CN100594561C - Composite insulating material and method for producing the same - Google Patents
Composite insulating material and method for producing the same Download PDFInfo
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- CN100594561C CN100594561C CN200710304231A CN200710304231A CN100594561C CN 100594561 C CN100594561 C CN 100594561C CN 200710304231 A CN200710304231 A CN 200710304231A CN 200710304231 A CN200710304231 A CN 200710304231A CN 100594561 C CN100594561 C CN 100594561C
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Abstract
The invention provides a composite insulating material, comprising toughness reinforcing epoxy resin, alumina trihydrate, alumina, estolide and the like curing agent and amine and the like accelerant.The method for preparing the composite insulating material of the invention is as follows: a toughness reinforcing epoxy resin system (6), the radioresistant alumina trihydrate (4) and the alumina powder (5) are mixed evenly, the evenly mixed compound is vacuum treated, the bubble-free raw material is cast into various insulating sub moulds and is vacuum solidified to prepare the composite insulating material (7) with the anti-aging of branches ability. The invention can change the electric field distribution along the surface of the insulating material, reduce the secondary emission coefficient along the surface of the insulating material, decrease the charge density on the surface of the insulating material, restrain the space charge inside an insulator from gathering and improve the ability of the insulating material to resist the aging of branches, thereby increasing the flashover voltage of vacuum surface of the insulator and prolonging the service life of the insulator. The invention can be applicable to the coating of an insulating component with a complicated shape and a vacuum contact surface (non-stress contact), which can obviously prolong the service life of the insulator.
Description
Technical field
The present invention relates to a kind of composite insulating material and preparation method thereof, particularly long insulation life, the anti-branch composite insulating material of anti-irradiation and preparation method thereof.
Background technology
Pulse power drive source High-Power Microwave emission, Laser emission, and more and more important effect is being brought into play in fields such as medical treatment, environmental protection.
The design of vacuum axial dielectric heap (being made up of insulator and grading ring) is most important for the pulse power drive source with vacuum system, has become the emphasis and the difficult point of such device development.The insulation heap is often used as the interface of gas (air, nitrogen, sulphur hexafluoride), liquid medium (water or oil) and vacuum.In order to improve, generally be designed to 45 degree inclined-planes along the face insulation.Its operating mode is abominable, and the insulating material of function admirable and reasonable insulation system efficiently are the keys that guarantees insulation heap performance.
Vacuum insulation heap in the present large-scale pulse power device, general Rexolite (cross-linked polystyrene interlinkage polystyrene), Urethane (urethanes), the Epoxy (epoxy resin) of adopting, Acrylic (acrylic resin), PMMA materials such as (polymethyl methacrylate).The mechanical tenacity of epoxy resin, acrylic resin, polymethyl methacrylate is relatively poor, anti-impact of water hammer ability often can not satisfy the work requirements of large-scale high efficiency pulse power device, the mechanical property of interlinkage polystyrene and urethanes is better, stronger impact resistance is arranged, but their anti-branch characteristic is relatively poor, and the life-span can't be guaranteed.Performance interlinkage polystyrene relatively preferably costs an arm and a leg, and the source of goods is limited.Conventional solid insulating material can't and be satisfied the demand on useful life simultaneously at dielectric strength, mechanical strength, anti-irradiation, general one group of insulation piles up once will clear up after the discharge, after using tens times, even just need several times to change, this is very consuming time spending concerning these main equipments, is unfavorable for that again experimental work is successional simultaneously.Studies show that branch is aging to be the main reason that the insulation heap destroys.
U.S. physics international corporation had once developed a kind of new coating material, can improve the useful life of insulation heap, with improving 80 times (11 than base material the useful life that the insulation of coating piles up under the high-energy radiation condition
ThIEEE PPC, Vol.1,1997), but the present prescription that does not also disclose this coating material.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art, improve the useful life of insulator under vacuum, the radiation parameter, propose a kind of NEW TYPE OF COMPOSITE insulating material, its adopts insulating material of polymer and inorganic powder material preparation, has low secondary electron yield, characteristics that anti-branch is aging.The present invention can make full use of the conductance property of composite material, reduce the inner and surperficial space charge accumulation of insulator, thereby reduce the material secondary electron emission coefficiency, suppress the development of the inner branch of insulator, improve the edge flashing field intensity of material to a certain extent, increase substantially the useful life of insulator.
Composite insulating material of the present invention uses mainly as coating material.It must be coated in it in conjunction with the good insulation performance material surface; Compare with bulk material, have better anti-edge flashing performance; Have the ability that anti-electric arc burns, can resist branchization aging; Satisfactory mechanical property, easily processing and fabricating; Cost is low.
The component of composite insulating material of the present invention is: toughened epoxy resin, aluminium hydroxide, aluminium oxide, acid anhydride type curing agent, amine type accelerator.Each constituent mass percentage is: toughened epoxy resin 26%～41%; Acid anhydride type curing agent 12.5%～21%; Amine type accelerator 1.5%～3%; Aluminium oxide 28%～48%; Aluminium hydroxide 7%～12%.
Less than 40Pas, epoxide number 0.40～0.55mol/100g, normal temperature are liquid epoxy resin down to described toughened epoxy resin viscosity in the time of 25 ℃; The grain diameter of described aluminium oxide is less than 3 microns; The particle diameter of aluminium hydroxide is between 30 to 50 μ m, and aluminium oxide and aluminium hydroxide were by 4: 1 percentage by weight proportionings.
The preparation method of composite insulating material of the present invention is as follows:
Aluminium oxide and aluminium hydroxide powder is mixed by 4: 1, at 100 ℃ of oven dryings greater than 1 hour; Toughened epoxy resin, acid anhydride type curing agent, amine type accelerator are heated down at 80 ± 5 ℃ respectively, about 20 minutes of heating time, epoxy resin, acid anhydride type curing agent are mixed, and under vacuum condition (vacuum degree is higher than 0.001MPa) stir about 15 minutes, it is fully mixed, slowly add aforementioned aluminium hydroxide and aluminium oxide mixed-powder while stirring through dried, after mixing fully, add amine type accelerator again with electric mixer (vacuum degree is higher than 0.001MPa) stir about 30 minutes under vacuum condition, make different materials fully mix the degassing; Bubble-free raw material is molded in (being preferably under the vacuum environment) all kinds of vacuum insulator moulds, heats up down at 80～105 ℃ and solidified 8～12 hours; Naturally cool to room temperature, the demoulding is taken out, and just obtains composite insulating material of the present invention, and material is blocks of solid white, and its shore hardness is 55 ± 5.
Dendroid aging phenomenon under the electric field is a kind of irreversible ionization aging damage phenomenon that occurs in organic insulating material, and its destruction passage is dendroid.The concentration of local of electric field and distortion are to cause the basic reason destroyed.Therefore a principle the most basic is exactly a uniform electric field in the insulating Design process, reduces local field strength as much as possible and concentrates.
Studies show that under the radiation of high energy particle, dielectric material can be injected into space charge and storage power, the release of these energy makes material surface generation flashover.The chamber is to the space charge measurement Research by experiment for we, and the result shows that also dielectric material can store a considerable amount of space charges, and this energy has the hold facility of long duration under the situation that high energy electron injects.Different materials produces different injection energy and injects the degree of depth with injection mode, under certain condition, irradiation can be so that material internal produces number MV/cm even higher concentration of local electric field, and this will reduce the insulation characterisitic of material greatly, is easy to generate the electricity tree and destroys.Therefore, reducing the charge storage capacity of dielectric material under high-energy electron irradiation is to improve the basic guideline of dielectric ageing resistance under the radiation parameter with the diffusion of raising space charge, transport ability.
The volume resistivity of the composite insulating material of process test the present invention preparation is 10
-8～10
-12Between the Ω m, surface resistivity is 10
-7～10
-10Between the Ω m.Much smaller than general insulating material, measure use standard three-electrode system, the super megger of EST121 type numeral; Composite insulating material does not ftracture behind impact experiment, and can keep original form, experimental technique substantially: 1m highly locates, and falls the sample center of hitting with the weight of 519g, the weight head is the hemisphere that diameter is 25cm, and specimen size is Φ 25 * 2mm; In vacuum degree 10
-2～10
-4Between the Pa, the direct current flashover voltage of insulator is greater than 10kV/cm, insulator under impulsive condition the flashover field intensity greater than 150kV/cm.Sample is dried processing earlier before carrying out flashover experiment, be about to sample and put into baking oven in vacuum condition, 70～100 ℃ following placement 1～3 hour, applies the pulsewidth 40ns of pulse for approximate square wave, and rising edge 8ns, flashover occur in the pulse ascent stage.
Epoxy resin toughened and the aluminium hydroxide that the present invention adopts, that aluminium oxide carries out blend is compound.Because insulator work is under the nanosecond pulse current field condition, characteristic that can expendable material part leakage current.Reduce the coating resistance rate, reduce its electric charge accumulation inner and surface, reach the aging purpose of anti-branchization, can suppress the secondary of material simultaneously, improve material useful life.Coating material of the present invention can be applicable to the surface that various difform insulating components contact with vacuum, can significantly improve its useful life, and can improve the vacuum edge flashing field intensity of insulation to a certain extent.The present invention can realize that coating material (19, be the composite insulating material of our preparation) itself has good toughness, is white in color with ripe chemical blend method, and its mechanical strength is by coated base material decision.
Description of drawings
Fig. 1 is polymethyl methacrylate electric charge accumulation figure after accepting electron irradiation, among the figure: 1 electrode position, 2 space charge accumulation curves, 3 insulating material (polymethyl methacrylate);
Fig. 2 is the constitutional diagram of preparation coating material, and among the figure: 4 is aluminium hydroxide powder, and 5 is alumina powder jointed, and 6 is epoxy-resin systems, 7 coating materials;
Fig. 3 is the schematic diagram of prepared in laboratory composite material, and among the figure: 8 are the vacuum degassing outlet, and 9 is blender, and 10 is thermometer, and 11 is composite material, and 12 is three mouthfuls of containers, and 13 is heater;
Fig. 4 has shown the typical process flow of preparation coating material;
Fig. 5 is the schematic diagram of the laboratory test sample of coating material, and 14,15,16,17 is four kinds of difform laboratory flashover test samples, and 18 is base material, and 19 is coating material;
Fig. 6 is the laboratory experiment measurement system diagram, and among the figure: 20 is high-field electrode, and 21 is earth terminal, and 22 are creeping discharge arc road;
Fig. 7 is that coating material uses figure in large-scale dead ring, and among the figure: 23 is anode, and 24 is negative electrode, and 25 are the insulation heap, and 26 is grading ring, and 27 is cathode collector bar, and 28 is anode rod, and 29 are load, and 30 is electronics or X ray;
Embodiment
Further specify the present invention below in conjunction with the drawings and specific embodiments.
When ray (electron beam, X ray) 30 irradiation to insulating material, the effect of gathering of space charge can take place in insulating material, forms concentrating of internal field in inside, causes the generation and the development of electric branch.Figure 1 shows that the space charge accumulation of common pmma material 3 after accepting electron irradiation distributes and time dependent collection of illustrative plates, 1 is electrode position, and 2 is the space charge accumulation curve.The space charge accumulation of coating material of the present invention is littler more than 5 times than general insulating material, reduces the probability that electric branch produces.
As shown in Figure 2, the component of coating material 7 is: by the epoxy-resin systems 6 that toughened epoxy resin, acid anhydride type curing agent, amine type accelerator are formed, and aluminium hydroxide powder 4, alumina powder jointed 5.The present invention selects following material for use in concrete enforcement: epoxy resin adopts the toughened epoxy resin of southeast chemical institute, and less than 40Pas, epoxide number is between 0.48～0.54mol/100g in the time of 25 ℃ for viscosity; Curing agent uses the special-purpose acid anhydride type curing agent of the toughness reinforcing epoxy of southeast chemical institute; Promoter is used the amine type accelerator of southeast chemical institute.Aluminium oxide is last marine products, and particle diameter is less than 3.00 microns.Aluminium hydroxide produces for the Shandong Aluminum, the high powder of filling of particle diameter 325 purposes.
Fig. 3 is the schematic diagram of prepared in laboratory container coating material.The preparation instrument of three mouthfuls of containers 12 as composite material 11 adopted in the laboratory usually; Temperature in thermometer 10 measuring vessels; Material in 9 pairs of containers of blender stirs, and makes its even mixing; Heating is finished by heater 13, and heater 13 can adopt modes such as heating collar, water-bath temperature control to realize.Vacuum degassing outlet 8 is the vacuum pump outlet of bleeding.
Fig. 5 is that prepared in laboratory goes out difform flashover test sample, and circular platform type 14,15 is arranged, and column type 16,17, sample white portion are base material 18, and black part is divided into coating material 19; The edge flashing field intensity that the laboratory records cooperates the electrode system measurement that comprises high-field electrode 20 and earth terminal 21 shown in Figure 6 to obtain on these samples, and discharge occurs in sample surfaces, produces arc road 22.
Figure 4 shows that the preparation process of coating material.Above-mentioned raw material are specifically implemented concrete preparation technology such as following examples respectively in conjunction with preparation composite insulating material technology by different proportionings.
High voltage is applied to high-field electrode 20 ends, electrode other end ground connection 21,
Embodiment 1:
1, with epoxy resin, acid anhydride type curing agent, amine type accelerator, aluminium hydroxide powder, alumina powder jointed 26%: 12.5%: 1.5% by mass percentage: 12%: 48% batching;
2,4: 1 by weight percentage good aluminium oxide and the aluminium hydroxide powders of proportioning mix, and put into 100 ℃ of baking ovens and carry out drying, 100 minutes heating times;
3, will be by the load weighted toughened epoxy resin of proportioning, acid anhydride type curing agent and amine promote to release agent and put into baking oven respectively 80 ± 5 ℃ of following heating 20 minutes, (vacuum degree is higher than 0.001MPa) mixes stirring with toughness reinforcing epoxy and anhydride curing agent with electric mixer under vacuum condition then, stir about 15 minutes, raw material is fully mixed, remove moisture and bubble in the raw material;
4, stir epoxy resin and acid anhydride type curing agent on one side fast, make its even mixing, from baking oven, take out aluminium oxide and the aluminium hydroxide mixed powder of handling well then, in epoxy resin that is stirring and acid anhydride type curing agent, slowly add aluminium oxide and aluminium hydroxide mixed powder, until adding fully, add amine type accelerator then.Stirred 30 minutes with electric mixer (vacuum degree is higher than 0.001MPa) under vacuum condition, make epoxy resin, acid anhydride type curing agent, amine type accelerator, aluminium oxide and aluminium hydroxide fully mix the degassing;
5, bubble-free raw material is molded in all kinds of vacuum insulator moulds, heats up down at 80 ℃ and solidified 12 hours;
6, naturally cool to room temperature, the demoulding just makes composite insulating material of the present invention.
Embodiment 2:
1, with epoxy resin, acid anhydride type curing agent, amine type accelerator, aluminium hydroxide powder, alumina powder jointed 26%: 12.5%: 1.5% by mass percentage: 12%: 48% batching;
2,4: 1 by weight percentage good aluminium oxide and the aluminium hydroxide powders of proportioning are mixed, putting into 100 ℃ of baking ovens carries out drying, 100 minutes heating times;
3, will be load weighted epoxy resin toughened by proportioning, acid anhydride type curing agent and amine promote to release agent and put into baking oven respectively 80 ± 5 ℃ of following heating 20 minutes, (vacuum degree is higher than 0.001MP) mixes stirring with toughness reinforcing epoxy and anhydride curing agent with electric mixer under vacuum condition then, stir about 15 minutes, raw material is fully mixed, remove moisture and bubble in the raw material;
4, stir epoxy resin and acid anhydride type curing agent on one side fast, make its even mixing, from baking oven, take out aluminium oxide and the aluminium hydroxide mixed powder of handling well then, in epoxy resin that is stirring and acid anhydride type curing agent, slowly add aluminium oxide and aluminium hydroxide mixed powder, until adding fully, add amine type accelerator then.Stirred 30 minutes with electric mixer (vacuum degree is higher than 0.001MPa) under vacuum condition, make epoxy resin, acid anhydride type curing agent, amine type accelerator, aluminium oxide and aluminium hydroxide fully mix the degassing;
5, bubble-free raw material is molded in all kinds of vacuum insulator moulds, heats up down at 95 ℃ and solidified 10 hours;
6, naturally cool to room temperature, the demoulding just makes composite insulating material of the present invention.
Embodiment 3:
1, with epoxy resin, acid anhydride type curing agent, amine type accelerator, aluminium hydroxide powder, alumina powder jointed 26%: 12.5%: 1.5% by mass percentage: 12%: 48% batching;
2,4: 1 by weight percentage good aluminium oxide and the aluminium hydroxide powders of proportioning are mixed, putting into 100 ℃ of baking ovens carries out drying, 100 minutes heating times;
3, will be load weighted epoxy resin toughened by proportioning, acid anhydride type curing agent and amine promote to release agent and put into baking oven respectively 80 ± 5 ℃ of following heating 20 minutes, (vacuum degree is higher than 0.001MPa) mixes stirring with toughness reinforcing epoxy and anhydride curing agent with electric mixer under vacuum condition then, stir about 15 minutes, raw material is fully mixed, remove moisture and bubble in the raw material;
4, stir epoxy resin and acid anhydride type curing agent on one side fast, make its even mixing, from baking oven, take out aluminium oxide and the aluminium hydroxide mixed powder of handling well then, in epoxy resin that is stirring and acid anhydride type curing agent, slowly add aluminium oxide and aluminium hydroxide mixed powder, until adding fully, add amine type accelerator then.Stirred 30 minutes with electric mixer (vacuum degree is higher than 0.001MPa) under vacuum condition, make epoxy resin, acid anhydride type curing agent, amine type accelerator, aluminium oxide and aluminium hydroxide fully mix the degassing;
5, bubble-free raw material is molded in all kinds of vacuum insulator moulds, heats up down at 105 ℃ and solidified 8 hours;
6, naturally cool to room temperature, the demoulding just makes composite insulating material of the present invention.
Embodiment 4:
1, with epoxy resin, acid anhydride type curing agent, amine type accelerator, aluminium hydroxide powder, alumina powder jointed 35%: 18%: 2% by mass percentage: 9%: 36% batching;
2,4: 1 by weight percentage good aluminium oxide and the aluminium hydroxide powders of proportioning are mixed, putting into 100 ℃ of baking ovens carries out drying, and heating time was greater than 60 minutes;
3, will be load weighted epoxy resin toughened by proportioning, acid anhydride type curing agent and amine promote to release agent and put into baking oven respectively 80 ± 5 ℃ of following heating 20 minutes, (vacuum degree is higher than 0.001MPa) mixes stirring with toughness reinforcing epoxy and anhydride curing agent with electric mixer under vacuum condition then, stir about 15 minutes, raw material is fully mixed, remove moisture and bubble in the raw material;
4, stir epoxy resin and acid anhydride type curing agent on one side fast, make its even mixing, from baking oven, take out aluminium oxide and the aluminium hydroxide mixed powder of handling well then, in epoxy resin that is stirring and acid anhydride type curing agent, slowly add aluminium oxide and aluminium hydroxide mixed powder, until adding fully, add amine type accelerator then.Stirred 30 minutes with electric mixer (vacuum degree is higher than 0.001MPa) under vacuum condition, make epoxy resin, acid anhydride type curing agent, amine type accelerator, aluminium oxide and aluminium hydroxide fully mix the degassing;
5, bubble-free raw material is molded in all kinds of vacuum insulator moulds, heats up down at 80 ℃ and solidified 12 hours;
6, naturally cool to room temperature, the demoulding just makes composite insulating material of the present invention.
Embodiment 5:
1, with epoxy resin, acid anhydride type curing agent, amine type accelerator, aluminium hydroxide powder, alumina powder jointed 35%: 18%: 2% by mass percentage: 9%: 36% batching;
2,4: 1 by weight percentage good aluminium oxide and the aluminium hydroxide powders of proportioning are mixed, putting into 100 ℃ of baking ovens carries out drying, and heating time was greater than 60 minutes;
3, will be load weighted epoxy resin toughened by proportioning, acid anhydride type curing agent and amine promote to release agent and put into baking oven respectively 80 ± 5 ℃ of following heating 20 minutes, (vacuum degree is higher than 0.001MPa) mixes stirring with toughness reinforcing epoxy and anhydride curing agent with electric mixer under vacuum condition then, stir about 15 minutes, raw material is fully mixed, remove moisture and bubble in the raw material;
4, stir epoxy resin and acid anhydride type curing agent on one side fast, make its even mixing, from baking oven, take out aluminium oxide and the aluminium hydroxide mixed powder of handling well then, in epoxy resin that is stirring and acid anhydride type curing agent, slowly add aluminium oxide and aluminium hydroxide mixed powder, until adding fully, add amine type accelerator then.Stirred 30 minutes with electric mixer (vacuum degree is higher than 0.001MPa) under vacuum condition, make epoxy resin, acid anhydride type curing agent, amine type accelerator, aluminium oxide and aluminium hydroxide fully mix the degassing;
5, bubble-free raw material is molded in all kinds of vacuum insulator moulds, heats up down at 95 ℃ and solidified 10 hours;
6, naturally cool to room temperature, the demoulding just makes composite insulating material of the present invention.
Embodiment 6:
1, with epoxy resin, acid anhydride type curing agent, amine type accelerator, aluminium hydroxide powder, alumina powder jointed 35%: 18%: 2% by mass percentage: 9%: 36% batching;
2,4: 1 good aluminium oxide and aluminium hydroxide powders of proportioning of percentage by weight are mixed, put into 100 ℃ of baking ovens and carry out drying, heating time was greater than 60 minutes;
3, will be load weighted epoxy resin toughened by proportioning, acid anhydride type curing agent and amine promote to release agent and put into baking oven respectively 80 ± 5 ℃ of following heating 20 minutes, (vacuum degree is higher than 0.001MPa) mixes stirring with toughness reinforcing epoxy and anhydride curing agent with electric mixer under vacuum condition then, stir about 15 minutes, raw material is fully mixed, remove moisture and bubble in the raw material;
4, stir epoxy resin and acid anhydride type curing agent on one side fast, make its even mixing, from baking oven, take out aluminium oxide and the aluminium hydroxide mixed powder of handling well then, in epoxy resin that is stirring and acid anhydride type curing agent, slowly add aluminium oxide and aluminium hydroxide mixed powder, until adding fully, add amine type accelerator then.Stirred 30 minutes with electric mixer (vacuum degree is higher than 0.001MPa) under vacuum condition, make epoxy resin, acid anhydride type curing agent, amine type accelerator, aluminium oxide and aluminium hydroxide fully mix the degassing;
5, bubble-free raw material is molded in all kinds of vacuum insulator moulds, heats up down at 105 ℃ and solidified 12 hours;
6, naturally cool to room temperature, the demoulding just makes composite insulating material of the present invention.
Embodiment 7:
1, with epoxy resin, acid anhydride type curing agent, amine type accelerator, aluminium hydroxide powder, alumina powder jointed 41%: 21%: 3% by mass percentage: 7%: 28% batching;
2,4: 1 by weight percentage good aluminium oxide and the aluminium hydroxide powders of proportioning are mixed, putting into 100 ℃ of baking ovens carries out drying, and heating time was greater than 60 minutes;
3, will be load weighted epoxy resin toughened by proportioning, acid anhydride type curing agent and amine promote to release agent and put into baking oven respectively 80 ± 5 ℃ of following heating 20 minutes, (vacuum degree is higher than 0.001MPa) mixes stirring with toughness reinforcing epoxy and anhydride curing agent with electric mixer under vacuum condition then, stir about 15 minutes, raw material is fully mixed, remove moisture and bubble in the raw material;
4, stir epoxy resin and acid anhydride type curing agent on one side fast, make its even mixing, from baking oven, take out aluminium oxide and the aluminium hydroxide mixed powder of handling well then, in epoxy resin that is stirring and acid anhydride type curing agent, slowly add aluminium oxide and aluminium hydroxide mixed powder, until adding fully, add amine type accelerator then.Stirred 30 minutes with electric mixer (vacuum degree is higher than 0.001MPa) under vacuum condition, make epoxy resin, acid anhydride type curing agent, amine type accelerator, aluminium oxide and aluminium hydroxide fully mix the degassing;
5, bubble-free raw material is molded in all kinds of vacuum insulator moulds, heats up down at 80 ℃ and solidified 12 hours;
6, naturally cool to room temperature, the demoulding just makes composite insulating material of the present invention.
Embodiment 8:
1, with epoxy resin, acid anhydride type curing agent, amine type accelerator, aluminium hydroxide powder, alumina powder jointed 41%: 21%: 3% by mass percentage: 7%: 28% batching;
2,4: 1 by weight percentage good aluminium oxide and the aluminium hydroxide powders of proportioning are mixed, putting into 100 ℃ of baking ovens carries out drying, and heating time was greater than 60 minutes;
3, will be load weighted epoxy resin toughened by proportioning, acid anhydride type curing agent and amine promote to release agent and put into baking oven respectively 80 ± 5 ℃ of following heating 20 minutes, (vacuum degree is higher than 0.001MPa) mixes stirring with toughness reinforcing epoxy and anhydride curing agent with electric mixer under vacuum condition then, stir about 15 minutes, raw material is fully mixed, remove moisture and bubble in the raw material;
4, stir epoxy resin and acid anhydride type curing agent on one side fast, make its even mixing, from baking oven, take out aluminium oxide and the aluminium hydroxide mixed powder of handling well then, in epoxy resin that is stirring and acid anhydride type curing agent, slowly add aluminium oxide and aluminium hydroxide mixed powder, until adding fully, add amine type accelerator then.Stirred 30 minutes with electric mixer (vacuum degree is higher than 0.001MPa) under vacuum condition, make epoxy resin, acid anhydride type curing agent, amine type accelerator, aluminium oxide and aluminium hydroxide fully mix the degassing;
5, bubble-free raw material is molded in all kinds of vacuum insulator moulds, heats up down at 95 ℃ and solidified 10 hours;
6, naturally cool to room temperature, the demoulding just makes composite insulating material of the present invention.
Embodiment 9:
1, with epoxy resin, acid anhydride type curing agent, amine type accelerator, aluminium hydroxide powder, alumina powder jointed 41%: 21%: 3% by mass percentage: 7%: 28% batching;
2,4: 1 by weight percentage good aluminium oxide and the aluminium hydroxide powders of proportioning are mixed, putting into 100 ℃ of baking ovens carries out drying, and heating time was greater than 60 minutes;
3, will be load weighted epoxy resin toughened by proportioning, acid anhydride type curing agent and amine promote to release agent and put into baking oven respectively 80 ± 5 ℃ of following heating 20 minutes, (vacuum degree is higher than 0.001MPa) mixes stirring with toughness reinforcing epoxy and anhydride curing agent with electric mixer under vacuum condition then, stir about 15 minutes, raw material is fully mixed, remove moisture and bubble in the raw material;
4, stir epoxy resin and acid anhydride type curing agent on one side fast, make its even mixing, from baking oven, take out aluminium oxide and the aluminium hydroxide mixed powder of handling well then, in epoxy resin that is stirring and acid anhydride type curing agent, slowly add aluminium oxide and aluminium hydroxide mixed powder, until adding fully, add amine type accelerator then.Stirred 30 minutes with electric mixer (vacuum degree is higher than 0.001MPa) under vacuum condition, make epoxy resin, acid anhydride type curing agent, amine type accelerator, aluminium oxide and aluminium hydroxide fully mix the degassing;
5, bubble-free raw material is molded in all kinds of vacuum insulator moulds, heats up down at 105 ℃ and solidified 12 hours;
6, naturally cool to room temperature, the demoulding just makes composite insulating material of the present invention.
Points for attention in the technical process: as shown in Figure 3, stir simultaneously and steep from 8 vacuum degassings outlet vacuumize degassing, vacuum degree should not be too big during beginning, because bubble is a lot of in the system, the surface tension conference that viscosity causes greatly makes the system rapid expanding enter vacuum pump; Gas clean-up again after stable stirs when vacuumizing and can the help system tear bubble and make minute bubbles merge into air pocket, and mixing speed is advisable with low speed, can not sneak into bubble like this, so after stirring 30 minutes, lower mixing speed, outgases 30 minutes.Three mouthfuls of containers are the reactor schematic diagram among Fig. 3, and preparation uses three mouthfuls of containers 12 to get final product in the laboratory.
Fig. 5 is the schematic diagram of the laboratory test sample of coating material.Sample base material 18 is a polyurethane among the figure, also can be the insulating material of other good toughness.As shown in Figure 6, sample is placed between the plate electrode uniform field electrode, sample 14,15 in vacuum degree greater than 10
-2During Pa, direct current flashover field intensity＞10kV/cm; 16,17 samples in vacuum degree greater than 10
-2During Pa, about 40 nanosecond halfwidth the impulse electric field effect under, flashover field intensity＞150kV/cm.
Fig. 7 has shown use and the environment for use thereof of this coating material in the insulation heap 25 of large-scale pulse-power apparatus.Substrate insulating material 18 is epoxy resin, epoxy resin fiberglass composite plate, polyurethane material etc.As shown in Figure 7, large-scale insulation heap 25 uses cup insuator to cooperate composition with grading ring 26, and diameter can reach more than the 3m.Draw cathode collector bar 27 from the negative electrode 24 of pulse-power apparatus and be added to load 29 1 ends, draw anode rod 28 from anode 23 and be applied to load 29 other ends, when high-voltage pulse affacts in the load 29, load 29 can be radiated high energy electron, X ray 30, the part high energy particle can be radiated the insulation heap, destroy the insulating material performance, reduce its useful life, adopt coating material 19, by die casting in base material 18 surface cure moulding, about 3 to 4mm is thick, compares with base material 18 with direct, can improve insulation and pile for 25 useful lifes.
Claims (3)
1, a kind of composite insulating material is characterized in that this material component is toughened epoxy resin, aluminium hydroxide, aluminium oxide, acid anhydride type curing agent, amine type accelerator; Each constituent mass percentage is: toughened epoxy resin 26%～41%; Acid anhydride type curing agent 12.5%～21%; Amine type accelerator 1.5%～2.5%; Aluminium oxide 28%～48%; Aluminium hydroxide 7%～12%.
2, composite insulating material according to claim 1 is characterized in that: less than 40Pas, epoxide number is between 0.48～0.54mol/100g in the time of 25 ℃ for described toughened epoxy resin viscosity, and normal temperature is liquid-state epoxy resin down; The powder granule diameter of described aluminium oxide is less than 3 microns, and the powder granule diameter of aluminium hydroxide is at 30～50 μ m.
3, a kind of method for preparing the described composite insulating material of claim 1 is characterized in that may further comprise the steps:
(1) by mass percentage with 26～41% toughened epoxy resins, 12.5～21% acid anhydride type curing agents, 1.5～2.5% amine type accelerators, 7～12% aluminium hydroxide powders, 28～48% alumina powder jointed batching;
(2) 4: the 1 by weight percentage good alumina powder jointed and aluminium hydroxide powders of proportioning are mixed, put into 100 ℃ of oven dryings, heating time was greater than 60 minutes;
(3) will be by the load weighted toughened epoxy resin of proportioning, acid anhydride type curing agent and amine type accelerator are put into baking oven respectively and were heated about 20 minutes down at 80 ± 5 ℃, under vacuum condition, toughened epoxy resin and acid anhydride type curing agent are mixed stirring with electric mixer then, stir about 15 minutes, raw material is fully mixed, remove moisture and bubble in the raw material;
(4) stir toughened epoxy resin and acid anhydride type curing agent on one side fast, from baking oven, take out aluminium oxide and the aluminium hydroxide mixed powder of handling well on one side, in toughened epoxy resin that is stirring and acid anhydride type curing agent, slowly add aluminium oxide and aluminium hydroxide mixed powder, after mixed fully, add amine type accelerator; Stirred 30 minutes under vacuum condition with electric mixer, make toughened epoxy resin, acid anhydride type curing agent, amine type accelerator, aluminium oxide and aluminium hydroxide fully mix the degassing;
(5) bubble-free raw material is molded in the vacuum insulator mould, heats up down at 80～105 ℃ and solidified 8～12 hours;
(6) naturally cool to room temperature, the demoulding just makes composite insulating material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| CN102081992B (en) * | 2009-11-30 | 2012-05-23 | 江苏恒神纤维材料有限公司 | Carbon fiber cable core |
| CN101950641B (en) * | 2010-07-26 | 2012-06-20 | 句容市华阳电器有限公司 | Preparation method of disc insulator |
| CN102276791B (en) * | 2011-07-08 | 2013-02-27 | 绵阳惠利电子材料有限公司 | Flame-retardant epoxy resin compound |
| CN103059511A (en) * | 2012-12-29 | 2013-04-24 | 中国科学院深圳先进技术研究院 | Epoxy-based composite dielectric material and preparation method thereof |
| CN105489326A (en) * | 2015-11-20 | 2016-04-13 | 国网山东省电力公司电力科学研究院 | Method for improving vacuum surface flashover performance of solid insulation medium |
| CN105440569A (en) * | 2015-12-23 | 2016-03-30 | 佛山早稻田科技服务有限公司 | Insulating material with high temperature resistance |
| CN113470907B (en) * | 2021-06-23 | 2022-07-12 | 西安交通大学 | Method for inhibiting partial discharge at flange of GIS/GIL supporting insulator |
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| US5032453A (en) * | 1988-08-18 | 1991-07-16 | Siemens Aktiengesellschaft | Insulating tape for making an impregnated insulating sleeve for electric conductors |
| CN1192461A (en) * | 1997-05-28 | 1998-09-09 | 何瑞明 | High-performance flame-retardant and insulation filling material |
| CN1273422A (en) * | 1999-03-15 | 2000-11-15 | 日本碍子株式会社 | Ceramic insulator for high voltage |
| CN1420503A (en) * | 2002-09-02 | 2003-05-28 | 王淑兰 | Method for mfg. insulator of multi-layer umbrella suspension glass fibre reinforced plastic insulator |
| CN1604237A (en) * | 2004-10-22 | 2005-04-06 | 西安交通大学 | vacuum insulator coating capable of increasing flashover voltage and method of preparation thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5032453A (en) * | 1988-08-18 | 1991-07-16 | Siemens Aktiengesellschaft | Insulating tape for making an impregnated insulating sleeve for electric conductors |
| CN1192461A (en) * | 1997-05-28 | 1998-09-09 | 何瑞明 | High-performance flame-retardant and insulation filling material |
| CN1273422A (en) * | 1999-03-15 | 2000-11-15 | 日本碍子株式会社 | Ceramic insulator for high voltage |
| CN1420503A (en) * | 2002-09-02 | 2003-05-28 | 王淑兰 | Method for mfg. insulator of multi-layer umbrella suspension glass fibre reinforced plastic insulator |
| CN1604237A (en) * | 2004-10-22 | 2005-04-06 | 西安交通大学 | vacuum insulator coating capable of increasing flashover voltage and method of preparation thereof |
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