CN116396677A - Conjugated polymer coating and preparation method thereof, vacuum insulator and preparation method thereof - Google Patents
Conjugated polymer coating and preparation method thereof, vacuum insulator and preparation method thereof Download PDFInfo
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- CN116396677A CN116396677A CN202310247309.XA CN202310247309A CN116396677A CN 116396677 A CN116396677 A CN 116396677A CN 202310247309 A CN202310247309 A CN 202310247309A CN 116396677 A CN116396677 A CN 116396677A
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- 239000012212 insulator Substances 0.000 title claims abstract description 129
- 239000011248 coating agent Substances 0.000 title claims abstract description 67
- 238000000576 coating method Methods 0.000 title claims abstract description 67
- 229920000547 conjugated polymer Polymers 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 80
- 239000000243 solution Substances 0.000 claims abstract description 68
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- 239000007853 buffer solution Substances 0.000 claims abstract description 42
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229960001149 dopamine hydrochloride Drugs 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- 238000001035 drying Methods 0.000 claims description 24
- 238000004140 cleaning Methods 0.000 claims description 21
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 18
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000003921 oil Substances 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 12
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 12
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000004793 Polystyrene Substances 0.000 claims description 11
- 229920002223 polystyrene Polymers 0.000 claims description 11
- 239000002131 composite material Substances 0.000 claims description 9
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 9
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 6
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 claims 3
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims 3
- 230000000694 effects Effects 0.000 abstract description 3
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 12
- 230000001590 oxidative effect Effects 0.000 description 9
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 9
- 238000011161 development Methods 0.000 description 8
- 239000011810 insulating material Substances 0.000 description 8
- 238000007334 copolymerization reaction Methods 0.000 description 6
- 229960003638 dopamine Drugs 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000012544 monitoring process Methods 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000009825 accumulation Methods 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000000872 buffer Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
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- 239000007800 oxidant agent Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004870 electrical engineering Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920001690 polydopamine Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
- C09D179/02—Polyamines
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/02—Cleaning by the force of jets or sprays
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0666—Polycondensates containing five-membered rings, condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0672—Polycondensates containing five-membered rings, condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B17/00—Insulators or insulating bodies characterised by their form
- H01B17/42—Means for obtaining improved distribution of voltage; Protection against arc discharges
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B19/00—Apparatus or processes specially adapted for manufacturing insulators or insulating bodies
- H01B19/02—Drying; Impregnating
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B19/00—Apparatus or processes specially adapted for manufacturing insulators or insulating bodies
- H01B19/04—Treating the surfaces, e.g. applying coatings
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention relates to a conjugated polymer coating and a preparation method thereof, a vacuum insulator and a preparation method thereof; the method solves the problems that the existing method for improving the surface pressure resistance is limited in application range and poor in pressure resistance improving effect; the preparation method of the conjugated polymer coating comprises the following steps of: preparing a buffer solution with pH value of more than or equal to 8 and less than or equal to 9; step 2, preparing a mixed reaction solution of dopamine-aniline hydrochloride: dissolving 0.1-0.4% of dopamine hydrochloride and 0.01-0.1% of aniline in the mass ratio in the buffer solution in the step 1 to obtain a mixed reaction solution of dopamine hydrochloride and aniline; the step 3 is that the mixed reaction solution of dopamine hydrochloride and aniline is cooled and solidified to obtain the conjugated polymer coating, and the invention also provides the conjugated polymer coating based on the method, a vacuum insulator and a preparation method thereof.
Description
Technical Field
The invention relates to a conjugated polymer coating and a preparation method thereof, and a vacuum insulator and a preparation method thereof.
Background
The insulator vacuum surface flashover refers to a breakdown discharge phenomenon which occurs along the interface between the insulator and the vacuum, the discharge voltage is far lower than the bulk breakdown voltage of the insulator and the vacuum, and the insulator vacuum surface flashover is the weakest zone in a vacuum insulation system. With the current development of pulse power systems toward high voltage and miniaturization, higher withstand voltage requirements are put forth on the withstand voltage level of insulators, and lower vacuum in-plane withstand voltage levels of insulators become bottleneck problems for limiting the development of pulse power systems (see Zhang G, su G, song B, et al pulsed flashover across asolid dielectric in vacuum [ J ]. IEEE Transactions on Dielectrics and Electrical operation.2018, 25 (6): 2321-2339, and Li S, nie Y, min D, et al research Progress on Vacuum Surface Flashover of Solid Dielectrics [ J ]. Transactions of China Electrotechnical society.2017,32 (8): 1-9).
In order to reveal the development mechanism of the vacuum surface flashover, researchers carry out a great deal of experiments and theoretical researches, and at present, it is generally considered that the surface flashover starts from initial electron emission at a cathode three-junction point, secondary electron avalanche is formed on the surface of an insulator through secondary electron multiplication, gas adsorbed on the surface of the insulator is continuously desorbed under the stimulation of the secondary electron avalanche, a low-pressure gas environment is formed on the surface of the insulator, and then the low-pressure gas is broken down to form the vacuum surface flashover; from the development process of flashover, it can be seen that electron emission and multiplication on the surface of the insulator are important factors influencing the surface voltage-withstanding performance of the insulator, and reducing the electron emission intensity of the surface or reducing the secondary electron emission coefficient of the insulating material can effectively prevent the development of flashover and promote the surface voltage-withstanding level of the insulator.
The method for improving the surface withstand voltage mainly comprises the steps of constructing a microstructure on the surface of an insulator and modifying chemical components on the surface of the insulator, wherein the modification of the chemical components on the surface can improve the surface withstand voltage level of the insulator substrate, which is an important way for improving the vacuum surface withstand voltage level of the insulator and is also a difficult problem faced by the current research, because the relation between the chemical components on the surface and the vacuum surface withstand voltage performance of the insulator is basically blank. Researchers have tried to improve the in-plane withstand voltage performance of insulators by means of fluorination, surface ceramic coating preparation (see Shao T, liu F, hai B, et al surface modification of epoxy using an atmospheric pressure dielectric barrier discharge to accelerate surface charge dissipation J IEEE Transactions on diagnostics and Electrical engineering 2017,24 (3): 1557-1565, and T.S.Sudarshan, J.D.Cross and k.d. srivasta va, "Prebreakdown Processes Associated with Surface Flashover of Solid Insulators in Vacuum," IEEE Transactions on Electrical Insulation EI-12 (3), 200-208 (1977)), but most methods have limited applicability and poor withstand voltage improvement.
Disclosure of Invention
The invention aims to solve the problems that the existing along-surface pressure resistance improving method is limited in application range and poor in pressure resistance improving effect, and provides a conjugated polymer coating and a preparation method thereof, a vacuum insulator and a preparation method thereof.
The technical scheme adopted by the invention is as follows:
the preparation method of the conjugated polymer coating is characterized by comprising the following steps of:
step 1: preparing a buffer solution with pH value of more than or equal to 8 and less than or equal to 9;
step 2: preparation of dopamine-aniline hydrochloride mixed reaction solution
Dissolving 0.1-0.4% of dopamine hydrochloride and 0.01-0.1% of aniline in the mass ratio in the buffer solution in the step 1 to obtain a mixed reaction solution of dopamine hydrochloride and aniline;
step 3: and cooling and solidifying the mixed reaction solution of dopamine-aniline hydrochloride to obtain the conjugated polymer coating.
Further, in the step 1, buffer solution with pH value of 8-9 is prepared by 0.1mol/L disodium hydrogen phosphate and 0.1mol/L potassium dihydrogen phosphate solution;
or preparing a buffer solution with pH value of 8-9 by using 0.1mol/L sodium bicarbonate and 0.1mol/L sodium carbonate solution.
The invention also provides a conjugated polymer coating, which is characterized by being prepared by adopting the preparation method of the conjugated polymer coating.
The invention also provides a preparation method of the vacuum insulator, which is characterized by comprising the following steps of:
step 1: preparing a buffer solution with pH value of more than or equal to 8 and less than or equal to 9;
step 2: preparation of dopamine-aniline hydrochloride mixed reaction solution
Dissolving 0.1-0.4% of dopamine hydrochloride and 0.01-0.1% of aniline in the mass ratio in the buffer solution in the step 1 to obtain a mixed reaction solution of dopamine hydrochloride and aniline;
step 3: preparation of vacuum insulator with conjugated polymer coating on surface
And (3) immersing the vacuum insulator into the mixed reaction solution obtained in the step (2), stirring and reacting for 24-36 h in air at room temperature, and cleaning and drying to obtain the universal vacuum insulator with the conjugated polymer coating on the surface.
Further, in step 3, the vacuum insulator is a vacuum insulator after removing surface oil stains and cleaning and drying, wherein the method for removing surface oil stains and cleaning and drying the vacuum insulator comprises the following steps:
ultrasonic cleaning is carried out for 1h through a surfactant or NaOH solution with the concentration of 1mol/L, oil stains on the surface are removed, and then ultrasonic cleaning and drying are carried out through deionized water.
Further, step 3 is specifically that the vacuum insulator after cleaning and drying is immersed into the mixed reaction solution in step 2, stirred and reacted for 24-36 hours at room temperature, washed cleanly by deionized water and dried for 6 hours at 60 ℃; a general vacuum insulator with a conjugated polymer coating on the surface is obtained.
Further, in the step 1, a buffer solution with ph=8 is prepared by 0.1mol/L of disodium hydrogen phosphate and 0.1mol/L of potassium dihydrogen phosphate;
in the step 2, 0.1% of dopamine hydrochloride and 0.01% of aniline in mass ratio are dissolved in the buffer solution in the step 1 to obtain a mixed reaction solution of dopamine hydrochloride and aniline;
in the step 3, an alumina ceramic insulator with the diameter of 30mm, the thickness of 10mm and the purity of 95% is ultrasonically cleaned for 1h by using a NaOH solution with the concentration of 1mol/L, oil stains on the surface are removed, the alumina ceramic insulator is cleaned and dried, the alumina ceramic insulator is immersed into the dopamine-aniline hydrochloride mixed reaction solution obtained in the step 2, stirred and reacted in air at room temperature for 24h, and the vacuum insulator with the conjugated polymer coating on the surface is obtained after cleaning and drying.
Further, in the step 1, a buffer solution with ph=8.5 is prepared by 0.1mol/L sodium bicarbonate and 0.1mol/L sodium carbonate solution;
in the step 2, 0.4% of dopamine hydrochloride and 0.1% of aniline in mass ratio are dissolved in the buffer solution in the step 1 to obtain a mixed reaction solution of dopamine hydrochloride and aniline;
in the step 3, the crosslinked polystyrene insulator with the diameter of 30mm and the thickness of 5mm is ultrasonically cleaned for 1h by using a NaOH solution with the concentration of 1mol/L, oil stains on the surface are removed, the crosslinked polystyrene insulator is cleaned and dried, the crosslinked polystyrene insulator is immersed into the mixed reaction solution of dopamine-aniline hydrochloride obtained in the step 2, stirred and reacted for 36h at room temperature in air, and the vacuum insulator with the conjugated polymer coating on the surface is obtained after cleaning and drying.
Further, in the step 1, a buffer solution with ph=9 is prepared by 0.1mol/L of disodium hydrogen phosphate and 0.1mol/L of potassium dihydrogen phosphate;
in the step 2, 0.2% of dopamine hydrochloride and 0.05% of aniline in mass ratio are dissolved in the buffer solution in the step 1 to obtain a mixed reaction solution of dopamine hydrochloride and aniline;
in the step 3, the crosslinked polystyrene/silicon dioxide composite insulator with the diameter of 30mm, the thickness of 5mm and the doping amount of 2% is ultrasonically cleaned for 1h by using a NaOH solution with the concentration of 1mol/L, oil stains on the surface are removed, the composite insulator is cleaned and dried, the composite insulator is immersed into the dopamine-aniline hydrochloride mixed reaction solution obtained in the step 2, stirred and reacted for 30h at room temperature in air, and the vacuum insulator with the conjugated polymer coating on the surface is obtained after cleaning and drying.
The invention also provides a vacuum insulator, which is characterized in that: the vacuum insulator is prepared by adopting the preparation method of the vacuum insulator.
The beneficial effects of the invention are as follows:
1. according to the invention, the conjugated polymer coating is prepared on the surface of the insulator, so that the secondary electron coefficient of the insulator can be effectively reduced, the charge transmission capacity of the insulator to the charge is enhanced, the charge migration capacity of the insulator is improved, the electric field distortion caused by charge accumulation is inhibited, the electron emission intensity of the surface of the insulator is further reduced, and the surface withstand voltage level of the insulator is improved; the amino group and catechol on the dopamine in the conjugated polymer coating have strong chemical activity, can be prepared on the surfaces of most vacuum insulator materials such as ceramics, polymers, composite materials and the like, and obviously improves the vacuum surface pressure resistance.
2. The conjugated polymer coating is formed by oxidizing and copolymerizing aniline and dopamine in a certain molar ratio in an aqueous solution, and dopamine molecules in the conjugated polymer coating have amino groups with strong reactivity and catechol groups on one hand and can be stably adhered to the surfaces of most insulating materials; on the other hand, the polymer with conjugated structure can be generated by oxidative copolymerization with aniline in the presence of oxygen, so that the conjugated polymer coating can be prepared on the surfaces of most insulators by the method.
3. After the conjugated polymer coating is prepared on the surface of the insulator, the original chemical components on the surface of the insulator are replaced by the conjugated polymer, and the conjugated polymer coating has an electron delocalization (electron sharing) structure, so that bombarded electrons can be buffered, decelerated and absorbed through the shared electrons when bombarded by electrons, and the secondary electron emission coefficient of the surface is reduced, namely, delocalized electrons contained in the conjugated structure in the coating can buffer, decelerate and capture the bombarded electrons in the development process of surface flashover, and the secondary electron emission coefficient of the surface of the insulator is reduced; meanwhile, the delocalized electrons can timely conduct surface charges, and electric field distortion caused by surface charge accumulation is relieved; thereby inhibiting the development process of flashover and improving the voltage withstand level of the surface of the insulator.
4. The purpose of the weakly alkaline buffer solution prepared by the invention is to buffer hydrochloric acid generated by copolymerization reaction, provide stable weakly alkaline environment for oxidative copolymerization of dopamine and aniline, and ensure stable growth of the conjugated coating on the surface of the insulator.
5. In the invention, the insulator is cleaned by adopting a method of 1mol/L NaOH solution ultrasonic cleaning for 1h, and the purpose is to remove oil stains remained in the surface processing process of the insulator, expose the insulator substrate, ensure that the conjugated polymer can grow on the insulator substrate and strengthen the bonding strength of the conjugated polymer coating and the substrate.
6. According to the invention, the preparation of the conjugated polymer coating can be carried out by removing the staining layer on the surface of the insulating material without special treatment, and the preparation method is simple and rapid and has low operation requirement.
7. The conjugated polymer coating is prepared by a liquid phase reaction method, is not limited by the shape and the size of the insulator, and can be prepared on the surfaces of insulators with various complex geometric shapes and various sizes.
Drawings
FIG. 1 is a schematic structural diagram of a molecular structure of a conjugated polymer coating in a general vacuum insulator with a conjugated polymer coating on a surface;
fig. 2 is a flow chart of a method for preparing a universal vacuum insulator with a conjugated polymer coating on the surface.
Detailed Description
The invention will be described in detail below with reference to the drawings and the detailed description.
The invention provides a conjugated polymer coating and a preparation method thereof, a vacuum insulator and a preparation method thereof, and as shown in figure 1, the conjugated polymer coating can be prepared on the surface of most insulating materials such as ceramics, polymers, composite materials and the like, and the vacuum surface pressure resistance of the insulating materials is greatly improved.
The conjugated polymer is formed by oxidizing and copolymerizing aniline and dopamine in a buffer solution according to a certain molar ratio, and dopamine molecules in the conjugated polymer coating have amino groups with strong reactivity and catechol groups on one hand and can be adhered to the surfaces of most insulating materials; on the other hand, the polymer with conjugated structure can be generated by oxidative copolymerization with aniline in the presence of oxygen, so that the conjugated polymer body layer can be prepared on the surface of most insulators by the method; the copolymerized polymer coating has a continuous conjugated electron structure (delocalized electron structure), delocalized electrons are similar to free electrons in metal, on one hand, collision electrons can be buffered, decelerated and captured, the secondary electron emission coefficient of the surface of an insulating material is reduced, on the other hand, the captured electrons can migrate and move in the conjugated structure, electric field distortion and field enhancement caused by charge accumulation are relieved, and the emission intensity of electrons is reduced; under the combined action of the two factors, the flashover development process of the surface of the insulator is strongly inhibited, so that the along-surface voltage-withstanding level of the insulator is greatly improved.
A specific preparation method of the conjugated polymer coating is shown in fig. 2, and comprises the following steps:
step 1: preparation of buffer solution
Preparing 0.1mol/L disodium hydrogen phosphate and potassium dihydrogen phosphate solution or preparing 0.1mol/L sodium bicarbonate and sodium carbonate solution, and regulating the ratio of the two solutions by utilizing a PH meter to perform online monitoring to prepare a weak alkaline buffer solution with the PH value of more than or equal to 8 and less than or equal to 9;
step 2: preparation of dopamine-aniline hydrochloride mixed reaction solution
Weighing dopamine hydrochloride according to the mass ratio of 0.1-0.4%, adding aniline according to the mass ratio of 0.01-0.1%, stirring and dissolving the mixture in the weakly alkaline buffer solution in the step 1 to obtain a mixed reaction solution of dopamine hydrochloride and aniline, and carrying out oxidative copolymerization on the dopamine hydrochloride and the aniline in the weakly alkaline buffer solution (pH is more than or equal to 8 and less than or equal to 9) in air in a stirring state to prepare a conjugated polymer coating, wherein an oxidant is derived from oxygen in the air, and a conjugated electron group in the conjugated polymer coating is a decisive factor for improving the surface withstand voltage of an insulator;
step 3: and cooling and solidifying the mixed reaction solution of dopamine-aniline hydrochloride to obtain the conjugated polymer coating.
The invention also provides a conjugated polymer coating prepared based on the method.
The invention also provides a preparation method of the vacuum insulator based on the method, which comprises the following steps:
step 1: preparation of buffer solution
Preparing 0.1mol/L disodium hydrogen phosphate and potassium dihydrogen phosphate solution or preparing 0.1mol/L sodium bicarbonate and sodium carbonate solution, and regulating the ratio of the two solutions by utilizing a PH meter to perform online monitoring to prepare a weak alkaline buffer solution with the PH value of more than or equal to 8 and less than or equal to 9;
step 2: preparation of dopamine-aniline hydrochloride mixed reaction solution
Weighing dopamine hydrochloride according to the mass ratio of 0.1-0.4%, adding aniline according to the mass ratio of 0.01-0.1%, stirring and dissolving the mixture in the weakly alkaline buffer solution in the step 1 to obtain a mixed reaction solution of dopamine hydrochloride and aniline, and carrying out oxidative copolymerization on the dopamine hydrochloride and the aniline in the weakly alkaline buffer solution (pH is more than or equal to 8 and less than or equal to 9) in air in a stirring state to prepare a conjugated polymer coating, wherein an oxidant is derived from oxygen in the air, and a conjugated electron group in the conjugated polymer coating is a decisive factor for improving the surface withstand voltage of an insulator;
step 3: preparation of vacuum insulator with conjugated polymer coating on surface
3.1, ultrasonically cleaning the processed and formed insulator for 1h by using a surfactant or a NaOH solution with the concentration of 1mol/L, removing greasy dirt on the surface, ultrasonically cleaning for three times by using deionized water, and drying;
3.2, immersing the cleaned and dried sample into the mixed reaction solution of dopamine-aniline hydrochloride, stirring at room temperature for reaction for 24-36 h, then washing with deionized water, and drying at 60 ℃ for 6h to finally prepare the vacuum insulator with the conjugated polymer coating on the surface, wherein the conjugated polymer coating comprehensively utilizes the adhesiveness of polydopamine and the high-concentration delocalized electronic structure of polyaniline, and can be prepared on the surface of any insulating material to form the delocalized electronic structure (the aim of preparing delocalized electronic groups on the surface of the vacuum insulator is fulfilled);
based on the preparation method of the vacuum insulator, the invention also provides the vacuum insulator prepared by the method.
In order to verify the performance of the vacuum insulator having the conjugated polymer coating layer on the surface prepared by the above method, the present invention provides the following examples:
example 1
Firstly, preparing a weak alkaline buffer solution with pH=8 by utilizing 0.1mol/L disodium hydrogen phosphate and potassium dihydrogen phosphate solution, and regulating the ratio of the disodium hydrogen phosphate to the potassium dihydrogen phosphate solution through online monitoring of a PH meter; weighing dopamine hydrochloride according to the mass ratio of 0.1%, adding aniline according to the mass ratio of 0.01%, and stirring and dissolving in the buffer solution; then ultrasonically cleaning an alumina ceramic insulator with the diameter of 30mm, the thickness of 10mm and the purity of 95% for 1h by using a NaOH solution with the concentration of 1mol/L to remove greasy dirt on the surface, and then cleaning for three times by using deionized water and drying; finally, immersing the cleaned and dried alumina ceramic insulator into the mixed reaction solution of dopamine hydrochloride and aniline, stirring at room temperature for reaction for 24 hours, then washing with deionized water, and drying at 60 ℃ for 6 hours; finally, the vacuum insulator with the conjugated polymer coating on the surface is prepared and is named as 'coating insulator 1'.
Example 2
Firstly, preparing a weak alkaline buffer solution with pH=8.5 by utilizing 0.1mol/L sodium bicarbonate and 0.1mol/L sodium carbonate solution, and regulating the ratio of the sodium bicarbonate to the sodium bicarbonate through online monitoring of a PH meter; weighing dopamine hydrochloride according to the mass ratio of 0.4%, adding aniline according to the mass ratio of 0.1%, and stirring to dissolve in the buffer solution; then ultrasonically cleaning a crosslinked polystyrene insulator with the diameter of 30mm and the thickness of 5mm for 1h by using a NaOH solution with the concentration of 1mol/L to remove greasy dirt on the surface, and then cleaning for three times by using deionized water and drying; finally, immersing the washed and dried crosslinked polystyrene insulator into the mixed reaction solution of dopamine hydrochloride and aniline, stirring at room temperature for reaction for 36 hours, then washing with deionized water, and drying at 60 ℃ for 6 hours; finally, the vacuum insulator with the conjugated polymer coating on the surface is prepared and is named as 'coating insulator 2'.
Example 3
Firstly, preparing a weak alkaline buffer solution with PH=9 by utilizing 0.1mol/L disodium hydrogen phosphate and potassium dihydrogen phosphate solution, and regulating the proportion of the disodium hydrogen phosphate and the potassium dihydrogen phosphate solution through online monitoring of a PH meter; weighing dopamine hydrochloride according to the mass ratio of 0.2%, adding aniline according to the mass ratio of 0.05%, and stirring and dissolving in the buffer solution; then ultrasonically cleaning a crosslinked polystyrene/silicon dioxide composite insulator with the diameter of 30mm, the thickness of 5mm and the doping amount of 2% for 1h by using a NaOH solution with the concentration of 1mol/L to remove greasy dirt on the surface, and then cleaning for three times by using deionized water and drying; finally, immersing the cleaned and dried sample into the mixed reaction solution of the dopamine hydrochloride and the aniline, stirring and reacting for 30 hours at room temperature, then washing the sample cleanly by using deionized water, and drying the sample at 60 ℃ for 6 hours; finally, the vacuum insulator with the conjugated polymer coating on the surface is prepared and is named as 'coating insulator 3'.
The conjugated polymer coated insulator prepared in the above example and the insulator of the corresponding material were subjected to a vacuum flashover voltage test on a pulse vacuum rim flashover characteristic test bench having a pulse width of 500nm as they are. The flashover voltage test results are shown in table 1:
table 1 test table for flashover voltage of insulators before and after preparation of conjugated polymer coating
The vacuum flashover voltage of the vacuum insulator with the conjugated polymer coating on the surface is improved by 40-150% compared with the vacuum flashover voltage of the corresponding insulator in the original state, which indicates that the preparation of the conjugated polymer coating can improve the vacuum surface flashover voltage of various insulators.
Claims (10)
1. A method for preparing a conjugated polymer coating, comprising the steps of:
step 1: preparing a buffer solution with pH value of more than or equal to 8 and less than or equal to 9;
step 2: preparation of dopamine-aniline hydrochloride mixed reaction solution
Dissolving 0.1-0.4% of dopamine hydrochloride and 0.01-0.1% of aniline in the mass ratio in the buffer solution in the step 1 to obtain a mixed reaction solution of dopamine hydrochloride and aniline;
step 3: and cooling and solidifying the mixed reaction solution of dopamine-aniline hydrochloride to obtain the conjugated polymer coating.
2. The method of preparing a conjugated polymer coating according to claim 1, characterized in that:
in the step 1, buffer solution with pH value of more than or equal to 8 and less than or equal to 9 is prepared by 0.1mol/L of disodium hydrogen phosphate and 0.1mol/L of monopotassium phosphate solution;
or preparing a buffer solution with pH value of 8-9 by 0.1mol/L sodium bicarbonate and 0.1mol/L sodium carbonate solution.
3. A conjugated polymer coating, characterized in that it is prepared by the method for preparing a conjugated polymer coating according to any one of claims 1-2.
4. The preparation method of the vacuum insulator is characterized by comprising the following steps of:
step 1: preparing a buffer solution with pH value of more than or equal to 8 and less than or equal to 9;
step 2: preparation of dopamine-aniline hydrochloride mixed reaction solution
Dissolving 0.1-0.4% of dopamine hydrochloride and 0.01-0.1% of aniline in the mass ratio in the buffer solution in the step 1 to obtain a mixed reaction solution of dopamine hydrochloride and aniline;
step 3: preparation of vacuum insulator with conjugated polymer coating on surface
And (3) immersing the vacuum insulator into the mixed reaction solution obtained in the step (2), stirring and reacting for 24-36 h in air at room temperature, and cleaning and drying to obtain the universal vacuum insulator with the conjugated polymer coating on the surface.
5. The method for manufacturing a surface vacuum insulator according to claim 4, wherein:
in step 3, the vacuum insulator is a vacuum insulator after removing surface oil stains and cleaning and drying, wherein the method for removing the surface oil stains and cleaning and drying the vacuum insulator comprises the following steps:
ultrasonic cleaning is carried out for 1h through a surfactant or a NaOH solution with the concentration of 1mol/L, oil stains on the surface are removed, and then ultrasonic cleaning and drying are carried out through deionized water.
6. The method for manufacturing a vacuum insulator according to claim 5, wherein:
step 3, immersing the cleaned and dried vacuum insulator into the mixed reaction solution in the step 2, stirring at room temperature for reaction for 24-36 h, washing with deionized water, and drying at 60 ℃ for 6h; a general vacuum insulator with a conjugated polymer coating on the surface is obtained.
7. The method for manufacturing a vacuum insulator according to claim 6, wherein:
in the step 1, a buffer solution with PH=8 is prepared by 0.1mol/L of disodium hydrogen phosphate and 0.1mol/L of monopotassium phosphate;
in the step 2, 0.1% of dopamine hydrochloride and 0.01% of aniline in mass ratio are dissolved in the buffer solution in the step 1 to obtain a mixed reaction solution of dopamine hydrochloride and aniline;
in the step 3, an alumina ceramic insulator with the diameter of 30mm, the thickness of 10mm and the purity of 95% is ultrasonically cleaned for 1h by using a NaOH solution with the concentration of 1mol/L, oil stains on the surface are removed, the alumina ceramic insulator is cleaned and dried, the alumina ceramic insulator is immersed into the mixed reaction solution of dopamine-aniline hydrochloride obtained in the step 2, stirred and reacted for 24h in air at room temperature, and the vacuum insulator with the conjugated polymer coating on the surface is obtained after cleaning and drying.
8. The method for manufacturing a vacuum insulator according to claim 6, wherein:
in the step 1, a buffer solution with PH=8.5 is prepared by 0.1mol/L sodium bicarbonate and 0.1mol/L sodium carbonate solution;
in the step 2, 0.4% of dopamine hydrochloride and 0.1% of aniline in mass ratio are dissolved in the buffer solution in the step 1 to obtain a mixed reaction solution of dopamine hydrochloride and aniline;
in the step 3, the crosslinked polystyrene insulator with the diameter of 30mm and the thickness of 5mm is ultrasonically cleaned for 1h by using a NaOH solution with the concentration of 1mol/L, oil stains on the surface are removed, the crosslinked polystyrene insulator is cleaned and dried, the crosslinked polystyrene insulator is immersed into the mixed reaction solution of dopamine-aniline hydrochloride obtained in the step 2, stirred and reacted for 36h at room temperature in air, and the vacuum insulator with the conjugated polymer coating on the surface is obtained after cleaning and drying.
9. The method for manufacturing a vacuum insulator according to claim 6, wherein:
in the step 1, a buffer solution with PH=9 is prepared by 0.1mol/L of disodium hydrogen phosphate and 0.1mol/L of monopotassium phosphate;
in the step 2, 0.2% of dopamine hydrochloride and 0.05% of aniline in mass ratio are dissolved in the buffer solution in the step 1 to obtain a mixed reaction solution of dopamine hydrochloride and aniline;
in the step 3, the crosslinked polystyrene/silicon dioxide composite insulator with the diameter of 30mm, the thickness of 5mm and the doping amount of 2% is ultrasonically cleaned for 1h by using a NaOH solution with the concentration of 1mol/L, oil stains on the surface are removed, the composite insulator is cleaned and dried, the composite insulator is immersed into the dopamine-aniline hydrochloride mixed reaction solution obtained in the step 2, stirred and reacted in air at room temperature for 30h, and the vacuum insulator with the conjugated polymer coating on the surface is obtained after cleaning and drying.
10. A vacuum insulator, characterized in that: a method for manufacturing a vacuum insulator according to any one of claims 4 to 9.
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| CN114855444A (en) * | 2022-04-18 | 2022-08-05 | 南京工业大学 | Surface coating modification method for ultra-high molecular weight polyethylene fiber |
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| CN114855444A (en) * | 2022-04-18 | 2022-08-05 | 南京工业大学 | Surface coating modification method for ultra-high molecular weight polyethylene fiber |
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