CN110564163A - preparation method of fluorosilicone rubber for high-temperature-resistant layer of high-temperature cable - Google Patents
preparation method of fluorosilicone rubber for high-temperature-resistant layer of high-temperature cable Download PDFInfo
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- CN110564163A CN110564163A CN201910786198.3A CN201910786198A CN110564163A CN 110564163 A CN110564163 A CN 110564163A CN 201910786198 A CN201910786198 A CN 201910786198A CN 110564163 A CN110564163 A CN 110564163A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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
- C08L83/04—Polysiloxanes
- C08L83/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/28—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances natural or synthetic rubbers
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- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention provides a preparation method of fluorosilicone rubber for a high-temperature-resistant layer of a high-temperature cable, which comprises the following steps: preheating an internal mixer to 80-90 ℃, then adding silicon rubber, and uniformly stirring; adding a lubricant, a white carbon black reinforcing agent, a silane assistant and a cerium oxide filler, uniformly mixing and agglomerating the raw materials; heating the internal mixer to 130 +/-5 ℃ to start rubber mixing, kneading for 60-70min, and keeping the vacuum degree at-0.08 MPa; discharging the banburying rubber, open-milling by an open mill, standing for 2 hours after a lower roll, and filtering to obtain open-milled rubber; and adding a vulcanizing agent into the open milling rubber, uniformly mixing, putting into a mold, and vulcanizing and molding to obtain the fluorosilicone rubber compound. According to the preparation method disclosed by the invention, the excellent ageing resistance of the fluorosilicone rubber is utilized, the white carbon black reinforcing agent and the cerium oxide filling agent are adopted to improve the high-temperature resistance of the high-temperature-resistant layer of the fluorosilicone rubber, the process parameters of each step are strictly controlled during preparation, and the prepared fluorosilicone rubber can enable a high-temperature cable to have a long service life at about 300 ℃, so that the high-temperature cable can adapt to a more severe use environment.
Description
Technical Field
The invention relates to the technical field of high-temperature heating cables, in particular to a preparation method of high-temperature-resistant and anti-aging fluorosilicone rubber for a high-temperature-resistant layer of a high-temperature cable.
Background
high temperature heating cables are used in civil and industrial fields to achieve heating or heat preservation effects. The high-temperature cable generally comprises an alloy or carbon fiber heating core wire, a flame-retardant high-temperature-resistant insulating layer, a high-temperature-resistant sheath (such as an aluminum foil layer), a shielding layer and an enameled wire from inside to outside; the flame-retardant high-temperature-resistant insulating layer wrapping the heating core wire is very critical to the performance influence of the high-temperature cable, and determines the heating temperature and the service life of the high-temperature cable. The existing flame-retardant high-temperature-resistant insulating layer generally adopts a silica gel layer, such as vinyl silicone rubber, and the silica gel has long service life and excellent ageing resistance at normal working temperature (180-200 ℃); however, when the heating temperature exceeds 200 ℃, the aging phenomenon of the silica gel is obvious, and the service life is rapidly reduced. Therefore, for a heating environment requiring a higher temperature, the current high-temperature cable using silicone rubber as a flame-retardant high-temperature-resistant insulating layer is not suitable, and a high-temperature cable flame-retardant high-temperature-resistant insulating layer having excellent aging resistance at a high temperature needs to be researched.
Disclosure of Invention
In view of the above-mentioned drawbacks of the conventional high-temperature cables, the present invention aims to provide a method for preparing a fluorosilicone rubber for a high-temperature resistant layer of a high-temperature cable, which is resistant to high temperature and aging, and the fluorosilicone rubber prepared by the method can be used as an insulating high-temperature resistant layer of a high-temperature cable, and can not only resist higher heating temperature, but also have excellent aging resistance.
in order to achieve the purpose of the invention, the preparation method of the fluorosilicone rubber for the high-temperature resistant layer of the high-temperature cable is characterized in that the fluorosilicone rubber is prepared from the following raw materials in parts by weight: 100 parts of silicon rubber; 38-43 parts of white carbon black reinforcing agent; 9-11.6 parts of a silane assistant; 2-3.5 parts of cerium oxide filler; 0.10-0.18 part of lubricant and 0.5-1.5 parts of vulcanizing agent; the silicone rubber is a mixture of raw methyl vinyl silicone rubber and raw fluorosilicone rubber in a weight ratio of 6:94, wherein the vinyl content of the raw methyl vinyl silicone rubber is 0.25-0.35%, and the vinyl content of the raw fluorosilicone rubber is 0.4-0.8%; the white carbon black reinforcing agent is formed by mixing white carbon black and siloxane containing active hydrogen according to the weight part of 100: 10-18; the vulcanizing agent is one or more of dicumyl peroxide, 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane and tert-butyl peroxybenzoate; the preparation method of the fluorosilicone rubber comprises the following steps:
s1, preheating the internal mixer to 80-90 ℃, then adding silicon rubber, and stirring for 20 minutes;
S2, adding a lubricant, a white carbon black reinforcing agent, a silane assistant and a cerium oxide filler, uniformly mixing, and agglomerating the raw materials;
S3, heating the internal mixer to 130 +/-5 ℃ to start rubber mixing, kneading for 60-70min, and obtaining rubber mixing under the vacuum degree of-0.08 MPa;
S4, discharging the banburying rubber, putting the banburying rubber into an open mill for uniform milling, standing the lower roll for 2 hours, and then putting the lower roll into a filter for filtering to obtain the open mill rubber;
s5, adding a vulcanizing agent into the open mixing rubber, uniformly mixing, putting into a mould, and vulcanizing and molding to obtain a fluorosilicone rubber compound; the vulcanization temperature is 170 +/-5 ℃, and the vulcanization time is 10 min.
Preferably, the siloxane containing active hydrogen in the white carbon black reinforcing agent is one or more of tetramethylcyclotetrasiloxane, trifluoropropylmethylcyclotrisiloxane and tetramethyldisiloxane.
More preferably, the content of active hydrogen in the siloxane containing active hydrogen in the white carbon black reinforcing agent is 0.2-0.28% by mass.
more preferably, the white carbon black in the white carbon black reinforcing agent has the particle size of 10-40nm and the specific surface area of 200-300m2Fumed silica/g.
Preferably, the silane assistant comprises one or more of hydroxyl-terminated polydimethylsiloxane, dimethyl diethoxysilane and hydroxyl fluorosilicone oil.
According to the preparation method of the fluorosilicone rubber for the high-temperature-resistant layer of the high-temperature cable, the excellent ageing resistance of the fluorosilicone rubber is utilized, the white carbon black reinforcing agent and the cerium oxide filling agent are adopted to improve the high-temperature resistance of the high-temperature-resistant layer of the fluorosilicone rubber, the technological parameters of each step are strictly controlled during preparation, and the prepared fluorosilicone rubber can enable the high-temperature cable to have long service life at about 300 ℃, so that the high-temperature cable can adapt to a more severe service environment.
Detailed Description
the features and advantages of the invention are described in detail below with reference to specific embodiments.
Compared with methyl vinyl silicone rubber, the fluorosilicone rubber has extremely excellent oil resistance, solvent resistance and chemical resistance; and the fluorosilicone rubber has little performance change under the harsh conditions of high temperature, low temperature, humidity, oil, solvent, chemicals, ozone and the like. However, since the pure fluorosilicone rubber is greatly affected by temperature, it is necessary to add a reinforcing agent, a rare earth filler, and the like to the fluorosilicone rubber to ensure that the fluorosilicone rubber has relatively high heat resistance.
specifically, according to an embodiment of the present invention, a preparation method of a fluorosilicone rubber for a high temperature resistant layer of a high temperature cable comprises the following steps: 100 parts of silicon rubber; 38-43 parts of white carbon black reinforcing agent; 9-11.6 parts of a silane assistant; 2-3.5 parts of cerium oxide filler; 0.10-0.18 part of lubricant and 0.5-1.5 parts of vulcanizing agent; the silicone rubber is a mixture of raw methyl vinyl silicone rubber and raw fluorosilicone rubber in a weight ratio of 6:94, wherein the vinyl content of the raw methyl vinyl silicone rubber is 0.25-0.35%, and the vinyl content of the raw fluorosilicone rubber is 0.4-0.8%; the white carbon black reinforcing agent is formed by mixing white carbon black and siloxane containing active hydrogen according to the weight part of 100: 10-18; the vulcanizing agent is one or more of dicumyl peroxide, 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane and tert-butyl peroxybenzoate; the preparation method of the fluorosilicone rubber comprises the following steps:
S1, preheating the internal mixer to 80-90 ℃, then adding silicon rubber, and stirring for 20 minutes; after the internal mixer is preheated, adding the raw rubber into the internal mixer for stirring, so that the raw rubber can be uniformly mixed to the maximum extent; the excessive preheating temperature can obviously soften raw rubber and various accessory ingredients added subsequently, which is not beneficial to uniform mixing;
S2, adding a lubricant, a white carbon black reinforcing agent, a silane assistant and a cerium oxide filler, uniformly mixing, and agglomerating the raw materials; in actual operation, in order to achieve the purpose of uniformly mixing the raw rubber and various compounding agents, the compounding agents can be added in batches for multiple times;
S3, heating the internal mixer to 130 +/-5 ℃ to start rubber mixing, kneading for 60-70min, and obtaining rubber mixing under the vacuum degree of-0.08 MPa;
S4, discharging the banburying rubber, putting the banburying rubber into an open mill for uniform milling, standing the lower roll for 2 hours, and then putting the lower roll into a filter for filtering to obtain the open mill rubber;
S5, adding a vulcanizing agent into the open mixing rubber, uniformly mixing, putting into a mould, and vulcanizing and molding to obtain a fluorosilicone rubber compound; the vulcanization temperature is less than or equal to 170 ℃, and the vulcanization time is 10 min; because the fluorosilicone rubber of the invention takes the methyl vinyl silicone rubber as a main component, the vulcanization temperature can be generally set to about 180 ℃, but the thickness of the high-temperature resistant layer for the high-temperature cable is very thin, the problem of vulcanization is not too high, otherwise, the vulcanization reversion phenomenon of the rubber is easily caused, and the physical property of the rubber is reduced, the vulcanization temperature of the invention is preferably set below 170 ℃, and the vulcanization temperature is more suitable at 160-170 ℃ through the verification of practical production tests.
In order to ensure the temperature resistance of the fluorosilicone rubber at high temperature, the oxide of the rare earth element cerium is added into the fluorosilicone rubber as a filler, and experiments prove that the performance stability of the fluorosilicone rubber at high temperature can be ensured when the mass part of cerium oxide in the fluorosilicone rubber reaches a certain degree, for example, in a preferred embodiment, when the mass part of cerium oxide reaches about 3, the fluorosilicone rubber still has good performance stability at high temperature about 350 ℃; when the mass fraction of the cerium oxide exceeds 3.5, the effect of the cerium oxide particles as impurity defects in the fluorine-containing silicone rubber matrix is obviously embodied, the thermal degradation of the rubber is very obvious, and the cerium oxide particles can be rapidly explained and fail at the temperature of over 400 ℃.
In addition, according to experiments, the white carbon black and siloxane are adopted as the reinforcing agent of the fluorosilicone rubber, so that the mechanical property of the fluorosilicone rubber can be obviously improved, the viscosity is reduced, and the processing performance of the fluorosilicone rubber is improved; in addition, the content of active hydrogen in the siloxane has a relatively obvious influence on the tensile strength of the fluorosilicone rubber within a certain range, in a more preferred embodiment, the content of the active hydrogen in the siloxane containing the active hydrogen in the white carbon black reinforcing agent is 0.2-0.28% by mass, and when the content of the active hydrogen exceeds 0.3% by mass, the influence on the performance of the fluorosilicone rubber is relatively insignificant.
in another preferred embodiment, the silica in the silica reinforcing agent has a particle size of 10-40nm and a specific surface area of 200-300m2The impurity defect effect of the fumed silica/g in the fluorine silicon rubber matrix is obviously reflected due to the overlarge particle size of the fumed silica, and rubber molecules cannot penetrate into carbon black particles, so that the reinforcing performance of the fumed silica on rubber is influenced; in addition, the addition amount of the white carbon black needs to be strictly controlled, the reinforcing effect is influenced if the addition amount of the white carbon black is too small, the dilution effect is generated if the addition amount of the white carbon black is too large, and the white carbon black cannot be well uniformly dispersed in the rubber.
In another preferred embodiment, the silane adjuvant comprises one or more of hydroxyl-terminated polydimethylsiloxane, dimethyldiethoxysilane and hydroxyl fluorosilicone oil.
the vulcanizing agent of the fluorosilicone rubber adopts one or more of dicumyl peroxide, 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane and tert-butyl peroxybenzoate with higher activity, so that the adverse effect of the vulcanizing agent on the crosslinking density of the rubber is reduced.
According to the high-temperature-resistant and anti-aging high-temperature-resistant cable fluorosilicone rubber high-temperature-resistant layer, the excellent anti-aging performance of fluorosilicone rubber is utilized, the white carbon black reinforcing agent and a proper amount of cerium oxide filling agent are adopted to improve the high-temperature-resistant performance of the high-temperature-resistant layer fluorosilicone rubber, the technological parameters of all steps are strictly controlled during preparation, and the prepared fluorosilicone rubber can enable a high-temperature cable to have a long service life at about 300 ℃, so that the high-temperature cable can adapt to a more severe use environment.
The present invention is not limited to the embodiments described above, and those skilled in the art may make modifications or changes within the scope of the disclosure without departing from the spirit of the present invention, so that the scope of the present invention is defined by the appended claims.
Claims (5)
1. a preparation method of fluorosilicone rubber for a high-temperature-resistant layer of a high-temperature cable is disclosed, wherein the fluorosilicone rubber is prepared from the following raw materials in parts by weight: 100 parts of silicon rubber; 38-43 parts of white carbon black reinforcing agent; 9-11.6 parts of a silane assistant; 2-3.5 parts of cerium oxide filler; 0.10-0.18 part of lubricant and 0.5-1.5 parts of vulcanizing agent; the silicone rubber is a mixture of raw methyl vinyl silicone rubber and raw fluorosilicone rubber in a weight ratio of 6:94, wherein the vinyl content of the raw methyl vinyl silicone rubber is 0.25-0.35%, and the vinyl content of the raw fluorosilicone rubber is 0.4-0.8%; the white carbon black reinforcing agent is formed by mixing white carbon black and siloxane containing active hydrogen according to the weight part of 100: 10-18; the vulcanizing agent is one or more of dicumyl peroxide, 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane and tert-butyl peroxybenzoate; the preparation method of the fluorosilicone rubber is characterized by comprising the following steps:
s1, preheating the internal mixer to 80-90 ℃, then adding silicon rubber, and stirring for 20 minutes;
S2, adding a lubricant, a white carbon black reinforcing agent, a silane assistant and a cerium oxide filler, uniformly mixing, and agglomerating the raw materials;
S3, heating the internal mixer to 130 +/-5 ℃ to start rubber mixing, kneading for 60-70min, and obtaining rubber mixing under the vacuum degree of-0.08 MPa;
S4, discharging the banburying rubber, putting the banburying rubber into an open mill for uniform milling, standing the lower roll for 2 hours, and then putting the lower roll into a filter for filtering to obtain the open mill rubber; and the number of the first and second groups,
S5, adding a vulcanizing agent into the open mixing rubber, uniformly mixing, putting into a mould, and vulcanizing and molding to obtain a fluorosilicone rubber compound; the vulcanization temperature is 170 +/-5 ℃, and the vulcanization time is 10 min.
2. the method for preparing fluorosilicone rubber for a high temperature resistant layer of a high temperature cable according to claim 1, wherein the active hydrogen-containing siloxane in the white carbon black reinforcing agent is one or more of tetramethylcyclotetrasiloxane, trifluoropropylmethylcyclotrisiloxane and tetramethyldisiloxane.
3. The method for preparing the fluorosilicone rubber for the high-temperature-resistant layer of the high-temperature cable according to claim 2, wherein the content of active hydrogen in the active hydrogen-containing siloxane in the white carbon black reinforcing agent is 0.2 to 0.28 mass percent.
4. the method for preparing the fluorosilicone rubber for the high temperature resistant layer of the high temperature cable according to claim 2, wherein the white carbon black in the white carbon black reinforcing agent has a particle size of 10-40nm and a specific surface area of 200-300m2fumed silica/g.
5. The preparation method of the fluorosilicone rubber for the high temperature resistant layer of the high temperature cable according to claim 1 or 2, wherein the silane adjuvant comprises one or more of hydroxyl terminated polydimethylsiloxane, dimethyldiethoxysilane and hydroxyl fluorosilicone oil.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111534105A (en) * | 2020-04-02 | 2020-08-14 | 浙江翔宇密封件有限公司 | Anti-aging silicone rubber sealing material for high-speed rail sealing element and preparation method thereof |
| CN114055818A (en) * | 2021-11-16 | 2022-02-18 | 内蒙古工业大学 | Rubber-based flexible composite material and preparation method thereof |
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