CN117736491A - Preparation method of starch/polyorganosiloxane biological composite super-electric insulation material with three-dimensional nano-pore structure - Google Patents
Preparation method of starch/polyorganosiloxane biological composite super-electric insulation material with three-dimensional nano-pore structure Download PDFInfo
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- CN117736491A CN117736491A CN202311594445.2A CN202311594445A CN117736491A CN 117736491 A CN117736491 A CN 117736491A CN 202311594445 A CN202311594445 A CN 202311594445A CN 117736491 A CN117736491 A CN 117736491A
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- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 229920002472 Starch Polymers 0.000 title claims abstract description 36
- 235000019698 starch Nutrition 0.000 title claims abstract description 36
- 239000008107 starch Substances 0.000 title claims abstract description 36
- 239000011148 porous material Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000012774 insulation material Substances 0.000 title claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 239000011810 insulating material Substances 0.000 claims abstract description 17
- 239000000725 suspension Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920002261 Corn starch Polymers 0.000 claims abstract description 7
- 239000008120 corn starch Substances 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000000499 gel Substances 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 10
- 239000011240 wet gel Substances 0.000 claims description 7
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 230000007062 hydrolysis Effects 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 3
- 239000003755 preservative agent Substances 0.000 claims description 2
- 230000002335 preservative effect Effects 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 4
- 230000001276 controlling effect Effects 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 description 19
- 239000002114 nanocomposite Substances 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000003989 dielectric material Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 238000002411 thermogravimetry Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000003878 thermal aging Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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- Organic Insulating Materials (AREA)
Abstract
The invention discloses a preparation method of a starch/polyorganosiloxane biological composite super-electric insulating material with a three-dimensional nano-pore structure, which comprises the following steps: s1, preparing starch suspension: mixing corn starch and deionized water, heating in water bath, stirring to obtain suspension starch liquid, and cooling to room temperature for standby; s2, preparing composite gel, and regulating and controlling the pH value by adding acetic acid; s3, preparing the starch/polyorganosiloxane biological composite super-electric insulating material S/PBID. The S/PBID prepared by the invention has good hydrophobicity and excellent performanceDielectric properties, excellent insulating properties, N 2 Also shows better insulating property under gas.
Description
Technical Field
The invention relates to the field of insulating materials, in particular to a preparation method of a starch/polyorganosiloxane biological composite super-electric insulating material with a three-dimensional nano-pore structure.
Background
Insulating materials are important components of electric equipment and electronic devices, and are widely applied to various industries and fields such as electric power, aerospace, rail transit and the like. The high breakdown field strength and the low dielectric loss are used as important indexes for evaluating the performance quality of the insulating material, and have important significance for miniaturization and safe operation of electric power equipment.
At present, the nano composite technology is widely considered as an effective means for improving various performances of an insulating material such as electricity, heat, mechanics and the like, and along with continuous optimization and development of the nano technology, nano dielectric is expected to become a third-generation high-performance insulating material with great application prospect, but a plurality of defects still exist at present. Firstly, the nano particles have the characteristics of large specific surface area and strong surface activity, and are easy to combine with other atoms to cause the phenomena of particle adsorption, agglomeration and the like. This will lead to difficulty in uniformly dispersing the nanofiller during the preparation of the nanoelectrolytes, inability to exert the full potential of the nanoelectrolytes, nanoparticle agglomerates may lead to reduced breakdown strength, reduced mechanical properties, etc. Secondly, the nanocomposite is an aggregate formed by mixing and fusing multiphase media, a large number of interfaces are necessarily introduced, interface polarization occurs in the formed interface area, the overall dielectric performance of the composite is easy to be reduced, particularly dielectric loss is easy to be increased, the composite is unacceptable in electric equipment, particularly in power frequency operation, and long-term operation can lead to temperature rise of the media, so that a series of problems such as insulation thermal aging and the like are caused. In addition, the nanocomposite technology mainly aims at solid and liquid dielectrics, and although the method can improve the dielectric breakdown strength to a certain extent, the macroscopic performance improvement of the nanocomposite technology only depends on the physicochemical properties and interface effects of nanoparticles, and the huge potential of the dielectrics is not exerted, so that the nanocomposite technology has a certain limit (usually not more than 30%) on the improvement of the electrical performance of materials. These problems seriously hamper the industrial application of nanocomposite dielectrics, and therefore we need to find new solutions to meet the development needs of electrical devices.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention prepares the novel starch/polyorganosiloxane biological composite insulating dielectric medium with a three-dimensional nano porous structure, namely S/PBID for short by utilizing natural and renewable corn starch and combining high-stability and heat-resistant methyltrimethoxysilane through a sol-gel method.
The technical scheme is as follows:
a preparation method of a starch/polyorganosiloxane biological composite super-electric insulation material with a three-dimensional nano-pore structure comprises the following steps:
s1, preparing starch suspension: mixing corn starch and deionized water, heating in water bath, stirring to obtain suspension starch liquid, and cooling to room temperature for standby;
s2, preparing composite gel:
s2-1, adding urea and F127 into the suspension starch solution to obtain a mixture;
s2-2, adding acetic acid into the mixture prepared in the step S2-1 to regulate the pH value;
s2-3, stirring the mixture prepared by the S2-2 at room temperature;
s2-4, adding methyltrimethoxysilane MTMS into the mixture prepared in the S2-2, and continuously stirring at room temperature to fully promote the hydrolysis; obtaining composite gel for standby;
s3, preparing a starch/polyorganosiloxane biological composite super-electric insulation material:
s3-1, ageing the composite gel at 60 ℃ and 80 ℃ in sequence;
s3-2, sequentially carrying out solvent exchange on the aged composite gel with ethanol and n-hexane for a plurality of times to obtain wet gel;
s3-3, drying the wet gel in a vacuum drying oven to obtain the starch/polyorganosiloxane biological composite super-electric insulation material.
In the preferred embodiment, in S1, the mass part ratio of the corn starch to the deionized water is 9:40.
in a preferred embodiment, in S1, the water bath heating temperature is 95 ℃, the stirring speed is 700rpm, and the stirring time is 1 hour.
In the preferred embodiment, in S2-1, the mass parts of the suspension starch liquid, urea and F127 are as follows: 40:8:3.
Specifically, in S2-2, the pH value is regulated and controlled by adding different amounts of acetic acid so as to obtain different pore diameters.
Specifically, in S2-2,
the mass ratio of the mixture to acetic acid is 255:4, obtaining the aperture of the starch/polyorganosiloxane biological composite super-electric insulating material is 44.72nm;
the mass portion of the mixture and acetic acid is 255:8, obtaining the aperture of the starch/polyorganosiloxane biological composite super-electric insulation material is 66.56nm;
the mass portion of the mixture and acetic acid is 85:4, obtaining the aperture of the starch/polyorganosiloxane biological composite super-electric insulating material is 106.54nm; the method comprises the steps of carrying out a first treatment on the surface of the
Wherein the concentration of acetic acid is 0.5mol L -1 。
In a preferred embodiment, the stirring speed is 400rpm in S2-2 and S2-3, the stirring time in S2-2 is 30min, and the stirring time in S2-3 is 10min.
In a preferred embodiment, in S3-1, the aging treatment is: adding absolute ethyl alcohol to the shaped composite gel to impregnate the gel, sealing the gel by using a preservative film to prevent the absolute ethyl alcohol from volatilizing, and placing a mold filled with the gel in a vacuum drying oven to dry for 12 hours.
In a preferred embodiment, in S3-2, the exchange of the solution of the complex gel with ethanol, complex gel and n-hexane is performed 3 times, each for 12 hours.
In a preferred embodiment, the wet gel is dried in a vacuum oven at 60 ℃ and at atmospheric pressure.
In a preferred embodiment, the room temperature mentioned herein is 25 ℃.
The beneficial effects of the invention are that
Compared with a nano-composite technology, the novel starch/polyorganosiloxane biological composite super-electric insulating material S/PBID has the advantages of excellent insulating property, environmental protection and renewable characteristics, and provides new possibility for future insulating material research and application.
The nanoporous structure inside the S/PBID effectively suppresses the electron avalanche process, which typically results in gas discharge, thus reducing the insulation of the material. However, due to the nano-porous structure of the S/PBID, the process is effectively inhibited, so that the breakdown field intensity of the material is obviously improved, and excellent insulating performance is shown. In addition, S/PBID is excellent in dielectric properties, has a relative dielectric constant of 1.72, which is only 38.4% of EP, making it one of the currently known insulating materials having the lowest relative dielectric constant. In addition, the S/PBID has the advantages of light weight, reproducibility, environmental protection, carbon fixation and the like, and the characteristics make the S/PBID an ideal insulating material.
Drawings
FIG. 1 is a microscopic topography of S/PBID ((a) S/PBID1, (b) S/PBID2, (c) S/PBID 3)
FIG. 2 is a schematic illustration of thermogravimetric analysis of S/PBID
FIG. 3 is a schematic view of the water contact angle of S/PBID
FIG. 4 is SF 6 AC breakdown field strength diagram of S/PBID under atmospheric pressure ((a) 0.1MPa, (b) 0.2MPa, (c) 0.3 MPa)
FIG. 5 is SF 6 Graph of alternating breakdown field strength of S/PBID in atmosphere versus gas pressure
FIG. 6 is N 2 AC breakdown field strength diagram of S/PBID under atmospheric pressure ((a) 0.1MPa, (b) 0.2MPa, (c) 0.3 MPa)
FIG. 7 is N 2 Schematic diagram of relation between alternating breakdown field strength of S/PBID and gas pressure in atmosphere
FIG. 8 is a schematic diagram of the relative dielectric constants of S/PBID and EP
Detailed Description
The invention is further illustrated below with reference to examples, but the scope of the invention is not limited thereto:
in this embodiment, the preparation method includes the following steps:
s1, preparing starch suspension: corn starch and deionized water were first mixed in a specific ratio to prepare a suspension (2.25 mg L -1 ) Heating in a water bath at 95 ℃ and stirring at 700rpm for 1 hour to obtain starch suspension, and cooling to room temperature for standby;
s2, preparing composite gel: to the starch suspension was added 2g of urea and 0.75g of polyoxyethylene polyoxypropylene ether (F127) to prepare a precursor solution, and various amounts of acetic acid (0.5 mol L) -1 Regulating pH to be acidic by 0.2, 0.4 and 0.6mL, and regulating the size of the medium nano pore diameter of the S/PBID (the prepared samples are respectively called S/PBID1-S/PBID 3); then magnetically stirring the obtained mixture at 400rpm for 30min, finally adding methyltrimethoxysilane (MTMS) into the mixed solution, and continuously stirring at room temperature for 10min to fully promote hydrolysis to obtain composite gel for later use;
s3, preparing a starch/polyorganosiloxane biological composite super-electric insulation material: firstly, ageing the composite gel at 60 ℃ and 80 ℃ respectively, and carrying out solvent exchange on the aged gel with ethanol and n-hexane for 3 times (12 h each time) respectively; and then drying the obtained wet gel in a vacuum drying oven at 60 ℃ and normal pressure to finally obtain the starch/polyorganosiloxane biological composite super-electric insulation material (S/PBID).
The main experimental raw materials are shown in table 1:
TABLE 1 list of main experimental raw materials
The preparation method of the starch/polyorganosiloxane biological composite super-electric insulation material with the three-dimensional nano-pore structure, which is developed by the invention, can adjust the pH value of a solution through acetic acid, further adjust the speed of hydrolysis condensation reaction, obtain S/PBID samples with different average pore sizes, and the SEM images of the S/PBID samples with different average pore sizes are shown in figure 1 (in the figure, a, b and c respectively correspond to the pore sizes of 44.72nm, 66.56nm and 106.54nm and are respectively marked as S/PBID1, S/PBID2 and S/PBID 3).
The S/PBID prepared by the invention has good thermal stability, and the thermal stability of the S/PBID is tested by adopting thermogravimetric analysis (TGA), and the result is shown as figure 2, wherein the S/PBID has two obvious weightlessness peaks at about 310 ℃ and 500 ℃ and respectively corresponds to starch and CH 3 The loss of the group, the curve becomes substantially flat as the temperature is further increased to 700 ℃, and it is shown from the above-mentioned study that S/PBID has good thermal stability.
The S/PBID prepared by the invention has good hydrophobicity, and as shown in figure 3, the water contact angle of the S/PBID is 132.2 degrees, has higher hydrophobicity and shows good self-cleaning performance. The excellent hydrophobic properties of S/PBID are attributed to the incorporation of a large number of hydrophobic methyl groups during the preparation process, which not only facilitates the composite dielectric to maintain the integrity of the frame structure during drying, but also reduces moisture content and dielectric loss.
The S/PBID prepared by the invention has excellent insulating property, the S/PBID is placed in a tank body sealed with insulating gas, an alternating current voltage test platform is used for researching the insulating property of the S/PBID, and a Weibull distribution diagram of the alternating current breakdown field intensity and a relation curve of air pressure and the alternating current breakdown field intensity of the S/PBID are provided. FIG. 4 is SF 6 The Weibull distribution diagram of the AC breakdown field strength of S/PBID under gas increases as the average pore diameter of S/PBID decreases. FIG. 5 shows the relationship between the AC breakdown field strength of S/PBID and the gas pressure at different SF 6 Under the air pressure, for the optimal S/PBID1 of the hole structure characteristics, the alternating current breakdown field strengths of the S/PBID1 are 28.89kV mm respectively -1 ，38.25kV mm -1 ，44.89kV mm -1 Relative to pure SF 6 The air gap has lifting amplitude of 310.95%,273.9% and 183.93% respectively, and shows excellent insulating performance.
In addition, the S/PBID prepared by the invention is N 2 Also shows better insulating property under gas. As shown in figure 6 of the drawings,from N 2 As can be seen from Weibull distribution graph of S/PBID AC breakdown field strength under atmosphere, under 0.3MPa, the breakdown field strength of S/PBID1 can reach 32kV mm -1 . FIG. 7 is a graph of the relationship between AC breakdown field strength and gas pressure for S/PBID, showing increasing trend of AC breakdown field strength and gas pressure for three groups of samples with different pore structures. Specifically, at 0.1MPa N 2 Under the condition that the AC breakdown field strength of S/PBID1 is 20.05kV mm -1 With pure N 2 Compared with the air gap, the lifting amplitude of the air gap can reach 520.74%; respectively reach 24.62kV mm under the gas pressure of 0.2MPa and 0.3MPa -1 ，32kV mm -1 。
The S/PBID prepared by the invention has excellent dielectric property, and the dielectric property of a sample is characterized by a broadband dielectric spectrometer, as shown in figure 8, the relative dielectric constants of S/PBID1, S/PBID2 and S/PBID3 at 50Hz characteristic points are respectively 1.96, 1.85 and 1.72, which are far lower than the relative dielectric constant (4.48) of epoxy resin which is a common insulating material, so that the excellent electric insulating property of the material is ensured, and the breakdown field intensity of a composite insulating system is improved.
The specific embodiments described herein are offered by way of example only to illustrate the spirit of the invention. Those skilled in the art may make various modifications or additions to the described embodiments or substitutions thereof without departing from the spirit of the invention or exceeding the scope of the invention as defined in the accompanying claims.
Claims (10)
1. The preparation method of the starch/polyorganosiloxane biological composite super-electric insulation material with the three-dimensional nano-pore structure is characterized by comprising the following steps:
s1, preparing starch suspension: mixing corn starch and deionized water, heating in water bath, stirring to obtain suspension starch liquid, and cooling to room temperature for standby;
s2, preparing composite gel:
s2-1, adding urea and F127 into the suspension starch solution to obtain a mixture;
s2-2, adding acetic acid into the mixture prepared in the step S2-1 to regulate the pH value;
s2-3, stirring the mixture prepared by the S2-2 at room temperature;
s2-4, adding methyltrimethoxysilane MTMS into the mixture prepared in the S2-2, and continuously stirring at room temperature to fully promote the hydrolysis; obtaining composite gel for standby;
s3, preparing a starch/polyorganosiloxane biological composite super-electric insulation material:
s3-1, ageing the composite gel at 60 ℃ and 80 ℃ in sequence;
s3-2, sequentially carrying out solvent exchange on the aged composite gel with ethanol and n-hexane for a plurality of times to obtain wet gel;
s3-3, drying the wet gel in a vacuum drying oven to obtain the starch/polyorganosiloxane biological composite super-electric insulation material.
2. The method according to claim 1, wherein in S1, the mass part ratio of the corn starch to the deionized water is 9:40.
3. the method according to claim 1, wherein in S1, the water bath heating temperature is 95 ℃, the stirring speed is 700rpm, and the stirring time is 1 hour.
4. The method according to claim 1, wherein in S2-1, the mass parts of the suspension starch solution, urea and F127 are: 40:8:3.
5. The method according to claim 1, wherein in S2-2, the pH is adjusted by adding different amounts of acetic acid to obtain different pore sizes.
6. The method according to claim 5, wherein in S2-2:
the mass ratio of the mixture to acetic acid is 255:4, obtaining the aperture of the starch/polyorganosiloxane biological composite super-electric insulating material is 44.72nm;
the mass portion of the mixture and acetic acid is 255:8, obtaining the aperture of the starch/polyorganosiloxane biological composite super-electric insulation material is 66.56nm;
the mass portion of the mixture and acetic acid is 85:4, obtaining the aperture of the starch/polyorganosiloxane biological composite super-electric insulating material is 106.54nm;
wherein the concentration of acetic acid is 0.5mol L -1 。
7. The method according to claim 1, wherein the stirring speed in S2-2 and S2-3 is 400rpm, the stirring time in S2-2 is 30min, and the stirring time in S2-3 is 10min.
8. The method according to claim 1, wherein in S3-1, the aging treatment means: adding absolute ethyl alcohol to the shaped composite gel to impregnate the gel, sealing the gel by using a preservative film to prevent the absolute ethyl alcohol from volatilizing, and placing a mold filled with the gel in a vacuum drying oven to dry for 12 hours.
9. The method according to claim 1, wherein in S3-2, the solution exchange of the complex gel with ethanol, complex gel and n-hexane is performed 3 times for 12 hours each.
10. The method according to claim 1, wherein in S3-3, the wet gel is dried in a vacuum oven at 60 ℃ under normal pressure.
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| CN202311594445.2A CN117736491A (en) | 2023-11-28 | 2023-11-28 | Preparation method of starch/polyorganosiloxane biological composite super-electric insulation material with three-dimensional nano-pore structure |
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