CN112186382A - Ultra-small sealed high-temperature high-pressure connector - Google Patents
Ultra-small sealed high-temperature high-pressure connector Download PDFInfo
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- CN112186382A CN112186382A CN202011086478.2A CN202011086478A CN112186382A CN 112186382 A CN112186382 A CN 112186382A CN 202011086478 A CN202011086478 A CN 202011086478A CN 112186382 A CN112186382 A CN 112186382A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
- H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
- H01R13/02—Contact members
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- C—CHEMISTRY; METALLURGY
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- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
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- C08K7/26—Silicon- containing compounds
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- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J179/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09J161/00 - C09J177/00
- C09J179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C09J179/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C09J179/085—Unsaturated polyimide precursors
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
- H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
- H01R13/40—Securing contact members in or to a base or case; Insulating of contact members
- H01R13/405—Securing in non-demountable manner, e.g. moulding, riveting
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- H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
- H01R13/46—Bases; Cases
- H01R13/502—Bases; Cases composed of different pieces
- H01R13/504—Bases; Cases composed of different pieces different pieces being moulded, cemented, welded, e.g. ultrasonic, or swaged together
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- H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
- H01R13/46—Bases; Cases
- H01R13/52—Dustproof, splashproof, drip-proof, waterproof, or flameproof cases
- H01R13/5216—Dustproof, splashproof, drip-proof, waterproof, or flameproof cases characterised by the sealing material, e.g. gels or resins
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Abstract
The invention relates to the field of connectors, in particular to an ultra-small sealed high-temperature and high-voltage connector which comprises an outer shell, an inner conductor and an insulating material, wherein the insulating material is arranged between the outer shell and the inner conductor; a pressure bearing table is arranged on the inner conductor at the pressure bearing end of the insulating material; and special adhesives are coated among the outer shell, the inner conductor and the insulating material. The coating of the special adhesive can solve the problem that the connector is loosened in the pressure bearing process or gaps are generated between the inner wall of the outer shell and the insulating material and the inner conductor, so that the sealing performance and the insulating performance are reduced.
Description
Technical Field
The invention relates to the field of connectors, in particular to an ultra-small sealed high-temperature and high-pressure connector.
Background
Most of high-temperature and high-pressure sealing connectors used by various well logging companies in China depend on imports, the price is high, the single-needle or multi-needle high-temperature and high-pressure sealing connectors basically adopt the processes of ceramic sintering or glass sintering, bonding and the like, and because the coefficients of linear expansion of the shell, the inner conductor and the insulating material are inconsistent in the sintering process, the bonding glue or the sintering material can deform under high temperature and high pressure, so that small gaps can be generated among the shell, the insulating material and the inner conductor, the sealing is poor and the leakage is caused, the sealing performance and the insulating performance of the connector are reduced, and the connector cannot be normally used.
Disclosure of Invention
In view of the above problems, the present invention provides a super-small sealed high-temperature high-voltage connector, which includes an outer housing, an inner conductor, and an insulating material, wherein the insulating material is disposed between the outer housing and the inner conductor; and a pressure bearing platform is arranged on the inner conductor and positioned at the pressure bearing end of the insulating material.
Preferably, a special adhesive is coated between the outer shell and the inner conductor and between the inner conductor and the insulating material.
Preferably, the thickness of the adhesive after drying is 2-10 μm.
Preferably, the special adhesive comprises the following components in parts by weight:
100 parts of bismaleimide modified resin, 20-40 parts of linear phenolic resin, 5-10 parts of metal oxide powder, 3-10 parts of polyvinyl alcohol, 0.1-5 parts of dispersing agent and 30-80 parts of organic solvent.
Preferably, the insulating material is prepared from a modified polytetramethylene adipamide material, and the modified polytetramethylene adipamide material is obtained by modifying polytetramethylene adipamide with an organic zirconium/halloysite nanotube.
Preferably, the metal oxide powder comprises one or more of titanium oxide, magnesium oxide, zirconium oxide or zinc oxide.
Preferably, the organic solvent is N-phenylmaleimide or N-methylpyrrolidone.
Preferably, the bismaleimide modified resin is obtained by modifying bismaleimide resin through modified halloysite nanotubes and bisphenol A epoxy resin.
Preferably, the preparation method of the modified halloysite nanotube comprises the following steps:
s1, weighing 2-pyridinecarboxamide, adding the 2-pyridinecarboxamide into N, N-dimethylformamide, and stirring the mixture uniformly to obtain a 2-pyridinecarboxamide solution; weighing potassium permanganate, adding the potassium permanganate into deionized water, stirring the mixture evenly, and then dropwise adding dilute sulfuric acid to adjust the pH of the solution to 2.0-3.0 to obtain an acidic potassium permanganate solution;
wherein in the 2-pyridine formamide solution, the mass ratio of 2-pyridine formamide to N, N-dimethylformamide is 1: 8-12; in the acidic potassium permanganate solution, the mass ratio of potassium permanganate to deionized water is 1: 20-30;
s2, weighing halloysite nanotubes, adding the halloysite nanotubes into deionized water, dropwise adding vinyl trimethoxy silane, ultrasonically dispersing until the mixture is uniform, then dropwise adding the acidic potassium permanganate solution, heating to 50-60 ℃, stirring for 3-5 hours, cooling to room temperature, filtering to obtain a solid, washing with purified water until the washing liquid is neutral, filtering again to obtain the solid, and drying at 80-100 ℃ to obtain the carboxylated halloysite nanotubes;
wherein the mass ratio of the halloysite nanotube to the vinyl trimethoxy silane to the deionized water to the acidic potassium permanganate solution is 1: 0.01-0.02: 8-10: 0.1-0.3;
s3, weighing the carboxylated halloysite nanotube, adding the carboxylated halloysite nanotube into the 2-pyridinecarboxamide solution, ultrasonically dispersing until the mixture is uniform, adding triethylamine, stirring and reacting for 5-10 hours at room temperature, filtering to obtain a solid, washing the solid with purified water until the washing liquid is neutral, washing the solid with dichloromethane for three times, and drying the solid under reduced pressure to obtain a modified halloysite nanotube;
wherein the mass ratio of the carboxylated halloysite nanotube to the triethylamine to the 2-pyridinecarboxamide solution is 1: 0.05-0.1: 10-15.
Preferably, the preparation method of the bismaleimide modified resin comprises the following steps:
s1, weighing bismaleimide resin, adding the bismaleimide resin into DMF (dimethyl formamide), stirring until the bismaleimide resin is completely dissolved, adding a modified halloysite nanotube, heating to 80-120 ℃, stirring for 5-10 hours, filtering to obtain a solid, and washing with trichloromethane for three times to obtain the modified halloysite nanotube grafted with bismaleimide;
wherein the mass ratio of the bismaleimide resin to the modified halloysite nanotube to the DMF is 1: 0.1-0.3: 5-10;
s2, weighing bisphenol A epoxy resin, heating to 60-70 ℃, adding bismaleimide resin, stirring uniformly, adding the modified halloysite nanotube grafted with bismaleimide, heating to 80-120 ℃, and stirring for 3-5 hours to obtain bismaleimide modified resin;
wherein the mass ratio of the bisphenol A epoxy resin to the bismaleimide resin to the modified halloysite nanotube grafted with bismaleimide is 1: 4-6: 0.05-0.2.
Preferably, the preparation steps of the special adhesive are as follows:
firstly, weighing 100 parts of bismaleimide modified resin, 20-40 parts of linear phenolic resin, 5-10 parts of metal oxide powder, 3-10 parts of polyvinyl alcohol, 0.1-5 parts of dispersing agent and 30-80 parts of organic solvent.
Secondly, adding the weighed bismaleimide modified resin and the weighed linear phenolic resin into a mixing stirrer, and stirring and reacting for 0.5-1 h at the temperature of 120-150 ℃ under the stirring condition to obtain a resin premix;
thirdly, adding the weighed metal oxide powder, polyvinyl alcohol and a dispersing agent into an organic solvent, stirring and carrying out ultrasonic treatment for 0.5-1 h to obtain an additive premix;
and fourthly, putting the additive premix and the resin premix into a mixing roll, and blending for 0.5-1 h at the temperature of 100-125 ℃ to obtain the special adhesive.
Preferably, the preparation method of the insulating material comprises the following steps:
s1, weighing zirconium acetylacetonate, adding the zirconium acetylacetonate into acetone, and stirring until the zirconium acetylacetonate is completely dissolved to obtain a zirconium acetylacetonate solution; weighing halloysite nanotubes, adding the halloysite nanotubes into ethanol, and performing ultrasonic dispersion until the mixture is uniform to obtain a halloysite nanotube dispersion solution;
wherein the mass ratio of the zirconium acetylacetonate to the acetone is 1: 5-7; the mass ratio of the halloysite nanotube to the ethanol is 1: 6-10;
s2, adding sodium ethoxide into the halloysite nanotube dispersion liquid, stirring until the mixture is uniform, heating to 70-80 ℃ under the protection of inert gas, dropwise adding a zirconium acetylacetonate solution, carrying out reflux reaction for 4-6 hours after the dropwise addition is finished, cooling to room temperature, and filtering to obtain a solid substance to obtain an organic zirconium/halloysite nanotube;
wherein the mass ratio of the halloysite nanotube dispersion liquid to the sodium ethoxide to the zirconium acetylacetonate solution is 1: 0.02-0.04: 0.5-0.8;
s3, putting the dried polytetramethylene adipamide into a high-speed stirrer, putting the organic zirconium/halloysite nanotube into the stirrer, melting and mixing the materials uniformly, transferring the materials into a double-screw extruder, extruding and granulating the materials to obtain a modified polytetramethylene adipamide material, namely an insulating material;
wherein the mass ratio of the polytetramethyleneadipamide to the organic zirconium/halloysite nanotubes is 1: 0.05-0.1.
The invention has the beneficial effects that:
1. the invention provides a super-small sealed high-temperature and high-pressure connector which comprises an outer shell, an inner conductor and an insulating material, wherein a pressure bearing table is arranged on the inner conductor and positioned at a pressure bearing end of the insulating material, the pressure bearing table can bear pressure when in use, and special adhesives with excellent bonding performance are coated on the bonding surfaces of the outer shell, the inner conductor and the insulating material. The coating of the special adhesive can solve the problem that the connector is loosened in the pressure bearing process or gaps are generated between the inner wall of the outer shell and the insulating material and the inner conductor, so that the sealing performance and the insulating performance are reduced.
2. The bismaleimide serving as a resin matrix of an advanced composite material has the advantages of good heat resistance, high strength, higher elastic modulus, proper hardness, good bonding property with inorganic matters and the like. However, the bismaleimide resin has problems that the cured product thereof is brittle due to high crosslinking density, low tensile strength, poor impact resistance, and the like, as in many thermosetting resins. The toughness of the bismaleimide resin condensate can be improved to a certain extent through modification of allyl compounds, epoxy resins, cyanate esters and the like, but the high requirements of advanced components on material hardness, strength and heat resistance cannot be met at the same time.
The halloysite nanotube is a natural nanotube material, silicate in molecules forms a unique halloysite nanotube layer, the pipe layer is inwards rolled by twenty-several layers to form a tubular structure, the unique structure enables the halloysite nanotube to have a large specific surface area, and the pipe layer surface of the halloysite nanotube contains a large amount of hydroxyl groups. In the modification process of bismaleimide, the modified halloysite nanotube is combined with bismaleimide, so that more maleimide can be adsorbed and grafted on the surface of the halloysite nanotube, the tube layer structure of the halloysite nanotube is fully exerted, and the phenomenon of peeling after damp and hot can be avoided. The modified halloysite nanotube can be grafted with bismaleimide more stably, exerts more excellent properties, and can play a great improvement role in the mechanical properties and toughness of the bismaleimide.
3. In addition, the halloysite nanotube is subjected to organic zirconium modification and then is combined with polytetramethylene adipamide to prepare the insulating material with excellent performance.
Currently, various insulating materials are prepared on the basis of polytetramethylene adipamide resin, and the polytetramethylene adipamide resin has high melting point and high crystallinity, and the chemical chain structure of the polytetramethylene adipamide resin is highly symmetrical, so that the polytetramethylene adipamide resin has extremely high crystallinity and higher melting point. However, the amide bond in the molecule of the polytetramethylene adipamide has higher water absorption, the performance of the polytetramethylene adipamide is greatly influenced under the conditions of high temperature, high pressure and moist heat, and meanwhile, the flame retardant property of the polytetramethylene adipamide resin is poorer, so that the polytetramethylene adipamide resin is limited to a certain extent in the application aspects of electronic appliances and the like due to the defects.
According to the invention, the halloysite with high adsorbability and large specific surface area is used for organic zirconium modification to obtain the flame-retardant and water-repellent additive, and the flame-retardant and water-absorbent performance of the polytetramethylene adipamide can be greatly improved after the flame-retardant additive is combined with the polytetramethylene adipamide. The preparation method comprises the following specific steps of adding sodium ethoxide with strong alkalinity into zirconium acetylacetonate, decomposing acetyl groups to form organic zirconium with ester groups, grafting and adsorbing the organic zirconium on the surface of halloysite, and enabling the halloysite nanotube to have a large specific surface area.
Drawings
The invention is further illustrated by means of the attached drawings, but the embodiments in the drawings do not constitute any limitation to the invention, and for a person skilled in the art, other drawings can be obtained on the basis of the following drawings without inventive effort.
FIG. 1 is a schematic view of a super-miniature hermetic high-temperature high-pressure connector according to the present invention;
reference numerals: the outer casing 1, inner conductor 2, insulating material 3 and pressure-bearing platform 4.
Detailed Description
The invention is further described with reference to the following examples.
Example 1
A super-small sealed high-temperature high-voltage connector comprises an outer shell 1, an inner conductor 2 and an insulating material 3, wherein the insulating material 3 is arranged between the outer shell 1 and the inner conductor 2; and a pressure bearing platform 4 is arranged at the pressure bearing end of the insulating material 3 on the inner conductor 2.
Special adhesives are coated between the outer shell 1 and the inner conductor 2 and between the inner conductor 2 and the insulating material 3.
The special adhesive comprises the following components in parts by weight:
100 parts of bismaleimide modified resin, 30 parts of linear phenolic resin, 8 parts of metal oxide powder, 7 parts of polyvinyl alcohol, 2 parts of dispersant and 50 parts of organic solvent.
The insulating material 3 is prepared from a modified polytetramethylene adipamide material, and the modified polytetramethylene adipamide material is obtained by modifying polytetramethylene adipamide with an organic zirconium/halloysite nanotube.
The metal oxide powder is prepared by mixing titanium oxide, magnesium oxide, zirconium oxide and zinc oxide according to the mass ratio of 1: 0.3: 0.7: 0.2.
The organic solvent is N-phenyl maleimide.
The bismaleimide modified resin is obtained by modifying bismaleimide resin through a modified halloysite nanotube and bisphenol A epoxy resin.
The preparation method of the modified halloysite nanotube comprises the following steps:
s1, weighing 2-pyridinecarboxamide, adding the 2-pyridinecarboxamide into N, N-dimethylformamide, and stirring the mixture uniformly to obtain a 2-pyridinecarboxamide solution; weighing potassium permanganate, adding the potassium permanganate into deionized water, stirring the mixture evenly, and then dropwise adding dilute sulfuric acid to adjust the pH of the solution to 2.0-3.0 to obtain an acidic potassium permanganate solution;
wherein in the 2-pyridine formamide solution, the mass ratio of 2-pyridine formamide to N, N-dimethylformamide is 1: 8-12; in the acidic potassium permanganate solution, the mass ratio of potassium permanganate to deionized water is 1: 20-30;
s2, weighing halloysite nanotubes, adding the halloysite nanotubes into deionized water, dropwise adding vinyl trimethoxy silane, ultrasonically dispersing until the mixture is uniform, then dropwise adding the acidic potassium permanganate solution, heating to 50-60 ℃, stirring for 3-5 hours, cooling to room temperature, filtering to obtain a solid, washing with purified water until the washing liquid is neutral, filtering again to obtain the solid, and drying at 80-100 ℃ to obtain the carboxylated halloysite nanotubes;
wherein the mass ratio of the halloysite nanotube to the vinyl trimethoxy silane to the deionized water to the acidic potassium permanganate solution is 1: 0.01-0.02: 8-10: 0.1-0.3;
s3, weighing the carboxylated halloysite nanotube, adding the carboxylated halloysite nanotube into the 2-pyridinecarboxamide solution, ultrasonically dispersing until the mixture is uniform, adding triethylamine, stirring and reacting for 5-10 hours at room temperature, filtering to obtain a solid, washing the solid with purified water until the washing liquid is neutral, washing the solid with dichloromethane for three times, and drying the solid under reduced pressure to obtain a modified halloysite nanotube;
wherein the mass ratio of the carboxylated halloysite nanotube to the triethylamine to the 2-pyridinecarboxamide solution is 1: 0.05-0.1: 10-15.
The preparation method of the bismaleimide modified resin comprises the following steps:
s1, weighing bismaleimide resin, adding the bismaleimide resin into DMF (dimethyl formamide), stirring until the bismaleimide resin is completely dissolved, adding a modified halloysite nanotube, heating to 80-120 ℃, stirring for 5-10 hours, filtering to obtain a solid, and washing with trichloromethane for three times to obtain the modified halloysite nanotube grafted with bismaleimide;
wherein the mass ratio of the bismaleimide resin to the modified halloysite nanotube to the DMF is 1: 0.1-0.3: 5-10;
s2, weighing bisphenol A epoxy resin, heating to 60-70 ℃, adding bismaleimide resin, stirring uniformly, adding the modified halloysite nanotube grafted with bismaleimide, heating to 80-120 ℃, and stirring for 3-5 hours to obtain bismaleimide modified resin;
wherein the mass ratio of the bisphenol A epoxy resin to the bismaleimide resin to the modified halloysite nanotube grafted with bismaleimide is 1: 4-6: 0.05-0.2.
The preparation steps of the special adhesive are as follows:
firstly, weighing 100 parts of bismaleimide modified resin, 30 parts of linear phenolic resin, 8 parts of metal oxide powder, 7 parts of polyvinyl alcohol, 2 parts of a dispersing agent and 50 parts of an organic solvent;
secondly, adding the weighed bismaleimide modified resin and the weighed linear phenolic resin into a mixing stirrer, and stirring and reacting for 0.5-1 h at the temperature of 120-150 ℃ under the stirring condition to obtain a resin premix;
thirdly, adding the weighed metal oxide powder, polyvinyl alcohol and a dispersing agent into an organic solvent, stirring and carrying out ultrasonic treatment for 0.5-1 h to obtain an additive premix;
and fourthly, putting the additive premix and the resin premix into a mixing roll, and blending for 0.5-1 h at the temperature of 100-125 ℃ to obtain the special adhesive.
The preparation method of the insulating material 3 comprises the following steps:
s1, weighing zirconium acetylacetonate, adding the zirconium acetylacetonate into acetone, and stirring until the zirconium acetylacetonate is completely dissolved to obtain a zirconium acetylacetonate solution; weighing halloysite nanotubes, adding the halloysite nanotubes into ethanol, and performing ultrasonic dispersion until the mixture is uniform to obtain a halloysite nanotube dispersion solution;
wherein the mass ratio of the zirconium acetylacetonate to the acetone is 1: 5-7; the mass ratio of the halloysite nanotube to the ethanol is 1: 6-10;
s2, adding sodium ethoxide into the halloysite nanotube dispersion liquid, stirring until the mixture is uniform, heating to 70-80 ℃ under the protection of inert gas, dropwise adding a zirconium acetylacetonate solution, carrying out reflux reaction for 4-6 hours after the dropwise addition is finished, cooling to room temperature, and filtering to obtain a solid substance to obtain an organic zirconium/halloysite nanotube;
wherein the mass ratio of the halloysite nanotube dispersion liquid to the sodium ethoxide to the zirconium acetylacetonate solution is 1: 0.02-0.04: 0.5-0.8;
s3, putting the dried polytetramethylene adipamide into a high-speed stirrer, putting the organic zirconium/halloysite nanotube into the stirrer, melting and mixing the materials uniformly, transferring the materials into a double-screw extruder, extruding and granulating the materials to obtain a modified polytetramethylene adipamide material, namely an insulating material;
wherein the mass ratio of the polytetramethyleneadipamide to the organic zirconium/halloysite nanotubes is 1: 0.08.
Example 2
A super-small sealed high-temperature high-voltage connector comprises an outer shell 1, an inner conductor 2 and an insulating material 3, wherein the insulating material 3 is arranged between the outer shell 1 and the inner conductor 2; and a pressure bearing platform 4 is arranged at the pressure bearing end of the insulating material 3 on the inner conductor 2.
Special adhesives are coated between the outer shell 1 and the inner conductor 2 and between the inner conductor 2 and the insulating material 3.
The special adhesive comprises the following components in parts by weight:
100 parts of bismaleimide modified resin, 20 parts of linear phenolic resin, 5 parts of metal oxide powder, 3 parts of polyvinyl alcohol, 0.1 part of dispersant and 30 parts of organic solvent.
The insulating material 3 is prepared from a modified polytetramethylene adipamide material, and the modified polytetramethylene adipamide material is obtained by modifying polytetramethylene adipamide with an organic zirconium/halloysite nanotube.
The metal oxide powder is titanium oxide.
The organic solvent is N-methyl pyrrolidone.
The bismaleimide modified resin is obtained by modifying bismaleimide resin through a modified halloysite nanotube and bisphenol A epoxy resin.
The preparation method of the modified halloysite nanotube comprises the following steps:
s1, weighing 2-pyridinecarboxamide, adding the 2-pyridinecarboxamide into N, N-dimethylformamide, and stirring the mixture uniformly to obtain a 2-pyridinecarboxamide solution; weighing potassium permanganate, adding the potassium permanganate into deionized water, stirring the mixture evenly, and then dropwise adding dilute sulfuric acid to adjust the pH of the solution to 2.0-3.0 to obtain an acidic potassium permanganate solution;
wherein in the 2-pyridine formamide solution, the mass ratio of 2-pyridine formamide to N, N-dimethylformamide is 1: 8-12; in the acidic potassium permanganate solution, the mass ratio of potassium permanganate to deionized water is 1: 20-30;
s2, weighing halloysite nanotubes, adding the halloysite nanotubes into deionized water, dropwise adding vinyl trimethoxy silane, ultrasonically dispersing until the mixture is uniform, then dropwise adding the acidic potassium permanganate solution, heating to 50-60 ℃, stirring for 3-5 hours, cooling to room temperature, filtering to obtain a solid, washing with purified water until the washing liquid is neutral, filtering again to obtain the solid, and drying at 80-100 ℃ to obtain the carboxylated halloysite nanotubes;
wherein the mass ratio of the halloysite nanotube to the vinyl trimethoxy silane to the deionized water to the acidic potassium permanganate solution is 1: 0.01-0.02: 8-10: 0.1-0.3;
s3, weighing the carboxylated halloysite nanotube, adding the carboxylated halloysite nanotube into the 2-pyridinecarboxamide solution, ultrasonically dispersing until the mixture is uniform, adding triethylamine, stirring and reacting for 5-10 hours at room temperature, filtering to obtain a solid, washing the solid with purified water until the washing liquid is neutral, washing the solid with dichloromethane for three times, and drying the solid under reduced pressure to obtain a modified halloysite nanotube;
wherein the mass ratio of the carboxylated halloysite nanotube to the triethylamine to the 2-pyridinecarboxamide solution is 1: 0.05-0.1: 10-15.
The preparation method of the bismaleimide modified resin comprises the following steps:
s1, weighing bismaleimide resin, adding the bismaleimide resin into DMF (dimethyl formamide), stirring until the bismaleimide resin is completely dissolved, adding a modified halloysite nanotube, heating to 80-120 ℃, stirring for 5-10 hours, filtering to obtain a solid, and washing with trichloromethane for three times to obtain the modified halloysite nanotube grafted with bismaleimide;
wherein the mass ratio of the bismaleimide resin to the modified halloysite nanotube to the DMF is 1: 0.1-0.3: 5-10;
s2, weighing bisphenol A epoxy resin, heating to 60-70 ℃, adding bismaleimide resin, stirring uniformly, adding the modified halloysite nanotube grafted with bismaleimide, heating to 80-120 ℃, and stirring for 3-5 hours to obtain bismaleimide modified resin;
wherein the mass ratio of the bisphenol A epoxy resin to the bismaleimide resin to the modified halloysite nanotube grafted with bismaleimide is 1: 4-6: 0.05-0.2.
The preparation steps of the special adhesive are as follows:
firstly, weighing 100 parts of bismaleimide modified resin, 20-40 parts of linear phenolic resin, 5-10 parts of metal oxide powder, 3-10 parts of polyvinyl alcohol, 0.1-5 parts of dispersing agent and 30-80 parts of organic solvent according to the weight.
Secondly, adding the weighed bismaleimide modified resin and the weighed linear phenolic resin into a mixing stirrer, and stirring and reacting for 0.5-1 h at the temperature of 120-150 ℃ under the stirring condition to obtain a resin premix;
thirdly, adding the weighed metal oxide powder, polyvinyl alcohol and a dispersing agent into an organic solvent, stirring and carrying out ultrasonic treatment for 0.5-1 h to obtain an additive premix;
and fourthly, putting the additive premix and the resin premix into a mixing roll, and blending for 0.5-1 h at the temperature of 100-125 ℃ to obtain the special adhesive.
The preparation method of the insulating material 3 comprises the following steps:
s1, weighing zirconium acetylacetonate, adding the zirconium acetylacetonate into acetone, and stirring until the zirconium acetylacetonate is completely dissolved to obtain a zirconium acetylacetonate solution; weighing halloysite nanotubes, adding the halloysite nanotubes into ethanol, and performing ultrasonic dispersion until the mixture is uniform to obtain a halloysite nanotube dispersion solution;
wherein the mass ratio of the zirconium acetylacetonate to the acetone is 1: 5-7; the mass ratio of the halloysite nanotube to the ethanol is 1: 6-10;
s2, adding sodium ethoxide into the halloysite nanotube dispersion liquid, stirring until the mixture is uniform, heating to 70-80 ℃ under the protection of inert gas, dropwise adding a zirconium acetylacetonate solution, carrying out reflux reaction for 4-6 hours after the dropwise addition is finished, cooling to room temperature, and filtering to obtain a solid substance to obtain an organic zirconium/halloysite nanotube;
wherein the mass ratio of the halloysite nanotube dispersion liquid to the sodium ethoxide to the zirconium acetylacetonate solution is 1: 0.02-0.04: 0.5-0.8;
s3, putting the dried polytetramethylene adipamide into a high-speed stirrer, putting the organic zirconium/halloysite nanotube into the stirrer, melting and mixing the materials uniformly, transferring the materials into a double-screw extruder, extruding and granulating the materials to obtain a modified polytetramethylene adipamide material, namely an insulating material;
wherein the mass ratio of the polytetramethyleneadipamide to the organic zirconium/halloysite nanotubes is 1: 0.05.
Example 3
A super-small sealed high-temperature high-voltage connector comprises an outer shell 1, an inner conductor 2 and an insulating material 3, wherein the insulating material 3 is arranged between the outer shell 1 and the inner conductor 2; and a pressure bearing platform 4 is arranged at the pressure bearing end of the insulating material 3 on the inner conductor 2.
Special adhesives are coated between the outer shell 1 and the inner conductor 2 and between the inner conductor 2 and the insulating material 3.
The special adhesive comprises the following components in parts by weight:
100 parts of bismaleimide modified resin, 40 parts of linear phenolic resin, 10 parts of metal oxide powder, 10 parts of polyvinyl alcohol, 5 parts of dispersant and 80 parts of organic solvent.
The insulating material 3 is prepared from a modified polytetramethylene adipamide material, and the modified polytetramethylene adipamide material is obtained by modifying polytetramethylene adipamide with an organic zirconium/halloysite nanotube.
The metal oxide powder is obtained by mixing titanium oxide and zirconium oxide according to the mass ratio of 1: 0.5.
The organic solvent is N-phenyl maleimide or N-methyl pyrrolidone.
The bismaleimide modified resin is obtained by modifying bismaleimide resin through a modified halloysite nanotube and bisphenol A epoxy resin.
The preparation method of the modified halloysite nanotube comprises the following steps:
s1, weighing 2-pyridinecarboxamide, adding the 2-pyridinecarboxamide into N, N-dimethylformamide, and stirring the mixture uniformly to obtain a 2-pyridinecarboxamide solution; weighing potassium permanganate, adding the potassium permanganate into deionized water, stirring the mixture evenly, and then dropwise adding dilute sulfuric acid to adjust the pH of the solution to 2.0-3.0 to obtain an acidic potassium permanganate solution;
wherein in the 2-pyridine formamide solution, the mass ratio of 2-pyridine formamide to N, N-dimethylformamide is 1: 8-12; in the acidic potassium permanganate solution, the mass ratio of potassium permanganate to deionized water is 1: 20-30;
s2, weighing halloysite nanotubes, adding the halloysite nanotubes into deionized water, dropwise adding vinyl trimethoxy silane, ultrasonically dispersing until the mixture is uniform, then dropwise adding the acidic potassium permanganate solution, heating to 50-60 ℃, stirring for 3-5 hours, cooling to room temperature, filtering to obtain a solid, washing with purified water until the washing liquid is neutral, filtering again to obtain the solid, and drying at 80-100 ℃ to obtain the carboxylated halloysite nanotubes;
wherein the mass ratio of the halloysite nanotube to the vinyl trimethoxy silane to the deionized water to the acidic potassium permanganate solution is 1: 0.01-0.02: 8-10: 0.1-0.3;
s3, weighing the carboxylated halloysite nanotube, adding the carboxylated halloysite nanotube into the 2-pyridinecarboxamide solution, ultrasonically dispersing until the mixture is uniform, adding triethylamine, stirring and reacting for 5-10 hours at room temperature, filtering to obtain a solid, washing the solid with purified water until the washing liquid is neutral, washing the solid with dichloromethane for three times, and drying the solid under reduced pressure to obtain a modified halloysite nanotube;
wherein the mass ratio of the carboxylated halloysite nanotube to the triethylamine to the 2-pyridinecarboxamide solution is 1: 0.05-0.1: 10-15.
The preparation method of the bismaleimide modified resin comprises the following steps:
s1, weighing bismaleimide resin, adding the bismaleimide resin into DMF (dimethyl formamide), stirring until the bismaleimide resin is completely dissolved, adding a modified halloysite nanotube, heating to 80-120 ℃, stirring for 5-10 hours, filtering to obtain a solid, and washing with trichloromethane for three times to obtain the modified halloysite nanotube grafted with bismaleimide;
wherein the mass ratio of the bismaleimide resin to the modified halloysite nanotube to the DMF is 1: 0.1-0.3: 5-10;
s2, weighing bisphenol A epoxy resin, heating to 60-70 ℃, adding bismaleimide resin, stirring uniformly, adding the modified halloysite nanotube grafted with bismaleimide, heating to 80-120 ℃, and stirring for 3-5 hours to obtain bismaleimide modified resin;
wherein the mass ratio of the bisphenol A epoxy resin to the bismaleimide resin to the modified halloysite nanotube grafted with bismaleimide is 1: 4-6: 0.05-0.2.
The preparation steps of the special adhesive are as follows:
firstly, weighing 100 parts of bismaleimide modified resin, 40 parts of linear phenolic resin, 10 parts of metal oxide powder, 10 parts of polyvinyl alcohol, 5 parts of dispersing agent and 80 parts of organic solvent.
Secondly, adding the weighed bismaleimide modified resin and the weighed linear phenolic resin into a mixing stirrer, and stirring and reacting for 0.5-1 h at the temperature of 120-150 ℃ under the stirring condition to obtain a resin premix;
thirdly, adding the weighed metal oxide powder, polyvinyl alcohol and a dispersing agent into an organic solvent, stirring and carrying out ultrasonic treatment for 0.5-1 h to obtain an additive premix;
and fourthly, putting the additive premix and the resin premix into a mixing roll, and blending for 0.5-1 h at the temperature of 100-125 ℃ to obtain the special adhesive.
The preparation method of the insulating material 3 comprises the following steps:
s1, weighing zirconium acetylacetonate, adding the zirconium acetylacetonate into acetone, and stirring until the zirconium acetylacetonate is completely dissolved to obtain a zirconium acetylacetonate solution; weighing halloysite nanotubes, adding the halloysite nanotubes into ethanol, and performing ultrasonic dispersion until the mixture is uniform to obtain a halloysite nanotube dispersion solution;
wherein the mass ratio of the zirconium acetylacetonate to the acetone is 1: 5-7; the mass ratio of the halloysite nanotube to the ethanol is 1: 6-10;
s2, adding sodium ethoxide into the halloysite nanotube dispersion liquid, stirring until the mixture is uniform, heating to 70-80 ℃ under the protection of inert gas, dropwise adding a zirconium acetylacetonate solution, carrying out reflux reaction for 4-6 hours after the dropwise addition is finished, cooling to room temperature, and filtering to obtain a solid substance to obtain an organic zirconium/halloysite nanotube;
wherein the mass ratio of the halloysite nanotube dispersion liquid to the sodium ethoxide to the zirconium acetylacetonate solution is 1: 0.02-0.04: 0.5-0.8;
s3, putting the dried polytetramethylene adipamide into a high-speed stirrer, putting the organic zirconium/halloysite nanotube into the stirrer, melting and mixing the materials uniformly, transferring the materials into a double-screw extruder, extruding and granulating the materials to obtain a modified polytetramethylene adipamide material, namely an insulating material;
wherein the mass ratio of the polytetramethyleneadipamide to the organic zirconium/halloysite nanotubes is 1: 0.1.
Comparative example
The special adhesive comprises the following components in parts by weight:
100 parts of bismaleimide modified resin, 30 parts of linear phenolic resin, 8 parts of metal oxide powder, 7 parts of polyvinyl alcohol, 2 parts of dispersant and 50 parts of organic solvent.
The metal oxide powder is prepared by mixing titanium oxide, magnesium oxide, zirconium oxide and zinc oxide according to the mass ratio of 1: 0.3: 0.7: 0.2.
The organic solvent is N-phenyl maleimide.
The bismaleimide modified resin is obtained by modifying bismaleimide resin through bisphenol A epoxy resin.
The preparation method of the bismaleimide modified resin comprises the following steps:
weighing bisphenol A epoxy resin, heating to 60-70 ℃, adding bismaleimide resin, stirring to be uniform, continuing to heat to 80-120 ℃, and stirring for 3-5 hours to obtain bismaleimide modified resin;
wherein the mass ratio of the bisphenol A epoxy resin to the bismaleimide resin to the modified halloysite nanotube grafted with bismaleimide is 1: 4-6: 0.05-0.2.
The preparation steps of the special adhesive are as follows:
firstly, weighing 100 parts of bismaleimide modified resin, 30 parts of linear phenolic resin, 8 parts of metal oxide powder, 7 parts of polyvinyl alcohol, 2 parts of a dispersing agent and 50 parts of an organic solvent;
secondly, adding the weighed bismaleimide modified resin and the weighed linear phenolic resin into a mixing stirrer, and stirring and reacting for 0.5-1 h at the temperature of 120-150 ℃ under the stirring condition to obtain a resin premix;
thirdly, adding the weighed metal oxide powder, polyvinyl alcohol and a dispersing agent into an organic solvent, stirring and carrying out ultrasonic treatment for 0.5-1 h to obtain an additive premix;
and fourthly, putting the additive premix and the resin premix into a mixing roll, and blending for 0.5-1 h at the temperature of 100-125 ℃ to obtain the special adhesive.
For a clearer illustration of the present invention, the special adhesives prepared in examples 1 to 3 and comparative example were tested and compared. The method specifically comprises the following steps: the special adhesive is sprayed or brushed on the surface of a polytetramethylene adipamide base material (marked as a base material I) and the surface of an alumina ceramic base material (marked as a base material II) in a ventilated environment, the special adhesive is cured according to the process of 150 ℃/1h +180 ℃/1h +220 ℃/2h, the thickness of the test adhesive after curing is 5-6 mu m, and the test of the thickness of the adhesive refers to GBT 13452.2.
Wherein the adhesion is measured by cross hatch method (GB/T9286); impact resistance (toughness) was tested according to GB 1732; hardness was measured by the pencil method (GB 6739); the humidity and heat resistance is detected after 30 days of treatment under the conditions of 60 ℃ and 95-100% of humidity; the high temperature resistance was measured after treatment in an oven at 250 ℃ for 500 hours.
The results are shown in Table 1.
TABLE 1 Performance testing of different adhesives
The insulation materials prepared in examples 1 to 3 and comparative example were compared with the existing commercial material polytetramethylene adipamide line test, wherein the flame retardancy was determined according to the oxygen index, and the test of the oxygen index was performed according to the standard ASTM D2863-77, and the results are shown in Table 2.
TABLE 2 Property measurements of insulating materials
| Example 1 | Example 2 | Example 3 | Polytetramethylene adipamide | |
| Oxygen index/% | 31.2 | 28.7 | 30.4 | 24.6 |
| Water absorption/%) | 0.12 | 0.17 | 0.11 | 2.03 |
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A super-small sealed high-temperature and high-voltage connector comprises an outer shell, an inner conductor and an insulating material, and is characterized in that the insulating material is arranged between the outer shell and the inner conductor; a pressure bearing table is arranged on the inner conductor at the pressure bearing end of the insulating material; and special adhesives are coated between the outer shell and the inner conductor and between the inner conductor and the insulating material.
2. The ultra-small sealed high-temperature high-pressure connector according to claim 1, wherein the special adhesive comprises the following components in parts by weight:
100 parts of bismaleimide modified resin, 20-40 parts of linear phenolic resin, 5-10 parts of metal oxide powder, 3-10 parts of polyvinyl alcohol, 0.1-5 parts of dispersing agent and 30-80 parts of organic solvent.
3. The ultra-small sealed high temperature and high pressure connector of claim 2, wherein the metal oxide powder comprises one or more of titanium oxide, magnesium oxide, zirconium oxide, or zinc oxide.
4. The ultra-small sealed high-temperature high-pressure connector according to claim 2, wherein the organic solvent is N-phenylmaleimide or N-methylpyrrolidone.
5. The ultra-small sealed high-temperature high-pressure connector according to claim 2, wherein the bismaleimide resin is obtained by modifying a bismaleimide resin with a modified halloysite nanotube and a bisphenol a epoxy resin.
6. The ultra-small sealed high-temperature high-pressure connector of claim 5, wherein the modified halloysite nanotubes are prepared by the following steps:
s1, weighing 2-pyridinecarboxamide, adding the 2-pyridinecarboxamide into N, N-dimethylformamide, and stirring the mixture uniformly to obtain a 2-pyridinecarboxamide solution; weighing potassium permanganate, adding the potassium permanganate into deionized water, stirring the mixture evenly, and then dropwise adding dilute sulfuric acid to adjust the pH of the solution to 2.0-3.0 to obtain an acidic potassium permanganate solution;
wherein in the 2-pyridine formamide solution, the mass ratio of 2-pyridine formamide to N, N-dimethylformamide is 1: 8-12; in the acidic potassium permanganate solution, the mass ratio of potassium permanganate to deionized water is 1: 20-30;
s2, weighing halloysite nanotubes, adding the halloysite nanotubes into deionized water, dropwise adding vinyl trimethoxy silane, ultrasonically dispersing until the mixture is uniform, then dropwise adding the acidic potassium permanganate solution, heating to 50-60 ℃, stirring for 3-5 hours, cooling to room temperature, filtering to obtain a solid, washing with purified water until the washing liquid is neutral, filtering again to obtain the solid, and drying at 80-100 ℃ to obtain the carboxylated halloysite nanotubes;
wherein the mass ratio of the halloysite nanotube to the vinyl trimethoxy silane to the deionized water to the acidic potassium permanganate solution is 1: 0.01-0.02: 8-10: 0.1-0.3;
s3, weighing the carboxylated halloysite nanotube, adding the carboxylated halloysite nanotube into the 2-pyridinecarboxamide solution, ultrasonically dispersing until the mixture is uniform, adding triethylamine, stirring and reacting for 5-10 hours at room temperature, filtering to obtain a solid, washing the solid with purified water until the washing liquid is neutral, washing the solid with dichloromethane for three times, and drying the solid under reduced pressure to obtain a modified halloysite nanotube;
wherein the mass ratio of the carboxylated halloysite nanotube to the triethylamine to the 2-pyridinecarboxamide solution is 1: 0.05-0.1: 10-15.
7. The ultra-small sealed high-temperature high-pressure connector according to claim 4, wherein the bismaleimide modified resin is prepared by a method comprising:
s1, weighing bismaleimide resin, adding the bismaleimide resin into DMF (dimethyl formamide), stirring until the bismaleimide resin is completely dissolved, adding a modified halloysite nanotube, heating to 80-120 ℃, stirring for 5-10 hours, filtering to obtain a solid, and washing with trichloromethane for three times to obtain the modified halloysite nanotube grafted with bismaleimide;
wherein the mass ratio of the bismaleimide resin to the modified halloysite nanotube to the DMF is 1: 0.1-0.3: 5-10;
s2, weighing bisphenol A epoxy resin, heating to 60-70 ℃, adding bismaleimide resin, stirring uniformly, adding the modified halloysite nanotube grafted with bismaleimide, heating to 80-120 ℃, and stirring for 3-5 hours to obtain bismaleimide modified resin;
wherein the mass ratio of the bisphenol A epoxy resin to the bismaleimide grafted modified halloysite nanotube is 1: 4-6: 0.05-0.2.
8. The ultra-small seal type high-temperature and high-pressure connector according to claim 2, wherein the special adhesive is prepared by the steps of:
firstly, weighing 100 parts of bismaleimide modified resin, 20-40 parts of linear phenolic resin, 5-10 parts of metal oxide powder, 3-10 parts of polyvinyl alcohol, 0.1-5 parts of dispersing agent and 30-80 parts of organic solvent.
Secondly, adding the weighed bismaleimide modified resin and the weighed linear phenolic resin into a mixing stirrer, and stirring and reacting for 0.5-1 h at the temperature of 120-150 ℃ under the stirring condition to obtain a resin premix;
thirdly, adding the weighed metal oxide powder, polyvinyl alcohol and a dispersing agent into an organic solvent, stirring and carrying out ultrasonic treatment for 0.5-1 h to obtain an additive premix;
and fourthly, putting the additive premix and the resin premix into a mixing roll, and blending for 0.5-1 h at the temperature of 100-125 ℃ to obtain the special adhesive.
9. The ultra-small sealed high-temperature high-pressure connector according to claim 1, wherein the insulating material is made of a modified polytetramethyleneadipamide material; the modified polytetramethylene adipamide material is obtained by modifying polytetramethylene adipamide through an organic zirconium/halloysite nanotube.
10. The ultra-small sealed high-temperature high-pressure connector according to claim 9, wherein the insulating material is prepared by a method comprising:
s1, weighing zirconium acetylacetonate, adding the zirconium acetylacetonate into acetone, and stirring until the zirconium acetylacetonate is completely dissolved to obtain a zirconium acetylacetonate solution; weighing halloysite nanotubes, adding the halloysite nanotubes into ethanol, and performing ultrasonic dispersion until the mixture is uniform to obtain a halloysite nanotube dispersion solution;
wherein the mass ratio of zirconium acetylacetonate to acetone is 1: 5-7; the mass ratio of the halloysite nanotube to the ethanol is 1: 6-10;
s2, adding sodium ethoxide into the halloysite nanotube dispersion liquid, stirring until the mixture is uniform, heating to 70-80 ℃ under the protection of inert gas, dropwise adding a zirconium acetylacetonate solution, carrying out reflux reaction for 4-6 hours after the dropwise addition is finished, cooling to room temperature, and filtering to obtain a solid substance to obtain an organic zirconium/halloysite nanotube;
wherein the mass ratio of the halloysite nanotube dispersion liquid to the sodium ethoxide to the zirconium acetylacetonate solution is 1: 0.02-0.04: 0.5-0.8;
s3, putting the dried polytetramethylene adipamide into a high-speed stirrer, putting the organic zirconium/halloysite nanotube into the stirrer, melting and mixing the materials uniformly, transferring the materials into a double-screw extruder, extruding and granulating the materials to obtain a modified polytetramethylene adipamide material, namely an insulating material;
wherein the mass ratio of the polytetramethyleneadipamide to the organic zirconium/halloysite nanotubes is 1: 0.05-0.1.
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| WO2019191411A1 (en) * | 2018-03-28 | 2019-10-03 | Zoltek Corporation | Electrically conductive sizing for carbon fibers |
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| CN1768099A (en) * | 2003-04-01 | 2006-05-03 | 天鹰技术公司 | Thermally conductive adhesive composition and process for device attachment |
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