CN102424725A - High-temperature resistant and erosion resistant rubber composition and preparation method thereof - Google Patents
High-temperature resistant and erosion resistant rubber composition and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-temperature resistant and erosion resistant rubber composition and a preparation method thereof. The high-temperature resistant and erosion resistant rubber composition is prepared by using the following components: 100 parts of silicon rubber, 5-30 parts of silicon dioxide, 5-50 parts of metallic oxide, 1-25 parts of nitride ceramic fibre, 0.5-20 parts of silicon carbide whisker, 20-100 parts of heat resistant packing, 0.01-0.5 parts of catalyst and 0-4 parts of cross-linking agent through double-roll milling, hot-pressing, vulcanizing and molding.
Description
Technical field
The present invention relates to a kind of high temperature resistant anti-ablation rubber combination and preparation method thereof, belong to polymer processing field.
Background technology
Zylox shows excellent properties in nature in high-low temperature resistant, weathering resistance, insulativity and physiology inertia etc.; Can be molded into the shape of various complicacies through processing means such as mold pressing and injection mouldings, have widespread use in fields such as electronics, electric, automobile, building, machinery, medical treatment.But simple Zylox does not generally have flame-retarding characteristic; Still can burn away from fire; Its anti-ablation property is also relatively poor simultaneously; Under some special applied environments; Usually can face complicated temperature condition like fields such as Special Wires and Cables, aerospace, require the material short period of time to be exposed under the excessive temperature condition such as combustion flame and still can have the certain physical mechanical property, like good snappiness, resilient seal performance and as the required mechanical strength of individual member; More extreme case then is that the requirement material can tolerate washing away in short-term of the high temperature and high speed gas-flow that live to surpass 1000 ℃ and keep the dynamic seal effect, thereby avoids electronic and electrical equipment, important structure and base material etc. to be exposed under the deleterious hot environment.Simple silastic material obviously can not satisfy this requirement, therefore must improve from matrix material molecules structure, heat stabilizing system, structure enhancing and anti-ablation scheme equal angles.
The flame-proof heat-resistant rubber composition is the polymer composite of a quasi-representative, its flame-proof heat-resistant performance mainly by the kind of the fire retardant in the system, heat conductive filler and kind and they that can in ablation process, form fine and close layer mineral filler in the Zylox matrix distribution situation and with the action mode decision of Zylox.Metal oxide filler (like the oxide compound of iron, Natural manganese dioxide, aluminium sesquioxide, zinc oxide etc.) has higher thermal conductivity; Thereby can conduct the effect that reduces system temperature that reaches to the heat that system absorbed faster; Also the someone thinks some MOX, like Natural manganese dioxide, and can be in combustion processes as free radical scavenger; Catch the radical that high temperature produces down, thereby reduce the decomposition rate of material; Mineral filler (like WHITE CARBON BLACK, ceramic fiber, carbon black, talcum powder, wollastonite etc.) itself just has excellent heat resisting; And in the incendiary process, help to form fine and close layer mineral; Starvation; Avoid silastic material by further oxygenolysis in the air thereby stop unburned matrix to be exposed to, also can play certain adiabatic effect simultaneously, thereby realize resistant to elevated temperatures purpose; And WHITE CARBON BLACK can play the effect of reinforcement, can improve the mechanical property of Zylox.
In order to improve the fire-retardant and resistance toheat of silastic material, existing more document patent report, the flame-proof silicon rubber cable of introducing like US 6239378 B1 of forming by ethenyl blocking Zylox, white carbon black, wollastonite, zeyssatite etc.; JP 317490/2002 has described thermotolerance and the reduction amount of being fuming that the platinic compound that adds the addition of ability catalysis silicon hydrogen can effectively improve material; The Sawada Japanese Patent is put down into and has been described the flame resistant cable with excellent flame retardancy in 09255125, has comprised glass powder, aluminum oxide, wollastonite and four kinds of mineral fillers of mica; US 6878410 B2 have reported with single component condensed type Zylox to be the heat insulating coat of matrix development; The trimeric cyanamide that has mainly added 8 %～20 % is as fire retardant; And contain the inorganic non-reinforced filling of 0～30 %, and coating 6mm is thick, and flame temperature is 1200 ℃; Behind the 4h, its back temperature is no more than 220 ℃.But these patents are paid close attention to the fire-retardant and flame retardant property of Zylox mostly, often seldom relate to the anti-ablation property of silastic material withstand high temperatures high velocity air, or material has certain anti-ablation ability; But can only exist with the form of coating; Be difficult to use, the more important thing is more existing schemes as individual member; Zylox forms inorganic layer than thickness portion or integral body after ablation; Though embody thermal protective performance preferably, but material has been lost elasticity and snappiness, has almost lost the function that seals especially dynamic seal.
A chance opportunity; We find through experimental study; When the compound system of some specific silicone rubber matrix and platinum class catalyzer, nitride ceramic fibre and silicon carbide whisker preparation can show some excellent properties in the high temperature ablation process; For example: the potteryization transformation can take place rapidly in this compound system material surface under high-temperature fuel gas stream environment, forms the ceramic layer as thin as a wafer that is about 0.1mm thickness, on the one hand because the mutual action of traction of potteryization primitive fiber makes that the ceramic layer as thin as a wafer that forms is fine and close, continuous and smooth; Prevent that common a large amount of crackles and cracked phenomenon from appearring in ceramic layer; On the other hand since the top layer as thin as a wafer in ceramic layer and the matrix ceramic fiber form continuous integral body, improved itself and the binding ability of matrix, firm difficult being washed away by combustion gas of surface ceramic thin layer comes off; Therefore effectively intercepted of the further ablation of high-temperature fuel gas stream to rubber matrix; The anti-ablation property of silastic material is greatly improved, and cooperates other adjuvant system, and Zylox still can effectively keep certain resilient seal performance and intensity under high temperature, ablation environment.Research shows, just demonstrates more excellent effect during these four kinds of system actings in conjunction that and if only if, and ceramic fiber just can better combine and form integral body with whisker with the surface ceramic layer.
Summary of the invention
The objective of the invention is deficiency to prior art; A kind of high temperature resistant anti-ablation rubber combination and preparation method thereof is provided; Owing to adopted the compound system that contains specific silicone rubber matrix and platinum class catalyzer, nitride ceramic fibre and silicon carbide whisker; And cooperate other adjuvant system, make its molding silicone rubber material have the anti-ablation property of remarkable improvement.
The object of the invention is realized by following technical measures.Wherein said raw material umber is parts by weight except that specified otherwise.
A kind of high temperature resistant anti-ablation rubber combination is characterized in that being made up of following components by part by weight:
100 parts in Zylox
5 ~ 30 parts of silicon-dioxide
5 ~ 50 parts of MOXs
1 ~ 25 part of nitride ceramic fibre
0.5 ~ 20 part of silicon carbide whisker
20 ~ 100 parts of heat-resistant fillers
0.01 ~ 0.5 part of catalyzer
0 ~ 4 part of linking agent
Wherein said Zylox is one or more mixed system in methyl vinyl silicone rubber, dimethyl silicone rubber, methyl phenyl vinyl silicone rubber, the trifluoropropyl siloxane; Wherein said methyl vinyl silicone rubber contents of ethylene is 0.05% ~ 2%; Molecular weight is 30 ~ 800,000; The methyl phenyl vinyl silicone rubber contents of ethylene is 0.05% ~ 2%, phenyl content 15% ~ 45%, molecular weight 40 ~ 900,000.
Wherein said silicon-dioxide is commercially available general fine silica powder, comprises but does not limit the precipitator method and vapor phase production silicon-dioxide, and preferred specific surface area is 50 ~ 500m
2The fine silica powder of/g.
Wherein said MOX is one or more in aluminum oxide, quicklime, zirconium white, cupric oxide, Natural manganese dioxide, zinc oxide, red stone, the iron protoxide.
Wherein said nitride ceramic fibre is SP 1 (BN) ceramic fiber, silicon nitride (Si
3N
4) in the ceramic fiber, SiBN ceramic fiber, SiBN (C) ceramic fiber one or more.
Wherein said silicon carbide whisker refers to the carborundum mono-crystal fiber that certain length-to-diameter ratio is arranged through synthetic preparation, comprises but is not limited to through gas-phase reaction method or the α type and the beta-type silicon carbide whisker of the preparation of solid material method.
Wherein said heat-resistant filler is one or more in wollastonite, mica, silicon nitride powder, silica powder, the zeyssatite.
Wherein said platinum compound is at least a composition of platinum black, platinum oxide, platinic hydroxide, Platinic chloride, Platinic chloride aldehyde cpd, Platinic chloride ether compound, Platinic chloride organo-siloxane complex compound.
Wherein said linking agent Di Cumyl Peroxide 99 (DCP), peroxo-two (2,4 dichloro-benzoyls), 2,5-dimethyl--2, in two (tert-butyl hydroperoxide) hexanes of 5-one or more.
A kind of method for preparing the described a kind of high temperature resistant anti-ablation rubber combination of claim 1, it is characterized in that: it may further comprise the steps:
A) in 25 ~ 60 ℃ of two roller mills, add Zylox, silicon-dioxide, catalyzer, MOX, nitride ceramic fibre, heat-resistant filler successively, open and refine to uniform mixing;
B) nature ageing 8 hours under the compound room temperature condition that obtains of step a;
C) mixture adds silicon carbide whisker, linking agent uniform mixing successively in two roller mills after the ageing, opens the refining time to be not less than 20 minutes;
D) nature ageing 24h under the compound room temperature condition of step c acquisition;
E) on 100 ~ 200 ℃ of vulcanizing presses through the hot-press vulcanization moulding, obtain high temperature resistant anti-ablation Zylox.
Present method has following obviously advantage:
1. said composition has the anti-ablation property of remarkable improvement;
2. said composition has favorable elasticity and mechanical property in the high temperature ablation process, still can effectively bring into play its sealing and dynamic seal effect within a certain period of time;
3. this material prepn and moulding process are simple, have extensive applicability.
Embodiment
Below be the present invention to be specifically described through embodiment; Be necessary to be pointed out that at this following examples can only be used for the present invention is further specified; Can not be interpreted as restriction to protection domain of the present invention; The person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above, and said umber is mass parts.
Embodiment 1: in 25 ℃ of two roller mills, add 100 parts of methyl vinyl silicone rubbers, vapor phase process SiO successively
230 parts, 0.5 part of platinum black, 10 parts of cupric oxide, 5 parts in aluminum oxide, 15 parts of boron nitride ceramics fibres, wollastonite are opened for 50 parts and are refined to uniform mixing; The ageing of room temperature nature continued mixing and adds 5 parts of α type silicon carbide whiskers, two (2,4 dichloro-benzoyls) 1.5 parts of peroxo-successively in two roller mills after 8 hours, opened refining slice after 20 minutes, in 200 ℃ of sulfuration moulding in 25 minutes down of vulcanizing press.
Embodiment 2: in 60 ℃ of two roller mills, add 50 parts of methyl vinyl silicone rubbers, 50 parts of methyl phenyl vinyl silicone rubbers, precipitator method SiO successively
220 parts, 0.8 part of Platinic chloride, 5 parts in Natural manganese dioxide, 20 parts of red stone, silicon nitride (Si
3N
4) 5 parts of ceramic fibers, mica open for 80 parts and refine to uniform mixing; The ageing of room temperature nature continued mixing and adds 15 parts of beta-type silicon carbide whiskers, 0.8 part of Di Cumyl Peroxide 99 successively in two roller mills after 8 hours, opened refining slice after 30 minutes, in 200 ℃ of sulfuration moulding in 30 minutes down of vulcanizing press.
Embodiment 3:In 25 ℃ of two roller mills, add 100 parts of dimethyl silicone rubbers, vapor phase process SiO successively
230 parts, 0.05 part in Platinic chloride organo-siloxane complex compound, 15 parts in zinc oxide, 25 parts of zirconium whites, 25 parts of SiBN ceramic fibers, 30 parts of silica powders, zeyssatite are opened for 30 parts and are refined to uniform mixing; The ageing of room temperature nature continued mixing and adds 1 part of silicon carbide whisker, 2 parts of ditert-butyl peroxides successively in two roller mills after 8 hours, opened refining slice after 30 minutes, in 180 ℃ of sulfuration moulding in 30 minutes down of vulcanizing press.
Embodiment 4:In 45 ℃ of two roller mills, add 70 parts of dimethyl silicone rubbers, 30 parts of trifluoropropyl siloxane, 0.3 part of platinum oxide, vapor phase process SiO successively
210 parts, 5 parts of iron protoxides, 20 parts in Natural manganese dioxide, 10 parts of SiBN (C) ceramic fibers, 40 parts of wollastonites, silicon nitride powder are opened for 10 parts and are refined to uniform mixing; The ageing of room temperature nature continued mixing and adds 15 parts of silicon carbide whiskers, 2 successively in two roller mills after 8 hours, 5-dimethyl--2, and 3 parts of two (tert-butyl hydroperoxide) hexanes of 5-are opened refining slice after 30 minutes, in 180 ℃ of sulfuration moulding in 25 minutes down of vulcanizing press.
Comparison example: in 25 ℃ of two roller mills, add 100 parts of methyl vinyl silicone rubbers, vapor phase process SiO successively
220 parts, open and refine to uniform mixing; The ageing of room temperature nature continued mixing and adds 1 part of Di Cumyl Peroxide 99 in two roller mills after 8 hours, opened refining slice after 20 minutes, in 170 ℃ of sulfuration moulding in 20 minutes down of vulcanizing press.
Table 1. embodiment ablation property data *
* 1000 ℃/30s of air ambient oxy-acetylene high-velocity jet flame.
Claims (9)
1. high temperature resistant anti-ablation rubber combination is characterized in that being made up of following components by part by weight:
100 parts in Zylox
5 ~ 30 parts of silicon-dioxide
5 ~ 50 parts of MOXs
1 ~ 25 part of nitride ceramic fibre
0.5 ~ 20 part of silicon carbide whisker
20 ~ 100 parts of heat-resistant fillers
0.01 ~ 0.5 part of catalyzer
0 ~ 4 part of linking agent
A kind of high temperature resistant anti-ablation rubber combination as claimed in claim 1; Wherein said Zylox is one or more mixed system in methyl vinyl silicone rubber, dimethyl silicone rubber, methyl phenyl vinyl silicone rubber, the trifluoropropyl siloxane; Wherein said methyl vinyl silicone rubber contents of ethylene is 0.05% ~ 2%, and molecular weight is 30 ~ 800,000, and the methyl phenyl vinyl silicone rubber contents of ethylene is 0.05% ~ 2%; Phenyl content 15% ~ 45%, molecular weight 40 ~ 900,000.
2. a kind of high temperature resistant anti-ablation rubber combination as claimed in claim 1, wherein said silicon-dioxide is commercially available general fine silica powder, comprises but does not limit the precipitator method and vapor phase production silicon-dioxide, preferred specific surface area is 50 ~ 500m
2The fine silica powder of/g.
3. a kind of high temperature resistant anti-ablation rubber combination as claimed in claim 1, wherein said MOX is one or more in aluminum oxide, quicklime, zirconium white, cupric oxide, Natural manganese dioxide, zinc oxide, red stone, the iron protoxide.
4. a kind of high temperature resistant anti-ablation rubber combination as claimed in claim 1, wherein said nitride ceramic fibre is SP 1 (BN) ceramic fiber, silicon nitride (Si
3N
4) in the ceramic fiber, SiBN ceramic fiber, SiBN (C) ceramic fiber one or more.
5. a kind of high temperature resistant anti-ablation rubber combination as claimed in claim 1; Wherein said silicon carbide whisker refers to the carborundum mono-crystal fiber that certain length-to-diameter ratio is arranged through synthetic preparation, comprises but is not limited to through gas-phase reaction method or the α type and the beta-type silicon carbide whisker of the preparation of solid material method.
6. a kind of high temperature resistant anti-ablation rubber combination as claimed in claim 1, wherein said heat-resistant filler is one or more in wollastonite, mica, silicon nitride powder, silica powder, the zeyssatite.
7. a kind of high temperature resistant anti-ablation rubber combination as claimed in claim 1, wherein said platinum compound is at least a composition of platinum black, platinum oxide, platinic hydroxide, Platinic chloride, Platinic chloride aldehyde cpd, Platinic chloride ether compound, Platinic chloride organo-siloxane complex compound.
8. a kind of high temperature resistant anti-ablation rubber combination as claimed in claim 1, wherein said linking agent Di Cumyl Peroxide 99 (DCP), peroxo-two (2,4 dichloro-benzoyls), 2,5-dimethyl--2, in two (tert-butyl hydroperoxide) hexanes of 5-one or more.
9. method for preparing the described a kind of high temperature resistant anti-ablation rubber combination of claim 1, it is characterized in that: it may further comprise the steps:
In 25 ~ 60 ℃ of two roller mills, add successively Zylox, silicon-dioxide, catalyzer, MOX,
Nitride ceramic fibre, heat-resistant filler are opened and are refined to uniform mixing;
B) nature ageing 8 hours under the compound room temperature condition that obtains of step a;
C) mixture adds silicon carbide whisker, linking agent uniform mixing successively in two roller mills after the ageing, opens the refining time to be not less than 20 minutes;
D) nature ageing 24h under the compound room temperature condition of step c acquisition;
E) on 100 ~ 200 ℃ of vulcanizing presses through the hot-press vulcanization moulding, obtain high temperature resistant anti-ablation Zylox.
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Application publication date: 20120425 |