CN113527888A - High-tear-resistance white carbon black/methyl vinyl silicone rubber composite material and preparation method thereof - Google Patents
High-tear-resistance white carbon black/methyl vinyl silicone rubber composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-tear-resistance white carbon black/methyl vinyl silicone rubber composite material and a preparation method thereof. The high tear-resistant silicone rubber composite material comprises 100 parts of methyl vinyl silicone rubber and epoxidized silicone rubber, 30-50 parts of white carbon black and 0.05-3 parts of vulcanizing agent, wherein 80-99.9 parts of methyl vinyl silicone rubber and 0.1-20 parts of epoxidized silicone rubber. The epoxy group in the epoxidized silicone rubber can react with the hydroxyl group on the surface of the white carbon black to inhibit the structuring of the white carbon black and improve the dispersibility, and simultaneously the epoxidized silicone rubber can participate in the crosslinking of the methyl vinyl silicone rubber to form a giant rigid crosslinking structure taking the white carbon black as the center, so that the stress is diffused through the crosslinking point of the white carbon black when the material is stressed, the composite material has high tearing strength, the tensile strength of the prepared silicone rubber composite material can reach 10MPa, the elongation at break can reach 600 percent, and the tearing strength can reach 60 kN/m.
Description
Technical Field
The invention relates to the field of polymer nano composite materials, in particular to a high-tear-resistance white carbon black/methyl vinyl silicone rubber composite material and a preparation method thereof.
Background
The silicone rubber molecule has main chain with siloxane bond as repeating unit and two groups connected to silicon atom. Ordinary silica gel is mainly connected with methyl and other groups. The silicon-oxygen bond has certain bond length and bond energy, so that the silicon rubber has small molecular chain interaction, good flexibility and thermal stability and better high and low temperature resistance. The Si-O bond distance was 1.64A, shorter than the sum of the covalent radii (1.76A), suggesting that the Si-O bond is characterized as a partial double bond. In fact, siloxanes are less basic than ethers. However, the barrier to rotation about the Si — O bond axis and the linearization barrier of SiOSi are both very low. Thus, the polysiloxane chain is extremely compliant. The silicone rubber has excellent low temperature resistance, oil resistance, chemical reagent resistance and biocompatibility. Therefore, the material can be applied to various fields, such as aerospace, automobiles and medical materials.
However, the interaction force between the silicon rubber molecular chains is weak, so that the mechanical properties, particularly the tear strength, of the silicon rubber are low. The conventional methods for preparing high tear resistance silicone rubber include two methods: the method C of using different vinyl silicone rubbers together or directly adding vinyl ring bodies and the method for preparing the liquid silicone rubber by adopting MQ resin reinforcement respectively can improve the tearing strength of the silicone rubber composite material to 50 kN/m. However, the silicone rubber with higher tear strength is difficult to achieve by adopting a similar method, but in the fields of electronics, aviation, food and sanitation, a large number of silicone rubber products are small parts with complex structures and are required to have higher tear resistance.
Disclosure of Invention
The invention aims to provide a high-tear-resistance white carbon black/methyl vinyl silicone rubber composite material and a preparation method thereof aiming at the defects of the prior art, so as to obtain the composite material with high tear strength.
One purpose of the invention is to provide a high-tear-resistance white carbon black/methyl vinyl silicone rubber composite material, which is obtained by vulcanizing raw materials comprising the following components in parts by weight:
preferably, the rubber composite comprises:
furthermore, in the 100 parts of methyl vinyl silicone rubber and epoxidized silicone rubber, 92-98 parts of methyl vinyl silicone rubber and 2-8 parts of epoxidized silicone rubber are used.
Wherein, the vinyl mole fraction of the methyl vinyl silicone rubber is preferably 0.03-0.24%, and more preferably 0.13-0.20%.
The vinyl content of the epoxidized silicone rubber is higher than that of the methyl vinyl silicone rubber, and the vinyl mole fraction of the epoxidized silicone rubber is preferably not less than 0.2%, and more preferably 0.25-0.60%.
The epoxy group mole fraction of the epoxidized silicone rubber is preferably 2.5-40%, and more preferably 5-20%.
The white carbon black is preferably gas-phase white carbon black and/or precipitation white carbon black.
The vulcanizing agent may be selected from those generally used in the art, and is preferably at least one selected from 2, 5-dimethyl-2, 5-di (t-butylperoxy) hexane (di-penta), benzoyl peroxide, and dicumyl peroxide.
The tearing reinforcement mechanism of the invention is as follows: epoxy groups in the epoxidized silicone rubber can react with hydroxyl groups on the surface of the white carbon black, so that the structuring of the white carbon black is inhibited, the dispersibility is improved, and the early damage of the white carbon black caused by stress concentration due to large aggregates generated by uneven dispersion is avoided; more importantly, the epoxidized silicone rubber can generate strong interface interaction with the white carbon black and can participate in the crosslinking of the methyl vinyl silicone rubber, so that a giant rigid crosslinking structure taking the white carbon black as the center is formed. As shown in fig. 1, the epoxy group on the epoxidized silicone rubber and the surface of the white carbon black form covalent bond interaction and hydrogen bond interaction, and are multipoint interaction. When the composite material is subjected to external stress, namely one interface action point is damaged due to stress concentration, and other action points still keep strong interaction with the white carbon black, so that the stress transmission between macromolecules and nano particles is ensured, the nano reinforcing efficiency of the white carbon black can be exerted, the stress is dispersed, a silicone rubber molecular chain is oriented along the stretching direction around the rigid giant cross-linking point of the white carbon black under a large strain state, the strong barrier effect on the growth of tearing cracks in the vertical and stretching directions is achieved, crack propagation paths are deflected, more tearing energy is consumed, and the composite material has ultrahigh tearing strength.
The second purpose of the invention is to provide a preparation method of the high-tear-resistance white carbon black/methyl vinyl silicone rubber composite material, which comprises the following steps: and mixing and vulcanizing the components to obtain the rubber composite material.
Preferably, the preparation method comprises the steps of mixing the methyl vinyl silicone rubber, the vulcanizing agent and the white carbon black, then adding the epoxidized silicone rubber for mixing, standing at room temperature for 12-30 h, then back-mixing and vulcanizing;
wherein the mixing time is 20-50 min; the vulcanization temperature is 135-180 ℃, and the vulcanization time is 5-10 min.
In the preparation process of the invention, the processes of mixing, milling and vulcanizing the raw material components can adopt the common rubber processing process in the prior art. The equipment used is also the equipment in the rubber processing in the prior art, such as a high-speed stirring mixer, an internal mixer, an open mill, a vulcanizing machine and the like.
According to a preferred embodiment of the present invention, the preparation method may include:
(1) weighing methyl vinyl silicone rubber, epoxidized silicone rubber, white carbon black and a vulcanizing agent;
(2) the roll temperature of the double-roll open mill is room temperature, after the methyl vinyl silicone rubber is pressed into sheets by the open mill at room temperature, vulcanizing agent and white carbon black are added in batches and mixed uniformly;
(3) adding epoxy silicon rubber, and mixing for 30 min.
(4) Standing at room temperature for 24h, remilling for 20min, and vulcanizing the sample by a flat vulcanizing machine.
The white carbon black/methyl vinyl silicone rubber composite material prepared by the invention has the advantages of tensile strength of 10MPa, elongation at break of 600%, tear strength of 60kN/m and Shore A hardness of 40.
Drawings
FIG. 1 is a schematic diagram of the cross-linked network structure of the epoxidized silicone rubber modified white carbon black/methyl vinyl silicone rubber.
Epoxy groups in the epoxidized silicone rubber (EMVQ) can react with hydroxyl groups on the surface of white carbon black (Silica), and can participate in crosslinking of the methyl vinyl silicone rubber (MVQ), so that a giant rigid crosslinking structure taking the white carbon black as the center is formed, silicone rubber molecular chains surround the rigid giant crosslinking point of the white carbon black in a large strain state and are oriented along the stretching direction, and therefore, a strong barrier effect is achieved on the increase of tearing cracks in the vertical and stretching directions, and the composite material has ultrahigh tearing strength.
Detailed Description
While the present invention will be described in detail with reference to the following examples, it should be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the present invention.
White carbon black by a gas phase method: AEROSIL200 from Germany Degussa;
methyl vinyl silicone rubber: dongjue Silicone Co., Ltd, type 110-2, with a vinyl content of 0.16%;
the epoxidized silicone rubber is self-made, and the preparation method respectively obtains the epoxidized silicone rubber with 10 percent of epoxy content and 0.28 percent of vinyl, the epoxidized silicone rubber with 15 percent of epoxy content and 0.25 percent of vinyl, and the epoxidized silicone rubber with 20 percent of epoxy content and 0.29 percent of vinyl according to the method in Chinese patent 201910003633.0 (a low-cost and environment-friendly method for preparing the epoxidized silicone rubber);
the other raw materials are all obtained in the market.
Example 1
(1) Taking 110-297.5 parts by weight of methyl vinyl silicone rubber, 2.5 parts by weight of epoxidized silicone rubber with the epoxy content of 15%, 40 parts by weight of fumed silica and 0.1 part by weight of vulcanizing agent (bis-di-penta);
(2) the roll temperature of the double-roll open mill is room temperature, the methyl vinyl silicone rubber 110-2 is pressed into sheets by the open mill at room temperature, and then vulcanizing agent and white carbon black are added in batches and mixed uniformly for 30 min;
(3) adding epoxy silicone rubber, and mixing for 30 min;
(4) standing at room temperature for 24h, remilling for 20min, and vulcanizing at 170 ℃ for 10min by a flat vulcanizing machine to obtain the vulcanized silicone rubber composite material.
Example 2
(1): taking 110-297.5 parts by weight of methyl vinyl silicone rubber, 2.5 parts by weight of epoxy silicone rubber with the epoxy content of 20%, 40 parts by weight of fumed silica and 0.1 part by weight of vulcanizing agent (bis-di-penta);
(2) the roll temperature of the double-roll open mill is room temperature, the methyl vinyl silicone rubber 110-2 is pressed into sheets by the open mill at room temperature, and then vulcanizing agent and white carbon black are added in batches and mixed uniformly for 30 min;
(3) adding epoxy silicone rubber, and mixing for 30 min;
(4) standing at room temperature for 24h, remilling for 20min, and vulcanizing at 170 ℃ for 10min by a flat vulcanizing machine to prepare the vulcanized silicone rubber composite material.
Example 3
(1): according to parts by weight, 110 parts of methyl vinyl silicone rubber, 295 parts of epoxidized silicone rubber with the epoxy content of 10 percent, 40 parts of fumed silica and 0.1 part of vulcanizing agent (bis-penta);
(2) the roll temperature of the double-roll open mill is room temperature, the methyl vinyl silicone rubber 110-2 is pressed into sheets by the open mill at room temperature, and then vulcanizing agent and white carbon black are added in batches and mixed uniformly for 30 min;
(3) adding epoxy silicon rubber, and mixing for 30 min.
(4) Standing at room temperature for 24h, remilling for 20min, and vulcanizing at 170 ℃ for 10min by a flat vulcanizing machine to prepare the vulcanized silicone rubber composite material.
Example 4
(1): according to parts by weight, 110 parts of methyl vinyl silicone rubber, 295 parts of epoxidized silicone rubber with the epoxy content of 20 percent, 40 parts of fumed silica and 0.1 part of vulcanizing agent (bis-penta);
(2) the roll temperature of the double-roll open mill is room temperature, the methyl vinyl silicone rubber 110-2 is pressed into sheets by the open mill at room temperature, and then vulcanizing agent and white carbon black are added in batches and mixed uniformly for 30 min;
(3) adding epoxy silicon rubber, and mixing for 30 min.
(4) Standing at room temperature for 24h, remilling for 20min, and vulcanizing at 170 ℃ for 10min by a flat vulcanizing machine to prepare the vulcanized silicone rubber composite material.
Comparative example 1
(1): taking 4 parts of methyl vinyl silicone rubber with the vinyl mole fraction of 0.3 percent, 96 parts of methyl vinyl rubber with the vinyl mole fraction of 0.06 percent, 40 parts of fumed silica, 2 parts of bis-di-penta serving as a vulcanizing agent and 4 parts of hydroxyl silicone oil serving as a structural control agent;
(2) the roll temperature of a double-roll open mill is room temperature, after methyl vinyl silicone rubber with different vinyl contents is pressed into sheets by the open mill at room temperature, hydroxyl silicone oil, white carbon black and a vulcanizing agent are added in batches and are mixed uniformly for 30 min;
(3) and vulcanizing at 170 ℃ for 10min by a flat vulcanizing machine to prepare the vulcanized silicone rubber composite material.
Comparative example 2
(1): in parts by weight, 2100 parts of methyl vinyl rubber, 40 parts of fumed silica, 0.8 part of bis-penta vulcanizing agent, 5 parts of hydroxy silicone oil serving as a structural control agent and 4 parts of tetramethyl tetravinylcyclotetrasiloxane (V4) serving as a concentrated crosslinking point forming agent are taken;
(2) the roll temperature of a double-roll open mill is room temperature, the methyl vinyl rubber 110-2 is pressed into a sheet by the open mill at room temperature, and then the fumed silica, the hydroxy silicone oil, the tetramethyl tetravinylcyclotetrasiloxane and the vulcanizing agent are added in batches and mixed uniformly for 30 min;
(3) and vulcanizing at 170 ℃ for 10min by a flat vulcanizing machine to prepare the vulcanized silicone rubber composite material.
The silicone rubber composite materials obtained in examples 1-4 and comparative examples 1-2 were subjected to performance tests, and the results are shown in table 1 below.
The stress-strain performance of the silicone rubber composite material is tested according to the national standard GB/T528- -;
testing the tearing strength of the silicone rubber composite material according to GB/T529 and 2008;
the hardness of the composite material is tested according to GB/T531-2008 by a Shore A durometer.
TABLE 1 composite Properties of examples and comparative examples
As can be seen from Table 1, the white carbon black/methyl vinyl silicone rubber composite material prepared by the invention has the maximum tensile strength of 10MPa, the elongation at break of 600%, the tear strength of 60kN/m and the Shore A hardness of 40.
Claims (9)
1. The high-tear-resistance white carbon black/methyl vinyl silicone rubber composite material is characterized by being obtained by vulcanizing raw materials comprising the following components in parts by weight:
100 parts of methyl vinyl silicone rubber and epoxy silicone rubber, wherein 80-99.9 parts of methyl vinyl silicone rubber and 0.1-20 parts of epoxy silicone rubber;
30-50 parts of white carbon black;
0.05-3 parts of a vulcanizing agent.
2. The white carbon black/methyl vinyl silicone rubber composite material according to claim 1, characterized in that the rubber composite material is obtained by vulcanizing raw materials comprising, in parts by weight:
100 parts of methyl vinyl silicone rubber and 100 parts of epoxidized silicone rubber, wherein 90-98 parts of methyl vinyl silicone rubber and 2-10 parts of epoxidized silicone rubber are adopted;
35-45 parts of white carbon black;
0.1-1 part of vulcanizing agent.
3. The white carbon black/methyl vinyl silicone rubber composite material according to claim 1, characterized in that:
the methyl vinyl silicone rubber has a vinyl mole fraction of 0.03 to 0.24%, preferably 0.13 to 0.20%.
4. The white carbon black/methyl vinyl silicone rubber composite material according to claim 1, characterized in that:
the vinyl mole fraction of the epoxidized silicone rubber is more than or equal to 0.2 percent, and preferably 0.25 to 0.60 percent.
5. The white carbon black/methyl vinyl silicone rubber composite material according to claim 1, characterized in that:
the epoxy group mole fraction of the epoxidized silicone rubber is 2.5-40%, preferably 5-20%.
6. The white carbon black/methyl vinyl silicone rubber composite material according to claim 1, characterized in that:
the white carbon black is fumed white carbon black and/or precipitated white carbon black.
7. The white carbon black/methyl vinyl silicone rubber composite material according to claim 1, characterized in that:
the vulcanizing agent is at least one selected from 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane, benzoyl peroxide and dicumyl peroxide.
8. The preparation method of the high tear resistance white carbon black/methyl vinyl silicone rubber composite material according to any one of claims 1 to 7, characterized by comprising the following steps:
and mixing and vulcanizing the components to obtain the rubber composite material.
9. The method for preparing white carbon black/methyl vinyl silicone rubber composite material according to claim 8, characterized by comprising the following steps:
mixing methyl vinyl silicone rubber, a vulcanizing agent and white carbon black, then adding epoxidized silicone rubber for mixing, standing at room temperature for 12-30 h, then back-mixing and vulcanizing;
wherein the mixing time is 20-50 min; the vulcanization temperature is 135-180 ℃, and the vulcanization time is 5-10 min.
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| CN114621593A (en) * | 2022-04-22 | 2022-06-14 | 国网山东省电力公司枣庄供电公司 | High-crosslinking-degree silicone rubber for cold-shrinkable cable accessories and preparation method thereof |
| CN114835901A (en) * | 2022-06-17 | 2022-08-02 | 四川大学 | Epoxy modified vinyl silicone rubber and preparation method and application thereof |
| CN115141489A (en) * | 2022-06-08 | 2022-10-04 | 浙江金凤凰电力科技有限公司 | Hot silicone rubber for insulating protective sleeve |
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