CN112375389A - High-temperature-resistant silicon rubber and preparation method and application thereof - Google Patents
High-temperature-resistant silicon rubber and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of silicone rubber, and discloses high-temperature-resistant silicone rubber as well as a preparation method and application thereof, wherein the high-temperature-resistant silicone rubber mainly comprises polysilazane, a platinum complex, basic silicone rubber, white carbon black, silicone oil and a vulcanizing agent, wherein the inventor finds that when the molecular weight of the polysilazane is 600-9000 and the mass proportion of platinum atoms in the platinum complex in the total formula raw materials of the high-temperature-resistant silicone rubber is 15.01-50ppm, the residual mass of a high-temperature-resistant silicone rubber product at high temperature (800 ℃) can be remarkably improved, and the invention overcomes the defect of poor compatibility of a common heat-resistant additive and the high-temperature-resistant silicone rubber by adding the polysilazane and the platinum complex as the heat-resistant additive, and simultaneously keeps the mechanical properties of the silicone rubber. The preparation method is simple, the raw materials are easy to obtain, and the preparation method has a good application prospect and is suitable for the aerospace field.
Description
Technical Field
The invention belongs to the technical field of silicone rubber, and particularly relates to high-temperature-resistant silicone rubber as well as a preparation method and application thereof.
Background
The silicone rubber is a special rubber which is formed by alternately bonding Si atoms and O atoms to form a molecular main chain skeleton and taking various organic groups as side groups. Because the carbon chain structure of the silicon rubber is different from that of common rubber, the silicon rubber has excellent high temperature resistance, low temperature resistance, weather resistance, electric insulation, mildew resistance, physiological inertia and the like. The common silicon rubber can be used for a long time at the temperature of-50-260 ℃ and keeps elasticity, and the heat-resistant temperature of the phenyl silicon rubber reaches 300-350 ℃. At present, the heat resistance of the silicone rubber is mainly improved by adding inorganic heat-resistant additives or silicone resin and the like. The common inorganic heat-resistant additive is iron oxide, cerium oxide, nickel oxide, cobalt oxide, white carbon black and the like, or the heat-resistant additive is prepared by modifying the metal oxides and mixing the metal oxides in different proportions.
However, with the development of science and technology, especially in the field of aerospace, the heat resistance of the current silicone rubber cannot meet the use requirements of some special fields. And the existing preparation method has the following defects: the metal oxide has larger polarity; the compatibility with silicon rubber is poor, and the dispersion is difficult; the elasticity and mechanical property of the silicon rubber are seriously reduced due to excessive addition; the compatibility of the silicone resin and the silicone rubber is good, but the improvement on the high-temperature resistance of the silicone rubber is limited, and the mechanical properties such as the hardness of the silicone rubber are also adversely affected to a certain extent. Therefore, there is a need for a preparation method capable of effectively improving the thermal stability of silicone rubber to prepare silicone rubber products with at least good high temperature resistance and mechanical properties.
Disclosure of Invention
The invention provides high-temperature-resistant silicon rubber and a preparation method and application thereof, which aim to solve one or more technical problems in the prior art and at least provide a beneficial choice or creation condition.
In order to overcome the technical problems, the technical scheme adopted by the invention is as follows:
a high temperature resistant silicon rubber is mainly prepared from the following raw materials: polysilazane, platinum complex, base silicone rubber, white carbon black, silicone oil and vulcanizing agent; wherein the molecular weight of the polysilazane is 600-9000; the mass ratio of platinum atoms in the platinum complex in the total formula raw materials of the high-temperature resistant silicon rubber is 15.01-50 ppm.
As a further improvement of the above scheme, the structural formula of the polysilazane is as follows: (R)1R2Si-NH)x(R3R4Si-NH)y(R5R6Si-NH)zX, y and z are independently selected from integers of 0-300, and x, y and z are not 0 at the same time; wherein R is1、R2、R3、R4、R5、R6Are each independently represented H, CH3、CmH2m+1、CH＝CH2And (CH)2)mCH＝CH2M is an integer of 1 to 7.
As a further improvement of the above aspect, the platinum complex is selected from at least one of an olefin siloxane complex of chloroplatinic acid, an isopropyl alcohol solution of chloroplatinic acid, a tetramethyldisiloxane complex of chloroplatinic acid, or a tetrahydrofuran solution of chloroplatinic acid.
As a further improvement of the above aspect, the vulcanizing agent is at least one selected from the group consisting of 2, 5-dimethyl-2, 5-di-tert-butylperoxyhexane, dicumyl peroxide and di-tert-butyl peroxide.
As a further improvement of the above aspect, the base silicone rubber includes methyl vinyl silicone rubber; preferably, the molecular weight of the methyl vinyl silicone rubber is 45-65 ten thousand; the mol percentage of the vinyl in the methyl vinyl silicone rubber is 0.04-1.0 mol%.
As a further improvement of the above aspect, the silicone oil includes a hydroxyl silicone oil.
As a further improvement of the scheme, the specific surface area of the white carbon black is 150-380m2/g。
As a further improvement of the scheme, the high-temperature-resistant silicon rubber is mainly prepared from the following raw materials in parts by weight: 100 parts of basic silicon rubber, 20-45 parts of white carbon black, 4-15 parts of silicone oil, 1.0-10 parts of polysilazane, 0.5-3 parts of vulcanizing agent and 0.2-1 part of platinum complex.
The preparation method of the high-temperature-resistant silicon rubber comprises the following steps:
(1) weighing raw materials according to the formula of the high-temperature-resistant silicon rubber, mixing basic silicon rubber, white carbon black and hydroxyl silicone oil, and then carrying out heat treatment, vacuum pumping mixing and cooling to obtain a basic rubber material;
(2) and mixing the basic rubber material with the rest raw materials, vulcanizing and forming, and then performing secondary vulcanization to obtain the high-temperature-resistant silicon rubber.
In the step (1), the mixing temperature is room temperature, and the mixing time is 2-4 h. The temperature of the heat treatment is 150-180 ℃; the duration of the heat treatment is 1-4 h; the time length of the vacuum pumping and mixing is 0.5-2 h. In the step (2), the vulcanizing temperature is 160-180 ℃, and the vulcanizing time is 0.1-0.5 h; the temperature of the second-stage vulcanization is 180-220 ℃, and the time of the second-stage vulcanization is 1-5 hours.
The high-temperature-resistant silicon rubber disclosed by the invention is applied to the field of aerospace.
The invention has the beneficial effects that:
the invention provides high-temperature-resistant silicon rubber and a preparation method and application thereof, and the high-temperature-resistant silicon rubber mainly comprises polysilazane, a platinum complex, basic silicon rubber, white carbon black, silicon oil and a vulcanizing agent, wherein the inventor finds that when the molecular weight of the polysilazane is 600-9000, and the mass proportion of platinum atoms in the platinum complex in the total formula raw materials of the high-temperature-resistant silicon rubber is 15.01-50ppm, the residual mass of a high-temperature-resistant silicon rubber product at high temperature (800 ℃) can be remarkably improved, and the invention overcomes the defect of poor compatibility of a common heat-resistant additive and the high-temperature-resistant silicon rubber by adding the polysilazane and the platinum complex as the heat-resistant additive, and simultaneously keeps the mechanical property of the silicon rubber. The preparation method is simple, the raw materials are easy to obtain, and the preparation method has a good application prospect and is suitable for the aerospace field.
Drawings
FIG. 1 is a photograph showing samples of the high temperature resistant silicone rubber products obtained in example 1 and comparative example 1 after being subjected to a high temperature treatment at 800 ℃.
Detailed Description
The present invention is specifically described below with reference to examples in order to facilitate understanding of the present invention by those skilled in the art. It should be particularly noted that the examples are given solely for the purpose of illustration and are not to be construed as limitations on the scope of the invention, as non-essential improvements and modifications to the invention may occur to those skilled in the art, which fall within the scope of the invention as defined by the appended claims. Meanwhile, the raw materials mentioned below are not specified in detail and are all commercially available products; the process steps or extraction methods not mentioned in detail are all process steps or extraction methods known to the person skilled in the art.
Example 1 preparation of high temperature resistant Silicone rubber
90 parts of methyl vinyl silicone rubber (molecular weight: 56 ten thousand) having a vinyl content of 0.06 mol%, 10 parts of methyl vinyl silicone rubber (molecular weight: 60 ten thousand) having a vinyl content of 1 mol%, and 40 parts of fumed silica (specific surface area: 260 m)2/g), 8 parts of a hydroxy silicone oil (hydroxyl group content 6 wt%) were mixed in a kneader and kneaded at room temperature for 4 hours. And heating to 150 ℃, continuously mixing for 2h, then vacuumizing and mixing for 1h, and cooling to room temperature to obtain the basic rubber material.
6 parts of polysilazane, 0.6 part of olefin siloxane complex of chloroplatinic acid (wherein the mass ratio of platinum atoms in the total formula raw materials of the high-temperature-resistant silicon rubber is 32ppm) and 2 parts of 2, 5-dimethyl-2, 5-di-tert-butyl peroxy hexane are added into the basic rubber on an open mill, and the mixture is uniformly mixed and then is taken out. Vulcanizing at 165 ℃ for 15min, and then vulcanizing at 200 ℃ for 4h for two times to obtain the high temperature resistant silicon rubber.
Wherein, the structural formula of the polysilazane is as follows: (R)1R2Si-NH)1(R3R4Si-NH)6(R5R6Si-NH)1(ii) a Wherein R is1、R3、R4、R5Are all CH3、R2Is H, R6Is CH ═ CH2。
Example 2 preparation of high temperature resistant Silicone rubber
90 parts of methyl vinyl silicone rubber (molecular weight: 50 ten thousand) having a vinyl content of 0.06 mol%, 10 parts of methyl vinyl silicone rubber (molecular weight: 60 ten thousand) having a vinyl content of 1 mol%, and 40 parts of fumed silica (specific surface area: 260 m)2/g), 8 parts of a hydroxy silicone oil (hydroxyl group content 6 wt%) were mixed in a kneader and kneaded at room temperature for 4 hours. And heating to 150 ℃, continuously mixing for 2h, then vacuumizing and mixing for 1h, and cooling to room temperature to obtain the basic rubber material.
Adding 6 parts of polysilazane, 0.6 part of isopropanol solution of chloroplatinic acid (wherein the mass ratio of platinum atoms in the total formula raw materials of the high-temperature-resistant silicon rubber is 32ppm) and 2 parts of 2, 5-dimethyl-2, 5-di-tert-butyl peroxy hexane into the basic rubber on an open mill, uniformly mixing and then obtaining the sheet. Vulcanizing at 165 ℃ for 15min, and then vulcanizing at 200 ℃ for 4h for two times to obtain the high temperature resistant silicon rubber.
Wherein, the structural formula of the polysilazane is as follows: (R)1R2Si-NH)8(R3R4Si-NH)80(R5R6Si-NH)8(ii) a Wherein R is1、R3、R4、R5Are all CH3、R2Is H, R6Is CH ═ CH2。
Example 3 preparation of high temperature resistant Silicone rubber
50 parts of methyl vinyl silicone rubber having a vinyl content of 0.07 mol% (molecular weight: 56 ten thousand) and 50 parts of methyl vinyl silicone rubber having a vinyl content of 0.25 mol% (molecular weight: 60 ten thousand), and 40 parts of fumed silica (specific surface area: 260 m)2(g), 6 parts of a hydroxy silicone oil (hydroxyl group content 6 wt%) were mixed in a kneader and kneaded at room temperature for 4 hours. And heating to 150 ℃, continuously mixing for 2h, then vacuumizing and mixing for 1h, and cooling to room temperature to obtain the basic rubber material.
6 parts of polysilazane, 0.6 part of tetramethyldisiloxane complex of chloroplatinic acid (wherein the mass ratio of platinum atoms in the total formula raw materials of the high-temperature-resistant silicon rubber is 32ppm) and 2 parts of 2, 5-dimethyl-2, 5-di-tert-butyl peroxy hexane are added into the basic rubber on an open mill, and the mixture is uniformly mixed and then is taken out. Vulcanizing at 165 ℃ for 15min, and then vulcanizing at 180 ℃ for 4h for two times to obtain the high temperature resistant silicon rubber.
Wherein, polyThe silazane has the structural formula: (R)1R2Si-NH)4(R3R4Si-NH)40(R5R6Si-NH)4(ii) a Wherein R is1、R3、R4、R5Are all CH3、R2Is H, R6Is CH ═ CH2。
Example 4 preparation of high temperature resistant Silicone rubber
50 parts of methyl vinyl silicone rubber having a vinyl content of 0.07 mol% (molecular weight: 56 ten thousand) and 50 parts of methyl vinyl silicone rubber having a vinyl content of 0.25 mol% (molecular weight: 60 ten thousand), and 40 parts of fumed silica (specific surface area: 260 m)2(g), 6 parts of a hydroxy silicone oil (hydroxyl group content 6 wt%) were mixed in a kneader and kneaded at room temperature for 4 hours. And heating to 150 ℃, continuously mixing for 2h, then vacuumizing and mixing for 1h, and cooling to room temperature to obtain the basic rubber material.
5 parts of polysilazane, 0.6 part of tetrahydrofuran solution of chloroplatinic acid (wherein the mass ratio of platinum atoms in the total formula raw materials of the high-temperature-resistant silicon rubber is 15.01ppm) and 2 parts of 2, 5-dimethyl-2, 5-di-tert-butyl peroxy hexane are added into the basic rubber on an open mill, and the mixture is uniformly mixed and then is taken out. Vulcanizing at 165 ℃ for 15min, and then vulcanizing at 180 ℃ for 4h for two times to obtain the high temperature resistant silicon rubber.
Wherein, the structural formula of the polysilazane is as follows: (R)1R2Si-NH)4(R3R4Si-NH)40(R5R6Si-NH)4(ii) a Wherein R is1、R3、R4、R5Are all CH3、R2Is H, R6Is CH ═ CH2。
Example 5 preparation of high temperature resistant Silicone rubber
80 parts of methyl vinyl silicone rubber having a vinyl content of 0.04 mol% (molecular weight: 56 ten thousand) and 20 parts of methyl vinyl silicone rubber having a vinyl content of 0.3 mol% (molecular weight: 59 ten thousand), and 40 parts of fumed silica (specific surface area: 260 m)2(g), 5 parts of a hydroxy silicone oil (hydroxyl group content: 6 wt%) were mixed in a kneader and kneaded at room temperature for 4 hours. And heating to 150 ℃, continuously mixing for 2h, then vacuumizing and mixing for 1h, and cooling to room temperature to obtain the basic rubber material.
And (2) adding 10 parts of polysilazane, 0.6 part of olefin siloxane complex of chloroplatinic acid (wherein the mass ratio of platinum atoms in the total formula raw materials of the high-temperature-resistant silicon rubber is 50ppm) and 2 parts of 2, 5-dimethyl-2, 5-di-tert-butyl peroxy hexane into the basic rubber on an open mill, uniformly mixing and then obtaining the sheet. Vulcanizing at 165 ℃ for 15min, and then vulcanizing at 220 ℃ for 4h for two times to obtain the high temperature resistant silicon rubber.
Wherein, the structural formula of the polysilazane is as follows: (R)1R2Si-NH)4(R3R4Si-NH)40(R5R6Si-NH)4(ii) a Wherein R is1、R3、R4、R5Are all CH3、R2Is H, R6Is CH ═ CH2。
Example 6 preparation of high temperature resistant Silicone rubber
80 parts of methyl vinyl silicone rubber having a vinyl content of 0.04 mol% (molecular weight: 56 ten thousand) and 20 parts of methyl vinyl silicone rubber having a vinyl content of 0.3 mol% (molecular weight: 59 ten thousand), and 40 parts of fumed silica (specific surface area: 260 m)2(g), 5 parts of a hydroxy silicone oil (hydroxyl group content: 6 wt%) were mixed in a kneader and kneaded at room temperature for 4 hours. And heating to 150 ℃, continuously mixing for 2h, then vacuumizing and mixing for 1h, and cooling to room temperature to obtain the basic rubber material.
5 parts of polysilazane, 0.6 part of isopropanol solution of chloroplatinic acid (wherein the mass ratio of platinum atoms in the total formula raw materials of the high-temperature-resistant silicon rubber is 32ppm) and 2 parts of 2, 5-dimethyl-2, 5-di-tert-butyl peroxy hexane are added into the basic rubber on an open mill, and the mixture is uniformly mixed and then is taken out. Vulcanizing at 165 ℃ for 15min, and then vulcanizing at 220 ℃ for 4h for two times to obtain the high temperature resistant silicon rubber.
Wherein, the structural formula of the polysilazane is as follows: (R)1R2Si-NH)4(R3R4Si-NH)40(R5R6Si-NH)4(ii) a Wherein R is1、R3、R4、R5Are all CH3、R2Is H, R6Is CH ═ CH2。
Comparative example 1 (polysilazane added in an amount of 0)
90 parts of methyl vinyl silicone rubber (molecular weight: 56 ten thousand) having a vinyl content of 0.05 mol%, 10 parts of methyl vinyl silicone rubber (molecular weight: 60 ten thousand) having a vinyl content of 1 mol%, and 40 parts of fumed silica (specific surface area: 260 m)2(g), 8 parts of a hydroxy silicone oil (hydroxyl group content 6 wt%) were mixed in a kneader and kneaded at room temperature for 4 hours. And then heating to 150 ℃, continuing to mix for 2h, vacuumizing and mixing for 1h, and cooling to room temperature to obtain the basic rubber material.
Adding 0.6 part of tetrahydrofuran solution of chloroplatinic acid (wherein the mass ratio of platinum atoms in the total formula raw materials of the high-temperature-resistant silicon rubber is 32ppm) and 2 parts of 2, 5-dimethyl-2, 5-di-tert-butyl peroxy hexane into the basic rubber on an open mill, uniformly mixing and then discharging the sheet. Vulcanizing at 165 ℃ for 15min, and then vulcanizing at 200 ℃ for 4h for two times to obtain a sample for testing high temperature resistance and mechanical properties.
Comparative example 2 (molecular weight of polysilazane > 9000)
90 parts of methyl vinyl silicone rubber (molecular weight: 56 ten thousand) having a vinyl content of 0.05 mol%, 10 parts of methyl vinyl silicone rubber (molecular weight: 60 ten thousand) having a vinyl content of 1 mol%, and 40 parts of fumed silica (specific surface area: 260 m)2(g), 8 parts of a hydroxy silicone oil (hydroxyl group content 6 wt%) were mixed in a kneader and kneaded at room temperature for 4 hours. And then heating to 150 ℃, continuing to mix for 2h, vacuumizing and mixing for 1h, and cooling to room temperature to obtain the basic rubber material.
5 parts of polysilazane, 0.6 part of olefin siloxane complex of chloroplatinic acid (wherein the mass ratio of platinum atoms in the total formula raw materials of the high-temperature-resistant silicon rubber is 32ppm) and 2 parts of 2, 5-dimethyl-2, 5-di-tert-butyl peroxy hexane are added into the basic rubber on an open mill, and the mixture is uniformly mixed and then the sheet is obtained. Vulcanizing at 165 ℃ for 15min, and then vulcanizing at 200 ℃ for 4h for two times to obtain a sample for testing high temperature resistance and mechanical properties.
Wherein, the structural formula of the polysilazane is as follows: (R)1R2Si-NH)12(R3R4Si-NH)120(R5R6Si-NH)12(ii) a Wherein R is1、R3、R4、R5Is CH3、R2Is H, R6Is CH ═ CH2。
Comparative example 3 (platinum atom added in an amount of 0)
90 parts of methyl vinyl silicone rubber (molecular weight: 56 ten thousand) having a vinyl content of 0.05 mol%, 10 parts of methyl vinyl silicone rubber (molecular weight: 60 ten thousand) having a vinyl content of 1 mol%, and 40 parts of fumed silica (specific surface area: 260 m)2(g), 8 parts of a hydroxy silicone oil (hydroxyl group content 6 wt%) were mixed in a kneader and kneaded at room temperature for 4 hours. And then heating to 150 ℃, continuing to mix for 2h, vacuumizing and mixing for 1h, and cooling to room temperature to obtain the basic rubber material.
And (3) adding 5 parts of polysilazane and 2 parts of 2, 5-dimethyl-2, 5-di-tert-butyl peroxy hexane into the basic rubber on an open mill, uniformly mixing and then obtaining the sheet. Vulcanizing at 165 ℃ for 15min, and then vulcanizing at 200 ℃ for 4h for two times to obtain a sample for testing high temperature resistance and mechanical properties.
Wherein, the structural formula of the polysilazane is as follows: (R)1R2Si-NH)4(R3R4Si-NH)40(R5R6Si-NH)4(ii) a Wherein R is1、R3、R4、R5Are all CH3、R2Is H, R6Is CH ═ CH2。
Comparative example 4 (mass ratio of platinum atom in the total raw Material > 50ppm)
90 parts of methyl vinyl silicone rubber (molecular weight: 56 ten thousand) having a vinyl content of 0.05 mol%, 10 parts of methyl vinyl silicone rubber (molecular weight: 60 ten thousand) having a vinyl content of 1 mol%, and 40 parts of fumed silica (specific surface area: 260 m)2(g), 8 parts of a hydroxy silicone oil (hydroxyl group content 6 wt%) were mixed in a kneader and kneaded at room temperature for 4 hours. And then heating to 150 ℃, continuing to mix for 2h, vacuumizing and mixing for 1h, and cooling to room temperature to obtain the basic rubber material.
5 parts of polysilazane and 0.6 part of olefin siloxane complex of chloroplatinic acid (wherein the mass ratio of platinum atoms in the total formula raw materials of the high-temperature-resistant silicon rubber is 100ppm) and 2 parts of 2, 5-dimethyl-2, 5-di-tert-butyl peroxy hexane are added into the basic rubber on an open mill, and the mixture is uniformly mixed and then is taken out. Vulcanizing at 165 ℃ for 15min, and then vulcanizing at 200 ℃ for 4h for two times to obtain a sample for testing high temperature resistance and mechanical properties.
Wherein, the structural formula of the polysilazane is as follows: (R)1R2Si-NH)4(R3R4Si-NH)40(R5R6Si-NH)4(ii) a Wherein R is1、R3、R4、R5Are all CH3、R2Is H, R6Is CH ═ CH2。
Comparative example 5 (without addition of platinum Complex and polysilazane)
Comparative example 5 differs from comparative example 1 in that 0.6 part of a tetrahydrofuran solution of chloroplatinic acid (in which the mass ratio of platinum atoms in the total formulation raw material of the high temperature resistant silicone rubber is 32ppm) and 2 parts of 2, 5-dimethyl-2, 5-di-tert-butylperoxyhexane were added to the mill instead of 2 parts of 2, 5-dimethyl-2, 5-di-tert-butylperoxyhexane.
Product performance testing
Respectively carrying out performance detection on the high-temperature-resistant silicon rubber products prepared in the examples 1-6 and the comparative examples 1-5, and firstly, measuring the tensile strength and the elongation at break of the high-temperature-resistant silicon rubber according to GB/T528-2009; then, the tearing strength of the high-temperature-resistant silicon rubber is determined according to GB/T529-; determining the Shore A hardness of the high-temperature-resistant silicon rubber according to GB/T531-2008; and testing the thermal stability parameters of the high-temperature-resistant silicon rubber through thermal gravimetric analysis, and treating the high-temperature-resistant silicon rubber in a muffle furnace to obtain the appearance of the high-temperature-resistant silicon rubber after high-temperature treatment.
The results are shown in Table 1 and FIG. 1 (in FIG. 1, a is a sample of the high temperature resistant silicone rubber of example 1 after being treated at a high temperature of 800 ℃ and b is a sample of the high temperature resistant silicone rubber of comparative example 1 after being treated at a high temperature of 800 ℃).
TABLE 1 mechanical and high temperature resistance of high temperature resistant Silicone rubber
As can be seen from Table 1, comparative example 4 has a residual mass of 50 wt% at 700 ℃ under a nitrogen atmosphere, and the thermal stability of the silicone rubber is improved to some extent mainly due to platinum catalyzing the crosslinking of the silicone rubber under a nitrogen atmosphere. Comparative examples 1-3, 5 have a residual mass of only 30-33 wt.% at 700 ℃ under nitrogen, much less than 66-76 wt.% of examples 1-6. In contrast, the residual masses at comparative examples 1 to 5700 ℃ are only 44 to 47 wt.%, which are far from 64 to 73 wt.% of examples 1 to 6, under an air atmosphere. Wherein, the photo of the high temperature resistant silicone rubber of comparative example 1 after being treated at a high temperature of 800 ℃ is shown as b in fig. 1, and it can be seen that the high temperature resistant silicone rubber of comparative example 1 is pyrolyzed and converted to generate a large amount of white silica. The residual quality of the high temperature resistant silicone rubber of example 1 at 700 ℃ is 69-75 wt%, and the photograph after the high temperature treatment at 800 ℃ is shown as a in fig. 1. The high temperature resistant silicone rubber of example 1 retained its original shape after treatment at a high temperature of 800 ℃. The heat-resistant additive used in the invention can obviously improve the high-temperature resistance of the high-temperature-resistant silicon rubber. Meanwhile, the mechanical properties of the high-temperature-resistant silicon rubbers in the examples 1 to 6 are equivalent to those of the high-temperature-resistant silicon rubbers in the comparative examples 1 to 5, which shows that the heat-resistant additive does not damage the mechanical properties of the high-temperature-resistant silicon rubbers. Therefore, the high-temperature-resistant silicon rubber has excellent high-temperature resistance and mechanical property.
It will be obvious to those skilled in the art that many simple derivations or substitutions can be made without inventive effort without departing from the inventive concept. Therefore, simple modifications to the present invention by those skilled in the art according to the present disclosure should be within the scope of the present invention. The above embodiments are preferred embodiments of the present invention, and all similar processes and equivalent variations to those of the present invention should fall within the scope of the present invention.
Claims (10)
1. The high-temperature-resistant silicon rubber is characterized by being mainly prepared from the following raw materials: polysilazane, platinum complex, base silicone rubber, white carbon black, silicone oil and vulcanizing agent; wherein the molecular weight of the polysilazane is 600-9000; the mass ratio of platinum atoms in the platinum complex in the total formula raw materials of the high-temperature resistant silicon rubber is 15.01-50 ppm.
2. According to the claimsThe high-temperature-resistant silicone rubber obtained in claim 1 is characterized in that the polysilazane has a structural formula: (R)1R2Si-NH)x(R3R4Si-NH)y(R5R6Si-NH)zX, y and z are independently selected from integers of 0-300, and x, y and z are not 0 at the same time; wherein R is1、R2、R3、R4、R5、R6Are each independently represented H, CH3、CmH2m+1、CH＝CH2And (CH)2)mCH＝CH2M is an integer of 1 to 7.
3. The high temperature resistant silicone rubber of claim 1, wherein the platinum complex is selected from at least one of an olefin siloxane complex of chloroplatinic acid, an isopropanol solution of chloroplatinic acid, a tetramethyldisiloxane complex of chloroplatinic acid, or a tetrahydrofuran solution of chloroplatinic acid.
4. The high temperature resistant silicone rubber of claim 1, wherein the vulcanizing agent is selected from at least one of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide, dicumyl peroxide, or di-tert-butyl peroxide.
5. The high temperature resistant silicone rubber of claim 1, wherein the base silicone rubber comprises methyl vinyl silicone rubber; preferably, the molecular weight of the methyl vinyl silicone rubber is 45-65 ten thousand; preferably, the mole percentage of vinyl groups in the methyl vinyl silicone rubber is 0.04-1.0 mol%.
6. The high temperature resistant silicone rubber of claim 1, wherein the silicone oil comprises a hydroxyl silicone oil.
7. The high temperature resistant silicone rubber as recited in claim 1, wherein the specific surface area of said silica white is 150-380m2/g。
8. The high-temperature-resistant silicone rubber according to claim 1, wherein the high-temperature-resistant silicone rubber is mainly prepared from the following raw materials in parts by weight: 100 parts of basic silicon rubber, 20-45 parts of white carbon black, 4-15 parts of silicone oil, 1.0-10 parts of polysilazane, 0.5-3 parts of vulcanizing agent and 0.2-1 part of platinum complex.
9. The preparation method of the high temperature resistant silicon rubber according to any one of claims 1 to 8, which comprises the following steps:
(1) weighing raw materials according to the formula of the high-temperature-resistant silicon rubber, mixing basic silicon rubber, white carbon black and silicon oil, and then carrying out heat treatment, vacuumizing, mixing and cooling to obtain a basic rubber material;
(2) mixing the basic rubber material with the rest raw materials, vulcanizing and forming, and then performing secondary vulcanization to obtain the high-temperature-resistant silicon rubber.
10. Use of the high temperature resistant silicone rubber of any one of claims 1-8 in the field of aerospace.
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