A fluororubber compound having excellent release properties and mechanical properties simultaneously

Abstract

The application provides a fluororubber mixing rubber with excellent demolding performance and mechanical performance, and belongs to the field of rubber. The fluororubber mixing rubber comprises the following components in parts by weight: 100 parts of a masterbatch, 2-6 parts of a coagulant, 1-4 parts of a vulcanizing agent, 10-40 parts of carbon black and 2-5 parts of a metal oxide; the masterbatch is composed of fluororubber, fluorine oil and hollow glass microbeads. The peroxide fluororubber mixing rubber provided by the application has excellent demolding performance and mechanical performance without adding a demolding agent, and has a wide application prospect. The preparation method of the peroxide fluororubber mixing rubber is simple and suitable for industrial production.

Description

Technical Field

[0001] This invention belongs to the field of rubber, and specifically relates to a fluororubber compound that has both excellent release properties and mechanical properties. Background Technology

[0002] In the rubber industry, fluororubber possesses unparalleled superior properties compared to other rubbers, such as resistance to high temperatures, oil, corrosion from various strong acids and alkalis and chemicals, resistance to ozone and various oxidants, and radiation. Fluororubber is widely used in military and aerospace, petrochemical, machinery manufacturing, construction engineering, instrumentation, and automobile manufacturing. The special properties of fluororubber are determined by its molecular structure containing fluorine atoms; however, this structural characteristic also brings shortcomings, such as difficulty in demolding during processing.

[0003] To address the aforementioned issues, researchers typically add release agents during the processing of fluororubber. For example, patent application CN113943467A discloses a fluororubber composition comprising the following components in parts by weight: 100 parts fluororubber P757; 15-30 parts fluororesin; 10-15 parts silica; 0.8-1.2 parts vulcanizing agent; 2.4-3.6 parts crosslinking agent; and 0.5-1 parts release agent HT290. This application effectively reduces the dynamic friction coefficient by adding release agent HT290 to the total raw materials used in the preparation of the fluororubber composition. When the amounts of release agent, crosslinking agent, and vulcanizing agent increase, the amount of fluororesin can be reduced, thereby decreasing both the dynamic and static friction coefficients to some extent and improving release performance.

[0004] However, on the one hand, long-term exposure to release agents may harm the operator's respiratory system, and if harmful substances come into contact with the skin, they may also cause skin allergies; on the other hand, excessive release agents may lead to a decline in the mechanical properties of fluororubber.

[0005] Therefore, it is of great significance to develop a fluororubber compound that can simultaneously possess excellent release properties and mechanical properties without the addition of a release agent. Summary of the Invention

[0006] The purpose of this invention is to provide a fluororubber compound that has both excellent release properties and mechanical properties.

[0007] This invention provides a fluororubber compound composition comprising the following components in parts by weight: 100 parts masterbatch, 2-6 parts vulcanizing agent, 1-4 parts vulcanizing agent, 10-40 parts carbon black, and 2-5 parts metal oxide; wherein the masterbatch is composed of fluororubber, fluorinated oil, and hollow glass microspheres.

[0008] Furthermore, the fluororubber compound composition comprises the following components in parts by weight: 100 parts masterbatch, 4 parts vulcanizing agent, 1.5 parts vulcanizing agent, 20-30 parts carbon black, and 3 parts metal oxide.

[0009] Furthermore, the fluororubber compound composition comprises the following components in parts by weight: 100 parts masterbatch, 4 parts vulcanizing agent, 1.5 parts vulcanizing agent, 25 parts carbon black, and 3 parts metal oxide.

[0010] Furthermore, in the fluororubber compound composition, the fluororubber is a peroxyfluororubber.

[0011] Furthermore, in the fluororubber compound composition, the co-curing agent is triallyl isocyanurate; the curing agent is 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane.

[0012] Furthermore, in the fluororubber compound composition, the metal oxide is magnesium oxide or zinc oxide.

[0013] Furthermore, in the fluororubber compound, the mass ratio of fluororubber, fluorinated oil and hollow glass microspheres in the masterbatch is (50-100):(1-20):(1-10).

[0014] Furthermore, in the fluororubber compound, the mass ratio of fluororubber, fluorinated oil and hollow glass microspheres in the masterbatch is 100:(2-5):(2-10).

[0015] Furthermore, in the fluororubber compound, the mass ratio of fluororubber, fluorinated oil, and hollow glass microspheres in the masterbatch is 100:2:2, 100:2:5, or 100:2:10.

[0016] Furthermore, the present invention also provides a method for preparing the fluororubber compound composition, which includes the following steps:

[0017] (1) Fluorine oil and hollow glass microspheres are stirred evenly in a beaker according to the proportion, and then mixed with fluororubber in a mixer; then the mixture is passed through a thin filter to obtain masterbatch.

[0018] (2) Plasticize the masterbatch in an internal mixer; add the remaining components and mix; then pass through a thin tube to obtain a fluororubber compound.

[0019] Further, in step (1), the mixing temperature is 90-110℃, the time is 8-12 min, and the number of thin passes is 8-12; preferably, in step (1), the mixing temperature is 100℃, the time is 10 min, and the number of thin passes is 10.

[0020] In step (2), the plasticizing temperature is 50-70℃ and the time is 2-5 min; the mixing temperature is 80-100℃ and the time is 2-5 min; and the number of thin passes is 8-12. Preferably, in step (2), the plasticizing temperature is 60℃ and the time is 3.5 min; the mixing temperature is 90℃ and the time is 3.5 min; and the number of thin passes is 10.

[0021] The present invention also provides the use of the fluororubber compound composition in the preparation of fluororubber products.

[0022] As is well known to those skilled in the art, fluororubber is divided into two main categories based on different vulcanization systems: one is the bisphenol vulcanization system, and the other is the peroxy vulcanization system. Peroxy fluororubber refers to fluororubber using the peroxy vulcanization system.

[0023] The peroxyfluororubber compound provided by this invention has both excellent release properties and mechanical properties without the addition of a release agent, and has broad application prospects.

[0024] The method for preparing peroxyfluorinated rubber compound provided by this invention is simple and suitable for industrial production.

[0025] 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.

[0026] 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 examples. All technologies implemented based on the above-described content of the present invention fall within the scope of the present invention. Attached Figure Description

[0027] Figure 1 The demolding effect of the peroxyfluorinated rubber compound prepared in Comparative Example 1 is shown.

[0028] Figure 2 The demolding effect of the peroxyfluorinated rubber compound prepared in Example 2 of the present invention. Detailed Implementation

[0029] The raw materials and equipment used in this invention are all known products, obtained by purchasing commercially available products.

[0030] FS masterbatch is composed of fluoropolymer peroxide, fluorinated oil, and hollow glass microspheres. The fluoropolymer peroxide refers to fluoropolymer peroxide with a Mooney viscosity of 15-60, grade: DTR-7830L; the fluorinated oil is purchased from Sichuan Hongfu New Materials Co., Ltd., product number F100, with a molecular weight of 1000-15000; the hollow glass microspheres are purchased from Shanghai Kuaisirui, product number D178U, with a particle size of 10-250 micrometers and a wall thickness of 1-2 micrometers.

[0031] TAIC stands for triallyl isocyanurate, which is a vulcanizing agent; bis2.5 stands for 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane, which is also a vulcanizing agent; HT290 is a mold release agent.

[0032] The formulations of the peroxyfluorinated rubber compound in Examples 1-3 are shown in Table 1. The mass ratios of peroxyfluorinated rubber, fluorinated oil, and hollow glass microspheres in the FS masterbatch of Examples 1-3 are shown in Table 2.

[0033] Example 1: Preparation of peroxyfluorinated rubber compound

[0034] The oxyfluorinated rubber compound was prepared according to the formulation of Example 1 in Tables 1 and 2.

[0035] 1. Preparation of FS masterbatch

[0036] 1.1) Put the fluoropolymer into a mixer and masticate it at a temperature of 60°C for 3.5 minutes;

[0037] 1.2) Then pour the pre-stirred fluorinated oil and hollow glass microspheres into the internal mixer and mix for 10 minutes until molten. The mixing temperature is 100℃.

[0038] 1.3) Then, the mixed material is passed through a two-roll mill 10 times to obtain FS masterbatch, which is then set aside.

[0039] 2. Preparation of peroxyfluororubber compound

[0040] The prepared FS masterbatch was plasticized in an internal mixer at 60°C for 2-5 minutes. Then, TAIC, bis 2.5, carbon black, and metal oxides were added to the internal mixer and mixed at 90°C for 3.5 minutes. The mixed fluororubber compound was then passed through a two-roll mill 10 times to obtain the fluororubber compound.

[0041] Example 2: Preparation of peroxyfluorinated rubber compound

[0042] According to the formulation of Example 2 in Tables 1 and 2, and referring to the preparation method of Example 1, the peroxyfluorinated rubber compound was obtained.

[0043] Example 3: Preparation of peroxyfluorinated rubber compound

[0044] According to the formulation of Example 3 in Tables 1 and 2, and referring to the preparation method of Example 1, the peroxyfluorinated rubber compound was obtained.

[0045] Table 1. Formulations of peroxyfluorinated rubber compounds in Examples 1-3

[0046] Example 1 Example 2 Example 3 FS masterbatch (g) 100 100 100 TAIC(g) 4 4 4 Double 2.5g 1.5 1.5 1.5 Carbon black (g) 20 25 30 Metal oxides (g) 3 3 3

[0047] The metal oxides in Table 1 can be magnesium oxide or zinc oxide; zinc oxide is specifically used here.

[0048] Table 2. Mass ratio of peroxyfluororubber, fluorinated oil and hollow glass microspheres in the FS masterbatch of Examples 1-3

[0049] Example 1 Example 2 Example 3 Peroxyfluororubber 100 100 100 Fluorinated oil 2 2 2 Hollow glass microspheres 2 5 10

[0050] Example 4: Preparation of peroxyfluorinated rubber compound

[0051] The oxyfluorinated rubber compound was prepared according to the formulation of Example 1 in Tables 1 and 2.

[0052] 1. Preparation of FS masterbatch

[0053] 1.1) Put the fluoropolymer into a mixer for plasticizing at a temperature of 50-70℃ for 2-5 minutes;

[0054] 1.2) Then pour the pre-stirred fluorinated oil and hollow glass microspheres into the internal mixer and mix for 10 minutes until molten. The mixing temperature is 90-110℃.

[0055] 1.3) Then, the mixed material is passed through a two-roll mill 10 times to obtain FS masterbatch, which is then set aside.

[0056] 2. Preparation of peroxyfluororubber compound

[0057] The prepared FS masterbatch is put into an internal mixer for mastication at a temperature of 50-70℃ for 2-5 minutes. Then, TAIC, bis 2.5, carbon black, and metal oxides are added to the internal mixer for mixing at a temperature of 80-100℃ for 2 minutes. The mixed fluororubber compound is then passed through a two-roll mill 10 times to obtain the fluororubber compound.

[0058] The following is a method for preparing a comparative fluoropolymer compound.

[0059] Comparative Example 1: Preparation of a control fluororubber compound

[0060] Formula: 100g of fluoropolymer, 4g of TAIC, 1.5g of 2.5, 30g of carbon black, 1g of HT290, and 3g of metal oxide, specifically zinc oxide.

[0061] Preparation method: According to the above formula, except that fluorinated oil and hollow glass microspheres are not used, the preparation method of Example 1 is followed to prepare the control peroxyfluorinated rubber compound.

[0062] The following experimental examples demonstrate the beneficial effects of the present invention.

[0063] Experiment Example 1: Mechanical Performance Testing

[0064] 1. Experimental Samples

[0065] The peroxyfluorinated rubber compound prepared in Examples 1-3, and the control peroxyfluorinated rubber compound prepared in Comparative Example 1.

[0066] 2. Experimental Methods

[0067] The Shore A hardness of each fluororubber compound was obtained by referring to the national standard GB / T531.1-2008; the tensile strength, elongation at break and 100% tensile strength of each fluororubber compound were obtained by referring to the national standard GB / T 528-2009.

[0068] 3. Experimental Results

[0069] The test results are shown in Table 3. It can be seen that, compared with the control fluororubber compound prepared in Comparative Example 1, the fluororubber compounds prepared using FS masterbatch in Examples 1-3 of this invention have higher hardness, higher tensile strength, and higher 100% elongation strength. This indicates that the mechanical properties of the fluororubber compounds prepared using FS masterbatch in this invention are significantly improved.

[0070] Table 3. Performance test results of various fluororubber compounds

[0071]

[0072] Experiment Example 2: Demolding Effect Test

[0073] 1. Experimental Methods

[0074] The peroxyfluorinated rubber compound prepared in Example 2 and the control peroxyfluorinated rubber compound prepared in Comparative Example 1 were demolded. The demolding conditions were as follows: the test block was placed in the mold, vulcanized at 180°C for 300s under a pressure of 15mPa, and then manually demolded.

[0075] 2. Experimental Results

[0076] like Figure 1 and Figure 2 As shown, it can be seen that compared with the control fluororubber compound prepared in Comparative Example 1, the fluororubber compound prepared in Example 2 of the present invention is less prone to mold contamination and has a significantly improved demolding effect.

[0077] The above experimental results show that, compared with the control fluororubber compound that used release agent HT290, the fluororubber compound prepared by the present invention using FS masterbatch has significantly improved release performance without the use of release agent. The present invention has achieved unexpected technical effects.

[0078] In summary, this invention provides a fluororubber compound with both excellent release properties and mechanical properties. The peroxyfluororubber compound prepared using FS masterbatch exhibits higher hardness, higher tensile strength, and 100% tensile strength, resulting in significantly improved mechanical properties. Furthermore, the peroxyfluororubber compound prepared using FS masterbatch demonstrates significantly improved release properties without the use of a release agent, achieving unexpected technical benefits.

Claims

1. A fluororubber compound composition, characterized in that: The fluororubber compound composition comprises the following components in parts by weight: 100 parts masterbatch, 4 parts triallyl isocyanurate, 1.5 parts 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane, 20 parts carbon black, and 3 parts zinc oxide; the masterbatch is composed of fluororubber, fluorinated oil, and hollow glass microspheres; the mass ratio of fluororubber, fluorinated oil, and hollow glass microspheres in the masterbatch is 100:2:

2. Alternatively, it comprises the following components in parts by weight: 100 parts masterbatch, 4 parts triallyl isocyanurate, 1.5 parts 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane, 30 parts carbon black, and 3 parts zinc oxide; wherein the masterbatch is composed of fluororubber, fluorinated oil, and hollow glass microspheres; and wherein the mass ratio of fluororubber, fluorinated oil, and hollow glass microspheres in the masterbatch is 100:2:

10. The fluororubber is peroxyfluororubber.

2. The method for preparing the fluororubber compound composition according to claim 1, characterized in that: The preparation method of the fluororubber compound includes the following steps: (1) Fluorine oil and hollow glass microspheres are stirred evenly in a beaker in proportion, and then mixed with fluororubber in an internal mixer; then the mixture is passed through a thin pass to obtain masterbatch. (2) Plasticize the masterbatch in an internal mixer; add the remaining components and mix; then pass through a thin tube to obtain a fluororubber compound.

3. The preparation method according to claim 2, characterized in that: In step (1), the mixing temperature is 90-110℃, the time is 8-12 min, and the number of thin passes is 8-12. In step (2), the plasticizing temperature is 50-70℃ and the time is 2-5 min, the mixing temperature is 80-100℃ and the time is 2-5 min, and the thin pass is 8-12 times.

4. The preparation method according to claim 3, characterized in that: In step (1), the mixing temperature is 100℃, the time is 10 min, and the number of thin passes is 10. In step (2), the plasticizing temperature is 60°C and the time is 3.5 min; the mixing temperature is 90°C and the time is 3.5 min; and the number of thin passes is 10.

5. Use of the fluororubber compound composition of claim 1 in the preparation of fluororubber products.

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