CN101121820A - Halogen-free anti-flaming silicon rubber and its preparing method and use - Google Patents
Halogen-free anti-flaming silicon rubber and its preparing method and use Download PDFInfo
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- CN101121820A CN101121820A CNA2007100461277A CN200710046127A CN101121820A CN 101121820 A CN101121820 A CN 101121820A CN A2007100461277 A CNA2007100461277 A CN A2007100461277A CN 200710046127 A CN200710046127 A CN 200710046127A CN 101121820 A CN101121820 A CN 101121820A
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Abstract
A halogen-free flame retardant silicone rubber is made by the vulcanization of the compound with the methyl vinyl silicone rubber as the basic gel and the vulcanization agent; the compound consists of the two-component mixing gel; according to the weight shares, the compound includes: A component: 10 to 30 shares of methyl vinyl silicone rubber with the high content of vinyl, 20 to 40 shares of methyl vinyl silicone rubber with the low content of vinyl, 0.25 to 1 share of hydrogen silicone oil, 2 to 4 shares of hydroxy silicone oil, 20 to 40 shares of white carbon; B component: 90 to 110 shares of methyl vinyl silicone rubber with the low content of vinyl, 0.5 to 2 shares of methyl silicone oil, 0.25 to 1 share of hydrogen silicone oil, 50 to 70 shares of aluminum hydroxide and virgule or cyanuric melamine, and 2 to 5 shares of zinc borate. The preparation method is to mix and refine well the silicone rubber with the high and low content of vinyl; the hydrogen silicone oil, hydroxy silicone oil and white carbon are added to make the mixed and refined gel A; the silicone rubber with the low content of vinyl, the methyl silicone oil, hydrogen oil, aluminum hydroxide and virgule or cyanuric melamine, zinc borate are added to make the mixed and refined gel B; the mixed and refined gel A and B are mixed and vulcanized ; the fire-retardant performance can reach to the level of FV-0.
Description
Technical field
The present invention relates to a kind of halogen-free anti-flaming silicon rubber and its production and use, especially a kind of halogen-free anti-flaming silicon rubber that is used for coated fiber cloth.
Background technology
The range of application of flame-proof silicon rubber is wide, patent No. ZL97107706.1 discloses and has a kind ofly made the self cure flame-proof silicon rubber that fire retardant prepares with cyanogen urea acid trimeric cyanamide or cyanogen urea acid trimeric cyanamide with decabromodiphynly oxide, has good self-extinguishing when running into flame, and when proposing addition less than 5 weight parts from putting out weak effect, and when being higher than 100 weight parts, the obvious variation of composition process performance is for researchdevelopment afterwards provides the foundation.But its flame retardant properties has certain limitation.
For example apply glasscloth as a kind of emerging product tool vast market prospect with flame-proof silicon rubber, have good electric insulating quality, higher temperature tolerance, can be used as and flexibly connect device and be used for solving and expand with heat and contract with cold to pipeline destroyed the silica gel cloth preservative property, resistance to deterioration, elasticity and flexible good, as non-metal compensator, antiseptic property is good, the intensity height, be applied to construction sealing materials, good flame resistance can be used as fire screen and uses.For these reasons, the applied research that now flame-proof silicon rubber is applied is both at home and abroad paid much attention to.
It is base-material that number of patent application 200410077503.5 discloses a kind of silicon rubber with different contents of ethylene, add containing hydrogen silicone oil, hydroxy silicon oil, strengthening agent, metal hydroxides, and contain Platinic chloride at least, a kind of in the tetrafluoroethylene, this silicon rubber flame-retardant excellent performance, but because Halogen, when the preparation silica gel cloth, can have the strong impulse smell, and be unfavorable for environmental protection, and use aluminium hydroxide, during inorganic combustion inhibitors such as magnesium hydroxide, often to could play useful effect by very big addition, processing characteristics and physical and mechanical properties, the especially tear resistance of this grievous injury silicon rubber that is bound to.
Summary of the invention
The object of the present invention is to provide a kind of flame retardant properties excellence, having no irritating odor is beneficial to the halogen-free anti-flaming silicon rubber of environmental protection.
Another purpose of the present invention is to provide a kind of preparation method of halogen-free anti-flaming silicon rubber.
A further object of the present invention is to provide a kind of purposes of halogen-free fireproof rubber.
The present invention solves the problems of the technologies described above the technical scheme of taking: a kind of halogen-free anti-flaming silicon rubber, form by the composition and the vulcanizing agent sulfuration that with methyl vinyl silicone rubber are basic glue, described composition forms by the two-pack rubber unvulcanizate is mixing, comprises by weight:
The A component:
High-vinyl-content methyl vinyl silicone rubber 10～30
Low vinyl content methyl vinyl silicone rubber 20～40
Containing hydrogen silicone oil 0.25～1
Hydroxy silicon oil 2～4
White carbon black 20～40;
The B component:
Low vinyl content methyl vinyl silicone rubber 90～110
Methyl-silicone oil 0.5～2
Containing hydrogen silicone oil 0.25～1
Aluminium hydroxide+melamine cyanurate 50～70
Zinc borate 2～5;
Wherein, the vinyl molar content of described silicone rubber with high content of vinyl group is 0.2～0.5%, specifically can be: 0.2,0.23,0.25,0.3,0.35,0.4,0.45,0.5%; The vinyl molar content of described low vinyl content silicon rubber is 0.03～0.10%, specifically can be: 0.03,0.04,0.05,0.06,0.07,0.08,0.09,0.10%.
In the A component, high-vinyl-content methyl vinyl silicone rubber consumption can be: 10,12,14,16,18,20,22,24,26,28,30; Low vinyl content methyl vinyl silicone rubber consumption can be: 20,22,25,27,30,33,35,38,40; The containing hydrogen silicone oil consumption can be: 0.25,0.3,0.35,0.4,0.45,0.5,0.55,0.6,0.7,0.8,0.9,1; The hydroxy silicon oil consumption can be: 2,2.2,2.5,2.7,3,3.2,3.5,3.7,4; The about 380m of the preferred reference area of described white carbon black
2/ g, consumption can be: 20,22,25,28,30,32,35,38,40.
In the B component, low vinyl content methyl vinyl silicone rubber consumption can be 90,92,94,96,98,100,102,104,106,108,110; The methyl-silicone oil consumption can be: 0.5,0.6,0.7,0.8,0.9,1,1.1,1.2,1.5,1.8,2; The containing hydrogen silicone oil consumption can be 0.25,0.3,0.4,0.5,0.6,0.65,0.7,0.75,0.8,0.85,0.9,0.95,1; Aluminium hydroxide and/or melamine cyanurate (MCA) consumption can be: 50,52,55,58,60,63,65,67,70; The zinc borate consumption can be: 2,3,4,4.3,4.5,4.8,5.
A kind of preparation method of above-mentioned halogen-free anti-flaming silicon rubber comprises the steps:
(1) high-vinyl-content methyl vinyl silicone rubber and low vinyl content methyl vinyl silicone rubber is mixing evenly;
(2) in the mixture of (1), add containing hydrogen silicone oil, hydroxy silicon oil and gas-phase silica, mixing, make rubber unvulcanizate A;
(3) the low vinyl content methyl vinyl silicone rubber is mixing evenly, add methyl-silicone oil, containing hydrogen silicone oil, mixing even;
(4) in the mixture of (3), add aluminium hydroxide and/or melamine cyanurate, zinc borate, mixing, make rubber unvulcanizate B;
(5) rubber unvulcanizate A, the B that (2) and (4) is made mixes, and adds vulcanizing agent and vulcanizes, and makes silicon rubber.
On the basis of such scheme, mixing in the described step (4), be included in 150～200 ℃ mixing 2～4 hours down, cooling is carried out the secondary back mixing with the sizing material after mixing, makes rubber unvulcanizate B.
A kind of preparation method is provided on the basis of such scheme, and described sulfuration process makes sulphurated siliastic for the mixture with (5) adds vulcanizing agent through sulfuration.
Another kind of preparation method is provided, described sulfuration process adds solvent sherwood oil or No. 120 gasoline for the mixture with (5), mixture and solvent are 1: 1.5～2.5 by weight, after preferably mixing by weight 1: 2, add vulcanizing agent, being uniformly dispersed through high-speed stirring is coated on the cloth cover, makes sulphurated siliastic based on cloth cover through sulfuration.
A kind of purposes of above-mentioned halogen-free anti-flaming silicon rubber is used to prepare silicon rubber flame-retardant cloth.
On the such scheme basis, described cloth is glasscloth.
The invention has the beneficial effects as follows:
1, silicon of the present invention on the basis of fire retardant aluminium hydroxide and melamine cyanurate and usefulness, by composite with zinc borate, produces the cooperative flame retardant effect as glue flame retardant properties excellence, and flame retardant properties reaches the FV-0 level;
2, silicon rubber of the present invention has reduced the consumption of aluminium hydroxide, makes mechanical property be equivalent to Halogen silicon rubber, tear strength 20KM/N, tensile strength 5MPa;
3, the used fire retardant of silicon rubber of the present invention mainly is not halogenous aluminium hydroxide and MCA, can not give off poisonous gas during burning, can not bring pollution in the band border, belongs to the environmental protection flame retardant material;
4, the glasscloth good weatherability of Silicone Rubber Coated of the present invention is used for-70 ℃～230 ℃; Anti-ozone, oxygen, light and weathering age, the field usage weathering resistance is good, and the life-span can reach 10 years; Have higher insulating property, can bear high-voltage loaded, specific inductivity 3～3.2, voltage breakdown 20～50KV/MM; Can make the pipeline flexible connecting device is used for solving and expands with heat and contract with cold to pipeline destroyed elasticity and flexible good; Antiseptic property is good, and ageing resistance is good, can make the inside and outside anticorrosive coating of pipeline, storage tank; Silicone Rubber Coated glass fibre membrane structure material can be applicable to construction sealing materials; Can be used as fire screen uses.
Embodiment
Embodiment 1
(1) with molecular weight 600000, high-vinyl-content methyl vinyl silicone rubber 20 weight parts and the molecular weight 580000 of vinyl molar content 0.23%, low vinyl content methyl vinyl silicone rubber 30 weight parts of vinyl molar content 0.08% in two roller mills mixing 3～5 minutes, mixing evenly;
(2) adding 0.4 weight part containing hydrogen silicone oil, 4 weight part hydroxy silicon oils and 25 weight part ratio surface-area successively in the mixture of (1) is 380m
2The gas-phase silica of/g, mixing even, make rubber unvulcanizate A;
(3) with molecular weight 580000, low vinyl content methyl vinyl silicone rubber 100 weight parts of vinyl molar content 0.08% in two roller mills mixing 3～5 minutes, mixing even, add 1 weight part methyl-silicone oil, 0.8 weight part containing hydrogen silicone oil successively, mixing even;
(4) in the mixture of (3), add 55 weight part aluminium hydroxides, 5 weight part zinc borates, mixing even, to descend mixing 2～4 hours at 150～200 ℃, cooling is carried out the secondary back mixing with the sizing material after mixing, makes rubber unvulcanizate B;
(5) rubber unvulcanizate A, the B that (2) and (4) is made mixes, and adds 1 weight part vulcanizing agent 2,5-dimethyl-2, the 5-di-t-butyl hexane peroxide, 5 minutes slices of 180 ℃ of sulfurations on vulcanizing press, 200 ℃ of post cures 2 hours in baking oven again, cooling is parked and is made sulphurated siliastic C.
Embodiment 2
Step (1)～(4) are all identical with embodiment 1.
(5) rubber unvulcanizate A, the B that (2) and (4) is made mixes, add the solvent sherwood oil, mixture and solvent are after mixing at 1: 2 by weight, add 1 weight part vulcanizing agent 2,5-dimethyl-2,5-di-t-butyl hexane peroxide, be uniformly dispersed through high-speed stirring and be coated on the glasscloth, 5 minutes slices of 180 ℃ of sulfurations on vulcanizing press, 200 ℃ of post cures 2 hours in baking oven again, cooling is parked and is obtained Halogen silicon rubber glasscloth.
Embodiment 3
The even embodiment of other steps and consumption 1 is identical, and just 55 weight part aluminium hydroxides change the melamine cyanurate of 55 weight parts into, make sulphurated siliastic D through sulfuration.
Sulphurated siliastic C, D are carried out performance test (wherein flame retardant rating is tested by GB/T13488-92), and the result is as shown in table 1.
Table 1
Embodiment 4
The even embodiment of other steps and consumption 1 is identical, and just 55 weight part aluminium hydroxides change the mixture of 30 weight part aluminium hydroxides and 25 weight part melamine cyanurates into, make sulphurated siliastic E through sulfuration.
Reference examples
The even embodiment of other steps and consumption 3 is identical, and glue A and glue B do not add aluminium hydroxide and/or melamine cyanurate, but add 1 weight part tetrafluoroethylene after mixing, and make sulphurated siliastic F through sulfuration.
Sulphurated siliastic E, F are carried out performance test (wherein flame retardant rating is tested by GB/T13488-92), and the result is as shown in table 2.
Table 2
By table 2 as seen, under with the energy experiment condition, halogen-free anti-flaming silicon rubber of the present invention and the flame-proof silicon rubber that adds halogen, both mechanical properties are suitable.
Claims (8)
1. a halogen-free anti-flaming silicon rubber is formed by the composition and the vulcanizing agent sulfuration that with methyl vinyl silicone rubber are basic glue, and described composition forms by the two-pack rubber unvulcanizate is mixing, comprises by weight:
The A component:
High-vinyl-content methyl vinyl silicone rubber 10～30
Low vinyl content methyl vinyl silicone rubber 20～40
Containing hydrogen silicone oil 0.25～1
Hydroxy silicon oil 2～4
White carbon black 20～40;
The B component:
Low vinyl content methyl vinyl silicone rubber 90～110
Methyl-silicone oil 0.5～2
Containing hydrogen silicone oil 0.25～1
Aluminium hydroxide and/or melamine cyanurate 50～70
Zinc borate 2～5;
Wherein, the vinyl molar content of described silicone rubber with high content of vinyl group is 0.2～0.5%, and the vinyl molar content of described low vinyl content silicon rubber is 0.03～0.1%.
2. the preparation method at the described halogen-free anti-flaming silicon rubber of claim 1 comprises the steps:
(1) high-vinyl-content methyl vinyl silicone rubber and low vinyl content methyl vinyl silicone rubber is mixing evenly;
(2) in the mixture of (1), add containing hydrogen silicone oil, hydroxy silicon oil and white carbon black, mixing, make rubber unvulcanizate A;
(3) the low vinyl content methyl vinyl silicone rubber is mixing evenly, add methyl-silicone oil, containing hydrogen silicone oil, mixing even;
(4) in the mixture of (3), add 40～80 weight part aluminium hydroxides and/or melamine cyanurate, zinc borate, mixing, make rubber unvulcanizate B;
(5) rubber unvulcanizate A, the B that (2) and (4) is made mixes, and makes finished product through sulfuration process.
3. the preparation method of halogen-free anti-flaming silicon rubber according to claim 2 is characterized in that: mixing in the described step (4), be included in 150～200 ℃ mixing 2～4 hours down, cooling is carried out the secondary back mixing with the sizing material after mixing, makes rubber unvulcanizate B.
4. the preparation method of halogen-free anti-flaming silicon rubber according to claim 2 is characterized in that: described sulfuration process is mixture adding vulcanizing agent that will (5), makes sulphurated siliastic through sulfuration.
5. the preparation method of halogen-free anti-flaming silicon rubber according to claim 2, it is characterized in that: described sulfuration process adds solvent for the mixture with (5), mixture and solvent be by weight 1: 1.5～2.5 mix after, add vulcanizing agent, being uniformly dispersed through high-speed stirring is coated on the cloth cover, makes sulphurated siliastic based on cloth cover through sulfuration.
6. the preparation method of halogen-free anti-flaming silicon rubber according to claim 5, it is characterized in that: described solvent is sherwood oil or gasoline.
7. the purposes at the described halogen-free anti-flaming silicon rubber of claim 1 is used to prepare silicon rubber flame-retardant cloth.
8. the purposes of halogen-free anti-flaming silicon rubber according to claim 7, it is characterized in that: described cloth is glasscloth.
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| CN114539618A (en) * | 2022-02-15 | 2022-05-27 | 东莞市宏泰基阻燃材料有限公司 | Silicon rubber halogen-free flame retardant and preparation method and application thereof |
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