CN115214138A - Preparation method of gradient insulator made of nano zinc oxide modified epoxy resin material - Google Patents
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- CN115214138A CN115214138A CN202210850798.3A CN202210850798A CN115214138A CN 115214138 A CN115214138 A CN 115214138A CN 202210850798 A CN202210850798 A CN 202210850798A CN 115214138 A CN115214138 A CN 115214138A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
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Abstract
The invention discloses a preparation method of a gradient insulator made of a nano zinc oxide modified epoxy resin material, which realizes gradient distribution by using centrifugal force to realize the concentration of nano particles, and comprises the following steps: preparing an insulator pouring mold by using a 3D printing technology; preparing an epoxy group mixture; vacuum treatment and degassing; placing the epoxy-based mixture in a prepared mould, installing the mould on a centrifugal machine, and starting the centrifugal machine; stopping the centrifugal machine, curing the insulator at high temperature and demolding; the invention can effectively improve the distribution condition of the surface electric field of the insulator, improve the electric resistance characteristic of the insulator and prolong the actual service life.
Description
Technical Field
The invention belongs to the technical field of high-voltage insulation, and relates to a preparation method of a gradient insulator made of a nano zinc oxide modified epoxy resin material.
Background
The rapid development of the power industry makes the ultra-high voltage and extra-high voltage technology an important means for power transmission in China. The requirement for insulating equipment is increased along with the continuous increase of voltage grades, and the research on insulators is more and more extensive. In order to ensure the excellent insulating property and the excellent aging resistance, high temperature resistance and the like of the insulator, the nano modification becomes one of important means for improving the insulating material.
For most extra-high voltage and extra-high voltage power equipment, the electric field of the insulation equipment is usually not uniformly distributed. The excessively concentrated electric field strength not only reduces the electric resistance of the insulator, but also causes a partial discharge phenomenon of the insulator, thereby increasing insulation degradation. Aiming at the problem of electric fields inside and along the surface of the existing insulator, the traditional methods such as increasing the insulation size and the like have limited effect on improving the electric field distribution. While functionally graded materials provide a better solution to this problem.
At present, most of the application and preparation methods of the functional gradient material are suitable for metal and ceramic materials and are not suitable for epoxy-based insulating equipment. The nano zinc oxide is used as a field nonlinear conductive nano filler, has the advantages of integrating nano modification and a dielectric function gradient material, and is widely applied to epoxy-based high polymer materials. Therefore, the development of a preparation process of a gradient insulator made of a high molecular polymer composite material is needed to meet the development needs of the insulation field in the present generation and the future.
Disclosure of Invention
The invention aims to provide a preparation method of a gradient insulator made of a nano zinc oxide modified epoxy resin material, which improves the distribution of nano particles and the appearance structure of the insulator, optimizes the distribution of the electric field intensity along the surface of the insulator and improves the flashover resistance along the surface of the insulator while giving consideration to the performance of the insulator material.
The technical scheme adopted by the invention is that the preparation method of the gradient insulator made of the nano zinc oxide modified epoxy resin material is implemented according to the following steps:
step 6, placing the epoxy-based mixture into the mold processed in the step 5, and fixing the insulator mold on a centrifuge;
step 7, starting a centrifugal machine;
and 8, stopping the centrifugal machine, placing the insulator mold into an oven, and curing at high temperature.
The invention is also characterized in that:
wherein the step 1 is implemented according to the following steps:
step 1.1, analyzing and optimizing the distribution characteristic of the electric field intensity along the surface of the insulator by using COMSOL software to obtain an optimized curve of the side surface of the insulator and construct an insulator morphology structure model;
step 1.2, drawing an insulator mold model for the structure model by using Soildworks software, and slicing the insulator mold model by using Cura software;
step 1.3, printing and manufacturing the insulator mold by using a 3D printing technology;
wherein in the step 2, the grain size of the nano zinc oxide particles is 30-60 nm, and the purity is more than or equal to 99 percent;
wherein the step 2 is implemented according to the following steps:
step 2.1, placing nano zinc oxide on an insulating medium plate;
2.2, fluorinating by adopting a DBD plasma fluorination device;
step 2.3, collecting the processed powder for later use;
wherein the fluorination conditions in step 2.2 are as follows: setting a pulse wave with the power voltage of 7kV and the discharge frequency of 9kHz, wherein the air pressure of a reaction cavity is 13.5kPa, and the volume ratio of carbon tetrafluoride gas to nitrogen is 25:1, the fluorination treatment time is 10min;
wherein the step 3 is implemented according to the following steps:
step 3.1, respectively weighing the following components of epoxy resin, curing agent, accelerator, toughening agent and nano zinc oxide according to the mass ratio, wherein 80g of curing agent, 0.8g of accelerator, 20g of toughening agent and 24.818g of nano zinc oxide are added into every 100g of epoxy resin;
step 3.2, mechanically mixing the epoxy resin weighed in the step 3.1 with the nano zinc oxide powder;
step 3.3, adding the curing agent, the accelerating agent and the toughening agent weighed in the step 3.1 into the nano zinc oxide/epoxy resin mixture mixed in the step 3.2; stirring for 20min according to the mechanical mixing condition of the step 3.2;
wherein the mechanical mixing conditions in step 3.2 are as follows: mechanically stirring for 20min under the condition of a water bath at 50 ℃, wherein the mechanical rotation speed is 1200r/min, and the ultrasonic frequency is 35kHz;
wherein the centrifugation time in the step 8 is 10-45 min, and the rotation speed of the centrifuge is 6500-9000 r/min;
wherein the curing temperature and curing time are as follows: 80 ℃/1h +110 ℃/1h +140 ℃/1h +160 ℃/1h;
wherein the epoxy resin is bisphenol A type epoxy resin E-51; the curing agent is methyl tetrahydrophthalic anhydride; the accelerant is 1-cyanoethyl-2-ethyl-4-methylimidazole; the toughening agent is CGR040; the release agent is JD-909A.
The invention has the beneficial effects that:
the insulator prepared by the preparation method of the gradient insulator made of the nano zinc oxide modified epoxy resin material has the advantages of improving the distribution of nano particles and the appearance structure of the insulator while considering the performance of the insulator material, optimizing the distribution of the electric field intensity of the edge surface of the insulator, improving the flashover resistance of the edge surface of the insulator, effectively improving the distribution condition of the electric field of the edge surface of the insulator, improving the electric resistance of the insulator and prolonging the actual service life.
Drawings
FIG. 1 is a flow chart of the preparation method of the gradient insulator made of the nano zinc oxide modified epoxy resin material according to the present invention;
FIG. 2 shows the distribution of the electric field along the surface of the gradient insulator and the non-gradient insulator prepared by the method for preparing the gradient insulator made of the nano zinc oxide modified epoxy resin material.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention provides a preparation method of a gradient insulator made of a nano zinc oxide modified epoxy resin material, which is specifically implemented according to the following steps as shown in figure 1:
step 1.1, analyzing and optimizing the distribution characteristic of the electric field intensity along the surface of the insulator by using COMSOL software to obtain an optimized curve of the side surface of the insulator and construct an insulator morphology structure model;
and 1.2, drawing an insulator mold model for the structural model by using Soildworks software. Slicing the insulator mold model by using Cura software;
step 1.3, printing and manufacturing the insulator mold by using a 3D printing technology;
step 2.1, weighing 50g of nano zinc oxide on an insulating medium plate;
step 2.2, adopting a DBD plasma fluorination device, setting a pulse wave with the power voltage of 7kV and the discharge frequency of 9kHz, setting the air pressure of a reaction cavity to be 13.5kPa, and setting the volume ratio of carbon tetrafluoride gas to nitrogen gas to be 25:1, the fluorination treatment time is 10min;
step 2.3, collecting the treated powder for later use;
step 3.1, respectively weighing the following components of epoxy resin, curing agent, accelerant, toughening agent and nano zinc oxide according to the mass ratio, wherein 80g of curing agent, 0.8g of accelerant, 20g of toughening agent and 2.028-24.818 g of nano zinc oxide are added into every 100g of epoxy resin;
and 3.2, mechanically stirring the epoxy resin and the nano zinc oxide powder weighed in the step 3.1 for 20min by ultrasonic waves under the condition of a water area of 50 ℃. Wherein the mechanical rotating speed is 1200r/min, and the ultrasonic frequency is 35kHz;
and 3.3, adding the curing agent, the accelerating agent and the toughening agent weighed in the step 3.1 into the nano zinc oxide/epoxy resin mixture. Stirring for 20min according to the conditions of step 3.2.
Preferably, the epoxy resin is bisphenol A type epoxy resin E-51; the curing agent is methyl tetrahydrophthalic anhydride; the accelerant is 1-cyanoethyl-2-ethyl-4-methylimidazole; the flexibilizer is CGR040; the particle size of the nano zinc oxide is 30-60 nm, and the purity is more than or equal to 99 percent; the release agent is JD-909A;
step 6, placing the epoxy group mixture into a processed mold, and fixing the insulator mold on a centrifuge;
step 7, starting the centrifugal machine, wherein the centrifugal time is 10-45 min, and the rotating speed of the centrifugal machine is 6500-9000 r/min;
step 8, stopping the centrifugal machine, placing the insulator mold in an oven and curing at high temperature; the curing temperature and curing time were: 80 ℃/1h +110 ℃/1h +140 ℃/1h +160 ℃/1h.
Example 1
A preparation method of a gradient insulator made of a nano zinc oxide modified epoxy resin material comprises the following steps:
step 1.1, analyzing and optimizing the distribution characteristics of the electric field intensity of the edge surface of the insulator by using COMSOL software to obtain an optimized curve of the side surface of the insulator, and constructing a shape structure model of the insulator.
And 1.2, drawing an insulator mold model for the structural model by using Soildworks software. The insulator mold model was sliced using Cura software.
And step 1.3, printing and manufacturing the insulator mold by using a 3D printing technology.
step 2.1, weighing 50g of nano zinc oxide on an insulating medium plate;
step 2.2, adopting a DBD plasma fluorination device, setting a pulse wave with the power voltage of 7kV and the discharge frequency of 9kHz, wherein the air pressure of a reaction cavity is 13.5kPa, and the volume ratio of carbon tetrafluoride gas to nitrogen is 25:1, the fluorination treatment time is 10min;
and 2.3, collecting the treated powder for later use.
step 3.1, respectively weighing the following components of epoxy resin, curing agent, accelerant, toughening agent and nano zinc oxide according to the mass ratio, wherein 80g of curing agent, 0.8g of accelerant, 20g of toughening agent and 2.028g of nano zinc oxide are added into every 100g of epoxy resin;
and 3.2, mechanically stirring the epoxy resin and the nano zinc oxide powder weighed in the step 3.1 for 20min by ultrasonic waves under the condition of a water area of 50 ℃. Wherein the mechanical rotating speed is 1200r/min, and the ultrasonic frequency is 35kHz;
and 3.3, adding the curing agent, the accelerating agent and the toughening agent weighed in the step 3.1 into the nano zinc oxide/epoxy resin mixture. Stirring for 20min according to the conditions of step 3.2.
Preferably, the epoxy resin is bisphenol A type epoxy resin E-51; the curing agent is methyl tetrahydrophthalic anhydride; the accelerant is 1-cyanoethyl-2-ethyl-4-methylimidazole; the flexibilizer is CGR040; the particle size of the nano zinc oxide is 30-60 nm, and the purity is more than or equal to 99 percent; the release agent is JD-909A;
step 6, placing the epoxy group mixture into a processed mold, and fixing the insulator mold on a centrifuge;
step 7, starting the centrifugal machine, wherein the centrifugal time is 10min, and the rotating speed of the centrifugal machine is 6500r/min;
step 8, stopping the centrifugal machine, placing the insulator mold into an oven and curing at high temperature, wherein the curing temperature and the curing time are as follows: 80 ℃/1h +110 ℃/1h +140 ℃/1h +160 ℃/1h.
Example 2
A preparation method of a gradient insulator made of a nano zinc oxide modified epoxy resin material comprises the following steps:
step 1.1, analyzing and optimizing the distribution characteristics of the electric field intensity along the surface of the insulator by using COMSOL software to obtain an optimized curve of the side surface of the insulator and construct an insulator morphology structure model.
Step 1.2, drawing an insulator mold model for the structure model by using Soildworks software, and slicing the insulator mold model by using Cura software;
step 1.3, printing and manufacturing the insulator mold by using a 3D printing technology;
step 2.1, weighing 50g of nano zinc oxide on an insulating medium plate;
step 2.2, adopting a DBD plasma fluorination device, setting a pulse wave with the power voltage of 7kV and the discharge frequency of 9kHz, wherein the air pressure of a reaction cavity is 13.5kPa, and the volume ratio of carbon tetrafluoride gas to nitrogen is 25:1, the fluorination treatment time is 10min;
step 2.3, collecting the processed powder for later use;
step 3.1, respectively weighing the following components of epoxy resin, curing agent, accelerator, toughening agent and nano zinc oxide according to the mass ratio, and adding 80g of curing agent, 0.8g of accelerator, 20g of toughening agent and 15.114g of nano zinc oxide into every 100g of epoxy resin;
and 3.2, mechanically stirring the epoxy resin and the nano zinc oxide powder weighed in the step 3.1 for 20min by ultrasonic waves under the condition of a water area of 50 ℃. Wherein the mechanical rotating speed is 1200r/min, and the ultrasonic frequency is 35kHz;
step 3.3, adding the curing agent, the accelerating agent and the toughening agent weighed in the step 3.1 into the nano zinc oxide/epoxy resin mixture; stirring for 20min according to the conditions of the step 3.2;
preferably, the epoxy resin is bisphenol A type epoxy resin E-51; the curing agent is methyl tetrahydrophthalic anhydride; the accelerant is 1-cyanoethyl-2-ethyl-4-methylimidazole; the flexibilizer is CGR040; the particle size of the nano zinc oxide is 30-60 nm, and the purity is more than or equal to 99 percent; the release agent is JD-909A.
step 6, placing the epoxy mixture in a processed mould, and fixing the insulator mould on a centrifuge;
step 7, starting a centrifugal machine, wherein the centrifugal time is 20min, and the rotating speed of the centrifugal machine is 8000r/min;
and 8, stopping the centrifugal machine, placing the insulator mould into an oven and curing at high temperature, wherein the curing temperature and the curing time are as follows: 80 ℃/1h +110 ℃/1h +140 ℃/1h +160 ℃/1h.
Example 3
A preparation method of a gradient insulator made of a nano zinc oxide modified epoxy resin material comprises the following steps:
step 1.1, analyzing and optimizing the distribution characteristic of the electric field intensity along the surface of the insulator by using COMSOL software to obtain an optimized curve of the side surface of the insulator and construct an insulator morphology structure model;
step 1.2, drawing an insulator mold model for the structure model by using Soildworks software; the insulator mold model was sliced using Cura software.
Step 1.3, printing and manufacturing the insulator mold by using a 3D printing technology;
step 2.1, weighing 50g of nano zinc oxide on an insulating medium plate;
step 2.2, adopting a DBD plasma fluorination device, setting a pulse wave with the power voltage of 7kV and the discharge frequency of 9kHz, wherein the air pressure of a reaction cavity is 13.5kPa, and the volume ratio of carbon tetrafluoride gas to nitrogen is 25:1, the fluorination treatment time is 10min;
step 2.3, collecting the treated powder for later use;
step 3.1, respectively weighing the following components of epoxy resin, curing agent, accelerator, toughening agent and nano zinc oxide according to the mass ratio, and adding 80g of curing agent, 0.8g of accelerator, 20g of toughening agent and 24.818g of nano zinc oxide into every 100g of epoxy resin;
step 3.2, mechanically stirring the epoxy resin and the nano zinc oxide powder weighed in the step 3.1 by ultrasonic waves for 20min under the condition of a water area at 50 ℃; wherein the mechanical rotating speed is 1200r/min, and the ultrasonic frequency is 35kHz;
and 3.3, adding the curing agent, the accelerating agent and the toughening agent weighed in the step 3.1 into the nano zinc oxide/epoxy resin mixture. Stirring for 20min according to the conditions of step 3.2.
Preferably, the epoxy resin is bisphenol A type epoxy resin E-51; the curing agent is methyl tetrahydrophthalic anhydride; the accelerant is 1-cyanoethyl-2-ethyl-4-methylimidazole; the flexibilizer is CGR040; the particle size of the nano zinc oxide is 30-60 nm, and the purity is more than or equal to 99 percent; the release agent is JD-909A.
step 6, placing the epoxy mixture in a processed mould, and fixing the insulator mould on a centrifuge;
step 7, starting a centrifugal machine, wherein the centrifugal time is 45min, and the rotating speed of the centrifugal machine is 9000r/min;
step 8, stopping the centrifugal machine, placing the insulator mold in an oven and curing at high temperature; the curing temperature and curing time were: 80 ℃/1h +110 ℃/1h +140 ℃/1h 160 ℃/1h.
The distribution of the electric field intensity along the surface of the gradient insulator and the non-gradient insulator is shown in the attached figure 2; as is evident from fig. 2, compared with the non-gradient insulator, the gradient insulator has a smoother and more linear electric field intensity curve along the surface, and the electric field intensity distribution along the surface is more uniform.
Claims (10)
1. The preparation method of the gradient insulator made of the nano zinc oxide modified epoxy resin material is characterized by comprising the following steps:
step 1, manufacturing an insulator gradient centrifugal mold by using a 3D printing technology;
step 2, carrying out fluorination modification treatment on the nano zinc oxide particles;
step 3, mixing epoxy resin, a curing agent, an accelerator, a toughening agent and fluorinated nano zinc oxide to prepare an epoxy group mixture;
step 4, carrying out vacuum pumping treatment on the epoxy group mixture, wherein the vacuum pumping time is 40min;
step 5, spraying a release agent on the mold manufactured in the step 1, and putting the mold into an oven at 80 ℃ to dry the release agent;
step 6, placing the epoxy-based mixture into the mold processed in the step 5, and fixing the insulator mold on a centrifuge;
step 7, starting the centrifuge;
and 8, stopping the centrifugal machine, placing the insulator mold into an oven and curing at high temperature.
2. The method for preparing the gradient insulator made of the nano zinc oxide modified epoxy resin material according to claim 1, wherein the step 1 is implemented by the following steps:
step 1.1, analyzing and optimizing the distribution characteristic of the electric field intensity along the surface of the insulator by using COMSOL software to obtain an optimized curve of the side surface of the insulator and construct an insulator morphology structure model;
step 1.2, drawing an insulator mold model for the structure model by using Soildworks software, and slicing the insulator mold model by using Cura software;
and step 1.3, printing and manufacturing the insulator mold by using a 3D printing technology.
3. The method for preparing the gradient insulator made of the nano zinc oxide modified epoxy resin material according to claim 1, wherein the particle size of the nano zinc oxide particles in the step 2 is 30-60 nm, and the purity is more than or equal to 99%.
4. The method for preparing the gradient insulator made of the nano zinc oxide modified epoxy resin material according to claim 1, wherein the step 2 is specifically implemented according to the following steps:
step 2.1, placing nano zinc oxide on an insulating medium plate;
2.2, fluorinating by adopting a DBD plasma fluorination device;
and 2.3, collecting the treated powder for later use.
5. The method for preparing the gradient insulator of the nano zinc oxide modified epoxy resin material according to claim 4, wherein the fluorination conditions in the step 2.2 are as follows: setting a pulse wave with the power voltage of 7kV and the discharge frequency of 9kHz, wherein the air pressure of a reaction cavity is 13.5kPa, and the volume ratio of carbon tetrafluoride gas to nitrogen is 25: and 1, the fluorination treatment time is 10min.
6. The method for preparing the gradient insulator made of the nano zinc oxide modified epoxy resin material according to claim 1, wherein the step 3 is specifically implemented according to the following steps:
step 3.1, respectively weighing the following components of epoxy resin, curing agent, accelerator, toughening agent and nano zinc oxide according to the mass ratio, and adding 80g of curing agent, 0.8g of accelerator, 20g of toughening agent and 24.818g of nano zinc oxide into every 100g of epoxy resin;
step 3.2, mechanically mixing the epoxy resin weighed in the step 3.1 with the nano zinc oxide powder;
step 3.3, adding the curing agent, the accelerating agent and the toughening agent weighed in the step 3.1 into the nano zinc oxide/epoxy resin mixture mixed in the step 3.2; stirring for 20min according to the mechanical mixing conditions of step 3.2.
7. The method for preparing the gradient insulator of the nano zinc oxide modified epoxy resin material according to claim 6, wherein the mechanical mixing conditions in the step 3.2 are as follows: and (3) carrying out ultrasonic mechanical stirring for 20min under the water bath condition of 50 ℃, wherein the mechanical rotating speed is 1200r/min, and the ultrasonic frequency is 35kHz.
8. The method for preparing the gradient insulator made of the nano zinc oxide modified epoxy resin material according to claim 1, wherein the centrifugation time in the step 8 is 10-45 min, and the rotation speed of a centrifuge is 6500-9000 r/min.
9. The method for preparing the gradient insulator made of the nano zinc oxide modified epoxy resin material according to claim 1, wherein the curing temperature and the curing time are as follows: 80 ℃/1h +110 ℃/1h +140 ℃/1h +160 ℃/1h.
10. The method for preparing the gradient insulator made of the nano zinc oxide modified epoxy resin material according to claim 1, wherein the epoxy resin is bisphenol A epoxy resin E-51; the curing agent is methyl tetrahydrophthalic anhydride; the accelerant is 1-cyanoethyl-2-ethyl-4-methylimidazole; the flexibilizer is CGR040; the release agent is JD-909A.
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| CN105679473A (en) * | 2016-01-18 | 2016-06-15 | 西安交通大学 | Lamination fabrication method of dielectric functionally graded insulator |
| CN112613215A (en) * | 2020-12-23 | 2021-04-06 | 平高集团有限公司 | Basin-type insulator optimization method |
| WO2022123924A1 (en) * | 2020-12-07 | 2022-06-16 | 株式会社 東芝 | Insulating resin composition, insulating member formed of cured product of same, and electrical device |
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2022
- 2022-07-20 CN CN202210850798.3A patent/CN115214138A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101428844A (en) * | 2008-12-04 | 2009-05-13 | 东华大学 | Method for processing barometric-pressure, normal-temperature plasma modification on nano-zinc oxide surface |
| CN102391620A (en) * | 2011-08-30 | 2012-03-28 | 西安交通大学 | Epoxy resin matrix nano-zinc oxide composite material and preparation method thereof |
| CN105542399A (en) * | 2016-01-18 | 2016-05-04 | 西安交通大学 | Centrifugal manufacturing method for dielectric functional gradient insulator |
| CN105679473A (en) * | 2016-01-18 | 2016-06-15 | 西安交通大学 | Lamination fabrication method of dielectric functionally graded insulator |
| WO2022123924A1 (en) * | 2020-12-07 | 2022-06-16 | 株式会社 東芝 | Insulating resin composition, insulating member formed of cured product of same, and electrical device |
| CN112613215A (en) * | 2020-12-23 | 2021-04-06 | 平高集团有限公司 | Basin-type insulator optimization method |
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