CN116218227A - High-temperature-resistant silicone rubber and preparation method thereof - Google Patents
High-temperature-resistant silicone rubber and preparation method thereof Download PDFInfo
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- CN116218227A CN116218227A CN202310273806.7A CN202310273806A CN116218227A CN 116218227 A CN116218227 A CN 116218227A CN 202310273806 A CN202310273806 A CN 202310273806A CN 116218227 A CN116218227 A CN 116218227A
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- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
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Abstract
The invention discloses a high-temperature-resistant silicone rubber and a preparation method thereof, which relate to the field of silicone rubber, and the formula comprises the following components in percentage by weight: 100 parts of silicone rubber compound, 4-9 parts of cross-linking agent, 1-3 parts of vulcanizing agent and 5-30 parts of heat resistant agent (FS). The high-temperature resistant silicone rubber prepared by the invention can be used for a long time at 300 ℃, and after 300 ℃/72h high-temperature ageing, the tensile strength is 4.20MPa, which is beneficial to widening the application field of the silicone rubber, so that the development of the silicone rubber which can be used for a long time at 300 ℃ is a very significant matter.
Description
Technical Field
The invention relates to the field of silicon rubber, in particular to high-temperature-resistant silicon rubber and a preparation method thereof.
Background
Silicone rubber is a special rubber with both inorganic and organic characteristics, has excellent weather resistance, electrical insulation, high and low temperature resistance and the like, and is widely used in the fields of electronics, transportation, medical treatment and the like. The use temperature of the silicone rubber which is common in the market ranges from minus 50 ℃ to 250 ℃, along with the progress of technology, the silicone rubber is expected to have higher temperature resistance, and particularly in special fields, such as aerospace, the silicone rubber is expected to have higher temperature resistance, but the existing silicone rubber cannot meet the requirement, so that the preparation of the silicone rubber with higher temperature resistance is very interesting.
The high temperature resistant modification of silicone rubber has been reported, CN 110330795a, to provide a solution for improving the high temperature resistance of silicone rubber, but this solution has a problem that the preparation of heat resistant agent is difficult. In CN102643553A, CN114836038, it is reported that the high temperature resistance of the silicone rubber is improved by synthesizing a polymer material containing metal elements, the synthesis process is complex, mass production is difficult to realize, and CN104530715A reports that the preparation of the high temperature resistant silicone rubber is that the prepared silicone rubber has a tensile strength of about 1.2MPa after 250 ℃/24 hours, and the strength is too low to be beneficial to the improvement of the application range of the silicone rubber. Therefore, it is necessary to prepare a high temperature resistant silicone rubber which is used for a long time at 300 ℃ and has a simple process and is easy to realize mass production.
Disclosure of Invention
The invention aims to prepare the high-temperature-resistant silicone rubber which can be used for a long time at 300 ℃, and meanwhile, the preparation process is simple and the mass production is easy to realize. The invention provides high-temperature-resistant silicone rubber and a preparation method thereof, and in order to achieve the purposes, the invention adopts the following technical scheme:
the high-temperature-resistant silicone rubber comprises the following raw materials in parts by weight:
100 parts of silicone rubber compound;
4-9 parts of cross-linking agent; for example, the crosslinking agent is 4 parts, 4.5 parts, 5 parts, 5.5 parts, 6 parts, 6.5 parts, 7 parts, 7.5 parts, 8 parts, 8.5 parts, or 9 parts;
1-3 parts of vulcanizing agent; for example, the vulcanizing agent is 1 part, 1.2 parts, 1.4 parts, 1.6 parts, 1.8 parts, 2 parts, 2.2 parts, 2.4 parts, 2.6 parts, 2.8 parts, or 3 parts;
5-30 parts of a heat resistant agent (FS); for example, the heat-resistant agent is 5 parts, 5.5 parts, 6 parts, 6.5 parts, 7 parts, 7.5 parts, 8 parts, 8.5 parts, 9 parts, 9.5 parts, 10 parts, 10.5 parts, 11 parts, 11.5 parts, 12 parts, 12.5 parts, 13 parts, 13.5 parts, 14 parts, 14.5 parts, 15 parts, 15.5 parts, 16 parts, 16.5 parts, 17 parts, 17.5 parts, 18 parts, 18.5 parts, 19 parts, 19.5 parts, 20 parts, 20.5 parts, 21 parts, 21.5 parts, 22 parts, 22.5 parts, 23 parts, 23.5 parts, 24 parts, 24.5 parts, 25 parts, 25.5 parts, 26 parts, 26.5 parts, 27 parts, 27.5 parts, 28 parts, 28.5 parts, 29 parts, 29.5 parts, or 30 parts.
Further, the raw materials of the high-temperature-resistant silicone rubber comprise silicone rubber compound, a cross-linking agent, a vulcanizing agent and a heat-resistant agent; wherein, based on 100 parts by weight of the silicone rubber compound, the cross-linking agent is 4-9 parts by weight, the vulcanizing agent is 1-3 parts by weight, and the heat-resistant agent (FS) is 5-30 parts by weight.
Further, the cross-linking agent is one or three of hydroxyl silicone oil, vinyl silicone oil and hexamethyldisilazane.
Further, the vulcanizing agent is one or two of two-four and two-five.
Further, the heat-resistant agent (FS) inorganic matters containing iron and tin are prepared by mixing ferric chloride and stannic chloride and sequentially carrying out coprecipitation and high temperature sintering.
The high temperature sintering temperature is 300 ℃, 400 ℃, 500 ℃, 600 ℃ or 650 ℃.
The proportion of the ferric chloride to the stannic chloride is 1-3 mol:5 to 7mol. For example, the ratio of ferric chloride to stannic chloride is 1mol:5 to 7mol, 1.2mol:5 to 7mol, 1.5mol:5 to 7mol, 1.7mol:5 to 7mol and 2mol:5 to 7mol, 2.2mol:5 to 7mol, 2.5mol:5 to 7mol, 2.7mol:5 to 7mol and 3mol:5 to 7mol and 1mol:5.2 to 7mol and 1.2mol:5.5 to 7mol and 1.5mol:5.7 to 7mol and 1.7mol:5.9 to 7mol and 2mol:6 to 7mol, 2.2mol:6.2 to 7mol and 2.5mol:6.5 to 7mol, 2.7mol:6.7 to 7mol or 3mol:6.9 to 7mol. For example, the molar ratio of ferric chloride to stannic chloride is 2, 2.5, 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5 or 7, preferably 2, 2.5 or 7.
A process for preparing a rubber as claimed in any one of the preceding claims, comprising the steps of:
(1) Adding tin chloride and ferric chloride into deionized water, stirring until solid particles are completely dissolved, coprecipitating, stirring, centrifuging, washing to remove chloride ions in the solution, drying to obtain a crude product, grinding the obtained crude product, sintering, and cooling to room temperature after sintering to obtain a heat resistant agent;
(2) And (3) uniformly mixing the silicone rubber compound, the cross-linking agent and the heat-resistant agent obtained in the step (1) on a mixing mill, adding the vulcanizing agent, uniformly mixing, vulcanizing, and cooling to room temperature to obtain the high-temperature-resistant silicone rubber.
Specifically, the method for preparing the rubber according to any one of the above comprises the following steps:
(1) Adding tin chloride and ferric chloride into deionized water, stirring until solid particles are completely dissolved, regulating the PH to be 7-9, stirring, centrifuging, washing to remove chloride ions in the solution, drying to obtain a crude product, grinding the obtained crude product, sintering at 300-650 ℃ for 5-6 hours, and cooling to room temperature after sintering to obtain a heat resistant agent;
(2) Uniformly mixing the silicone rubber compound, the cross-linking agent and the heat-resistant agent obtained in the step (1) on a mixing mill, adding the vulcanizing agent, uniformly mixing, vulcanizing at 150-160 ℃ for 0.5-1 hour, and cooling to room temperature to obtain the high-temperature-resistant silicone rubber.
Further, wherein, for example, in step (1), the pH is 7, 8 or 9.
The beneficial effects of the invention are as follows:
1. the high-temperature resistant silicon rubber prepared by the invention can be used for a long time at 300 ℃, has high mechanical strength, and has tensile strength of 4.20MP after 300 ℃/72h high-temperature heat aging.
2. The high-temperature-resistant silicon rubber prepared by the invention has the advantages of simple process, stable quality and easy realization of mass production.
The term "high temperature resistant" in the present invention means a temperature resistance of 300 ℃.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples are intended to be illustrative only and the scope of the invention is to be construed as including the full breadth of the claims and by the recitation of the following examples, the full breadth of the claims can be fully set forth by those skilled in the art.
The partial raw materials and equipment adopted in the invention are as follows:
silicone rubber compound (nankyotong silicone limited, 4452);
hydroxy silicone oils and vinyl silicone oils (pharmaceutical chemicals, inc., industrial grade, martinal);
biwu (michao fine chemical limited, industrial grade);
high temperature sintering furnace (Luoyang family furnace Co., ltd., model KR);
mixing roll (Chang hucho open mixer, SK-160).
Example 1
Adding 5mol of stannic chloride and 2mol of ferric chloride into 2L of deionized water, stirring until solid particles are completely dissolved, regulating the PH to be approximately equal to 8, centrifuging and washing to remove chloride ions in the solution after continuously stirring for 20 minutes, drying at 90 ℃ for 5 hours to obtain a crude product, grinding the obtained crude product on a mortar, and then placing the ground crude product into a high-temperature sintering furnace for sintering, wherein the sintering is as follows: sintering at 300 ℃ for 1 hour, then sintering at 400 ℃ for 1 hour, then sintering at 500 ℃ for 1 hour, then sintering at 600 ℃ for 1 hour, finally sintering at 650 ℃ for 1 hour, and cooling to room temperature after sintering is completed to obtain the heat resistant agent (FS).
100 parts by weight of silicone rubber compound, 1.5 parts by weight of hydroxyl silicone oil, 1.5 parts by weight of vinyl silicone oil, 1.5 parts by weight of hexamethyldisilazane and 10 parts of heat-resistant agent (FS) are uniformly mixed on a mixer, 1.5 parts by weight of biwu-compound is added, uniformly mixed, vulcanized for 1 hour at 160 ℃, and cooled to room temperature to obtain the product.
Example 2
Adding 6mol of stannic chloride and 3mol of ferric chloride into 2L of deionized water, stirring until solid particles are completely dissolved, regulating the PH to be approximately equal to 8, centrifuging and washing to remove chloride ions in the solution after continuously stirring for 30 minutes, drying at 90 ℃ for 5 hours to obtain a crude product, grinding the obtained crude product on a mortar, and then placing the ground crude product into a high-temperature sintering furnace for sintering, wherein the sintering is as follows: sintering at 300 ℃ for 1 hour, then sintering at 400 ℃ for 1 hour, then sintering at 500 ℃ for 1 hour, then sintering at 600 ℃ for 1 hour, finally sintering at 650 ℃ for 1 hour, and cooling to room temperature after sintering is completed to obtain the heat resistant agent (FS).
100 parts by weight of silicone rubber compound, 2 parts by weight of hydroxyl silicone oil, 2 parts by weight of vinyl silicone oil, 2 parts by weight of hexamethyldisilazane and 15 parts of heat resistant agent (FS) are uniformly mixed on a mixer, 1.5 parts by weight of biwu-compound is added, uniformly mixed, vulcanized for 1 hour at 160 ℃, and cooled to room temperature to obtain the product.
Example 3
Adding 7mol of stannic chloride and 1mol of ferric chloride into 2L of deionized water, stirring until solid particles are completely dissolved, regulating the PH to be approximately equal to 8, centrifuging and washing to remove chloride ions in the solution after continuously stirring for 30 minutes, drying at 90 ℃ for 5 hours to obtain a crude product, grinding the obtained crude product on a mortar, and then placing the ground crude product into a high-temperature sintering furnace for sintering, wherein the sintering is as follows: sintering at 300 ℃ for 1 hour, then sintering at 400 ℃ for 1 hour, then sintering at 500 ℃ for 1 hour, then sintering at 600 ℃ for 1 hour, finally sintering at 650 ℃ for 1 hour, and cooling to room temperature after sintering is completed to obtain the heat resistant agent (FS).
100 parts by weight of silicone rubber compound, 2.5 parts by weight of hydroxyl silicone oil, 2.5 parts by weight of vinyl silicone oil, 2.5 parts by weight of hexamethyldisilazane and 20 parts of heat-resistant agent (FS) are uniformly mixed on a mixer, 1 part by weight of biwu-compound is added, uniformly mixed, vulcanized for 1 hour at 160 ℃, and cooled to room temperature to obtain the product.
Comparative example
100 parts by weight of silicone rubber compound is mixed uniformly on a mixer, 1 part by weight of biwu is added, the mixture is vulcanized for 1 hour at 160 ℃, and the mixture is cooled to room temperature to obtain the product.
The products prepared in the examples and comparative examples of the present invention were tested for tensile strength and elongation at break after low temperature and high temperature according to GB/T528-2009 test for tensile stress strain properties of vulcanized rubber or thermoplastic rubber, wherein high temperature samples were prepared according to GB/T3512-2001 test for accelerated hot air aging and heat resistance of vulcanized rubber or thermoplastic rubber, and specifically the samples were prepared as type I dumbbell type, and the samples were placed in an aging oven for 24 and 72 hours at 300 ℃. The experimental data were measured as follows:
remarks: the comparative example was such that the silicone rubber without the heat resistant agent (FS) failed after 300 ℃/24h and 300 ℃/72h after which the rubber failed to give tensile strength and elongation at break.
The present invention is not described in detail in part as being well known to those skilled in the art. The above examples are merely illustrative of preferred embodiments of the invention, which are not exhaustive of all details, nor are they intended to limit the invention to the particular embodiments disclosed. Various modifications and improvements of the technical scheme of the present invention will fall within the protection scope of the present invention as defined in the claims without departing from the design spirit of the present invention.
Claims (10)
1. The high temperature resistant silicone rubber is characterized in that: the high-temperature-resistant silicon rubber raw material formula comprises the following components in parts by weight:
100 parts of silicone rubber compound;
4-9 parts of cross-linking agent;
1-3 parts of vulcanizing agent;
5-30 parts of heat resistant agent (FS).
2. A high temperature resistant silicone rubber according to claim 1, wherein the heat resistant agent (FS) is an inorganic substance containing iron and tin;
preferably, the silicone rubber compound contains Si, C, O, H and other elements.
3. The high temperature resistant silicone rubber of claim 1 wherein the cross-linking agent is one, two or three of hydroxy silicone oil, vinyl silicone oil and hexamethyldisilazane.
4. The high temperature resistant silicone rubber of claim 1 wherein the vulcanizing agent is one or both of two-four and two-five.
5. The high temperature resistant silicone rubber according to claim 2, wherein the inorganic substances containing iron and tin are prepared by mixing ferric chloride and tin chloride, and sintering at 300-650 ℃ by a coprecipitation method.
6. A high temperature resistant silicone rubber according to claim 1, wherein the cross-linking agent is 5 parts of hydroxy silicone oil or vinyl silicone oil or hexamethyldisilazane or 1.5 to 3 parts of hydroxy silicone oil, vinyl silicone oil and hexamethyldisilazane, respectively.
7. The high temperature resistant silicone rubber of claim 5, wherein the molar ratio of ferric chloride to stannic chloride is 1-3: 5 to 7.
8. A high temperature resistant silicone rubber as defined in claim 5, wherein the high temperature sintering is at a temperature of 300 ℃, 400 ℃, 500 ℃, 600 ℃ and 650 ℃.
9. A process for preparing a rubber according to any one of claims 1 to 8, comprising the steps of:
(1) Adding tin chloride and ferric chloride into deionized water, stirring until solid particles are completely dissolved, regulating the PH to be 7-9, stirring, centrifuging, washing to remove chloride ions in the solution, drying to obtain a crude product, grinding the obtained crude product, sintering, and cooling to room temperature after sintering to obtain a heat resistant agent;
(2) Uniformly mixing the silicone rubber compound, the cross-linking agent and the heat-resistant agent obtained in the step (1) on a mixing mill, adding the vulcanizing agent, uniformly mixing, vulcanizing at 150-160 ℃ for 0.5-1 hour, and cooling to room temperature to obtain the high-temperature-resistant silicone rubber.
10. The method of claim 9, wherein the step of determining the position of the substrate comprises,
in the step (1), the sintering is as follows: sintering at 300 ℃ for 1 hour, then at 400 ℃ for 1 hour, then at 500 ℃ for 1 hour, then at 600 ℃ for 1 hour, and finally at 650 ℃ for 1 hour.
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| CN202310273806.7A CN116218227A (en) | 2023-03-21 | 2023-03-21 | High-temperature-resistant silicone rubber and preparation method thereof |
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| CN202310273806.7A CN116218227A (en) | 2023-03-21 | 2023-03-21 | High-temperature-resistant silicone rubber and preparation method thereof |
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