A wearable multi-element fluororubber compound
By using diversified components and specific preparation methods in fluoroelastic mixing glue, the interface interaction between fluoroelastic rubber and alkaline white carbon black is improved, and the problem of insufficient tear strength of existing fluoroelastic mixing glue is solved, achieving higher tear strength and better stress transmission effect.
Patent Information
- Application Number
- CN202411940912.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-26
- Publication Date
- 2025-04-04
AI Technical Summary
In places where existing fluoroelastomer mixing glues need to be frequently deformed, the tear strength is insufficient and cannot meet certain application needs.
Using diverse fluoro-rubber raw rubber, alkaline white carbon black, TAIC crosslinking agent, double 25 vulcanizing agent, processing aid and synthetic wax, through specific preparation methods, including raw rubber plasticizing, blending and extrusion, mixing rubber and tableting steps, the interface interaction between fluoro-rubber and alkaline white carbon black is improved and tear strength is improved.
By improving interface interaction and uniform dispersing of filler structure, the tear strength of fluoroelastomer is significantly improved, and stress can be transmitted and dispersed more effectively, preventing crack propagation, and is suitable for applications requiring high tear strength.
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of fluororubbers, in particular to a wearable multi-component fluororubber compound. Background Art
[0002] Fluororubber straps are becoming more and more popular in the sports and fashion watch market due to their lightness, comfort, heat resistance, corrosion resistance and other characteristics. Especially in high temperature environments, the advantages of fluororubber straps are more obvious because they are not easily corroded by sweat and provide a better wearing experience. Compared with metal straps, fluororubber straps are more breathable and skin-friendly; compared with leather straps, fluororubber straps are suitable for various harsh environments and have become the first choice for sports diving smart wearable watches and equipment.
[0003] CN104558975B discloses a modified fluororubber compound and a preparation method thereof. The invention uses thermal cracking carbon black as a filler for fluororubber. Compared with general furnace carbon black, the particle size of thermal cracking carbon black is relatively large and the dispersibility is better, but the reinforcement performance is low. It can only improve the tear strength of fluororubber to a certain extent and cannot be used in places where frequent deformation is required. Summary of the invention
[0004] The object of the present invention is to provide a wearable multi-component fluororubber compound to solve the problems raised in the above-mentioned background technology.
[0005] To achieve the above object, the present invention provides the following technical solution: a wearable multi-component fluororubber compound, the wearable multi-component fluororubber compound comprising the following components in parts by weight: 100 parts of diversified fluororubber raw rubber, 15-50 parts of basic white carbon black, 3-5 parts of TAIC crosslinking agent, 0.5-3 parts of dipentadienyl vulcanizing agent, 0.5-2.3 parts of processing aid, and 0.4-0.7 parts of synthetic wax;
[0006] The diversified fluororubber raw rubber is one or more of fluororubber 26, fluororubber 246, and GF series fluororubber produced by Chemours, and the synthetic wax is a mixture of OPE wax and EVA wax, and the mass ratio of OPE wax to EVA wax is 1:(1-9);
[0007] The preparation method of the wearable multi-element fluororubber mixing comprises the following steps:
[0008] S1. Raw rubber plasticizing: set the roller temperature of the internal mixer to 95-100°C, the roller speed of the internal mixer to 20-30rpm, and put the multi-element fluororubber into the internal mixer for breaking and kneading for 30-60s;
[0009] S2, co-extrusion: firstly, place OPE wax and EVA wax in a mixing tank and heat them to 60-80°C, mix them by a disperser for 1 hour and gradually heat the mixing tank to 100-110°C to obtain molten synthetic wax, then spread alkaline silica on the liquid surface of the molten synthetic wax, evacuate the mixing tank to 87-98 kPa, mix them by a disperser for 30 minutes, take them out, place them in an extruder for extrusion and granulation to obtain a modified filler;
[0010] S3, mixing rubber material: adding modified filler, TAIC crosslinking agent, dipentadienyl vulcanizing agent vulcanizing agent into an internal mixer in sequence, mixing and kneading for 10 to 15 minutes, discharging the material, and obtaining a mixed rubber material;
[0011] S4, sheeting: firstly, the mixed rubber material is put into an open mixer for refining at 80-90° C. for 5-8 min, then filtered, and finally put into a tablet press for calendering to obtain the wearable multi-element fluororubber mixed rubber.
[0012] Optionally, the silicon dioxide content in the basic white carbon black is 87% to 95%, and the average particle size of the basic white carbon black is 16 to 100 nm.
[0013] Optionally, the acid value of the OPE wax is 16 mgKOH / g, and the mass fraction of vinyl acetate in the EVA wax is 13% to 15%.
[0014] Optionally, the processing aid is one of calcium oxide, light magnesium oxide, zinc oxide, and calcium hydroxide.
[0015] Compared with the prior art, the present invention has the following beneficial effects:
[0016] 1. The present invention significantly improves the interface interaction between basic silica and fluororubber matrix through the bridging effect of synthetic wax. The addition of synthetic wax helps to reduce the surface energy of basic silica particles and improve their compatibility with fluororubber, thereby forming a stronger binding force at the interface. This enhanced interface interaction helps to transfer and disperse stress during the tearing process and prevent the rapid expansion of cracks. In addition, when basic silica is uniformly dispersed in fluororubber, it can serve as a stress concentration point. When subjected to external force, the tear strength of fluororubber is improved through interaction between particles and energy dissipation;
[0017] 2. The present invention ensures uniform dispersion of basic silica in molten synthetic wax through mixing and vacuum treatment in a disperser. This uniformly dispersed filler structure helps to form a uniform reinforcement network in the fluororubber, so that the tear strength remains consistent throughout the material. DETAILED DESCRIPTION
[0018] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0019] Embodiment 1: The present invention provides a wearable multi-element fluororubber compound, the wearable multi-element fluororubber compound comprising the following components in parts by weight: 100 parts of diversified fluororubber raw rubber, 15 parts of basic white carbon black, 3 parts of TAIC crosslinking agent, 0.5 parts of di-pentane vulcanizing agent, 0.5 parts of processing aid, and 0.4 parts of synthetic wax;
[0020] Among them, the diversified fluororubber raw rubber is fluororubber 26, the synthetic wax is a mixture of OPE wax and EVA wax, and the mass ratio of OPE wax to EVA wax is 1:1.
[0021] The preparation method of the wearable multi-element fluororubber compound comprises the following steps:
[0022] S1. Raw rubber plasticizing: set the roller temperature of the internal mixer to 95°C and the roller speed of the internal mixer to 20rpm, and put the multi-element fluororubber into the internal mixer for rubber breaking and kneading for 30s;
[0023] S2, co-extrusion: firstly, place OPE wax and EVA wax in a mixing tank and heat them to 60°C, mix them by a disperser for 1 hour and gradually heat the mixing tank to 100°C to obtain molten synthetic wax, then spread alkaline silica on the liquid surface of the molten synthetic wax, evacuate the mixing tank to 87 kPa, mix them by a disperser for 30 minutes, take them out, place them in an extruder for extrusion and granulation to obtain a modified filler;
[0024] S3, mixing rubber material: adding modified filler, TAIC crosslinking agent, dipentadienyl vulcanizing agent vulcanizing agent into an internal mixer in sequence, mixing and kneading for 10 minutes, discharging the material, and obtaining a mixed rubber material;
[0025] S4, sheeting: firstly, the mixed rubber material is put into an open mixer and refined at 80° C. for 5 minutes, then filtered, and finally put into a tablet press to calender and sheet out, so as to obtain the wearable multi-element fluororubber mixed rubber.
[0026] Embodiment 2: The present invention provides a wearable multi-element fluororubber compound, the wearable multi-element fluororubber compound comprising the following components in parts by weight: 100 parts of diversified fluororubber raw rubber, 30 parts of basic white carbon black, 4 parts of TAIC crosslinking agent, 1 part of dipentadienyl vulcanizing agent, 1 part of processing aid, and 0.5 parts of synthetic wax;
[0027] Among them, the diversified fluororubber raw rubber is fluororubber 246, the synthetic wax is a mixture of OPE wax and EVA wax, and the mass ratio of OPE wax to EVA wax is 1:4.
[0028] The preparation method of the wearable multi-element fluororubber compound comprises the following steps:
[0029] S1. Raw rubber plasticizing: set the roller temperature of the internal mixer to 96°C and the roller speed of the internal mixer to 25 rpm, and put the multi-element fluororubber into the internal mixer for rubber breaking and kneading for 40 seconds;
[0030] S2, co-extrusion: firstly, place OPE wax and EVA wax in a mixing tank and heat them to 65°C, mix them by a disperser for 1h and gradually heat the mixing tank to 105°C to obtain molten synthetic wax, then spread alkaline silica on the liquid surface of the molten synthetic wax, evacuate the mixing tank to 90 kPa, mix them by a disperser for 30min, take them out, place them in an extruder for extrusion and granulation to obtain a modified filler;
[0031] S3, mixing rubber material: adding modified filler, TAIC crosslinking agent, dipentadienyl vulcanizing agent vulcanizing agent into an internal mixer in sequence, mixing and kneading for 12 minutes, discharging the material, and obtaining a mixed rubber material;
[0032] S4, sheeting: firstly, the mixed rubber material is put into an open mixer for refining at 85° C. for 6 minutes, then filtered, and finally put into a tablet press for calendering to obtain the wearable multi-element fluororubber mixed rubber.
[0033] Embodiment 3: The present invention provides a wearable multi-element fluororubber compound, the wearable multi-element fluororubber compound comprising the following components in parts by weight: 100 parts of diversified fluororubber raw rubber, 40 parts of basic silica, 4 parts of TAIC crosslinking agent, 2 parts of dipentadienyl vulcanizing agent, 2 parts of processing aid, and 0.5 parts of synthetic wax;
[0034] Among them, the diversified fluororubber raw rubber is GF-200 fluororubber produced by Chemours, and the synthetic wax is a mixture of OPE wax and EVA wax, and the mass ratio of OPE wax to EVA wax is 1:7.
[0035] The preparation method of the wearable multi-element fluororubber compound comprises the following steps:
[0036] S1. Raw rubber plasticizing: set the roller temperature of the internal mixer to 98°C and the roller speed of the internal mixer to 28rpm, and put the multi-element fluororubber into the internal mixer for rubber breaking and kneading for 50s;
[0037] S2, co-extrusion: firstly, the OPE wax and the EVA wax are placed in a mixing tank and heated to 75°C, mixed by a disperser for 1 hour and the mixing tank is gradually heated to 108°C to obtain molten synthetic wax, and then the alkaline silica is spread on the liquid surface of the molten synthetic wax, the mixing tank is evacuated to 95 kPa, and then mixed by a disperser for 30 minutes, taken out, placed in an extruder for extrusion and granulation to obtain a modified filler;
[0038] S3, mixing rubber material: adding modified filler, TAIC crosslinking agent, dipentadienyl vulcanizing agent vulcanizing agent into an internal mixer in sequence, mixing and kneading for 14 minutes, discharging the material, and obtaining a mixed rubber material;
[0039] S4, sheeting: firstly, the mixed rubber material is put into an open mixer for refining at 88° C. for 7 minutes, then filtered, and finally put into a tablet press for calendering to obtain the wearable multi-element fluororubber mixed rubber.
[0040] Embodiment 4: The present invention provides a wearable multi-element fluororubber compound, the wearable multi-element fluororubber compound comprising the following components in parts by weight: 100 parts of diversified fluororubber raw rubber, 50 parts of basic silica, 5 parts of TAIC crosslinking agent, 3 parts of di-pentane vulcanizing agent, 2.3 parts of processing aid, and 0.7 parts of synthetic wax;
[0041] Among them, the diversified fluororubber raw rubber is GF-300 fluororubber produced by Chemours, and the synthetic wax is a mixture of OPE wax and EVA wax, and the mass ratio of OPE wax to EVA wax is 1:9.
[0042] The preparation method of the wearable multi-element fluororubber compound comprises the following steps:
[0043] S1. Raw rubber plasticizing: set the roller temperature of the internal mixer to 100°C and the roller speed of the internal mixer to 30rpm, and put the multi-element fluororubber into the internal mixer for rubber breaking and kneading for 60s;
[0044] S2, co-extrusion: firstly, place OPE wax and EVA wax in a mixing tank and heat them to 80°C, mix them by a disperser for 1h and gradually heat the mixing tank to 110°C to obtain molten synthetic wax, then spread alkaline silica on the liquid surface of the molten synthetic wax, evacuate the mixing tank to 98 kPa, mix them by a disperser for 30min, take them out, place them in an extruder for extrusion and granulation to obtain a modified filler;
[0045] S3, mixing rubber material: adding modified filler, TAIC crosslinking agent, dipentadienyl vulcanizing agent vulcanizing agent into an internal mixer in sequence, mixing and kneading for 15 minutes, discharging the material, and obtaining a mixed rubber material;
[0046] S4, sheeting: firstly, the mixed rubber material is put into an open mixer for refining at 90° C. for 8 minutes, then filtered, and finally put into a tablet press for calendering to obtain the wearable multi-element fluororubber mixed rubber.
[0047] Examples 1 to 4 can all prepare wearable multi-element fluororubber compound rubbers using the above preparation method. In Examples 1 to 4, the silica content in the basic white carbon black is 90%, and the average particle size of the basic white carbon black is 50 nm. The acid value of the OPE wax is 16 mgKOH / g, and the mass fraction of vinyl acetate in the EVA wax is 15%.
[0048] The molecular chain of OPE wax carries a certain amount of carbonyl and hydroxyl groups, has good affinity with alkaline silica, and has better wettability and dispersibility in polar systems than polyethylene wax, while also having coupling properties. The surface of EVA wax carries polar groups, and has good affinity with alkaline silica. The present invention first heats OPE wax and EVA wax to 60-80°C to reduce the viscosity difference between the two during the mixing process, improve the mixing uniformity, and continue to heat to 100-110°C to achieve a uniform flow state between the two. The present invention evacuates the alkaline silica to reduce the gas content in the pores of the alkaline silica, which helps the molten synthetic wax to enter the pores during the stirring and mixing process, increases the interfacial bonding strength, and enhances the affinity and compatibility of the molten synthetic wax with the alkaline silica. During the mixing and kneading of the multi-fluororubber, the modified filler
[0049] Test Example 1
[0050] Test content: According to the determination method disclosed in "Determination of tear strength of vulcanized rubber or thermoplastic rubber" (GB / T 529-2008), the wearable multi-element fluororubber compound prepared in Examples 1 to 4 is made into a trouser-shaped sample, and the trouser-shaped sample is continuously stretched by a tensile testing machine until the trouser-shaped sample breaks, and the tensile force F when the trouser-shaped sample is torn is recorded in N. According to the formula: T a =F / d, calculate the tear strength T a , in kN / m. Wherein, d is the median thickness of the sample, in millimeters (mm). The tear strength test results of Examples 1 to 4 are recorded in Table 1.
[0051] Table 1 Tear strength test results
[0052] Tension F(N) Median thickness of sample (mm) Tear strength (kN / m) Example 1 0.014 2.5 5.6 Example 2 0.015 2.5 6.0 Example 3 0.016 2.5 6.4 Example 4 0.018 2.5 7.2
[0053] The wearable multi-element fluororubber compound disclosed in the present invention can be applied to watch straps, can be compositely bonded with various materials such as metals, plastics, ceramics, magnets and powder metallurgy, and can withstand tearing damage caused by plugging and unplugging the watch strap holes.
[0054] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.
Claims
1. A wearable multi-element fluororubber compound, characterized in that: The wearable multi-component fluororubber compound rubber comprises the following components in parts by weight: 100 parts of diversified fluororubber raw rubber, 15-50 parts of basic white carbon black, 3-5 parts of TAIC crosslinking agent, 0.5-3 parts of dipentadienyl vulcanizing agent, 0.5-2.3 parts of processing aid, and 0.4-0.7 parts of synthetic wax; The diversified fluororubber raw rubber is one or more of fluororubber 26, fluororubber 246, and GF series fluororubber produced by Chemours, and the synthetic wax is a mixture of OPE wax and EVA wax, and the mass ratio of OPE wax to EVA wax is 1:(1-9); The preparation method of the wearable multi-element fluororubber mixing comprises the following steps: S1. Raw rubber plasticizing: set the roller temperature of the internal mixer to 95-100°C, the roller speed of the internal mixer to 20-30rpm, and put the multi-element fluororubber into the internal mixer for breaking and kneading for 30-60s; S2, co-extrusion: firstly, place OPE wax and EVA wax in a mixing tank and heat them to 60-80°C, mix them by a disperser for 1 hour and gradually heat the mixing tank to 100-110°C to obtain molten synthetic wax, then spread alkaline silica on the liquid surface of the molten synthetic wax, evacuate the mixing tank to 87-98 kPa, mix them by a disperser for 30 minutes, take them out, place them in an extruder for extrusion and granulation to obtain a modified filler; S3, mixing rubber material: adding modified filler, TAIC crosslinking agent, dipentadienyl vulcanizing agent vulcanizing agent into an internal mixer in sequence, mixing and kneading for 10 to 15 minutes, discharging the material, and obtaining a mixed rubber material; S4, sheeting: firstly, the mixed rubber material is put into an open mixer for refining at 80-90° C. for 5-8 min, then filtered, and finally put into a tablet press for calendering to obtain the wearable multi-element fluororubber mixed rubber.
2. A wearable multi-element fluororubber compound according to claim 1, characterized in that: The silicon dioxide content in the basic white carbon black is 87% to 95%, and the average particle size of the basic white carbon black is 16 to 100 nm.
3. A wearable multi-element fluororubber compound according to claim 1, characterized in that: The acid value of the OPE wax is 16 mgKOH / g, and the mass fraction of vinyl acetate in the EVA wax is 13% to 15%.
4. A wearable multi-element fluororubber compound according to claim 1, characterized in that: The processing aid is one of calcium oxide, light magnesium oxide, zinc oxide and calcium hydroxide.
Citation Information
Patent Citations
A kind of modified fluorine rubber compound and preparation method thereof
CN104558975B