CN1746224A - High and low temperature-resistant rubber with high damping - Google Patents
High and low temperature-resistant rubber with high damping Download PDFInfo
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- CN1746224A CN1746224A CN 200510021768 CN200510021768A CN1746224A CN 1746224 A CN1746224 A CN 1746224A CN 200510021768 CN200510021768 CN 200510021768 CN 200510021768 A CN200510021768 A CN 200510021768A CN 1746224 A CN1746224 A CN 1746224A
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Abstract
A high and low temperature resistant damping silicon rubber consists of organic polysiloxane 55-70%, hydrophobic carbon white 25-38%, polysiloxane or silane 0-7.6%, peroxide cross-linking initiating agent 0.4-3.0% or/and ferric oxide<=4%. The chain general formula of organic polysiloxane is R1xR2ySiO(4-x-y)/2, among them x+y is positive integral of 1-3, R1 is monoacidic alkyl, R2 is monoacidic unsaturated group such as phenyl, vinyl and allyl etc., content of phenyl is 5-15mol%, content of vinyl is 0.05-0.23mol% and molecular weight of polymer is 45-60 ten thousand. The process is carried out by mediating, mixing and vulcanizing. It has better damping characteristic, less compression deformation and higher mechanical strength. It can be used for aircraft damping absorber.
Description
Technical field:
The present invention relates to a kind of high and low temperature-resistant rubber with high damping, particularly, the present invention relates to a kind of high damping hot sulfurization organosilicon rubber unvulcanizate with high energy-obsorbing and damping decrease of noise functions, this silicon rubber especially is suitable as the damping vibration attenuation material on the aerospace appts.
Background technology:
Common silicon rubber generally has good high and low temperature resistance, can adapt to the application in some particular surroundingss, as aerospace flight vehicle etc., but its vibration and noise reducing poor performance.And usually mostly be urethane or polyalkenyl resin etc. as the organic high molecular polymer of damping vibration attenuation material, though in specific temperature range, have outstanding damping vibration attenuation performance, but its significant disadvantage is that temperature resistant range is narrow, generally all significantly descend, be not suitable for use in the damping vibration attenuation material on the aerospace appts especially in its damping vibration attenuation performance below-20 ℃ or more than 60 ℃ and mechanics of machinery intensity.
In order to improve the damping vibration attenuation performance of silicon rubber, a large amount of research was arranged all both at home and abroad.For example: participate in the silicone rubber formulations system with polytetrafluorethylepowder powder by the disclosed patented invention of the special public clear 63-218762 of Japanese Patent, its damping factor tan δ is brought up between 0.115~0.2 by 0.1, but its damping capacity is still on the low side.Japanese patent laid-open 3-281663 participates in the silicone rubber formulations with sulfurized isoprene-isobutylene rubber powder or viton powder, the vibration damping silicon rubber that the temperature dependency of resonant frequency and the vibration transmissibility of improving obviously reduces, but its low temperature range only reaches-30 ℃, more the situation under the low temperature and indeterminate.Because isoprene-isobutylene rubber that it participated in, the resistance to low temperature of viton are not very good, under-50 ℃ all crystallization become fragile, hanging down under the low temperature that reaches-50 ℃ so can estimate the silicon rubber of its modification, the damping vibration attenuation performance will worsen.The Japanese Patent spy opens among the 2002-60624, methyl phenyl silicone rubber with not fatty family unsaturated group is major ingredient, be equipped with few part contains the hot-vulcanized silicone rubber composition that the polysiloxane of vinyl and other auxiliary composition such as constitution controller, reinforced filling, peroxide crosslinking initiator etc. constitute, its damping factor is greatly improved, and tan δ has brought up to more than 0.5 from common 0.15.But because the restriction of its cross-linking density, also may there be the excessive problem of compression set in its tensile strength less than 1.5MPa.Its range of application will be restricted like this, particularly is not suitable for vibroshock, anti-vibration pad that certain heavy burden is arranged.Because this class device has higher mechanical strength and compression set requirement to material.
Summary of the invention:
The purpose of this invention is to provide a kind of high and low temperature-resistant rubber with high damping, this silicon rubber has high strength, compression set little (≤20%) and high damping characteristic characteristics such as (tan δ 〉=0.2) is arranged in-50~100 ℃ of temperature ranges, can be used in the damping shock absorber of preparation based on aerospace applications.
Concrete technical scheme of the present invention is as follows:
A kind of high and low temperature-resistant rubber with high damping, it is characterized in that it be by the following weight proportion raw material through mediate, mixing after, what revulcanization made in 4 hours under 200 ℃ temperature after sulfuration 15 minutes, the demoulding earlier between 160~180 ℃ under 3~14MPa pressure,
Organopolysiloxane 55~70%
White carbon black 25~38%
The polysiloxane of hydroxyl or silane 0~7.6%
Peroxide crosslinking initiator 0.4~3.0%
And/or ferric oxide≤4%
Described organopolysiloxane is a base polymer, and its chain link general formula is by R
1 xR
2 ySiO
(4-x-y)/2Expression (x+y is 1~3 positive integer), wherein, R
1Be 1 valency alkyl such as methyl, ethyl etc., R
2Be 1 valency unsaturated group such as phenyl, vinyl, allyl group etc.In this polysiloxane phenyl content between 5~15mol%, contents of ethylene is between 0.05~0.23mol%.Polymericular weight is 45~600,000.
Described white carbon black is a reinforced filling, and its surface comprises median size 5~30nm, specific surface area 360~440m through the silazane hydrophobic treatment
2The thermal silica of/g and/or median size 5~30 μ m, specific surface area 170~220m
2The precipitated silica of/g.
The polysiloxane of described hydroxyl or silane are constitution controller, and its general formula is HO[(C
6H
5)
2SiO]
n[(CH
3)
2SiO]
mH, wherein, n is 1~20, m is 0~20, as phenylbenzene dihydroxyl silane.
Described peroxide crosslinking initiator is the general superoxide of organosilicon rubber unvulcanizate, as di-t-butyl peroxide, dicumyl peroxide, 2,5-dimethyl-2,5-di-t-butyl hexane peroxide etc.Its concrete consumption is different slightly variant because of the superoxide kind.
Described ferric oxide is a thermo-stabilizer, in order to the thermotolerance of dyeing or raising silicon rubber.
The invention has the advantages that:
The present invention is by the effective control to 1 valency alkyl in the organopolysiloxane raw material and 1 valency unsaturated group mass contg, thereby it is wide to have obtained temperature resistant range of the present invention, the silicon rubber that damping vibration attenuation performance and mechanics of machinery intensity all can not descend with the change of temperature, promptly to have an energy-obsorbing and damping decrease of noise functions strong for this silicon rubber, low compression set little (≤20%) and characteristics such as high damping characteristic (tan δ 〉=0.2), high mechanical strength are arranged in-50~100 ℃ of temperature ranges is particularly useful for preparing the damping shock absorber based on aerospace applications.
Below for the testing standard and the method for the every index of silicon rubber of the present invention institute foundation:
1, mechanical property characterizes by the test of the method for GB defined: wherein, tensile strength and elongation at break press GB/T 528-1998, tear strength and are pressed the method mensuration that GB/T 529-1991, shore a hardness press GB/T 531-1992.
2, compression set characterizes with following method test:
Be shaped to diameter phi 28mm, high h by fixing cure conditions (vulcanize earlier between 160~180 ℃ under 3~14MPa pressure behind 15 minutes, the demoulding in 200 ℃ of left and right sides revulcanization 4 hours)
OThe cylindrical print of=12.4mm is put the equilibrium between two stainless keeper plate of steels of this print then and is compressed to h
S=9.4mm places whole pressing plate 100 ℃ of baking oven heating 22 hours again, unclamps pressing plate after the taking-up, and coupons is being recovered to measure the print height h after recovering more than 2 hours under the room temperature normal pressure
L, compression set is calculated by following formula:
C%=100×(h
O-h
L)/(h
O-h
S)
Relevant damping loss factor is measured by dynamic viscoelasticity spectrum experiment D.M.A.Test specimens is the cylindrical glue sample of diameter phi 10mm, high 8mm by above-mentioned cure conditions sulfidization molding, with dynamic hot mechanical test instrument with compressive set pattern test 40Hz, compression deformation rate 0.3%, storage modulus, out-of-phase modulus and corresponding dissipation factor tan δ from-90 ℃ to 100 ℃ of temperature ranges.
Embodiment:
Embodiment 1
A kind of high and low temperature-resistant rubber with high damping, it is characterized in that it is by the following weight proportion raw material: methyl phenyl vinyl polysiloxane (wherein phenyl content 7.24%, contents of ethylene 0.19% molecular weight 480,000) 100 weight parts, white carbon black (handle by the silazane surface hydrophobicity, 40 weight parts down together), phenylbenzene dihydroxyl silane 4 weight parts evenly obtain rubber unvulcanizate through the kneader kneading.This rubber unvulcanizate of per 100 weight parts adds 2,5-dimethyl-2, and 5-di-t-butyl hexane peroxide 0.5 weight part fully mixing after evenly in the mill, makes test sample through fixedly cure conditions sulfuration mentioned above.Test its tensile strength, elongation at break, tear strength, shore a hardness, compression set, each temperature section damping loss factor tan δ etc., see Table 1.
The preparation method of described methyl phenyl vinyl polysiloxane is: in capillary bottom insert canal, temperature is taken into account with vacuum system links to each other reaction flask, and the mixed methylcyclosiloxane (Me that adding is obtained by dimethyldichlorosilane(DMCS) and the condensation of diphenyl dichlorosilane cohydrolysis and catalytic pyrolysis
2SiO)
a(Ph
2SiO)
b(a, b=1~3 a+b=4), add (the Me that presses proportional quantity again
2SiO)
4, (MeViSiO)
4And Me
3SiO (Me
2SiO)
2~5SiMe
3, make Ph in the system
2SiO chain link mole number is 7.24%, MeViSiO chain link mole number is 0.19%, add Tetramethylammonium hydroxide catalyzer at last by the quality 0.01% that always feeds intake, with system decompression, feed nitrogen in the kapillary, heating up keeps 48~50 ℃ to dewater 30 minutes down, then is warming up to about 2 hours of 100 ℃ of polymerizations.Finish to be warming up to after the reaction 170~180 ℃ and 2.66kPa and destroy catalyzer down and pull out low-boiling-point substance, obtain the methyl phenyl vinyl polysiloxane.
Embodiment 2
A kind of high and low temperature-resistant rubber with high damping, it is characterized in that it is by the following weight proportion raw material: methyl phenyl vinyl polysiloxane (wherein phenyl content 7.24%, the contents of ethylene 0.19% of pressing the described synthetic method preparation of embodiment 1, molecular weight 480,000) 100 weight parts, white carbon black 45 weight parts, phenylbenzene dihydroxyl silane 9 weight parts evenly obtain rubber unvulcanizate through the kneader kneading.This rubber unvulcanizate of per 100 weight parts adds 2,5-dimethyl-2, and 5-di-t-butyl hexane peroxide 0.5 weight part fully mixing after evenly in the mill, makes test sample through fixedly cure conditions sulfuration mentioned above.Test its tensile strength, elongation at break, tear strength, shore a hardness, compression set, each temperature section damping loss factor tan δ etc., see Table 1.
Embodiment 3
A kind of high and low temperature-resistant rubber with high damping, it is characterized in that it is by the following weight proportion raw material: methyl phenyl vinyl polysiloxane (wherein phenyl content 7.24%, the contents of ethylene 0.19% of pressing the described synthetic method preparation of embodiment 1, molecular weight 480,000) 100 weight parts, white carbon black 50 weight parts, phenylbenzene dihydroxyl silane 5 weight parts evenly obtain rubber unvulcanizate through the kneader kneading.This rubber unvulcanizate of per 100 weight parts adds 2,5-dimethyl-2, and 5-di-t-butyl hexane peroxide 0.5 weight part fully mixing after evenly in the mill, makes test sample through fixedly cure conditions sulfuration mentioned above.Test its tensile strength, elongation at break, tear strength, shore a hardness, compression set, each temperature section damping loss factor tan δ etc., see Table 1.
Embodiment 4
A kind of high and low temperature-resistant rubber with high damping, it is characterized in that it is by the following weight proportion raw material: methyl phenyl vinyl polysiloxane (wherein phenyl content 7.24%, the contents of ethylene 0.19% of pressing the described synthetic method preparation of embodiment 1, molecular weight 480,000) 100 weight parts, white carbon black 60 weight parts, phenylbenzene dihydroxyl silane 6 weight parts, ferric oxide 1.7 weight parts evenly obtain rubber unvulcanizate through the kneader kneading.This rubber unvulcanizate of per 100 weight parts adds 2,5-dimethyl-2, and 5-di-t-butyl hexane peroxide 0.5 weight part fully mixing after evenly in the mill, makes test sample through fixedly cure conditions sulfuration mentioned above.Test its tensile strength, elongation at break, tear strength, shore a hardness, compression set, each temperature section damping loss factor tan δ etc., see Table 1.
Embodiment 5
A kind of high and low temperature-resistant rubber with high damping, it is characterized in that it is by the following weight proportion raw material: methyl phenyl vinyl polysiloxane (wherein phenyl content 7.15%, the contents of ethylene 0.10% of pressing the described synthetic method preparation of embodiment 1, molecular weight 480,000) 100 weight parts, white carbon black 50 weight parts, phenylbenzene dihydroxyl silane 5 weight parts evenly obtain rubber unvulcanizate through the kneader kneading.This rubber unvulcanizate of per 100 weight parts adds 2,5-dimethyl-2, and 5-di-t-butyl hexane peroxide 0.5 weight part fully mixing after evenly in the mill, makes test sample through fixedly cure conditions sulfuration mentioned above.Test its tensile strength, elongation at break, tear strength, shore a hardness, compression set, each temperature section damping loss factor tan δ etc., see Table 1.
Embodiment 6
A kind of high and low temperature-resistant rubber with high damping, it is characterized in that it is by the following weight proportion raw material: methyl phenyl vinyl polysiloxane (wherein phenyl content 7.15%, the contents of ethylene 0.10% of pressing the described synthetic method preparation of embodiment 1, molecular weight 480,000) 100 weight parts, white carbon black 60 weight parts, phenylbenzene dihydroxyl silane 12 weight parts evenly obtain rubber unvulcanizate through the kneader kneading.This rubber unvulcanizate of per 100 weight parts adds 2,5-dimethyl-2, and 5-di-t-butyl hexane peroxide 0.5 weight part fully mixing after evenly in the mill, makes test sample through fixedly cure conditions sulfuration mentioned above.Test its tensile strength, elongation at break, tear strength, shore a hardness, compression set, each temperature section damping loss factor tan δ etc., see Table 1.
Embodiment 7
A kind of high and low temperature-resistant rubber with high damping, it is characterized in that it is by the following weight proportion raw material: methyl phenyl vinyl polysiloxane (wherein phenyl content 10.01%, the contents of ethylene 0.19% of pressing the described synthetic method preparation of embodiment 1, molecular weight 490,000) 100 weight parts, white carbon black 60 weight parts, phenylbenzene dihydroxyl silane 12 weight parts evenly obtain rubber unvulcanizate through the kneader kneading.This rubber unvulcanizate of per 100 weight parts adds 2,5-dimethyl-2, and 5-di-t-butyl hexane peroxide 0.5 weight part fully mixing after evenly in the mill, makes test sample through fixedly cure conditions sulfuration mentioned above.Test its tensile strength, elongation at break, tear strength, shore a hardness, compression set, each temperature section damping loss factor tan δ etc., see Table 1.
Embodiment 8 simultaneous tests
Comparative example 1
A kind of silicon rubber is made by the following weight proportion raw material: commercially available methyl phenyl vinyl polysiloxane (trade(brand)name 120-1 phenyl siloxane rubber, wherein phenyl content 3.09%, contents of ethylene 0.16%, molecular weight 500,000) 100 weight parts, white carbon black 60 weight parts, phenylbenzene dihydroxyl silane 12 weight parts evenly obtain rubber unvulcanizate through the kneader kneading.This rubber unvulcanizate of per 100 weight parts adds 2,5-dimethyl-2, and 5-di-t-butyl hexane peroxide 0.5 weight part fully mixing after evenly in the mill, makes test sample through fixedly cure conditions sulfuration mentioned above.Test its tensile strength, elongation at break, tear strength, shore a hardness, compression set, each temperature section damping loss factor tan δ etc., see Table 1.
Comparative example 2
A kind of silicon rubber is made by the following weight proportion raw material: commercially available methyl phenyl vinyl polysiloxane (trade(brand)name 120-2 phenyl siloxane rubber, wherein phenyl content 7.70%, contents of ethylene 0.24%, molecular weight 510,000) 100 weight parts, white carbon black 60 weight parts, phenylbenzene dihydroxyl silane 12 weight parts evenly obtain rubber unvulcanizate through the kneader kneading.This rubber unvulcanizate of per 100 weight parts adds 2,5-dimethyl-2, and 5-di-t-butyl hexane peroxide 0.5 weight part fully mixing after evenly in the mill, makes test sample through fixedly cure conditions sulfuration mentioned above.Test its tensile strength, elongation at break, tear strength, shore a hardness, compression set, each temperature section damping loss factor tan δ etc., see Table 1.
Table 1
Tensile strength MPa | Elongation % | Tear strength kN/m | Shao Er A hardness | Compression set, % | Dissipation factor tan δ (40Hz) | |||
-50℃ | 25℃ | 100℃ | ||||||
Embodiment 1 | 9.96 | 709 | 17.8 | 29 | 15.3 | 0.209 | 0.240 | 0.265 |
Embodiment 2 | 9.68 | 746 | 28.6 | 34 | 14.8 | 0.209 | 0.248 | 0.236 |
Embodiment 3 | 9.37 | 676 | 22.0 | 35 | 15.1 | 0.214 | 0.260 | 0.238 |
Embodiment 4 | 8.94 | 525 | 23.5 | 46 | 13.9 | 0.225 | 0.265 | 0.289 |
Embodiment 5 | 10.0 | 816 | 32.3 | 32 | 15.4 | 0.246 | 0.284 | 0.270 |
Embodiment 6 | 7.10 | 752 | 37 | 36 | 14.2 | 0.215 | 0.284 | 0.310 |
Embodiment 7 | 7.98 | 492 | 26.7 | 43 | 13.3 | 0.269 | 0.254 | 0.233 |
Comparative example 1 | 8.64 | 669 | 28.5 | 51 | 13.4 | 0.139 | 0.227 | 0.244 |
Comparative example 2 | 8.23 | 432 | 21.0 | 56 | 14.7 | 0.184 | 0.215 | 0.226 |
In comparative example 1, the content of phenyl is 3.09% in the methyl phenyl vinyl polysiloxane, is lower than the Schwellenwert 5% of the present invention's control, and in Comparative Examples 2, the content of vinyl is 0.24% in the methyl phenyl vinyl polysiloxane, is higher than the maximum 0.23% of the present invention's control.Can find out from table 1: though the test result of embodiment and comparative example does not have too big-difference on mechanical property, just under the situation of equity prescription, shore a hardness is slightly littler than comparative example.But on dissipation factor, difference is obvious.Comparative example 1 and 2 all less at the dissipation factor tan of cold zone δ is lower than 0.2, and is also much smaller relatively in the normal temperature district, is exactly in the high-temperature zone, also is less than normal.This result shows that silicon rubber of the present invention has better damping, vibrationproof performance, and because its compression set is smaller, is applicable to the making vibroshock.
Claims (5)
1, a kind of high and low temperature-resistant rubber with high damping, it is characterized in that it be by the following weight proportion raw material through mediate, mixing after, what revulcanization made in 4 hours under 200 ℃ temperature after sulfuration 15 minutes, the demoulding earlier between 160~180 ℃ under 3~14MPa pressure
Organopolysiloxane 55~70%
White carbon black 25~38%
The polysiloxane of hydroxyl or silane 0~7.6%
Peroxide crosslinking initiator 0.4~3.0%
And/or ferric oxide≤4%
Described organopolysiloxane is a base polymer, and its chain link general formula is by R
1 xR
2 ySiO
(4-x-y)/2Expression, wherein, x+y is 1~3 positive integer, R
1Be 1 valency alkyl such as methyl, ethyl, R
2Be 1 valency unsaturated group such as phenyl, vinyl, allyl group, in this polysiloxane phenyl content between 5~15mol%, contents of ethylene between 0.05~0.23mol%, polymericular weight is 45~600,000.
2, high and low temperature-resistant rubber with high damping as claimed in claim 1 is characterized in that described white carbon black is a reinforced filling, and its surface comprises median size 5~30nm, specific surface area 360~440m through the silazane hydrophobic treatment
2The thermal silica of/g and/or median size 5~30 μ m, specific surface area 170~220m
2The precipitated silica of/g.
3, high and low temperature-resistant rubber with high damping as claimed in claim 1 is characterized in that the polysiloxane of described hydroxyl or silane are constitution controller, and its general formula is HO[(C
6H
5)
2SiO]
n[(CH
3)
2SiO]
mH, wherein, n is 1~20, m is 0~20.
4, high and low temperature-resistant rubber with high damping as claimed in claim 1 is characterized in that described peroxide crosslinking initiator comprises di-t-butyl peroxide, dicumyl peroxide, 2,5-dimethyl-2,5-di-t-butyl hexane peroxide.
5, high and low temperature-resistant rubber with high damping as claimed in claim 1 is characterized in that described ferric oxide is the thermo-stabilizer in order to dyeing or raising silicon rubber heat-resisting.
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