CN106009693A - Silicone rubber with excellent tracking resistance and high heat conductivity - Google Patents
Silicone rubber with excellent tracking resistance and high heat conductivity Download PDFInfo
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- CN106009693A CN106009693A CN201610439847.9A CN201610439847A CN106009693A CN 106009693 A CN106009693 A CN 106009693A CN 201610439847 A CN201610439847 A CN 201610439847A CN 106009693 A CN106009693 A CN 106009693A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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Abstract
The invention discloses silicone rubber with excellent tracking resistance and high heat conductivity. The silicone rubber is prepared from a methyl vinyl silicone rubber base body, inorganic nanoparticles, a vulcanizing agent, a cross-linking agent (TAIC), hydroxyl silicone oil and a silane coupling agent. The inorganic nanoparticles including aluminum hydroxide (ATH) and boron nitride (BN) are used as filler and are combined with the silicone rubber in a mixing and doping mode to obtain unitary and binary doped silicon rubber composite insulating material excellent in heat conductivity and tracking resistance. As ATH and BN are doped into the silicone rubber, tracking resistance and heat conductivity of the silicon rubber can be improved greatly.
Description
Technical field
The invention belongs to electric insulation polymeric material field, particularly to the preparation method of a kind of silicone rubber with anti creepage trace ability and high heat conductance.
Background technology
Composite insulator with silicone rubber as matrix has good mechanical strength, electrical insulating property and chemical stability, and light weight, and operation maintenance is convenient, uses in high pressure occasion very reliable, replaces glass and ceramic insulator the most more and more.
But, when silicon rubber compound insulator surface exists filthy, can discharge on surface, owing to the heat conductivity of material is poor, cause temperatures at localized regions to rise hundreds of degree Celsius, if local energy is beyond energy between the atom of silicone rubber strand own, silicon rubber composite material will decompose, and leaves tungsten carbide/conductive passage at insulator surface, and time serious, material surface can occur to burn in short-term, cause insulator to lose efficacy, threaten electric power netting safe running.Therefore, the heat conductivility and the anti creepage trace ability that improve silicone rubber are very important, can be effectively improved the service life of silicon rubber compound insulator, reduce the failure problems caused because insulator lost efficacy.
At present, the method that the anti creepage trace performance of raising high polymer composite material is commonly used is to add metal-oxide, e.g., MgO, TiO2Deng.B. X.
Du etc. study Epoxy/Nano Al2O3Anti creepage trace performance, find loading the biggest, epoxy anti creepage trace ability is the best.See B. X.
Du, Y. G. Guo, Tracking resistance
of epoxy/ Al2O3 nanocomposites
under DC voltage, IEEE Transactions on Dielectrics and Electrical Insulation,
2015; 22: 109-116。
Summary of the invention
It is an object of the invention to, the defect existed for existing silicone rubber heat conductivility and anti creepage trace ability aspect, it is provided that a kind of silicone rubber with anti creepage trace ability and high heat conductance.
The technical scheme that the present invention realizes is as follows: present invention aluminium hydroxide (ATH) and two kinds of inorganic nanoparticles of boron nitride (BN) are as filler, be combined with silicone rubber in mixing and doping mode, obtained thermal conductivity and the extraordinary unitary of anti creepage trace ability, binary doped silicon rubber composite insulation material.
The present invention is a kind of has excellent anti creepage trace ability and the silicone rubber of high heat conductance, including methyl vinyl silicone rubber matrix, inorganic nanoparticles, vulcanizing agent, cross-linking agent (TAIC), hydroxy silicon oil and silane coupler.The raw materials quality score ratio that described silicone rubber is constituted is:
Methyl vinyl silicone rubber matrix: be set to 1, the mass percent of other raw materials is the most below；
Inorganic nanoparticles: 25 ~ 100%；Vulcanizing agent: 0.5%；TAIC:0.5%；Hydroxy silicon oil: 1%；Silane coupler: 5%.
Described inorganic nanoparticles filler is ATH and BN；
The particle diameter of ATH nanoparticle fillers be the particle diameter of 50nm, BN nanoparticle fillers be 50nm.
Described ATH nanoparticle fillers is respectively as follows: with 5 kinds of doping quality fraction set conjunctions of BN nanoparticle fillers
ATH nanoparticle fillers doping is 100%；
BN nanoparticle fillers doping is 100%；
ATH nanoparticle fillers doping 25%, BN nanoparticle fillers doping 75%；
ATH nanoparticle fillers doping 50%, BN nanoparticle fillers doping 50%；
ATH nanoparticle fillers doping 75%, BN nanoparticle fillers doping 25%；
Described vulcanizing agent is double-2, and 5 vulcanizing agents, silane coupler is VTES.
The preparation method of described silicone rubber is:
(1) taking ethanol and pour beaker into, add silane coupler in ethanol, add acetic acid and water, stirring obtains silane-water solution；
(2) adding in silane-water solution by inorganic nanoparticles, stirring obtains inorganic nano-particle aqueous solution；
(3) being placed on rubber mixing machine by methyl vinyl silicone rubber matrix, be gradually added into nanoparticle aqueous solution after bag roller, mixing uniformly obtain the blend of silicone rubber and emulsion, heating roller makes ethanol volatilize；
(4) treat that roller temperature is down to less than 25 DEG C, be sequentially added into hydroxy silicon oil, TAIC, vulcanizing agent, mixing uniformly, obtain elastomeric compound；
(5) elastomeric compound is put in mould, use vulcanizing press, carry out one step cure；
(6) after one step cure terminates, put in convection oven, carry out post vulcanization, after post vulcanization terminates, cool down and take out, obtain final sample.
The mass fraction adding ethanol in described step (1) is 3:2 with the ratio of inorganic nanoparticles mass fraction in step (2).
Adding the mass fraction of acetic acid in described step (1) is 1:450 with the ratio of ethanol mass fraction.
Adding the mass fraction of water in described step (1) is 1:4 with the ratio of silane coupler mass fraction.
In described step (1), silane coupler aqueous solution uses electromagnetic mixer to be stirred, and mixing time is 40min；In described step (2), inorganic nano-particle aqueous solution uses electromagnetic mixer to be stirred, and mixing time is 40min.
In described step (5), one step cure needs the 15MPa that pressurizes, and temperature is 160 DEG C, and the time is 20min；Post vulcanization temperature is 180 DEG C, time 5h.
The invention has the beneficial effects as follows, the present invention, by ATH and BN that adulterate in silicone rubber, is greatly improved anti creepage trace ability and the thermal conductivity of silicone rubber.BN doping can strengthen the adhesion with silicone rubber matrix, and have the biggest lifting to sample thermal conductivity, but anti creepage trace ability is more weak；ATH doping can strengthen the anti creepage trace ability of sample, but be combined more weak with silicone rubber matrix；When ATH doping is 75%, and BN doping is 25%, the anti creepage trace ability of silicone rubber reaches optimal, and promotes the thermal conductivity of silicone rubber substantially, and this proportioning is the optimum proportioning of binary doped silicone rubber sample.
Accompanying drawing explanation
Fig. 1 is the silicone rubber preparation flow block diagram of anti creepage trace ability of the present invention and high heat conductance；
Fig. 2 (a) is the thermal conductivity variation with temperature curve comparison figure of silicone rubber sample in embodiment 1, embodiment 2；
Fig. 2 (b) is the thermal conductivity variation with temperature curve comparison figure of the silicone rubber sample in embodiment 3, embodiment 4 and embodiment 5；
Fig. 3 (a) is embodiment 1 and the average quality loss comparison diagram that embodiment 5 creepage trace experiment artificial pollution liquid is during A liquid 50；
Fig. 3 (b) is embodiment 1 and the average quality loss comparison diagram that embodiment 5 creepage trace experiment artificial pollution liquid is during B liquid 100；
Fig. 4 (a) is the SEM figure of silicone rubber sample in embodiment 1；
Fig. 4 (b) is the SEM figure of silicone rubber sample in embodiment 2；
Fig. 4 (c) is the SEM figure of silicone rubber sample in embodiment 4；
Fig. 5 (a) is the TG curve of silicone rubber sample in embodiment 1；
Fig. 5 (b) is the TG curve of silicone rubber sample in embodiment 2.
Detailed description of the invention
Below in conjunction with drawings and Examples, the invention will be further described.
The present invention implements step as shown in Figure 1.
Embodiment 1:
(1) taking mass fraction is that 100%(is relative to silicone rubber matrix) nanometer ATH, nanoparticle is carried out surface process, step is: takes the ethanol that mass fraction is 150% and pours beaker into, sequentially add the silane coupler that mass fraction is 5%, mass fraction be 0.3% acetic acid and mass fraction be the water of 1.25%, regulation solution ph is about 5, makes silane coupler be fully hydrolyzed with electromagnetic mixer stirring 40min, obtains silane-water solution；ATH particle is added in silane-water solution, stirs 40min with electromagnetic mixer, obtain inorganic nano-particle solution.
(2) silicone rubber matrix mixes with inorganic nano-particle solution: be placed on rubber mixing machine by methyl vinyl silicone rubber matrix, the inorganic nano-particle solution being gradually added in step 1) after bag roller, mixing uniformly obtaining the blend of silicone rubber and emulsion, heating roller makes ethanol volatilize afterwards；
(3) add other auxiliary agent: treat that roller temperature is down to less than 25 DEG C, be sequentially added into hydroxy silicon oil that mass fraction is 1%, mass fraction be 0.5% TAIC, mass fraction be the vulcanizing agent of 0.5%, mixing uniformly, obtain elastomeric compound；
(4) carrying out one section and post vulcanization: put into by elastomeric compound in metal die, use vulcanizing press, adjusting temperature is 160 DEG C, and pressure is 15MPa, carries out one step cure, and cure time is 20min；After one step cure terminates, putting in convection oven, adjusting temperature is 180 DEG C, carries out post vulcanization, and cure time is 5h；After post vulcanization terminates, cool down and take out, obtain final sample.
Embodiment 2
By the ATH that the mass fraction in embodiment 1 is 100%, the nanoparticle of doping is replaced with the BN that mass fraction is 100%, and the consumption of other reagent is constant；Other steps are same as in Example 1.
Fig. 2 (a) be sample preparation environment identical with other reagent dosage proportionings in the case of, doping particle is respectively the ATH of 100%, BN(embodiment 1-2 of 100%) thermal conductivity variation with temperature curve comparison figure, find that ATH and BN all has castering action to silicone rubber thermal conductivity, and the thermal conductivity ascensional range of BN filled silicon rubber is more than ATH filling, reaches as high as 0.6Wm-1k-1。
Embodiment 3
By the ATH that the mass fraction in embodiment 1 is 100%, the nanoparticle of doping being replaced with ATH that mass fraction is 25% and mass fraction is the BN of 75%, the consumption of other reagent is constant；Other steps are same as in Example 1.
Embodiment 4
By the ATH that the mass fraction in embodiment 1 is 100%, the nanoparticle of doping being replaced with ATH that mass fraction is 50% and mass fraction is the BN of 50%, the consumption of other reagent is constant；Other steps are same as in Example 1.
Embodiment 5
By the ATH that the mass fraction in embodiment 1 is 100%, the nanoparticle of doping being replaced with ATH that mass fraction is 75% and mass fraction is the BN of 25%, the consumption of other reagent is constant；Other steps are same as in Example 1.
Fig. 2 (b) be sample preparation environment identical with other reagent dosage proportionings in the case of, binary doped sample (embodiment 3-5) the thermal conductivity variation with temperature curve comparison figure that doping particle ratio is different, finding that the thermal conductivity of binary doped sample promotes along with BN doping and promotes, this is possibly due to the thermal conductivity of BN itself, and bigger than ATH (BN thermal conductivity is 33 Wm-1K-1).
In creepage trace is tested, ATH unitary doped silicon rubbery sample anti creepage trace ability is strong, and BN unitary doping sample is easily formed surface carbonation path during creepage trace, and for insulator, carbonized path can cause insulator surface breakdown and lose efficacy；Binary doped sample B N doping is unsuitable too much the most still can form carbonized path, and when ATH doping is 75%, and BN doping is 25%, sample anti creepage trace ability is the strongest.
Fig. 3 (a) is that two kinds of samples (embodiment 1, the embodiment 5) creepage trace that in unitary and binary doped sample, anti creepage trace ability is the strongest tests average quality loss comparison diagram when artificial pollution liquid is A liquid 50；Fig. 3 (b) is that two kinds of samples (embodiment 1, the embodiment 5) creepage trace that in unitary and binary doped sample, anti creepage trace ability is the strongest tests average quality loss comparison diagram when artificial pollution liquid is B liquid 100, it can be seen that binary doped silicone rubber sample anti creepage trace ability is substantially better than unitary doping sample.
Fig. 4 (a), Fig. 4 (b), Fig. 4 (c) are respectively the SEM figure of the silicone rubber sample (embodiment 1, embodiment 2, embodiment 4) adding different nanoparticle, find that BN doping sample is combined very well with silicone rubber matrix, but ATH doping can form a kind of chondritic with silicone rubber matrix effect, this structure is weak with the silicone rubber matrix bond strength of surrounding, and the addition of binary doped middle BN makes chondritic significantly reduce.
Fig. 5 (a) and Fig. 5 (b) is the TG curve of unitary doped silicon rubber (embodiment 1, embodiment 2), it appeared that, ATH adds makes silicone rubber sample decomposition temperature move to low temperature, in creepage trace is tested, ATH doped silicon rubbery sample catabolic process constantly absorbs heat, makes specimen surface temperature reduce, and the carbon produced with specimen surface reacts, prevent that carbonized path, ATH doped silicon rubber have good anti creepage trace ability.
In sum, BN doping can strengthen the adhesion with silicone rubber matrix, and have the biggest lifting to sample thermal conductivity, but anti creepage trace ability is more weak；ATH doping can strengthen the anti creepage trace ability of sample, but be combined more weak with silicone rubber matrix；When ATH doping is 75%, and BN doping is 25%, the anti creepage trace ability of silicone rubber reaches optimal, and promotes the thermal conductivity of silicone rubber substantially, and this proportioning is the optimum proportioning of binary doped silicone rubber sample.
Claims (10)
1. one kind has excellent anti creepage trace ability and the silicone rubber of high heat conductance, it is characterised in that the raw materials quality score ratio that described silicone rubber is constituted is:
Methyl vinyl silicone rubber matrix: be set to 1, the mass percent of other raw materials is the most below；
Inorganic nanoparticles: 25 ~ 100%；
Vulcanizing agent: 0.5%；
TAIC:0.5%；
Hydroxy silicon oil: 1%；
Silane coupler: 5%.
A kind of have excellent anti creepage trace ability and the silicone rubber of high heat conductance, it is characterised in that:
Described inorganic nanoparticles filler is ATH and BN；
The particle diameter of ATH nanoparticle fillers be the particle diameter of 50nm, BN nanoparticle fillers be 50nm.
A kind of have excellent anti creepage trace ability and the silicone rubber of high heat conductance, it is characterised in that:
Described ATH nanoparticle fillers is respectively as follows: with 5 kinds of doping quality fraction set conjunctions of BN nanoparticle fillers
ATH nanoparticle fillers doping is 100%；
BN nanoparticle fillers doping is 100%；
ATH nanoparticle fillers doping 25%, BN nanoparticle fillers doping 75%；
ATH nanoparticle fillers doping 50%, BN nanoparticle fillers doping 50%；
ATH nanoparticle fillers doping 75%, BN nanoparticle fillers doping 25%.
A kind of have excellent anti creepage trace ability and the silicone rubber of high heat conductance, it is characterised in that: described vulcanizing agent is double-2, and 5 vulcanizing agents, silane coupler is VTES.
A kind of have excellent anti creepage trace ability and the silicone rubber of high heat conductance, it is characterised in that the preparation method of described silicone rubber is:
(1) taking ethanol and pour beaker into, add silane coupler in ethanol, add acetic acid and water, stirring obtains silane-water solution；
(2) adding in silane-water solution by inorganic nanoparticles, stirring obtains inorganic nano-particle aqueous solution；
(3) being placed on rubber mixing machine by methyl vinyl silicone rubber matrix, be gradually added into nanoparticle aqueous solution after bag roller, mixing uniformly obtain the blend of silicone rubber and emulsion, heating roller makes ethanol volatilize；
(4) treat that roller temperature is down to less than 25 DEG C, be sequentially added into hydroxy silicon oil, TAIC, vulcanizing agent, mixing uniformly, obtain elastomeric compound；
(5) elastomeric compound is put in mould, use vulcanizing press, carry out one step cure；
(6) after one step cure terminates, put in convection oven, carry out post vulcanization, after post vulcanization terminates, cool down and take out, obtain final sample.
A kind of preparation method of the silicone rubber with excellent anti creepage trace ability and high heat conductance, it is characterised in that: the mass fraction adding ethanol in described step (1) is 3:2 with the ratio of inorganic nanoparticles mass fraction in step (2).
A kind of have excellent anti creepage trace ability and the silicone rubber of high heat conductance, it is characterised in that: adding the mass fraction of acetic acid in described step (1) is 1:450 with the ratio of ethanol mass fraction.
A kind of have excellent anti creepage trace ability and the silicone rubber of high heat conductance, it is characterised in that: adding the mass fraction of water in described step (1) is 1:4 with the ratio of silane coupler mass fraction.
A kind of have excellent anti creepage trace ability and the silicone rubber of high heat conductance, it is characterised in that: in described step (1), silane coupler aqueous solution uses electromagnetic mixer to be stirred, and mixing time is 40min；In described step (2), inorganic nano-particle aqueous solution uses electromagnetic mixer to be stirred, and mixing time is 40min.
The most according to claim 5 a kind of have excellent anti creepage trace ability and the silicone rubber of high heat conductance, it is characterised in that: in described step (5), one step cure needs the 15MPa that pressurizes, and temperature is 160 DEG C, and the time is 20min；Post vulcanization temperature is 180 DEG C, time 5h.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106433283A (en) * | 2016-10-13 | 2017-02-22 | 重庆大学 | Preparing method of high thermal conductivity super-hydrophobic glass insulator painting |
| CN107033602A (en) * | 2017-05-17 | 2017-08-11 | 醴陵市时代鑫湘科技有限公司 | Used in composite insulator high-strength silicone rubber insulating materials |
| CN107129689A (en) * | 2017-04-18 | 2017-09-05 | 华南理工大学 | High-performance anti creepage trace add-on type liquid silicon rubber composition and preparation method thereof |
| CN110483863A (en) * | 2019-08-01 | 2019-11-22 | 中国南方电网有限责任公司超高压输电公司检修试验中心 | A kind of anti creepage trace neoprene packing material and preparation method thereof |
| CN114420360A (en) * | 2022-01-08 | 2022-04-29 | 马鞍山新地优特威光纤光缆有限公司 | Loose sleeve layer stranded flame-retardant cable for coal mine |
| CN114874632A (en) * | 2022-06-13 | 2022-08-09 | 温州益坤电气股份有限公司 | Anti-fouling wear-resistant silicon rubber material for high-speed motor train unit and preparation method thereof |
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| CN102585506A (en) * | 2011-12-20 | 2012-07-18 | 西安交通大学 | Silicon rubber with excellent electric arc resistant performance and preparation method thereof |
| CN104845378A (en) * | 2015-03-20 | 2015-08-19 | 国家电网公司 | Silicon rubber composition with high-voltage electric corrosion resistance for composite insulator and preparation method of silicon rubber composition |
| CN105238055A (en) * | 2015-09-25 | 2016-01-13 | 宿松县焕然机电有限责任公司 | Motor slot wedge heat-resistance insulation composite material and preparation method thereof |
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| CN102585506A (en) * | 2011-12-20 | 2012-07-18 | 西安交通大学 | Silicon rubber with excellent electric arc resistant performance and preparation method thereof |
| CN104845378A (en) * | 2015-03-20 | 2015-08-19 | 国家电网公司 | Silicon rubber composition with high-voltage electric corrosion resistance for composite insulator and preparation method of silicon rubber composition |
| CN105238055A (en) * | 2015-09-25 | 2016-01-13 | 宿松县焕然机电有限责任公司 | Motor slot wedge heat-resistance insulation composite material and preparation method thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106433283A (en) * | 2016-10-13 | 2017-02-22 | 重庆大学 | Preparing method of high thermal conductivity super-hydrophobic glass insulator painting |
| CN107129689A (en) * | 2017-04-18 | 2017-09-05 | 华南理工大学 | High-performance anti creepage trace add-on type liquid silicon rubber composition and preparation method thereof |
| CN107033602A (en) * | 2017-05-17 | 2017-08-11 | 醴陵市时代鑫湘科技有限公司 | Used in composite insulator high-strength silicone rubber insulating materials |
| CN110483863A (en) * | 2019-08-01 | 2019-11-22 | 中国南方电网有限责任公司超高压输电公司检修试验中心 | A kind of anti creepage trace neoprene packing material and preparation method thereof |
| CN110483863B (en) * | 2019-08-01 | 2021-09-21 | 中国南方电网有限责任公司超高压输电公司检修试验中心 | Tracking-resistant chloroprene rubber sealing material and preparation method thereof |
| CN114420360A (en) * | 2022-01-08 | 2022-04-29 | 马鞍山新地优特威光纤光缆有限公司 | Loose sleeve layer stranded flame-retardant cable for coal mine |
| CN114874632A (en) * | 2022-06-13 | 2022-08-09 | 温州益坤电气股份有限公司 | Anti-fouling wear-resistant silicon rubber material for high-speed motor train unit and preparation method thereof |
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Application publication date: 20161012 |