CN112143006A - Method for preparing epoxy glass cloth insulating cylinder - Google Patents

Method for preparing epoxy glass cloth insulating cylinder Download PDF

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Publication number
CN112143006A
CN112143006A CN202011084156.4A CN202011084156A CN112143006A CN 112143006 A CN112143006 A CN 112143006A CN 202011084156 A CN202011084156 A CN 202011084156A CN 112143006 A CN112143006 A CN 112143006A
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glass cloth
insulating cylinder
epoxy resin
oven
epoxy
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CN112143006B (en
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潘德忠
徐晓风
吴斌
顾健峰
徐庆华
马俊锋
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Suzhou Taihu Electric Advanced Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/24Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2363/00Characterised by the use of epoxy resins; Derivatives of epoxy resins
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/04Ingredients characterised by their shape and organic or inorganic ingredients
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2237Oxides; Hydroxides of metals of titanium
    • C08K2003/2241Titanium dioxide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/14Glass
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/22Expanded, porous or hollow particles
    • C08K7/24Expanded, porous or hollow particles inorganic
    • C08K7/26Silicon- containing compounds

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Medicinal Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Epoxy Resins (AREA)
  • Insulating Bodies (AREA)
  • Reinforced Plastic Materials (AREA)

Abstract

The invention relates to a method for preparing an epoxy glass cloth insulating cylinder, which comprises the following steps: firstly, putting the glass cloth into an oven to be baked for more than 24 hours; and (II) uniformly mixing an inorganic filler and a dispersing agent in a high-speed stirrer to prepare white slurry, wherein the inorganic filler is titanium dioxide, calcium carbonate and fumed silica according to a mass ratio of 1-3: 1: 1-3; thirdly, winding the alkali-free glass cloth on a mould covered with a high-temperature film or a mould coated with a release agent by using a cloth winding machine; mixing the white slurry with epoxy resin and the like to prepare epoxy resin prepreg, and uniformly impregnating the epoxy resin prepreg on glass cloth; and (V) curing, taking the mold out of the oven after curing is finished, cooling, and taking the cured epoxy glass cloth insulating cylinder blank off from the mold. The glass cloth insulating cylinder manufactured by the invention has the advantages of withstand voltage of more than 35KV, high mechanical strength, good corrosion resistance, simple process, less equipment investment and low cost.

Description

Method for preparing epoxy glass cloth insulating cylinder
The invention is a divisional application of Chinese invention patent application with application date of 2017, 12 and 5, application number of 201711265271X and name of 'preparation method of epoxy glass cloth insulating cylinder'.
Technical Field
The invention relates to the technical field of thin-wall dry-type transformer insulating materials, in particular to a method for preparing an epoxy glass cloth insulating cylinder.
Background
The dry-type transformer is widely used in places such as local illumination, high-rise buildings, airports, wharf CNC mechanical equipment and the like. With the continuous development of infrastructure construction in China, the usage amount of the composite material is always kept increasing at a high speed. The dry-type transformer has excellent performance and low manufacturing and maintenance cost, and about 50 percent of the existing transformers in China adopt the dry-type transformer, wherein the thin insulation dry-type transformer is developed rapidly. The main insulating material of the thin insulating dry type transformer is mainly an epoxy glass fiber reinforced insulating cylinder and an epoxy glass cloth reinforced insulating cylinder at present. The epoxy glass cloth reinforced insulating cylinder is widely applied because of good insulating property, simple manufacturing process and low cost. However, in the process of manufacturing the epoxy glass cloth insulating cylinder, defects such as surface wrinkles, delamination, bubbles and the like are easy to occur, and the service performance of the epoxy glass cloth insulating cylinder is seriously influenced. These problems severely limited their development, resulting in a significant portion of customers being forced to choose fiberglass reinforced epoxy insulation cartridges.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for preparing an epoxy glass cloth insulating cylinder which has smooth surface, no layering, no air bubbles in the interior, excellent mechanical property, electrical property and heat-conducting property and lower cost.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of an epoxy glass cloth insulating cylinder comprises the following steps:
firstly, putting the glass cloth into an oven, and baking at the temperature of 60-80 ℃;
and (II) uniformly mixing an inorganic filler and a dispersing agent in a high-speed mixer according to the mass ratio of 1: 0.8-3 to prepare white slurry, wherein the inorganic filler is titanium dioxide, calcium carbonate and fumed silica according to the mass ratio of 1-3: 1: 1-3, wherein the particle size of titanium dioxide is 250-350 nm, the particle size of calcium carbonate is 1-10 microns, and the particle size of fumed silica is 20-30 nm;
thirdly, winding the glass cloth on a mould coated with a high-temperature film or a release agent by using a cloth winding machine, wherein the number of winding turns is determined according to the thickness requirement of the insulating cylinder;
fourthly, mixing the white slurry with epoxy resin, a curing agent and a curing accelerator to prepare epoxy resin prepreg, putting the mould subjected to the third step into vacuum impregnation equipment, and uniformly impregnating the epoxy resin prepreg on glass cloth through a vacuum pressure impregnation process;
and (V) placing the mold subjected to the step (IV) into an oven, curing at 140-180 ℃, taking the mold out of the oven after curing is completed, cooling, and taking the cured epoxy glass cloth insulating cylinder blank out of the mold.
Further, in the step (one), the baking time is 24 hours or more, preferably 36 hours or more, and more preferably 48 hours or more. The baking temperature is preferably 60-70 ℃.
Preferably, the alkali-free glass cloth is roving alkali-free glass cloth with single filament fineness of 30-50 dtex.
Preferably, the number of winding turns of the glass cloth is determined according to the following formula:
N=T÷D+3
wherein N is the winding number of the glass cloth; t is the thickness required by the insulating cylinder; d is the thickness of the single-layer glass cloth.
Preferably, in the step (two), the mass ratio of titanium dioxide, calcium carbonate and fumed silica is 2:1: 2.
preferably, in the step (two), the dispersant is a mixture of an organic silicon defoamer and two or more selected from ethyl acetate, butyl acetate and acetone, wherein the mass content of the organic silicon defoamer in the dispersant is 0.5-1.5%. In one embodiment, the silicone defoamer is present in the dispersant in an amount of about 1% by weight. The addition of the defoaming agent effectively prevents the foaming phenomenon in the dipping and curing process and avoids the foaming phenomenon in the insulating cylinder.
Preferably, the silicone defoamer is a silicone modified epoxy resin, such as commercially available shin Etsu ES-1001N.
Preferably, in the step (two), the weight ratio of the inorganic filler to the dispersant is 1: 1 to 3.
According to the invention, the high-temperature film can be a high-temperature polypropylene film, and the release agent can be a commercially available organic silicon release agent.
Preferably, the epoxy resin is hydantoin epoxy resin or bisphenol a epoxy resin or phenolic aldehyde modified bisphenol a epoxy resin. Specifically, the bisphenol A type epoxy resin may be E-51 type or E-44 type. The phenolic-modified bisphenol A epoxy resin is preferably F-51 type or F-44 type.
Preferably, the curing agent is one or two of methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride and methyl nadic anhydride.
Preferably, the curing accelerator is a tertiary amine curing agent such as DMP-30, N-dimethylbenzylamine or an imidazole curing agent such as liquid 2-ethyl-4-methylimidazole.
Preferably, the preparation process of the epoxy resin prepreg comprises the following steps: baking epoxy resin in an oven to reduce the viscosity of the epoxy resin, mixing 40-55 parts of epoxy resin, 35-40 parts of curing agent, 10-25 parts of white slurry and 0.1-0.2 part of curing accelerator according to parts by weight, and dispersing by using a high-speed stirrer to obtain the epoxy resin prepreg. Wherein the baking temperature can be 70-80 ℃, and the stirring dispersion time is 5min for example.
Preferably, the white pulp is prepared by the following steps: and (3) putting the dispersing agent into a stirring barrel of a high-speed stirrer, starting stirring, heating to 50-70 ℃, then sequentially and slowly adding titanium dioxide, calcium carbonate and fumed silica, and stirring at a high speed until the dispersing agent is uniformly dispersed to obtain the titanium dioxide/calcium carbonate/fumed silica.
According to one aspect of the invention, the vacuum pressure impregnation is carried out under the specific process conditions of the pressure of 0.05-0.07 MPa, the impregnation time of 2-4 times, preferably 3 times, and the time of 1-1.5 hours. The control of the pressure in the vacuum impregnation VPI process well solves the problem that the glass cloth is easy to wrinkle, and internal defects are reduced. The pressure control is very important, and the outer surface is easy to be starved due to the overhigh pressure; too low a pressure tends to cause a lack of glue on the inner surface, and also causes too long impregnation times and increased times.
According to another aspect of the present invention, in the step (v), the curing process is: and controlling the rotating speed of the mold in the oven at 20-30 revolutions per minute. The surface sizing material is easy to drop due to the over-high rotating speed, and the sizing material is easy to drop due to the over-low rotating speed, so that the sizing material loss is caused, and the serious quality problem is caused.
According to the invention, in the step (V), the curing is carried out at high temperature and low temperature, the temperature of the oven is controlled to be 160-180 ℃ between 0-40 min, and the temperature of the oven is controlled to be 135-155 ℃ between 40-120 min.
After solidification, the mold is placed at room temperature and cooled for 10-15 min to perform demolding treatment, the insulating cylinder is prone to wrinkling and deformation due to insufficient cooling time, demolding is difficult due to too long cooling time, and the insulating cylinder is prone to damage or damage.
Due to the implementation of the scheme, compared with the prior art, the invention has the following advantages:
the glass cloth insulating cylinder manufactured by the invention has the advantages of withstand voltage of more than 35KV, long-term use at 140-210 ℃ according to different materials, high mechanical strength and good corrosion resistance, and is widely applied to the field of insulation of thin-wall dry type transformers. In addition, the manufacturing method of the insulating cylinder also has the advantages of simple process, less equipment investment, low cost and the like.
Detailed Description
The technical problem to be solved by the invention is to provide a method for preparing an epoxy glass cloth insulating cylinder, so as to prepare the epoxy glass cloth insulating cylinder with smooth surface, no layering, no air bubbles in the interior, excellent mechanical property, electrical property and heat-conducting property and lower cost; in addition, the invention also solves the problems of overlong preparation time and low production efficiency in the prior art, and obviously improves the economic benefit.
The technical scheme adopted by the invention for solving the problems comprises the following steps:
alkali-free glass cloth is selected, and the filament number is 30-50 dtex. And before use, the glass cloth is put into an oven and baked for 24 hours, preferably more than 48 hours at the temperature of 60-80 ℃.
The inorganic filler is made of different materials with different particle sizes, the particle size of titanium dioxide is about 300 nanometers, the particle size of calcium carbonate is about 1 micrometer, the particle size of fumed silica is about 30 nanometers, and the inorganic filler, the titanium dioxide, the calcium carbonate and the fumed silica are mixed according to the mass ratio of 2:1: 2. The three materials exert the following functions: the titanium dioxide has strong covering power and good appearance quality of the product; the calcium carbonate is easy to disperse, and is beneficial to the uniform dispersion of other two materials, and in addition, the price is lower, so that the cost can be reduced; the fumed silica mainly plays a role in improving the heat-conducting property and reinforcing.
The inorganic filler was dispersed in the liquid dispersant in advance and dispersed for 3 hours with a high-speed stirrer to prepare a white slurry. When the epoxy resin prepreg is prepared subsequently, the phenomenon of uneven dispersion can not occur.
The dispersing agent contains the organic silicon defoaming agent, so that foaming in the subsequent epoxy resin impregnation and curing processes can be effectively prevented, and the phenomenon of foaming in the insulating cylinder is avoided.
By adopting a vacuum impregnation VPI process, the vacuum pressure is accurately controlled to be 0.05-0.07 MPa, and the outer surface is easy to be starved of glue due to overhigh pressure; too low a pressure tends to cause a lack of glue on the inner surface and also to cause too long and increased times of impregnation, where pressure control is very important.
The curing process is carried out at high temperature and then at low temperature, the temperature of the oven is controlled to be above 160 ℃ within 0-40 min, and the temperature of the oven is controlled to be 135-155 ℃ within 40-120 min.
When the mold is cured, the rotating speed of the mold is controlled to be 20-30 revolutions per minute, the surface sizing material is easy to fall off due to too high rotating speed, and the sizing material is easy to drip off due to too low rotating speed, so that the sizing material loss is caused, and the serious quality problem is caused.
After solidification, the mold is placed at room temperature and cooled for 10-15 min to perform demolding treatment, the insulating cylinder is prone to wrinkling and deformation due to insufficient cooling time, demolding is difficult due to too long cooling time, and the insulating cylinder is prone to damage or damage.
The inorganic filler used in the invention is made of different materials and is prepared according to the particle size in a grading way, so that the internal stress of the cured insulating cylinder can be greatly reduced, and the delamination and cracking can be prevented; the addition of the white carbon black enhances the heat conductivity coefficient, so that the high-temperature short-time curing of the epoxy resin prepreg becomes possible, the curing time is greatly shortened, and the production efficiency is improved; the addition of the defoaming agent effectively prevents the foaming phenomenon in the dipping and curing processes, so that the foaming phenomenon in the insulating cylinder is solved; the control of the pressure in the vacuum impregnation VPI process well solves the problem that the outer surface is easy to wrinkle, greatly improves the product quality, reduces the workload of post-processing and improves the working efficiency.
The present invention will be described in further detail with reference to specific examples. It is to be understood that these examples are for the purpose of illustrating the general principles, essential features and advantages of the present invention, and the present invention is not limited by the following examples. The implementation conditions used in the examples can be further adjusted according to specific requirements, and the implementation conditions not indicated are generally the conditions in routine experiments. All the raw materials used in the examples are industrial products.
In the embodiment, the glass cloth is roving alkali-free glass cloth without twist, the single-layer thickness is 0.1mm, and the single-fiber fineness is 30-50 dtex.
Example 1
A preparation method of an epoxy glass cloth insulating cylinder comprises the following steps:
(1) and (3) putting the glass cloth into an oven, and baking for more than 48 hours at the temperature of 60 ℃.
(2) 1kg of Xinyue organic silicon modified epoxy resin ES-1001N is added into a mixture consisting of 50 kg of ethyl acetate and 49 kg of butyl acetate, and the mixture is stirred uniformly to prepare the dispersing agent.
(3) 40 kg of titanium dioxide with the particle size of about 300 nm, 20 kg of calcium carbonate with the particle size of about 1 micron and 40 kg of fumed silica with the particle size of about 30 nm are weighed.
(4) Heating 100 kg of dispersing agent to 60 ℃, slowly adding the weighed titanium dioxide, calcium carbonate and fumed silica into the dispersing agent in sequence, and stirring for about 3 hours at about 60 ℃ by using a high-speed stirrer to prepare white slurry.
(5) Winding the glass cloth on the die covered with the high-temperature polypropylene film by using a cloth winding machine, winding the glass cloth on the die by using the cloth winding machine, and winding for 33 circles.
(6) Heating E-51 bisphenol A epoxy resin at 80 ℃ for 4 hours; weighing 50 kg of E-51 bisphenol A epoxy resin, 35 kg of methyl tetrahydrophthalic anhydride, 15 kg of white slurry and 0.2 kg of DMP-30, and uniformly mixing by using a high-speed mixer to prepare the epoxy resin prepreg.
(7) Pouring the epoxy resin prepreg into VPI equipment, controlling the temperature in the equipment to be about 40 ℃, and putting the mould wound with the glass cloth into vacuum impregnation equipment. The vacuum pressure is controlled to be about 0.06MPa, the dipping times are controlled to be 3 times, and the time is controlled to be about 1 hour.
(8) And (3) raising the temperature of the oven to 170 ℃, putting the mould into the oven, curing for 40min at the rotation speed of 20 r/min and at the temperature of 170 +/-5 ℃, adjusting the temperature of the oven to 150 +/-5 ℃, and continuously curing for 80 min.
(9) And after the curing is finished, taking the mold out of the oven, standing at room temperature for cooling for 15min, taking out the cured glass cloth epoxy resin insulating cylinder blank by using a demolding machine, and taking the cured glass cloth epoxy resin insulating cylinder blank off the mold.
(10) And cutting, stripping and polishing according to the specified size in sequence, and processing to the specified size.
Example 2
A preparation method of an epoxy glass cloth insulating cylinder comprises the following steps:
(1) and (3) putting the glass cloth into an oven, and baking for more than 36 hours at the temperature of 70 ℃.
(2) 1kg of Xinyue organic silicon modified epoxy resin ES-1001N is added into a mixture consisting of 50 kg of ethyl acetate and 49 kg of butyl acetate, and the mixture is stirred uniformly to prepare the dispersing agent.
(3) 40 kg of titanium dioxide with the particle size of about 300 nm, 20 kg of calcium carbonate with the particle size of about 1 micron and 40 kg of fumed silica with the particle size of about 30 nm are weighed.
(4) Heating 100 kg of dispersing agent to 60 ℃, slowly adding the weighed titanium dioxide, calcium carbonate and fumed silica into the dispersing agent in sequence, and stirring for about 3 hours at about 60 ℃ by using a high-speed stirrer to prepare white slurry.
(5) Winding the glass cloth on a die attached with a high-temperature polypropylene film by using a cloth winding machine, winding the glass cloth on the die by using the cloth winding machine, and winding for 33 circles.
(6) Heating E-44 bisphenol A epoxy resin at 60 ℃ for 4 hours; weighing 55 kg of E-44 bisphenol A epoxy resin, 30 kg of methyl tetrahydrophthalic anhydride, 15 kg of white slurry and 0.2 kg of DMP-30, and uniformly mixing by using a high-speed mixer to prepare the epoxy resin prepreg.
(7) Pouring the epoxy resin prepreg into VPI equipment, controlling the temperature in the equipment to be about 40 ℃, and putting the mould wound with the glass cloth into vacuum impregnation equipment. The vacuum pressure is controlled to be about 0.07MPa, the dipping times are controlled to be 3 times, and the time is controlled to be about 1 hour.
(8) And (3) raising the temperature of the oven to 160 ℃, putting the mould into the oven, curing for 40min at the rotation speed of 20 r/min and under the condition of 160 +/-5 ℃, then adjusting the temperature of the oven to 140 +/-5 ℃, and continuing to cure for 80 min.
(9) And after the curing is finished, taking the mold out of the oven, standing at room temperature for cooling for 15min, taking out the cured glass cloth epoxy resin insulating cylinder blank by using a demolding machine, and taking the cured glass cloth epoxy resin insulating cylinder blank off the mold.
(10) And cutting, stripping and polishing according to the specified size in sequence, and processing to the specified size.
Example 3
A preparation method of an epoxy glass cloth insulating cylinder comprises the following steps:
(1) and (3) putting the glass cloth into an oven, and baking for more than 48 hours at the temperature of 60 ℃.
(2) 1kg of Xinyue organic silicon modified epoxy resin ES-1001N is added into a mixture consisting of 50 kg of ethyl acetate and 49 kg of butyl acetate, and the mixture is stirred uniformly to prepare the dispersing agent.
(3) 40 kg of titanium dioxide with the particle size of about 300 nm, 20 kg of calcium carbonate with the particle size of about 1 micron and 40 kg of fumed silica with the particle size of about 30 nm are weighed.
(4) Heating 100 kg of dispersing agent to 60 ℃, slowly adding the weighed titanium dioxide, calcium carbonate and fumed silica into the dispersing agent in sequence, and stirring for about 3 hours at about 60 ℃ by using a high-speed stirrer to prepare white slurry.
(5) Winding the glass cloth on a die attached with a high-temperature polypropylene film by using a cloth winding machine, winding the glass cloth on the die by using the cloth winding machine, and winding for 33 circles.
(6) Heating F-51 bisphenol A epoxy resin at 60 ℃ for 4 hours; weighing 50 kg of F-51 bisphenol A epoxy resin, 35 kg of methyl tetrahydrophthalic anhydride, 15 kg of white slurry and 0.1 kg of 2-ethyl-4-methylimidazole, and uniformly mixing by using a high-speed mixer to prepare the epoxy resin prepreg.
(7) Pouring the epoxy resin prepreg into VPI equipment, controlling the temperature in the equipment to be about 40 ℃, and putting the mould wound with the glass cloth into vacuum impregnation equipment. The vacuum pressure is controlled to be about 0.07MPa, the dipping times are controlled to be 3 times, and the time is controlled to be about 1 hour.
(8) And (3) raising the temperature of the oven to 170 ℃, putting the mould into the oven, maintaining the rotating speed at 20 r/min, curing for 40min at the temperature of 170 +/-5 ℃, adjusting the temperature of the oven to 150 +/-5 ℃, and continuously curing for 80 min.
(9) And after the curing is finished, taking the mold out of the oven, standing at room temperature for cooling for 15min, taking out the cured glass cloth epoxy resin insulating cylinder blank by using a demolding machine, and taking the cured glass cloth epoxy resin insulating cylinder blank off the mold.
(10) And cutting, stripping and polishing according to the specified size in sequence, and processing to the specified size.
Example 4
A preparation method of an epoxy glass cloth insulating cylinder comprises the following steps:
(1) and (3) putting the glass cloth into an oven, and baking for more than 48 hours at the temperature of 60 ℃.
(2) 1kg of Xinyue organic silicon modified epoxy resin ES-1001N is added into a mixture consisting of 50 kg of ethyl acetate and 49 kg of butyl acetate, and the mixture is stirred uniformly to prepare the dispersing agent.
(3) 40 kg of titanium dioxide with the particle size of about 300 nm, 20 kg of calcium carbonate with the particle size of about 1 micron and 40 kg of fumed silica with the particle size of about 30 nm are weighed.
(4) Heating 100 kg of dispersing agent to 60 ℃, slowly adding the weighed titanium dioxide, calcium carbonate and fumed silica into the dispersing agent in sequence, and stirring for about 3 hours at about 60 ℃ by using a high-speed stirrer to prepare white slurry.
(5) Winding the glass cloth on a die attached with a high-temperature polypropylene film by using a cloth winding machine, winding the glass cloth on the die by using the cloth winding machine, and winding for 33 circles.
(6) Heating hydantoin epoxy resin at 60 ℃ for 4 hours; weighing 45 kg of hydantoin epoxy resin, 45 kg of methyl nadic anhydride, 15 kg of white slurry and 0.2 kg of 4-methylbenzylamine, and uniformly mixing by using a high-speed mixer to prepare the epoxy resin prepreg.
(7) Pouring the epoxy resin prepreg into VPI equipment, controlling the temperature in the equipment to be about 40 ℃, and putting the mould wound with the glass cloth into vacuum impregnation equipment. The vacuum pressure is controlled to be about 0.07MPa, the dipping times are controlled to be 3 times, and the time is controlled to be about 1 hour.
(8) And (3) raising the temperature of the oven to 170 ℃, putting the mould into the oven, maintaining the rotating speed at 20 r/min, curing for 40min at the temperature of 170 +/-5 ℃, adjusting the temperature of the oven to 150 +/-5 ℃, and continuously curing for 80 min.
(9) And after the curing is finished, taking the mold out of the oven, standing at room temperature for cooling for 15min, taking out the cured glass cloth epoxy resin insulating cylinder blank by using a demolding machine, and taking the cured glass cloth epoxy resin insulating cylinder blank off the mold.
(10) And cutting, stripping and polishing according to the specified size in sequence, and processing to the specified size.
Various performance indexes of the epoxy glass cloth insulating cylinder prepared according to the method of examples 1 to 4 were measured, and the results are shown in the following table.
Figure BDA0002719750660000081
Note: the heat conductivity coefficient of the common epoxy glass cloth insulating cylinder is 0.5 w/m.k.
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the invention, and not to limit the scope of the invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.

Claims (10)

1. A method of making an epoxy glass cloth insulating cylinder, comprising the steps of:
putting the glass cloth into an oven, and baking at 60-80 ℃ for more than 24 hours;
and (II) uniformly mixing an inorganic filler and a dispersing agent in a high-speed mixer according to the mass ratio of 1: 0.8-3 to prepare white slurry, wherein the inorganic filler is titanium dioxide, calcium carbonate and fumed silica according to the mass ratio of 1-3: 1: 1-3;
thirdly, winding the glass cloth on a mould coated with a high-temperature film or a release agent by using a cloth winding machine, wherein the number of winding turns is determined according to the thickness requirement of the insulating cylinder; wherein, the winding turns of the glass cloth are determined according to the following formula:
n = T ÷ D +3, where N is the number of windings of the glass cloth; t is the thickness required by the insulating cylinder; d is the thickness of the single-layer glass cloth;
fourthly, mixing the white slurry with epoxy resin, a curing agent and a curing accelerator to prepare epoxy resin prepreg, putting the mould subjected to the third step into vacuum impregnation equipment, and uniformly impregnating the epoxy resin prepreg on glass cloth through a vacuum pressure impregnation process; wherein the specific process conditions of the vacuum pressure impregnation are as follows: the pressure is 0.05-0.07 MPa, the dipping times are 2-4 times, and the time is 1-1.5 hours;
the preparation process of the epoxy resin prepreg comprises the following steps: putting the epoxy resin into an oven for baking to reduce the viscosity of the epoxy resin, then mixing 40-55 parts of the epoxy resin, 35-40 parts of a curing agent, 10-25 parts of white pulp and 0.1-0.2 part of a curing accelerator according to parts by mass, and dispersing by using a high-speed stirrer to obtain the epoxy resin prepreg;
fifthly, placing the mold subjected to the step (four) into an oven for curing, taking the mold out of the oven after curing is completed, cooling at room temperature for 10-15 min, and taking the cured epoxy glass cloth insulating cylinder blank out of the mold; wherein, the curing process is carried out at high temperature and then at low temperature, the temperature of the oven is controlled to be 160-180 ℃ between 0-40 min, the temperature of the oven is controlled to be 135-155 ℃ between 40-120 min, and the rotating speed of the die in the oven is controlled to be 20-30 r/min.
2. The method of making an epoxy glass cloth insulating cylinder of claim 1, wherein: in the step (I), the baking temperature is 60-70 ℃, and the baking time is more than 36 hours.
3. The method of making an epoxy glass cloth insulating cylinder of claim 1, wherein: the glass cloth is roving alkali-free glass cloth without twists, and the filament number of the single filament is 30-50 dtex.
4. The method of making an epoxy glass cloth insulating cylinder of claim 1, wherein: the particle size of the titanium dioxide is 250-350 nanometers, the particle size of the calcium carbonate is 1-10 micrometers, and the particle size of the fumed silica is 20-30 nanometers.
5. The method of making an epoxy glass cloth insulating cylinder of claim 1, wherein: in the step (II), the white pulp is prepared by the following steps: and (3) putting the dispersing agent into a stirring barrel of a high-speed stirrer, starting stirring, heating to 50-70 ℃, then sequentially and slowly adding titanium dioxide, calcium carbonate and fumed silica, and stirring at a high speed until the dispersing agent is uniformly dispersed to obtain the titanium dioxide/calcium carbonate/fumed silica.
6. The method of making an epoxy glass cloth insulating cylinder of claim 1, wherein: in the step (ii), the mass ratio of the inorganic filler to the dispersant is 1: 1 to 3.
7. The method of making an epoxy glass cloth insulating cylinder of claim 1, wherein: the dispersing agent is a mixture of an organic silicon defoaming agent and two or more than two of ethyl acetate, butyl acetate and acetone, wherein the mass content of the organic silicon defoaming agent in the dispersing agent is 0.5-1.5%.
8. The method of making an epoxy glass cloth insulating cylinder of claim 1, wherein: the high-temperature film is a high-temperature polypropylene film, and the release agent is an organic silicon release agent.
9. The method of making an epoxy glass cloth insulating cylinder of claim 1, wherein: the epoxy resin is hydantoin epoxy resin, bisphenol A epoxy resin or phenolic aldehyde modified bisphenol A epoxy resin; the curing agent is one or two of methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride and methyl nadic anhydride; the curing accelerator is a tertiary amine curing agent or an imidazole curing agent.
10. The method of making an epoxy glass cloth insulating cylinder of claim 1, wherein: and taking the cured insulating cylinder out of the oven, cooling the insulating cylinder for 10-15 min at normal temperature, taking the insulating cylinder out of the mold, cutting, stripping and polishing the insulating cylinder after the insulating cylinder is completely cooled to room temperature after the insulating cylinder is taken out.
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