CN115110335A - Novel nano modified insulating paper and preparation method and application thereof - Google Patents
Novel nano modified insulating paper and preparation method and application thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/675—Oxides, hydroxides or carbonates
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/69—Water-insoluble compounds, e.g. fillers, pigments modified, e.g. by association with other compositions prior to incorporation in the pulp or paper
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/50—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by form
- D21H21/52—Additives of definite length or shape
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/48—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances fibrous materials
- H01B3/52—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances fibrous materials wood; paper; press board
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F27/00—Details of transformers or inductances, in general
- H01F27/28—Coils; Windings; Conductive connections
- H01F27/32—Insulating of coils, windings, or parts thereof
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Abstract
The invention discloses novel nano modified insulating paper and a preparation method and application thereof. The novel insulating material has better breakdown characteristic, pore structure and dielectric characteristic. The preparation method comprises the following steps: mixing the alumina nano particles with absolute ethyl alcohol and oleic acid together, performing ultrasonic dispersion, centrifugal separation, cleaning, drying and grinding to obtain alumina nano particles, and mixing the alumina nano particles with transformer oil to obtain the nano modified oil. Preparing paper pulp from a paperboard, mixing and stirring the paper pulp and the nano modified oil, and putting the mixture into a paper forming machine to obtain the nano modified insulating paper. According to the invention, the nano alumina particles are utilized to modify the insulating paper, so that the pore structure of the insulating paper is changed, the breakdown characteristic of the insulating paper is improved, the dielectric constant of fibers in the insulating paper is changed, and the overall performance is improved.
Description
Technical Field
The invention belongs to the technical field of special paper preparation, and particularly relates to novel nano modified insulating paper, a preparation method and application thereof.
Background
The power transformer is a core device of a power system network, is key equipment for power transmission and conversion, and is widely applied to large power transformers by taking oil-immersed insulating paper as an insulating material and taking an oil-paper insulating system as an insulating structure. During long-term operation, the oil paper insulation system is affected by thousands of lightning pulses, which is called cumulative effect, and the cumulative effect can cause irreversible damage to the insulation paper and even cause premature failure of the insulation paper, thereby seriously affecting the insulation performance and the operation safety of the transformer. At present, the study of scholars at home and abroad on the accumulation effect is less, the study on the modification of the insulating paper by adding inorganic nano alumina particles is only reported, and the improvement of the performance of the insulating paper by the nanotechnology has a great development space.
Disclosure of Invention
Based on the problems in the existing nano modification technology, the invention provides novel nano modified insulating paper and a preparation method and application thereof. The method is based on the manufacturing industry of the traditional nanometer modified insulating paper, the insulating paper is modified by doping nanometer alumina particles, and systematic experimental study and theoretical analysis are carried out on the breakdown characteristic, the pore structure, the dielectric characteristic and the like of the modified paper. Research results show that the breakdown characteristic of the insulating paper can be improved by modifying the insulating paper through the nano modified oil immersion, the pore structure of the insulating paper is changed, the dielectric constant of fibers in the insulating paper is changed, and the overall performance is improved.
A preparation method of novel nanometer modified insulating paper is characterized by comprising the following steps: the method comprises the following steps:
s1, preparation of nano modified oil: after the transformer oil and the alumina nanoparticles are respectively dried in a vacuum drying oven at 85-95 ℃ for 45-55 hours, adding the transformer oil into the particles containing the nano alumina, and performing ultrasonic dispersion to obtain nano modified oil;
wherein: 1-5 wt% of nano alumina particles in the nano modified oil;
s2, drying the nano modified oil: drying the nano modified oil prepared by the S1 in a vacuum drying oven at 85-95 ℃ for 45-55 hours to prepare dried nano modified oil for later use;
s3, preparation of a paper sample: the method comprises the following steps of (1) disassembling a paperboard, completely soaking the paperboard in deionized water for 20-30 hours, putting the paperboard into a beater, draining to obtain paper pulp, mixing the paper pulp with the deionized water to obtain a sample, putting the sample into a dissociator, adjusting the beating degree to 45 DEG SR, and dissociating for 1-3 times to obtain a paper sample;
s4, surface modification treatment: adding the alumina nanoparticles and KH550 into absolute ethyl alcohol, uniformly mixing to obtain a mixture, ultrasonically dispersing the mixture in a constant-temperature water bath at the temperature of 80-90 ℃ until the mixture becomes milky liquid to obtain nano liquid, mixing the paper sample obtained in S3 with the nano liquid, stirring in a magnetic stirrer, and putting in a paper forming machine to obtain nano modified paper;
wherein: the mass ratio of the alumina nano particles to the KH550 is 50: 0.5 to 5; 1-5 wt% of alumina nanoparticles in the mixture; the mass ratio of the paper sample to the nano liquid is 15-25: 1.
s5, preparing nano modified insulating paper: and (3) carrying out vacuum drying on the S4 nano modified paper, injecting purified and vacuum-degassed nano modified oil after drying, and soaking in oil for 40-55 hours to obtain the nano modified insulating paper.
In the technical scheme of the invention: the content of the nano alumina particles in the nano modified oil in S1 is 1-5 wt%.
The technical scheme of the invention is as follows: the mass ratio of the alumina nanoparticles to the KH550 in S4 is 50: 0.5 to 1.5.
The technical scheme of the invention is as follows: the mass ratio of the paper sample to the nano liquid in the S4 is 18-22: 1.
a novel nanometer modified insulating paper is prepared by the method.
In the technical scheme of the invention, the novel nano modified insulating paper prepared by the preparation method is applied to a transformer as insulating paper. Further, the breakdown field strength is a direct current breakdown field strength and/or a power frequency breakdown field strength.
According to the application, the insulating paper is modified by using the alumina nanoparticles, compared with the non-modified insulating paper, the breakdown voltage reaches a peak value when the alumina nanoparticles are 2 wt%, the dielectric constant of fibers in the insulating paper is reduced, the relative dielectric constant of the fibers and the insulating oil is closer, in 1 wt% and 2 wt% of the modified paper, the pore structure of the insulating paper is obviously changed, the number of small pores is very large, the number of large pores is much smaller, and the number of large pores of the 2 wt% of the modified paper is smaller than that of the 1 wt% of the modified paper. The phenomenon shows that the doping of the alumina nano particles with certain mass concentration can increase the number of small holes, reduce the number of large holes, change the pore structure, improve the breakdown voltage and reduce the dielectric constant, which has very important significance for improving the electrical performance of the insulating paper.
The technical scheme of the invention is as follows: the electrical performance of the nano modified insulating paper is enhanced by changing the gap structure of the nano modified insulating paper, and further, the alumina nano particles in the step S4 of preparing the novel nano modified insulating paper are 1 wt%; preferably, the alumina nanoparticles in the step of preparing the novel nano modified insulating paper S4 are 5 wt%; still more preferably, the alumina nanoparticles in the step S4 of preparing the novel nano modified insulation paper are 2 wt%.
The technical scheme of the invention is as follows: the novel nano modified insulating paper is beneficial to improving the breakdown characteristic and reducing the insulation breakdown and discharge caused by the abnormal insulating structure of the insulating paper in the converter transformer, the application of the novel nano modified insulating paper in the breakdown field strength is beneficial to improving the overall performance of the electrical equipment and ensuring the safe operation of the electrical equipment,
the novel nano modified insulating paper disclosed by the invention is applied to reducing the relative dielectric constant and/or dielectric loss and/or volume conductivity of the nano modified insulating paper.
The invention has the beneficial effects that:
1) the nanometer modified insulating paper prepared by the method is doped with alumina nanoparticles with different concentrations to change the pore structure of the cellulose paper and improve the breakdown characteristic of the insulating paper. The alumina nano particles have obvious influence on the breakdown characteristic of the insulating paper, the decomposition voltage of the modified paper at positive voltage is increased and then reduced along with the increase of the concentration of the nano particles, and the positive voltage is the maximum when the nano particles are 2 wt%. For negative voltages, the decomposition voltage of the modified paper gradually decreased with increasing nanoparticle concentration. The modified insulating oil-impregnated cellulose paper has stronger capability of resisting repeated pulse. The nano particles are beneficial to the dissipation of space charges, and the accumulation of the space charges is avoided, so that the distortion of an electric field is weakened, and the breakdown characteristic of the insulating paper is improved.
2) The nanometer modified insulating paper prepared by the invention changes the pore structure of the cellulose paper by doping alumina nanoparticles with different concentrations, enhances the bonding strength of the insulating paper and increases the breakdown field strength. The oil pores are considered as weak points in the oil paper composite insulation, and fail firstly under the impact voltage, compared with the common insulation paper, the nano modified insulation paper has the advantages that the number of small pores is increased, the number of large pores is reduced, and the pore structure is well improved. The modified paper having 1 wt% and 2 wt% of nanoparticles has a pore number of pores (hereinafter referred to as small pores) having a diameter of 5000nm to 10000nm, which is very large. Wherein the pore number of pores (hereinafter referred to as macropores) with the diameter of 5000-10000 nm is much smaller in the modified paper with 1 wt% and 2 wt% of nano particles, the macropore number of the modified paper with 2 wt% is smaller than that of the modified paper with 1 wt%, and the pore size distribution of the modified paper with 5 wt% is similar to that of the fresh cellulose paper. Test results show that the quantity of small holes can be increased and the quantity of large holes can be reduced by nano doping with proper mass concentration, and the dielectric breakdown field strength is inversely proportional to the gap distance, namely the breakdown field strength is higher when the hole diameter is smaller, so that the bonding strength is enhanced, and the breakdown field strength is increased
3) The nanometer modified insulating paper prepared by the method changes the pore structure of the cellulose paper by doping the alumina nanoparticles with different concentrations, and reduces the dielectric constant of the insulating paper. At a measurement frequency of 1MHz, the relative dielectric constant of the cellulose dropped to 2.44 at 2 wt% nanoparticles. Compared with the nanometer insulating paper with the nanometer particles and the cellulose which cannot be stably combined, the relative dielectric constant of the insulating paper is effectively reduced, and the method has very important significance for improving the ageing damage resistance of the transformer insulating system and reducing the dielectric loss.
Drawings
FIG. 1 shows the breakdown voltage of the modified insulating paper under different mass percentages of nanoparticles.
FIG. 2 shows the relative dielectric constant of the modified insulating paper under different mass percentages of nanoparticles.
FIG. 3 is a graph showing the change in the number of pores in modified paper for different mass percentages of nanoparticles.
FIG. 4 is a simplified model diagram of the relative dielectric constant of the oiled paper composite insulating material.
FIG. 5 is a graph of the effect of nanoparticles on dielectric properties.
FIG. 6 is the scanning electron microscope images of the fresh paper and the nano modified paper.
FIG. 7 Electron micrograph of nanoparticles.
FIG. 8 Electron micrograph of nanoparticles of S1 of example 1.
Detailed Description
The invention is further illustrated by the following examples, without limiting the scope of the invention:
the sources and purities of the chemical reagents used for sample preparation in the method of the invention are shown in table 1:
table 1 summary of main experimental materials
The types and sources of main experimental instruments for sample preparation in the method are shown in Table 2:
table 2 summary of sample preparation main experimental apparatus
The present invention is further illustrated by the following specific examples, which are not intended to limit the invention, so that those skilled in the art can better understand the invention and can practice it.
Example 1
S1, preparation of nanoparticles: drying the alumina nanoparticles at 75-85 ℃ for 48 hours, adding some alumina nanoparticles into absolute ethyl alcohol (the mass ratio of the alumina nanoparticles to the absolute ethyl alcohol is 1: 20), uniformly mixing, and then sequentially adding a certain amount of oleic acid and absolute ethyl alcohol to finally enable the mass ratio of the oleic acid to the absolute ethyl alcohol in the mixture to be 1: 100, performing ultrasonic dispersion for 30 minutes, after the ultrasonic dispersion, stirring the mixture in a water bath cabinet at 80 ℃ for 4 hours to obtain a centrifugal separation liquid mixture, washing the alumina nanoparticles by using absolute ethyl alcohol (the process is repeated for four times), placing the alumina nanoparticles at 80 ℃ for 48 hours for drying, and then grinding the alumina nanoparticles into powder to obtain nanoparticles (the particle size of the nanoparticles is 130nm, and the scanning electron microscope image of the nanoparticles is shown in figure 8).
S2, preparation of nano modified oil: after the transformer oil and the alumina nanoparticles are respectively dried in a vacuum drying oven at 85-95 ℃ for 48 hours, the transformer oil is added into a beaker containing the nano alumina particles (the weight percent of the alumina nanoparticles is 2 percent), and then ultrasonic dispersion is carried out for 45 minutes to obtain the nano modified oil.
S3, drying the nano modified oil: and (3) drying the nano modified oil prepared by the step S2 in a vacuum drying oven at 90 ℃ for 48 hours to prepare dried nano modified oil for later use.
S4, preparation of a paper sample: the paper board is disassembled, the paper board is thoroughly soaked in deionized water for 24 hours to fully unfold the paper board, then all pulp and water for soaking the pulp are slowly added into a beating machine, and the pulp is obtained after draining. Taking 20g of paper pulp, mixing the paper pulp with deionized water to obtain a sample, putting the sample into a dissociator, adjusting the beating degree to 45 DEG SR, and repeatedly dissociating the sample for 3 times to obtain a paper sample.
S5, surface modification treatment: firstly, 0.08g of alumina nano particles are taken, and then the alumina nano particles and KH550 are mixed according to the mass ratio of 50: 1, adding the mixture into a beaker, adding absolute ethyl alcohol to obtain a mixture, enabling the alumina nanoparticles in the mixture to be 1 wt%, ultrasonically dispersing the mixture in a thermostatic water bath at 90 ℃ until the mixture becomes milky white liquid to obtain nano liquid, mixing the paper sample obtained in S6 with the nano liquid (the mass ratio of the paper sample to the nano liquid is 19: 1), stirring in a magnetic stirrer, and putting in a paper forming machine to obtain the nano modified paper.
S6, sample treatment: sealing the paper sample in a bag for 48 hours, and after the paper sample reaches the water balance, putting the paper sample into a grinding machine to remove the burrs on the surface and increase the density of the paper sample.
S7, preparing nano modified insulating paper: drying the nanometer modified paper in a vacuum drying oven at 90 deg.C for 48h, stopping heating, injecting purified and vacuum degassed nanometer oil (nanometer modified oil prepared by S3), and soaking in the nanometer oil for 48h to obtain nanometer modified insulating paper NOIP (0 #).
The addition of the nano particles produces certain changes to the internal structure of the paper, and scanning electron microscope images of the fresh paper and the nano modified paper are shown in FIG. 7.
Example 2
In this example, NOIP (1#) was produced in the same manner as in example 1 except that 2 wt% of alumina nanoparticles were used in S2 and S7.
Example 3
In this example, NOIP (2#) was produced in the same manner as in example 1 except that 5 wt% of alumina nanoparticles were used in S2 and S7.
Example 4 analysis of breakdown characteristics of Nano-modified insulating paper
In the embodiment, the influence of the mass percentage of the alumina nanoparticles on the breakdown field strength of the nano modified insulating paper in the preparation step of the nano modified oil is examined.
The experiment was divided into three groups, the differences of each group being shown in table 3:
TABLE 3 addition ratio
For the NIOP sample, when the standard lightning pulse voltage is used for testing the breakdown voltage of the sample, the equivalent frequency (about 1MHz) of the standard lightning pulse is selected as the characteristic frequency, the change of the breakdown strength of the sample is observed along with the increase of the mass percentage of the alumina nanoparticles, and the breakdown characteristics of the modified insulating paper under different mass percentages of the nanoparticles are shown in FIG. 2.
NOIP (0#) sample, with 1 wt% alumina nanoparticles, showed a breakdown positive voltage of 42.5kV and a negative voltage of 60.2 kV.
The NOIP (1#) sample, when the alumina nanoparticles were 2 wt%, showed a breakdown positive voltage of 46.3kV and a negative voltage of 59.5 kV.
The NOIP (2#) sample, when the alumina nanoparticles are 5 wt%, has a breakdown positive voltage of 45.1kV and a negative voltage of 56.3 kV.
In summary, as the mass percentage of the alumina nanoparticles increases, the breakdown positive voltage increases and then decreases, the breakdown positive voltage reaches a peak value when the alumina nanoparticles are 2 wt%, and the breakdown negative voltage decreases as the mass percentage of the alumina nanoparticles increases.
Example 5 analysis of dielectric constant of Nano-modified insulating paper
The Novocontrol Concept 80 broadband dielectric spectrometer is adopted to perform NOIP (0#), NOIP (1#) and NOIP (2#) dielectric property tests, and the nano particles can generate certain influence on the dielectric property thereof, as shown in FIG. 6
The experiment was divided into three groups, the differences of each group being shown in table 4:
NOIP (0#) sample, the relative dielectric constant ε of the nano-modified insulation paper when the alumina nanoparticles are 1 wt% r Was 2.47.
NOIP (1#) sample, when the alumina nano-particles are 2 wt%, the relative dielectric constant epsilon of the nano-modified insulating paper r Is 2.44.
NOIP (2#) sample, when the alumina nano-particles are 5 wt%, the relative dielectric constant epsilon of the nano-modified insulating paper r Is 2.56.
The simplified model of the relative dielectric constant is shown in fig. 5, and in summary, the screened alumina nanoparticles are 1-5 wt% according to the experimental results of (1) - (3), wherein, as shown in fig. 3, the breakdown strength of the modified paper is changed, as shown in fig. 4, the number of pores of the modified paper is changed, as shown in fig. 2, when the alumina nanoparticles are 2 wt%, the relative dielectric constant epsilon of the prepared nano modified insulating paper is r The effect is optimal when the concentration is 2.44.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (7)
1. A preparation method of novel nanometer modified insulating paper is characterized by comprising the following steps: the method comprises the following steps:
s1, preparation of nano modified oil: respectively drying the transformer oil and the alumina nanoparticles in a vacuum drying oven at 85-95 ℃ for 45-55 hours, adding the transformer oil into the particles containing the nano alumina, and performing ultrasonic dispersion to obtain nano modified oil;
wherein: 1-5 wt% of nano alumina particles in the nano modified oil;
s2, drying the nano modified oil: drying the nano modified oil prepared by the S1 in a vacuum drying oven at 85-95 ℃ for 45-55 hours to prepare dried nano modified oil for later use;
s3, preparation of a paper sample: the method comprises the following steps of (1) disassembling a paperboard, completely soaking the paperboard in deionized water for 20-30 hours, putting the paperboard into a beater, draining to obtain paper pulp, mixing the paper pulp with the deionized water to obtain a sample, putting the sample into a dissociator, adjusting the beating degree to 45 DEG SR, and dissociating for 1-3 times to obtain a paper sample;
s4, surface modification treatment: adding the alumina nanoparticles and the KH550 into absolute ethyl alcohol, uniformly mixing to obtain a mixture, ultrasonically dispersing the mixture in a constant-temperature water bath at the temperature of 80-90 ℃ until the mixture becomes milky liquid to obtain nano liquid, mixing the paper sample obtained in S3 with the nano liquid, stirring in a magnetic stirrer, and putting into a paper forming machine to obtain nano modified paper;
wherein: the mass ratio of the alumina nano particles to the KH550 is 50: 0.5 to 5; 1-5 wt% of alumina nanoparticles in the mixture; the mass ratio of the paper sample to the nano liquid is 15-25: 1.
s5, preparing nanometer modified insulating paper: and (3) carrying out vacuum drying on the S4 nano modified paper, injecting the purified and vacuum degassed nano modified oil after drying, and soaking in oil for 40-55 hours to obtain the nano modified insulation paper.
2. The method for preparing the novel nano modified insulating paper according to claim 1, wherein the method comprises the following steps: the content of the nano alumina particles in the nano modified oil in S1 is 1-5 wt%.
3. The method for preparing the novel nano modified insulating paper according to claim 1, wherein the method comprises the following steps: the mass ratio of the alumina nanoparticles to the KH550 in S4 is 50: 0.5 to 1.5.
4. The method for preparing the novel nano modified insulating paper according to claim 1, wherein the method comprises the following steps: the mass ratio of the paper sample to the nano liquid in the S4 is 18-22: 1.
5. a novel nanometer modified insulating paper is characterized in that: the insulating paper is prepared by any one of claims 1-3.
6. The use of the novel nano-modified insulating paper prepared by the preparation method of claim 1 as insulating paper in a transformer.
7. Use according to claim 6, characterized in that the breakdown field strength is a direct current breakdown field strength and/or a power frequency breakdown field strength.
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