CN116199831A - High-temperature-resistant and irradiation-resistant sealing rubber and preparation method thereof - Google Patents

High-temperature-resistant and irradiation-resistant sealing rubber and preparation method thereof Download PDF

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CN116199831A
CN116199831A CN202310305835.7A CN202310305835A CN116199831A CN 116199831 A CN116199831 A CN 116199831A CN 202310305835 A CN202310305835 A CN 202310305835A CN 116199831 A CN116199831 A CN 116199831A
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parts
rubber
resistant
vulcanization
temperature
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王春宏
张悦
张明
张荣发
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Yangzhou University
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/04—Acids; Metal salts or ammonium salts thereof
    • C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic
    • C08K7/26—Silicon- containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
    • C08K2003/2213—Oxides; Hydroxides of metals of rare earth metal of cerium

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Sealing Material Composition (AREA)

Abstract

The scheme relates to a high temperature resistant and irradiation resistant sealing rubber and a preparation method thereof, wherein phenyl silicone rubber is used as a rubber matrix, cerium oxide is used as a heat stabilizer, lead methacrylate is used as a functional filler, and additives such as diphenyl silicon glycol, white carbon black, hexamethyldisilazane, KH550, diphenyl dimethoxy silane, DCP and the like are used as rubber formulas, and the final product is prepared through banburying, high temperature treatment, vulcanization and two-stage vulcanization. The lead methacrylate can be used as an auxiliary crosslinking agent to perform crosslinking reaction with phenyl silicone rubber to improve heat resistance of the rubber, can also be used as a radiation-shielding functional filler, and can reduce radiation damage of rays to the material through photoelectric effect, so that the service life of the material is prolonged, and the radiation-resisting effect is achieved; the method is simple to operate, and the prepared high-temperature-resistant and radiation-resistant rubber has excellent comprehensive performance and can be used as a radiation-resistant sealing ring in the nuclear industry for a long time.

Description

High-temperature-resistant and irradiation-resistant sealing rubber and preparation method thereof
Technical Field
The invention relates to the technical field of rubber preparation, in particular to high-temperature-resistant irradiation sealing rubber and a preparation method thereof.
Background
The silicone rubber (methyl vinyl silicone rubber) is a linear polymer with Si-O-Si chain segments as main chains and organic groups as side chains, is a typical semi-organic semi-inorganic polymer, and has the workability of organic polymer materials and the heat resistance of inorganic polymers. Because of the specificity of the main chain structure of the silicone rubber, the larger bond energy between Si-O is not easy to be damaged by high temperature, and the introduction of phenyl further enhances the high temperature resistance of the silicone rubber. Phenyl silicone rubber is therefore often used as sealing rings, gaskets, tubing, rods, etc. for ablation-, heat aging-or radiation-resistant parts. However, under certain extreme working conditions in the field of nuclear industry, rubber materials are required to have high and low temperature resistance, irradiation resistance and the like, and the conventional methyl vinyl silicone rubber cannot meet the requirements.
The heat-resistant and irradiation-resistant modification of the phenyl silicone rubber produced by the prior art is mainly used for prolonging the service life of the phenyl silicone rubber in the fields of aerospace, chemical industry, electric power, nuclear industry and the like, and in the practical use condition, the phenyl silicone rubber is generally modified by adding a heat stabilizer, and regarding the modification of the silicone rubber, the applicant Zhan Xuegui reports that the heat stabilizer is different metal oxides, so that the high-temperature-resistant silicone rubber is successfully prepared, and the material has good high-temperature resistance at 350 ℃; applicant Xu Jijun solves the problems existing in the preparation of silicon rubber added with metal oxide by solving the problems of CeO 2 Has poor compatibility with silicon rubber, and successfully prepares the high temperature resistant silicon rubber sealing ring. Although the thermal modification of the silicon rubber is studied more, the irradiation-resistant modification is rarely reported, and no working condition ring capable of completely meeting the high temperature and high irradiation dose of one rubber exists at presentIn environmental use, it is therefore urgent to study a material resistant to high temperature and radiation.
Disclosure of Invention
Aiming at the defects in the prior art, the invention selects phenyl silicone rubber as a matrix, and the rubber has good high-temperature radiation resistance by adding cerium oxide (CeO) 2 ) As the heat stabilizer, lead methacrylate (Pb (MAA) was used 2 ) As a radiation-resistant auxiliary agent, the novel high-temperature-resistant radiation-resistant rubber is prepared by adopting a blending mode, so that the service life of the rubber in a high-temperature radiation environment is greatly prolonged.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a preparation method of high-temperature-resistant and irradiation-resistant sealing rubber comprises the following steps:
1) Banburying by an internal mixer:
setting the banburying temperature to 120+/-1 ℃ and the rotating speed to 30+/-3 r/min, putting the phenyl silicone rubber into the banburying device, and carrying out banburying for 2min; then adding cerium oxide, diphenyl silicon glycol and lead methacrylate in batches, and banburying for 5min;
adding all the white carbon black with diphenyl dimethoxy silane, KH550 and hexamethyldisilazane drops into an internal mixer, banburying for 5min, and taking out the mixed rubber;
2) High temperature treatment:
putting the rubber compound into an open mill to be discharged, and putting the rubber compound into an oven to be treated for 1h at 150+/-1 ℃;
3) Vulcanizing:
cutting the rubber compound treated in the step 2) into blocks, putting the blocks into an internal mixer again, adding a vulcanizing agent DCP, and banburying for 5min at 60+/-1 ℃; after the banburying is finished, placing for 24 hours, and vulcanizing; then, the mixed rubber is vulcanized for a period of time on a plate vulcanizing instrument, wherein the vulcanization temperature is 175+/-1 ℃ and the vulcanization time is 15min;
4) Two-stage vulcanization:
and (3) performing secondary vulcanization on the finished product subjected to primary vulcanization, wherein the vulcanization conditions are stage temperature rise, vulcanization for 1h at 0-100 ℃, vulcanization for 1h at 100-150 ℃ and vulcanization for 4h at 150-200 ℃ to obtain the final sheet, namely the high-temperature-resistant and irradiation-resistant sealing rubber.
Further, the weight portions of the raw materials are as follows: 100 parts of phenyl silicone rubber, 5-10 parts of cerium oxide, 3-5 parts of diphenyl silicon glycol, 2-6 parts of diphenyl dimethyl silane, 1-3 parts of KH550, 4-6 parts of hexamethyldisilazane, 50 parts of white carbon black, 1-5 parts of vulcanizing agent DCP and 10-30 parts of lead methacrylate.
The invention further provides the high-temperature-resistant and irradiation-resistant sealing rubber prepared by the preparation method.
The beneficial effects of the invention are as follows:
1. the invention takes phenyl silicone rubber as a matrix material and adds Pb (MAA) 2 The filler can further improve the crosslinking degree of the phenyl silicone rubber in an irradiation environment, has a certain shielding effect, and can prolong the service life of the material in the irradiation environment;
2. in order to improve the heat resistance of the material, cerium oxide is added as a heat stabilizer, and a heat-resistant additive is added to prevent oxidation of a side methyl group, so that the aim of improving the heat resistance of the silicone rubber is fulfilled, and the heat resistance of the silicone rubber can be greatly improved;
3. the method is simple to operate, and the prepared high-temperature-resistant and radiation-resistant rubber has excellent comprehensive performance and can be used as a radiation-resistant sealing ring in the nuclear industry for a long time.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a thermogravimetric test of the samples prepared in examples 1-6.
Detailed Description
The following description of the embodiments of the present invention will be made apparent and fully in view of the accompanying drawings, in which some, but not all embodiments of the invention are shown. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In addition, the technical features of the different embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
Examples: a preparation method of high-temperature-resistant and irradiation-resistant sealing rubber comprises the following steps:
1) Banburying by an internal mixer:
setting the banburying temperature to 120+/-1 ℃ and the rotating speed to 30+/-3 r/min, putting the phenyl silicone rubber into the banburying device, and carrying out banburying for 2min; then adding cerium oxide, diphenyl silicon glycol and lead methacrylate in batches, and banburying for 5min;
adding all the white carbon black with diphenyl dimethoxy silane, KH550 and hexamethyldisilazane drops into an internal mixer, banburying for 5min, and taking out the mixed rubber;
2) High temperature treatment:
putting the rubber compound into an open mill to be discharged, and putting the rubber compound into an oven to be treated for 1h at 150+/-1 ℃;
3) Vulcanizing:
cutting the rubber compound treated in the step 2) into blocks, putting the blocks into an internal mixer again, adding a vulcanizing agent DCP, and banburying for 5min at 60+/-1 ℃; after the banburying is finished, placing for 24 hours, and vulcanizing; then, the mixed rubber is vulcanized for a period of time on a plate vulcanizing instrument, wherein the vulcanization temperature is 175+/-1 ℃ and the vulcanization time is 15min;
4) Two-stage vulcanization:
and (3) performing secondary vulcanization on the finished product subjected to primary vulcanization, wherein the vulcanization conditions are stage temperature rise, vulcanization for 1h at 0-100 ℃, vulcanization for 1h at 100-150 ℃ and vulcanization for 4h at 150-200 ℃ to obtain the final sheet, namely the high-temperature-resistant and irradiation-resistant sealing rubber.
The weight portions of the raw materials in the steps are as follows: 100 parts of phenyl silicone rubber, 5-10 parts of cerium oxide, 3-5 parts of diphenyl silicon glycol, 2-6 parts of diphenyl dimethyl silane, 1-3 parts of KH550, 4-6 parts of hexamethyldisilazane, 50 parts of white carbon black, 1-5 parts of vulcanizing agent DCP and 10-30 parts of lead methacrylate.
The composition of the raw materials in the specific examples is as follows
Example 1:
100 parts of phenyl silicone rubber, 0 part of cerium oxide, 3 parts of diphenyl silicon glycol, 2 parts of diphenyl dimethyl silane, 550 parts of KH, 4 parts of hexamethyldisilazane, 50 parts of white carbon black, 1 part of vulcanizing agent DCP and 10 parts of lead methacrylate;
material a prepared according to the above procedure.
Example 2:
100 parts of phenyl silicone rubber, 5 parts of cerium oxide, 3 parts of diphenyl silicon glycol, 2 parts of diphenyl dimethyl silane, 550 parts of KH, 4 parts of hexamethyldisilazane, 50 parts of white carbon black, 1 part of vulcanizing agent DCP and 0 part of lead methacrylate;
material B prepared according to the above procedure.
Example 3:
100 parts of phenyl silicone rubber, 5 parts of cerium oxide, 3 parts of diphenyl silicon glycol, 2 parts of diphenyl dimethyl silane, 550 parts of KH, 4 parts of hexamethyldisilazane, 50 parts of white carbon black, 1 part of vulcanizing agent DCP and 10 parts of lead methacrylate;
material C prepared according to the above procedure.
Example 4:
100 parts of phenyl silicone rubber, 5 parts of cerium oxide, 3 parts of diphenyl silicon glycol, 2 parts of diphenyl dimethyl silane, 550 parts of KH, 4 parts of hexamethyldisilazane, 50 parts of white carbon black, 1 part of vulcanizing agent DCP and 20 parts of lead methacrylate;
material D prepared according to the above procedure.
Example 5:
100 parts of phenyl silicone rubber, 5 parts of cerium oxide, 3 parts of diphenyl silicon glycol, 2 parts of diphenyl dimethyl silane, 550 parts of KH, 4 parts of hexamethyldisilazane, 50 parts of white carbon black, 1 part of vulcanizing agent DCP and 30 parts of lead methacrylate;
material E prepared according to the above procedure.
Example 6:
100 parts of phenyl silicone rubber, 0 part of cerium oxide, 3 parts of diphenyl silicon glycol, 2 parts of diphenyl dimethyl silane, 550 parts of KH, 4 parts of hexamethyldisilazane, 50 parts of white carbon black, 1 part of vulcanizing agent DCP and 0 part of lead methacrylate;
material F prepared according to the above procedure.
The above materials were tested, including mechanical properties before aging (tensile strength, elongation at break), mechanical properties after thermal oxidative aging at 280℃for 2 hours, mechanical properties of the materials after 10Ky irradiation, and temperature at 5% weight loss, and the results are shown in Table 1.
TABLE 1
Figure BDA0004146821890000061
Example 1 contained no cerium oxide, example 2 contained no lead methacrylate, 10 parts of lead methacrylate in examples 3-5 increased to 30 parts, and example 6 contained no cerium oxide and lead methacrylate. From the comparison of the data in table 1, the temperature change of the embodiment 1 and the embodiment 6 at the weight loss of 5% is not obvious, and the temperatures of the embodiments 2 to 5 at the weight loss of 5% are obviously improved from the embodiment 6 through the thermal weight test (fig. 1), which shows that the heat-resistant modification effect of the cerium oxide on the silicon rubber is obvious; and the performance retention rate is good after aging for 2 hours at 280 ℃, the addition of cerium oxide effectively prevents the growth of molecular chains at a higher temperature, and the heat resistance of the silicone rubber is improved well.
As can be seen from Table 1, the radiation-resistant silicone rubber prepared in the examples of the invention has good mechanical properties, good temperature resistance and good radiation resistance, and the comparative examples 3 to 5 have good retention rate of tensile strength and elongation at break after 10Gy irradiation as the shielding property of the material is increased with the increase of the addition amount of methacrylic acid, and the addition of lead methacrylate plays a certain role in crosslinking of the material.
In the present case, ceO is added 2 The heat-resistant modification is carried out on the p-phenyl silicone rubber, so that the service life of the p-phenyl silicone rubber at high temperature is prolonged; and Pb (MAA) is added 2 The free radical copolymerization is carried out with the double bond of the phenyl silicone rubber end group in the irradiation process, so that the crosslinking degree can be improved, the problem of difficult crosslinking of the phenyl silicone rubber is solved, and meanwhile Pb (MAA) is produced 2 Pb contained in the material can play a role in shielding and reduce high-energy radiationThe damage of the pair molecular chain is avoided, the service life of the material is prolonged, and the novel high-temperature-resistant radiation-proof material is provided to be used as a sealing ring.
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown and described, it is well suited to various fields of use for which the invention would be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the specific details and illustrations shown and described herein, without departing from the general concepts defined in the claims and their equivalents.

Claims (3)

1. The preparation method of the high-temperature-resistant and irradiation-resistant sealing rubber is characterized by comprising the following steps of:
1) Banburying by an internal mixer:
setting the banburying temperature to 120+/-1 ℃ and the rotating speed to 30+/-3 r/min, putting the phenyl silicone rubber into the banburying device, and carrying out banburying for 2min; then adding cerium oxide, diphenyl silicon glycol and lead methacrylate in batches, and banburying for 5min;
adding all the white carbon black with diphenyl dimethoxy silane, KH550 and hexamethyldisilazane drops into an internal mixer, banburying for 5min, and taking out the mixed rubber;
2) High temperature treatment:
putting the rubber compound into an open mill to be discharged, and putting the rubber compound into an oven to be treated for 1h at 150+/-1 ℃;
3) Vulcanizing:
cutting the rubber compound treated in the step 2) into blocks, putting the blocks into an internal mixer again, adding a vulcanizing agent DCP, and banburying for 5min at 60+/-1 ℃; after the banburying is finished, placing for 24 hours, and vulcanizing; then, the mixed rubber is vulcanized for a period of time on a plate vulcanizing instrument, wherein the vulcanization temperature is 175+/-1 ℃ and the vulcanization time is 15min;
4) Two-stage vulcanization:
and (3) performing secondary vulcanization on the finished product subjected to primary vulcanization, wherein the vulcanization conditions are stage temperature rise, vulcanization for 1h at 0-100 ℃, vulcanization for 1h at 100-150 ℃ and vulcanization for 4h at 150-200 ℃ to obtain the final sheet, namely the high-temperature-resistant and irradiation-resistant sealing rubber.
2. The method for preparing the high-temperature-resistant and irradiation-resistant sealing rubber according to claim 1, which is characterized by comprising the following raw materials in parts by weight: 100 parts of phenyl silicone rubber, 5-10 parts of cerium oxide, 3-5 parts of diphenyl silicon glycol, 2-6 parts of diphenyl dimethyl silane, 1-3 parts of KH550, 4-6 parts of hexamethyldisilazane, 50 parts of white carbon black, 1-5 parts of vulcanizing agent DCP and 10-30 parts of lead methacrylate.
3. A high temperature-resistant and irradiation-resistant sealing rubber produced by the production method according to claim 1 or 2.
CN202310305835.7A 2023-03-27 2023-03-27 High-temperature-resistant and irradiation-resistant sealing rubber and preparation method thereof Pending CN116199831A (en)

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