CN115820204A - Adhesive and preparation method and application thereof - Google Patents
Adhesive and preparation method and application thereof Download PDFInfo
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- CN115820204A CN115820204A CN202211530709.3A CN202211530709A CN115820204A CN 115820204 A CN115820204 A CN 115820204A CN 202211530709 A CN202211530709 A CN 202211530709A CN 115820204 A CN115820204 A CN 115820204A
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- 239000000853 adhesive Substances 0.000 title claims abstract description 49
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 57
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000011259 mixed solution Substances 0.000 claims abstract description 34
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 239000007822 coupling agent Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000012212 insulator Substances 0.000 claims abstract description 13
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002131 composite material Substances 0.000 claims abstract description 12
- 229910000077 silane Inorganic materials 0.000 claims abstract description 12
- 239000002244 precipitate Substances 0.000 claims abstract description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 238000000576 coating method Methods 0.000 claims description 32
- 239000011248 coating agent Substances 0.000 claims description 25
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 12
- 229960000583 acetic acid Drugs 0.000 claims description 11
- 239000012362 glacial acetic acid Substances 0.000 claims description 11
- 229920002379 silicone rubber Polymers 0.000 claims description 11
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 claims description 8
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 6
- 239000003431 cross linking reagent Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 4
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 4
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 4
- -1 polydimethylsiloxane Polymers 0.000 claims description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 4
- 229920002554 vinyl polymer Polymers 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000004945 silicone rubber Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 230000007797 corrosion Effects 0.000 abstract description 6
- 238000005260 corrosion Methods 0.000 abstract description 6
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 10
- 230000032683 aging Effects 0.000 description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 230000004888 barrier function Effects 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 239000011521 glass Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 4
- 239000004593 Epoxy Substances 0.000 description 3
- 239000006087 Silane Coupling Agent Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical group C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000007306 functionalization reaction Methods 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000004528 spin coating Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- CLWRFNUKIFTVHQ-UHFFFAOYSA-N [N].C1=CC=NC=C1 Chemical group [N].C1=CC=NC=C1 CLWRFNUKIFTVHQ-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000000627 alternating current impedance spectroscopy Methods 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
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- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010073 coating (rubber) Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000001453 impedance spectrum Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
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- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229920002631 room-temperature vulcanizate silicone Polymers 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention belongs to the technical field of electric power, and particularly relates to an adhesive and a preparation method and application thereof. The preparation method of the adhesive comprises the following steps: s1, functionalized g-C 3 N 4 The preparation of (1): preparing silane solution, adding ethanol and water to obtain mixed solution, and adding g-C 3 N 4 The pH value of the solution is adjusted for the first time, and thenStanding, regulating pH value of the solution for the second time, heating, keeping the temperature, filtering to obtain lower-layer precipitate, washing, and drying to obtain functionalized g-C 3 N 4 (ii) a S2, preparing an adhesive: preparing an ethanol aqueous solution, adjusting the pH value of the solution, and adding the functionalized g-C prepared in the step S1 3 N 4 Stirring and carrying out ultrasonic treatment to obtain a mixed solution, adding a coupling agent, stirring and reacting to obtain the adhesive. The adhesive prepared by the invention has excellent corona resistance and NO resistance 2 The gas corrosion and water resistance can effectively prolong the service life of the composite insulator.
Description
Technical Field
The invention belongs to the technical field of electric power, and particularly relates to an adhesive and a preparation method and application thereof.
Background
The composite insulator has the advantages of excellent hydrophobicity, light weight, high strength and the like, and is increasingly emphasized in high-voltage transmission lines, particularly in heavily polluted areas, and the number of the composite insulators in service is increased year by year. The composite insulator is composed of a high-temperature vulcanized silicone rubber HTV shed sheath, an epoxy glass fiber core rod and an end hardware fitting, and the shed sheath and the core rod are required to be combined together through an interface adhesive, so that the interface becomes one of weak links of the composite insulator. The adhesive used in the prior art is generally a silane coupling agent, has the characteristics of high bonding strength, high temperature resistance and the like, plays the role of main interface hydrogen bond and chemical bond crosslinking, but the conventional interface adhesive only can provide the function of bonding the umbrella skirt sheath with the epoxy glass fiber core rod and does not have the function of NO generated by high-voltage-resistant corona like silicon rubber 2 Function, but interface is long-termTo NO 2 The corrosion easily causes interface failure, the strength of the epoxy core rod is reduced, and the problems of abnormal heating, breakdown, even brittle fracture, brittle fracture and the like of the insulator occur. The interface adhesive used in the present composite insulator industrial production is mainly a micromolecular silane coupling agent which is used for forming firm interface adhesion between a sheath and a core rod, but when the interface has defects, the aging process cannot be slowed down, and NO cannot be resisted 2 The intrusion of (1). Thus, an intensive understanding of NO 2 Aging mechanism of silicon rubber and improvement of NO of silicon rubber 2 Barrier property to improve NO in strong oxidizing gas 2 The application in the equal-pole environment has important significance.
Disclosure of Invention
The invention aims to provide an adhesive and a preparation method and application thereof. The adhesive prepared by the preparation method has excellent corona resistance and NO resistance 2 The gas corrosion and the water barrier capability can effectively prolong the service life of the composite insulator.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of the adhesive comprises the following steps:
s1, functionalized g-C 3 N 4 The preparation of (1):
preparing silane solution, adding ethanol and water to obtain mixed solution, and adding g-C 3 N 4 Firstly adjusting the pH value of the solution, standing, secondly adjusting the pH value of the solution, heating, preserving heat, filtering to obtain a lower-layer precipitate, washing and drying to obtain the functionalized g-C 3 N 4 ;
S2, preparing an adhesive:
preparing an ethanol aqueous solution, adjusting the pH value of the solution, and adding the functionalized g-C prepared in the step S1 3 N 4 Stirring and carrying out ultrasonic treatment to obtain a mixed solution, adding a coupling agent, stirring and reacting to obtain the adhesive.
Preferably, the step S1 includes at least one of the following (1) to (8):
(1) The silane solution is a mixed solution of tetraethoxysilane and triethoxysilane, wherein the mass percentage of tetraethoxysilane and triethoxysilane is 75: (20-25);
(2) The volume ratio of the ethanol solution to the water solution to the silane solution is 70: (5-15): (15-25);
(3) The g to C 3 N 4 The proportion of the mixed solution is that 10mg g-C is added into each milliliter of the mixed solution 3 N 4 ;
(4) The pH value of the first adjustment solution is adjusted to 4.5-5.0 by selecting glacial acetic acid;
(5) The pH value of the second adjustment solution is adjusted to 8.0-8.5 by using a sodium hydroxide solution with the concentration of 2.5 wt.%;
(6) The mixture is placed at room temperature for 35-45 h;
(7) The heating is to 60-65 ℃;
(8) The heat preservation time is 2-4 h.
Preferably, the step S2 includes at least one of the following (1) to (8):
(1) The volume ratio of the ethanol solution to the water in the ethanol aqueous solution is 75: (20-25);
(2) The pH value of the solution is adjusted to 4 by selecting glacial acetic acid;
(3) Said functionalized g-C 3 N 4 The addition amount of (A) is 10-15 mg/ml;
(4) The stirring time is 5-15 min;
(5) The ultrasonic time is 10-15 min;
(6) The volume ratio of the coupling agent to the mixed solution is 1: (10-15);
(7) The coupling agent comprises vinyl triethoxysilane;
(8) The reaction is carried out for 1 to 2 hours at a temperature of between 60 and 70 ℃.
An adhesive prepared by the preparation method of the adhesive.
A modified RTV coating comprises the following components in parts by weight:
90-100 parts of silicon rubber, 10-20 parts of filler, 2-5 parts of adhesive, 1-2 parts of catalyst and 1-2 parts of cross-linking agent.
Preferably, the modified RTV coating comprises at least one of the following (1) to (4):
(1) The silicone rubber comprises vinyl polydimethylsiloxane;
(2) The filler comprises gas phase SiO 2 ;
(3) The catalyst comprises dibutyltin dilaurate;
(4) The cross-linking agent comprises ethyl orthosilicate.
A preparation method of the modified RTV coating comprises the following steps:
and (2) stirring the silicon rubber, the filler and the adhesive for 2-3 hours at 100-120 ℃ in vacuum, adding the catalyst and the crosslinking agent, and continuously stirring for 10-15 minutes to obtain the RTV coating.
The application of the adhesive in the composite insulator is used for sealing and bonding the interface between the composite insulator sheath and the core rod.
The invention adopts a sol-gel method to process g-C 3 N 4 Is functionally modified at g-C 3 N 4 The surface is grafted with a large amount of silane, so that the interface compatibility of the filler and the silicon rubber is enhanced to a certain extent, and NO is reduced 2 Free volume of gas diffusion. Nanostructure g-C 3 N 4 Has a large specific surface area (300 m) 2 g -1 ) And good chemical stability, especially at g-C 3 N 4 In the triazine structure, sp2 hybridized pyridine nitrogen atom has lone pair electrons, so that the triazine structure has unique solid basic property and can be used for attracting NO 2 Can help to improve NO resistance of interface air gap 2 The ability of the gas to corrode, thereby slowing down the diffusion of the gas into the interior of the coating. At the same time, functionally modifying g-C 3 N 4 The nano-sheets can also play a role in cross connection and strengthening RTV matrix, and further reduce NO 2 The free volume of gas molecule diffusion is increased, thereby increasing NO generated by the interface adhesive to corona and the like 2 The anti-aging performance of corrosive gas and the water-blocking capability of the interface adhesive. In addition, in g-C 3 N 4 Surface ofGrafting a large amount of silane, breaking its internal van der Waals interactions, to make g-C 3 N 4 The sheet is stripped and dispersed, and the method changes the polarity of molecular chains and improves the modified g-C 3 N 4 The interface compatibility with the nonpolar RTV silicon rubber coating ensures that the prepared adhesive has corona resistance.
Compared with the prior art, the invention has the following beneficial effects:
the invention selects the coupling agent pair g-C 3 N 4 The adhesive prepared by modification has excellent corona resistance and NO resistance 2 The gas corrosion and the water barrier capability effectively prolong the service life of the composite insulator.
Drawings
FIG. 1 is a Bode plot of the RTV coatings obtained in the examples of the invention and comparative examples, as well as of the conventional coatings after immersion in a 3.5% NaCl solution for 96 h.
FIG. 2 shows RTV coatings of examples 1 to 3 (a) to (c) of the present invention and comparative examples 1 to 2 (d) to (e) of the present invention on NO 2 Bode plot after 24h gas treatment.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the examples and comparative examples, the experimental methods used were conventional unless otherwise specified, and the materials, reagents and the like used were commercially available unless otherwise specified.
Example 1 preparation of an adhesive
S1, functionalized g-C 3 N 4 The preparation of (1):
preparing ethyl orthosilicate and triethoxysilane with the mass percentage of 75:25, based on ethanol, water, a silane solutionThe volume percentage is 70:15:15 preparing a mixed solution, and mixing the solution according to the proportion of 10mg g-C per milliliter of the mixed solution 3 N 4 In a proportion of g-C 3 N 4 Dispersing with g-C by using glacial acetic acid 3 N 4 Adjusting the pH value of the mixed solution to 4.5, standing at room temperature for 40 hours, adjusting the pH value of the solution to 8.5 by using a sodium hydroxide solution (2.5 wt.%), keeping the temperature at 65 ℃ for 3 hours, obtaining a lower-layer precipitate, cleaning and drying the lower-layer precipitate to obtain functionalized g-C 3 N 4 ;
S2, preparing an adhesive:
according to the volume ratio of ethanol to water of 75:25 aqueous ethanol solution and adjusting the pH of the solution to 4 using glacial acetic acid, followed by functionalization of g-C at 10mg per ml of aqueous ethanol solution 3 N 4 Adding functionalized g-C in a proportion of 3 N 4 And after stirring for 5min, carrying out ultrasonic treatment for 15min to obtain a mixed solution, wherein the volume ratio of the mixed solution to the coupling agent is 1:10 adding a coupling agent, stirring for 10min, and then placing the mixture into a 60 ℃ oven for treatment for 1h to obtain the adhesive.
Wherein the coupling agent is vinyl triethoxysilane.
Example 2 preparation of an adhesive
S1, functionalized g-C 3 N 4 The preparation of (1):
preparing ethyl orthosilicate and triethoxysilane, wherein the weight percentage of the ethyl orthosilicate and the triethoxysilane is 75:25, based on the weight percentage of ethanol, water and silane solution as 70:5:25 preparing a mixed solution, and mixing the solution according to the proportion of 10mg g-C per milliliter of the mixed solution 3 N 4 In a proportion of g-C 3 N 4 Dispersing with g-C by using glacial acetic acid 3 N 4 Adjusting the pH value of the mixed solution to 5.0, standing at room temperature for 35 hours, adjusting the pH value of the solution to 8.0 by using a sodium hydroxide solution (2.5 wt.%), keeping the temperature at 60 ℃ for 2 hours, obtaining a lower-layer precipitate, cleaning and drying the lower-layer precipitate to obtain functionalized g-C 3 N 4 ;
S2, preparing an adhesive:
according to the volume ratio of ethanol to water of 75:25, and adjusting the pH value of the solution to 4 by using glacial acetic acid, and then adding the solution to the solution according to the proportion of ethanol water per milliliterSolution 12mg functionalized g-C 3 N 4 Adding functionalized g-C in a proportion of 3 N 4 And carrying out ultrasonic treatment for 12min after stirring for 10min to obtain a mixed solution, wherein the volume ratio of the mixed solution to the coupling agent is 1:12 adding a coupling agent, stirring for 5min, and then placing in a 65 ℃ oven for treatment for 1.5h to obtain the adhesive.
Wherein the coupling agent is vinyl triethoxysilane.
Example 3 preparation of an adhesive
S1, functionalized g-C 3 N 4 The preparation of (1):
preparing ethyl orthosilicate and triethoxysilane with the mass percentage of 75:20, based on the weight percentage of ethanol, water and silane solution as 70:10:20 preparing a mixed solution, and mixing the solution according to the proportion of 10mg g-C per milliliter of the mixed solution 3 N 4 In a proportion of g-C 3 N 4 Dispersing with g-C by using glacial acetic acid 3 N 4 Adjusting the pH value of the mixed solution to 4.5, standing at room temperature for 45 hours, adjusting the pH value of the solution to 8.5 by using a sodium hydroxide solution (2.5 wt.%), keeping the temperature at 65 ℃ for 4 hours, and cleaning and drying a lower-layer precipitate to obtain functionalized g-C 3 N 4 ;
S2, preparing an adhesive:
according to the volume ratio of ethanol to water of 75:20 aqueous ethanol solution and adjusting the pH of the solution to 4 using glacial acetic acid, followed by functionalization of g-C at 15mg per ml of aqueous ethanol solution 3 N 4 Adding functionalized g-C in a proportion of 3 N 4 And after stirring for 15min, carrying out ultrasonic treatment for 15min to obtain a mixed solution, wherein the volume ratio of the mixed solution to the coupling agent is 1:15 adding a coupling agent, stirring for 15min, and then placing the mixture into an oven at 70 ℃ for processing for 2h to obtain the adhesive.
Wherein the coupling agent is vinyl triethoxysilane.
Comparative example 1
The comparative example differs from example 1 only in that g to C 3 N 4 Simple mixing with coupling agent.
Preparation of the adhesive:
according to the volume ratio of 75:25 preparing an aqueous alcohol solution of ethanol and water, adjusting the pH of the solution to 4 using glacial acetic acid, and then adjusting the pH to 10mg g-C per ml of aqueous alcohol solution 3 N 4 In a proportion of g-C 3 N 4 And after stirring for 5min, carrying out ultrasonic treatment for 15min to obtain a mixed solution, wherein the volume ratio of the mixed solution to the coupling agent is 1:10, adding a coupling agent, and stirring for 10min to obtain the adhesive.
Wherein the coupling agent is vinyl triethoxysilane.
Comparative example 2
The comparative example differs from example 1 only in that the step S1 mixed solution contains 30mg g-C/ml of mixed solution 3 N 4 In a ratio of g to C 3 N 4 。
The preparation process is referred to example 1.
Test example one, resistance to NO 2 Determination of Corrosion Properties
1. Experimental sample
Examples 1 to 3 and comparative examples 1 to 2 adhesives RTV coatings, ordinary RTV coatings, were prepared in the following manner.
The preparation method of the RTV coating comprises the following steps:
100 parts of vinyl polydimethylsiloxane and 20 parts of gas-phase SiO 2 And 2 parts of adhesive, stirring the mixture for 2 hours in vacuum at the temperature of 120 ℃, adding 1 part of dibutyltin dilaurate and 1 part of ethyl orthosilicate, and continuously stirring the mixture for 10 minutes to obtain the RTV coating. And uniformly spin-coating the prepared RTV coating on the surface of the ITO glass, putting the ITO glass into a thermostat at 60 ℃ for curing for 2h, and then curing at room temperature for 24h to obtain the RTV coating.
The preparation method of the common RTV coating comprises the following steps:
100 parts of vinyl polydimethylsiloxane, 20 parts of gas phase SiO 2 And 2 parts of coupling agent (vinyl triethoxysilane) are stirred for 2 hours in vacuum at 120 ℃, 1 part of dibutyltin dilaurate and 1 part of ethyl orthosilicate are added after the stirring is finished, and the stirring is continued for 10 minutes to obtain the RTV coating. And uniformly spin-coating the prepared RTV coating on the surface of the ITO glass, putting the ITO glass into a thermostat at 60 ℃ for curing for 2h, and then curing at room temperature for 24h to obtain a common RTV coating.
2. Experimental methods
Coating with NO 2 Barrier properties against water before gas aging: measuring the AC impedance spectrum of each RTV coating sample in an environment of 3.5 percent of NaCl solution soaking for 96 h;
coating with NO 2 Barrier properties against water after gas aging: samples of each coating were tested in NO 2 Treatment in a closed glass vessel with a gas concentration of 115mg/L for 24h, followed by immersion in 3.5% NaCl solution for 96h, AC impedance spectroscopy of the coating using an electrochemical workstation;
test coating NO 2 Barrier properties against water before and after gas ageing, and NO resistance of the reaction coating 2 And (4) performance. The test results are shown in FIGS. 1 to 2.
As can be seen from FIG. 1, the coating layers obtained in examples 1 to 3 of the present invention and comparative examples 1 to 2 and the conventional coating layer each had an impedance mode value of 10 9 Ωcm 2 On the other hand, this indicates that the coating has better water-blocking performance at this time.
As can be seen from FIG. 2, the RTV coatings (a) to (c) obtained in examples 1 to 3 of the present invention underwent NO treatment 2 The coatings (d) to (e) prepared in comparative examples 1 to 2, which still retain good water-blocking properties after gas ageing, were coated with NO 2 The gas has a significantly reduced impedance modulus after aging. It can be stated that when g-C is used 3 N 4 With vinyl silane coupling agents either simply mixed or in functionalized g-C 3 N 4 g-C added during the preparation 3 N 4 In an inappropriate proportion to the mixed solution, all contribute to the NO resistance of the adhesive 2 The corrosion properties become poor.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (8)
1. The preparation method of the adhesive is characterized by comprising the following steps of:
s1, functionalized g-C 3 N 4 The preparation of (1):
preparing silane solution, adding ethanol and water to obtain mixed solution, and adding g-C 3 N 4 Firstly adjusting the pH value of the solution, standing, secondly adjusting the pH value of the solution, heating, preserving heat, filtering to obtain a lower-layer precipitate, washing and drying to obtain the functionalized g-C 3 N 4 ;
S2, preparing an adhesive:
preparing an ethanol aqueous solution, adjusting the pH value of the solution, and adding the functionalized g-C prepared in the step S1 3 N 4 Stirring and carrying out ultrasonic treatment to obtain a mixed solution, adding a coupling agent, stirring and reacting to obtain the adhesive.
2. The method for producing an adhesive according to claim 1, wherein the step S1 includes at least one of the following (1) to (8):
(1) The silane solution is a mixed solution of tetraethoxysilane and triethoxysilane, wherein the mass percentage of tetraethoxysilane and triethoxysilane is 75: (20-25);
(2) The volume ratio of the ethanol solution to the water solution to the silane solution is 70: (5-15): (15-25);
(3) The g to C 3 N 4 The proportion of the mixed solution is that 10mg g-C is added into each milliliter of the mixed solution 3 N 4 ;
(4) The pH value of the first adjustment solution is adjusted to 4.5-5.0 by selecting glacial acetic acid;
(5) The pH value of the second adjustment solution is adjusted to 8.0-8.5 by using a sodium hydroxide solution with the concentration of 2.5 wt.%;
(6) The mixture is placed at room temperature for 35-45 h;
(7) The heating is carried out to 60-65 ℃;
(8) The heat preservation time is 2-4 h.
3. The method for producing an adhesive according to claim 1, wherein the step S2 includes at least one of the following (1) to (8):
(1) The volume ratio of the ethanol solution to the water in the ethanol aqueous solution is 75: (20-25);
(2) The pH value of the solution is adjusted to 4 by selecting glacial acetic acid;
(3) Said functionalized g-C 3 N 4 The addition amount of (A) is 10-15 mg/ml;
(4) The stirring time is 5-15 min;
(5) The ultrasonic time is 10-15 min;
(6) The volume ratio of the coupling agent to the mixed solution is 1: (10-15);
(7) The coupling agent comprises vinyl triethoxysilane;
(8) The reaction is carried out for 1 to 2 hours at a temperature of between 60 and 70 ℃.
4. An adhesive prepared by the method of any one of claims 1 to 3.
5. The modified RTV coating is characterized by comprising the following components in parts by weight:
90-100 parts of silicon rubber, 10-20 parts of filler, 2-5 parts of adhesive according to claim 4, 1-2 parts of catalyst and 1-2 parts of cross-linking agent.
6. The modified RTV coating of claim 5, comprising at least one of the following (1) to (4):
(1) The silicone rubber comprises vinyl polydimethylsiloxane;
(2) The filler comprises gas phase SiO 2 ;
(3) The catalyst comprises dibutyltin dilaurate;
(4) The cross-linking agent comprises ethyl orthosilicate.
7. A process for the preparation of a modified RTV coating according to any one of claims 5 to 6, comprising the steps of:
stirring silicon rubber, filler and the adhesive according to claim 4 at 100-120 ℃ for 2-3 hours in vacuum, adding a catalyst and a crosslinking agent, and continuously stirring for 10-15 minutes to obtain the RTV coating.
8. Use of the adhesive according to claim 4 in a composite insulator for interfacial sealing bonding between a sheath of the composite insulator and a core rod.
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CN202211530709.3A CN115820204A (en) | 2022-12-01 | 2022-12-01 | Adhesive and preparation method and application thereof |
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