CN107641466B - Organic silicon solvent-free impregnating varnish and preparation method thereof - Google Patents
Organic silicon solvent-free impregnating varnish and preparation method thereof Download PDFInfo
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Abstract
The invention provides an organosilicon solvent-free impregnating varnish, wherein a molecular chain of the organosilicon solvent-free impregnating varnish contains four long chains connected to a tetrafunctional silica unit, the structural formula of the organosilicon solvent-free impregnating varnish is shown as a formula (1), and the molar weight of the tetrafunctional silica unit in the molecular chain of the organosilicon solvent-free impregnating varnish accounts for 1-10% of the molar weight of total chain unit. The invention also provides a preparation method of the organic silicon solvent-free impregnating varnish, and the preparation method introduces SiRnX4‑nThe organic silicon monomer B reserves silicon vinyl or silicon hydrogen group in the molecular chain of the organic silicon prepolymer, and the organic silicon solvent-free impregnating varnish containing the organic silicon shown in the formula (1) can be obtained through silicon hydrogen addition reaction during later curing. The impregnating varnish prepared by the method has no low molecular weight substance coming off when being cured into a film, does not influence the electrical property, has no pollution, and simultaneously has good electrical property and mechanical property.
Description
Technical Field
The invention belongs to the field of paint chemical industry, and particularly relates to organic silicon solvent-free impregnating varnish and a preparation method thereof.
Background
The organic silicon resin is a common resin at present, and is widely applied to the fields of impregnating varnish, paint, mica tape adhesive, modification of organic silicon resin such as polyester and epoxy resin and the like. The organic silicon impregnating varnish is a very important organic silicon insulating variety taking organic silicon resin as a binder, and is a thermosetting polysiloxane system with a highly cross-linked structure. From the basic components of the resin, most of the organic silicon resin varieties at home and abroad are methyl trichlorosilane and dimethyl dichlorosilane4 basic monomers such as silane, phenyltrichlorosilane, diphenyldichlorosilane and the like are used as raw materials; based on the binder composition of the impregnating varnish, the basic structural units of the impregnating varnish are 4, namely M (R)3SiO0.5)、D(R2SiO)、T(RSiO1.5) And Q (SiO)2) Units, and T units or Q units are indispensable components, to which organic groups such as Me, Et, Pr, Vi, Ph, etc. are bonded; according to the molecular chain composition in the silicone resin, the silicone resin can be divided into two categories, namely pure silicone resin and modified silicone resin; it can be classified into a low molar mass and a high molar mass according to the molecular molar mass; according to the different crosslinking and curing modes, silicone resins are classified into condensation type, peroxide initiation type and addition type.
The prepolymer used for the condensed type organic silicon resin mainly contains functional groups such as Si-OH, Si-OR, Si-OCOR and the like, and the groups can be further condensed and crosslinked into a solid product under the action of heating and a catalyst. The addition type organic silicon impregnating varnish has the advantages that the lacquer base silicon resin exists in a liquid state, is dissolved without any organic solvent, does not contain organic solvent, has mild curing condition, and has excellent internal dryness, thermal conductivity, corona resistance, thermal shock resistance and the like, and the process is characterized in that: when the resin is cured into a film, low molecular substances are not removed, air bubbles and sand holes are not generated, the electrical performance is not influenced, and the resin is pollution-free, and belongs to an environment-friendly insulating impregnating resin product. However, compared with the condensation impregnating varnish, the synthesis process is complex, the cost is relatively high, and the condensation impregnating varnish generally needs to be composed of a base resin, a cross-linking agent, a reactive diluent, a platinum complex catalyst and an inhibitor. In addition, the silicone impregnating varnish resin which is formed by matching with a platinum catalyst initiation system and takes hydrosilylation curing as a mechanism also has the defects of poor mechanical strength and easy cracking of a silicone material, so that a paint film on the surface of a motor is damaged due to cracking in the application process, the insulating service life of the motor is influenced, and the application field of the silicone resin is limited.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects and shortcomings in the background technology and providing the environment-friendly organic silicon solvent-free impregnating varnish which is high in mechanical strength, not easy to crack after film forming and the preparation method thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the organic silicon solvent-free impregnating varnish comprises four long chains connected to a tetrafunctional silica unit in a molecular chain, and the structural formula of the organic silicon solvent-free impregnating varnish is shown as the formula (1):
wherein R is1、R2、R3…RnAre respectively selected from one of methyl, phenyl, hydroxyl, vinyl and hydrogen;
representing continuation or omission of the molecular chain, and in-Si-O-molecular chain, the remaining bonds on Si are bound by R1To RnIs filled with the group of (1);
the mol weight of the tetrafunctional silica unit in the molecular chain of the organic silicon solvent-free impregnating varnish accounts for 1-10% of the mol weight of the total chain unit.
The organic silicon solvent-free impregnating varnish disclosed by the invention has the advantages that the molecular chain structure contains four long-chain structural units connected to the tetrafunctional silica unit, the cohesion of a paint film after organic silicon resin is cured can be improved, and the organic silicon solvent-free impregnating varnish has the anti-cracking performance. The molar weight of the tetrafunctional silica unit needs to be controlled within the range of the invention, if the molar weight is lower than the range of the invention, the crosslinking density of molecular chains is small, the intermolecular attraction is small, the mechanical strength of the resin after curing is low, and the effect of enhancing mechanical mild cracking resistance cannot be achieved; however, if the content is outside the range of the present invention, the crosslinking density of the molecular chains becomes high, so that the brittleness of the paint film increases and the paint film is also easily cracked.
As a general inventive concept, the present invention also provides a method for preparing the above silicone solventless impregnating varnish, comprising the steps of:
(1) mixing an organic silicon monomer A and an organic silicon monomer B to obtain an initial organic silicon monomer;
(2) adding water and a solvent into a flask;
(3) slowly dripping the initial organic silicon monomer in the step (1) into the flask in the step (2), reacting, then concentrating, and separating out a resin layer;
(4) washing the resin layer separated in the step (3) with water, refluxing and curing to remove a solvent and low-boiling-point substances, measuring the viscosity of the resin by using a rotary viscometer according to the GB/t15022-2009 standard, filtering after meeting the requirement, and discharging to obtain an organic silicon resin prepolymer;
(5) and (3) adding a platinum catalyst (such as a platinum catalyst Kanst and a chloroplatinic acid isopropanol solution) into the organic silicon resin prepolymer obtained in the step (4), carrying out a hydrosilylation reaction shown in the formula (2), and reacting to obtain the organic silicon solvent-free impregnating varnish product.
In the above preparation method, preferably, the structural formula of the organosilicon monomer B in the step (1) is SiRnX4-nWherein R is vinyl or hydrogen, X is a hydrolyzable group, X is at least one of chlorine atom, methoxy and ethoxy, and n is 0, 1, 2 or 3; the organosilicon monomer B is at least one of ethyl orthosilicate, silicon tetrachloride, vinyl trimethoxy silane, vinyl triethoxy silane, butyl orthosilicate, trimethoxy hydrosilane, triethoxy hydrosilane, dimethoxy dihydrosilane, diethoxy dihydrosilane, divinyl dimethoxy silane, divinyl diethoxy silane, trihydrochloro silane, dihydrodichloro silane, divinyl dichloro silane, trihydromethoxy silane, trihydroethoxy silane, trivinyl chlorosilane, trivinyl methoxy silane and trivinyl ethoxy silane.
In the above preparation method, preferably, the organosilicon monomer A in the step (1) is an organosilicon silane monomer containing methyl, phenyl, vinyl and/or hydrosilyl, specifically, the silane coupling agent is at least one of dimethyldichlorosilane, diphenyldimethoxysilane, dimethyldiethoxysilane, diphenyldiethoxysilane, diphenyldichlorosilane, monophenyltrichlorosilane, monophenyltrimethoxysilane, methylphenyldichlorosilane, methylphenyldimethoxysilane, methyltriethoxysilane, methylvinyldichlorosilane, methylvinyldimethoxysilane, tetramethyldivinyldisiloxane, vinyltrimethoxysilane, methylhydrodichlorosilane, methylhydrodiethoxysilane, tetramethyldihydrodisiloxane, phenylhydrogendichlorosilane, methyltrichlorosilane, hexamethyldisiloxane and trimethylchlorosilane.
In the preparation method, preferably, the R/Si value of the starting organosilicon monomer in the step (1) is 1.4-1.8.
In the preparation method, preferably, the addition amount of the water in the step (2) is 1-6 times of the molar amount of the initial organosilicon monomer. Water participates in hydrolysis in the reaction process and can be used for dissolving byproducts such as hydrogen chloride, methanol or ethanol and the like obtained by hydrolysis, the adding amount of the water needs to be controlled within the range of the invention, otherwise, the reaction can not be smoothly carried out.
In the above preparation method, preferably, the solvent in the step (2) is at least one of toluene, xylene, cycloalkane, halogenated hydrocarbon, ethyl acetate and butyl acetate; the adding amount of the solvent is 1-4 times of the molar amount of the initial organic silicon monomer.
In the preparation method, preferably, the dropwise adding reaction in the step (3) is carried out at a temperature of 5-70 ℃ for 3-6 hours.
In the preparation method, preferably, the temperature of the reflux curing process in the step (4) is 80-120 ℃, and the time is 2-5 hours.
Compared with the prior art, the invention has the advantages that:
(1) the organic silicon solvent-free impregnating varnish disclosed by the invention contains four long chains connected to a tetrafunctional silica unit in a molecular chain, and is formed in the synthetic process or the curing process of an organic silicon prepolymer by introducing an organic silicon monomer B; when n is 0, the structural formula of the organosilicon monomer B is SiX4Hydrolyzing the resulting product to form a tetrafunctional siloxy unit to obtain a silicone solventless impregnation product containing four long chains linked to the tetrafunctional siloxy unit as shown in formula (1)Painting; when n is 1, 2 or 3, the introduction of the organosilicon monomer B reserves a silicon vinyl group or a silicon hydrogen group in the molecular chain of the organosilicon prepolymer, and the organosilicon solvent-free impregnating varnish containing four long-chain structures connected with tetrafunctional silica units shown in the formula (1) can be obtained through a hydrosilylation reaction during later-stage curing; and when n is 1, 2 or 3, because X groups and R groups exist in the system at the same time, the X groups are cohydrolyzed with other silane monomers in the early stage, and the R groups are subjected to hydrosilylation reaction during later curing, so that the obtained resin has more reasonable viscosity, the cured paint film has higher cohesive force and high mechanical strength, and is not easy to crack.
(2) The impregnating varnish of the invention has no low molecular weight substance coming off when curing to form a film, does not influence the electrical performance, has no pollution, and simultaneously has good electrical performance and mechanical performance.
(3) The preparation method has the advantages of simple process, convenient operation, short production period and high efficiency.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a photograph of a copper sheet after impregnation with the silicone solventless impregnating varnish of example 1 of the present invention;
FIG. 2 is a photograph of a copper sheet after impregnation of the copper sheet with the silicone solvent-free impregnating varnish of comparative example 1 according to the present invention;
FIG. 3 is a photograph of a paint film formed on the surface of an object to be impregnated after the silicone solvent-free impregnating varnish of example 1 of the present invention is cured;
FIG. 4 is a photograph of a paint film formed on the surface of an object to be impregnated after the silicone solvent-free impregnating varnish of comparative example 1 of the present invention was cured.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the preparation method of the organic silicon solvent-free impregnating varnish comprises the following steps:
(1) taking monomers of monophenyl trichlorosilane, dimethyl dichlorosilane, diphenyl dimethoxysilane, methyl vinyl dimethoxysilane, methyl hydrogen dichlorosilane, hexamethyldisiloxane and ethyl orthosilicate, determining the proportion according to the R/Si value of 1.65, and mixing to obtain an initial organic silicon monomer; (2) adding 5 times of water and 3 times of toluene solvent by mol of the initial organic silicon monomer into a flask; (3) slowly dripping an initial organic silicon monomer into a flask with quick stirring at the temperature of 5-60 ℃, dripping hydrolysis reaction for 4 hours, concentrating, and separating out a resin layer; (4) washing the separated resin layer with water, then refluxing and curing for 4 hours at 80-120 ℃ to obtain a hydrolyzed prepolymer, removing the solvent and low-boiling-point substances, measuring the viscosity of the resin to reach the required viscosity, filtering, and discharging to obtain an organic silicon resin prepolymer; (5) adding a platinum catalytic inhibitor into the organic silicon resin prepolymer, and reacting to obtain the organic silicon solvent-free impregnating varnish product.
The molecular chain of the silicone solvent-free impregnating varnish product prepared in the embodiment contains four long chains connected with tetrafunctional silica units as shown in formula (1), wherein R is1、R2、R3…RnAre respectively selected from one of methyl, phenyl, hydroxyl, vinyl and hydrogen;
representing continuation or omission of the molecular chain, and in-Si-O-molecular chain, the remaining bonds on Si are bound by R1To RnIs filled with the groups in (1). The molar amount of the tetrafunctional silica units in the molecular chain of the silicone solvent-free impregnating varnish accounts for 5.5 percent of the molar amount of the total chain units.
Example 2:
the preparation method of the organic silicon solvent-free impregnating varnish comprises the following steps:
(1) taking monomers of mono-phenyl trichlorosilane, methyl triethoxysilane, dimethyl dichlorosilane, diphenyl dimethoxysilane, methyl vinyl dimethoxysilane, methyl hydrogen diethoxysilane, hexamethyldisiloxane and vinyl triethoxysilane, determining the proportion according to the R/Si value of 1.72, and mixing to obtain an initial organic silicon monomer; (2) adding 4 times of water and 2 times of xylene solvent of the molar amount of the initial organic silicon monomer into a flask; (3) slowly dripping an initial organic silicon monomer into a flask with quick stirring at the temperature of 5-60 ℃, dripping hydrolysis reaction for 4 hours, concentrating, and separating out a resin layer; (4) washing the separated resin layer with water, then refluxing and curing for 4 hours at 80-120 ℃ to obtain a hydrolyzed prepolymer, removing the solvent and low-boiling-point substances, measuring the viscosity of the resin to reach the required viscosity, filtering, and discharging to obtain an organic silicon resin prepolymer; (5) adding a platinum catalytic inhibitor into the organic silicon resin prepolymer, and reacting to obtain the organic silicon solvent-free impregnating varnish product.
The molecular chain of the silicone solvent-free impregnating varnish product prepared in the embodiment contains four long chains connected with tetrafunctional silica units as shown in formula (1), wherein R is1、R2、R3…RnAre respectively selected from one of methyl, phenyl, hydroxyl, vinyl and hydrogen;
representing continuation or omission of the molecular chain, and in-Si-O-molecular chain, the remaining bonds on Si are bound by R1To RnIs filled with the groups in (1). The organic silicon is solvent-freeThe molar amount of the tetrafunctional silica units in the molecular chain of the agent impregnating varnish accounts for 8 percent of the molar amount of the total chain unit.
Example 3:
the preparation method of the organic silicon solvent-free impregnating varnish comprises the following steps:
(1) taking monomers of monophenyl trimethoxy silane, dimethyl dichlorosilane, methyl phenyl dimethoxy silane, methyl vinyl dimethoxy silane, methyl hydrogen diethoxy silane, hexamethyldisiloxane, divinyl dichlorosilane and trimethoxy hydrosilane, determining the mixture ratio according to the R/Si value of 1.58, and mixing to obtain an initial organosilicon monomer; (2) adding 6 times of water and 4 times of mixed solvent of toluene and ethyl acetate by mol of the initial organic silicon monomer into a flask; (3) slowly dripping an initial organic silicon monomer into a flask with rapid stirring at the temperature of 5-62 ℃, dripping hydrolysis reaction for 4 hours, then concentrating, and separating out a resin layer; (4) washing the separated resin layer with water, then refluxing and curing for 4 hours at 80-120 ℃ to obtain a hydrolyzed prepolymer, removing the solvent and low-boiling-point substances, measuring the viscosity of the resin to reach the required viscosity, filtering, and discharging to obtain an organic silicon resin prepolymer; (5) adding a platinum catalytic inhibitor into the organic silicon resin prepolymer, and reacting to obtain the organic silicon solvent-free impregnating varnish product.
The molecular chain of the silicone solvent-free impregnating varnish product prepared in the embodiment contains four long chains connected with tetrafunctional silica units as shown in formula (1), wherein R is1、R2、R3…RnAre respectively selected from one of methyl, phenyl, hydroxyl, vinyl and hydrogen;
representing continuation or omission of the molecular chain, and in-Si-O-molecular chain, the remaining bonds on Si are bound by R1To RnIs filled with the groups in (1). The mol amount of the tetrafunctional silica unit in the molecular chain of the silicone solvent-free impregnating varnish accounts for 3 percent of the mol amount of the total chain unit.
Comparative example 1:
a preparation method of organic silicon solvent-free impregnating varnish comprises the following steps:
(1) taking monophenyl trichlorosilane, dimethyldichlorosilane, diphenyl dimethoxysilane, methyl vinyl dimethoxysilane, methyl hydrogen dichlorosilane and hexamethyldisiloxane, determining the proportion according to the R/Si value of 1.7, and mixing to obtain an initial organic silicon monomer; (2) adding 5 times of water and 3 times of toluene solvent by mol of the initial organic silicon monomer into a flask; (3) slowly dripping an initial organic silicon monomer into a flask with quick stirring at the temperature of 5-60 ℃, dripping hydrolysis reaction for 4 hours, concentrating, and separating out a resin layer; (4) washing the separated resin layer with water, then refluxing and curing for 4 hours at 80-120 ℃ to obtain a hydrolyzed prepolymer, removing the solvent and low-boiling-point substances, measuring the viscosity of the resin to reach the required viscosity, filtering, and discharging to obtain an organic silicon resin prepolymer; (5) adding a platinum catalytic inhibitor into the organic silicon resin prepolymer, and reacting to obtain the organic silicon solvent-free impregnating varnish product.
The mechanical strength of the silicone solvent-free impregnating varnish products prepared in inventive examples 1 to 3 and comparative example 1 was tested, and the test results are shown in table 1, and it can be seen from table 1 that the mechanical properties of the silicone solvent-free impregnating varnish products of inventive examples 1 to 3 are significantly improved as compared to the comparative example.
TABLE 1 comparative data on mechanical Strength of Silicone solventless impregnating varnish products in examples 1-3 and comparative example 1
| NO. | Item | Example 1 | Example 2 | Example 3 | Comparative example 1 |
| 1 | Adhesive Strength (MPa) | 78.5 | 81.2 | 77.9 | 69.4 |
| 2 | Tensile Strength (MPa) | 18.2 | 17.8 | 18.1 | 15.2 |
| 3 | Flexural Strength (MPa) | 29.4 | 30.6 | 30.2 | 25.6 |
Taking the organic silicon solvent-free impregnating varnish in the embodiment 1 of the invention and the comparative example 1 to respectively cure and impregnate the copper sheet, wherein the photo of the copper sheet after impregnating the copper sheet by using the impregnating varnish in the embodiment 1 is shown in figure 1, and the photo of a paint film formed on the surface of an impregnated object after curing is shown in figure 3; the photo of the copper sheet after the copper sheet is impregnated with the impregnating varnish in the comparative example 1 is shown in FIG. 2, and the photo of the paint film formed on the surface of the impregnated object after curing is shown in FIG. 4; comparing fig. 1 with fig. 2, and fig. 3 with fig. 4, it can be seen that the paint film of comparative example 1 is clearly cracked, while the paint film of example 1 is not cracked, which indicates that the silicone solvent-free impregnating varnish of the present invention has higher cohesion of the paint film after curing and is not easy to crack.
Claims (5)
1. A preparation method of organic silicon solvent-free impregnating varnish comprises the following steps that the molecular chain of the organic silicon solvent-free impregnating varnish contains four long chains connected with a tetrafunctional silica unit, and the structural formula of the organic silicon solvent-free impregnating varnish is shown as a formula (1):
wherein R is1、R2、R3…RnAre respectively selected from one of methyl, phenyl, hydroxyl, vinyl and hydrogen;
representing continuation or omission of the molecular chain, and in-Si-O-molecular chain, the remaining bonds on Si are bound by R1To RnIs filled with the group of (1);
the mol weight of the tetrafunctional silica unit in the molecular chain of the organic silicon solvent-free impregnating varnish accounts for 1-10% of the mol weight of the total chain unit;
the preparation method of the organic silicon solvent-free impregnating varnish is characterized by comprising the following steps:
(1) mixing an organic silicon monomer A and an organic silicon monomer B to obtain an initial organic silicon monomer;
(2) adding water and a solvent into a flask;
(3) slowly dripping the initial organic silicon monomer in the step (1) into the flask in the step (2), reacting, then concentrating, and separating out a resin layer;
(4) washing the resin layer separated in the step (3) with water, refluxing and curing, measuring the viscosity of the resin, filtering after meeting the requirement, and discharging to obtain an organic silicon resin prepolymer;
(5) adding a platinum catalyst into the organic silicon resin prepolymer obtained in the step (4), and reacting to obtain an organic silicon solvent-free impregnating varnish product;
the structural formula of the organic silicon monomer B in the step (1) is SiRnX4-nWherein R is vinyl orA hydrogen radical, X is a hydrolysable group, X is at least one of a chlorine atom, a methoxy group and an ethoxy group, and n is 0, 1, 2 or 3; the organosilicon monomer B is at least one of ethyl orthosilicate, silicon tetrachloride, vinyl trimethoxy silane, vinyl triethoxy silane, butyl orthosilicate, trimethoxy silane, triethoxy silane, divinyl dichlorosilane, trivinyl chlorosilane and trivinyl ethoxy silane;
the organosilicon monomer A in the step (1) is an organosilicon silane monomer containing methyl, phenyl, vinyl and/or hydrosilyl, and specifically is at least one of dimethyldichlorosilane, diphenyldimethoxysilane, dimethyldiethoxysilane, diphenyldiethoxysilane, diphenyldichlorosilane, monophenyltrichlorosilane, monophenyltrimethoxysilane, methylphenyldichlorosilane, methylphenyldimethoxysilane, methyltriethoxysilane, methylvinyldichlorosilane, methylvinyldimethoxysilane, tetramethyldivinyldisiloxane, vinyltrimethoxysilane, methylhydrodichlorosilane, methylhydrodiethoxysilane, tetramethyldihydrodisiloxane, phenyldichlorosilane, methyltrichlorosilane, hexamethyldisiloxane and trimethylchlorosilane;
the R/Si value of the initial organic silicon monomer in the step (1) is 1.4-1.8.
2. The preparation method according to claim 1, wherein the water is added in the step (2) in an amount of 1 to 6 times the molar amount of the starting organosilicon monomer.
3. The method according to claim 1, wherein the solvent in the step (2) is at least one of toluene, xylene, cycloalkane, halogenated hydrocarbon, ethyl acetate, and butyl acetate; the adding amount of the solvent is 1-4 times of the molar amount of the initial organic silicon monomer.
4. The preparation method according to claim 1, wherein the dropwise addition reaction in the step (3) is carried out at a temperature of 5 to 70 ℃ for 3 to 6 hours.
5. The preparation method according to claim 1, wherein the temperature of the reflux curing process in the step (4) is 80 to 120 ℃ and the time is 2 to 5 hours.
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| C级无溶剂有机硅树脂性能及应用;陈宗旻等;《上海大中型电机 3》;20021231(第3期);33-36 * |
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