CN113881232A - Ceramic organic silica gel material for medium-voltage fire-resistant cable and preparation method thereof - Google Patents
Ceramic organic silica gel material for medium-voltage fire-resistant cable and preparation method thereof Download PDFInfo
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- CN113881232A CN113881232A CN202111301690.0A CN202111301690A CN113881232A CN 113881232 A CN113881232 A CN 113881232A CN 202111301690 A CN202111301690 A CN 202111301690A CN 113881232 A CN113881232 A CN 113881232A
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- silica gel
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- resistant cable
- silicone resin
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 239000000741 silica gel Substances 0.000 title claims abstract description 60
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 60
- 230000009970 fire resistant effect Effects 0.000 title claims abstract description 37
- 239000000919 ceramic Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 title abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 39
- 229920002050 silicone resin Polymers 0.000 claims abstract description 35
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 32
- 239000010703 silicon Substances 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 26
- 239000003365 glass fiber Substances 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 16
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000009826 distribution Methods 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 31
- 239000002131 composite material Substances 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 20
- 239000003054 catalyst Substances 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 19
- 239000000178 monomer Substances 0.000 claims description 17
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 14
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 13
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 11
- 229920002379 silicone rubber Polymers 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 8
- 230000004580 weight loss Effects 0.000 claims description 8
- 238000010521 absorption reaction Methods 0.000 claims description 7
- 239000007809 chemical reaction catalyst Substances 0.000 claims description 7
- 238000006482 condensation reaction Methods 0.000 claims description 7
- 239000003921 oil Substances 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000004945 silicone rubber Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000005054 agglomeration Methods 0.000 claims description 5
- 230000002776 aggregation Effects 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000012360 testing method Methods 0.000 claims description 5
- 229910020388 SiO1/2 Inorganic materials 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 4
- 239000011256 inorganic filler Substances 0.000 claims description 4
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 238000002468 ceramisation Methods 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910007161 Si(CH3)3 Inorganic materials 0.000 claims description 2
- 229910020487 SiO3/2 Inorganic materials 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 125000004122 cyclic group Chemical group 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical group [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 229920001843 polymethylhydrosiloxane Polymers 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 238000007142 ring opening reaction Methods 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 239000011800 void material Substances 0.000 claims description 2
- 239000013464 silicone adhesive Substances 0.000 claims 2
- 238000001125 extrusion Methods 0.000 claims 1
- 150000003376 silicon Chemical class 0.000 claims 1
- 239000000853 adhesive Substances 0.000 abstract description 8
- 230000001070 adhesive effect Effects 0.000 abstract description 8
- 239000013013 elastic material Substances 0.000 abstract description 4
- 238000004132 cross linking Methods 0.000 abstract description 3
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 10
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 6
- 238000007731 hot pressing Methods 0.000 description 5
- 238000005086 pumping Methods 0.000 description 5
- 238000004513 sizing Methods 0.000 description 5
- OPKOKAMJFNKNAS-UHFFFAOYSA-N N-methylethanolamine Chemical compound CNCCO OPKOKAMJFNKNAS-UHFFFAOYSA-N 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 239000010445 mica Substances 0.000 description 4
- 229910052618 mica group Inorganic materials 0.000 description 4
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000012671 ceramic insulating material Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- UESSEMPSSAXQJC-UHFFFAOYSA-N ethanol;methanamine Chemical compound NC.CCO UESSEMPSSAXQJC-UHFFFAOYSA-N 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000011148 porous material 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
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 239000004944 Liquid Silicone Rubber Substances 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000012700 ceramic precursor Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- -1 hydrogen siloxane Chemical class 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000008096 xylene Substances 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/46—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes silicones
-
- 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
- C08K2201/003—Additives being defined by their diameter
-
- 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
- C08K2201/004—Additives being defined by their length
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
- Y02A30/14—Extreme weather resilient electric power supply systems, e.g. strengthening power lines or underground power cables
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Organic Insulating Materials (AREA)
Abstract
The invention discloses a ceramic organic silica gel material for a medium-voltage fire-resistant cable and a preparation method thereof, wherein the raw materials comprise 30-70 parts of low-carbon-hydrogen-content methyl silicone resin, 30-70 parts of dimethyl liquid silica gel, 130-300 parts of spherical silica powder, 1-5 parts of a curing agent and 2-10 parts of glass fiber powder, the weight percentage of the carbon-hydrogen component in the formed organic silica gel is within 13%, and the weight percentage of the spherical silica powder is more than 65%. According to the invention, the high-strength elastic material system is formed by crosslinking and curing the methyl silicone resin with low hydrogen content and the dimethyl liquid silica gel, and the powder combination with high bulk density is formed by adopting the nearly spherical silica with multimodal particle size distribution, so that the material has good mechanical and insulating properties at normal temperature, becomes a high-temperature adhesive after high-temperature ceramic, and sinters the silicon micropowder into compact ceramic together with glass fibers to realize high-temperature pressure resistance, thereby greatly reducing the porosity of the ceramic insulating layer, and being suitable for medium-pressure and above cables.
Description
Technical Field
The invention relates to the technical field of conductive materials, in particular to a ceramic organic silica gel material for a medium-voltage fire-resistant cable and a preparation method thereof.
Background
At present, with the increase of high-rise buildings and the improvement of fire-fighting regulations, the maintenance of the operation of electrical equipment during a fire disaster is more and more important for escape and rescue, the fire-resistant performance of the fire-resistant cable as a main infrastructure for connecting all electrical equipment plays an important role in the fire-resistant performance of the high-rise buildings, and the improvement of the heat-resistant temperature and the fire-resistant time of the fire-resistant cable and the normal working range of the cable under different combustion and fire-extinguishing conditions are important directions in the future. Common fire resistant cables are divided into: magnesium oxide mineral insulation fire-resistant cable, mica tape fire-resistant cable and ceramic fire-resistant cable. The magnesium oxide mineral insulated fire-resistant cable is not the mainstream in the future due to the inconvenience of transportation, use and the like; the mica tape fire-resistant cable is mainly applied at low voltage, and the destruction and insulation failure of a mica layer can be caused by the spraying and vibration accompanied with the fire extinguishing in the fire disaster, so that the mica tape fire-resistant cable has huge hidden danger; the ceramic fire-resistant cable is characterized in that an organic ceramic precursor capable of being subjected to ceramic formation is used as an adhesive, such as organic silicon rubber, and is an organic insulating material before a fire disaster occurs, so that the ceramic fire-resistant cable has the advantages of high insulating property, good flexibility, excellent mechanical strength, high and low temperature resistance and the like, ceramics with certain strength are formed after high-temperature ceramic formation, and the high-density ceramic insulating material can bear medium voltage of more than 30 kV. The main indexes influencing the pressure resistance of the ceramic are the components and the porosity of the material, particularly the porosity, and the lowest pressure resistance of vacuum and gas, and in order to resist medium-voltage breakdown, the requirements of improving the compactness and reducing the porosity are inevitable.
Organic compoundsSilica gel has certain cost advantage as the adhesive of the fire-resistant cable, can be quickly converted into a ceramic insulating material at high temperature, has low toxicity or no toxic smoke, and the formed ceramic silicon oxide has low thermal conductivity, is flame-retardant and heat-insulating, has certain mechanical strength after being converted into ceramic, and can ensure that the cable is electrified normally at high temperature. The general silicone rubber has a chemical structure of-SiO (CH)3)2-, loss of (CH) at high temperature3)2SiO is left behind and loses about 40% of its weight in a closed environment, resulting in a SiO density of 2.13g/cm3If the light hydrocarbons are discrete, the volume shrinks by 70%; conversion to SiO in air2The volume shrinkage was reduced, about 64%. The root cause of the volume shrinkage is known from the chemical structure of silicone gum, which is that the proportion of low-density hydrocarbons in the structure is too high, accounting for about 40% of the total weight. In order to reduce the high-temperature shrinkage of the silica gel, a large amount of inorganic filler is added in the formula, and simultaneously, low-melting-point glass powder is also added to increase the high-temperature adhesion. In order to ensure manufacturability and insulation and mechanical properties before ceramization, the volume content of the organic silicon in the silica gel formula needs to exceed 30 percent, even 40 percent, so the ceramized insulation layer has porosity of about 20 percent or even 30 percent of volume ratio, and the high porosity is not suitable for medium-voltage and above cable application.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a ceramic organic silicon adhesive material for a medium-voltage fire-resistant cable, which is prepared by crosslinking and curing methyl silicone resin with low carbon-hydrogen content and dimethyl liquid silica gel to form a high-strength elastic material system, forming a high-bulk-density powder combination by adopting nearly spherical silica with multimodal particle size distribution, so that the material has good mechanical and insulating properties at normal temperature, forming a high-temperature adhesive after high-temperature ceramic, sintering silicon micropowder with glass fibers to compact ceramic to realize high-temperature pressure resistance, and greatly reducing the porosity of an insulating layer after ceramic, and a preparation method thereof.
In order to solve the defects of low organic silica gel ceramic conversion rate, high porosity, insufficient pressure resistance in medium-voltage cable application and the like in the prior art, the invention adopts the following technical scheme: a ceramic organic silica gel for a medium-voltage fire-resistant cable comprises the following raw materials: 30-70 parts of low-hydrocarbon-content methyl silicone resin, 30-70 parts of dimethyl liquid silica gel, 130-300 parts of spherical silica powder, 1-5 parts of a curing agent and 2-10 parts of glass fiber powder; the weight percentage of hydrocarbon components in the formed organic silicon adhesive is within 13 percent, preferably within 9 percent, and the weight percentage of the spherical silicon micro powder is more than 65 percent.
The organic silica gel has the following characteristics: density of>1.6g/cm3The Shore A hardness is 70-85, the tensile strength is better than 5MPa, the elongation at break is more than 70%, and the dielectric strength is more than 20 kV/mm; the weight loss after sintering for 90 minutes at 950 ℃ in the air is not more than 10 percent, the air holes are closed-hole mesopores, and the dielectric strength is better than 10 kV/mm; the volume content of the inorganic filler is more than 50 percent, and the glue density is more than 1.6g/cm3(preferably the inorganic filler is present in an amount of more than 60% by volume and the gum density is more than 1.7g/cm3) The coating has high fluidity, can meet the requirement of an extruder for coating cables, and the fluidity of the glue is the maximum at 70-100 ℃.
The chemical structure of the low-carbon hydrogen content methyl silicone resin is as follows: ((CH)3)3SiO1/2)a(CH3SiO3/2)bHcWherein a, b and c are integers, b/a is more than or equal to 5 and less than or equal to 30, b/c is more than or equal to 10 and less than or equal to 20, a + b + c is more than or equal to 32 and less than or equal to 50, the weight ratio of the content of carbon and hydrogen is less than 30 percent, preferably the content of carbon and hydrogen is less than 27 percent, and the methyl silicone resin can be dissolved in organic solvents such as liquid silica gel, chloroform, ethanol, n-butanol, xylene and the like.
The chemical structure of the dimethyl liquid silica gel is as follows: ((CH)3)3SiO1/2)a((CH3)2SiO)b(CH3C2H2SiO)cHdWherein a, b, c and d are integers, b/a is more than or equal to 50 and less than or equal to 500, b/c is more than or equal to 50 and less than or equal to 500, b/d is more than or equal to 50 and less than or equal to 500, and a + b + c + d is more than or equal to 200 and less than or equal to 2000; or ring-opening of organosilicon monomer D4 and condensation synthesis of vinyl trimethoxy silane are adopted, the weight ratio of organosilicon monomer D4 to vinyl trimethoxy silane is 100: 3 to 10.
The silica gel curing agent is linear or cyclic methyl with low polymerization degreeA complex of a hydrogen siloxane and a catalyst, the linear or cyclic methylhydrogen siloxane of low degree of polymerization being (CH)3)3SiO(CH3HSiO)3Si(CH3)3、 (CH3)3SiO(CH3HSiO)5Si(C2H5)3、(CH3HSiO)4Any one of (a); the catalyst is platinum chloroacid.
The purity of the spherical silicon micro powder is more than 99.5%, the particle size distribution is multimodal, the maximum particle size is less than 50 microns, the D50 is 1-20 microns, and the bulk density is more than 1.3g/cm3Preferably greater than 1.6g/cm3(ii) a The oil absorption is less than 30mL/100g, preferably less than 23mL/100 g.
Preferably, the glass fiber powder used has a diameter of 5 to 20 micrometers and a length of 0.3 to 5 mm.
The production process of the ceramic organic silica gel for the medium-voltage fire-resistant cable comprises the following steps:
step 1: sequentially adding methyl silicone resin, vinyl dimethyl silica gel or an organic silicon monomer D4, vinyl trimethoxy silane and 1 part of 1% aminoethanol solution into a spiral ribbon stirring reaction kettle with a cooling circulator, adding 1 part of deionized water for hydrolysis of methoxyl if the vinyl trimethoxy silane is adopted, taking ammonia as a condensation reaction catalyst, uniformly stirring, adding spherical silicon micropowder, uniformly stirring, adding glass fiber powder, uniformly stirring at the stirring speed of 60-200 rpm, and adding a proper amount of n-butyl alcohol and chloroform to adjust the viscosity to be proper if the viscosity is too high and nonuniform agglomeration occurs;
step 2: heating to 50 ℃, reacting for 3-5 hours, heating to 70-80 ℃, reacting for 5-10 hours until the viscosity reaches 30-50 Pa.s, cooling the gasified catalyst, the organic silicon monomer and the organic solvent in the reaction process, and circulating the cooled catalyst, the organic silicon monomer and the organic solvent back to the reaction kettle;
and step 3: and cooling the reaction kettle to 50 ℃, vacuumizing, drying the catalyst and the solvent, and cooling to room temperature to obtain the silicone resin modified silica powder and liquid silicone rubber solid composite material.
The basic using method comprises the following steps: adding a curing agent into the composite material by using an internal mixer and the like, extruding and coating the surface of the copper cable, and vulcanizing the cable at 130-180 ℃.
When the silica gel test sample piece is prepared, an internal mixer, a double-roller machine or a screw mixer is adopted, the silicon resin modified silica powder and liquid silica gel solid composite material are uniformly mixed with the organic silicon curing agent, and the mixture is extruded into a sheet; hot-press forming on a vulcanizing machine, preparing various test sample pieces by using a stamping method, and measuring tensile strength, pressure resistance and the like.
And (3) heating and ceramizing the shaped sheet in a muffle furnace at 950 ℃ to obtain a ceramic sample, and measuring the mechanical property, the pressure resistance, the void ratio, the density and the like.
According to the invention, the high-strength elastic material system is formed by crosslinking and curing the methyl silicone resin with low hydrogen content and the dimethyl liquid silica gel, and the powder combination with high bulk density is formed by adopting the nearly spherical silica with multimodal particle size distribution, so that the material has good mechanical and insulating properties at normal temperature, and becomes a high-temperature adhesive after high-temperature ceramic, and the high-temperature adhesive and glass fibers sinter the silicon micropowder into compact ceramic to realize high-temperature pressure resistance, and the porosity of the ceramic insulating layer is greatly reduced to below 10%, so that the high-strength elastic material system is suitable for medium-pressure and above cables.
Detailed Description
The present invention is further illustrated by the following specific examples. In the present embodiment, all the parts and percentages are by weight unless otherwise specified. All the raw materials can be purchased from the market or belong to raw materials commonly used in the industry.
Example 1
The preparation of the ceramic organic silica gel for the medium-voltage fire-resistant cable is carried out according to the following process: preparing raw materials: 70 parts of low-hydrocarbon-content methyl silicone resin, 30 parts of dimethyl liquid silica gel, 240 parts of spherical silica powder, 4 parts of curing agent and 5 parts of 2 mm-long glass fiber powder. The silicone resin is solid, and a + b + c in the molecular structure is approximately equal to 40; the a + b + c in the molecular structure of the liquid silica gel is approximately equal to 300, the particle size peak values of the silica powder are respectively 12 microns, 4 microns and 1 micron, and the oil absorption rate is 25mL/100 g. Sequentially adding methyl silicone resin, dimethyl liquid silica gel and 1 part of 1% concentration methylaminoethanol solution into a spiral belt stirring reaction kettle with a cooling circulator, uniformly stirring ammonia which is a condensation reaction catalyst, adding silica micropowder into a system, uniformly stirring, adding glass fiber powder, and uniformly stirring at a stirring speed of 60-200 rpm in the kettle. If the viscosity is too high, uneven agglomeration occurs, and a small amount of n-butanol and chloroform may be added to adjust the viscosity to be appropriate.
And heating the reaction kettle to 50 ℃, reacting for 3-5 hours, heating the temperature of the reaction kettle to 80 ℃, reacting for 5-10 hours until the viscosity reaches 30 pas, and cooling the gasified catalyst and the organic solvent to flow back into the reaction kettle in the whole process. And after the reaction is finished, reducing the temperature of the reaction kettle to 50 ℃, vacuumizing, completely pumping out the catalyst and the solvent from the system, and reducing the temperature to room temperature to obtain the silicone resin and liquid silica gel micropowder solid composite sizing material.
Heating and softening the composite material by using an internal mixer, adding 4 parts of curing agent into the composite material, uniformly mixing, and carrying out hot pressing at 150 ℃ to obtain the silica gel sheet. Measuring its physical and chemical properties, and measuring its density to be 1.76g/cm3The hardness Shore A is 85, the tensile strength is 5.2MPa, the elongation at break is 71 percent, and the dielectric strength is 22 kV/mm. The weight loss of the silica gel sheet after being sintered for 90 minutes at 950 ℃ in the air is 9 percent, the air holes are closed holes and mesopores, and the dielectric strength is 11 kV/mm.
Example 2
The preparation of the ceramic organic silica gel for the medium-voltage fire-resistant cable is carried out according to the following process: 70 parts of low-hydrocarbon-content methyl silicone resin, 30 parts of organic silicon monomer D4 and vinyl trimethoxy silane, 240 parts of spherical silicon micropowder, 1 part of deionized water, 4 parts of curing agent and 5 parts of 2 mm-long glass fiber powder. The silicone resin is solid, a + b + c in the molecular structure of the silicone resin is approximately equal to 40, and the weight ratio of the organosilicon monomer D4 to the vinyltrimethoxysilane is 100: 5, the particle size peak values of the micro powder are respectively 12, 4 and 1 micron, and the oil absorption rate is 25mL/100 g. Methyl silicone resin, an organic silicon monomer D4, vinyl trimethoxy silane, deionized water and 1 part of 1% concentration methylaminoethanol solution are sequentially added into a spiral belt stirring reaction kettle with a cooling circulator, and methylamine is a condensation reaction catalyst and is stirred uniformly. And adding the silicon micropowder into the system, uniformly stirring, adding the glass fiber powder, and uniformly stirring at a stirring speed of 60-200 rpm in the kettle.
And heating the reaction kettle to 50 ℃, reacting for 3-5 hours, heating the temperature of the reaction kettle to 80 ℃, reacting for 5-10 hours until the viscosity reaches 30 pas, and cooling the gasified catalyst and the organic silicon monomer to flow back into the reaction kettle in the whole process. And after the reaction is finished, reducing the temperature of the reaction kettle to 50 ℃, vacuumizing, completely pumping out the catalyst from the system, and cooling to room temperature to obtain the silicone resin and liquid silica gel micropowder solid composite sizing material.
Heating and softening the composite material by using an internal mixer, adding 4 parts of curing agent into the composite material, uniformly mixing, and carrying out hot pressing at 150 ℃ to obtain the silica gel sheet. The physical and chemical properties were measured to find that the density was 1.75g/cm3The Shore A hardness is 83, the tensile strength is 5.3MPa, the elongation at break is 72%, and the dielectric strength is 21 kV/mm. The weight loss of the silica gel sheet after being sintered for 90 minutes at 950 ℃ in the air is 9 percent, the air holes are closed holes and mesopores, and the dielectric strength is 12 kV/mm.
Example 3
The preparation of the ceramic organic silica gel for the medium-voltage fire-resistant cable is carried out according to the following process: 65 parts of low-hydrocarbon-content methyl silicone resin, 35 parts of organic silicon monomer D4 and vinyl trimethoxy silane, 210 parts of spherical silicon powder, 4 parts of curing agent, 1 part of deionized water and 7 parts of 1 mm-long glass fiber powder. The silicone resin is solid, a + b + c in the molecular structure of the silicone resin is approximately equal to 45, and the weight ratio of the organosilicon monomer D4 to the vinyltrimethoxysilane is 100: 5, the peak values of the particle sizes of the silicon micro powder are 15 microns, 5 microns and 2 microns respectively, and the oil absorption rate is 22mL/100 g. Sequentially adding methyl silicone resin, an organic silicon monomer D4, vinyl trimethoxy silane, deionized water and 1 part of 1% concentration methylaminoethanol solution into a spiral belt stirring reaction kettle with a cooling circulator, wherein the methylaminoethanol is a condensation reaction catalyst and is uniformly stirred; adding the silicon micropowder into the system and uniformly stirring; and adding the glass fiber powder, and uniformly stirring at a stirring speed of 60-200 rpm in the kettle.
And heating the reaction kettle to 50 ℃, reacting for 3-5 hours, heating the temperature of the reaction kettle to 80 ℃, reacting for 5-10 hours until the viscosity reaches 40 Pa.s, and cooling the gasified catalyst and the organic silicon monomer to flow back into the reaction kettle in the whole process. And after the reaction is finished, reducing the temperature of the reaction kettle to 50 ℃, vacuumizing, completely pumping out the catalyst from the system, and cooling to room temperature to obtain the silicone resin and liquid silica gel micropowder solid composite sizing material.
Heating and softening the composite material by using an internal mixer, adding 4 parts of curing agent into the composite material, uniformly mixing, and carrying out hot pressing at 150 ℃ to obtain the silica gel sheet. The physical and chemical properties of the material are measured, and the measured density is 1.72g/cm3, the hardness Shore A is 82, the tensile strength is 5.5MPa, the elongation at break is 70 percent, and the dielectric strength is 22 kV/mm. The weight loss of the silica gel sheet after being sintered for 90 minutes at 950 ℃ in the air is 10 percent, the air holes are closed holes and mesopores, and the dielectric strength is 11 kV/mm.
Example 4
The preparation of the ceramic organic silica gel for the medium-voltage fire-resistant cable is carried out according to the following process: 60 parts of low-hydrocarbon-content methyl silicone resin, 40 parts of dimethyl liquid silica gel, 220 parts of spherical silica powder, 3 parts of curing agent and 5 parts of 1 mm-long glass fiber powder. The silicone resin is a solid, a + b + c in the molecular structure of the silicone resin is approximately equal to 50, a + b + c in the molecular structure of the liquid silica gel is approximately equal to 700, the particle size peak values of the silica micropowder are respectively 15 micrometers, 5 micrometers and 2 micrometers, the oil absorption rate is 22mL/100g, the methyl silicone resin, the dimethyl liquid silica gel and 1 part of 1% concentration methylamine ethanol solution are sequentially added into a spiral-ribbon stirring reaction kettle with a cooling circulator, and the methylamine is a condensation reaction catalyst and is uniformly stirred; adding the uniformly mixed silicon micropowder into the kettle, and uniformly stirring; and adding the glass fiber powder, and uniformly stirring at a stirring speed of 60-200 rpm in the kettle. If the viscosity is too high, uneven agglomeration occurs, and a small amount of n-butanol and chloroform may be added to adjust the viscosity to be appropriate.
And heating the reaction kettle to 50 ℃, reacting for 3-5 hours, heating the temperature of the reaction kettle to 80 ℃, reacting for 5-10 hours until the viscosity reaches 40 Pa.s, and cooling the gasified catalyst and the organic solvent in the whole process to flow back into the reaction kettle. And after the reaction is finished, reducing the temperature of the reaction kettle to 50 ℃, vacuumizing, completely pumping out the catalyst and the solvent from the system, and reducing the temperature to room temperature to obtain the silicone resin and liquid silica gel micropowder solid composite sizing material.
Heating and softening the composite material by using an internal mixer, adding 3 parts of curing agent into the composite material, uniformly mixing, hot-pressing at 160 ℃ to obtain a silica gel sheet, and measuring the physical and chemical properties of the silica gel sheet, wherein the density is 1.72g/cm3, the hardness Shore A is 80, the tensile strength is 5.2MPa, the elongation at break is 76% and the dielectric strength is 22 kV/mm. The weight loss of the silica gel sheet after being sintered for 90 minutes at 950 ℃ in the air is 10 percent, the air holes are closed holes and mesopores, and the dielectric strength is 11 kV/mm.
Comparative example
For comparison of the above examples, dimethyl liquid silica gel was used in place of low-hydrogen content methyl silicone resin, 100 parts, 190 parts spherical silica powder, 4 parts curing agent, and 5 parts 1mm long glass fiber powder. A + b + c in the molecular structure of the liquid silica gel is approximately equal to 1500, the particle size peak values of the silicon micropowder are respectively 15 micrometers, 5 micrometers and 2 micrometers, the oil absorption rate is 22mL/100g, the dimethyl liquid silica gel and 1 part of 1% concentration methylamine ethanol solution are sequentially added into a spiral belt stirring reaction kettle with a cooling circulator, and the methylamine is a condensation reaction catalyst and is uniformly stirred; and adding the silicon micropowder into the kettle, uniformly stirring, adding the glass fiber powder, and uniformly stirring at a stirring speed of 60-200 rpm in the kettle. If the viscosity is too high, uneven agglomeration may occur, and a small amount of n-butanol and chloroform may be added to adjust the viscosity.
And heating the reaction kettle to 50 ℃, reacting for 3-5 hours, heating the temperature of the reaction kettle to 80 ℃, reacting for 5-10 hours until the viscosity reaches 40 Pa.s, and cooling the gasified catalyst and the organic solvent in the whole process to flow back into the reaction kettle. And after the reaction is finished, reducing the temperature of the reaction kettle to 50 ℃, vacuumizing, completely pumping out the catalyst and the solvent from the system, and reducing the temperature to room temperature to obtain the liquid silica gel micro powder solid composite sizing material.
Adding 4 parts of curing agent into the composite material by using an internal mixer, uniformly mixing, hot-pressing at 160 ℃ to form a silica gel sheet, measuring the physical and chemical properties of the silica gel sheet, and measuring the density to be 1.55g/cm3The hardness Shore A is 62, the tensile strength is 3.1MPa, the elongation at break is 210 percent, and the dielectric strength is 22 kV/mm. The weight loss of the silica gel sheet after being sintered for 90 minutes at 950 ℃ in the air is 14 percent, only half of pores are closed-pore mesopores, and the dielectric strength is 7 kV/mm.
Specific value pairs table 1:
table 1: and (5) comparing the performances of the fire-resistant cable materials.
| Serial number | Performance of | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example |
| 1 | Density, g/cm3 | 1.76 | 1.75 | 1.72 | 1.72 | 1.55 |
| 2 | Hardness Shore A | 85 | 83 | 82 | 80 | 62 |
| 3 | Tensile strength, MPa | 5.2 | 5.3 | 5.5 | 5.2 | 3.1 |
| 4 | Tensile elongation at break,% | 71 | 72 | 70 | 76 | 210 |
| 5 | Ablation weight loss,% | 9 | 9 | 10 | 10 | 14 |
| 6 | Dielectric strength (rubber), kV | 22 | 21 | 22 | 22 | 22 |
| 7 | Dielectric strength (ceramic), kV | 11 | 12 | 11 | 11 | 7 |
The present invention has been described in detail, and it should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
Claims (10)
1. The ceramic organic silica gel for the medium-voltage fire-resistant cable is characterized in that: the silicone adhesive comprises the following raw materials, 30-70 parts of low-carbon-hydrogen-content methyl silicone resin, 30-70 parts of dimethyl liquid silica gel, 130-300 parts of spherical silica powder, 1-5 parts of a curing agent and 2-10 parts of glass fiber powder, wherein the weight percentage of the carbon-hydrogen component in the formed silicone adhesive is within 13%, and the weight percentage of the spherical silica powder is more than 65%.
2. The ceramicized silicone rubber for a medium voltage fire resistant cable according to claim 1, wherein: the organic silica gel has the following characteristics: density of>1.6g/cm3The Shore A hardness is 70-85, the tensile strength is better than 5MPa, the elongation at break is more than 70%, and the dielectric strength is more than 20 kV/mm; the weight loss after sintering for 90 minutes at 950 ℃ in the air is not more than 10 percent, the air holes are closed-hole mesopores, and the dielectric strength is better than 10 kV/mm; the volume content of the inorganic filler is more than 50 percent, and the glue density is more than 1.6g/cm3The coating has high fluidity, can meet the requirement of an extruder for coating cables, and the fluidity of the glue is the maximum at 70-100 ℃.
3. The ceramicized silicone rubber for a medium voltage fire resistant cable according to claim 1, wherein: the chemical structure of the low-carbon hydrogen content methyl silicone resin is as follows: ((CH)3)3SiO1/2)a(CH3SiO3/2)b HcWherein a, b and c are integers, b/a is more than or equal to 5 and less than or equal to 30, b/c is more than or equal to 10 and less than or equal to 20, a + b + c is more than or equal to 32 and less than or equal to 50, and the content of hydrocarbonThe weight ratio of the methyl silicone resin is lower than 30 percent, and the methyl silicone resin with low hydrogen content can be dissolved in an organic solvent.
4. The ceramicized silicone rubber for a medium voltage fire resistant cable according to claim 1, wherein: the chemical structure of the dimethyl liquid silica gel is as follows: ((CH)3)3SiO1/2)a((CH3)2SiO)b(CH3C2H2SiO)c HdWherein a, b, c and d are integers, b/a is more than or equal to 50 and less than or equal to 500, b/c is more than or equal to 50 and less than or equal to 500, b/d is more than or equal to 50 and less than or equal to 500, and a + b + c + d is more than or equal to 200 and less than or equal to 2000; or ring-opening of organosilicon monomer D4 and condensation synthesis of vinyl trimethoxy silane are adopted, the weight ratio of organosilicon monomer D4 to vinyl trimethoxy silane is 100: 3 to 10.
5. The ceramified silicone gum for medium voltage fire-resistant cable according to claim 1, wherein the curing agent is a composite of a low-polymerization degree linear or cyclic methylhydrogensiloxane (CH) and a catalyst3)3SiO(CH3HSiO)3Si(CH3)3、(CH3)3SiO(CH3HSiO)5Si(C2H5)3、(CH3HSiO)4Any one of (a); the catalyst is platinum chloroacid.
6. The ceramicized silicone rubber for a medium voltage fire resistant cable according to claim 1, wherein: the purity of the spherical silicon micro powder is more than 99.5%, the particle size distribution is multimodal, the maximum particle size is less than 50 microns, the D50 is 1-20 microns, and the bulk density is more than 1.3g/cm3The oil absorption is lower than 30mL/100 g.
7. The ceramicized silicone rubber for a medium voltage fire resistant cable according to claim 1, wherein: the diameter of the used glass fiber powder is 5-20 microns, and the length is 0.3-5 mm.
8. The preparation process of the ceramized organic silica gel for the medium-voltage fire-resistant cable according to claim 1, which is characterized in that: the method comprises the following steps:
step 1: sequentially adding methyl silicone resin, vinyl dimethyl silica gel or an organic silicon monomer D4, vinyl trimethoxy silane and 1 part of 1% aminoethanol solution into a spiral ribbon stirring reaction kettle with a cooling circulator, and adding 1 part of deionized water for hydrolysis of methoxyl when the vinyl trimethoxy silane is adopted, wherein ammonia is a condensation reaction catalyst; stirring uniformly, adding the spherical silicon micropowder and stirring uniformly; adding glass fiber powder, and uniformly stirring at the stirring speed of 60-200 rpm; if the viscosity is too high and uneven agglomeration occurs, adding n-butanol and chloroform to adjust the viscosity;
step 2: heating to 50 ℃, and reacting for 3-5 hours; heating to 70-80 ℃, and reacting for 5-10 hours until the viscosity reaches 30-50 Pa.s; the gasified catalyst, the organic silicon monomer and the organic solvent are cooled and circulated back to the reaction kettle in the reaction process;
and step 3: cooling the reaction kettle to 50 ℃, vacuumizing, drying the catalyst and the solvent, and cooling to room temperature to obtain the silicone resin modified silica powder and liquid silica gel solid composite material;
when the composite material is used, a curing agent is added into the composite material, the surface of a copper cable is coated by extrusion, and the cable is vulcanized at 130-180 ℃.
9. The preparation process of the ceramization organosilica test sample for the medium-voltage fire-resistant cable according to claim 8, wherein the preparation process comprises the following steps: uniformly mixing the silicon resin modified silicon micropowder, the liquid silicon rubber solid composite material and the curing agent by adopting an internal mixer or a double-roller machine or a screw mixer, extruding into a sheet, carrying out hot press forming on a vulcanizing machine, preparing a test sample piece, and testing the tensile strength and the pressure resistance.
10. The sample preparation process of the ceramization organic silica gel for the medium voltage fire-resistant cable according to claim 9, wherein: and (3) heating and ceramizing the shaped sheet in a muffle furnace at 950 ℃ to obtain a ceramic sample, and measuring the mechanical property, the pressure resistance, the void ratio and the density.
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