CN115246991A - High-strength conductive liquid silicone rubber for cold-shrinkage cable accessory conductive stress cone and preparation method thereof - Google Patents
High-strength conductive liquid silicone rubber for cold-shrinkage cable accessory conductive stress cone and preparation method thereof Download PDFInfo
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- CN115246991A CN115246991A CN202110460121.4A CN202110460121A CN115246991A CN 115246991 A CN115246991 A CN 115246991A CN 202110460121 A CN202110460121 A CN 202110460121A CN 115246991 A CN115246991 A CN 115246991A
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 59
- 239000004944 Liquid Silicone Rubber Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 47
- -1 polysiloxane Polymers 0.000 claims abstract description 42
- 229910021485 fumed silica Inorganic materials 0.000 claims abstract description 41
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 41
- 239000011231 conductive filler Substances 0.000 claims abstract description 38
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 27
- 229920001971 elastomer Polymers 0.000 claims abstract description 25
- 239000003054 catalyst Substances 0.000 claims abstract description 18
- 239000003112 inhibitor Substances 0.000 claims abstract description 15
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 15
- 239000004945 silicone rubber Substances 0.000 claims abstract description 15
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000000806 elastomer Substances 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims description 40
- 239000000203 mixture Substances 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 18
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 14
- 229920002554 vinyl polymer Polymers 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 12
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 10
- 229920002545 silicone oil Polymers 0.000 claims description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 8
- 229910021389 graphene Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000006229 carbon black Substances 0.000 claims description 5
- VOMQDZMRGKGVQT-UHFFFAOYSA-N cyclohex-2-yn-1-ol Chemical compound OC1CCCC#C1 VOMQDZMRGKGVQT-UHFFFAOYSA-N 0.000 claims description 4
- MLRKYSNODSLPAB-UHFFFAOYSA-N hex-1-yn-1-ol Chemical compound CCCCC#CO MLRKYSNODSLPAB-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 3
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000000306 component Substances 0.000 description 60
- 239000005060 rubber Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 11
- 238000001723 curing Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- 238000006459 hydrosilylation reaction Methods 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 239000012756 surface treatment agent Substances 0.000 description 4
- 239000000945 filler Substances 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- MTEZSDOQASFMDI-UHFFFAOYSA-N 1-trimethoxysilylpropan-1-ol Chemical compound CCC(O)[Si](OC)(OC)OC MTEZSDOQASFMDI-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000012763 reinforcing filler Substances 0.000 description 2
- 239000000565 sealant Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- JQZGUQIEPRIDMR-UHFFFAOYSA-N 3-methylbut-1-yn-1-ol Chemical compound CC(C)C#CO JQZGUQIEPRIDMR-UHFFFAOYSA-N 0.000 description 1
- 239000004971 Cross linker Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000013006 addition curing Methods 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- SCPWMSBAGXEGPW-UHFFFAOYSA-N dodecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCC[Si](OC)(OC)OC SCPWMSBAGXEGPW-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- KAKZBPTYRLMSJV-UHFFFAOYSA-N vinyl-ethylene Natural products C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 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
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
-
- 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
-
- 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
-
- 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
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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 discloses a high-strength conductive liquid silicone rubber for a cold-contraction cable accessory conductive stress cone, which is prepared by preparing a component A and a component B from the following raw materials in parts by mass, and uniformly mixing the components according to the mass ratio of 1 to obtain the liquid silicone rubber; the component A comprises: 40-60 parts of polysiloxane, 3-8 parts of surface treating agent, 15-20 parts of fumed silica, 1-7 parts of conductive filler and 2-9 parts of platinum catalyst; the component B comprises: 40-60 parts of polysiloxane, 3-8 parts of surface treating agent, 15-20 parts of fumed silica, 1-7 parts of conductive filler, 1-6 parts of cross-linking agent and 1-3 parts of inhibitor. The prepared bi-component addition type high-strength conductive liquid silicone rubber is cured and molded to obtain the silicone rubber elastomer, has excellent physical and mechanical properties and conductivity, and is very suitable for manufacturing conductive stress cones for cold-shrinkable cable accessories of 10kV and above voltage levels.
Description
Technical Field
The invention relates to bi-component addition type high-strength conductive liquid silicone rubber and a preparation method thereof, and the prepared conductive liquid silicone rubber is a rubber material for a conductive stress cone of a cold-contraction cable accessory, belonging to the field of organosilicon materials used for cable accessories.
Background
The stress cone made of conductive liquid silicon rubber is embedded in the cold-contraction cable accessory and is a core component of the cold-contraction cable accessory, and the stress cone has the main function of homogenizing the electric field distribution of the wires and preventing discharge caused by overhigh local field intensity. Generally speaking, the stress cone requires good conductivity of the cured conductive liquid silicone rubber, and the volume resistivity of the stress cone is stable to 10-50 Ω · cm; and maintains good physical and mechanical properties to meet the requirements of expansion and retraction of cold-shrink cable accessories, and simultaneously has the requirements of controllable curing speed and good storage stability.
The prior patent document CN101787212A discloses a low-modulus and high-strength room temperature vulcanized conductive silicone rubber, which comprises the following components in parts by weight: 100 portions of raw silicon rubber, 10 to 30 portions of conductive filler, 2 to 5 portions of cross linker and 0.2 to 2 portions of catalyst are mixed, molded and pressed. The patent provides two embodiments of condensation type room temperature curing and addition type room temperature curing, wherein in the embodiment of a condensation type curing system, the tearing strength of rubber materials is lower than 30kN/m, and the requirement of a conductive stress cone for cold-shrink cable accessories on high tearing strength (more than or equal to 35 kN/m) is difficult to meet; while the examples of addition cure systems do not provide specific test data.
The prior patent document CN107325748A discloses a graphene-doped two-component conductive organosilicon sealant and a preparation method thereof, and the sealant is composed of two components: the component one is base paste composed of liquid vinyl polysiloxane raw rubber, reinforcing agent, conductive filler, catalyst, inhibitor and diluent, and the component two is cross-linking agent. In the patent embodiment, the conductive performance of the rubber material is excellent (the volume resistivity is 0.001-0.008 omega. Cm), but the physical and mechanical properties are poor, the tensile strength is only 1.2-2.0 MPa, and the requirement of the conductive stress cone for cold-shrink cable accessories on high strength cannot be met.
The prior patent document CN110003664A discloses a liquid conductive silicone rubber, and a preparation method and application thereof. The liquid conductive silicone rubber is prepared from the following raw materials in parts by weight: 25 to 30 portions of gas phase white carbon black, 100 to 110 portions of vinyl-terminated silicone oil, 37.4 to 50.8 portions of surface treating agent, 210 to 230 portions of conductive filler, 8 to 11 portions of hydrogen-containing silicone oil, 0.15 to 0.3 portion of inhibitor and 0.15 to 0.3 portion of catalyst. Wherein the surface treating agent comprises gamma-glycidoxypropyltrimethoxysilane, hexamethyldisilazane, dodecyltrimethoxysilane, vinyltriethoxysilane and tetramethyltetravinylsiloxane. In the data of the patent embodiment, the tensile strength of the rubber material is less than 2MPa, and the rubber material can only be applied to the occasions of sealing and filling of electronic devices and the like, and is difficult to be applied to the manufacture of the conductive stress cone for cold-shrink cable accessories.
In summary, no related inventions or research reports about the bi-component addition type high-strength conductive liquid silicone rubber suitable for the conductive stress cone of the cold-shrink cable accessory exist so far, and the current conductive silicone rubber material applied to the conductive stress cone of the cold-shrink cable accessory has excellent conductive performance and cannot simultaneously meet the requirements of the conductive stress cone on physical and mechanical properties, processing performance, curing speed, storage stability and the like.
Disclosure of Invention
The invention aims to solve the problem of poor physical and mechanical properties of conductive silicone rubber in the prior art, and provides high-strength conductive liquid silicone rubber for a cold-contraction cable accessory conductive stress cone.
The invention is realized by the following technical scheme: a high-strength conductive liquid silicone rubber for a cold-shrinkage cable accessory conductive stress cone is prepared by preparing a component A and a component B from the following raw materials in parts by mass, and uniformly mixing the components according to the mass ratio of 1 to obtain the liquid silicone rubber, wherein the silicone rubber meets the following performance indexes: volume resistivity is less than or equal to 50 omega-cm, and tearing strength is more than or equal to 35 kN-m -1 The tensile strength is more than or equal to 7MPa, and the elongation at break is more than or equal to 600 percent;
the component A comprises: 40-60 parts of polysiloxane, 3-8 parts of surface treating agent, 15-20 parts of fumed silica, 1-7 parts of conductive filler and 2-9 parts of platinum catalyst;
the component B comprises: 40-60 parts of polysiloxane, 3-8 parts of surface treating agent, 15-20 parts of fumed silica, 1-7 parts of conductive filler, 1-6 parts of cross-linking agent and 1-3 parts of inhibitor.
The polysiloxane is selected from linear polysiloxane with viscosity of 8-80Pa.s and vinyl content of 0.08-1%.
The surface treating agent is selected from two or three mixtures of silazane, vinyl triethoxysilane, hydroxy silicone oil and gamma-glycidoxypropyltrimethoxysilane.
The fumed silica is selected from fumed silica with the specific surface area of 300m 2 Fumed silica/g, specific surface area 380m 2 One or a mixture of two of the gas phase white carbon black.
The conductive filler is a mixture consisting of 80wt% of conductive carbon black and 20wt% of graphene.
The platinum catalyst is a complex of chloroplatinic acid and hexamethyldivinyl siloxane.
The cross-linking agent is selected from linear polysiloxane with the content of hydrosilyl of 0.5-0.8%.
The inhibitor is selected from alkynols containing at least one unsaturated bond and derivatives thereof; for example, one or two of methyl butynol, hexynol and cyclohexynol.
The invention also provides a preparation method of the high-strength conductive liquid silicone rubber for the cold-contraction cable accessory conductive stress cone, which comprises the following steps:
a. preparation of component A
Adding polysiloxane and a surface treating agent into a kneader according to parts by weight, uniformly stirring, then adding fumed silica in batches, adding a conductive filler after the fumed silica is stirred into a mass, heating the material to 150 ℃ after the conductive filler is agglomerated, starting a vacuum system when the material reaches 150 ℃, keeping the vacuum degree less than or equal to-0.09 MPa, continuously stirring for 3 hours under the condition, and cooling to room temperature; transferring the material to a three-roll grinder for grinding, transferring the material to a planetary stirrer after grinding, adding a platinum catalyst, and uniformly stirring to obtain a component A;
b. preparation of component B
Adding polysiloxane and a surface treating agent into a kneader according to parts by weight, uniformly stirring, then adding fumed silica in batches, adding a conductive filler after the fumed silica is stirred into a mass, heating the material to 150 ℃ after the conductive filler is agglomerated, starting a vacuum system when the material reaches 150 ℃, keeping the vacuum degree less than or equal to-0.09 MPa, continuously stirring for 3 hours under the condition, and cooling to room temperature; transferring the material to a three-roller grinder for grinding, transferring the material to a planetary stirrer after grinding, adding a cross-linking agent and an inhibitor, and uniformly stirring to obtain a component B;
c. preparation of Silicone rubber Elastomers
And (B) uniformly mixing the component A prepared in the step a and the component B prepared in the step B according to the mass ratio of 1.
The high-strength conductive liquid silicone rubber prepared by the invention can be used in the fields of conductive stress cones for cold-shrinkable cable accessories in voltage class of 10kV and above, conductive spraying and the like.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) The invention introduces fumed silica with high specific surface area (the specific surface area is 300 m) into the existing double-component silicon rubber formula 2 Per g, or 380m 2 The/g) is used as a reinforcing filler, and linear polysiloxane with the content of hydrosilation groups of 0.5-0.8% is selected to optimize a cross-linked network structure, so that the rubber material (A and B double components) has good physical and mechanical properties.
(2) According to the invention, conductive carbon black and graphene are selected as conductive fillers, and are connected to a polysiloxane macromolecular chain through a grafting reaction after surface treatment, and then under the shearing action of a kneading machine and a three-roll grinder, the conductive carbon black and the graphene can effectively form a conductive path in a rubber material, so that the cured liquid silicone rubber shows good conductive performance.
(3) Generally, conductive carbon black often contains a certain amount of impurities such as sulfur, nitrogen, volatile matters, etc., which can significantly affect the activity of the platinum catalyst, and lead to the uncured rubber compound. The surface of the conductive carbon black is subjected to grafting modification by the surface treating agent, and low molecules are removed under the conditions of high temperature (150 ℃) and high vacuum (less than or equal to-0.09 MPa), so that the catalytic activity of the platinum catalyst is ensured, and the rubber material can be quickly cured at the temperature of more than or equal to 100 ℃.
(4) In the preparation process, the fumed silica, the conductive filler, the surface treating agent and the polysiloxane are stirred and mixed by a kneader and perform corresponding chemical reaction under the conditions of high temperature (150 ℃) and high vacuum (less than or equal to-0.09 MPa), firstly, the active groups (such as hydroxyl) on the surfaces of the fumed silica and the conductive filler and the active groups (such as alkoxy, silanol and the like) of the surface treating agent perform coupling reaction, the redundant hydroxyl on the surface of the conductive filler is removed, and the compatibility of the filler and a polysiloxane macromolecular chain is improved; and secondly, functional groups such as vinyl and the like contained in the surface treating agent can be grafted to the surface of the filler, so that the crosslinking density is increased to improve the physical and mechanical properties of the rubber material. The whole process is simple and controllable, and is suitable for large-scale batch production.
(5) The bi-component addition type high-strength conductive liquid silicone rubber prepared by the invention can be quickly cured, the production efficiency is improved, no low molecules are released in the curing process of the rubber material, and the rubber material is safe, environment-friendly, nontoxic and harmless. Meanwhile, due to the good fluidity of the rubber material, the rubber material can be processed and molded into parts with various shapes by a liquid injection molding process, and the operation is simple and quick. In addition, the conductive stress cone has excellent physical and mechanical properties and conductive performance, so that the conductive stress cone is very suitable for manufacturing the conductive stress cone for cold-shrinkable cable accessories for voltage classes of 10kV and above.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1:
the embodiment relates to a high-strength conductive liquid silicone rubber for a cold-contraction cable accessory conductive stress cone, which is prepared by preparing a component A and a component B from the following raw materials in parts by mass, and uniformly mixing the raw materials in a mass ratio of 1:
the component A comprises: 40 parts of linear polysiloxane with the viscosity of 20Pa.s and the vinyl content of 0.5 percent, 3 parts of surface treatment agent (mixture of 2 parts of silazane and 1 part of vinyltriethoxysilane) and the specific surface area of 300m 2 18 parts of fumed silica per gram, 7 parts of conductive filler (a mixture consisting of 80wt% of conductive carbon black and 20wt% of graphene), and 9 parts of platinum catalyst (a complex of chloroplatinic acid and hexamethyl divinyl siloxane);
the component B comprises: 51 parts of polysiloxane with the viscosity of 60Pa.s and the vinyl content of 0.1 percent, 5 parts of surface treating agent (mixture of 2 parts of silazane and 3 parts of vinyltriethoxysilane) and 300m of specific surface area 2 17 parts of fumed silica per gram, 1 part of conductive filler (a mixture composed of 80wt% of conductive carbon black and 20wt% of graphene), 1 part of crosslinking agent (linear polysiloxane with the silicon hydrogen group content of 0.8% in percentage by mass) and 2 parts of inhibitor (cyclohexynol).
The specific preparation method of the high-strength conductive liquid silicone rubber comprises the following steps:
a. preparing a component A: adding polysiloxane and a surface treating agent into a kneader according to parts by weight, uniformly stirring, then adding fumed silica in batches, adding a conductive filler after the fumed silica is stirred into a mass, heating the material to 150 ℃ after the conductive filler is agglomerated, starting a vacuum system when the material reaches 150 ℃, keeping the vacuum degree less than or equal to-0.09 MPa, continuously stirring for 3 hours under the condition, and cooling to room temperature; transferring the material to a three-roll grinder for grinding, transferring the material to a planetary stirrer after grinding, adding a platinum catalyst, and uniformly stirring to obtain a component A;
b. preparing a component B: adding polysiloxane and a surface treating agent into a kneader according to parts by weight, uniformly stirring, then adding fumed silica in batches, adding a conductive filler after the fumed silica is stirred into a mass, heating the material to 150 ℃ after the conductive filler is agglomerated, starting a vacuum system when the material reaches 150 ℃, keeping the vacuum degree less than or equal to-0.09 MPa, continuously stirring for 3 hours under the condition, and cooling to room temperature; transferring the materials to a three-roll grinder for grinding, transferring the materials to a planetary stirrer after grinding, adding a cross-linking agent and an inhibitor, and uniformly stirring to obtain a component B;
c. preparation of Silicone rubber Elastomers
And (B) uniformly mixing the component A prepared in the step a and the component B prepared in the step B according to the mass ratio of 1.
Example 2:
the embodiment relates to a high-strength conductive liquid silicone rubber for a cold-shrinkage cable accessory conductive stress cone, which is prepared by preparing a component A and a component B from the following raw materials in parts by mass and uniformly mixing the components in a mass ratio of 1 to obtain the liquid silicone rubber:
the component A comprises: 50 parts of linear polysiloxane with the viscosity of 60Pa.s and the vinyl content of 0.2 percent, 5 parts of surface treating agent (mixture of 3 parts of hydroxyl silicone oil and 2 parts of gamma-glycidyl ether oxypropyl trimethoxy silane) and the specific surface area of 300m 2 15 parts of fumed silica per gram, 3 parts of conductive filler and 3.5 parts of platinum catalyst;
the component B comprises: 50 parts of linear polysiloxane with the viscosity of 60Pa.s and the vinyl content of 0.3 percent, 3 parts of surface treating agent (a mixture of 2 parts of silazane and 1 part of vinyltriethoxysilane), and the specific surface area of 300m 2 15 parts of fumed silica/g3 parts of electric filler, 2.5 parts of cross-linking agent (linear polysiloxane with the content of 0.7 percent of hydrosilyl group by mass) and 3 parts of inhibitor (cyclohexynol).
The specific preparation method of the high-strength conductive liquid silicone rubber of the embodiment is the same as that of the embodiment 1.
Example 3:
the embodiment relates to a high-strength conductive liquid silicone rubber for a cold-contraction cable accessory conductive stress cone, which is prepared by preparing a component A and a component B from the following raw materials in parts by mass, and uniformly mixing the raw materials in a mass ratio of 1:
the component A comprises: 50 parts of linear polysiloxane with the viscosity of 40Pa.s and the vinyl content of 0.4 percent, 6 parts of surface treating agent (mixture of 2 parts of silazane, 2 parts of vinyl triethoxysilane and 2 parts of hydroxyl silicone oil), and 380m of specific surface area 2 15 parts of fumed silica per gram, 3 parts of conductive filler and 2 parts of platinum catalyst;
the component B comprises: 40 parts of linear polysiloxane with the viscosity of 40Pa.s and the vinyl content of 0.5 percent, 8 parts of surface treating agent (a mixture of 4 parts of silazane and 4 parts of hydroxyl silicone oil), and the specific surface area of 380m 2 15 parts of fumed silica per gram, 5 parts of conductive filler, 6 parts of cross-linking agent (linear polysiloxane with the content of 0.6 percent of hydrosilation group by mass) and 2 parts of methylbutinol.
The specific preparation method of the high-strength conductive liquid silicone rubber of the embodiment is the same as that of the embodiment 1.
Example 4:
the embodiment relates to a high-strength conductive liquid silicone rubber for a cold-contraction cable accessory conductive stress cone, which is prepared by preparing a component A and a component B from the following raw materials in parts by mass, and uniformly mixing the raw materials in a mass ratio of 1:
the component A comprises: 55 parts of linear polysiloxane with the viscosity of 8Pa.s and the vinyl content of 1 percent, 8 parts of surface treatment agent (a mixture of 3 parts of silazane, 3 parts of gamma-glycidyl ether oxypropyltrimethoxysilane and 2 parts of hydroxyl silicone oil), and the specific surface area of the surface treatment agent is 300m 2 20 parts of fumed silica per gram, 4 parts of conductive filler and 5.5 parts of platinum catalyst;
the component B comprises: viscosity of 855 parts of linear polysiloxane with Pa.s and 0.12 percent of vinyl content, 8 parts of surface treating agent (mixture of 4 parts of silazane and 4 parts of hydroxyl silicone oil) and 300m of specific surface area 2 20 parts of fumed silica per gram, 4 parts of conductive filler, 3.5 parts of crosslinking agent (linear polysiloxane with the content of 0.5 percent of hydrosilation group by mass) and 2 parts of inhibitor (a mixture of 1 part of cyclohexylynol and 1 part of hexynol).
The specific preparation method of the high-strength conductive liquid silicone rubber of the embodiment is the same as that of the embodiment 1.
Example 5:
the embodiment relates to a high-strength conductive liquid silicone rubber for a cold-shrinkage cable accessory conductive stress cone, which is prepared by preparing a component A and a component B from the following raw materials in parts by mass and uniformly mixing the components in a mass ratio of 1 to obtain the liquid silicone rubber:
the component A comprises: 60 parts of linear polysiloxane with viscosity of 80Pa.s and vinyl content of 0.08 percent, 4 parts of surface treatment agent (mixture of 2 parts of silazane and 2 parts of hydroxyl silicone oil), and specific surface area of 300m 2 10 parts of fumed silica per gram, and the specific surface area of the fumed silica is 380m 2 10 parts of gas-phase white carbon black per gram, 1 part of conductive filler and 9 parts of platinum catalyst;
the component B comprises: 60 parts of linear polysiloxane with viscosity of 80Pa.s and vinyl content of 0.08%, 5 parts of surface treating agent (mixture of 3 parts of silazane and 3 parts of vinyltriethoxysilane), and specific surface area of 300m 2 10 parts of fumed silica per gram, and the specific surface area of the fumed silica is 380m 2 10 parts of fumed silica per gram, 7 parts of conductive filler, 1 part of crosslinking agent (linear polysiloxane with the content of 0.5 percent of hydrosilation group by mass) and 1 part of inhibitor (hexynol).
The specific preparation method of the high-strength conductive liquid silicone rubber of the embodiment is the same as that of the embodiment 1.
The silicone rubber elastomers obtained in examples 1 to 5 were subjected to product performance tests, and the results are shown in table 1.
According to the data, the bicomponent addition type high-strength conductive liquid silicone rubber prepared by the invention is cured to obtain the silicone rubber elastomer, and the rubber material has good physical and mechanical properties and conductivity: volume resistivity is less than or equal to 50 omega-cm, and tearing strength is more than or equal to 35 kN-m -1 The tensile strength is more than or equal to 7MPa, and the elongation at break is more than or equal to 600 percent.
Comparative example 1:
this comparative example was based on example 2, in which the polysiloxanes in components a and B had a viscosity of 5pa.s, with replacement of the polysiloxanes in components a and B. The other formulation components and preparation method are the same as example 2, and the product performance test is carried out on the silicone rubber elastomer prepared by the comparative example and the example 2, and the result is shown in table 2.
Comparative example 2:
in the comparative example, the fumed silica in the component A and the component B is replaced on the basis of the example 4, and in the comparative example, the specific surface areas of the component A and the component B are 200m 2 The gas phase white carbon black is used as reinforcing filler. The other formulation components and preparation method are the same as in example 4, and the product performance test is carried out on the silicone rubber elastomer prepared in the comparative example and the example 4, and the result is shown in table 3.
Comparative example 3:
in the comparative example, on the basis of example 5, the composition of the conductive filler in the component a and the component B is adjusted, and graphene is omitted. The other formulation components and preparation method are the same as example 5, and the silicone rubber elastomer prepared in the comparative example and example 5 is subjected to product performance test, and the results are shown in Table 4.
As shown in the test data of the comparative examples 1 to 3, in the invention, only by simultaneously introducing polysiloxane with higher viscosity, fumed silica with high specific surface area and conductive filler consisting of 80wt% of conductive carbon black and 20wt% of graphene, the prepared liquid silicone rubber has excellent physical and mechanical properties and conductivity, and can be used for manufacturing the conductive stress cone for cold-shrink cable accessories with voltage level of 10kV or above.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modifications and equivalent variations of the above embodiment according to the technical spirit of the present invention are within the scope of the present invention.
Claims (10)
1. The high-strength conductive liquid silicone rubber for the cold-contraction cable accessory conductive stress cone is characterized in that: the liquid silicone rubber is prepared by preparing a component A and a component B from the following raw materials in parts by mass, and uniformly mixing the components according to the mass ratio of 1: volume resistivity is less than or equal to 50 omega-cm, and tearing strength is more than or equal to 35 kN-m -1 The tensile strength is more than or equal to 7MPa, and the elongation at break is more than or equal to 600 percent;
the component A comprises: 40-60 parts of polysiloxane, 3-8 parts of surface treating agent, 15-20 parts of fumed silica, 1-7 parts of conductive filler and 2-9 parts of platinum catalyst;
the component B comprises: 40-60 parts of polysiloxane, 3-8 parts of surface treating agent, 15-20 parts of fumed silica, 1-7 parts of conductive filler, 1-6 parts of cross-linking agent and 1-3 parts of inhibitor.
2. The high-strength conductive liquid silicone rubber for the cold-shrink cable accessory conductive stress cone as claimed in claim 1, wherein: the polysiloxane is selected from linear polysiloxane with viscosity of 8-80Pa.s and vinyl content of 0.08-1%.
3. The high-strength conductive liquid silicone rubber for the cold-shrink cable accessory conductive stress cone as claimed in claim 1, wherein: the surface treating agent is selected from two or three mixtures of silazane, vinyl triethoxysilane, hydroxy silicone oil and gamma-glycidoxypropyltrimethoxysilane.
4. The high-strength conductive liquid silicone rubber for the cold-shrink cable accessory conductive stress cone as claimed in claim 1, wherein: the fumed silica is selected from fumed silica with the specific surface area of 300m 2 The specific surface area of the fumed silica is 380m 2 One or a mixture of two of the gas phase white carbon black per gram.
5. The high-strength conductive liquid silicone rubber for the cold-shrink cable accessory conductive stress cone as claimed in claim 1, wherein: the conductive filler is a mixture consisting of 80wt% of conductive carbon black and 20wt% of graphene.
6. The high-strength conductive liquid silicone rubber for the cold-shrink cable accessory conductive stress cone as claimed in claim 1, wherein: the platinum catalyst is a complex of chloroplatinic acid and hexamethyldivinyl siloxane.
7. The high-strength conductive liquid silicone rubber for the cold-shrink cable accessory conductive stress cone as claimed in claim 1, wherein: the cross-linking agent is selected from linear polysiloxane with the hydrosilyl group content of 0.5-0.8%.
8. The high-strength conductive liquid silicone rubber for the cold-shrink cable accessory conductive stress cone as claimed in claim 1, wherein: the inhibitor is selected from alkynols containing at least one unsaturated bond and derivatives thereof.
9. The high-strength conductive liquid silicone rubber for the cold-shrink cable accessory conductive stress cone as claimed in claim 1 or 8, wherein: the inhibitor is one or two of methylbutinol, hexynol and cyclohexynol.
10. A method for preparing the high-strength conductive liquid silicone rubber for the conductive stress cone of the cold-shrink cable accessory as claimed in claim 1, which is characterized by comprising the following steps:
a. preparation of component A
Adding polysiloxane and a surface treating agent into a kneader according to parts by weight, uniformly stirring, then adding fumed silica in batches, adding a conductive filler after the fumed silica is stirred into a mass, heating the material to 150 ℃ after the conductive filler is agglomerated, starting a vacuum system when the material reaches 150 ℃, keeping the vacuum degree less than or equal to-0.09 MPa, continuously stirring for 3 hours under the condition, and cooling to room temperature; transferring the material to a three-roll grinder for grinding, transferring the material to a planetary stirrer after grinding, adding a platinum catalyst, and uniformly stirring to obtain a component A;
b. preparation of component B
Adding polysiloxane and a surface treating agent into a kneader according to parts by weight, uniformly stirring, then adding fumed silica in batches, adding a conductive filler after the fumed silica is stirred into a mass, heating the material to 150 ℃ after the conductive filler is agglomerated, starting a vacuum system when the material reaches 150 ℃, keeping the vacuum degree less than or equal to-0.09 MPa, continuously stirring for 3 hours under the condition, and cooling to room temperature; transferring the material to a three-roller grinder for grinding, transferring the material to a planetary stirrer after grinding, adding a cross-linking agent and an inhibitor, and uniformly stirring to obtain a component B;
c. preparation of Silicone rubber Elastomers
And (B) uniformly mixing the component A prepared in the step a and the component B prepared in the step B according to the mass ratio of 1.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116285365A (en) * | 2023-03-30 | 2023-06-23 | 东莞市利群榕兴高分子科技有限公司 | Foaming conductive silicon rubber and preparation method thereof |
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| CN112638993A (en) * | 2018-09-28 | 2021-04-09 | 美国陶氏有机硅公司 | Liquid silicone rubber composition |
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