A fluororubber composition with low compression set, its preparation method and application

Abstract

This invention provides a fluororubber composition with low compression set, its preparation method, and its applications, belonging to the field of chemical materials processing. This invention adds ethylene fluorosilicone oil to fluororubber, effectively reducing the compression set while maintaining mechanical properties, thus improving its reliability and durability under high-temperature environments and showing promising application prospects.

Description

Technical Field

[0001] This invention belongs to the field of chemical materials processing, specifically relating to a fluororubber with low compression set, its preparation method, and its applications. Background Technology

[0002] Sealing components are essential basic parts in industries such as defense, chemical, machinery, and new energy, and have a crucial impact on the safety performance of equipment during use. Fluororubber (FKM) possesses a series of excellent properties, including oil resistance, high temperature resistance, solvent resistance, strong acid resistance, strong oxidant resistance, flame retardancy, and aging resistance, and has found wide application in cutting-edge technology fields such as defense, aerospace, electronics and communications, vehicles and ships, and petrochemicals. Rubber used in sealing components often needs to have a low compression set. Summary of the Invention

[0003] The purpose of this invention is to provide a fluororubber composition with low compression set, its preparation method, and its application.

[0004] The present invention provides a rubber composition prepared from the following raw materials in parts by weight: 100 parts of fluororubber, 5-60 parts of filler, 0.1-10 parts of crosslinking agent, 0.1-10 parts of vulcanizing agent, 0.01-2 parts of release agent, and 0.1-15 parts of ethylene fluorosilicone oil.

[0005] Ethylene fluorosilicone oil refers to fluorosilicone oil containing vinyl groups.

[0006] Furthermore, it is prepared from the following raw materials in parts by weight: 100 parts fluororubber, 15-45 parts filler, 2-6 parts crosslinking agent, 1-5 parts vulcanizing agent, 0.3-0.8 parts release agent, and 0.5-5 parts ethylene fluorosilicone oil;

[0007] Preferably, the composition includes 100 parts fluororubber, 30 parts filler, 4 parts crosslinking agent, 3 parts vulcanizing agent, 0.5 parts release agent, and 1-3 parts ethylene fluorosilicone oil.

[0008] Furthermore, the fluororubber is peroxyfluororubber, the filler is one or a mixture of metal silicates and carbon materials, the crosslinking agent is an olefin crosslinking agent, and the vulcanizing agent is a peroxy vulcanizing agent;

[0009] The release agent is an ester-based release agent;

[0010] The ethylene fluorosilicone oil is a copolymer of vinyl-containing fluorosiloxanes and siloxanes.

[0011] Furthermore, the filler is sodium aluminosilicate;

[0012] The carbon material is carbon black;

[0013] The crosslinking agent is triallyl isocyanurate;

[0014] The vulcanizing agent is 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane;

[0015] The release agent is HT290;

[0016] The ethylene fluorosilicone oil is a vinyl-terminated fluorosilicone oil.

[0017] Furthermore, the vinyl content in the ethylene fluorosilicone oil is 1%-8%.

[0018] Furthermore, the vinyl content in the ethylene fluorosilicone oil is 1%-3%.

[0019] The present invention also provides a method for preparing the above-mentioned rubber composition, the method comprising the following steps: mixing fluororubber, filler, crosslinking agent, vulcanizing agent, release agent and ethylene fluorosilicone oil evenly to form a compound, rolling, thinning, sheeting, and vulcanizing to obtain the rubber composition.

[0020] Furthermore, the vulcanization conditions are: pressure 10-20 MPa, temperature 170-190°C, and time 1-10 min.

[0021] Furthermore, the vulcanization conditions are: pressure 16 MPa, temperature 180 °C, and time 5 min.

[0022] The present invention also provides the application of the above-described rubber composition in the preparation of sealing materials, wherein the sealing material is preferably a high-temperature resistant sealing material.

[0023] Experimental results show that the addition of ethylene fluorosilicone oil to fluororubber in this invention effectively reduces the compression set of fluororubber while maintaining its mechanical properties, and improves its reliability and durability in high-temperature environments, thus showing good application prospects.

[0024] Obviously, based on the above description of the present invention, and according to common technical knowledge and conventional methods in the field, various other modifications, substitutions or alterations can be made without departing from the basic technical concept of the present invention.

[0025] The following detailed embodiments further illustrate the above-described content of the present invention. However, this should not be construed as limiting the scope of the present invention to the following embodiments. All technologies implemented based on the above-described content of the present invention fall within the scope of the present invention. Detailed Implementation

[0026] The raw materials and equipment used in this invention are all known products, obtained by purchasing commercially available products.

[0027] The peroxyfluororubber is the 246 type fluororubber from Shandong Dongyue Shenzhou New Material Co., Ltd.

[0028] HT290 is a German struktol internal release agent specifically for fluororubber peroxide.

[0029] The 1% vinyl end-ethylene fluorosilicone oil was purchased from Shandong Huaxia Shenzhou New Material Co., Ltd., model number DS441.

[0030] The high-ethylene fluorosilicone oil with a vinyl content of 8% was purchased from Shandong Huaxia Shenzhou New Materials Co., Ltd., model number DS442; the ordinary fluorosilicone oil was purchased from Shandong Huaxia Shenzhou New Materials Co., Ltd., model number DS401.

[0031] The "room temperature" referred to in this invention is 25±10℃.

[0032] The methods for preparing fluororubber materials in the embodiments and comparative examples of the present invention are as follows:

[0033] 1) Preparation of compound rubber: First, add the fluoropolymer to the two-roll mill and plasticize it fully at room temperature. Then, add all the remaining materials and mix them evenly. Adjust the roll gap to less than 1 mm to wrap the rolls, thinly pass through the triangular rolls and roll them up. Finally, adjust the roll gap to 2.2 mm to produce the sheet rubber.

[0034] 2) Vulcanization: The compound rubber is placed in a mold and vulcanized for 5 minutes under a pressure of 16 MPa and a temperature of 180°C to obtain fluororubber material.

[0035] In the formulations of the fluororubber materials in the embodiments and comparative examples of this invention, the parts of raw materials are by weight.

[0036] Example 1

[0037] Fluororubber materials were prepared using the following formula: 100 parts of peroxyfluororubber, 20 parts of sodium aluminosilicate filler, 10 parts of carbon black N325, 4 parts of TAIC (trimethylene isocyanurate), 3 parts of bis(2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane), 0.5 parts of HT290, and 1 part of ethylene-terminated fluorosilicone oil with a vinyl content of 1%.

[0038] Example 2

[0039] The amount of ethylene-terminated fluorosilicone oil in the formulation of Example 1 was replaced with 3 parts, and the rest was the same as in Example 1, to prepare fluororubber material.

[0040] Example 3

[0041] The amount of ethylene-terminated fluorosilicone oil in the formulation of Example 1 was replaced with 5 parts, and the rest was the same as in Example 1, to prepare fluororubber material.

[0042] Example 4

[0043] Fluororubber materials were prepared using the following formula: 100 parts of peroxyfluororubber, 20 parts of sodium aluminosilicate filler, 10 parts of carbon black N325, 4 parts of TAIC, 3 parts of bis(2,5)5, ​​0.5 parts of HT290, and 1 part of high-ethylene fluorosilicone oil with a vinyl content of 8%.

[0044] Example 6

[0045] The amount of high-ethylene fluorosilicone oil in the formulation of Example 4 was replaced with 3 parts, and the rest was the same as in Example 4, to prepare fluororubber material.

[0046] Example 6

[0047] The amount of high-ethylene fluorosilicone oil in the formulation of Example 4 was replaced with 5 parts, and the rest was the same as in Example 4, to prepare fluororubber material.

[0048] The following section describes the preparation of comparative samples.

[0049] Comparative Example 1

[0050] Fluororubber materials were prepared using the following formula: 100 parts of peroxyfluororubber, 20 parts of sodium aluminosilicate filler, 10 parts of carbon black N325, 4 parts of TAIC, 3 parts of bis(2,5)5, ​​and 0.5 parts of HT290.

[0051] Comparative Example 2

[0052] Fluororubber materials were prepared using the following formula: 100 parts of peroxyfluororubber, 20 parts of sodium aluminosilicate filler, 10 parts of carbon black N325, 4 parts of TAIC, 3 parts of bis(2,5)5, ​​0.5 parts of HT290, and 10 parts of ethylene-terminated fluorosilicone oil with a vinyl content of 1%.

[0053] Comparative Example 3

[0054] Fluororubber materials were prepared using the following formula: 100 parts of peroxyfluororubber, 20 parts of sodium aluminosilicate filler, 10 parts of carbon black N325, 4 parts of TAIC, 3 parts of bis(2,5)5, ​​0.5 parts of HT290, and 3 parts of ordinary fluorosilicone oil.

[0055] The following experimental examples demonstrate the beneficial effects of the present invention.

[0056] Experimental Example 1

[0057] 1. Experimental Methods

[0058] 1.1 Hardness Test

[0059] According to the national standard GB / T531.1-2008, the hardness of various fluororubber materials was measured using a Shore A hardness tester.

[0060] 1.2 Tensile Strength

[0061] The tensile strength was obtained according to the national standard GB / T 528-2009.

[0062] 1.3 Compression permanent deformation rate

[0063] According to the national standard GB / T 7759.1-2015, the compression set was tested at 200℃×70h and 250℃×70h.

[0064] 2. Experimental Results

[0065] The specific experimental results are shown in Table 1.

[0066] Table 1. Test results of mechanical properties of the samples

[0067]

[0068] Comparative Example 1 shows a fluororubber material without added fluorosilicone oil. In the above experimental results, ordinary fluorosilicone oil, as a small molecule compound, typically acts as a plasticizer when added to fluororubber, reducing its mechanical properties and failing to reduce the compression set, as shown in Comparative Example 3. However, in Examples 1-6, the addition of ethylene fluorosilicone oil significantly reduced the compression set of the fluororubber.

[0069] Comparing Examples 1-6 and Comparative Example 2, it can be seen that within the range of 1-5 parts of ethylene fluorosilicone oil, the compression set of fluororubber can be significantly reduced while maintaining mechanical properties. However, when the amount of ethylene fluorosilicone oil added is increased to 10 parts, the reduction effect on the compression set of fluororubber is not obvious, and mechanical properties such as hardness and tensile strength are significantly reduced. Therefore, it is necessary to control the amount of ethylene fluorosilicone oil used.

[0070] The above experimental results show that by adding a specific amount of ethylene fluorosilicone oil to fluororubber, the present invention significantly reduces the high-temperature compression set rate of fluororubber while maintaining its mechanical properties, thereby improving its reliability and durability in high-temperature environments.

[0071] In summary, this invention provides a fluororubber composition with low compression set, its preparation method, and its applications. By adding ethylene fluorosilicone oil to fluororubber, this invention effectively reduces the compression set of the fluororubber while maintaining its mechanical properties, demonstrating promising application prospects.

Claims

1. A rubber composition, characterized in that, It is prepared from the following raw materials in parts by weight: 100 parts of peroxyfluororubber, 15-45 parts of filler, 2-6 parts of crosslinking agent, 1-5 parts of vulcanizing agent, 0.3-0.8 parts of release agent, and 0.5-5 parts of ethylene fluorosilicone oil; The filler is one or a mixture of metal silicates, carbon materials; The ethylene fluorosilicone oil is a copolymer of vinyl-containing fluorosiloxanes and siloxanes; The vinyl content in the ethylene fluorosilicone oil is 1%-8%.

2. The rubber composition according to claim 1, characterized in that, It is prepared from the following raw materials in parts by weight: 100 parts of peroxyfluororubber, 30 parts of filler, 4 parts of crosslinking agent, 3 parts of vulcanizing agent, 0.5 parts of release agent, and 1-3 parts of ethylene fluorosilicone oil.

3. The rubber composition according to claim 1, characterized in that, The crosslinking agent is an olefin-based crosslinking agent, and the vulcanizing agent is a peroxide-based vulcanizing agent; The release agent is an ester-based release agent.

4. The rubber composition according to claim 1, characterized in that, The metal silicate is sodium aluminosilicate; The carbon material is carbon black; The crosslinking agent is triallyl isocyanurate; The vulcanizing agent is 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane; The release agent is HT290; The ethylene fluorosilicone oil is a vinyl-terminated fluorosilicone oil.

5. The rubber composition according to claim 1, characterized in that, The vinyl content in the ethylene fluorosilicone oil is 1%-3%.

6. A method for preparing the rubber composition according to any one of claims 1-5, characterized in that, The method includes the following steps: mixing fluoropolymer, filler, crosslinking agent, vulcanizing agent, release agent and ethylene fluorosilicone oil evenly to form a compound, rolling, thinning, sheeting, and vulcanizing to obtain a rubber composition.

7. The method according to claim 6, characterized in that, The vulcanization conditions are: pressure 10~20MPa, temperature 170~190℃, and time 1~10min.

8. The method according to claim 7, characterized in that, The vulcanization conditions are: pressure 16 MPa, temperature 180℃, and time 5 min.

9. The use of the rubber composition according to any one of claims 1-5 in the preparation of a sealing material, wherein the sealing material is a high-temperature resistant sealing material.

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