of the present invention better understood and make the above features, objects, and advantages of the present invention more comprehensible, the present invention is further described with reference to the following examples. The examples are intended to illustrate the invention only and are not intended to limit the scope of the invention.

Examples of the inventionThe amino-terminated liquid nitrile rubber is a nitrile rubber containing amino (-NH) at chain end₂) The liquid butyronitrile polymer (ATBN) has the number average molecular weight of 3500 and the amino content of about 17 percent, and is purchased from Shanghai Citylong industry Co., Ltd; the vinyl fluorosilicone oil is KX-205 vinyl fluorosilicone oil; the grade of the nitrile rubber is N41; other raw materials were all purchased commercially.

Example 1

The oil-resistant and tear-resistant sealing element material is characterized by being prepared from the following components in parts by weight: 15 parts of vinyl-terminated liquid nitrile rubber, 10 parts of 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate, 40 parts of nitrile rubber, 5 parts of vinyl fluorosilicone oil, 4 parts of trifluoro-chloro-chrysanthemic acid modified amino-terminated liquid nitrile rubber, 2 parts of coupling agent, 3 parts of nano boron fiber, 20 parts of filler and 1 part of photoinitiator.

The photoinitiator is 2-hydroxy-2-methyl-1-phenyl acetone; the filler is ordinary portland cement PO 42.5; the particle size of the filler is 400 meshes; the diameter of the nano boron fiber is 300nm, and the length-diameter ratio is 12: 1; the coupling agent is a silane coupling agent KH 550.

The preparation method of the amino-terminated liquid nitrile rubber modified by the trichloro-chrysanthemic acid comprises the following steps: adding the trifluoro-chloro-chrysanthemic acid and the amino-terminated liquid nitrile rubber into an organic solvent, stirring and reacting for 6 hours at the temperature of 30 ℃, and after the reaction is finished, removing the solvent by rotary evaporation to obtain the trifluoro-chloro-chrysanthemic acid modified amino-terminated liquid nitrile rubber; the mass ratio of the trifluoro chrysanthemic acid to the amino-terminated liquid nitrile rubber to the organic solvent is 0.1:3: 15; the organic solvent is ethyl acetate.

The grade of the vinyl-terminated liquid nitrile rubber is VTBN1300X 3.

The preparation method of the 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate comprises the following steps of: adding 2, 3-dimercaptosuccinic acid and amino-terminated liquid nitrile rubber into chlorobenzene, uniformly mixing, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 4-dimethylaminopyridine into the chlorobenzene, carrying out reflux stirring reaction for 6 hours at 110 ℃ in an inert gas atmosphere, carrying out rotary evaporation to remove a solvent and a byproduct after the reaction is finished, precipitating the product in water, washing the precipitated product with ethanol for 3 times, and finally carrying out rotary evaporation to remove the ethanol to obtain the 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate.

The molar ratio of the 2, 3-dimercaptosuccinic acid to the amino-terminated liquid nitrile rubber to the chlorobenzene to the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the 4-dimethylaminopyridine is 1:1:6:0.8: 0.5; the inert gas is nitrogen.

The preparation method of the oil-resistant and tear-resistant sealing element material is characterized by comprising the following steps of: according to the weight ratio, the components are put into an internal mixer to be mixed for 7 minutes, then the mixture is discharged to a cutting machine to be discharged, then the mixture is quickly placed into a die to be molded for 9 minutes at the temperature of 160 ℃ and under the pressure of 8MPa, and finally the oil-resistant anti-tearing sealing element material is prepared by illumination for 30 minutes under the ultraviolet light with the wavelength of 280nm at room temperature.

Example 2

The oil-resistant and tear-resistant sealing element material is characterized by being prepared from the following components in parts by weight: 17 parts of vinyl-terminated liquid nitrile rubber, 12 parts of 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate, 45 parts of nitrile rubber, 6 parts of vinyl fluorosilicone oil, 5 parts of trifluoro-chloro-chrysanthemic acid modified amino-terminated liquid nitrile rubber, 2.3 parts of coupling agent, 4 parts of nano boron fiber, 22 parts of filler and 1.5 parts of photoinitiator.

The photoinitiator is benzoin ethyl ether; the filler is glass fiber powder; the particle size of the filler is 500 meshes; the diameter of the nano boron fiber is 350nm, and the length-diameter ratio is 13: 1; the coupling agent is a silane coupling agent KH 560.

The preparation method of the amino-terminated liquid nitrile rubber modified by the trichloro-chrysanthemic acid comprises the following steps: adding the trifluoro-chloro-chrysanthemic acid and the amino-terminated liquid nitrile rubber into an organic solvent, stirring and reacting for 6.5 hours at 32 ℃, and after the reaction is finished, removing the solvent by rotary evaporation to obtain the trifluoro-chloro-chrysanthemic acid modified amino-terminated liquid nitrile rubber; the mass ratio of the trifluoro chrysanthemic acid to the amino-terminated liquid nitrile rubber to the organic solvent is 0.15:3.5: 17; the organic solvent is butyl acetate.

The grade of the vinyl-terminated liquid nitrile rubber is VTBN1300X 43.

The preparation method of the 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate comprises the following steps of: adding 2, 3-dimercaptosuccinic acid and amino-terminated liquid nitrile rubber into chlorobenzene, uniformly mixing, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 4-dimethylaminopyridine into the chlorobenzene, carrying out reflux stirring reaction for 6.5 hours at 120 ℃ in an inert gas atmosphere, carrying out rotary evaporation to remove a solvent and a by-product after the reaction is finished, precipitating the solvent and the by-product in water, washing the precipitate with ethanol for 4 times, and finally carrying out rotary evaporation to remove the ethanol to obtain a 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate; the molar ratio of the 2, 3-dimercaptosuccinic acid to the amino-terminated liquid nitrile rubber to the chlorobenzene to the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the 4-dimethylaminopyridine is 1:1:7:0.9: 0.5; the inert gas is helium.

The preparation method of the oil-resistant and tear-resistant sealing element material is characterized by comprising the following steps of: according to the weight portion ratio, the components are put into an internal mixer to be mixed for 8 minutes, then the mixture is discharged to a cutting machine to be discharged, then the mixture is quickly placed into a die to be molded for 10 minutes at the temperature of 165 ℃ and under the pressure of 9MPa, and finally the oil-resistant anti-tearing sealing element material is prepared by being irradiated under the ultraviolet light with the wavelength of 300nm for 32 minutes at room temperature.

Example 3

The oil-resistant and tear-resistant sealing element material is characterized by being prepared from the following components in parts by weight: 17 parts of vinyl-terminated liquid nitrile rubber, 15 parts of 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate, 50 parts of nitrile rubber, 7.5 parts of vinyl fluorosilicone oil, 6 parts of trifluoro chloro chrysanthemic acid modified amino-terminated liquid nitrile rubber, 2.5 parts of coupling agent, 4.5 parts of nano boron fiber, 25 parts of filler and 2 parts of photoinitiator.

The photoinitiator is benzoin isopropyl ether; the filler is white carbon black; the particle size of the filler is 600 meshes; the diameter of the nano boron fiber is 400nm, and the length-diameter ratio is 14: 1; the coupling agent is a silane coupling agent KH 570.

The preparation method of the amino-terminated liquid nitrile rubber modified by the trichloro-chrysanthemic acid comprises the following steps: adding the trifluoro-chloro-chrysanthemic acid and the amino-terminated liquid nitrile rubber into an organic solvent, stirring and reacting for 7 hours at 35 ℃, and after the reaction is finished, removing the solvent by rotary evaporation to obtain the trifluoro-chloro-chrysanthemic acid modified amino-terminated liquid nitrile rubber; the mass ratio of the trifluoro chrysanthemic acid to the amino-terminated liquid nitrile rubber to the organic solvent is 0.2:4: 20; the organic solvent is chlorobenzene.

The grade of the vinyl-terminated liquid nitrile rubber is VTBN1300X 3.

The preparation method of the 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate comprises the following steps of: adding 2, 3-dimercaptosuccinic acid and amino-terminated liquid nitrile rubber into chlorobenzene, uniformly mixing, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 4-dimethylaminopyridine into the chlorobenzene, carrying out reflux stirring reaction for 7 hours at 135 ℃ in an inert gas atmosphere, carrying out rotary evaporation to remove a solvent and a byproduct after the reaction is finished, precipitating the product in water, washing the precipitated product with ethanol for 5 times, and finally carrying out rotary evaporation to remove the ethanol to obtain a 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate; the molar ratio of the 2, 3-dimercaptosuccinic acid to the amino-terminated liquid nitrile rubber to the chlorobenzene to the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the 4-dimethylaminopyridine is 1:1:8:1: 0.5; the inert gas is neon.

The preparation method of the oil-resistant and tear-resistant sealing element material is characterized by comprising the following steps of: according to the weight ratio, the components are put into an internal mixer to be mixed for 8.5 minutes, then the mixture is discharged to a cutting machine to be discharged, then the mixture is quickly placed into a die to be pressed for 10.5 minutes at the temperature of 170 ℃ and under the pressure of 12MPa, and finally the mixture is irradiated for 35 minutes under the ultraviolet light with the wavelength of 320nm at room temperature to prepare the oil-resistant anti-tearing sealing element material.

Example 4

The oil-resistant and tear-resistant sealing element material is characterized by being prepared from the following components in parts by weight: 19 parts of vinyl-terminated liquid nitrile rubber, 18 parts of 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate, 58 parts of nitrile rubber, 9 parts of vinyl fluorosilicone oil, 7.5 parts of trifluoro-chloro-chrysanthemic acid modified amino-terminated liquid nitrile rubber, 2.8 parts of coupling agent, 5.5 parts of nano boron fiber, 28 parts of filler and 2.5 parts of photoinitiator.

The photoinitiator is formed by mixing 2-hydroxy-2-methyl-1-phenyl acetone, benzoin ethyl ether and benzoin isopropyl ether according to the mass ratio of 1:3: 2; the filler is formed by mixing ordinary portland cement PO42.5, glass fiber powder, white carbon black and walnut shell powder according to the mass ratio of 1:3:2: 2; the particle size of the filler is 750 meshes; the diameter of the nano boron fiber is 450nm, and the length-diameter ratio is 15: 1; the coupling agent is formed by mixing a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH570 according to a mass ratio of 1:3: 4.

The preparation method of the amino-terminated liquid nitrile rubber modified by the trichloro-chrysanthemic acid comprises the following steps: adding the trifluoro-chloro-chrysanthemic acid and the amino-terminated liquid nitrile rubber into an organic solvent, stirring and reacting for 7.8 hours at 38 ℃, and after the reaction is finished, removing the solvent by rotary evaporation to obtain the trifluoro-chloro-chrysanthemic acid modified amino-terminated liquid nitrile rubber; the mass ratio of the trifluoro chrysanthemic acid to the amino-terminated liquid nitrile rubber to the organic solvent is 0.25:4.5: 23; the organic solvent is methyl ethyl ketone. The grade of the vinyl-terminated liquid nitrile rubber is VTBN1300X 43.

The preparation method of the 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate comprises the following steps of: adding 2, 3-dimercaptosuccinic acid and amino-terminated liquid nitrile rubber into chlorobenzene, uniformly mixing, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 4-dimethylaminopyridine into the chlorobenzene, carrying out reflux stirring reaction for 7.5 hours at 140 ℃ in an inert gas atmosphere, carrying out rotary evaporation to remove a solvent and a by-product after the reaction is finished, precipitating the solvent and the by-product in water, washing the precipitate with ethanol for 6 times, and finally carrying out rotary evaporation to remove the ethanol to obtain a 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate; the molar ratio of the 2, 3-dimercaptosuccinic acid to the amino-terminated liquid nitrile rubber to the chlorobenzene to the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the 4-dimethylaminopyridine is 1:1:9.5:1.1: 0.5; the inert gas is argon.

The preparation method of the oil-resistant and tear-resistant sealing element material is characterized by comprising the following steps of: according to the weight ratio, the components are put into an internal mixer to be mixed for 9.5 minutes, then the mixture is discharged to a cutting machine to be discharged, then the mixture is quickly placed into a die to be molded for 11 minutes at the temperature of 175 ℃ and under the pressure of 14MPa, and finally the mixture is irradiated for 38 minutes under the ultraviolet light with the wavelength of 360nm at room temperature to prepare the oil-resistant anti-tearing sealing element material.

Example 5

The oil-resistant and tear-resistant sealing element material is characterized by being prepared from the following components in parts by weight: 20 parts of vinyl-terminated liquid nitrile rubber, 20 parts of 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate, 60 parts of nitrile rubber, 10 parts of vinyl fluorosilicone oil, 8 parts of trifluoro-chloro-chrysanthemic acid modified amino-terminated liquid nitrile rubber, 3 parts of coupling agent, 6 parts of nano boron fiber, 30 parts of filler and 3 parts of photoinitiator.

The photoinitiator is 2-hydroxy-2-methyl-1-phenyl acetone; the filling material is walnut shell powder; the particle size of the filler is 800 meshes; the diameter of the nano boron fiber is 500nm, and the length-diameter ratio is 16: 1; the coupling agent is a silane coupling agent KH 560.

The preparation method of the amino-terminated liquid nitrile rubber modified by the trichloro-chrysanthemic acid comprises the following steps: adding the trifluoro-chloro-chrysanthemic acid and the amino-terminated liquid nitrile rubber into an organic solvent, stirring and reacting for 8 hours at 40 ℃, and after the reaction is finished, removing the solvent by rotary evaporation to obtain the trifluoro-chloro-chrysanthemic acid modified amino-terminated liquid nitrile rubber; the mass ratio of the trifluoro chrysanthemic acid to the amino-terminated liquid nitrile rubber to the organic solvent is 0.3:5: 25; the organic solvent is dichloromethane.

The grade of the vinyl-terminated liquid nitrile rubber is VTBN1300X 3.

The preparation method of the 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate comprises the following steps of: adding 2, 3-dimercaptosuccinic acid and amino-terminated liquid nitrile rubber into chlorobenzene, uniformly mixing, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 4-dimethylaminopyridine into the chlorobenzene, carrying out reflux stirring reaction for 8 hours at 150 ℃ in an inert gas atmosphere, carrying out rotary evaporation to remove a solvent and a byproduct after the reaction is finished, precipitating the product in water, washing the precipitated product with ethanol for 6 times, and finally carrying out rotary evaporation to remove the ethanol to obtain the 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate.

The molar ratio of the 2, 3-dimercaptosuccinic acid to the amino-terminated liquid nitrile rubber to the chlorobenzene to the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the 4-dimethylaminopyridine is 1:1:10:1.2: 0.5; the inert gas is nitrogen.

The preparation method of the oil-resistant and tear-resistant sealing element material is characterized by comprising the following steps of: according to the weight portion ratio, the components are put into an internal mixer to be mixed for 10 minutes, then the mixture is discharged to a cutting machine to be discharged, then the mixture is quickly placed into a die to be molded for 12 minutes at the temperature of 180 ℃ and under the pressure of 15MPa, and finally the oil-resistant anti-tearing sealing element material is prepared by illumination for 40 minutes under the ultraviolet light with the wavelength of 380nm at room temperature.

Comparative example 1

This example provides an oil resistant, tear resistant seal material of substantially the same formulation and method of manufacture as in example 1, except that: no vinyl terminated liquid nitrile rubber was added.

Comparative example 2

This example provides an oil resistant, tear resistant seal material of substantially the same formulation and method of manufacture as in example 1, except that: 1, 3-propanedithiol is used to replace 2, 3-dimercaptosuccinic acid/amino-terminated liquid nitrile rubber polycondensate.

Comparative example 3

This example provides an oil resistant, tear resistant seal material of substantially the same formulation and method of manufacture as in example 1, except that: no vinyl fluorosilicone oil was added.

Comparative example 4

This example provides an oil resistant, tear resistant seal material of substantially the same formulation and method of manufacture as in example 1, except that: the amino-terminated liquid nitrile rubber is not modified by adding the trifluoro-chloro-chrysanthemic acid.

Comparative example 5

This example provides an oil resistant, tear resistant seal material of substantially the same formulation and method of manufacture as in example 1, except that: amino-terminated liquid nitrile rubber is used for replacing trifluoro-chloro-chrysanthemic acid modified amino-terminated liquid nitrile rubber.

The oil-resistant and tear-resistant sealing material of examples 1 to 5 and comparative examples 1 to 5 above was subjected to performance tests, the test methods and test results are shown in table 1; the heat resistance is characterized by the rate of change of tensile strength after aging at 70 ℃ for 96 hours.

TABLE 1 oil and tear resistant seal Material Performance test results

As can be seen from table 1, the oil-resistant and tear-resistant sealing material disclosed in the examples of the present invention has excellent oil resistance, mechanical properties, and thermal aging resistance, and has better tear resistance and air tightness, which are the result of the synergistic effect of the components.

The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.