CN111592766A - Preparation method of high-insulation solvent-free silicone resin for composite insulator - Google Patents
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- CN111592766A CN111592766A CN202010430607.9A CN202010430607A CN111592766A CN 111592766 A CN111592766 A CN 111592766A CN 202010430607 A CN202010430607 A CN 202010430607A CN 111592766 A CN111592766 A CN 111592766A
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/10—Block- or graft-copolymers containing polysiloxane sequences
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/045—Polysiloxanes containing less than 25 silicon atoms
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/44—Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
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- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The invention provides a preparation method of high-insulation solvent-free silicone resin for a composite insulator, which relates to the field of organic composite insulators. By introducing the vinyl group and adopting a hydrosilylation mode, secondary vulcanization is avoided, and the process steps and energy consumption are reduced. The toughness of the product is greatly improved by introducing the propyl group.
Description
Technical Field
The invention relates to the field of organic composite insulators, in particular to a preparation method of high-insulation solvent-free silicone resin for a composite insulator.
Background
The organic composite insulator is a new generation product of power transmission and transformation equipment with the advantages of small volume, light weight, high strength, pollution resistance, convenient cleaning and maintenance and the like. The high-temperature vulcanized silicone rubber composite insulator has excellent hydrophobicity, hydrophobicity migration, electromechanical properties and economy, has better tracking resistance and electric corrosion resistance, and gradually replaces the early materials such as epoxy resin, ethylene propylene rubber, room-temperature silicone rubber and the like.
The patent numbers are: the document CN201010591839.9 discloses a silicone rubber for composite insulators and a preparation method thereof, which is to obtain a finished insulator by secondary vulcanization of auxiliaries such as methyl vinyl silicone rubber, hydrogen-containing silicone oil, peroxide vulcanizing agent and the like under high temperature conditions.
The patent numbers are: the document CN200910110891.5 discloses a high temperature resistant composite silicone rubber insulator formula, which vulcanizes methyl vinyl silicone rubber, hydrogen-containing silicone oil, platinum complex and other additives at high temperature to obtain a finished insulator, and improves the high temperature resistance of the finished product by introducing the cerium-containing silicone heat resistant additive.
At present, most composite insulators are prepared by high-temperature vulcanized silicone rubber, but the high-temperature vulcanized silicone rubber still has the disadvantages of common stain resistance after long-time use, easy occurrence of pollution flashover accidents, common radiation resistance, poor mechanical properties such as tensile strength and tear strength and the like, and easy occurrence of aging, so that the service life of products is shortened.
Disclosure of Invention
The invention aims to provide a preparation method of high-insulation solvent-free silicone resin for a composite insulator, which aims to solve the general technical problems of poor tear strength and long-term use antifouling performance of the composite insulator.
In order to solve the technical problems, the invention adopts the following technical scheme: a preparation method of high-insulation solvent-free silicone resin for a composite insulator comprises the following preparation steps:
s1, placing water, a solvent and a catalyst in a reaction kettle, controlling the material temperature below 20 ℃, gradually dropwise adding a mixture of propyl trimethoxy silane, dimethyl dimethoxy silane and methyl vinyl trimethoxy silane, stirring for hydrolysis reaction for 1 hour, heating to 70 ℃, carrying out hydrolytic condensation for 3-5 hours, and removing low molecular substances such as the solvent under reduced pressure to obtain an intermediate product A, wherein the intermediate product A is trapezoidal propyl vinyl silsesquioxane containing 1-5% of hydroxyl and is an incompletely condensed trapezoidal structure oligomer;
s2, mixing vinyl-terminated polymethylvinylsiloxane and A in S1, carrying out negative pressure polycondensation for 3 hours at 130-150 ℃ in a reaction kettle, cooling to 50 ℃ after the reaction is finished, adding hexamethyldisilazane, stirring for 1 hour, and removing low molecular substances under reduced pressure to obtain an intermediate product B;
s3, preparing the intermediate product B in the S2, a reinforcing agent, ceramic powder and a catalyst into a component A according to the mass ratio of 100: 15-30: 40-60: 0.2-1; preparing the product B, the reinforcing agent, the ceramic powder, the cross-linking agent and the inhibitor in the S2 into a component B according to the mass ratio of 100: 15-30: 40-60: 5-15: 0.02-0.1; in later use, A, B components are uniformly mixed according to the proportion of 1:1, and the mixture is cured at high temperature to obtain a finished product.
Preferably, in S1, the solvent is one or more of ethanol, methanol, and isopropanol.
Preferably, in S1, the hydrolysis catalyst is one or a mixture of acetic acid and formic acid.
Preferably, in S2, the conditions for removing low molecular weight substances under reduced pressure are: 120 deg.C/0.093 MPa.
Preferably, in the S3, the catalyst is one or two of chloroplatinic acid and Karstedt catalyst.
Preferably, in S3, the inhibitor is one or more of 2-ethynyl butan-2-ol, 1-ethynyl-1-cyclopentanol and 1-ethynyl-1-cyclohexanol.
Preferably, in S3, the curing conditions of the finished product are as follows: 130 ℃ for 30 min.
The invention has the beneficial effects that:
the resin structure in the invention is vinyl propyl silicone resin structure, the silicone resin is a bigger three-dimensional structure crosslinked by three-dimensional structure molecules, compared with silicone rubber which is vulcanized and crosslinked into a three-dimensional structure after being reinforced by molecules with a linear structure, the silicone rubber has bigger crosslinking density, and better strength, stain resistance and aging resistance. By introducing the vinyl group and adopting a hydrosilylation mode, secondary vulcanization is avoided, and the process steps and energy consumption are reduced. The toughness of the product is greatly improved by introducing the propyl group.
Drawings
FIG. 1 is a flow chart of the preparation method of the present invention.
FIG. 2 is a schematic diagram of a production method of the present invention.
Detailed Description
In order to make the technical means, the original characteristics, the achieved purposes and the effects of the invention easily understood, the invention is further described below with reference to the specific embodiments and the attached drawings, but the following embodiments are only the preferred embodiments of the invention, and not all embodiments. Based on the embodiments in the implementation, other embodiments obtained by those skilled in the art without any creative efforts belong to the protection scope of the present invention.
The detection method in the following examples is as follows:
the Shore hardness test is carried out according to GB/T531.1-2008; the tensile strength and the elongation at break are tested according to GB/T528-2009; the tear strength is tested according to GB/T529-2008; heat ageing tests were carried out in accordance with GB/T3512-2001.
Specific embodiments of the present invention are described below with reference to the accompanying drawings.
Example 1:
adding 260kg of deionized water and 600kg of ethanol into a reaction kettle, adding 820kg of propyl trimethoxy silane, 116kg of vinyl dimethoxy silane and 134kg of dimethyl dimethoxy silane into a dropwise adding tank, starting stirring, uniformly stirring, dropwise adding a silane mixture, keeping the temperature below 20 ℃ during dropwise adding, keeping the temperature for reaction for one hour, heating to 80 ℃, keeping the temperature for reflux for 4 hours, heating and reducing the pressure under the conditions that the temperature is 100 ℃, the vacuum degree is-0.093 MPa, and removing a solvent, a catalyst and other low-boiling-point substances to obtain 661kg of trapezoidal propyl vinyl silsesquioxane;
661kg of trapezoidal propyl vinyl semi-siloxane and 660kg of terminal vinyl polymethylvinylsiloxane are added into a reaction kettle, the mixture is uniformly stirred, high-temperature negative-pressure dehydration condensation reaction is carried out, the reaction conditions are that the temperature is 150 ℃, the vacuum degree is-0.093 MPa, the temperature is reduced to 50 ℃ after the reaction is carried out for 2 hours, 80kg of hexamethyldisilazane is added, the mixture is stirred for 1 hour, low molecular substances are removed under reduced pressure, the conditions are that the temperature is 100 ℃, the vacuum degree is-0.093 MPa, and 1350kg of products are obtained.
Preparing a component A from a propyl vinyl MDT resin prepolymer, fumed silica, ceramic powder and a catalyst with platinum content of 3000ppm Karstedt according to a mass ratio of 100: 20: 50: 0.5; preparing propyl vinyl MDT resin prepolymer, fumed silica, ceramic powder, hydrogen-containing silicone oil with the hydrogen content of 1.58% and 1-ethynyl-1-cyclohexanol into component B according to the mass ratio of 100: 20: 50: 8: 0.05; uniformly mixing the component A and the component B according to the mass ratio of 1:1, defoaming in vacuum, curing for 2 hours at 130 ℃ to prepare a dumbbell-shaped test sample for testing, and detecting to obtain detection data shown in Table 1:
TABLE 1
Example 2:
(1) 260kg of deionized water and 600kg of ethanol are added into a reaction kettle, 820kg of propyl trimethoxy silane, 116kg of vinyl dimethoxy silane and 134kg of dimethyl dimethoxy silane are added into a dripping tank, stirring is started, and after uniform stirring, a silane mixture is dripped. The temperature was kept below 20 ℃ during the dropwise addition. After the reaction was carried out for one hour under heat preservation, the temperature was raised to 80 ℃ and the reflux was carried out for 4 hours under heat preservation, and the solvent, the catalyst and other low-boiling components were removed by heating under reduced pressure (temperature 100 ℃ C., degree of vacuum-0.093 MPa) to obtain 661kg of ladder-propyl vinyl silsesquioxane.
(2) 661kg of trapezoidal propyl vinyl semi-siloxane and 990kg of terminal vinyl polymethylvinylsiloxane are added into a reaction kettle, the mixture is uniformly stirred, high-temperature negative-pressure dehydration condensation reaction is carried out (the temperature is 150 ℃, the vacuum degree is-0.093 MPa), the temperature is reduced to 50 ℃ after the reaction is carried out for 2h, 80kg of hexamethyldisilazane is added, the mixture is stirred for 1h, the low molecular weight substances are removed under reduced pressure (the temperature is 100 ℃, the vacuum degree is-0.093 MPa), and 1350kg of products are obtained.
(3) Preparing a component A from a propyl vinyl MDT resin prepolymer, fumed silica, ceramic powder and a catalyst with platinum content of 3000ppm Karstedt according to a mass ratio of 100: 20: 50: 0.5; preparing propyl vinyl MDT resin prepolymer, fumed silica, ceramic powder, hydrogen-containing silicone oil with the hydrogen content of 1.58% and 1-ethynyl-1-cyclohexanol into component B according to the mass ratio of 100: 20: 50: 8: 0.05; uniformly mixing the component A and the component B according to the mass ratio of 1:1, defoaming in vacuum, curing for 2 hours at 130 ℃ to prepare a dumbbell type test sample for testing, and detecting to obtain detection data shown in Table 2:
TABLE 2
Example 3:
(1) 260kg of deionized water and 600kg of ethanol are added into a reaction kettle, 820kg of propyl trimethoxy silane, 116kg of vinyl dimethoxy silane and 134kg of dimethyl dimethoxy silane are added into a dripping tank, stirring is started, and after uniform stirring, a silane mixture is dripped. The temperature was kept below 20 ℃ during the dropwise addition. After the reaction was carried out for one hour under heat preservation, the temperature was raised to 80 ℃ and the reflux was carried out for 4 hours under heat preservation, and the solvent, the catalyst and other low-boiling components were removed by heating under reduced pressure (temperature 100 ℃ C., degree of vacuum-0.093 MPa) to obtain 661kg of ladder-propyl vinyl silsesquioxane.
(2) 661kg of trapezoidal vinyl propyl hemisiloxane and 660kg of terminal vinyl polymethylvinylsiloxane are added into a reaction kettle, the mixture is uniformly stirred, high-temperature negative-pressure dehydration condensation reaction is carried out (the temperature is 150 ℃, the vacuum degree is-0.093 MPa), the temperature is reduced to 50 ℃ after the reaction is carried out for 2h, 80kg of hexamethyldisilazane is added, the mixture is stirred for 1h, the low molecular weight substances are removed under reduced pressure (the temperature is 100 ℃, the vacuum degree is-0.093 MPa), and 1350kg of products are obtained.
(3) Preparing a component A from a propyl vinyl MDT resin prepolymer, fumed silica, ceramic powder and a catalyst with platinum content of 3000ppm Karstedt according to a mass ratio of 100: 30: 60: 0.5; preparing propyl vinyl MDT resin prepolymer, fumed silica, ceramic powder, hydrogen-containing silicone oil with the hydrogen content of 1.58% and 1-ethynyl-1-cyclohexanol into component B according to the mass ratio of 100: 30: 60: 8: 0.05; uniformly mixing the component A and the component B according to the mass ratio of 1:1, defoaming in vacuum, curing for 2 hours at 130 ℃ to prepare a dumbbell-shaped test sample for testing, and detecting to obtain detection data shown in Table 3:
TABLE 3
Comparing example 1 with example 2, 660kg and 990kg of vinyl-terminated polymethylvinylsiloxane are respectively added in the preparation process, and the detection result of the comparison finished product is as follows: the finished product obtained by adding 660kg of terminal vinyl polymethylvinylsiloxane has higher Shore hardness, higher tensile strength, the same elongation at break, slightly higher tear strength and higher retention rate of thermal aging tensile strength, so the finished resin product prepared by the method in the embodiment 1 has higher comprehensive quality, better strength, better pollution resistance and better aging resistance under the heating condition;
comparing the embodiment 1 with the embodiment 3, in the preparation process, the propyl vinyl MDT resin prepolymer, the fumed silica, the ceramic powder, the hydrogen-containing silicone oil with the hydrogen content of 1.58% and the 1-ethynyl-1-cyclohexanol are configured according to the proportion of 100: 20: 50: 8: 0.05 in the embodiment 1, and the proportion in the embodiment 3 is 100: 30: 60: 8: 0.05, and in the detection result, compared with the embodiment 3, the embodiment 1 has slightly lower Shore hardness, slightly lower tensile strength, slightly lower elongation at break, higher tear strength and higher retention rate of thermal aging tensile strength, and the retention rates of tear strength and thermal aging tensile strength are main standards for measuring the strength and aging resistance of the finished resin product, and the higher tear strength and the higher retention rate of thermal aging tensile strength are the better quality, so the comprehensive comparison shows that the preparation method in the embodiment 1 is the best preparation method, the resin with better strength, stain resistance and aging resistance can be prepared.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the preferred embodiments of the present invention are described in the above embodiments and the description, and are not intended to limit the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. A preparation method of high-insulation solvent-free silicone resin for a composite insulator is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
s1, placing water, a solvent and a catalyst in a reaction kettle, controlling the material temperature below 20 ℃, gradually dropwise adding a mixture of propyl trimethoxy silane, dimethyl dimethoxy silane and methyl vinyl trimethoxy silane, stirring for hydrolysis reaction for 1 hour, heating to 70 ℃, carrying out hydrolytic condensation for 3-5 hours, and removing low molecular substances such as the solvent under reduced pressure to obtain an intermediate product A, wherein the intermediate product A is trapezoidal propyl vinyl silsesquioxane containing 1-5% of hydroxyl and is an incompletely condensed trapezoidal structure oligomer;
s2, mixing vinyl-terminated polymethylvinylsiloxane and A in S1, carrying out negative pressure polycondensation for 3 hours at 130-150 ℃ in a reaction kettle, cooling to 50 ℃ after the reaction is finished, adding hexamethyldisilazane, stirring for 1 hour, and removing low molecular substances under reduced pressure to obtain an intermediate product B;
s3, preparing the intermediate product B in the S2, a reinforcing agent, ceramic powder and a catalyst into a component A according to the mass ratio of 100: 15-30: 40-60: 0.2-1; preparing the product B, the reinforcing agent, the ceramic powder, the cross-linking agent and the inhibitor in the S2 into a component B according to the mass ratio of 100: 15-30: 40-60: 5-15: 0.02-0.1; in later use, A, B components are uniformly mixed according to the proportion of 1:1, and the mixture is cured at high temperature to obtain a finished product.
2. The method for preparing the high-insulation solvent-free silicone resin for the composite insulator according to claim 1, wherein in S1, the solvent is one or a mixture of ethanol, methanol and isopropanol.
3. The method for preparing the high-insulation solvent-free silicone resin for the composite insulator according to claim 1, wherein in S1, the hydrolysis catalyst is one or a mixture of acetic acid and formic acid.
4. The method for preparing the high-insulation solvent-free silicone resin for the composite insulator according to claim 1, wherein in the step S2, the conditions for removing low molecular substances under reduced pressure are as follows: 120 deg.C/0.093 MPa.
5. The method for preparing the high-insulation solvent-free silicone resin for the composite insulator according to claim 1, wherein in S3, the catalyst is one or two of chloroplatinic acid and Karstedt catalyst.
6. The method for preparing the high-insulation solvent-free silicone resin for the composite insulator according to claim 1, wherein in S3, the inhibitor is one or more of 2-ethynylbutan-2-ol, 1-ethynyl-1-cyclopentanol and 1-ethynyl-1-cyclohexanol.
7. The method for preparing the high-insulation solvent-free silicone resin for the composite insulator according to claim 1, wherein in S3, the curing conditions of the finished product are as follows: 130 ℃ for 30 min.
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