CN114561071A - Low-temperature-resistant nano silicon modified fluororubber composite material and preparation method thereof - Google Patents
Low-temperature-resistant nano silicon modified fluororubber composite material and preparation method thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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Abstract
The invention relates to a low-temperature-resistant nano silicon modified fluororubber composite material and a preparation method thereof, wherein the raw materials comprise the following components in parts by mass: 80-100 parts of fluororubber, 10-40 parts of carbon black, 1.5-5 parts of a vulcanizing agent, 1-4 parts of a vulcanization accelerator, 4-9 parts of an acid acceptor, 1-2.5 parts of a processing aid and 5-20 parts of a silane coupling agent modified nano silicon filler. The composite formula of the invention endows the traditional fluororubber with low temperature resistance, improves the performance of the fluororubber, has good mechanical properties, and enhances the use quality of the fluororubber; the modified fluororubber is obtained by the preparation methods of mixing, remilling and vulcanizing, and the production process is simple, low in cost and easy for industrial production.
Description
Technical Field
The invention belongs to the field of rubber composite materials, and particularly relates to a low-temperature-resistant nano silicon modified fluororubber composite material and a preparation method thereof.
Background
The fluororubber is a synthetic polymer elastomer with fluorine atoms on carbon atoms of a main chain or a side chain, and has good mechanical properties, and excellent high-temperature resistance, acid and alkali resistance, oil resistance, high vacuum resistance and the like. However, since the molecular chain of the fluororubber contains fluorine atoms, the polarity thereof is increased and the low temperature resistance is deteriorated. With the increasing demand of fluororubber, the requirements on the performance of the fluororubber are more and more strict, and particularly under the conditions of using sealing parts in aerospace, vehicle brake sealing, plateau alpine regions and the like, higher requirements on the low-temperature resistance of fluororubber products are provided, the rubber is required to keep the capability of high elasticity at low temperature, and the sealing parts cannot be hardened and shrunk at extreme temperature to cause failure of the sealing parts.
The cold resistance of fluororubber is mainly determined by the glass transition temperature of high polymer, the glass transition temperature is the transition temperature of rubber molecule chain segment from moving to freezing, and the chain segment movement is realized by the rotation in main chain single bond, so the flexibility of molecule chain is the key for determining the cold resistance of rubber. There are two main methods for lowering the glass transition temperature of fluororubbers: firstly, through the main chain modification, change the rubber base and improve its low temperature resistance, but many modify to the chain segment structure of silicon rubber or fluorine silicon rubber among the prior art, and fluororubber has the polarity lateral group again because its main chain is saturated, and rubber molecule regularity and steric hindrance are all great, thereby it is extremely high directly to improve its low temperature resistance's the degree of difficulty through improving fluororubber molecular chain segment structure, and this method development time is long, manufacturing cost is high moreover, popularization and application all receive the restriction. Another modification method is to change the formula of the rubber composite material, for example, to improve the properties of the rubber matrix by blending rubbers, which is relatively easy compared with changing the structure of the chain segment, so that the method is commonly used in the prior art to improve the properties of the fluororubber, but in the method, because the matrix is made of different rubbers, the variable factors are increased, the compatibility between different rubbers and auxiliary materials needs to be considered, and the method is still disadvantageous for simplifying the process and reducing the cost.
Disclosure of Invention
In order to solve the problems, the invention provides a low-temperature-resistant nano silicon modified fluororubber composite material and a preparation method thereof, so that the low-temperature-resistant nano silicon modified fluororubber composite material has excellent low-temperature resistance while maintaining good mechanical properties.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention relates to a low-temperature-resistant nano silicon modified fluororubber composite material which comprises the following raw materials in parts by weight: 80-100 parts of fluororubber, 10-40 parts of carbon black, 1.5-5 parts of a vulcanizing agent, 1-4 parts of a vulcanization accelerator, 4-9 parts of an acid acceptor, 1-2.5 parts of a processing aid and 5-20 parts of a silane coupling agent modified nano silicon filler.
The vulcanizing agent is any one of a bisphenol vulcanizing agent (such as bisphenol AF) or a peroxide vulcanizing agent (such as 2, 5-dimethyl-2, 5-di-tert-butyl peroxy hexane, dicumyl peroxide and the like).
When the vulcanizing agent is a bisphenol vulcanizing agent, the vulcanization accelerator is benzyltriphenylphosphonium chloride (BPP), and when the vulcanizing agent is a peroxide vulcanizing agent, the vulcanization accelerator is triallyl isocyanurate or triallyl cyanurate.
The acid acceptor is one or more of magnesium oxide, calcium hydroxide, zinc oxide and calcium oxide.
The processing aid is mainly a mold release agent and is one or more of WS280, model 935P, subterminal L-24 and carnauba wax.
The silane coupling agent is one or more of epoxy silanes (such as KH560 and the like), vinyl silanes (such as A172 and the like), amino silanes (such as KH540 and the like), sulfur silanes (such as KH590 and the like), acyloxy silanes (such as KH570 and the like).
The size of the nano silicon is 50-100nm, and the structure of the nano silicon is any one of nano particles, nano rods and nano sheets.
The method for obtaining the silane coupling agent modified nano silicon filler comprises the following steps:
s1, adding nano silicon powder into a mixed solution of absolute ethyl alcohol/deionized water in a ratio of 1:1, and performing ultrasonic dispersion for 1-2 hours;
s2, dispersing a silane coupling agent in absolute ethyl alcohol, dropwise adding oxalic acid to enable the pH value of the solution to be 4-4.5, and hydrolyzing for 10-12 hours;
s3, uniformly mixing the solutions obtained in the steps S1 and S2, and stirring in a water bath at the temperature of 75-85 ℃ for 5-7 hours;
s4, carrying out suction filtration on the solution obtained in the step S3, washing, and carrying out vacuum drying for 10-20 h at 80 ℃.
The invention also aims to provide a preparation method of the low-temperature-resistant nano silicon modified fluororubber composite material, which comprises the following steps:
(1) weighing fluororubber according to the raw material ratio, and plasticating the fluororubber for 10-20 times;
(2) weighing an acid-absorbing agent, carbon black, a silane coupling agent modified nano-silicon filler, a processing aid, a vulcanizing agent and a vulcanization accelerator according to the raw material ratio, then mixing with the plasticated fluororubber in the step (1), wherein the mixing temperature is less than or equal to 50 ℃, the mixing time is 40-60 min, and standing for 16-24 h after mixing is finished;
(3) remilling the mixed rubber material treated in the step (2), wherein the remilling temperature is less than or equal to 40 ℃;
(4) vulcanizing the rubber remilled in the step (3), wherein the vulcanization temperature is 170-175 ℃, the pressure is 15-20 tons, and the vulcanization time is 5-8 min;
(5) performing secondary vulcanization on the rubber treated in the step (4), wherein the vulcanization temperature is 230-250 ℃, and the vulcanization time is 10-12 h; naturally cooling to room temperature, and standing for 8-16 h.
The invention has the beneficial effects that: the invention designs a proper fluororubber composite formula, and the fluororubber is crosslinked and vulcanized by selecting a proper vulcanizing agent to form a crosslinked network, wherein after the silane coupling agent is modified, the nano silicon particles have longer Si-O bonds and larger Si-O-Si bond angles, and have low internal rotation resistance and strong flexibility. The surface modification of the nano silicon particles realizes the grafting of organic components, so that the nano particles are in chain connection and are wound with the rubber matrix in a staggered way, the compatibility and the dispersibility of the nano particles with the rubber matrix are improved, and the nano particles can be uniformly distributed in the rubber matrix. The composite formula of the invention endows the fluororubber with low temperature resistance, improves the performance of the fluororubber, enhances the use quality of the fluororubber, and has the advantages of economical and practical preparation method, obvious social benefit and suitability for popularization.
Detailed Description
In order to better understand the present invention, the following examples further illustrate the invention, the examples are only used for explaining the invention, not to constitute any limitation of the invention.
Example 1
The low-temperature-resistant nano silicon modified fluororubber composite material is composed of the following raw materials in parts by mass: 100 parts of fluororubber, 5 parts of carbon black, 3.2 parts of bisphenol AF, 1.8 parts of BPP, 6 parts of magnesium oxide, 3 parts of calcium hydroxide, 2801 parts of WS, 1.5 parts of carnauba wax and 15 parts of KH560 modified nano silicon filler.
The low-temperature-resistant fluororubber is prepared on an open mill according to the formula, and the operation steps are as follows:
(1) weighing fluororubber according to the mass ratio, and plasticating for 20 times by using a mode of thin passing, rolling and triangular wrapping on an open mill;
(2) weighing the raw materials according to the mass part ratio, respectively putting the fluororubber plasticated in the step (1), magnesium oxide, calcium hydroxide, carbon black, KH560 modified nano silicon filler, WS280, carnauba wax, bisphenol AF and BPP into an open mill, uniformly mixing at 50 ℃, packaging in triangular bags for 8, blanking and standing for 16 hours;
(3) putting the mixed rubber material in the step (2) into an open mill again, remilling at the temperature of 40 ℃, thinly passing for 10 times, and rolling and discharging;
(4) putting the rubber remilled in the step (3) into a vulcanization mould, and putting the rubber into a vulcanizing machine for vulcanization treatment, wherein the vulcanization temperature is 170 ℃, the pressurization is 15 tons, and the vulcanization time is 5 min;
(5) performing secondary vulcanization on the rubber in the step (4) in an aging oven, wherein the vulcanization temperature is 230 ℃, and the vulcanization time is 10 hours; naturally cooling to room temperature, and standing for 8 h.
The performance of the fluororubber prepared in example 1 is detected according to a detection method (wherein the Shore A hardness test refers to GB/T531-2008; the tensile test refers to GB/T528-2009; and the low-temperature brittleness test refers to GB/T1682-2014), and the results are as follows:
table 1 example 1 performance parameters
Example 2
The low-temperature-resistant nano silicon modified fluororubber composite material is prepared from the following raw materials in parts by weight: 100 parts of fluororubber, 10 parts of carbon black, 1.5 parts of bis (2, 5-dimethyl-2, 5-di-tert-butylperoxyhexane), 4 parts of TAIC (tri-isopropyl cyanurate), 6 parts of magnesium oxide, 3 parts of calcium hydroxide, 935P1 parts of Model and 20 parts of KH540 modified nano silicon filler.
The low-temperature-resistant fluororubber is prepared on an open mill according to the formula, and the operation steps are as follows:
(1) weighing fluororubber according to the mass ratio, and plasticating for 20 times by using a mode of thin passing, rolling and triangular wrapping on an open mill;
(2) weighing the raw materials according to the mass part ratio, respectively putting the fluororubber plasticated in the step (1), magnesium oxide, calcium hydroxide, carbon black, KH540 modified nano silicon filler, model 935P, bis-2, 5 and TAIC into an open mill, uniformly mixing at the temperature of below 40 ℃, packaging in triangular bags for 6, blanking, and standing for 24 hours;
(3) putting the mixed rubber material in the step (2) into an open mill again, remilling at the temperature of 30 ℃, thinly passing for 15 times, and rolling and discharging;
(4) putting the rubber remilled in the step (3) into a vulcanization mould, and putting the rubber into a vulcanizing machine for vulcanization treatment, wherein the vulcanization temperature is 160 ℃, the pressurization is 20 tons, and the vulcanization time is 8 min;
(5) performing secondary vulcanization on the rubber in the step (4) in an aging oven, wherein the vulcanization temperature is 230 ℃, and the vulcanization time is 12 hours; naturally cooling to room temperature, and standing for 16 h.
The properties of the fluororubber composite prepared in this example are substantially the same as those of example 1, and are not described again.
Example 3
The low-temperature-resistant nano silicon modified fluororubber composite material is prepared from the following raw materials in parts by weight: 100 parts of fluororubber, 5 parts of carbon black, 3.2 parts of bisphenol AF, 1.8 parts of BPP, 6 parts of magnesium oxide, 3 parts of calcium hydroxide, 3 parts of ethylene-propylene-diene copolymer L-241 and 10 parts of KH570 modified nano silicon filler.
The low-temperature-resistant fluororubber is prepared on an open mill according to the formula, and the operation steps are as follows:
(1) weighing fluororubber according to the mass ratio, and plasticating for 15 times by using a mode of thin passing, rolling and triangular wrapping on an open mill;
(2) weighing the raw materials according to the mass part ratio, respectively putting the fluororubber plasticated in the step (1), magnesium oxide, calcium hydroxide, carbon black, KH570 modified nano silicon filler, Sutiao auxiliary L-24, bisphenol AF and BPP into an open mill, mixing for 50min at the temperature of below 30 ℃, packaging in triangular bags for 6, blanking and standing for 20 h;
(3) putting the mixed rubber material in the step (2) into an open mill again, remilling at the temperature of 20 ℃, thinly passing for 12 times, and rolling and discharging;
(4) putting the rubber remilled in the step (3) into a vulcanization mould, and putting the rubber into a vulcanizing machine for vulcanization treatment, wherein the vulcanization temperature is 175 ℃, the pressurization is 20 tons, and the vulcanization time is 6 min;
(5) performing secondary vulcanization on the rubber in the step (4) in an aging oven, wherein the vulcanization temperature is 240 ℃, and the vulcanization time is 10 h; naturally cooling to room temperature, and standing for 20 h.
The performance of the fluororubber composite material prepared in this example is substantially the same as that of example 1, and the detailed description is omitted.
Comparative example 1
Compared with the example 1, the difference is that the modified nano-silicon filler is not added, the other components and the process are not changed, the performance of the prepared fluororubber is detected according to the same method as the example 1, and the result is as follows:
table 2 comparative example 1 performance parameters
It can be seen from tables 1 and 2 that the fluororubber composite material of the present invention has significantly improved properties after the addition of the modified nano-silicon filler, wherein the brittleness temperature is significantly reduced, which indicates that the low temperature resistance is improved, and other mechanical properties are significantly improved compared with the fluororubber without the addition of the modified nano-silicon filler.
The above mentioned matters are not related, and all the matters are applicable to the prior art.
Claims (11)
1. The low-temperature-resistant nano silicon modified fluororubber composite material is characterized by comprising the following raw materials in parts by mass: 80-100 parts of fluororubber, 10-40 parts of carbon black, 1.5-5 parts of a vulcanizing agent, 1-4 parts of a vulcanization accelerator, 4-9 parts of an acid acceptor, 1-2.5 parts of a processing aid and 5-20 parts of a silane coupling agent modified nano silicon filler.
2. The low temperature resistant nano-silicon modified fluororubber composite according to claim 1, characterized in that the vulcanizing agent is any one of a bisphenol vulcanizing agent or a peroxide vulcanizing agent.
3. The low temperature resistant nano-silicon modified fluororubber composite according to claim 2, wherein the bisphenol vulcanizing agent is bisphenol AF, and the peroxide vulcanizing agent is 2,5 dimethyl-2, 5-di-tert-butylperoxyhexane or dicumyl peroxide.
4. The low temperature resistant nano-silicon modified fluororubber composite according to claim 2, wherein if the vulcanizing agent is a bisphenol vulcanizing agent, the vulcanization accelerator is benzyltriphenylphosphonium chloride; if the vulcanizing agent is a peroxide vulcanizing agent, the vulcanization accelerator is any one of triallylisocyanurate or triallylcyanurate.
5. The low temperature resistant nano-silicon modified fluororubber composite according to claim 1, wherein the acid scavenger is one or more of magnesium oxide, calcium hydroxide, zinc oxide, calcium oxide.
6. The low temperature resistant nano silicon modified fluororubber composite according to claim 1, wherein the processing aid is a mold release agent, and the processing aid is one or more of WS280, manicure 935P, yata-co-L-24, and carnauba wax.
7. The low temperature resistant nano-silicon modified fluororubber composite according to claim 1, wherein the silane coupling agent is one or more of epoxy silanes, vinyl silanes, amino silanes, sulfur silanes, and acyloxy silanes.
8. The low temperature resistant nano-silicon modified fluororubber composite according to claim 7, wherein the epoxysilane coupling agent is KH560, the vinylsilane coupling agent is A172, the aminosilane coupling agent KH540, the thiosilane coupling agent is KH590, and the acyloxysilane coupling agent is KH 570.
9. The low-temperature-resistant nano-silicon modified fluororubber composite material according to claim 1, wherein the silane coupling agent modified nano-silicon filler adopts nano-silicon with a size of 50-100nm and has any one of nano-particles, nano-wires and nano-sheets.
10. The low temperature resistant nano-silicon modified fluororubber composite according to claim 1, wherein the silane coupling agent modified nano-silicon filler is obtained by the following method:
s1, adding nano silicon powder into a mixed solution of absolute ethyl alcohol/deionized water with a volume ratio of 1:1, and performing ultrasonic dispersion for 1-2 hours;
s2, dispersing a silane coupling agent in absolute ethyl alcohol, dropwise adding oxalic acid to enable the pH of the solution to be 4-4.5, and hydrolyzing for 10-12 hours;
s3, uniformly mixing the solutions obtained in the steps S1 and S2, and stirring in a water bath at the temperature of 75-85 ℃ for 5-7 hours;
s4, carrying out suction filtration on the solution obtained in the step S3, washing, and carrying out vacuum drying for 10-20 h at 80 ℃.
11. The preparation method of the low-temperature-resistant nano silicon modified fluororubber composite material according to any one of claims 1 to 10, characterized by comprising the following steps:
(1) weighing fluororubber according to the raw material ratio, and plasticating the fluororubber for 10-20 times;
(2) weighing an acid-absorbing agent, carbon black, a silane coupling agent modified nano silicon filler, a processing aid, a vulcanizing agent and a vulcanization accelerator according to the raw material ratio, mixing with the plasticated fluororubber in the step (1), wherein the mixing temperature is less than or equal to 50 ℃, the mixing time is 40-60 min, and standing for 16-24 h after the mixing is finished;
(3) remilling the mixed rubber material treated in the step (2), wherein the remilling temperature is less than or equal to 40 ℃;
(4) vulcanizing the rubber remilled in the step (3), wherein the vulcanization temperature is 170-175 ℃, the pressure is 15-20 tons, and the vulcanization time is 5-8 min;
(5) performing secondary vulcanization on the rubber treated in the step (4), wherein the vulcanization temperature is 230-250 ℃, and the vulcanization time is 10-12 h; naturally cooling to room temperature, and standing for 8-16 h.
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