CN105086465B - A kind of high heat conduction flame-proof silicon rubber composition and preparation method thereof - Google Patents
A kind of high heat conduction flame-proof silicon rubber composition and preparation method thereof Download PDFInfo
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- CN105086465B CN105086465B CN201510481653.0A CN201510481653A CN105086465B CN 105086465 B CN105086465 B CN 105086465B CN 201510481653 A CN201510481653 A CN 201510481653A CN 105086465 B CN105086465 B CN 105086465B
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Abstract
The invention discloses a kind of high heat conduction flame retardant rubber composition, in parts by weight, including following components：30 60 parts of polydimethyldiphenyl vinylsiloxane, 20 50 parts of hydroxy-end capped dimethyl silicone polymer, 10 20 parts of wollastonite, 5 15 parts of nm-class boron nitride, 13 parts of nano-sized magnesium hydroxide, 5 10 parts of vinyl silicone oil, 0.5 5 parts of crosslinking agent, 14 parts of catalyst, 0.5 3.5 parts of dispersant.The invention also discloses the preparation method of the rubber composition.The rubber composition thermal conductivity is good, and excellent fireproof performance, high- and low-temperature resistance, ageing-resistant, chemical resistance is good, there is preferable insulating properties, and release property is good, nontoxic.
Description
Technical field：
The present invention relates to polymeric material field, a kind of high heat conduction flame-proof silicon rubber composition is specifically related to.
Background technology：
Silicon rubber is the macromolecular elastomer using Si-O-Si as main chain, compared with natural rubber and other synthetic rubber, silicon
Rubber has high- and low-temperature resistance, ageing-resistant, electric insulation, physiological inertia, a series of excellent properties such as release property is good, in aviation boat
My god, electric, chemical industry, machinery, building, communications and transportation, be widely used in terms of health care.It is high temperature vulcanized
Rubber ratio liquid silastic has higher heat endurance, while having excellent simulation quality and release property.
But with the development of science and technology, traditional melting silicone rubber material has been difficult to meet particular/special requirement, therefore tool
The liquid silicon rubber material of standby specific function arises at the historic moment, such as fire-retardant, heat-conducting silicon rubber.At present, modified liquid silicon rubber
Method mainly has：Add functional stuffing, change filler composition and proportioning, to silicon rubber main chain carry out graft modification or and its
His high polymer material blending etc..
The content of the invention：
It is an object of the present invention to provide a kind of high heat conduction flame-proof silicon rubber composition, its thermal conductivity is good, and excellent fireproof performance is resistance to
High and low temperature, ageing-resistant, chemical resistance is good, there is preferable insulating properties, and release property is good, nontoxic.
It is a further object to provide the preparation method of the high heat conduction flame-proof silicon rubber composition.
To achieve the above object, the present invention uses following technical scheme：
A kind of high heat conduction flame-proof silicon rubber composition, in parts by weight, including following components：
30-60 parts of polydimethyldiphenyl vinylsiloxane,
20-50 parts of hydroxy-end capped dimethyl silicone polymer,
10-20 parts of wollastonite, 5-15 parts of nm-class boron nitride,
1-3 parts of nano-sized magnesium hydroxide, 5-10 parts of vinyl silicone oil,
0.5-5 parts of crosslinking agent, 1-4 parts of catalyst, 0.5-3.5 parts of dispersant.
As the preferred of above-mentioned technical proposal, a kind of high heat conduction flame-proof silicon rubber composition, in parts by weight, including it is following
Component：
50 parts of polydimethyldiphenyl vinylsiloxane,
50 parts of hydroxy-end capped dimethyl silicone polymer,
12 parts of wollastonite, 10 parts of nm-class boron nitride,
2.5 parts of nano-sized magnesium hydroxide, 8 parts of vinyl silicone oil,
3 parts of crosslinking agent, 1.5 parts of catalyst, 1 part of dispersant.
As the preferred of above-mentioned technical proposal, the particle size of the wollastonite is 1-2 μm.
As the preferred of above-mentioned technical proposal, the particle size of the nm-class boron nitride is 80-100nm.
As the preferred of above-mentioned technical proposal, the particle size of the nano-sized magnesium hydroxide is 30-40nm.
As the preferred of above-mentioned technical proposal, the crosslinking agent be gamma-aminopropyl-triethoxy-silane, N- β (aminoethyl)-
One or both of γ aminopropyl trimethoxysilanes are mixed.
As the preferred of above-mentioned technical proposal, the catalyst is the isostearoyl epoxide titanate esters of isopropyl three, four isopropyls
One or more mixing in base double (two pungent phosphates) titanate esters, iso-cyanuric acid triallyl esters.
As the preferred of above-mentioned technical proposal, the dispersant is Emulsifier EL-60, guar gum, polyoxyethylene
One or more mixing in sugar alcohol acid anhydride monoleate, sorbitan monooleate.
A kind of preparation method of high heat conduction flame-proof silicon rubber composition, comprises the following steps：
(1) wollastonite, nm-class boron nitride, nano-sized magnesium hydroxide, vinyl silicone oil, dispersant and absolute ethyl alcohol are mixed and stirred
Mix uniform, the ultrasound 2-5h under 800-1000W power is stirred at 60-80 DEG C, is removed absolute ethyl alcohol, is obtained mixed material；
(2) mixed material for obtaining step (1) is transferred in banbury, adds polydimethyldiphenyl vinyl silica
Alkane, hydroxy-end capped dimethyl silicone polymer, crosslinking agent, catalyst, it is 0.05-0.1MPa to keep vacuum state vacuum,
Kneaded 1-2 hours at 150-180 DEG C, stop vacuum, 30-60min is stirred in the state of 5000-8000 revs/min, height is obtained and leads
Thermal resistance fires rubber composition.
As the preferred of above-mentioned technical proposal, in step (1), the ultrasonic power is 1000W, the ultrasonic time
For 3h.
The invention has the advantages that：
The present invention is changed using dispersant, vinyl silicone oil to wollastonite, nm-class boron nitride, nano-sized magnesium hydroxide first
Property, make its stable dispersion in system, it is the thin slice within 10nm that nm-class boron nitride, which is stripped into thickness, in the presence of ultrasound,
It causes the thermal conductivity of silicon rubber to greatly improve, larger mainly due to thermal conductivity factor of the boron nitride on its (002) crystal face；Receive
Rice magnesium hydroxide, the synergy of wollastonite so that silicon rubber flame-retardant performance is improved；
The rubber composition high- and low-temperature resistance that the present invention is provided, ageing-resistant, chemical resistance is good, there is preferable insulating properties, takes off
Mould is good, nontoxic.
Embodiment：
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solution
The present invention is released, any restriction will not be constituted to the present invention.
Embodiment 1
A kind of high heat conduction flame-proof silicon rubber composition, in parts by weight, including following components：
30 parts of polydimethyldiphenyl vinylsiloxane,
20 parts of hydroxy-end capped dimethyl silicone polymer,
10 parts of wollastonite, 5 parts of nm-class boron nitride,
1 part of nano-sized magnesium hydroxide, 5 parts of vinyl silicone oil,
0.5 part of crosslinking agent, 1 part of catalyst, 0.5 part of dispersant.
Its preparation method comprises the following steps：
(1) wollastonite, nm-class boron nitride, nano-sized magnesium hydroxide, vinyl silicone oil, dispersant and absolute ethyl alcohol are mixed and stirred
Mix uniform, the ultrasound 2h under 800W power is stirred at 60 DEG C, is removed absolute ethyl alcohol, is obtained mixed material；
(2) mixed material for obtaining step (1) is transferred in banbury, adds polydimethyldiphenyl vinyl silica
Alkane, hydroxy-end capped dimethyl silicone polymer, crosslinking agent, catalyst, it is 0.05-0.1MPa to keep vacuum state vacuum,
Kneaded 1 hour at 150 DEG C, stop vacuum, stir 30min in the state of 5000 revs/min, obtain high heat conduction flame-proof silicon rubber group
Compound.
Embodiment 2
A kind of high heat conduction flame-proof silicon rubber composition, in parts by weight, including following components：
60 parts of polydimethyldiphenyl vinylsiloxane,
50 parts of hydroxy-end capped dimethyl silicone polymer,
20 parts of wollastonite, 15 parts of nm-class boron nitride,
3 parts of nano-sized magnesium hydroxide, 10 parts of vinyl silicone oil,
5 parts of crosslinking agent, 4 parts of catalyst, 3.5 parts of dispersant.
Its preparation method comprises the following steps：
(1) wollastonite, nm-class boron nitride, nano-sized magnesium hydroxide, vinyl silicone oil, dispersant and absolute ethyl alcohol are mixed and stirred
Mix uniform, the ultrasound 5h under 1000W power is stirred at 80 DEG C, is removed absolute ethyl alcohol, is obtained mixed material；
(2) mixed material for obtaining step (1) is transferred in banbury, adds polydimethyldiphenyl vinyl silica
Alkane, hydroxy-end capped dimethyl silicone polymer, crosslinking agent, catalyst, it is 0.05-0.1MPa to keep vacuum state vacuum,
Kneaded 2 hours at 180 DEG C, stop vacuum, stir 60min in the state of 8000 revs/min, obtain high heat conduction flame-proof silicon rubber group
Compound.
Embodiment 3
A kind of high heat conduction flame-proof silicon rubber composition, in parts by weight, including following components：
40 parts of polydimethyldiphenyl vinylsiloxane,
30 parts of hydroxy-end capped dimethyl silicone polymer,
12 parts of wollastonite, 7 parts of nm-class boron nitride,
1.5 parts of nano-sized magnesium hydroxide, 6 parts of vinyl silicone oil,
1 part of crosslinking agent, 2 parts of catalyst, 1 part of dispersant.
Its preparation method comprises the following steps：
(1) wollastonite, nm-class boron nitride, nano-sized magnesium hydroxide, vinyl silicone oil, dispersant and absolute ethyl alcohol are mixed and stirred
Mix uniform, the ultrasound 3h under 850W power is stirred at 65 DEG C, is removed absolute ethyl alcohol, is obtained mixed material；
(2) mixed material for obtaining step (1) is transferred in banbury, adds polydimethyldiphenyl vinyl silica
Alkane, hydroxy-end capped dimethyl silicone polymer, crosslinking agent, catalyst, it is 0.05-0.1MPa to keep vacuum state vacuum,
Kneaded 1.2 hours at 165 DEG C, stop vacuum, stir 40min in the state of 6000 revs/min, obtain high heat conduction flame-proof silicon rubber
Composition.
Embodiment 4
A kind of high heat conduction flame-proof silicon rubber composition, in parts by weight, including following components：
45 parts of polydimethyldiphenyl vinylsiloxane,
35 parts of hydroxy-end capped dimethyl silicone polymer,
14 parts of wollastonite, 9 parts of nm-class boron nitride,
2 parts of nano-sized magnesium hydroxide, 7 parts of vinyl silicone oil,
2 parts of crosslinking agent, 2.5 parts of catalyst, 1.5 parts of dispersant.
Its preparation method comprises the following steps：
(1) wollastonite, nm-class boron nitride, nano-sized magnesium hydroxide, vinyl silicone oil, dispersant and absolute ethyl alcohol are mixed and stirred
Mix uniform, the ultrasound 3.5h under 900W power is stirred at 70 DEG C, is removed absolute ethyl alcohol, is obtained mixed material；
(2) mixed material for obtaining step (1) is transferred in banbury, adds polydimethyldiphenyl vinyl silica
Alkane, hydroxy-end capped dimethyl silicone polymer, crosslinking agent, catalyst, it is 0.05-0.1MPa to keep vacuum state vacuum,
Kneaded 1.4 hours at 170 DEG C, stop vacuum, stir 45min in the state of 6500 revs/min, obtain high heat conduction flame-proof silicon rubber
Composition.
Embodiment 5
A kind of high heat conduction flame-proof silicon rubber composition, in parts by weight, including following components：
50 parts of polydimethyldiphenyl vinylsiloxane,
40 parts of hydroxy-end capped dimethyl silicone polymer,
16 parts of wollastonite, 11 parts of nm-class boron nitride,
2.5 parts of nano-sized magnesium hydroxide, 8 parts of vinyl silicone oil,
4 parts of crosslinking agent, 3 parts of catalyst, 2 parts of dispersant.
Its preparation method comprises the following steps：
(1) wollastonite, nm-class boron nitride, nano-sized magnesium hydroxide, vinyl silicone oil, dispersant and absolute ethyl alcohol are mixed and stirred
Mix uniform, the ultrasound 4h under 950W power is stirred at 75 DEG C, is removed absolute ethyl alcohol, is obtained mixed material；
(2) mixed material for obtaining step (1) is transferred in banbury, adds polydimethyldiphenyl vinyl silica
Alkane, hydroxy-end capped dimethyl silicone polymer, crosslinking agent, catalyst, it is 0.05-0.1MPa to keep vacuum state vacuum,
Kneaded 1.6 hours at 175 DEG C, stop vacuum, stir 50min in the state of 7000 revs/min, obtain high heat conduction flame-proof silicon rubber
Composition.
Embodiment 6
A kind of high heat conduction flame-proof silicon rubber composition, in parts by weight, including following components：
55 parts of polydimethyldiphenyl vinylsiloxane,
45 parts of hydroxy-end capped dimethyl silicone polymer,
18 parts of wollastonite, 13 parts of nm-class boron nitride,
2.8 parts of nano-sized magnesium hydroxide, 9 parts of vinyl silicone oil,
4.5 parts of crosslinking agent, 3.5 parts of catalyst, 3 parts of dispersant.
Its preparation method comprises the following steps：
(1) wollastonite, nm-class boron nitride, nano-sized magnesium hydroxide, vinyl silicone oil, dispersant and absolute ethyl alcohol are mixed and stirred
Mix uniform, the ultrasound 4.5h under 980W power is stirred at 80 DEG C, is removed absolute ethyl alcohol, is obtained mixed material；
(2) mixed material for obtaining step (1) is transferred in banbury, adds polydimethyldiphenyl vinyl silica
Alkane, hydroxy-end capped dimethyl silicone polymer, crosslinking agent, catalyst, it is 0.05-0.1MPa to keep vacuum state vacuum,
Kneaded 1..8 hours at 180 DEG C, stop vacuum, stir 55min in the state of 7500 revs/min, obtain the fire-retardant silicon rubber of high heat conduction
Glue composition.
Performance test is carried out to the rubber composition that the present invention is provided below.
(1) mechanical property
Silicon rubber standard test piece is made, is intercepted respectively with dumbbell and right angle cut-off knife.Tensile strength uses GB/T 528-1998
Tested, tearing strength is tested using GB/T 529-1999.
Table 1
(2) fire resistance
Oxygen index (OI) is tested by GB/T 10707-1989, and vertical combustion is tested according to GB/T 13448-1992.
Table 2
(3) heat conductivility
Thermal conductivity is tested according to GB11205-1989, and liquid nitrogen makees cooling agent, 30-150 DEG C of temperature elevating range, heating rate
10 DEG C/min, sample thickness is 2mm, a diameter of 2cm circular test piece.
Table 3
From the point of view of table 1,2,3, the Mechanical Properties of Silicone Rubber that the present invention is provided is excellent, and flame-retarded heat-conducting effect is good.
Claims (9)
1. a kind of high heat conduction flame-proof silicon rubber composition, it is characterised in that in parts by weight, including following components：
30-60 parts of polydimethyldiphenyl vinylsiloxane,
20-50 parts of hydroxy-end capped dimethyl silicone polymer,
10-20 parts of wollastonite, 5-15 parts of nm-class boron nitride,
1-3 parts of nano-sized magnesium hydroxide, 5-10 parts of vinyl silicone oil,
0.5-5 parts of crosslinking agent, 1-4 parts of catalyst, 0.5-3.5 parts of dispersant；
Its preparation method comprises the following steps：
(1) wollastonite, nm-class boron nitride, nano-sized magnesium hydroxide, vinyl silicone oil, dispersant and absolute ethyl alcohol are mixed equal
Even, the ultrasound 2-5h under 800-1000W power is stirred at 60-80 DEG C, is removed absolute ethyl alcohol, is obtained mixed material；
(2) mixed material for obtaining step (1) is transferred in banbury, addition polydimethyldiphenyl vinylsiloxane,
Hydroxy-end capped dimethyl silicone polymer, crosslinking agent, catalyst, it is 0.05-0.1MPa to keep vacuum state vacuum, in 150-
Kneaded 1-2 hours at 180 DEG C, stop vacuum, 30-60min is stirred in the state of 5000-8000 revs/min, obtain high heat conduction resistance
Fire rubber composition.
2. a kind of high heat conduction flame-proof silicon rubber composition as claimed in claim 1, it is characterised in that in parts by weight, including
Following components：
50 parts of polydimethyldiphenyl vinylsiloxane,
50 parts of hydroxy-end capped dimethyl silicone polymer,
12 parts of wollastonite, 10 parts of nm-class boron nitride,
2.5 parts of nano-sized magnesium hydroxide, 8 parts of vinyl silicone oil,
3 parts of crosslinking agent, 1.5 parts of catalyst, 1 part of dispersant.
3. a kind of high heat conduction flame-proof silicon rubber composition as claimed in claim 1, it is characterised in that the particle diameter of the wollastonite
Size is 1-2 μm.
4. a kind of high heat conduction flame-proof silicon rubber composition as claimed in claim 1, it is characterised in that the nm-class boron nitride
Particle size is 80-100nm.
5. a kind of high heat conduction flame-proof silicon rubber composition as claimed in claim 1, it is characterised in that the nano-sized magnesium hydroxide
Particle size be 30-40nm.
6. a kind of high heat conduction flame-proof silicon rubber composition as claimed in claim 1, it is characterised in that the crosslinking agent be γ-
One or both of aminopropyl triethoxysilane, N- β (aminoethyl)-γ aminopropyl trimethoxysilanes are mixed.
7. a kind of high heat conduction flame-proof silicon rubber composition as claimed in claim 1, it is characterised in that the catalyst is isopropyl
In the isostearoyl epoxide titanate esters of base three, tetra isopropyl double (two pungent phosphates) titanate esters, iso-cyanuric acid triallyl esters
One or more mixing.
8. a kind of high heat conduction flame-proof silicon rubber composition as claimed in claim 1, it is characterised in that the dispersant is polyoxy
One or more in ethylene castor oil, guar gum, polyoxyethylene sorbitan monooleate, sorbitan monooleate
Mixing.
9. a kind of high heat conduction flame-proof silicon rubber composition as claimed in claim 1, it is characterised in that in step (1), described super
The power of sound is 1000W, and the ultrasonic time is 3h.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103131381A (en) * | 2013-03-06 | 2013-06-05 | 广州市高士实业有限公司 | High-performance environmentally-friendly flame retardant type organic electron pouring sealant and preparation method thereof |
| CN103289414A (en) * | 2012-02-29 | 2013-09-11 | 中化蓝天集团有限公司 | Heat-resistant and flame-retardant room-temperature vulcanized silicone rubber composition |
| CN103483829A (en) * | 2013-09-30 | 2014-01-01 | 江苏天辰硅材料有限公司 | High-temperature-resistant and flame-retardant silicone rubber and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103289414A (en) * | 2012-02-29 | 2013-09-11 | 中化蓝天集团有限公司 | Heat-resistant and flame-retardant room-temperature vulcanized silicone rubber composition |
| CN103131381A (en) * | 2013-03-06 | 2013-06-05 | 广州市高士实业有限公司 | High-performance environmentally-friendly flame retardant type organic electron pouring sealant and preparation method thereof |
| CN103483829A (en) * | 2013-09-30 | 2014-01-01 | 江苏天辰硅材料有限公司 | High-temperature-resistant and flame-retardant silicone rubber and preparation method thereof |
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