CN115466516A - High-tear-resistance flame-retardant silicone rubber composition and preparation method thereof - Google Patents
High-tear-resistance flame-retardant silicone rubber composition and preparation method thereof Download PDFInfo
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- CN115466516A CN115466516A CN202211117094.1A CN202211117094A CN115466516A CN 115466516 A CN115466516 A CN 115466516A CN 202211117094 A CN202211117094 A CN 202211117094A CN 115466516 A CN115466516 A CN 115466516A
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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
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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
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/006—Additives being defined by their surface area
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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
- C08L2201/02—Flame or fire retardant/resistant
Abstract
The invention belongs to the field of silicone rubber preparation, and discloses a high-tear-resistance flame-retardant silicone rubber composition and a preparation method thereof. The composition comprises the following components: 30-70 parts of methyl vinyl silicone rubber; 10-25 parts of white carbon black; 10-40 parts of a flame retardant; 1-5 parts of a functional auxiliary agent; 0-6 parts of high tear resistance auxiliary agent; 2-5 parts of a structural control agent; 0.05 to 0.5 portion of internal release agent; 0-1 part of vulcanizing agent. According to the invention, the superfine aluminum hydroxide powder and the platinum complex are compounded, so that the specific gravity of the silicone rubber flame-retardant adhesive is reduced, and the mechanical strength is improved.
Description
Technical Field
The invention belongs to the field of silicone rubber preparation, and particularly relates to a high-tear-resistance flame-retardant silicone rubber composition and a preparation method thereof.
Background
The silicon rubber has good aging resistance, electrical appliance insulation performance and high and low temperature resistance, and the application of the silicon rubber composite material in the fields of automobiles, medical treatment and spaceflight is rapidly developed, but the silicon rubber is influenced by the chemical structure, and the mechanical strength of the silicon rubber is lower than that of natural rubber and styrene butadiene rubber. The need to further improve the mechanical strength of silicone rubbers, in particular the tear strength, is becoming increasingly important. Chinese patent CN107964248A discloses a low-modulus high-tear-strength silicone rubber and a preparation method thereof, which is mainly prepared by mixing different vinyl raw rubbers, white carbon black and a silane coupling agent. Chinese patent CN104559202A discloses a preparation method of a high-tear-resistance silicon rubber compound, which is mainly obtained by mixing methyl vinyl silica gel, white carbon black, zinc stearate and vinyl silicone oil, but the preparation method is complex. Chinese patent CN106589964A discloses a high-tear strength type high-temperature vulcanized silicone rubber, a preparation method and application thereof, wherein the high-tear strength type high-temperature vulcanized silicone rubber is mainly prepared by mixing methyl vinyl raw rubber, a filler, a crosslinking assistant, a vulcanizing agent and the like.
Therefore, a new high-tear-resistance flame-retardant silicone rubber composition and a preparation method thereof are urgently needed to be provided.
Disclosure of Invention
The invention aims to provide a high-tear-resistance flame-retardant silicone rubber composition and a preparation method thereof, aiming at the defects of the prior art. According to the invention, the superfine aluminum hydroxide powder and the platinum complex are compounded, so that the specific gravity of the silicone rubber flame-retardant adhesive is reduced, and the mechanical strength is improved.
In order to achieve the above object, one aspect of the present invention provides a high tear-resistant flame retardant silicone rubber composition comprising the following components:
30-70 parts of methyl vinyl silicone rubber;
10-25 parts of white carbon black;
10-40 parts of a flame retardant;
1-5 parts of a functional auxiliary agent;
0-6 parts of high tear resistance auxiliary agent;
2-5 parts of a structural control agent;
0.05 to 0.5 portion of internal release agent;
0-1 part of vulcanizing agent.
According to the invention, preferably, the methyl vinyl silicone rubber is compounded by a first methyl vinyl silicone rubber and a second methyl vinyl silicone rubber with a mass ratio of 95-50; wherein, the mol content of vinyl in the first methyl vinyl silicone rubber is 0.03-0.09%, and the molecular weight is 60-75 ten thousand; the second vinyl silicone rubber has a vinyl molar content of 1.0-3.5% and a molecular weight of 50-65 ten thousand.
According to the invention, preferably, the white carbon black is fumed white carbon black and/or precipitated white carbon black, and the specific surface area of the white carbon black is not less than 150m 2 /g。
According to the present invention, preferably, the flame retardant is ultrafine aluminum hydroxide powder having a particle size of less than 3 μm.
According to the present invention, preferably, the structural control agent is at least one of hydroxyl silicone oil, alkoxy silicone oil, vinyl hydroxyl silicone oil, diphenyl silicone glycol and triphenyl silicone alcohol. Further preferably, the vinyl hydroxyl silicone oil is hydroxyl-terminated vinyl silicone oil, and the structural formula is shown as formula (1):
wherein: me is methyl, vi is vinyl, m is the number of methyl links, n is the number of vinyl links,
m＝8-20，n＝1-10，m+n≤30；
the content of vinyl is 4-6% by the total weight of the hydroxyl vinyl silicone oil;
the viscosity of the hydroxyl vinyl silicone oil is 30-50 cst.
According to the invention, preferably, the internal mould release agent is stearic acid and/or a stearate. Further preferably, the internal mold release agent is at least one of zinc stearate, magnesium stearate, and calcium stearate.
According to the present invention, preferably, the functional auxiliary agent is at least one of platinum complex, imidazole compound, magnesium aluminum hydrotalcite, boric acid new, cerium oxide and iron oxide.
According to the present invention, preferably, the functional assistant is at least one of hexamethyldisilazane, dimethyldimethoxysilane, dimethyldiethoxysilane, and vinyltriethoxysilane.
According to the present invention, preferably, the high tear resistance auxiliary agent is a silane coupling agent containing a vinyl group and/or a vinyl silicon resin. Preferably, the high tear resistance additive is at least one of vinyltrimethoxysilane, vinyltriethoxysilane, vinyl silicone resin and tetramethyldivinylsilazane.
According to the invention, preferably, the vulcanizing agent is bis-tetra- (2, 4-dichlorobenzoyl peroxide) peroxide and/or bis-penta- (2, 5-dimethyl-2, 5-di-tert-butylperoxyhexane).
The invention also provides a preparation method of the high-tear-resistance flame-retardant silicone rubber composition, which comprises the following steps:
s1: mixing and kneading the methyl vinyl silicone rubber, the white carbon black, the flame retardant, the structural control agent and the internal mold release agent until the surface of the obtained rubber material is bright, and carrying out heat treatment on the obtained rubber material;
s2: carrying out high-temperature vacuum banburying treatment and cooling filtration on the rubber material subjected to heat treatment in the step S1 to obtain a banburied rubber;
s3: and mixing the internal mixing rubber and the functional auxiliary agent in an open mill to obtain the high-tear-resistance flame-retardant silicone rubber composition.
According to the present invention, preferably, in step S1,
the mixing temperature is 90-130 ℃;
the heat treatment temperature is 120-130 deg.C, and the time is 55-65min.
According to the present invention, preferably, in step S2, the conditions of the high-temperature vacuum banburying treatment include: the temperature is 125-135 ℃, the vacuum degree is-0.06 MPa-0.08 MPa, and the high-temperature banburying time is 0.5-1.5 h.
The technical scheme of the invention has the following beneficial effects:
according to the invention, the superfine aluminum hydroxide powder and the platinum complex are compounded, so that the specific gravity of the silicone rubber flame-retardant adhesive is reduced, and the mechanical strength is improved. Meanwhile, the silicone rubber flame retardant adhesive has the advantages of low specific gravity, excellent physical properties, good flame retardance, high insulativity and the like, and can be applied to the fields of electronics, electrics, wires, cables and the like.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
The raw materials in the following examples are all commercially available products.
The first and second methyl vinyl silicone rubbers are each available from Dongju Silicone (Nanjing) Inc.;
the hydrophobic fumed silica is purchased from Guangzhou Jibisheng scientific and technical industry Co., ltd;
the vinyl hydroxyl silicone oil is purchased from tin-free all-dimensional chemical company Limited.
Example 1
The embodiment provides a high-tear-resistance flame-retardant silicone rubber composition, which comprises the following components:
95 parts of methyl vinyl silicone rubber which is end-capped by dimethyl vinyl, has the molecular weight of 65 ten thousand and the molar content of vinyl of 0.08 percent;
5 parts of methyl vinyl silicone rubber which is end-capped by dimethyl vinyl, has the molecular weight of 55 ten thousand and the molar content of vinyl of 3.0 percent;
the specific surface area is 200m 2 25 parts of hydrophobic fumed silica per gram;
30 parts of superfine aluminum hydroxide powder with the particle size of 0.5-1.5 mu m;
0.5 part of platinum complex with the platinum content of 2000ppm and 0.3 part of benzotriazole;
3 parts of vinyl hydroxyl silicone oil with the viscosity of 35cst, wherein the content of vinyl is 5 percent based on the total weight of the hydroxyl vinyl silicone oil; 2 parts of vinyl silicone resin; 1 part of bis (2, 5-dimethyl-2, 5-di-tert-butylperoxy hexane); 0.1 part of zinc stearate.
The structural formula of the vinyl hydroxyl silicone oil is shown as the formula (1):
wherein: me is methyl, vi is vinyl, m is the number of methyl links, the number of n vinyl links, m =8-20, n =1-10, and m + n is less than or equal to 30;
the preparation method of the high-tear-resistance flame-retardant silicone rubber composition comprises the following steps:
s1: adding the methyl vinyl silicone rubber with the molecular weight of 65 ten thousand and the vinyl molar content of 0.08 percent, the dimethyl vinyl terminated silicone rubber, the vinyl hydroxy silicone oil and the zinc stearate into a kneader, adding the white carbon black and the superfine aluminum hydroxide powder into the kneader for four times, and controlling the powder feeding temperature to be 90-130 ℃; after the powder is eaten, kneading the surface of the sizing material to be bright, and then carrying out heat treatment for 60min at the temperature of 120-130 ℃;
s2: heating the rubber material subjected to heat treatment in the step S1 to 125-135 ℃, carrying out vacuum high-temperature banburying for 1h under the vacuum degree of-0.07 MPa, cooling and filtering to obtain a dense rubber;
s3: and mixing the banburying adhesive, a platinum complex with the platinum content of 2000ppm and benzotriazole in an open mill to obtain the high-tear-resistance flame-retardant silicone rubber composition.
Example 2
This example provides a high tear resistant flame retardant silicone rubber composition, which differs from example 1 only in that: the composition of this example includes the following components:
95 parts of methyl vinyl silicone rubber which is end-capped by dimethyl vinyl, has the molecular weight of 65 ten thousand and the molar content of vinyl of 0.08 percent;
5 parts of methyl vinyl silicone rubber which is terminated by dimethyl vinyl, has the molecular weight of 55 ten thousand and contains 2.0 percent of vinyl in mole;
the specific surface area is 200m 2 20 parts of hydrophobic fumed silica per gram;
30 parts of superfine aluminum hydroxide powder with the particle size of 1.0-1.5 mu m;
0.6 part of platinum complex with the platinum content of 2000ppm and 0.5 part of benzotriazole;
3 parts of vinyl hydroxyl silicone oil with the viscosity of 35cst, wherein the content of vinyl is 5 percent based on the total weight of the hydroxyl vinyl silicone oil; 1 part of vinyl silicone resin; 1 part of bis (2, 5-dimethyl-2, 5-di-tert-butylperoxy hexane); 0.3 part of calcium stearate.
The structural formula of the vinyl hydroxyl silicone oil is shown as the formula (1):
wherein: me is methyl, vi is vinyl, m is the number of methyl links, n is the number of vinyl links, m =8-20, n =1-10, and m + n is less than or equal to 30.
Example 3
This example provides a high tear resistant flame retardant silicone rubber composition, which differs from example 1 only in that: the composition of this example comprises the following components:
95 parts of methyl vinyl silicone rubber with a dimethyl vinyl end capping, the molecular weight of 65 ten thousand and the vinyl molar content of 0.08 percent;
5 parts of methyl vinyl silicone rubber which is end-capped by dimethyl vinyl, has the molecular weight of 55 ten thousand and the molar content of vinyl of 3.0 percent;
the specific surface area is 250m 2 30 parts of hydrophobic fumed silica per gram;
30 parts of superfine aluminum hydroxide powder with the particle size of 0.5-1.5 mu m;
0.5 part of platinum complex with the platinum content of 2000ppm and 0.3 part of benzotriazole;
5 parts of vinyl hydroxyl silicone oil with the viscosity of 30cst, wherein the content of vinyl is 5 percent based on the total weight of the hydroxyl vinyl silicone oil; 1 part of vinyl silane coupling agent; 1 part of bis (2, 5-dimethyl-2, 5-di-tert-butylperoxy hexane); 0.3 part of zinc stearate.
The structural formula of the vinyl hydroxyl silicone oil is shown as the formula (1):
wherein: me is methyl, vi is vinyl, m is the number of methyl links, n is the number of vinyl links, m =8-20, n =1-10, and m + n is less than or equal to 30.
Example 4
This example provides a high tear resistant flame retardant silicone rubber composition, which differs from example 1 only in that: the composition of this example comprises the following components:
95 parts of methyl vinyl silicone rubber which is end-capped by dimethyl vinyl, has the molecular weight of 65 ten thousand and the molar content of vinyl of 0.08 percent;
5 parts of methyl vinyl silicone rubber which is end-capped by dimethyl vinyl, has the molecular weight of 55 ten thousand and the molar content of vinyl of 3.0 percent;
the specific surface area is 200m 2 30 parts of hydrophobic fumed silica per gram;
20 parts of superfine aluminum hydroxide powder with the particle size of 0.5-1.5 mu m;
0.5 part of platinum complex with the platinum content of 2000ppm and 0.3 part of benzotriazole;
4 parts of vinyl hydroxyl silicone oil with the viscosity of 35cst, wherein the content of vinyl is 5 percent based on the total weight of the hydroxyl vinyl silicone oil; 2 parts of vinyl silicone resin; 1 part of bis (2, 5-dimethyl-2, 5-di-tert-butylperoxy hexane); 0.1 part of zinc stearate.
The structural formula of the vinyl hydroxyl silicone oil is shown as the formula (1):
wherein: me is methyl, vi is vinyl, m is the number of methyl links, n is the number of vinyl links, m =8-20, n =1-10, and m + n is less than or equal to 30.
Test example
In this test example, the silicone rubber flame retardant adhesive compositions obtained in examples 1 to 4 were subjected to performance tests, and the results are shown in table 1.
Testing the dielectric constant and the dielectric loss tangent value of the flame-retardant adhesive composition; the obtained silicone rubber flame-retardant rubber composition is tested for flame retardance according to the national standard with the standard number GB/T10707-2008. The results are shown in table 1:
table 1 examples 1-4 test results
| Item | Example 1 | Example 2 | Example 3 | Example 4 |
| Hardness, A | 60 | 58 | 62 | 65 |
| Density, g/cm 3 | 1.32 | 1.35 | 1.36 | 1.34 |
| Tensile strength, MPa | 8.5 | 8.9 | 8.2 | 8.0 |
| Tear strength, kN/m | 45.3 | 42.6 | 47.5 | 40.3 |
| Elongation percentage of% | 450 | 405 | 410 | 415 |
| Volume resistivity, Ω · cm | 3×10 15 | 2.5×10 15 | 4.5×10 15 | 3.2×10 15 |
| Dielectric strength, kV/mm | 29 | 28 | 28 | 29 |
| Dielectric constant (50 Hz) | 3.8 | 3.8 | 3.8 | 3.9 |
| Dielectric loss Angle (tan. Delta.) | 2×10 -2 | 3×10 -2 | 1.5×10 -2 | 4×10 -2 |
| Flame retardant grade | FV-0 | FV-0 | FV-0 | FV-0 |
As can be seen from Table 1, the high-tear-resistance silicone rubber flame retardant adhesive composition provided by the invention has good physical and mechanical properties, flame retardant properties and insulating properties.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (10)
1. The high-tear-resistance flame-retardant silicone rubber composition is characterized by comprising the following components:
30-70 parts of methyl vinyl silicone rubber;
10-25 parts of white carbon black;
10-40 parts of a flame retardant;
1-5 parts of a functional auxiliary agent;
0-6 parts of high tear resistance auxiliary agent;
2-5 parts of a structural control agent;
0.05-0.5 part of internal mold release agent;
0-1 part of vulcanizing agent.
2. The high tear flame retardant silicone rubber composition according to claim 1,
the methyl vinyl silicone rubber is compounded by a first methyl vinyl silicone rubber and a second methyl vinyl silicone rubber in a mass ratio of 95-50; wherein, the mol content of vinyl in the first methyl vinyl silicone rubber is 0.03-0.09%, and the molecular weight is 60-75 ten thousand; the second vinyl silicone rubber contains 1.0 to 3.5 mol percent of vinyl and has the molecular weight of 50 to 65 ten thousand;
the white carbon black is fumed white carbon black and/or precipitated white carbon black, and the specific surface area of the white carbon black is not less than 150m 2 /g；
The flame retardant is superfine aluminum hydroxide powder with the particle size of less than 3 mu m;
the structural control agent is at least one of hydroxyl silicone oil, alkoxy silicone oil, vinyl hydroxyl silicone oil, diphenyl silanediol and triphenyl silanol;
the internal mold release agent is stearic acid and/or stearate.
3. The high tear flame retardant silicone rubber composition according to claim 2,
the vinyl hydroxyl silicone oil is hydroxyl-terminated vinyl silicone oil, and the structural formula is shown as the formula (1):
wherein: me is methyl, vi is vinyl, m is the number of methyl links, the number of n vinyl links,
m＝8-20，n＝1-10，m+n≤30；
the content of vinyl is 4-6% by the total weight of the hydroxyl vinyl silicone oil;
the viscosity of the hydroxyl vinyl silicone oil is 30-50 cst.
4. The high tear flame retardant silicone rubber composition according to claim 2, wherein the internal mold release agent is at least one of zinc stearate, magnesium stearate, and calcium stearate.
5. The high tear resistant flame retardant silicone rubber composition according to claim 1, wherein the functional auxiliary agent is at least one of platinum-gold complex, imidazole compound, magnesium aluminum hydrotalcite, zinc borate, cerium oxide, and iron oxide.
6. The high tear flame retardant silicone rubber composition of claim 1, wherein the functional assistant is at least one of hexamethyldisilazane, dimethyldimethoxysilane, dimethyldiethoxysilane, and vinyltriethoxysilane.
7. The high tear flame retardant silicone rubber composition of claim 1,
the high tear-resistant auxiliary agent is a silane coupling agent containing vinyl and/or vinyl silicone resin;
the vulcanizing agent is peroxide bis-di-tetra (2, 4-dichlorobenzoyl peroxide) and/or bis-penta (2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide).
8. The high tear flame retardant silicone rubber composition of claim 7, wherein the high tear aid is at least one of vinyltrimethoxysilane, vinyltriethoxysilane, vinyl silicone resin and tetramethyldivinylsilazane.
9. The method for preparing a high tear-resistant flame retardant silicone rubber composition according to any one of claims 1 to 8, characterized in that the preparation method comprises the steps of:
s1: mixing and kneading the methyl vinyl silicone rubber, the white carbon black, the flame retardant, the structural control agent and the internal release agent until the surface of the obtained rubber material is bright, and carrying out heat treatment on the obtained rubber material;
s2: carrying out high-temperature vacuum banburying treatment and cooling filtration on the rubber material subjected to heat treatment in the step S1 to obtain a banburied rubber;
s3: and mixing the internal mixing rubber and the functional auxiliary agent in an open mill to obtain the high-tear-resistance flame-retardant silicone rubber composition.
10. The method of preparing a high tear flame retardant silicone rubber composition according to claim 9,
in the step S1, the first step is performed,
the mixing temperature is 90-130 ℃;
the temperature of the heat treatment is 120-130 ℃, and the time is 55-65min;
in step S2, the conditions of the high-temperature vacuum banburying treatment include: the temperature is 125-135 ℃, the vacuum degree is-0.06 MPa to-0.08 MPa, and the high-temperature banburying time is 0.5-1.5 h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101157801A (en) * | 2007-09-19 | 2008-04-09 | 上海回天化工新材料有限公司 | Highly ripping-resistant high temperature sulfidation silicon rubber and method for making same |
| WO2017070893A1 (en) * | 2015-10-29 | 2017-05-04 | 国家纳米科学中心 | Ceramic silicone rubber, preparation method and use thereof |
| CN108239402A (en) * | 2018-01-11 | 2018-07-03 | 东爵有机硅(南京)有限公司 | A kind of silicon rubber insulation glue composition and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101157801A (en) * | 2007-09-19 | 2008-04-09 | 上海回天化工新材料有限公司 | Highly ripping-resistant high temperature sulfidation silicon rubber and method for making same |
| WO2017070893A1 (en) * | 2015-10-29 | 2017-05-04 | 国家纳米科学中心 | Ceramic silicone rubber, preparation method and use thereof |
| CN108239402A (en) * | 2018-01-11 | 2018-07-03 | 东爵有机硅(南京)有限公司 | A kind of silicon rubber insulation glue composition and preparation method thereof |
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