CN106832946A - A kind of epoxy-modified silicon rubber and preparation method thereof and its application - Google Patents
A kind of epoxy-modified silicon rubber and preparation method thereof and its application Download PDFInfo
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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
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
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Abstract
The invention discloses a kind of epoxy-modified silicon rubber and preparation method thereof and its application, methyl vinyl silicone rubber with octamethylcy-clotetrasiloxane as Material synthesis is modified prepared epoxy-modified silicon rubber to methyl vinyl silicone rubber as sizing material using epoxy silane coupling.It is an advantage of the invention that：The silicon rubber that methyl ethylene is blocked is modified using epoxy silane coupling, and be equipped with the materials such as a certain amount of white carbon, hydroxy silicon oil, containing hydrogen silicone oil, active aluminium hydroxide and zinc oxide new material for producing composite insulator external insulation umbrella sets is obtained, the material not only has the physical property of similar elastomeric compound, and cause that silicon rubber is integral type structure with epoxy resin fiberglass rod tight bond, with the characteristic for improving contact interface caking ability.
Description
Technical field
The present invention relates to one kind for making composite insulator external insulation umbrella sets and external insulation umbrella sets and plug can be improved
The epoxy-modified silicon rubber and its preparation formula of bonding interface degree.
Background technology
Composite insulator operation over time, still some portioned products the power grid security thing caused by interior insulation quality problems
Therefore, such as interface breakdown accident.Interface breakdown accident is bad mainly due to sheath and plug bonding interface, and bonding interface mainly by
The artificial coupling agent applied in mandrel surface serves as a connection.
It is base rubber that conventional composite insulator external insulation umbrella sets use silicon rubber gross rubber, be equipped with reinforcing agent, filler and
Various additives（Not plus coupling agent）, need artificially to apply coupling agent in mandrel surface in external insulation umbrella sets injection moulding, but
Due to factors such as operative employee's proficiency, painting ways, cause plug holiday, brush inequality, it is impossible to ensure the interface of product
There is serious potential safety hazard in bonding quality, product longtime running, in view of problem above is, it is necessary to a kind of new technical scheme is solved
Certainly above mentioned problem.
The content of the invention
The purpose of the present invention is directed to above-mentioned weak point and provides one kind and can improve external insulation umbrella sets and plug interface glues
The epoxy-modified silicone rubber formulations of degree of connecing.
The technical solution adopted by the present invention is：
A kind of epoxy-modified silicon rubber, with octamethylcy-clotetrasiloxane（D4）For the methyl vinyl silicone rubber of Material synthesis is
Sizing material, preferably, molecular weight is that 60-70 ten thousand, contents of ethylene is the methyl vinyl silicone rubber of 0.07-0.24mol%.Using
Epoxy silane coupling is modified prepared epoxy-modified silicon rubber to methyl vinyl silicone rubber.In modifying process, silicon
Group in alkane is hydrolyzed, and the hydroxyl after hydrolysis occurs dehydration with the surface of inorganic filler in methyl vinyl silicone rubber
Chemical bond connection is carried out, that is, obtains modified silicon rubber.In composite insulator external insulation umbrella sets manufacturing process, in sizing material injection
When, there is complicated chemical reaction in the epoxide group in modified silicon rubber so that injection molding with the epoxy resin in plug
Closely it is bonded together between silicon rubber external insulation umbrella sets and plug.Its mechanism is：The structural formula of epoxy silane coupling is：
Y-R-Si-X3, wherein, X is that, with reference to hydrolization group on the silicon atoms, Y is organo-functional group, and R is with saturation or insatiable hunger
With the carbochain of key.
The each group of epoxy-modified silicon rubber is divided into：The weight on the basis of methyl vinyl silicone rubber, also including with methyl
The weight of vinylsiloxane rubber is than the white carbon for 30-60%, the hydroxy silicon oil of 1-8%, the containing hydrogen silicone oil of 2-10%, 100-300%
Active aluminium hydroxide, the zinc oxide of 2-10%, double two or five vulcanizing agents of the color masterbatch of 0.5-2% and 0.5-2%, the epoxy radicals
Silane coupler is 2-5% with the weight ratio of methyl vinyl silicone rubber.
Preferably, specific surface area is 150-300m3The gas-phase silica of/g.
Preferably, median is 5 active aluminium hydroxide.
Preferably, hydrogen content is >=1.58% containing hydrogen silicone oil.
Preferably, hydroxy radical content is the hydroxy silicon oil of 3.6-4.5%.
Vulcanizing agent is preferably double two or five vulcanizing agents of peroxide.
Preferably, purity >=97% of epoxy silane coupling.
Specific preparation method：Methyl vinyl silicone rubber with octamethylcy-clotetrasiloxane as Material synthesis as sizing material,
Directly epoxy silane coupling is added in methyl vinyl silicone rubber and is well mixed in kneading, at warm high
Add double two or five vulcanizing agents and color masterbatch that epoxy-modified silicon rubber is obtained after reason.
Methyl vinyl silicone rubber, white carbon, hydroxy silicon oil, containing hydrogen silicone oil, the activity that will first have been matched before kneading
Aluminium hydroxide and zinc oxide material knead agglomerating in banbury, and kneading is then carried out in kneader, will be matched during kneading
Epoxy silane coupling add and be well mixed, the temperature of kneading is 140-175 DEG C, and kneading vacuum is 0.04-
0.08MPa, the kneading time is 1-3h, be cooled to after kneading 40 DEG C thin it is logical park 48h, be subsequently adding the epoxy radicals silicone hydride for having matched
Coupling agent and color masterbatch obtain epoxy-modified silicon rubber after thin logical filter glue.
Using epoxy-modified silicon rubber as the making material of composite insulator external insulation umbrella sets, need not manually brush occasionally
In the case of connection agent, composite insulator external insulation umbrella sets and plug can be significantly improved（Epoxy resin fiberglass rod）Contact circle
Caking ability between face, production the compound inslation period of the day from 11 p.m. to 1 a.m, coupling agent brushing link can be saved so that external insulation umbrella sets inject when and core
Rod is made tight bond overall structure together, not only increases production efficiency, and the quality of product is ensured.
It is an advantage of the invention that：The silicon rubber that methyl ethylene is blocked is modified using epoxy silane coupling,
And be equipped with the materials such as a certain amount of white carbon, hydroxy silicon oil, containing hydrogen silicone oil, active aluminium hydroxide and zinc oxide and be obtained for producing
The new material of composite insulator external insulation umbrella sets, the material not only has the physical property of similar elastomeric compound, but also has
There is the chemical reaction of complexity between the performance that similar elastomeric compound does not have, i.e. silicon rubber and epoxy resin fiberglass rod and produce
New chemical bond is attached, and to cause that silicon rubber and epoxy resin fiberglass rod tight bond are integral type structure, has
Improve the characteristic of contact interface caking ability.
Specific embodiment
Embodiment 1
With octamethylcy-clotetrasiloxane（D4）For the methyl vinyl silicone rubber of Material synthesis is sizing material, being chosen at molecular weight is
As a example by 60-65 ten thousand, contents of ethylene is for the methyl vinyl silicone rubber of 0.07-0.15mol%.
It is 150-300m by methyl vinyl silicone rubber 100g, 30g specific surface area3The gas-phase silica of/g, 1g hydroxyls contain
It is >=1.58% containing hydrogen silicone oil, the reactive hydrogen that 100g medians are 5 to measure the hydroxy silicon oil for 3.6-4.5%, 2g hydrogen contents
(fineness is with 320 mesh wet screening residues, fineness≤0.2% for aluminum oxide and 2g nanometer active zinc oxides）Kneaded in banbury it is agglomerating,
Then kneading is carried out in kneader, adds the γ-glycidyl ether oxygen propyl trimethoxy silicane of 2g purity >=97% during kneading
Enter and be well mixed, the temperature of kneading is 140 DEG C, and kneading vacuum is 0.08MPa, and the kneading time is 3h, is cooled to after kneading
40 DEG C thin logical to park 48h, is subsequently adding the epoxy silane coupling of 0.5g and 0.5g color masterbatches and obtains ring after thin logical filter glue
Epoxide modified silicon rubber.Composite insulator is produced using the epoxy-modified silicon rubber as raw material, then External Insulation umbrella cover
Caking ability and between plug is tested, and obtains the extraction force of 500N/ roots（Reference, GB/T14450-2008 test methods）.
Embodiment 2
With octamethylcy-clotetrasiloxane（D4）For the methyl vinyl silicone rubber of Material synthesis is sizing material, being chosen at molecular weight is
As a example by 66-70 ten thousand, contents of ethylene is for the methyl vinyl silicone rubber of 0.16-0.24mol%.
It is 150-300m by methyl vinyl silicone rubber 100g, 60g specific surface area3The gas-phase silica of/g, 8g hydroxyls contain
It is >=1.58% containing hydrogen silicone oil, the reactive hydrogen that 300g medians are 5 to measure the hydroxy silicon oil for 3.6-4.5%, 10g hydrogen contents
(fineness is with 320 mesh wet screening residues, fineness≤0.2% for aluminum oxide and 10g nanometer active zinc oxides）Kneaded into banbury
Group, then carries out kneading, by the γ of 5g purity >=97%-glycidyl ether oxygen propyl trimethoxy silicon during kneading in kneader
Alkane is added and is well mixed, and the temperature of kneading is 175 DEG C, and kneading vacuum is 0.04MPa, and the kneading time is 1h, is dropped after kneading
Temperature to 40 DEG C thin it is logical park 48h, be subsequently adding 2g epoxy silane couplings and 2g color masterbatches and obtain epoxy after thin logical filter glue
Base modified silicon rubber.Using the epoxy-modified silicon rubber as raw material with the equal ambient of embodiment 1 and under the conditions of produce rule
Lattice identical composite insulator, then the caking ability between External Insulation umbrella cover and plug tested, obtain the extraction of 510N/ roots
Power（Reference, GB/T14450-2008 test methods）.
Embodiment 3
With octamethylcy-clotetrasiloxane（D4）For the methyl vinyl silicone rubber of Material synthesis is sizing material, being chosen at molecular weight is
As a example by 60-70 ten thousand, contents of ethylene is for the methyl vinyl silicone rubber of 0.07-0.12mol%.
It is 150-300m by methyl vinyl silicone rubber 100g, 40g specific surface area3The gas-phase silica of/g, 4g hydroxyls contain
It is >=1.58% containing hydrogen silicone oil, the reactive hydrogen that 200g medians are 5 to measure the hydroxy silicon oil for 3.6-4.5%, 5g hydrogen contents
(fineness is with 320 mesh wet screening residues, fineness≤0.2% for aluminum oxide and 5g nanometer active zinc oxides）Kneaded in banbury it is agglomerating,
Then kneading is carried out in kneader, adds the γ-glycidyl ether oxygen propyl trimethoxy silicane of 3g purity >=97% during kneading
Enter and be well mixed, the temperature of kneading is 150 DEG C, and kneading vacuum is 0.06MPa, and the kneading time is 2h, is cooled to after kneading
40 DEG C thin logical to park 48h, is subsequently adding 1g epoxy silane couplings and 1g color masterbatches and obtains epoxy radicals after thin logical filter glue and changes
Property silicon rubber.Using the epoxy-modified silicon rubber as raw material with the equal ambient of embodiment 1 and under the conditions of production specification phase
With composite insulator, then the caking ability between External Insulation umbrella cover and plug tested, obtain the extraction force of 498N/ roots
（Reference, GB/T14450-2008 test methods）.
Comparative example 1
With octamethylcy-clotetrasiloxane（D4）For the methyl vinyl silicone rubber of Material synthesis is sizing material, being chosen at molecular weight is
As a example by 60-65 ten thousand, contents of ethylene is for the methyl vinyl silicone rubber of 0.07-0.15mol%.
It is 150-300m by methyl vinyl silicone rubber 100g, 30g specific surface area3The gas-phase silica of/g, 1g hydroxyls contain
It is >=1.58% containing hydrogen silicone oil, the reactive hydrogen that 100g medians are 5 to measure the hydroxy silicon oil for 3.6-4.5%, 2g hydrogen contents
(fineness is with 320 mesh wet screening residues, fineness≤0.2% for aluminum oxide and 2g nanometer active zinc oxides）Kneaded in banbury it is agglomerating,
Then kneading is carried out in kneader, the temperature of kneading is 140 DEG C, and kneading vacuum is 0.08MPa, and the kneading time is 3h, is pinched
Be cooled to after refining 40 DEG C thin it is logical park 48h, be subsequently adding 0.5g epoxy silane couplings and 0.5g color masterbatches through thin logical filter glue
After obtain epoxy-modified silicon rubber.Using the epoxy-modified silicon rubber as raw material with the equal ambient of embodiment 1 and bar
Before production specification identical composite insulator under part, and production, it is coupled in the surface artificial brushing 2g epoxy radicals silicone hydrides of plug
Agent, then the caking ability between External Insulation umbrella cover and plug tested, obtain the extraction force of 350N/ roots（Reference, GB/
T14450-2008 test methods）.
Comparative example 2
With octamethylcy-clotetrasiloxane（D4）For the methyl vinyl silicone rubber of Material synthesis is sizing material, being chosen at molecular weight is
As a example by 66-70 ten thousand, contents of ethylene is for the methyl vinyl silicone rubber of 0.16-0.24mol%.
It is 150-300m by methyl vinyl silicone rubber 100g, 60g specific surface area3The gas-phase silica of/g, 8g hydroxyls contain
It is >=1.58% containing hydrogen silicone oil, the reactive hydrogen that 300g medians are 5 to measure the hydroxy silicon oil for 3.6-4.5%, 10g hydrogen contents
(fineness is with 320 mesh wet screening residues, fineness≤0.2% for aluminum oxide and 10g nanometer active zinc oxides）Kneaded into banbury
Group, then carries out kneading in kneader, and the temperature of kneading is 175 DEG C, and kneading vacuum is 0.04MPa, and the kneading time is 1h,
Be cooled to after kneading 40 DEG C thin it is logical park 48h, be subsequently adding 2g epoxy silane couplings and 2g color masterbatches after thin logical filter glue
Obtain epoxy-modified silicon rubber.Using the epoxy-modified silicon rubber as raw material with the equal ambient of embodiment 1 and condition
Lower production same size composite insulator, and before producing, in the surface artificial brushing 5g epoxy silane couplings of plug, so
The caking ability between External Insulation umbrella cover and plug is tested afterwards, obtains the extraction force of 340N/ roots（Reference, GB/T14450-
2008 test methods）.
Comparative example 3
With octamethylcy-clotetrasiloxane（D4）For the methyl vinyl silicone rubber of Material synthesis is sizing material, being chosen at molecular weight is
As a example by 60-70 ten thousand, contents of ethylene is for the methyl vinyl silicone rubber of 0.07-0.12mol%.
It is 150-300m by methyl vinyl silicone rubber 100g, 40g specific surface area3The gas-phase silica of/g, 4g hydroxyls contain
It is >=1.58% containing hydrogen silicone oil, the reactive hydrogen that 200g medians are 5 to measure the hydroxy silicon oil for 3.6-4.5%, 5g hydrogen contents
(fineness is with 320 mesh wet screening residues, fineness≤0.2% for aluminum oxide and 5g nanometer active zinc oxides）Kneaded in banbury it is agglomerating,
Then kneading is carried out in kneader, the temperature of kneading is 150 DEG C, and kneading vacuum is 0.06MPa, and the kneading time is 2h, is pinched
Be cooled to after refining 40 DEG C thin it is logical park 48h, be subsequently adding 1g epoxy silane couplings and 1g color masterbatches after thin logical filter glue
To epoxy-modified silicon rubber.Using the epoxy-modified silicon rubber as raw material with the equal ambient of embodiment 1 and under the conditions of
Production specification identical composite insulator, and before producing, in the surface artificial brushing 3g epoxy silane couplings of plug, so
The caking ability between External Insulation umbrella cover and plug is tested afterwards, obtains the extraction force of 345N/ roots（Reference, GB/T14450-
2008 test methods）.
Data Comparison：By above example and the Data Comparison of comparative example, it can be deduced that, technical scheme energy
Enough significantly improve the caking ability between silicon rubber external insulation umbrella sets and plug.
Claims (12)
1. a kind of epoxy-modified silicon rubber, it is characterised in that：Ethylene methacrylic with octamethylcy-clotetrasiloxane as Material synthesis
Base silicon rubber is sizing material, and prepared epoxy-modified silicone is modified to methyl vinyl silicone rubber using epoxy silane coupling
Rubber, the structural formula of the epoxy silane coupling is：Y-R-Si-X3, wherein, X is water-disintegrable with reference on the silicon atoms
Group, Y is organo-functional group, and R is the carbochain with saturation or unsaturated bond.
2. epoxy-modified silicon rubber according to claim 1, it is characterised in that：The methyl vinyl silicone rubber point
Son amount is 60-70 ten thousand, and contents of ethylene is 0.07-0.24mol%.
3. epoxy-modified silicon rubber according to claim 1 and 2, it is characterised in that：It is with methyl vinyl silicone rubber
Pivot weight, also including the weight with methyl vinyl silicone rubber than white carbon, the hydroxy silicon oil of 1-8%, the 2- for 30-60%
10% containing hydrogen silicone oil, the active aluminium hydroxide of 100-300%, the zinc oxide of 2-10%, the color masterbatch of 0.5-2% and 0.5-2%'s is double
Two or five vulcanizing agents, the epoxy silane coupling is 2-5% with the weight ratio of methyl vinyl silicone rubber.
4. epoxy-modified silicon rubber according to claim 3, it is characterised in that：The white carbon is for specific surface area
150-300m3The gas-phase silica of/g.
5. epoxy-modified silicon rubber according to claim 3, it is characterised in that：The active aluminium hydroxide median
It is 5.
6. epoxy-modified silicon rubber according to claim 3, it is characterised in that：Hydrogen content in the containing hydrogen silicone oil is
≥1.58%。
7. epoxy-modified silicon rubber according to claim 3, it is characterised in that：The Hydroxyl Content in Hydroxysilicone fluid is
3.6-4.5%。
8. epoxy-modified silicon rubber according to claim 3, it is characterised in that：Double two or five vulcanizing agents were preferably
Oxide curative agent.
9. epoxy-modified silicon rubber according to claim 3, it is characterised in that：The epoxy silane coupling it is pure
Degree >=97%.
10. a kind of preparation method of epoxy-modified silicon rubber, it is characterised in that：With octamethylcy-clotetrasiloxane as Material synthesis
Methyl vinyl silicone rubber be sizing material, epoxy silane coupling is directly added to methyl vinyl silicone rubber in kneading
In and be well mixed, by after high-temperature heat treatment plus double two or five vulcanizing agents and color masterbatch are obtained epoxy-modified silicon rubber.
11. preparation methods according to claim 10, it is characterised in that：The ethylene methacrylic that will first have been matched before kneading
Base silicon rubber, white carbon, hydroxy silicon oil, containing hydrogen silicone oil, active aluminium hydroxide and zinc oxide material kneaded in banbury it is agglomerating,
Then kneading is carried out in kneader, the epoxy silane coupling that will have been matched during kneading is added and is well mixed, kneading
Temperature is 140-175 DEG C, and kneading vacuum is 0.04-0.08MPa, and the kneading time is 1-3h, 40 DEG C thin is cooled to after kneading and is led to
48h is parked, the epoxy silane coupling that has matched is subsequently adding and color masterbatch is obtained epoxy-modified silicone after thin logical filter glue
Rubber.
12. according to any described epoxy-modified silicon rubber in claim 1-2,4-11, it is characterised in that：As compound exhausted
The making material of edge external insulation umbrella sets.
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| CN111048266A (en) * | 2019-12-30 | 2020-04-21 | 江东金具设备有限公司 | Anti-crisp composite insulator and preparation method thereof |
| CN111253755A (en) * | 2019-12-30 | 2020-06-09 | 江东金具设备有限公司 | High-mechanical-property insulating silicone rubber material and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111410745A (en) * | 2019-01-07 | 2020-07-14 | 北京化工大学 | Ultra-low temperature-resistant epoxidized silicone rubber and preparation method thereof |
| CN109994291A (en) * | 2019-04-10 | 2019-07-09 | 江苏东源电器集团股份有限公司 | A kind of silicon rubber insulation casing and its manufacture craft |
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| CN113527888A (en) * | 2020-04-22 | 2021-10-22 | 北京化工大学 | High-tear-resistance white carbon black/methyl vinyl silicone rubber composite material and preparation method thereof |
| CN113527888B (en) * | 2020-04-22 | 2022-11-29 | 北京化工大学 | High-tear-resistance white carbon black/methyl vinyl silicone rubber composite material and preparation method thereof |
| CN111979791A (en) * | 2020-08-11 | 2020-11-24 | 南通金秋服装辅料有限公司 | Polyurethane modified silicone rubber and preparation method thereof |
| CN114835901A (en) * | 2022-06-17 | 2022-08-02 | 四川大学 | Epoxy modified vinyl silicone rubber and preparation method and application thereof |
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