CN109705531A - A kind of poured with epoxy resin insulating materials and preparation method thereof and application method - Google Patents
A kind of poured with epoxy resin insulating materials and preparation method thereof and application method Download PDFInfo
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- CN109705531A CN109705531A CN201811643056.3A CN201811643056A CN109705531A CN 109705531 A CN109705531 A CN 109705531A CN 201811643056 A CN201811643056 A CN 201811643056A CN 109705531 A CN109705531 A CN 109705531A
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Abstract
The present invention provides a kind of poured with epoxy resin insulating materials and preparation method thereof and application method, poured with epoxy resin insulating materials is the suitable nano-titanium dioxide filler by the coupling agent modified processing of silane surface of addition before bisphenol A type epoxy resin solidifies.The modified nano-titanium dioxide in surface can form inhibiting effect by chemical bond and the chain combination of epoxy resin host molecule, and then to the warm-up movement of epoxy resin host molecule chain, to promote poured with epoxy resin material glass transition temperature.The present invention can be used in electrician and equip promotion with poured with epoxy resin insulating materials temperature resistant grade.The glass transition temperature of pure epoxy resin mould material is 81 DEG C, is promoted to 116 DEG C by the glass transition temperature using poured with epoxy resin material of the method for modifying.
Description
Technical field
The present invention relates to a kind of method of modifying of poured with epoxy resin insulating materials, and in particular to a kind of poured with epoxy resin
Insulating materials and preparation method thereof and application method.
Background technique
With the extensive use of high-voltage large-capacity electrical equipment and high-power electric and electronic equipment and device, epoxy resin is poured
Cast parts insulating materials has become important insulating materials.Poured with epoxy resin insulating materials is generally used for high-voltage isulation drawing
Bar, power electronic devices insulation-encapsulated, the supporting insulator in gas-insulated switchgear and disc insulator, bushing,
Electric power electric transformer, high-voltage mutual inductor etc..
Electrician is mostly bisphenol A-type with epoxy resin, the operating temperature of poured with epoxy resin insulating materials be environment temperature extremely
Glass transition temperature, therefore the glass transition temperature for promoting poured with epoxy resin insulating materials is conducive to expand making for material
With temperature range, the mechanical property of reinforcing material.But the transition temperature of electrician's epoxy resin is high not enough at present, so that its
High temperature resistant grade is lower.
Summary of the invention
The purpose of the present invention is to provide a kind of poured with epoxy resin insulating materials and preparation method thereof and application method, with
The glass transition temperature such as poured with epoxy resin insulating materials is promoted, to promote insulating materials temperature resistant grade.
In order to achieve the above objectives, the invention adopts the following technical scheme:
A kind of poured with epoxy resin material, in terms of mass fraction, raw material includes following components:
100 parts of epoxy resin, 0.1-5 parts of nano-titanium dioxide fillers, 0.001-0.150 parts of coupling agents and 80 parts of solidifications
Agent.
It further include 0.1-3 parts of promotors, the promotor is amine type accelerator.
The curing agent is liquid acids anhydride curing agent;The coupling agent uses γ-glycidyl ether oxygen propyl trimethoxy
Base silane;The epoxy resin is bisphenol A type epoxy resin.
The average grain diameter of the nano-titanium dioxide filler is 20-80nm.
A kind of preparation method of poured with epoxy resin material, is used to prepare above-mentioned poured with epoxy resin material, with mass parts
Number meter, comprising the following steps:
S1: 0.1-5 parts of nano-titanium dioxide fillers are mixed with sufficient dehydrated alcohol and ultrasonic disperse, ultrasonic disperse are complete
Then Cheng Hou is added 0.001-0.150 parts of coupling agents and carries out ultrasonic disperse, obtains mixed liquor A after ultrasonic disperse is uniform;So
Mixed liquor A is subjected to homogeneous processing afterwards, obtains mixed liquid B;
S2: being added mixed liquid B in 100 parts of epoxy resin and be uniformly mixed, and then stirring is until dehydrated alcohol is waved completely
Hair, obtains mixed liquor C;
S3: 80 parts of curing agent being added in mixed liquor C and are uniformly mixed, mixture D is obtained, and mixture D progress vacuum is taken off
Gas disposal obtains the poured with epoxy resin material.
In S1, mixed liquor A is heated to 30-80 DEG C and carries out homogeneous processing, obtains mixed liquid B.
In S2, mixed liquid B is added in epoxy resin and is uniformly mixed, then at 60-120 DEG C circulation stirring until nothing
Water-ethanol volatilizees completely.
In S3, it is also added into 0.1-3 parts of promotors into mixed liquor C, curing agent and promotor are added in mixed liquor C and mixed
It closes uniform.
In S3, mixture D is subjected to Fruit storage while stirring, the time of Fruit storage is
10min-60min。
The application method of above-mentioned poured with epoxy resin material, the use process is as follows:
The poured with epoxy resin material is solidified at 80-150 DEG C by 4-12h using ladder-elevating temperature method, is subsequently cooled to
Room temperature.
Compared with prior art, the invention has the following advantages:
Poured with epoxy resin material of the invention is by adding 0.1-5 mass parts into the epoxy resin of every 100 mass parts
Nano-titanium dioxide, 0.001-0.150 mass parts coupling agent and 80 parts of curing agent, nano-titanium dioxide pass through coupling agent
It is modified, the modified nano-titanium dioxide in surface can be by chemical bond and the chain combination of epoxy resin host molecule, and then to ring
The warm-up movement of oxygen resin host molecule chain forms inhibiting effect, to promote poured with epoxy resin material glass transition temperature.This
The glass transition temperature of invention poured with epoxy resin material can reach 83~116 DEG C, of the invention relative to existing material
Poured with epoxy resin material temperature resistant grade is promoted.
Further, the raw material of poured with epoxy resin material of the present invention further includes 0.1-3 parts of promotors, and the promotor is
Amine type accelerator can speed up the solidification process of poured with epoxy resin material of the present invention by the promotor.
As aforementioned present invention poured with epoxy resin material beneficial effect it is found that ring made from preparation method through the invention
Oxygen resin-cast material glass transition temperature can reach 83~116 DEG C, relative to existing material, epoxy resin of the invention
Mould material temperature resistant grade is promoted.
When in use, the poured with epoxy resin material is solidified at 80-150 DEG C for poured with epoxy resin material of the present invention
4-12h is then cooled to room temperature, so that poured with epoxy resin material solidification of the invention, reaches preferable using effect, is guaranteed
Its glass transition temperature and temperature resistant grade.
Detailed description of the invention
Fig. 1 is that the casting insulated material of pure epoxy resin (neat epoxy) nano-titanium dioxide addition different with the present invention contains
Measure the differential scanning calorimetric curve figure of the lower casting insulated material of modified epoxy.
Specific embodiment
The present invention is described in further details with reference to the accompanying drawings and examples.
In following embodiment, epoxy resin is bisphenol A type epoxy resin, and coupling agent uses γ-glycidyl ether oxygen propyl
Trimethoxy silane, curing agent are liquid acids anhydride curing agent, and promotor is amine type accelerator.
Embodiment 1
The preparation process of the present embodiment poured with epoxy resin material is as follows:
Step 1 by quality weighs 100 parts of epoxy resin, 80 parts of curing agent, 0.3 part of promotor, 0.1 part of nanometer two first
Titanium oxide filler and 0.0015 part of coupling agent.
Weighed nano-titanium dioxide filler is mixed with dehydrated alcohol and carries out ultrasonic disperse by step 2, and step is then added
Rapid 1 weighed coupling agent and be uniformly mixed obtain mixed liquor A, by mixed liquor A be heated to 60 DEG C and by homogenizer processing after obtain
Obtain mixed liquid B.
Above-mentioned mixed liquid B is added in weighed epoxy resin and is uniformly mixed by step 3, is then recycled and is stirred at 90 DEG C
It mixes to ethyl alcohol and is cooled to room temperature after volatilizing completely, obtain mixed liquor C.
Then gained mixed liquor C is uniformly mixed by step 4 with weighed curing agent and promotor, obtain mixture D, and
The Fruit storage of mixture D progress 30min will be obtained while stirring, obtains the poured with epoxy resin material.
The poured with epoxy resin material that the present embodiment is prepared when in use, by poured with epoxy resin material at 80 DEG C
After solidifying 2h, in 105 DEG C of heat preservation 2h, solidifies 8h at 120 DEG C, be cooled to room temperature after molding.
Embodiment 2
The preparation process of the present embodiment poured with epoxy resin material is as follows:
Step 1 by quality weighs 100 parts of epoxy resin, 80 parts of curing agent, 3 parts of promotors, 1 part of nanometer titanium dioxide first
Titanium filler and 0.01 part of coupling agent.
Weighed nano-titanium dioxide filler is mixed with dehydrated alcohol and carries out ultrasonic disperse by step 2, and step is then added
Rapid 1 weighed coupling agent and be uniformly mixed obtain mixed liquor A, by mixed liquor A be heated to 30 DEG C and by homogenizer processing after obtain
Obtain mixed liquid B.
Above-mentioned mixed liquid B is added in weighed epoxy resin and is uniformly mixed by step 3, is then recycled and is stirred at 60 DEG C
It mixes to ethyl alcohol and is cooled to room temperature after volatilizing completely, obtain mixed liquor C.
Then gained mixed liquor C is uniformly mixed by step 4 with weighed curing agent and promotor, obtain mixture D, and
The Fruit storage of mixture D progress 10min will be obtained while stirring, obtains the poured with epoxy resin material.
The poured with epoxy resin material that the present embodiment is prepared when in use, by poured with epoxy resin material at 80 DEG C
Solidify 2h at 150 DEG C after solidification 2h, is cooled to room temperature after molding.
Embodiment 3
The preparation process of the present embodiment poured with epoxy resin material is as follows:
Step 1 by quality weighs 100 parts of epoxy resin, 80 parts of curing agent, 0.1 part of promotor, 5 parts of nano-silicas first
Change titanium filler and 0.15 part of coupling agent.
Then weighed nano-titanium dioxide filler is mixed with dehydrated alcohol respectively and carries out ultrasonic disperse by step 2, so
The weighed coupling agent of step 1 is added afterwards and is uniformly mixed and obtains mixed liquor A, mixed liquor A is heated to 80 DEG C and passes through homogenizer
Mixed liquid B is obtained after processing.
Above-mentioned mixed liquid B is added in weighed epoxy resin and is uniformly mixed by step 3, is then recycled and is stirred at 150 DEG C
It mixes to ethyl alcohol and is cooled to room temperature after volatilizing completely, obtain mixed liquor C.
Then gained mixed liquor C is uniformly mixed by step 4 with weighed curing agent and promotor, obtain mixture D, and
The Fruit storage of mixture D progress 60min will be obtained while stirring, obtains the poured with epoxy resin material.
The poured with epoxy resin material that the present embodiment is prepared when in use, by poured with epoxy resin material at 120 DEG C
Solidify 2h, is cooled to room temperature after solidifying 8h molding at 140 DEG C.
To poured with epoxy resin insulating materials glass transition temperature testing experiment produced by the present invention
Gained poured with epoxy resin insulating materials and the epoxy resin after nano-titanium dioxide is compound in implementation are poured
Note insulating materials respectively takes 8mg, is placed in differential scanning calorimeter.200 DEG C are heated to from 20 DEG C with the heating rate of 10 DEG C/min
Heat preservation 2min is cooled to 20 DEG C later to eliminate the thermal history of material with the rate of -10 DEG C/min, keeps 5min, then with 10 DEG C/
The heating rate of min is heated to 200 DEG C.Using secondary temperature elevation curve, glass transition temperature is obtained as shown in table 1 and Fig. 1, table
1 adds the glass transition temperature of poured with epoxy resin insulating materials under content, in Fig. 1, curve 1 for different nano-titanium dioxides
For the differential scanning calorimetric curve of pure epoxy resin, curve 2 is differential scanning when 100 parts of epoxies add 0.1 part of titanium dioxide
Calorimetric curve, curve 3 are differential scanning calorimetric curve when 100 parts of epoxies add 0.5 part of titanium dioxide, and curve 4 is 100 parts of rings
Oxygen adds differential scanning calorimetric curve when 1 part of titanium dioxide, and curve 5 is differential when 100 parts of epoxies add 3 parts of titanium dioxide
Scanning calorimetric curve, curve 6 are differential scanning calorimetric curve when 100 parts of epoxies add 5 parts of titanium dioxide.
Table 1
By Fig. 1 and table 1 can be obvious find out, poured with epoxy resin material glass transition temperature of the invention can reach 83
~116 DEG C, relative to existing pure epoxy resin material, poured with epoxy resin material temperature resistant grade of the invention is promoted.
Therefore the present invention can be used in electrician and equip promotion with poured with epoxy resin insulating materials temperature resistant grade.
Claims (10)
1. a kind of poured with epoxy resin material, which is characterized in that in terms of mass fraction, raw material includes following components:
100 parts of epoxy resin, 0.1-5 parts of nano-titanium dioxide fillers, 0.001-0.150 parts of coupling agents and 80 parts of curing agent.
2. a kind of poured with epoxy resin material according to claim 1, which is characterized in that the original of poured with epoxy resin material
Material further includes 0.1-3 parts of promotors, and the promotor is amine type accelerator.
3. a kind of poured with epoxy resin material according to claim 1, which is characterized in that the curing agent is liquid anhydride
Class curing agent;The coupling agent uses γ-glycidyl ether oxygen propyl trimethoxy silicane;The epoxy resin is bisphenol A-type
Epoxy resin.
4. a kind of poured with epoxy resin material according to claim 1, which is characterized in that the nano-titanium dioxide filler
Average grain diameter be 20-80nm.
5. a kind of preparation method of poured with epoxy resin material, which is characterized in that in terms of mass fraction, comprising the following steps:
S1: 0.1-5 parts of nano-titanium dioxide fillers are mixed with sufficient dehydrated alcohol and ultrasonic disperse, ultrasonic disperse are completed
Afterwards, 0.001-0.150 parts of coupling agents are then added and carry out ultrasonic disperse, obtain mixed liquor A after ultrasonic disperse is uniform;Then
Mixed liquor A is subjected to homogeneous processing, obtains mixed liquid B;
S2: by mixed liquid B be added 100 parts of epoxy resin in and be uniformly mixed, then stirring until dehydrated alcohol volatilize completely, obtain
To mixed liquor C;
S3: 80 parts of curing agent being added in mixed liquor C and are uniformly mixed, mixture D is obtained, and mixture D is carried out at vacuum outgas
Reason, obtains the poured with epoxy resin material.
6. a kind of preparation method of poured with epoxy resin material according to claim 5, which is characterized in that in S1, will mix
It closes liquid A and is heated to the 30-80 DEG C of homogeneous processing of progress, obtain mixed liquid B.
7. a kind of preparation method of poured with epoxy resin material according to claim 5, which is characterized in that in S2, will mix
Close liquid B be added epoxy resin in and be uniformly mixed, then at 60-120 DEG C circulation stirring until dehydrated alcohol volatilize completely.
8. a kind of preparation method of poured with epoxy resin material according to claim 5, which is characterized in that in S3, to mixed
It closes in liquid C and is also added into 0.1-3 parts of promotors, curing agent and promotor are added in mixed liquor C and are uniformly mixed.
9. a kind of preparation method of poured with epoxy resin material according to claim 5, which is characterized in that in S3, will mix
It closes object D and carries out Fruit storage while stirring, the time of Fruit storage is 10min-60min.
10. the application method of poured with epoxy resin material described in claim 1-4, which is characterized in that the use process is as follows:
The poured with epoxy resin material is solidified at 80-150 DEG C by 4-12h using ladder-elevating temperature method, is then cooled to room temperature.
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Cited By (1)
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CN115386196A (en) * | 2022-08-25 | 2022-11-25 | 云南电网有限责任公司临沧供电局 | Preparation method of epoxy resin composite material for solid cabinet |
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Cited By (2)
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CN115386196B (en) * | 2022-08-25 | 2023-10-24 | 云南电网有限责任公司临沧供电局 | Preparation method of epoxy resin composite material for solid cabinet |
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