CN111995833A - Fluoroplastic insulating high-temperature-resistant compensation cable - Google Patents

Fluoroplastic insulating high-temperature-resistant compensation cable Download PDF

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CN111995833A
CN111995833A CN202010857484.7A CN202010857484A CN111995833A CN 111995833 A CN111995833 A CN 111995833A CN 202010857484 A CN202010857484 A CN 202010857484A CN 111995833 A CN111995833 A CN 111995833A
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李坤
居盛文
吴云
方伟
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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
    • C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08L27/18—Homopolymers or copolymers or tetrafluoroethene
    • 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
    • H01B3/44—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 vinyl resins; acrylic resins
    • H01B3/443—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 vinyl resins; acrylic resins from vinylhalogenides or other halogenoethylenic compounds
    • H01B3/445—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 vinyl resins; acrylic resins from vinylhalogenides or other halogenoethylenic compounds from vinylfluorides or other fluoroethylenic compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B7/00—Insulated conductors or cables characterised by their form
    • H01B7/17—Protection against damage caused by external factors, e.g. sheaths or armouring
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B7/00—Insulated conductors or cables characterised by their form
    • H01B7/17—Protection against damage caused by external factors, e.g. sheaths or armouring
    • H01B7/18—Protection against damage caused by wear, mechanical force or pressure; Sheaths; Armouring
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B7/00—Insulated conductors or cables characterised by their form
    • H01B7/17—Protection against damage caused by external factors, e.g. sheaths or armouring
    • H01B7/28—Protection against damage caused by moisture, corrosion, chemical attack or weather
    • H01B7/282—Preventing penetration of fluid, e.g. water or humidity, into conductor or cable
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B7/00—Insulated conductors or cables characterised by their form
    • H01B7/17—Protection against damage caused by external factors, e.g. sheaths or armouring
    • H01B7/29—Protection against damage caused by extremes of temperature or by flame
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Abstract

The invention discloses a fluoroplastic insulated high-temperature-resistant compensation cable which comprises the following raw materials in parts by weight: 80-100 parts of polytetrafluoroethylene, 8-10 parts of high-temperature resistant filler, 8-10 parts of toughening filler, 3-5 parts of antioxidant and 2-5 parts of lubricant; hydrolyzing dimethyl diethoxy silane, methyl triethoxy silane and diphenyl diethoxy silane to generate corresponding silanol, further polymerizing the silanol to prepare organic silicon resin, and further fully mixing toluene in the organic silicon resin solution with the modified phosphorus lime to ensure that the organic silicon resin is coated on the surface of the modified phosphorus lime to prepare the high-temperature-resistant filler, so that the prepared compensation cable has good high-temperature resistance; the toughening filler is prepared, has good mechanical properties, contains a large amount of fluorine on the toughening filler molecule, has the characteristic of migrating fluorine to the surface of a polymer, and is easy to enrich on the surface of the polymer, so that the hydrophobicity of the compensating cable is increased, and the water-resistant effect is improved.

Description

Fluoroplastic insulating high-temperature-resistant compensation cable
Technical Field
The invention belongs to the technical field of cable preparation, and particularly relates to a fluoroplastic insulating high-temperature-resistant compensation cable.
Background
The compensating cable is suitable for multipoint connection of automatic thermometers in industries such as electric power, metallurgy, petroleum, chemical engineering, light textile and the like and departments such as national defense and scientific research, and severe environments such as a high temperature area or an electromagnetic interference area and the like are sometimes required to be penetrated in the using process, so that the compensating cable has the problems of aging phenomenon, unstable signal transmission and the like, and the production requirement of people in special environments cannot be met.
The high temperature resistance of the existing compensation cable is general, the performance of the cable is reduced under the high-temperature environment, the cable is easy to damage, and the compensation cable is low in toughness, so that cracks are easy to appear on the surface of the cable after the compensation cable is moved and bent for many times, and the cable can not be normally used.
Disclosure of Invention
The invention aims to provide a fluoroplastic insulated high-temperature-resistant compensation cable.
The technical problems to be solved by the invention are as follows:
the high temperature resistance of the existing compensation cable is general, the performance of the cable is reduced under the high-temperature environment, the cable is easy to damage, and the compensation cable is low in toughness, so that cracks are easy to appear on the surface of the cable after the compensation cable is moved and bent for many times, and the cable can not be normally used.
The purpose of the invention can be realized by the following technical scheme:
a fluoroplastic insulating high-temperature-resistant compensation cable comprises the following raw materials in parts by weight: 80-100 parts of polytetrafluoroethylene, 8-10 parts of high-temperature resistant filler, 8-10 parts of toughening filler, 3-5 parts of antioxidant and 2-5 parts of lubricant;
the compensation cable is manufactured by the following steps:
step S1: heating polytetrafluoroethylene at the temperature of 350-400 ℃ until the polytetrafluoroethylene is completely molten, adding high-temperature-resistant filler and toughening filler, mixing for 10-15min, adding antioxidant and lubricant, and continuously mixing for 15-20min to obtain a rubber material;
step S2: tabletting the rubber material at the temperature of 350-400 ℃ to obtain rubber sheets with the thickness of 3-5mm, granulating to obtain rubber particles, adding the rubber particles into a five-section single-screw extruder, and extruding at the temperature of 350 ℃, 380 ℃, 400 ℃, 380 ℃ and 350 ℃ to obtain a rubber sheath;
step S3: and (5) coating the rubber sheath prepared in the step S2 on the surface of the copper wire to prepare the compensation cable.
Further, the antioxidant is one or two of 2, 4-dimethyl-6- (1-methylpentadecyl) -phenol and 1, 2-bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine mixed in any proportion, and the lubricant is one or two of polyethylene wax and ethylene bis stearamide mixed in any proportion.
Further, the high-temperature-resistant filler is prepared by the following steps:
step A1: adding calcium chloride into deionized water, stirring until the calcium chloride is completely dissolved, adding a sodium hydroxide solution, stirring for 5-10min at the rotation speed of 200-300r/min, dropwise adding a phosphoric acid solution, continuously stirring for 1-1.5h, keeping the temperature at 50-60 ℃ for 20-25h, filtering to remove filtrate, and drying a filter cake at 80 ℃ to obtain the hydroxyapatite;
step A2: adding ethanol, deionized water and sodium hydroxide into a reaction kettle, stirring the mixture until the mixture is uniformly mixed under the condition that the rotating speed is 120-150r/min, adding the hydroxyl phosphorus lime and the phenyl trimethoxy silane prepared in the step A1 under the condition that the temperature is 80-90 ℃, performing reflux reaction for 4-6h, distilling the mixture under the condition that the temperature is 100 ℃, and continuously preserving the heat for 20-30min under the condition that the temperature is 115-120 ℃ to prepare the modified phosphorus lime;
step A3: mixing dimethyl diethoxy silane, methyl triethoxy silane and diphenyl diethoxy silane to prepare a mixed solution, adding ethanol and deionized water into a reaction kettle, stirring and adding the mixed solution under the conditions that the rotating speed is 200-300r/min and the temperature is 25-30 ℃, reacting for 1-1.5 hours at the temperature of 60-70 ℃, heating to 80 ℃, removing the ethanol, standing to remove a water layer, continuously heating to the temperature of 160-200 ℃, and reacting for 5-8 hours to prepare the organic silicon resin;
step A4: and (2) adding the organic silicon resin prepared in the step A3 into toluene, adding the modified phosphorous lime prepared in the step A2 after the organic silicon resin is completely dissolved, stirring for 20-30min under the condition that the rotation speed is 800-1000r/min, carrying out ultrasonic treatment for 5-10min under the condition that the frequency is 3-5kHz, and distilling to remove toluene at the temperature of 120 ℃ to prepare the high-temperature-resistant filler.
Further, the using amount ratio of the calcium chloride, the sodium hydroxide solution and the phosphoric acid solution in the step A1 is 1g:3mL:5mL, the mass fraction of the sodium hydroxide solution is 30-35%, the mass fraction of the phosphoric acid solution is 40-50%, the using amount ratio of the ethanol, the deionized water, the sodium hydroxide and the hydroxy phosphorus lime in the step A2 is 2mL:5mL:0.3-0.5g:1g, the using amount of the phenyltrimethoxysilane is 3-5% of the mass of the hydroxy phosphorus lime, the using amount of the dimethyldiethoxysilane and the monomethyltriethoxysilane in the step A3 is 1:1, the using amount of the ethanol, the deionized water and the mixed solution is 1:3:2, and the using amount of the organic silicon resin and the modified phosphorus lime in the step A4 is 2: 1-1.5.
Further, the toughening filler is prepared by the following steps:
step B1: adding m-bis (trifluoromethyl) benzene into a reaction kettle, stirring and slowly adding mixed acid under the conditions that the rotation speed is 120-150 ℃ and the temperature is 3-5 ℃, keeping the temperature for 5-10min under the condition that the temperature is 60-65 ℃, stirring for 3-5h under the condition that the temperature is 35-40 ℃, standing until the mixed acid at the lower layer is removed by layering, adding ferric chloride into the organic liquid at the upper layer and introducing chlorine, and reacting under the condition that the temperature is 20-25 ℃ to obtain an intermediate 1;
the reaction process is as follows:
Figure BDA0002646886690000031
Figure BDA0002646886690000041
step B2: dissolving the intermediate 1 prepared in the step B1 in dimethylformamide, adding potassium carbonate and hexafluorobisphenol A, reacting for 20-25h at the rotation speed of 200-300r/min and the temperature of 130-140 ℃, filtering, distilling the filtrate at the temperature of 160 ℃ to remove the dimethylformamide, and drying to obtain an intermediate 2;
the reaction process is as follows:
Figure BDA0002646886690000042
step B3: adding iron powder, ethanol and deionized water into a reaction kettle, adjusting the pH value to 4-5, preserving the heat for 1-1.5h at the temperature of 90-95 ℃, adding the intermediate 2 prepared in the step B2, performing reflux reaction for 3-5h at the rotation speed of 150-200r/min and the temperature of 80-90 ℃, filtering, adjusting the pH value of the filtrate to 9-10, performing secondary filtration, and drying the filter cake to prepare an intermediate 3;
the reaction process is as follows:
Figure BDA0002646886690000043
step B4: and adding polyoxypropylene glycol into a reaction kettle, introducing nitrogen for protection and adding toluene diisocyanate under the conditions that the rotation speed is 120-one-year old at 150r/min and the temperature is 70-75 ℃, reacting for 2-3h, adding the intermediate 3 prepared in the step B3 under the condition that the temperature is 40-50 ℃, reacting for 2-3h under the condition that the temperature is 60-70 ℃, and then preserving heat for 10-15h under the condition that the temperature is 80-85 ℃ to prepare the toughening filler.
Further, the mass ratio of the m-bis (trifluoromethyl) benzene to the mixed acid in the step B1 is 1:2-2.2, the mixed acid is prepared by mixing concentrated nitric acid and concentrated sulfuric acid in a molar ratio of 1:3, the mass fraction of the concentrated nitric acid is 68-70%, the mass fraction of the concentrated sulfuric acid is 70-75%, the molar ratio of the organic liquid to chlorine is 2:1, the amount of ferric chloride is 5-8% of the mass of the organic liquid, the mass ratio of the intermediate 1, potassium carbonate and hexafluorobisphenol A in the step B2 is 2:1:1.5-1.6, the mass ratio of the iron powder, ethanol, deionized water and the intermediate 2 in the step B3 is 3-4g:10mL:10mL:7.5-8g, and the mass ratio of the polyoxypropylene glycol, the toluene diisocyanate and the intermediate 3 in the step B4 is 1:1.05: 0.85.
The invention has the beneficial effects that: the invention prepares a high temperature resistant filler in the process of preparing a fluoroplastic insulation high temperature resistant compensation cable, the high temperature resistant filler is prepared by firstly preparing hydroxyl phosphorus lime which has good heat resistance, and the surface of the hydroxyl phosphorus lime contains a large amount of active hydroxyl, then hydrolyzing phenyltrimethoxysilane to obtain silanol, condensing the silanol and the active hydroxyl to generate covalent bonds to be attached to the surface of the hydroxyl phosphorus lime, carrying out condensation reaction on adjacent silanol to generate a polysiloxane network structure of the hydroxyl phosphorus lime, enabling phenyl to be positioned on the surface of the hydroxyl phosphorus lime, further improving the high temperature resistance of the hydroxyl phosphorus lime, hydrolyzing dimethyl diethoxy silane, methyl triethoxy silane and diphenyl diethoxy silane to generate corresponding silanol, further polymerizing the silanol to prepare organic silicon resin, then, fully mixing the organic silicon resin solution with the modified phosphorus lime, and removing toluene to ensure that the organic silicon resin is coated on the surface of the modified phosphorus lime to prepare the high-temperature-resistant filler, so that the prepared compensation cable has good high-temperature resistance; the toughening filler is prepared by taking m-bis (trifluoromethyl) benzene as a raw material, inserting nitro on a benzene ring under the action of m-bis (trifluoromethyl) benzene mixed acid, further inserting chlorine atoms under the catalysis of ferric chloride to prepare an intermediate 1, further reacting the intermediate 1 with hexafluorobisphenol A to insert the molecule of the intermediate 1 on the molecule of the hexafluorobisphenol A to prepare an intermediate 2, reducing the nitro into amino by the intermediate 2 under the action of iron powder, further preparing a polyurethane elastomer by using polyoxypropylene diol and toluene diisocyanate, and further using the intermediate 3 as a chain extender to prepare the toughening filler, wherein the toughening filler has good mechanical property, and has a large amount of fluorine on the molecule, the fluorine has the characteristic of migrating to the surface of a polymer and is easy to enrich on the surface of the polymer, so that the hydrophobicity of a compensation cable is increased, the water-resistant effect is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A fluoroplastic insulating high-temperature-resistant compensation cable comprises the following raw materials in parts by weight: 80 parts of polytetrafluoroethylene, 8 parts of high-temperature-resistant filler, 8 parts of toughening filler, 3 parts of 2, 4-dimethyl-6- (1-methylpentadecyl) -phenol and 2 parts of polyethylene wax;
the compensation cable is manufactured by the following steps:
step S1: heating polytetrafluoroethylene at the temperature of 350 ℃ until the polytetrafluoroethylene is completely melted, adding high-temperature-resistant filler and toughening filler, mixing for 10min, adding 2, 4-dimethyl-6- (1-methylpentadecyl) -phenol and polyethylene wax, and continuously mixing for 15min to obtain a rubber material;
step S2: tabletting a rubber material at the temperature of 350 ℃ to obtain rubber sheets with the thickness of 3mm, cutting into particles to obtain rubber particles, adding the rubber particles into a five-section single-screw extruder, and extruding at the temperature of 350 ℃, 380 ℃, 400 ℃, 380 ℃ and 350 ℃ to obtain a rubber sheath;
step S3: and (5) coating the rubber sheath prepared in the step S2 on the surface of the copper wire to prepare the compensation cable.
The high-temperature resistant filler is prepared by the following steps:
step A1: adding calcium chloride into deionized water, stirring until the calcium chloride is completely dissolved, adding a sodium hydroxide solution, stirring for 5min at the rotation speed of 200r/min, dropwise adding a phosphoric acid solution, continuously stirring for 1h, keeping the temperature at 50 ℃ for 20h, filtering to remove filtrate, and drying a filter cake at the temperature of 80 ℃ to obtain the hydroxyl-phosphorus lime;
step A2: adding ethanol, deionized water and sodium hydroxide into a reaction kettle, stirring the mixture until the mixture is uniformly mixed under the condition that the rotating speed is 120r/min, adding the hydroxyl phosphorus lime and the phenyl trimethoxy silane prepared in the step A1 under the condition that the temperature is 80 ℃, performing reflux reaction for 4 hours, distilling the mixture under the condition that the temperature is 100 ℃, and continuously preserving the temperature of a substrate for 20min under the condition that the temperature is 115 ℃ to prepare modified phosphorus lime;
step A3: mixing dimethyl diethoxy silane, monomethyl triethoxy silane and diphenyl diethoxy silane to prepare a mixed solution, adding ethanol and deionized water into a reaction kettle, stirring and adding the mixed solution under the conditions that the rotating speed is 200r/min and the temperature is 25 ℃, reacting for 1 hour at the temperature of 60 ℃, heating to 80 ℃, removing the ethanol, standing to remove a water layer, continuously heating to 160 ℃, and reacting for 5 hours to prepare the organic silicon resin;
step A4: and B, adding the organic silicon resin prepared in the step A3 into toluene, adding the modified lime phosphate prepared in the step A2 after the organic silicon resin is completely dissolved, stirring for 20min under the condition that the rotation speed is 800r/min, carrying out ultrasonic treatment for 5min under the condition that the frequency is 3kHz, and distilling to remove toluene under the condition that the temperature is 120 ℃ to prepare the high-temperature-resistant filler.
The toughening filler is prepared by the following steps:
step B1: adding m-bis (trifluoromethyl) benzene into a reaction kettle, stirring and slowly adding mixed acid under the conditions that the rotating speed is 120 ℃ and the temperature is 3 ℃, keeping the temperature for 5min under the condition that the temperature is 60 ℃, stirring for 3h under the condition that the temperature is 35 ℃, standing until the mixed acid at the lower layer is removed by layering, adding ferric chloride into the organic liquid at the upper layer, introducing chlorine, and reacting under the condition that the temperature is 20 ℃ to obtain an intermediate 1;
step B2: dissolving the intermediate 1 prepared in the step B1 in dimethylformamide, adding potassium carbonate and hexafluorobisphenol A, reacting for 20 hours at the rotation speed of 200r/min and the temperature of 130 ℃, filtering, distilling the filtrate at the temperature of 160 ℃ to remove the dimethylformamide, and drying to obtain an intermediate 2;
step B3: adding iron powder, ethanol and deionized water into a reaction kettle, adjusting the pH value to be 4, keeping the temperature at 90 ℃ for 1h, adding the intermediate 2 prepared in the step B2, performing reflux reaction at the rotation speed of 150r/min and the temperature of 80 ℃ for 3h, filtering, adjusting the pH value of the filtrate to be 9, filtering again, and drying the filter cake to obtain an intermediate 3;
step B4: and (2) adding polyoxypropylene glycol into a reaction kettle, introducing nitrogen for protection and adding toluene diisocyanate under the conditions that the rotating speed is 120r/min and the temperature is 70 ℃, reacting for 2 hours, adding the intermediate 3 prepared in the step B3 under the condition that the temperature is 40 ℃, reacting for 2 hours under the condition that the temperature is 60 ℃, and preserving heat for 10 hours under the condition that the temperature is 80 ℃ to prepare the toughening filler.
Example 2
A fluoroplastic insulating high-temperature-resistant compensation cable comprises the following raw materials in parts by weight: 90 parts of polytetrafluoroethylene, 9 parts of high-temperature resistant filler, 9 parts of toughening filler, 4 parts of 2, 4-dimethyl-6- (1-methylpentadecyl) -phenol and 3 parts of polyethylene wax;
the compensation cable is manufactured by the following steps:
step S1: heating polytetrafluoroethylene at the temperature of 380 ℃ until the polytetrafluoroethylene is completely molten, adding high-temperature-resistant filler and toughening filler, mixing for 13min, adding 2, 4-dimethyl-6- (1-methylpentadecyl) -phenol and polyethylene wax, and continuously mixing for 18min to obtain a rubber material;
step S2: tabletting a rubber material at the temperature of 380 ℃ to obtain rubber sheets with the thickness of 4mm, cutting the rubber sheets into particles to obtain rubber particles, adding the rubber particles into a five-section single-screw extruder, and extruding the rubber particles at the temperature of 350 ℃, 380 ℃, 400 ℃, 380 ℃ and 350 ℃ to obtain a rubber sheath;
step S3: and (5) coating the rubber sheath prepared in the step S2 on the surface of the copper wire to prepare the compensation cable.
The high-temperature resistant filler is prepared by the following steps:
step A1: adding calcium chloride into deionized water, stirring until the calcium chloride is completely dissolved, adding a sodium hydroxide solution, stirring for 8min at the rotation speed of 250r/min, dropwise adding a phosphoric acid solution, continuously stirring for 1.3h, keeping the temperature at 55 ℃ for 23h, filtering to remove filtrate, and drying a filter cake at the temperature of 80 ℃ to obtain the hydroxy phosphorite;
step A2: adding ethanol, deionized water and sodium hydroxide into a reaction kettle, stirring the mixture until the mixture is uniformly mixed under the condition that the rotating speed is 130r/min, adding the hydroxyl phosphorus lime and the phenyl trimethoxy silane prepared in the step A1 under the condition that the temperature is 85 ℃, performing reflux reaction for 5 hours, distilling the mixture under the condition that the temperature is 100 ℃, and continuously preserving the temperature of a substrate for 25min under the condition that the temperature is 118 ℃ to prepare modified phosphorus lime;
step A3: mixing dimethyl diethoxy silane, monomethyl triethoxy silane and diphenyl diethoxy silane to prepare a mixed solution, adding ethanol and deionized water into a reaction kettle, stirring and adding the mixed solution under the conditions that the rotating speed is 250r/min and the temperature is 28 ℃, reacting for 1.3 hours at the temperature of 65 ℃, heating to 80 ℃, removing the ethanol, standing to remove a water layer, continuously heating to 180 ℃, and reacting for 6 hours to prepare the organic silicon resin;
step A4: and B, adding the organic silicon resin prepared in the step A3 into toluene, adding the modified lime phosphate prepared in the step A2 after the organic silicon resin is completely dissolved, stirring for 25min under the condition that the rotating speed is 900r/min, carrying out ultrasonic treatment for 8min under the condition that the frequency is 4kHz, and distilling to remove toluene under the condition that the temperature is 120 ℃ to prepare the high-temperature-resistant filler.
The toughening filler is prepared by the following steps:
step B1: adding m-bis (trifluoromethyl) benzene into a reaction kettle, stirring and slowly adding mixed acid under the conditions that the rotating speed is 130 ℃ and the temperature is 4 ℃, keeping the temperature for 8min under the condition that the temperature is 63 ℃, stirring for 4h under the condition that the temperature is 38 ℃, standing until the mixed acid at the lower layer is removed by layering, adding ferric chloride into the organic liquid at the upper layer, introducing chlorine, and reacting under the condition that the temperature is 23 ℃ to prepare an intermediate 1;
step B2: dissolving the intermediate 1 prepared in the step B1 in dimethylformamide, adding potassium carbonate and hexafluorobisphenol A, reacting for 22 hours at 140 ℃ at the rotation speed of 250r/min, filtering, distilling the filtrate at 160 ℃ to remove the dimethylformamide, and drying to obtain an intermediate 2;
step B3: adding iron powder, ethanol and deionized water into a reaction kettle, adjusting the pH value to be 5, keeping the temperature at 95 ℃ for 1.5h, adding the intermediate 2 prepared in the step B2, performing reflux reaction at the rotation speed of 200r/min and the temperature of 85 ℃ for 4h, filtering, adjusting the pH value of the filtrate to be 10, filtering again, and drying the filter cake to obtain an intermediate 3;
step B4: and (2) adding polyoxypropylene glycol into a reaction kettle, introducing nitrogen for protection and adding toluene diisocyanate under the conditions that the rotating speed is 130r/min and the temperature is 72 ℃, reacting for 3 hours, adding the intermediate 3 prepared in the step B3 under the condition that the temperature is 45 ℃, reacting for 3 hours under the condition that the temperature is 65 ℃, and preserving heat for 13 hours under the condition that the temperature is 82 ℃ to prepare the toughening filler.
Example 3
A fluoroplastic insulating high-temperature-resistant compensation cable comprises the following raw materials in parts by weight: 100 parts of polytetrafluoroethylene, 10 parts of high-temperature-resistant filler, 10 parts of toughening filler, 5 parts of 2, 4-dimethyl-6- (1-methylpentadecyl) -phenol and 5 parts of polyethylene wax;
the compensation cable is manufactured by the following steps:
step S1: heating polytetrafluoroethylene at the temperature of 400 ℃ until the polytetrafluoroethylene is completely melted, adding high-temperature-resistant filler and toughening filler, mixing for 15min, adding 2, 4-dimethyl-6- (1-methylpentadecyl) -phenol and polyethylene wax, and continuously mixing for 20min to obtain a rubber material;
step S2: tabletting a rubber material at the temperature of 400 ℃ to obtain rubber sheets with the thickness of 5mm, cutting into particles to obtain rubber particles, adding the rubber particles into a five-section single-screw extruder, and extruding under the conditions that the temperature of the five sections is 350 ℃, 380 ℃, 400 ℃, 380 ℃ and 350 ℃ respectively to obtain a rubber sheath;
step S3: and (5) coating the rubber sheath prepared in the step S2 on the surface of the copper wire to prepare the compensation cable.
The high-temperature resistant filler is prepared by the following steps:
step A1: adding calcium chloride into deionized water, stirring until the calcium chloride is completely dissolved, adding a sodium hydroxide solution, stirring for 10min at the rotation speed of 300r/min, dropwise adding a phosphoric acid solution, continuously stirring for 1.5h, keeping the temperature at 60 ℃ for 25h, filtering to remove filtrate, and drying a filter cake at the temperature of 80 ℃ to obtain the hydroxy phosphorite;
step A2: adding ethanol, deionized water and sodium hydroxide into a reaction kettle, stirring the mixture until the mixture is uniformly mixed under the condition that the rotating speed is 150r/min, adding the hydroxyl phosphorus lime and the phenyl trimethoxy silane prepared in the step A1 under the condition that the temperature is 90 ℃, performing reflux reaction for 6 hours, distilling the mixture under the condition that the temperature is 100 ℃, and continuously preserving the temperature of a substrate for 30min under the condition that the temperature is 120 ℃ to prepare modified phosphorus lime;
step A3: mixing dimethyl diethoxy silane, monomethyl triethoxy silane and diphenyl diethoxy silane to prepare a mixed solution, adding ethanol and deionized water into a reaction kettle, stirring and adding the mixed solution under the conditions that the rotating speed is 300r/min and the temperature is 30 ℃, reacting for 1.5 hours at the temperature of 70 ℃, heating to 80 ℃, removing the ethanol, standing to remove a water layer, continuously heating to 200 ℃, and reacting for 8 hours to prepare the organic silicon resin;
step A4: and B, adding the organic silicon resin prepared in the step A3 into toluene, adding the modified lime phosphate prepared in the step A2 after the organic silicon resin is completely dissolved, stirring for 30min under the condition that the rotating speed is 1000r/min, carrying out ultrasonic treatment for 10min under the condition that the frequency is 5kHz, and distilling to remove toluene under the condition that the temperature is 120 ℃ to prepare the high-temperature-resistant filler.
The toughening filler is prepared by the following steps:
step B1: adding m-bis (trifluoromethyl) benzene into a reaction kettle, stirring and slowly adding mixed acid under the conditions that the rotating speed is 150 ℃ and the temperature is 5 ℃, keeping the temperature for 10min under the condition that the temperature is 65 ℃, stirring for 5h under the condition that the temperature is 40 ℃, standing until the mixed acid on the lower layer is removed by layering, adding ferric chloride into the organic liquid on the upper layer, introducing chlorine, and reacting under the condition that the temperature is 25 ℃ to prepare an intermediate 1;
step B2: dissolving the intermediate 1 prepared in the step B1 in dimethylformamide, adding potassium carbonate and hexafluorobisphenol A, reacting for 25 hours at the rotation speed of 300r/min and the temperature of 140 ℃, filtering, distilling the filtrate at the temperature of 160 ℃ to remove the dimethylformamide, and drying to obtain an intermediate 2;
step B3: adding iron powder, ethanol and deionized water into a reaction kettle, adjusting the pH value to be 5, keeping the temperature at 95 ℃ for 1.5h, adding the intermediate 2 prepared in the step B2, performing reflux reaction at the rotation speed of 200r/min and the temperature of 90 ℃ for 5h, filtering, adjusting the pH value of the filtrate to be 10, filtering again, and drying the filter cake to obtain an intermediate 3;
step B4: and (2) adding polyoxypropylene glycol into a reaction kettle, introducing nitrogen for protection and adding toluene diisocyanate under the conditions that the rotating speed is 150r/min and the temperature is 75 ℃, reacting for 3 hours, adding the intermediate 3 prepared in the step B3 under the condition that the temperature is 50 ℃, reacting for 3 hours under the condition that the temperature is 70 ℃, and preserving heat for 15 hours under the condition that the temperature is 85 ℃ to prepare the toughening filler.
Comparative example
The comparative example is a common compensating cable on the market.
The performance tests were performed on the compensation cables prepared in examples 1 to 3 and comparative example, and the test results are shown in table 1 below;
TABLE 1
Figure BDA0002646886690000121
Figure BDA0002646886690000131
As can be seen from Table 1 above, the compensation cables prepared in examples 1-3 have a heat distortion temperature of 446-453 ℃, a bending strength of 41.9-42.8MPa, and a bending modulus of 2.03-2.06GPa, and the compensation cables prepared in comparative examples have a heat distortion temperature of 352 ℃, a bending strength of 31.6MPa, and a bending modulus of 1.63GPa, so that the invention has good high temperature resistance and flexibility.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.

Claims (6)

1. The utility model provides a fluoroplastics insulating high temperature resistant compensation cable which characterized in that: the feed comprises the following raw materials in parts by weight: 80-100 parts of polytetrafluoroethylene, 8-10 parts of high-temperature resistant filler, 8-10 parts of toughening filler, 3-5 parts of antioxidant and 2-5 parts of lubricant;
the compensation cable is manufactured by the following steps:
step S1: heating polytetrafluoroethylene at the temperature of 350-400 ℃ until the polytetrafluoroethylene is completely molten, adding high-temperature-resistant filler and toughening filler, mixing for 10-15min, adding antioxidant and lubricant, and continuously mixing for 15-20min to obtain a rubber material;
step S2: tabletting the rubber material at the temperature of 350-400 ℃ to obtain rubber sheets with the thickness of 3-5mm, granulating to obtain rubber particles, adding the rubber particles into a five-section single-screw extruder, and extruding at the temperature of 350 ℃, 380 ℃, 400 ℃, 380 ℃ and 350 ℃ to obtain a rubber sheath;
step S3: and (5) coating the rubber sheath prepared in the step S2 on the surface of the copper wire to prepare the compensation cable.
2. A fluoroplastic insulated high-temperature-resistant compensation cable according to claim 1, wherein: the antioxidant is one or two of 2, 4-dimethyl-6- (1-methyl pentadecyl) -phenol and 1, 2-bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine mixed in any proportion, and the lubricant is one or two of polyethylene wax and ethylene bis stearamide mixed in any proportion.
3. A fluoroplastic insulated high-temperature-resistant compensation cable according to claim 1, wherein: the high-temperature resistant filler is prepared by the following steps:
step A1: adding calcium chloride into deionized water, stirring until the calcium chloride is completely dissolved, adding a sodium hydroxide solution, stirring for 5-10min at the rotation speed of 200-300r/min, dropwise adding a phosphoric acid solution, continuously stirring for 1-1.5h, keeping the temperature at 50-60 ℃ for 20-25h, filtering to remove filtrate, and drying a filter cake at 80 ℃ to obtain the hydroxyapatite;
step A2: adding ethanol, deionized water and sodium hydroxide into a reaction kettle, stirring the mixture until the mixture is uniformly mixed under the condition that the rotating speed is 120-150r/min, adding the hydroxyl phosphorus lime and the phenyl trimethoxy silane prepared in the step A1 under the condition that the temperature is 80-90 ℃, performing reflux reaction for 4-6h, distilling the mixture under the condition that the temperature is 100 ℃, and continuously preserving the heat for 20-30min under the condition that the temperature is 115-120 ℃ to prepare the modified phosphorus lime;
step A3: mixing dimethyl diethoxy silane, methyl triethoxy silane and diphenyl diethoxy silane to prepare a mixed solution, adding ethanol and deionized water into a reaction kettle, stirring and adding the mixed solution under the conditions that the rotating speed is 200-300r/min and the temperature is 25-30 ℃, reacting for 1-1.5 hours at the temperature of 60-70 ℃, heating to 80 ℃, removing the ethanol, standing to remove a water layer, continuously heating to the temperature of 160-200 ℃, and reacting for 5-8 hours to prepare the organic silicon resin;
step A4: and (2) adding the organic silicon resin prepared in the step A3 into toluene, adding the modified phosphorous lime prepared in the step A2 after the organic silicon resin is completely dissolved, stirring for 20-30min under the condition that the rotation speed is 800-1000r/min, carrying out ultrasonic treatment for 5-10min under the condition that the frequency is 3-5kHz, and distilling to remove toluene at the temperature of 120 ℃ to prepare the high-temperature-resistant filler.
4. A fluoroplastic insulated high-temperature-resistant compensation cable according to claim 3, wherein: the using amount ratio of the calcium chloride, the sodium hydroxide solution and the phosphoric acid solution in the step A1 is 1g to 3mL to 5mL, the mass fraction of the sodium hydroxide solution is 30-35%, the mass fraction of the phosphoric acid solution is 40-50%, the using amount ratio of the ethanol, the deionized water, the sodium hydroxide and the hydroxy phosphorus lime in the step A2 is 2mL to 5mL to 0.3-0.5g to 1g, the using amount of the phenyltrimethoxysilane is 3-5% of the mass of the hydroxy phosphorus lime, the volume ratio of the dimethyldiethoxysilane to the monomethyltriethoxysilane in the step A3 is 1:1, the using amount of the ethanol, the deionized water and the mixed solution is 1:3:2, and the using amount ratio of the organic silicon resin and the modified phosphorus lime in the step A4 is 2: 1-1.5.
5. A fluoroplastic insulated high-temperature-resistant compensation cable according to claim 1, wherein: the toughening filler is prepared by the following steps:
step B1: adding m-bis (trifluoromethyl) benzene into a reaction kettle, stirring and slowly adding mixed acid under the conditions that the rotation speed is 120-150 ℃ and the temperature is 3-5 ℃, keeping the temperature for 5-10min under the condition that the temperature is 60-65 ℃, stirring for 3-5h under the condition that the temperature is 35-40 ℃, standing until the mixed acid at the lower layer is removed by layering, adding ferric chloride into the organic liquid at the upper layer and introducing chlorine, and reacting under the condition that the temperature is 20-25 ℃ to obtain an intermediate 1;
step B2: dissolving the intermediate 1 prepared in the step B1 in dimethylformamide, adding potassium carbonate and hexafluorobisphenol A, reacting for 20-25h at the rotation speed of 200-300r/min and the temperature of 130-140 ℃, filtering, distilling the filtrate at the temperature of 160 ℃ to remove the dimethylformamide, and drying to obtain an intermediate 2;
step B3: adding iron powder, ethanol and deionized water into a reaction kettle, adjusting the pH value to 4-5, preserving the heat for 1-1.5h at the temperature of 90-95 ℃, adding the intermediate 2 prepared in the step B2, performing reflux reaction for 3-5h at the rotation speed of 150-200r/min and the temperature of 80-90 ℃, filtering, adjusting the pH value of the filtrate to 9-10, performing secondary filtration, and drying the filter cake to prepare an intermediate 3;
step B4: and adding polyoxypropylene glycol into a reaction kettle, introducing nitrogen for protection and adding toluene diisocyanate under the conditions that the rotation speed is 120-one-year old at 150r/min and the temperature is 70-75 ℃, reacting for 2-3h, adding the intermediate 3 prepared in the step B3 under the condition that the temperature is 40-50 ℃, reacting for 2-3h under the condition that the temperature is 60-70 ℃, and then preserving heat for 10-15h under the condition that the temperature is 80-85 ℃ to prepare the toughening filler.
6. A fluoroplastic insulated high-temperature-resistant compensation cable according to claim 5, wherein: the mass ratio of the m-bis (trifluoromethyl) benzene to the mixed acid in the step B1 is 1:2-2.2, the mixed acid is prepared by mixing concentrated nitric acid and concentrated sulfuric acid in a molar ratio of 1:3, the mass fraction of the concentrated nitric acid is 68-70%, the mass fraction of the concentrated sulfuric acid is 70-75%, the mass ratio of organic liquid to chlorine is 2:1, the mass ratio of ferric chloride is 5-8% of the mass of the organic liquid, the mass ratio of the intermediate 1, potassium carbonate and hexafluorobisphenol A in the step B2 is 2:1:1.5-1.6, the mass ratio of the iron powder, ethanol, deionized water and the intermediate 2 in the step B3 is 3-4g:10mL:10mL:7.5-8g, and the mass ratio of the polyoxypropylene glycol, the toluene diisocyanate and the intermediate 3 in the step B4 is 1:1.05: 0.85.
CN202010857484.7A 2020-08-24 2020-08-24 Fluoroplastic insulating high-temperature-resistant compensation cable Withdrawn CN111995833A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112544421A (en) * 2020-12-09 2021-03-26 安徽南北现代林业科技有限公司 Soilless culture method for tomato breeding
CN115536538A (en) * 2022-09-23 2022-12-30 濮阳市盛通聚源新材料有限公司 Fluorine-containing diamine, fluorine-containing high-temperature-resistant nylon and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112544421A (en) * 2020-12-09 2021-03-26 安徽南北现代林业科技有限公司 Soilless culture method for tomato breeding
CN115536538A (en) * 2022-09-23 2022-12-30 濮阳市盛通聚源新材料有限公司 Fluorine-containing diamine, fluorine-containing high-temperature-resistant nylon and preparation method thereof
CN115536538B (en) * 2022-09-23 2023-09-26 濮阳市盛通聚源新材料有限公司 Fluorine-containing diamine, fluorine-containing high-temperature-resistant nylon and preparation method thereof

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