CN112521750A - Modified silicone rubber composition and preparation method and application thereof - Google Patents
Modified silicone rubber composition and preparation method and application thereof Download PDFInfo
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 113
- 239000004945 silicone rubber Substances 0.000 title claims abstract description 106
- 239000000203 mixture Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title abstract description 23
- 229920002545 silicone oil Polymers 0.000 claims abstract description 50
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 40
- 239000001257 hydrogen Substances 0.000 claims abstract description 39
- 238000002156 mixing Methods 0.000 claims abstract description 32
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 17
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003085 diluting agent Substances 0.000 claims abstract description 8
- 239000000945 filler Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 8
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 8
- 229920001971 elastomer Polymers 0.000 claims abstract description 6
- -1 ethyl phenylene Chemical group 0.000 claims description 25
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 229920002050 silicone resin Polymers 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 13
- 229920002554 vinyl polymer Polymers 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- GNXAWBMPGLNMOG-UHFFFAOYSA-N C(=C)C([Pt](C)(C)C)C=C Chemical group C(=C)C([Pt](C)(C)C)C=C GNXAWBMPGLNMOG-UHFFFAOYSA-N 0.000 claims description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- BITPLIXHRASDQB-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane Chemical compound C=C[Si](C)(C)O[Si](C)(C)C=C BITPLIXHRASDQB-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 7
- 239000011347 resin Substances 0.000 claims description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 4
- 239000000347 magnesium hydroxide Substances 0.000 claims description 4
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- LAQFLZHBVPULPL-UHFFFAOYSA-N methyl(phenyl)silicon Chemical compound C[Si]C1=CC=CC=C1 LAQFLZHBVPULPL-UHFFFAOYSA-N 0.000 claims description 4
- 150000002825 nitriles Chemical class 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 239000006229 carbon black Substances 0.000 claims description 3
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 claims description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 3
- 229920005560 fluorosilicone rubber Polymers 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000010445 mica Substances 0.000 claims description 3
- 229910052618 mica group Inorganic materials 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
- 230000032683 aging Effects 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 230000002195 synergetic effect Effects 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 11
- 239000003822 epoxy resin Substances 0.000 description 6
- 229920000647 polyepoxide Polymers 0.000 description 6
- 229920004482 WACKER® Polymers 0.000 description 4
- 238000009413 insulation Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 150000003376 silicon Chemical class 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 239000010754 BS 2869 Class F Substances 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 description 1
- RYZGGGMGTVKVLI-UHFFFAOYSA-N [Mo].[CH]1C=CC=C1 Chemical compound [Mo].[CH]1C=CC=C1 RYZGGGMGTVKVLI-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010125 resin casting Methods 0.000 description 1
- 229910021487 silica fume Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
Classifications
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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
-
- 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
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
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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)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a modified silicon rubber composition and a preparation method and application thereof, wherein the modified silicon rubber composition comprises the following components in percentage by weight: 8-40% of modified silicone rubber, 3-10% of hydrogen-containing silicone oil, 4-15% of diluent, 0.5-2% of platinum complex and 40-70% of filler. The preparation method of the modified silicone rubber composition comprises the following steps: mixing the modified silicone rubber and a diluent to obtain a component A; mixing hydrogen-containing silicone oil, a platinum complex and a filler to obtain a component B, and mixing the component A and the component B to obtain the modified silicone rubber composition. The modified silicone rubber and the hydrogen-containing silicone oil have synergistic effect in fire resistance, so that the temperature resistance grade of the modified silicone rubber composition can reach C level (220 ℃), and the modified silicone rubber composition has good heat conduction, aging resistance and no moisture absorption, and is suitable for the field of rubber materials for dry transformers.
Description
Technical Field
The invention belongs to the field of rubber materials for dry transformers, and relates to a modified silicone rubber composition, and a preparation method and application thereof.
Background
China is the country with the largest dry-type transformer production and sales in the world. A common insulation method of the dry-type transformer is epoxy resin casting. CN107674380A discloses a method for manufacturing epoxy resin for dry-type transformer, comprising the following steps: 100 parts of modified epoxy resin, 150-270 parts of organic solvent, 25-40 parts of pentaerythritol triacrylate, 17-30 parts of dodecyl dimethyl tertiary amine, 0.1-1 part of bis (cyclopentadienyl molybdenum tricarbonyl), 15-23 parts of zinc phosphate, 7-13 parts of silicon powder, 0.6-1.2 parts of flame retardant and 0.3-1.8 parts of plasticizer are mixed according to parts by weight, heat treatment is carried out at the temperature of 140-150 ℃, and then cooling and grinding are carried out to prepare the dry-type transformer epoxy resin. The invention has the advantages that: the prepared dry-type transformer epoxy resin has good insulating property, good heat resistance and small influence of electrothermal aging. However, the dry-type transformer poured by epoxy resin has poor heat transfer capability, is easy to age and absorb moisture, and the insulation temperature level can only reach B level (130 ℃) and F level (155 ℃), and needs to be further improved.
Therefore, in the field, development of a modified silicone rubber composition for a dry type transformer, which has good heat conductivity, aging resistance, no moisture absorption and higher temperature resistance level, is desired.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a modified silicone rubber composition, and a preparation method and application thereof. The modified silicone rubber and the hydrogen-containing silicone oil have synergistic effect in fire resistance, so that the temperature resistance grade of the modified silicone rubber composition can reach C level (220 ℃), and the modified silicone rubber composition has good heat conduction, aging resistance and no moisture absorption, and is suitable for the field of rubber materials for dry transformers.
In order to achieve the purpose, the invention adopts the following technical scheme:
in one aspect, the invention provides a modified silicone rubber composition, which comprises the following components in percentage by weight:
in the invention, the cross-linked body of the modified silicon rubber and the hydrogen-containing silicone oil is a high-molecular main material for realizing C-level fire resistance, the diluent is used for reducing the viscosity of the silicon rubber and facilitating the silicon rubber to effectively permeate into gaps of wires and cables, the platinum complex is a catalyst, and the filler plays roles in heat dissipation and mechanical property enhancement.
In the present invention, among the components of the modified silicone rubber composition, the modified silicone rubber may be used in an amount of 8%, 15%, 20%, 25%, 30%, 35%, 40%, or the like.
In the present invention, the hydrogen-containing silicone oil may be used in an amount of 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, or the like, among the components of the modified silicone rubber composition.
In the present invention, among the components of the modified silicone rubber composition, the diluent may be used in an amount of 4%, 8%, 10%, 12%, 14%, 15%, or the like.
In the present invention, the amount of the platinum complex used in the components of the modified silicone rubber composition may be 0.5%, 0.8%, 1%, 1.2%, 1.5%, 2%, or the like.
In the present invention, the filler may be used in an amount of 40%, 50%, 55%, 60%, 65%, 70%, or the like, among the components of the modified silicone rubber composition.
In the invention, the preparation method of the modified silicone rubber comprises the following steps: adding silicon resin and room temperature vulcanized silicone rubber into an extruder, and mixing and extruding under the protection of nitrogen to obtain the modified silicone rubber.
In the invention, the preparation method of the silicone resin comprises the following steps: adding tetramethyl divinyl disiloxane and tetraethoxysilane (such as Si40) into an aqueous solution containing a catalyst, reacting for 2-4 h (such as 2h, 3h or 4 h) at 70-90 ℃ (such as 70 ℃, 75 ℃, 80 ℃ or 90 ℃ and the like), and then adding toluene for reflux reaction to obtain the silicon resin.
Preferably, the catalyst is hydrochloric acid.
Preferably, the concentration of the hydrochloric acid in the aqueous solution is 20% to 36.5%, such as 20%, 25%, 30%, 36.5%, etc., in terms of its solute.
Preferably, the amount of the tetraethoxysilane added is 30 to 40g, for example, 30g, 32g, 35g, 38g, 40g or the like, relative to 40g of tetramethyldivinyldisiloxane.
Preferably, the time of the reflux reaction is 1-3 h, such as 1h, 2h or 3 h.
In the preparation method of the modified silicone rubber, the room temperature vulcanized silicone rubber is any one or a combination of at least two of dimethyl silicone rubber, methyl vinyl silicone rubber, methyl phenyl silicone rubber, fluorosilicone rubber, nitrile silicone rubber, ethyl silicone rubber or ethyl phenylene silicone rubber. Combinations of the at least two, such as dimethyl silicone rubber and methyl vinyl silicone rubber, methylphenyl silicone rubber and fluoro silicone rubber, nitrile silicone rubber, and the like.
In the preparation method of the modified silicone rubber, the amount of the silicone resin is 20-60 g, such as 20g, 30g, 40g, 50g or 60g, relative to 100g of room temperature vulcanized silicone rubber.
Preferably, the temperature of the mixing extrusion is 50-80 ℃, for example, 50 ℃, 60 ℃, 70 ℃ or 80 ℃.
Preferably, the mixing and extruding time is 5-30 min, such as 5min, 10min, 15min, 20min or 30 min.
In the invention, the hydrogen-containing silicone oil is any one of methyl hydrogen-containing silicone oil, phenyl hydrogen-containing silicone oil or methyl phenyl hydrogen-containing silicone oil or the combination of at least two of methyl hydrogen-containing silicone oil, phenyl hydrogen-containing silicone oil and methyl phenyl hydrogen-containing silicone oil. Combinations of at least two of the foregoing, for example, methyl hydrogen-containing silicone oil and phenyl hydrogen-containing silicone oil, and methylphenyl hydrogen-containing silicone oil and the like.
Preferably, the hydrogen content of the hydrogen-containing silicone oil is 1-10%, such as 1%, 3%, 5% or 10%.
In the present invention, the diluent is a vinyl liquid silicone oil.
Preferably, the viscosity of the vinyl liquid silicone oil is 500 to 2000 pas, for example, 500 pas, 1000 pas, 1500 pas, 2000 pas, or the like.
In the present invention, the platinum complex is a divinyltetramethyl platinum complex.
Preferably, the filler is any one or a combination of at least two of silica micropowder, white carbon black, mica powder, quartz powder, kaolin, calcium carbonate, alumina, aluminum hydroxide or magnesium hydroxide. Combinations of the at least two, such as silica fume and white carbon black, mica powder and quartz powder, kaolin and calcium carbonate, alumina, and the like.
In another aspect, the present invention provides a method for preparing the modified silicone rubber composition as described above, the method comprising: mixing the modified silicone rubber and a diluent to obtain a component A; mixing hydrogen-containing silicone oil, a platinum complex and a filler to obtain a component B, and mixing the component A and the component B to obtain the modified silicone rubber composition.
In the invention, the component A and the component B need to be prepared and used as before, if the components are mixed in advance, the modified silicone rubber and the hydrogen-containing silicone oil can be crosslinked slowly, and the use effect is influenced; the modified silicone rubber and the hydrogen-containing silicone oil have a synergistic effect in realizing C-level fire resistance.
In a further aspect, the present invention provides the use of a modified silicone rubber composition as described above in a rubber material for a dry transformer.
Compared with the prior art, the invention has the following beneficial effects:
the modified silicone rubber and the hydrogen-containing silicone oil have a synergistic effect in fire resistance, so that the temperature resistance grade of the modified silicone rubber composition can reach the C level, and the modified silicone rubber composition also has the properties of good heat conduction, aging resistance, no moisture absorption and the like, and is suitable for the field of rubber materials for dry transformers.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
In this embodiment, a modified silicone rubber composition is provided, which comprises the following components in percentage by weight:
wherein the methyl hydrogen-containing silicone oil is purchased from Sancheng science and technology Limited and has the model of SDA 3211; the vinyl liquid silicone oil is purchased from Cheng Dasci Co Ltd, and has a model number of SDA 3222; divinyltetramethyl platinum complexes were purchased from wacker, germany; silica micropowder was purchased from Xin atlas powder Co.
The preparation method of the modified silicone rubber comprises the following steps: adding 30g of silicon resin and 100g of dimethyl silicone rubber into an extruder, and mixing and extruding for 20min at 60 ℃ under the protection of nitrogen to obtain the modified silicone rubber.
The preparation method of the silicone resin comprises the following steps: 40g of tetramethyldivinyldisiloxane and 35g of Si40 were added to an aqueous solution containing hydrochloric acid (concentration: 20%), and reacted at 75 ℃ for 4 hours, followed by reflux reaction with toluene for 2 hours to obtain the silicone resin.
The preparation method of the modified silicone rubber composition comprises the following steps: mixing the modified silicone rubber and vinyl liquid silicone oil to obtain a component A; and mixing methyl hydrogen-containing silicone oil, divinyl tetramethyl platinum complex and silicon micropowder to obtain a component B, and mixing the component A and the component B to obtain the modified silicone rubber composition.
Example 2
In this embodiment, a modified silicone rubber composition is provided, which comprises the following components in percentage by weight:
the phenyl hydrogen-containing silicone oil is purchased from Sancheng science and technology Limited and has the model of SDA 3212; the vinyl liquid silicone oil is purchased from Cheng Dasci Co Ltd, and has a model number of SDA 3221; divinyltetramethyl platinum complexes were purchased from wacker, germany; quartz powder was purchased from Xin atlas powder, Inc.
The preparation method of the modified silicone rubber comprises the following steps: adding 20g of silicone resin and 100g of methyl phenyl silicone rubber into an extruder, and mixing and extruding for 30min at 50 ℃ under the protection of nitrogen to obtain the modified silicone rubber.
The preparation method of the silicone resin comprises the following steps: 40g of tetramethyldivinyldisiloxane and 30g of Si40 were added to an aqueous solution containing hydrochloric acid (concentration: 36.5%), and reacted at 90 ℃ for 3 hours, followed by reflux reaction with toluene for 1 hour to obtain the silicone resin.
The preparation method of the modified silicone rubber composition comprises the following steps: mixing the modified silicone rubber and vinyl liquid silicone oil to obtain a component A; and mixing phenyl hydrogen-containing silicone oil, a divinyl tetramethyl platinum complex and quartz powder to obtain a component B, and mixing the component A and the component B to obtain the modified silicone rubber composition.
Example 3
In this embodiment, a modified silicone rubber composition is provided, which comprises the following components in percentage by weight:
the methyl phenyl hydrogen-containing silicone oil is purchased from Sancheng science and technology Limited and has the model of SDA 3213; the vinyl liquid silicone oil is purchased from Cheng Dasci Co Ltd, and has a model number of SDA 3224; divinyltetramethyl platinum complexes were purchased from wacker, germany; alumina was purchased from zibo ribokang.
The preparation method of the modified silicone rubber comprises the following steps: adding 50g of silicon resin and 100g of nitrile silicon rubber into an extruder, and mixing and extruding for 5min at 80 ℃ under the protection of nitrogen to obtain the modified silicon rubber.
The preparation method of the silicone resin comprises the following steps: 40g of tetramethyldivinyldisiloxane and 35g of Si40 were added to an aqueous solution containing hydrochloric acid (concentration: 30%), and reacted at 70 ℃ for 2 hours, followed by reflux reaction with toluene for 3 hours to obtain the silicone resin.
The preparation method of the modified silicone rubber composition comprises the following steps: mixing the modified silicone rubber and vinyl liquid silicone oil to obtain a component A; and mixing methyl phenyl hydrogen-containing silicone oil, a divinyl tetramethyl platinum complex and alumina to obtain a component B, and mixing the component A and the component B to obtain the modified silicone rubber composition.
Example 4
In this embodiment, a modified silicone rubber composition is provided, which comprises the following components in percentage by weight:
wherein the methyl hydrogen-containing silicone oil is purchased from Sancheng science and technology Limited and has the model of SDA 3211-2; the vinyl liquid silicone oil is purchased from Cheng Dasci Co Ltd, and has a model number of SDA 3223; divinyltetramethyl platinum complexes were purchased from wacker, germany; magnesium hydroxide was purchased from Yingxin chemical industry.
The preparation method of the modified silicone rubber comprises the following steps: adding 60g of silicon resin and 100g of ethyl silicone rubber into an extruder, and mixing and extruding for 10min at 70 ℃ under the protection of nitrogen to obtain the modified silicone rubber.
The preparation method of the silicone resin comprises the following steps: 40g of tetramethyldivinyldisiloxane and 40g of Si40 were added to an aqueous solution containing hydrochloric acid (concentration: 25%), and reacted at 80 ℃ for 3 hours, followed by reflux reaction with toluene for 2 hours to obtain the silicone resin.
The preparation method of the modified silicone rubber composition comprises the following steps: mixing the modified silicone rubber and vinyl liquid silicone oil to obtain a component A; and mixing methyl hydrogen-containing silicone oil, a divinyl tetramethyl platinum complex and magnesium hydroxide to obtain a component B, and mixing the component A and the component B to obtain the modified silicone rubber composition.
Comparative example 1
This comparative example is different from example 1 only in that, in the preparation method of the modified silicone rubber composition, the modified silicone rubber composition was obtained by mixing together the modified silicone rubber, the vinyl liquid silicone oil, the methyl hydrogen-containing silicone oil, the divinyltetramethylplatinum complex, and the fine silicon powder.
Comparative example 2
This comparative example is different from example 1 only in that the modified silicone rubber was replaced with the same amount of silicone resin, and the remaining raw materials, the method of preparing the silicone resin, and the like were the same as example 1.
Comparative example 3
This comparative example differs from example 1 only in that methyl hydrogen silicone oil was not included in the modified silicone rubber composition, and the amount of the modified silicone rubber was 43%.
The modified silicone rubber compositions of examples 1 to 4 and comparative examples 1 to 3 were subjected to performance tests as follows:
(1) the thermal conductivity was tested according to astm d 5470;
(2) tensile strength and elongation at break were tested according to the methods of GB/T528-;
(3) the dielectric constant is measured by a dielectric property tester;
(4) the temperature resistance is measured by thermogravimetric analyzer test.
The results of the performance tests are shown in table 1.
TABLE 1
Coefficient of thermal conductivity W/m.k | Tensile strength MPa | Elongation at break% | Dielectric constant | Temperature resistant grade | |
Example 1 | 0.65 | 3.3 | 230 | 2.85 | Class C |
Example 2 | 0.71 | 3.4 | 260 | 2.91 | Class C |
Example 3 | 0.63 | 3.3 | 240 | 2.88 | Class C |
Example 4 | 0.68 | 3.5 | 235 | 2.93 | Class C |
Comparative example 1 | 0.43 | 2.1 | 200 | 3.01 | Class F |
Comparative example 2 | 0.31 | 1.6 | 140 | 3.31 | Class A |
Comparative example 3 | 0.11 | 1.1 | 160 | 4.24 | Can not reach A grade |
As can be seen from Table 1, the modified silicone rubber composition has the advantages of high thermal conductivity coefficient (more than 0.63W/m.k), high tensile strength (more than 3.3 Mpa), high elongation at break (more than 230%), low dielectric constant (less than 2.93) and temperature resistance grade reaching C level. The temperature-resistant grades are Y A, E, B, F, H and C from low to high. In comparative example 3, since a crosslinked system could not be formed, it could not be used as an insulating and temperature-resistant material.
The applicant states that the present invention is illustrated by the above examples of the modified silicone rubber composition of the present invention and the method of preparing the same, but the present invention is not limited to the above examples, that is, it does not mean that the present invention must be practiced by relying on the above examples. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
2. the modified silicone rubber composition according to claim 1, wherein the modified silicone rubber is prepared by: adding silicon resin and room temperature vulcanized silicone rubber into an extruder, and mixing and extruding under the protection of nitrogen to obtain the modified silicone rubber.
3. The modified silicone rubber composition according to claim 2, wherein the silicone resin is prepared by a method comprising: adding tetramethyl divinyl disiloxane and ethyl orthosilicate into an aqueous solution containing a catalyst, reacting for 2-4 hours at 70-90 ℃, and then adding toluene for reflux reaction to obtain the silicon resin;
preferably, the catalyst is hydrochloric acid;
preferably, the concentration of the hydrochloric acid in the aqueous solution is 20-36.5% by the solute;
preferably, the adding amount of the tetraethoxysilane is 30-40 g relative to 40g of tetramethyl divinyl disiloxane;
preferably, the time of the reflux reaction is 1-3 h.
4. The modified silicone rubber composition according to claim 2, wherein the room temperature vulcanizing silicone rubber is any one of or a combination of at least two of a dimethyl silicone rubber, a methyl vinyl silicone rubber, a methylphenyl silicone rubber, a fluorosilicone rubber, a nitrile silicone rubber, an ethyl silicone rubber, or an ethyl phenylene silicone rubber.
5. The modified silicone rubber composition according to claim 2, wherein the amount of the silicone resin is 20 to 60g relative to 100g of the room-temperature vulcanized silicone rubber;
preferably, the temperature of the mixing extrusion is 50-80 ℃;
preferably, the mixing and extruding time is 5-30 min.
6. The modified silicone rubber composition according to any one of claims 1 to 5, wherein the hydrogen-containing silicone oil is any one of methyl hydrogen-containing silicone oil, phenyl hydrogen-containing silicone oil, or methylphenyl hydrogen-containing silicone oil, or a combination of at least two of them;
preferably, the hydrogen content of the hydrogen-containing silicone oil is 1-10%.
7. The modified silicone rubber composition according to any one of claims 1 to 6, wherein the diluent is a vinyl liquid silicone oil;
preferably, the viscosity of the vinyl liquid silicone oil is 500-2000 Pa-s.
8. The modified silicone rubber composition according to any one of claims 1 to 7, wherein the platinum complex is a divinyltetramethyl platinum complex;
preferably, the filler is any one or a combination of at least two of silica micropowder, white carbon black, mica powder, quartz powder, kaolin, calcium carbonate, alumina, aluminum hydroxide or magnesium hydroxide.
9. The method for producing the modified silicone rubber composition according to any one of claims 1 to 8, characterized in that the production method is: mixing the modified silicone rubber and a diluent to obtain a component A; mixing hydrogen-containing silicone oil, a platinum complex and a filler to obtain a component B, and mixing the component A and the component B to obtain the modified silicone rubber composition.
10. Use of the modified silicone rubber composition according to any one of claims 1 to 8 in a rubber material for a dry transformer.
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CN105238069A (en) * | 2015-11-17 | 2016-01-13 | 江苏天辰新材料股份有限公司 | Halogen-free non-dripping two-component addition type flame retardant silicone rubber and preparation method thereof |
CN111909519A (en) * | 2020-07-27 | 2020-11-10 | 深圳市新亚新材料有限公司 | Flexible heat-conducting silicon rubber and preparation method and application thereof |
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CN103436018A (en) * | 2013-08-23 | 2013-12-11 | 深圳市鸿富诚屏蔽材料有限公司 | High-toughness ultrathin heat-conducting silica gel gasket and preparation method thereof |
CN105238069A (en) * | 2015-11-17 | 2016-01-13 | 江苏天辰新材料股份有限公司 | Halogen-free non-dripping two-component addition type flame retardant silicone rubber and preparation method thereof |
CN111909519A (en) * | 2020-07-27 | 2020-11-10 | 深圳市新亚新材料有限公司 | Flexible heat-conducting silicon rubber and preparation method and application thereof |
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