CN112646315A - Epoxy resin nano composite insulating material with low temperature coefficient of electrical conductivity and preparation method thereof - Google Patents
Epoxy resin nano composite insulating material with low temperature coefficient of electrical conductivity and preparation method thereof Download PDFInfo
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- CN112646315A CN112646315A CN202011394075.4A CN202011394075A CN112646315A CN 112646315 A CN112646315 A CN 112646315A CN 202011394075 A CN202011394075 A CN 202011394075A CN 112646315 A CN112646315 A CN 112646315A
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- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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Abstract
The invention relates to an epoxy resin nano composite insulating material with low temperature coefficient of electrical conductivity and a preparation method thereof, which is technically characterized in that: the epoxy resin nano composite insulating material comprises the following raw material components in parts by weight: 0.05-0.5 part of graphene oxide, 100 parts of epoxy resin and 85 parts of curing agent. The preparation method of the insulating material comprises a raw material mixing step and a material curing step. The invention has reasonable design, reduces the temperature dependence characteristic of the conductivity by doping the graphene oxide into the epoxy resin material, weakens the electric field distortion in the electrical equipment, provides an effective scheme for the homogenization of the electric field and the structural optimization of the electrical equipment, effectively solves the problem of the electric field distortion of the direct current electrical equipment caused by the temperature, and can be widely applied to the field of insulating materials of direct current power systems.
Description
Technical Field
The invention belongs to the technical field of insulating materials, and particularly relates to an epoxy resin nano composite insulating material with a low temperature coefficient of electrical conductivity and a preparation method thereof.
Background
With the continuous development of power systems, trans-regional and long-distance power transmission has become one of the important ways to solve energy transmission. The transmission distance between a large energy source and a load center is typically 1000-3000 km. The traditional extra-high voltage alternating current system can not meet the requirement of large-capacity long-distance power transmission. High voltage direct current transmission (HVDC), especially ultra-high voltage direct current transmission (UHVDC), has been proved to be an ideal solution for long-distance, efficient and reliable transmission by virtue of its characteristics of low loss, large capacity, small occupied area, high efficiency and stability.
In dc power systems, the main problem of electrical insulation is the electric field distribution problem. In the alternating current case, the electric field of the insulating material depends on the dielectric constant of the insulating material, which is not sensitive to temperature; the direct current condition is greatly different from the alternating current condition, the electric field distribution under the direct current depends on the conductivity of the insulating material, the conductivity highly depends on the temperature, according to the Arrhenius equation, the conductivity and the temperature are in a nonlinear exponential relationship, so that the conductivity of the insulating material shows the difference in order of magnitude under the influence of the temperature gradient, the electric field inside the electric equipment is seriously distorted under the actual operation condition, and the conductivity multiplied by the order of magnitude can cause overlarge leakage current and abnormal heating. Particularly, in the high-voltage direct-current bushing, heat is generated by joule heating of a conductor under high current, and an insulating medium is usually a 'hot poor conductor', so that the heat dissipation problem of the bushing is serious, and the temperature gradient distribution from inside to outside is presented on the whole. In addition, the main insulation of the sleeve is a multi-layer aluminum foil-crepe paper-epoxy resin composite structure, and an interface has a remarkable space charge effect under the action of direct current, so that the electric field distribution in the insulating material is distorted, the accelerated degradation of the insulating material is caused, and even the service life is shortened.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides an epoxy resin nano composite insulating material with a low temperature coefficient of electrical conductivity and a preparation method thereof, and solves the problem of electric field distortion of direct-current electrical equipment caused by temperature.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
the epoxy resin nano composite insulating material with the low temperature coefficient of electrical conductivity comprises the following raw material components in parts by mass:
0.05-0.5 part of graphene oxide;
100 parts of epoxy resin;
and 85 parts of a curing agent.
Further, the graphene oxide is flaky graphene oxide particles with the thickness of less than 3nm and the sheet diameter of less than 10 μm; the epoxy resin is low-viscosity bisphenol A epoxy resin E51; the curing agent is methyl tetrahydrophthalic anhydride.
Further, the graphene oxide accounts for 0.05 part, 0.1 part or 0.5 part, and the prepared epoxy resin nano composite insulating material with the low temperature coefficient of electrical conductivity is EP/GO-0.05, EP/GO-0.1 or EP/GO-0.5.
A preparation method of an epoxy resin nano composite insulating material with low temperature coefficient of electrical conductivity comprises the following steps:
step 2, material curing step: mixing a mixture of epoxy resin and graphene oxide with a curing agent, stirring with a magnetic stirrer, degassing the mixture obtained by stirring to remove air bubbles, pouring the degassed mixture into a mold, and then curing.
Further, in the step 1, ethanol and graphene oxide are mixed according to a weight ratio of 1: 100 to obtain a mixed solution of graphene oxide and ethanol.
Further, the time of the ultrasonic treatment in the step 1 is 1 hour.
Further, the stirring in step 1 was performed by uniformly stirring with a magnetic stirrer at 90 ℃ for 6 hours.
Further, the stirring of step 2 is performed by stirring with a magnetic stirrer for 30 minutes.
Further, the degassing treatment of step 2 is carried out by degassing in a vacuum oven at 50 ℃ for 1 hour.
Further, the curing process of step 2 is as follows: first at 100 ℃ for 15 hours and then at 145 ℃ for 20 hours.
The invention has the advantages and positive effects that:
the invention has reasonable design, reduces the temperature dependence characteristic of the conductivity by doping the graphene oxide into the epoxy resin material, weakens the electric field distortion in the electrical equipment, provides an effective scheme for the homogenization of the electric field and the structural optimization of the electrical equipment, effectively solves the problem of the electric field distortion of the direct current electrical equipment caused by the temperature, and can be widely applied to the field of insulating materials of direct current power systems.
Drawings
FIG. 1 is a schematic diagram of the preparation process of the epoxy resin nanocomposite insulating material with low temperature coefficient of electrical conductivity according to the present invention;
FIG. 2 is a scanning electron microscope image of an epoxy resin/graphene oxide nanocomposite insulating material, wherein (a) is an epoxy resin material, (b) is an EP/GO-0.05 material, (c) is an EP/GO-0.1 material, and (d) is an EP/GO-0.5 material;
FIG. 3 is a reciprocal plot of DC conductivity versus temperature (1000/T) at 8kV/mm for neat epoxy and various EP/GO nanocomposites.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
Example 1
The epoxy resin nano composite insulating material with the low temperature coefficient of electrical conductivity is prepared from the following raw materials in parts by weight:
0.05 part of flaky graphene oxide particles
100 parts of epoxy resin matrix
85 parts of curing agent
Wherein the Graphene oxide particles are provided by Suzhou Tangfeng Graphene Technology, and have a thickness of less than 3nm and a lamella diameter of less than 10 μm. The epoxy resin matrix adopts low-viscosity bisphenol A epoxy resin E51, and has the characteristics of low viscosity and liquid at room temperature. The curing agent is methyl tetrahydrophthalic anhydride (MTHPA) curing agent.
The preparation method of the epoxy resin nanocomposite insulating material with low temperature coefficient of electrical conductivity of the embodiment, as shown in fig. 1, includes the following steps:
step 2, carrying out ultrasonic treatment on the mixed solution of graphene oxide and ethanol for 1 hour to obtain a uniformly dispersed suspension solution;
step 3, adding the weighed epoxy resin into the suspension, wherein the weight proportion of the filler is 0.05 percent of the weight of the epoxy resin;
step 4, carrying out ultrasonic treatment on the mixture obtained in the step 3 for one hour to obtain uniform dispersion; then stirred with a magnetic stirrer at 90 ℃ for 6 hours to remove ethanol. After evaporation of the ethanol a mixture of epoxy resin and graphene oxide is obtained, defined herein as EP/GO-0.05;
step 5, mixing the following components in a weight ratio of 100: 85 the mixture obtained in step 4 is mixed with a curing agent.
Step 6, stirring for 30 minutes by using a magnetic stirrer;
step 7, the obtained mixture was degassed in a vacuum oven at 50 ℃ for 1 hour to remove air bubbles.
Step 8, pouring the degassed mixture into a container with an internal dimension of 10X 0.5mm3Or 10X 0.2mm3Was cured at 100 ℃ for 15 hours and then at 145 ℃ for 20 hours to obtain a test sample, wherein the sample had a thickness of 0.2mm for conductivity test and a thickness of 0.5mm for scanning electron microscope test.
The steps 1-5 are filler dispersing processes, and the steps 5-8 are material curing processes.
The low-temperature-coefficient-of-conductivity epoxy resin nanocomposite insulation material prepared by the embodiment is defined as an EP/GO-0.05 material.
Example 2
The epoxy resin nanocomposite insulating material with the low temperature coefficient of electrical conductivity of the embodiment is prepared from the following raw materials in parts by weight:
0.1 part of flaky graphene oxide particles
100 parts of epoxy resin matrix
85 parts of curing agent
Wherein the Graphene oxide particles are provided by Suzhou Tangfeng Graphene Technology, and have a thickness of less than 3nm and a lamella diameter of less than 10 μm; the epoxy resin matrix is low-viscosity bisphenol A epoxy resin E51, and has the characteristics of low viscosity and liquid at room temperature; the curing agent is methyl tetrahydrophthalic anhydride (MTHPA) curing agent.
The doping amount of this example is 0.1 wt%, and the preparation method of the low temperature coefficient of electrical conductivity epoxy resin composite insulating material is the same as that of example 1.
The low-temperature-coefficient-of-conductivity epoxy resin nanocomposite insulating material prepared in the embodiment is defined as an EP/GO-0.1 material.
Example 3
The low-temperature-coefficient-of-conductivity epoxy resin nanocomposite insulating material is prepared from the following raw materials in parts by weight:
0.5 part of flaky graphene oxide particles
100 parts of epoxy resin matrix
85 parts of curing agent
Wherein the Graphene oxide particles are provided by Suzhou Tangfeng Graphene Technology, and have a thickness of less than 3nm and a lamella diameter of less than 10 μm; the epoxy resin matrix is low-viscosity bisphenol A epoxy resin E51, and has the characteristics of low viscosity and liquid at room temperature; the curing agent is methyl tetrahydrophthalic anhydride (MTHPA) curing agent.
The doping amount of this example is 0.5 wt%, and the preparation method of the low temperature coefficient of electrical conductivity epoxy resin composite insulating material is the same as that of example 1.
The low-temperature-coefficient-of-conductivity epoxy resin nanocomposite insulating material prepared in the embodiment is defined as EP/GO-0.5 material.
The properties of the low-temperature coefficient of conductivity epoxy resin nanocomposite insulation material of the present invention were analyzed below.
Fig. 2 shows scanning electron microscope images of the fractured surfaces of EP/GO nanocomposite insulation materials with different additive contents, and it is evident that the graphene oxide particles are uniformly dispersed in the resin, with a diameter of about 5 μm, consistent with the parameters provided by the supplier.
As shown in FIG. 3, for pure epoxy, it is charged at room temperature and 100 deg.CPermeability of 7.70X 10-17And 4.55X 10-13S/m, the difference between the two is more than three orders of magnitude. The electric conductivities of the EP/GO-0.05, the EP/GO-0.1 and the EP/GO-0.5 nano composite materials at 100 ℃ are respectively 3.89 multiplied by 10-13、2.79×10-13And 5.89X 10-13S/m, nearly equal to the conductivity of pure epoxy. While the electrical conductivity of the composite materials of EP/GO-0.05, EP/GO-0.1 and EP/GO-0.5 at room temperature (20 ℃) is 4.77 multiplied by 10-16、1.81×10-15And 4.33X 10-15S/m, the conductivity is improved along with the increase of the graphene oxide filler, and the maximum improvement amplitude of EP/GO-0.5 is about 5.6 multiplied by 1 orders of magnitude. It can be seen that the temperature coefficient of electrical conductivity gradually decreases with the addition of graphene oxide, but the effect is no longer significant when the addition content reaches 0.1 wt%.
It should be emphasized that the embodiments described herein are illustrative rather than restrictive, and thus the present invention is not limited to the embodiments described in the detailed description, but also includes other embodiments that can be derived from the technical solutions of the present invention by those skilled in the art.
Claims (10)
1. A low-conductivity temperature coefficient epoxy resin nano composite insulating material is characterized in that: the raw material components and the parts by weight of the components are as follows:
0.05-0.5 part of graphene oxide;
100 parts of epoxy resin;
and 85 parts of a curing agent.
2. The low temperature coefficient of conductance epoxy nanocomposite insulation material of claim 1, wherein: the graphene oxide is flaky graphene oxide particles with the thickness of less than 3nm and the sheet diameter of less than 10 mu m; the epoxy resin is low-viscosity bisphenol A epoxy resin E51; the curing agent is methyl tetrahydrophthalic anhydride.
3. The low temperature coefficient of conductivity epoxy resin nanocomposite insulation of claim 1 or 2, wherein: the graphene oxide accounts for 0.05 part, 0.1 part or 0.5 part, and the prepared epoxy resin nano composite insulating material with the low temperature coefficient of electrical conductivity is EP/GO-0.05, EP/GO-0.1 or EP/GO-0.5.
4. A method for preparing the low temperature coefficient of conductivity epoxy resin nanocomposite insulation material according to claim 1, 2 or 3, comprising the steps of:
step 1, raw material mixing step: adding graphene oxide into ethanol to obtain a graphene oxide ethanol mixed solution; adding epoxy resin into the graphene oxide ethanol mixed solution, and performing ultrasonic treatment to obtain a uniform dispersion; uniformly stirring by using a magnetic stirrer to remove ethanol, and obtaining a mixture of epoxy resin and graphene oxide;
step 2, material curing step: mixing a mixture of epoxy resin and graphene oxide with a curing agent, stirring with a magnetic stirrer, degassing the mixture obtained by stirring to remove air bubbles, pouring the degassed mixture into a mold, and then curing.
5. The method for preparing the epoxy resin nanocomposite insulation material with low temperature coefficient of electrical conductance according to claim 4, wherein: in the step 1, ethanol and graphene oxide are mixed according to a weight ratio of 1: 100 to obtain a mixed solution of graphene oxide and ethanol.
6. The method for preparing the epoxy resin nanocomposite insulation material with low temperature coefficient of electrical conductance according to claim 4, wherein: the time of the ultrasonic treatment in the step 1 is 1 hour.
7. The method for preparing the epoxy resin nanocomposite insulation material with low temperature coefficient of electrical conductance according to claim 4, wherein: the stirring in step 1 was performed by uniformly stirring at 90 ℃ for 6 hours using a magnetic stirrer.
8. The method for preparing the epoxy resin nanocomposite insulation material with low temperature coefficient of electrical conductance according to claim 4, wherein: the stirring of step 2 is completed by stirring with a magnetic stirrer for 30 minutes.
9. The method for preparing the epoxy resin nanocomposite insulation material with low temperature coefficient of electrical conductance according to claim 4, wherein: the degassing treatment of step 2 is carried out by degassing in a vacuum oven at 50 ℃ for 1 hour.
10. The method for preparing the epoxy resin nanocomposite insulation material with low temperature coefficient of electrical conductance according to claim 4, wherein: the curing process of the step 2 comprises the following steps: first at 100 ℃ for 15 hours and then at 145 ℃ for 20 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011394075.4A CN112646315A (en) | 2020-12-03 | 2020-12-03 | Epoxy resin nano composite insulating material with low temperature coefficient of electrical conductivity and preparation method thereof |
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| CN202011394075.4A CN112646315A (en) | 2020-12-03 | 2020-12-03 | Epoxy resin nano composite insulating material with low temperature coefficient of electrical conductivity and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113278251A (en) * | 2021-04-26 | 2021-08-20 | 厦门理工学院 | Epoxy resin for flexible circuit board, preparation method and device thereof, and computer equipment |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286189A (en) * | 2011-06-24 | 2011-12-21 | 中国科学院理化技术研究所 | Method for preparing graphene oxide/epoxide resin nano composite material |
| CN103627139A (en) * | 2013-09-25 | 2014-03-12 | 杭州师范大学 | Preparation method of functionalized graphene oxide/epoxy resin nanocomposite |
| US20180312647A1 (en) * | 2017-04-28 | 2018-11-01 | The Boeing Company | Nano-reinforcement filler material for epoxy resin systems and methods of making the same |
| CN111763406A (en) * | 2020-08-05 | 2020-10-13 | 兰州交通大学 | Preparation process of graphene nanocomposite |
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2020
- 2020-12-03 CN CN202011394075.4A patent/CN112646315A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286189A (en) * | 2011-06-24 | 2011-12-21 | 中国科学院理化技术研究所 | Method for preparing graphene oxide/epoxide resin nano composite material |
| CN103627139A (en) * | 2013-09-25 | 2014-03-12 | 杭州师范大学 | Preparation method of functionalized graphene oxide/epoxy resin nanocomposite |
| US20180312647A1 (en) * | 2017-04-28 | 2018-11-01 | The Boeing Company | Nano-reinforcement filler material for epoxy resin systems and methods of making the same |
| CN111763406A (en) * | 2020-08-05 | 2020-10-13 | 兰州交通大学 | Preparation process of graphene nanocomposite |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113278251A (en) * | 2021-04-26 | 2021-08-20 | 厦门理工学院 | Epoxy resin for flexible circuit board, preparation method and device thereof, and computer equipment |
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Application publication date: 20210413 |