CN115028556A - Gemini surfactant for insulator surface RTV stripping and preparation method and application thereof - Google Patents

Gemini surfactant for insulator surface RTV stripping and preparation method and application thereof Download PDF

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CN115028556A
CN115028556A CN202210796760.2A CN202210796760A CN115028556A CN 115028556 A CN115028556 A CN 115028556A CN 202210796760 A CN202210796760 A CN 202210796760A CN 115028556 A CN115028556 A CN 115028556A
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dimethyl
cyclohexene
gemini surfactant
acid
rtv
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夏晓健
林德源
万芯瑗
洪毅成
陈云翔
韩纪层
严康骅
陈奕扬
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Electric Power Research Institute of State Grid Fujian Electric Power Co Ltd
State Grid Fujian Electric Power Co Ltd
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Electric Power Research Institute of State Grid Fujian Electric Power Co Ltd
State Grid Fujian Electric Power Co Ltd
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    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C309/00Sulfonic acids; Halides, esters, or anhydrides thereof
    • C07C309/01Sulfonic acids
    • C07C309/28Sulfonic acids having sulfo groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton
    • C07C309/45Sulfonic acids having sulfo groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton
    • C07C309/51Sulfonic acids having sulfo groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton at least one of the nitrogen atoms being part of any of the groups, X being a hetero atom, Y being any atom
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    • C07C303/00Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
    • C07C303/02Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
    • C07C303/22Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof from sulfonic acids, by reactions not involving the formation of sulfo or halosulfonyl groups; from sulfonic halides by reactions not involving the formation of halosulfonyl groups
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    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C303/00Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
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    • C09D9/00Chemical paint or ink removers
    • C09D9/04Chemical paint or ink removers with surface-active agents
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    • C09K23/00Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
    • C09K23/22Amides or hydrazides
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    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2601/00Systems containing only non-condensed rings
    • C07C2601/12Systems containing only non-condensed rings with a six-membered ring
    • C07C2601/16Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated

Abstract

The invention discloses a gemini surfactant for insulator surface RTV stripping and a preparation method thereof, which comprises the steps of firstly carrying out Diels-Alder reaction on 2, 3-dimethyl-1, 3-dibutene and maleic acid to generate 1, 2-dimethyl-4, 5-dicarboxylic acid-cyclohexene; then reacting the product with thionyl chloride to generate 1, 2-dimethyl-4, 5-diformyl chloride-cyclohexene; then reacting the intermediate with sulfanilic acid to generate 1, 2-dimethyl-4, 5-dimethylamide benzenesulfonic acid-cyclohexene; finally, the product reacts with long-chain alkyl bromide to generate gemini surfactant. The gemini surfactant prepared by the method contains a cyclohexene structure, so that the cleaning capability of RTV surface pollutants on the surface of the insulator is improved; brominated alkanes with different chain lengths can be selected to regulate and control the performance of the gemini surfactant; the contained sulfonic acid group is a protonic acid and can perform the cracking function on the RTV on the surface of the insulator.

Description

Gemini surfactant for insulator surface RTV stripping and preparation method and application thereof
Technical Field
The invention belongs to the technical field of preparation of surfactants, and particularly relates to a preparation method of a gemini surfactant capable of greatly reducing the surface tension of a system and promoting the RTV cracking of the surface of an insulator in the field of RTV stripping of the surface of the insulator.
Background
Electric power transportation is a foundation of the high-speed development of the country, and the most common device in a transmission circuit is an insulator. According to different insulating materials, ceramic insulators, glass insulators and composite insulators are generally adopted, wherein the most common ceramic insulators and glass insulators are adopted. In some regions with bad weather or serious pollution, the surface of a ceramic or glass insulator is coated with a room temperature vulcanized silicone Rubber (RTV) coating to increase the hydrophobicity and hydrophobic migration performance of the surface of the insulator, so that the flashover voltage of the insulator is improved, and the risk of flashover pollution of the insulator is reduced. With the lapse of time and the influence of ultraviolet rays, the hydrophobicity and the hydrophobic migration performance of the RTV coating can be reduced or even lost, and the circuit transmission safety is seriously influenced. The existing solution is to directly replace the insulator with the RTV coating, and the cost is high.
The currently developed stripping solution for the insulator surface RTV adopts a combination of an organic solvent and a strong acid, for example, the invention patent CN202010283201.2 discloses a special stripping agent for room temperature vulcanized silicone rubber for insulators and a stripping method, which utilizes a highly soluble solvent butanone or acetone in combination with concentrated hydrochloric acid and concentrated sulfuric acid to strip the RTV. Wherein, the acetone and the butanone belong to dangerous chemicals and can be burnt and exploded when exposed to open fire. Concentrated sulfuric acid and concentrated hydrochloric acid have strong corrosivity and are harmful to human safety.
Disclosure of Invention
In order to solve the technical problems, the invention provides an RTV stripping gemini surfactant used for the surface of an insulator, which serves as a stripping aid and has the function of a surfactant. The gemini surfactant prepared by the method is a sulfonic surfactant, can provide protons and is beneficial to cracking Si-O-Si bonds; the cleaning agent has the performance of a surfactant, and can be beneficial to rinsing RTV and organic solvent remained on the surface of the insulator after stripping; in addition, the gemini surfactant prepared by the invention has excellent performance, and can be also applied to other fields.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a gemini surfactant for RTV stripping on the surface of an insulator has the following structural formula:
Figure 100002_DEST_PATH_IMAGE001
the preparation method of the gemini surfactant comprises the following steps:
(1) under the condition of low-temperature condensed water reflux, a certain amount of 2, 3-dimethyl-1, 3-dibutene and maleic acid in a corresponding proportion are taken into a reactor. Dichloromethane was added as a solvent and the reaction was refluxed for 24 h. And removing the solvent and the redundant reactants by rotary evaporation to obtain the product 1, 2-dimethyl-4, 5-dicarboxylic acid-cyclohexene.
(2) And (2) adding a certain amount of the product 1, 2-dimethyl-4, 5-dicarboxylic acid-cyclohexene obtained in the step (2) and a catalyst into a three-neck flask provided with a reflux condenser tube, a dropping funnel and a stirrer, slowly raising the temperature of the oil bath to 70-80 ℃, slowly dropwise adding thionyl chloride, and maintaining the reaction temperature for 2 hours. And after the reaction is finished, removing excessive thionyl chloride by reduced pressure distillation to obtain a product 1, 2-dimethyl-4, 5-diformyl chloride-cyclohexene.
(3) And (3) dropwise adding the product 1, 2-dimethyl-4, 5-diformyl chloride-cyclohexene dissolved in pyridine in the step (2) into a reactor filled with sulfanilic acid in a corresponding proportion for continuous reaction for 4 hours under the condition of ice-water bath. After the reaction is finished, recrystallizing by using diethyl ether to obtain the product 1, 2-dimethyl-4, 5-dimethylamide benzenesulfonic acid-cyclohexene.
(4) And (3) dissolving the product 1, 2-dimethyl-4, 5-dimethylamide benzenesulfonic acid-cyclohexene obtained in the step (3) in toluene, adding a corresponding amount of bromoalkane into the reactor, and carrying out reflux reaction at 95 ℃ for 4 hours. And purifying to obtain the final product gemini surfactant.
Preferably, in the step (1), the molar ratio of the 2, 3-dimethyl-1, 3-dibutene to the maleic acid is 1: 0.8-1.
Preferably, in the step (2), the molar ratio of the 1, 2-dimethyl-4, 5-dicarboxylic acid-cyclohexene to the thionyl chloride is 1: 2.5-3.
Preferably, the catalyst in the step (2) is 2-aminopyridine, and the adding amount of the catalyst is 0.4-0.6% of the mass of the maleic acid.
Preferably, in the step (3), the molar ratio of the 1, 2-dimethyl-4, 5-diformyl chloride-cyclohexene to the sulfanilic acid is 1: 2.5-3.
Preferably, the molar ratio of the 1, 2-dimethyl-4, 5-dimethylaminobenzenesulfonic acid-cyclohexene to the bromoalkane in the step (4) is 1: 2.5-3.
Preferably, the brominated alkane in the step (4) refers to one of n-octyl bromide, n-decabromoalkane, n-dodecane bromide and n-tetradecane bromide.
Compared with the prior art, the invention has the following technical advantages:
(1) the surfactant prepared by the invention has an activating effect on RTV stripping. The surfactant prepared by the invention is a sulfonic acid surfactant, and belongs to protonic acid. In the stripping process of the RTV, the sulfonic acid group releases protons to attack and break Si-O-Si bonds in the RTV, and the RTV is cut into fragments from the original whole. The swelling effect of the solvent is matched, the molecular gap of the RTV is enlarged, and the surfactant can deeply destroy the internal Si-O-Si bond. Under the synergistic action of the surfactant and the organic solvent, the stripping process of the RTV is gradually completed.
(2) The surfactant prepared by the invention is beneficial to the subsequent cleaning process. The RTV coating is still adsorbed on the surface of the insulator after peeling, and needs to be washed or wiped by a high-pressure water gun. The surfactant prepared by the invention can reduce the surface tension of water, is more favorable for dispersing RTV fragments in water and is convenient to be carried away by water. When the cleaning agent is used for cleaning, the hydrophobic tail chain in the surfactant molecule can be tightly combined with the RTV due to hydrophobicity, and the surfactant is wrapped on the surface layer of the RTV fragments to form a surfactant molecule layer. The hydrophilic groups of the surfactant are located at the periphery of the molecular layer. In water, the hydrophilic group binds to a water molecule to form a vesicle structure in the structure of "water-hydrophilic group-hydrophobic tail-RTV fragment". When the washing machine is used for washing, the vesicles are dispersed in a water body and are easily taken away by water, so that the washing purpose is achieved.
(3) The surfactant prepared by the invention structurally belongs to a gemini surfactant. The polymer contains two hydrophilic groups and two hydrophobic tail chains on one molecule. When the common surfactants are arranged on the surface of water in an oriented manner, the common surfactants cannot be closely arranged due to the influence of intermolecular repulsion, and further the activity of the surfactants is limited. The gemini surfactant connects the two hydrophilic groups together through covalent bonds, and the distance between the hydrophilic groups is pulled in, so that the arrangement of the surfactant is tighter, and the effect of reducing the surface tension of water is more obvious.
Drawings
FIG. 1 is a flow chart of a method for producing a gemini surfactant for RTV stripping on an insulator surface according to the present invention;
FIG. 2 is a surface tension test chart of a surfactant prepared according to the present invention; as can be seen from the figure, the surfactants G08 prepared in examples 1 to 4; g10; g12; g14 has better performance of reducing surface tension, and the cmc concentration is lower, so that the use requirement can be met by less use amount;
FIG. 3 shows the result of RTV stripping on the surface of an insulator, and comparing the result before and after stripping, it can be seen that the RTV on the surface of the insulator can be stripped cleanly after the surfactant prepared by the invention is added;
FIG. 4 is a nuclear magnetic hydrogen spectrum of the gemini surfactant prepared in example 1.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
Example 1
(1) 8.2 g of 2, 3-dimethyl-1, 3-dibutylene (0.1 mol) and 11.6 g of maleic acid (0.1 mol) were taken in a reactor under the condition of refluxing with low-temperature condensed water at 10 ℃. 100 mL of methylene chloride was added as a solvent, and the reaction was refluxed at 40 ℃ for 24 hours. And removing the solvent and the redundant reactants by rotary evaporation to obtain the product 1, 2-dimethyl-4, 5-dicarboxylic acid-cyclohexene.
(2) 9.9 g of 1, 2-dimethyl-4, 5-dicarboxylic acid-cyclohexene of step (2) (0.5 mol) and 0.05 g of 2-aminopyridine were placed in a three-necked flask equipped with a reflux condenser, a dropping funnel and a stirrer, the oil bath temperature was slowly raised to 80 ℃ and 14.3 g of thionyl chloride (1.2 mol) was slowly added dropwise while maintaining the reaction temperature for 2 hours. And after the reaction is finished, removing excessive thionyl chloride by reduced pressure distillation to obtain a product 1, 2-dimethyl-4, 5-diformyl chloride-cyclohexene.
(3) 11.7 g of the product 1, 2-dimethyl-4, 5-diformylcyclohexene (0.5 mol) from step (2) dissolved in pyridine were added dropwise to a reactor containing 17.3 g of aminobenzenesulfonic acid under ice-water bath conditions for 4 h. And after the reaction is finished, recrystallizing the product by using diethyl ether to obtain the product 1, 2-dimethyl-4, 5-dimethylamide benzenesulfonic acid-cyclohexene.
(4) 5.08 g of 1, 2-dimethyl-4, 5-dimethylaminobenzenesulfonic acid-cyclohexene (0.01 mol) of the product of the step (3) is dissolved in 60 mL of toluene, and 3.86 g of bromo-n-octane (0.02 mol) is added into the reactor to carry out reflux reaction for 4 h at 95 ℃. And purifying to obtain the final product gemini surfactant G08.
Example 2
(1) 8.2 g of 2, 3-dimethyl-1, 3-dibutylene (0.1 mol) and 11.6 g of maleic acid (0.1 mol) were taken in a reactor under the condition of refluxing with low-temperature condensed water at 10 ℃. 100 mL of methylene chloride was added as a solvent, and the reaction was refluxed at 40 ℃ for 24 hours. And removing the solvent and the redundant reactants by rotary evaporation to obtain the product 1, 2-dimethyl-4, 5-dicarboxylic acid-cyclohexene.
(2) 9.9 g of the product 1, 2-dimethyl-4, 5-dicarboxylic acid-cyclohexene of step (2) (0.5 mol) and 0.05 g of 2-aminopyridine were placed in a three-necked flask equipped with a reflux condenser, a dropping funnel and a stirrer, the oil bath temperature was slowly raised to 70 ℃ and 14.3 g of thionyl chloride (1.2 mol) was slowly added dropwise, maintaining the reaction temperature for 2 hours. And after the reaction is finished, removing excessive thionyl chloride by reduced pressure distillation to obtain a product 1, 2-dimethyl-4, 5-diformylchloride-cyclohexene.
(3) 11.7 g of the product 1, 2-dimethyl-4, 5-diformylcyclohexene (0.5 mol) from step (2) dissolved in pyridine were added dropwise to a reactor containing 17.3 g of aminobenzenesulfonic acid in an ice-water bath and the reaction was continued for 4 hours. And after the reaction is finished, recrystallizing the product by using diethyl ether to obtain the product 1, 2-dimethyl-4, 5-dimethylamide benzenesulfonic acid-cyclohexene.
(4) 5.08 g of 1, 2-dimethyl-4, 5-dimethylaminobenzenesulfonic acid-cyclohexene (0.01 mol) of the product of step (3) was dissolved in 60 mL of toluene, and 4.42 g of bromodecane (0.02 mol) was added to the reactor, followed by reflux reaction at 95 ℃ for 4 hours. And purifying to obtain the final product gemini surfactant G10.
Example 3
(1) 8.2 g of 2, 3-dimethyl-1, 3-dibutylene (0.1 mol) and 11.6 g of maleic acid (0.1 mol) were taken in a reactor under reflux of low-temperature condensed water at 10 ℃. 100 mL of methylene chloride was added as a solvent, and the reaction was refluxed at 40 ℃ for 24 hours. And removing the solvent and the redundant reactants by rotary evaporation to obtain the product 1, 2-dimethyl-4, 5-dicarboxylic acid-cyclohexene.
(2) 9.9 g of 1, 2-dimethyl-4, 5-dicarboxylic acid-cyclohexene of step (2) (0.5 mol) and 0.05 g of 2-aminopyridine were placed in a three-necked flask equipped with a reflux condenser, a dropping funnel and a stirrer, the oil bath temperature was slowly raised to 80 ℃ and 14.3 g of thionyl chloride (1.2 mol) was slowly added dropwise while maintaining the reaction temperature for 2 hours. And after the reaction is finished, removing excessive thionyl chloride by reduced pressure distillation to obtain a product 1, 2-dimethyl-4, 5-diformyl chloride-cyclohexene.
(3) 11.7 g of the product 1, 2-dimethyl-4, 5-diformylcyclohexene (0.5 mol) from step (2) dissolved in pyridine were added dropwise to a reactor containing 17.3 g of aminobenzenesulfonic acid in an ice-water bath and the reaction was continued for 4 hours. And after the reaction is finished, recrystallizing the product by using diethyl ether to obtain the product 1, 2-dimethyl-4, 5-dimethylamide benzenesulfonic acid-cyclohexene.
(4) 5.08 g of 1, 2-dimethyl-4, 5-dimethylaminobenzenesulfonic acid-cyclohexene (0.01 mol) of the product of step (3) are dissolved in 60 mL of toluene, and 4.98 g of bromododecane (0.02 mol) are added to the reactor and the reaction is refluxed at 95 ℃ for 4 hours. And purifying to obtain the final product gemini surfactant G12.
Example 4
(1) 8.2 g of 2, 3-dimethyl-1, 3-dibutylene (0.1 mol) and 11.6 g of maleic acid (0.1 mol) were taken in a reactor under the condition of refluxing with low-temperature condensed water at 10 ℃. 100 mL of methylene chloride was added as a solvent, and the reaction was refluxed at 40 ℃ for 24 hours. And removing the solvent and the redundant reactants by rotary evaporation to obtain the product 1, 2-dimethyl-4, 5-dicarboxylic acid-cyclohexene.
(2) 9.9 g of 1, 2-dimethyl-4, 5-dicarboxylic acid-cyclohexene of step (2) (0.5 mol) and 0.05 g of 2-aminopyridine were placed in a three-necked flask equipped with a reflux condenser, a dropping funnel and a stirrer, the oil bath temperature was slowly raised to 80 ℃ and 14.3 g of thionyl chloride (1.2 mol) was slowly added dropwise while maintaining the reaction temperature for 2 hours. And after the reaction is finished, removing excessive thionyl chloride by reduced pressure distillation to obtain a product 1, 2-dimethyl-4, 5-diformyl chloride-cyclohexene.
(3) 11.7 g of the product 1, 2-dimethyl-4, 5-diformylcyclohexene (0.5 mol) from step (2) dissolved in pyridine were added dropwise to a reactor containing 17.3 g of aminobenzenesulfonic acid in an ice-water bath and the reaction was continued for 4 hours. After the reaction is finished, recrystallizing by using diethyl ether to obtain the product 1, 2-dimethyl-4, 5-dimethylamide benzenesulfonic acid-cyclohexene.
(4) 5.08 g of 1, 2-dimethyl-4, 5-dimethylaminobenzenesulfonic acid-cyclohexene (0.01 mol) of the product of step (3) was dissolved in 60 mL of toluene, and 5.54 g of bromotetradecane (0.02 mol) was added to the solution in the reactor and reacted at 95 ℃ under reflux for 4 hours. And purifying to obtain the final product gemini surfactant G14.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. This application is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims.
It is to be understood that the present invention is not limited to what has been described above, and that various modifications and changes may be made without departing from the scope thereof. The scope of the invention is limited only by the appended claims.

Claims (9)

1. A gemini surfactant for RTV stripping on the surface of an insulator is characterized in that the gemini surfactant has the following structural formula:
Figure DEST_PATH_IMAGE001
2. the preparation method of the gemini surfactant for insulator surface RTV stripping according to claim 1, characterized by comprising the following steps:
under the condition of low-temperature condensed water reflux, taking 2, 3-dimethyl-1, 3-dibutene and maleic acid in a reactor, adding dichloromethane as a solvent, carrying out reflux reaction for 24 hours, and removing the solvent and redundant reactants by rotary evaporation to obtain a product 1, 2-dimethyl-4, 5-dicarboxylic acid-cyclohexene;
adding the product 1, 2-dimethyl-4, 5-dicarboxylic acid-cyclohexene obtained in the step (2) and a catalyst into a three-neck flask provided with a reflux condenser tube, a dropping funnel and a stirrer, slowly raising the temperature of an oil bath to 70-80 ℃, slowly dropwise adding thionyl chloride, maintaining the reaction temperature for 2 hours, and removing excessive thionyl chloride through reduced pressure distillation after the reaction is finished to obtain a product 1, 2-dimethyl-4, 5-diformylchloride-cyclohexene;
under the condition of ice-water bath, dropwise adding the product 1, 2-dimethyl-4, 5-diformyl chloride-cyclohexene dissolved in pyridine in the step (2) into a reactor filled with sulfanilic acid for continuous reaction for 4 hours, and recrystallizing with diethyl ether after the reaction is finished to obtain the product 1, 2-dimethyl-4, 5-diformylamide benzenesulfonic acid-cyclohexene;
and (3) dissolving the product 1, 2-dimethyl-4, 5-dimethylamide benzenesulfonic acid-cyclohexene obtained in the step (3) in toluene, adding bromoalkane into the reactor, carrying out reflux reaction at 95 ℃ for 4 hours, and purifying to obtain the gemini surfactant.
3. The method for preparing the gemini surfactant for insulator surface RTV stripping according to claim 2, characterized in that: in the step (1), the molar ratio of 2, 3-dimethyl-1, 3-dibutene to maleic acid is 1: 0.8-1.
4. The method for preparing the gemini surfactant for insulator surface RTV peeling according to claim 2, characterized in that: in the step (2), the molar ratio of the 1, 2-dimethyl-4, 5-dicarboxylic acid-cyclohexene to the thionyl chloride is 1: 2.5-3.
5. The method for preparing the gemini surfactant for insulator surface RTV peeling according to claim 2, characterized in that: the catalyst in the step (2) is 2-aminopyridine, and the adding amount of the catalyst is 0.4-0.6% of the mass of maleic acid.
6. The method for preparing the gemini surfactant for insulator surface RTV peeling according to claim 2, characterized in that: in the step (3), the molar ratio of the 1, 2-dimethyl-4, 5-diformyl chloride-cyclohexene to the sulfanilic acid is 1: 2.5-3.
7. The method for preparing the gemini surfactant for insulator surface RTV peeling according to claim 2, characterized in that: in the step (4), the molar ratio of the 1, 2-dimethyl-4, 5-dimethylaminobenzenesulfonic acid-cyclohexene to the bromoalkane is 1: 2.5-3.
8. The method for preparing the gemini surfactant for insulator surface RTV peeling according to claim 2 or 7, characterized in that: one of bromoalkane position n-bromooctane, n-bromodecane, n-bromododecane and n-bromotetradecane in the step (4).
9. Use of the gemini surfactant according to claim 1 in stripping an insulator surface RTV.
CN202210796760.2A 2022-07-07 2022-07-07 Gemini surfactant for insulator surface RTV stripping and preparation method and application thereof Pending CN115028556A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116041227A (en) * 2022-11-30 2023-05-02 福化微(厦门)电子材料有限公司 Sulfonic acid gemini surfactant and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1410426A (en) * 1964-08-05 1965-09-10 Du Pont photographic elements and compositions
JP2008085289A (en) * 2006-08-30 2008-04-10 National Institute Of Advanced Industrial & Technology Liquid crystal organic semiconductor material and organic semiconductor device using the same
CN111171623A (en) * 2018-11-09 2020-05-19 北京世纪航凯电力科技股份有限公司 Water-based cleaning agent for RTV (room temperature vulcanized) organic silicon coating for insulator
CN114702659A (en) * 2022-03-28 2022-07-05 江苏斯德瑞克化工有限公司 Rosin-based defoaming agent for cleaning electronic devices and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1410426A (en) * 1964-08-05 1965-09-10 Du Pont photographic elements and compositions
JP2008085289A (en) * 2006-08-30 2008-04-10 National Institute Of Advanced Industrial & Technology Liquid crystal organic semiconductor material and organic semiconductor device using the same
CN111171623A (en) * 2018-11-09 2020-05-19 北京世纪航凯电力科技股份有限公司 Water-based cleaning agent for RTV (room temperature vulcanized) organic silicon coating for insulator
CN114702659A (en) * 2022-03-28 2022-07-05 江苏斯德瑞克化工有限公司 Rosin-based defoaming agent for cleaning electronic devices and preparation method thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
SANKAPPA RAI, U. ET AL: "pyrazole chalcones and heterocyclic diamides as potential anticancer agents", 《ARABIAN JOURNAL OF CHEMISTRY》, vol. 8, no. 3, pages 317 - 321 *
许志龙等: "高压绝缘子瓷瓶除垢清洁剂的研制及应用", 《南通大学学报(自然科学版)》, vol. 14, no. 4, pages 36 - 40 *
邹平等: "支柱绝缘子表面污秽带电清洗剂的制备与清洗特性研究", 《广东化工》, vol. 44, no. 1, pages 39 - 40 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116041227A (en) * 2022-11-30 2023-05-02 福化微(厦门)电子材料有限公司 Sulfonic acid gemini surfactant and preparation method thereof

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