CN109401331A - A kind of energy-absorbing high-temperature silicon disulfide rubber and preparation method thereof - Google Patents
A kind of energy-absorbing high-temperature silicon disulfide rubber and preparation method thereof Download PDFInfo
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 60
- 239000005060 rubber Substances 0.000 title claims abstract description 60
- KHDSWONFYIAAPE-UHFFFAOYSA-N silicon sulfide Chemical compound S=[Si]=S KHDSWONFYIAAPE-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 50
- XDVOLDOITVSJGL-UHFFFAOYSA-N 3,7-dihydroxy-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound O1B(O)OB2OB(O)OB1O2 XDVOLDOITVSJGL-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 36
- 239000004945 silicone rubber Substances 0.000 claims abstract description 29
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 27
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract description 27
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 27
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 claims abstract description 25
- -1 polysiloxane Polymers 0.000 claims abstract description 18
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 19
- 229940008099 dimethicone Drugs 0.000 claims description 18
- 229920005573 silicon-containing polymer Polymers 0.000 claims description 17
- 239000004088 foaming agent Substances 0.000 claims description 16
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 14
- 229920002545 silicone oil Polymers 0.000 claims description 14
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 12
- 238000005187 foaming Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 229920002554 vinyl polymer Polymers 0.000 claims description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000000748 compression moulding Methods 0.000 claims description 6
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 5
- DMWVYCCGCQPJEA-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane Chemical compound CC(C)(C)OOC(C)(C)CCC(C)(C)OOC(C)(C)C DMWVYCCGCQPJEA-UHFFFAOYSA-N 0.000 claims description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- OLLFKUHHDPMQFR-UHFFFAOYSA-N dihydroxy(diphenyl)silane Chemical group C=1C=CC=CC=1[Si](O)(O)C1=CC=CC=C1 OLLFKUHHDPMQFR-UHFFFAOYSA-N 0.000 claims description 4
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 239000004408 titanium dioxide Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 2
- 239000005977 Ethylene Substances 0.000 claims 3
- 239000005995 Aluminium silicate Substances 0.000 claims 2
- 235000012211 aluminium silicate Nutrition 0.000 claims 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 229910000062 azane Inorganic materials 0.000 claims 1
- 239000006229 carbon black Substances 0.000 claims 1
- 239000003610 charcoal Substances 0.000 claims 1
- 239000012071 phase Substances 0.000 claims 1
- 238000007670 refining Methods 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 239000012808 vapor phase Substances 0.000 claims 1
- 230000035939 shock Effects 0.000 abstract description 14
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 229920001296 polysiloxane Polymers 0.000 abstract description 5
- 239000002131 composite material Substances 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 16
- 230000001133 acceleration Effects 0.000 description 8
- 229910021485 fumed silica Inorganic materials 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 229910003978 SiClx Inorganic materials 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 239000005864 Sulphur Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000006260 foam Substances 0.000 description 3
- 229920000260 silastic Polymers 0.000 description 3
- PFJFNQUFMTYCHB-UHFFFAOYSA-N C[SiH2]N[SiH3] Chemical compound C[SiH2]N[SiH3] PFJFNQUFMTYCHB-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000003139 buffering effect Effects 0.000 description 2
- 239000008119 colloidal silica Substances 0.000 description 2
- 239000003517 fume Substances 0.000 description 2
- 229910052622 kaolinite Inorganic materials 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- OGPNXGJLKXGASM-UHFFFAOYSA-N [Si].CC=C Chemical compound [Si].CC=C OGPNXGJLKXGASM-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000001451 organic peroxides Chemical class 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/32—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof from compositions containing microballoons, e.g. syntactic foams
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/22—Expandable microspheres, e.g. Expancel®
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use 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; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use 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; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use 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; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
The invention discloses a kind of energy-absorbing high-temperature silicon disulfide rubbers, it is characterized in that its component and weight ratio are as follows: 80-120 parts of methyl vinyl silicone rubber, 0-110 parts of reinforced filling, 0.1-3 parts of vulcanizing agent, 0.5-15 parts of constitution controller, 0.1-10 parts of tear-proof agent, 2-50 parts of pyroboric acid modified dimethyl polysiloxane.The invention also discloses specific preparation methods.The modified hydroxy-terminated polysiloxane of pyroboric acid and high-temperature silicon disulfide rubber progress is compound, the two has good compatibility, both neat strong point can be collected, the weakness of the two is made up, the energy-absorbing composite material with shock resistance of initial configuration can be restored to after being impacted.
Description
Technical field
The invention belongs to technical field of polymer composite materials, and it is compound to be related to modified polyorganosiloxane/high-temperature silicon disulfide rubber
The preparation method of material
Background technique
Pyroboric acid modified polyorganosiloxane is a kind of gel-like material with shear hardening effect.Under low rate effect,
Material shows the property of rheid, it is easy to deform, or even the same slow flowing of fluid can occur；But it is acted in high-speed
Under, material shows high intensity at once, maintains original shape and stands up to the impact of external force, plays buffering and energy-absorbing
Effect.Its physics, chemical property are stablized, and shock resistance is excellent.But deformation occurs when being impacted due to it to restore, institute
Not use directly generally, need to be used in combination with other substrates.
High-temperature silicon disulfide rubber is the polysiloxane (i.e. raw rubber) of high molecular weight (molecular weight is generally 40~800,000)
Reinforced filling and various other additives is added, uses organic peroxide for vulcanizing agent, (molding squeezes, pressure for pressurized molding
Prolong) or injection moulding, and it is cross-linked into rubber at high temperature.High-temperature silicon disulfide rubber have good resistant of high or low temperature, weatherability,
The excellent properties such as ozone resistance and elasticity, but the performance of its shock resistance is general, need to be improved.
Summary of the invention
The purpose of the present invention is to solve prior art problems, and provide a kind of with the high temperature vulcanized of shock resistance
Silicon rubber, the present invention also provides preparation methods.
The technical solution of the present invention is as follows:
A kind of energy-absorbing high-temperature silicon disulfide rubber (non-foamed), component and weight ratio are as follows: methyl vinyl silicone rubber 80-
120 parts, 0-110 parts of reinforced filling, 0.1-3 parts of vulcanizing agent, 0.5-15 parts of constitution controller, 0.1-10 parts of tear-proof agent, burnt boron
Sour modified dimethyl polysiloxane 2-50 parts.
Further, the energy-absorbing high-temperature silicon disulfide rubber, component and weight ratio are as follows: methyl vinyl silicone rubber 100
Part, 0-100 parts of reinforced filling, 0.5-1 parts of vulcanizing agent, 1-10 parts of constitution controller, 0.2-5 parts of tear-proof agent, pyroboric acid is modified
5-45 parts of dimethyl silicone polymer.
Preferably, the energy-absorbing high-temperature silicon disulfide rubber, component and weight ratio are as follows: methyl vinyl silicone rubber 100
Part, 2 parts of reinforced filling, 0.5 part of vulcanizing agent, 1 part of constitution controller, 1 part of tear-proof agent, pyroboric acid modified dimethyl polysiloxane
18.4 parts.100 parts of methyl vinyl silicone rubber, 10 parts of reinforced filling, 0.5 part of vulcanizing agent, 1 part of constitution controller, tear-proof agent
0.5 part, 12.4 parts of pyroboric acid modified dimethyl polysiloxane.
Preferably, reinforced filling includes fume colloidal silica, precipitated silica, organo montmorillonite, titanium dioxide, kaolinite
At least one of soil, calcium carbonate；Vulcanizing agent includes di-t-butyl peroxide (DTBP), cumyl peroxide (DCP), 2,5-
At least one of dimethyl -2,5- bis- (t-butylperoxy) hexane (DBPMH)；Constitution controller is diphenyl silanediol, six
At least one of methyl disilazane, the hydroxyl-terminated injecting two methyl siloxane of small-molecular-weight, cyclosilazane；Tear-proof agent is more
Vinyl silicone oil；The molecular weight of dimethicone is 20,000-10 ten thousand；The mass ratio 0.1%-10% of pyroboric acid and dimethicone；
The modified dimethyl silicone polymer of pyroboric acid is that dimethicone and pyroboric acid are reacted 3- in 120-160 DEG C of vacuum kneader
6 hours and be made.
The preparation method of the energy-absorbing high-temperature silicon disulfide rubber, steps are as follows:
(1) methyl vinyl silicone rubber, reinforced filling, vulcanizing agent, constitution controller, tear-proof agent are separately added into mixing
Room temperature mixing 10 minutes in machine, add the modified dimethyl silicone polymer of pyroboric acid, and room temperature mixing 20-30 minutes；
(2) step (1) resulting mixture is taken, is put into mold, in pressure 10MPa, 155 DEG C -170 DEG C of temperature of plate
Vulcanize 15min-20min on vulcanizer；
(3) high-temperature silicon disulfide rubber overvulcanization 1-4h in 200 DEG C of baking ovens obtained by step (2) is taken, energy-absorbing high temperature is obtained
Sulphurated siliastic.
A kind of energy-absorbing high-temperature silicon disulfide rubber (foaming), component and weight ratio are as follows: 100 parts of methyl vinyl silicone rubber,
0-100 parts of reinforced filling, 0.5-1 parts of vulcanizing agent, 1-10 parts of constitution controller, 0.2-5 parts of tear-proof agent, pyroboric acid modified poly- two
5-45 parts of methylsiloxane, 1-4 parts of foaming agent.
Preferably, the energy high-temperature silicon disulfide rubber, it is characterised in that its component and weight ratio are as follows: methyl ethylene silicon
100 parts of rubber, 2 parts of reinforced filling, 0.5 part of vulcanizing agent, 1 part of constitution controller, 1 part of tear-proof agent, the modified poly- diformazan of pyroboric acid
18.4 parts of radical siloxane, 4 parts of foaming agent；
It can also be 100 parts of methyl vinyl silicone rubber, 10 parts of reinforced filling, 0.5 part of vulcanizing agent, constitution controller 1
Part, 0.5 part of tear-proof agent, 12.8 parts of pyroboric acid modified dimethyl polysiloxane, 4 parts of foaming agent.
Preferably, reinforced filling includes fume colloidal silica, precipitated silica, organo montmorillonite, titanium dioxide, kaolinite
At least one of soil, calcium carbonate；Vulcanizing agent includes di-t-butyl peroxide (DTBP), cumyl peroxide (DCP), 2,5-
At least one of dimethyl -2,5- bis- (t-butylperoxy) hexane (DBPMH)；Constitution controller is diphenyl silanediol, six
At least one of methyl disilazane, the hydroxyl-terminated injecting two methyl siloxane of small-molecular-weight, cyclosilazane；Tear-proof agent is more second
Alkenyl silicone oil；The molecular weight of dimethicone is 20,000-10 ten thousand；The mass ratio 0.1%-10% of pyroboric acid and dimethicone；It will
Dimethicone and pyroboric acid react 3-6 hours in 120-160 DEG C of vacuum kneader, obtain the modified poly dimethyl of pyroboric acid
Siloxanes；Foaming agent is microballoon foaming agent, blowing temperature≤vulcanizing agent curing temperature.
The preparation method of the energy-absorbing high-temperature silicon disulfide rubber, steps are as follows:
(1) methyl vinyl silicone rubber, reinforced filling, vulcanizing agent, constitution controller, tear-proof agent are separately added into mixing
Room temperature mixing 10 minutes in machine add foaming agent mixing 10min, add the modified dimethyl silicone polymer of pyroboric acid, often
Warm mixing 20-30 minutes；
(2) step (1) resulting mixture is taken, is put into mold, in pressure 10MPa, 155 DEG C -170 DEG C of temperature of plate
Vulcanize 15min-20min on vulcanizer；
(3) high-temperature silicon disulfide rubber overvulcanization 1-4h in 200 DEG C of baking ovens obtained by step (2) is taken, foaming energy-absorbing is obtained
High-temperature silicon disulfide rubber.
Preferably, the methyl vinyl silicone rubber molecular weight 400,000-80 ten thousand, vinyl chain link molar fraction
0.03%-0.24%.
The utility model has the advantages that
The modified hydroxy-terminated polysiloxane of pyroboric acid and high-temperature silicon disulfide rubber progress is compound, and the two has good compatible
Property, both neat strong point can be collected, make up the weakness of the two, initial configuration can be restored to after being impacted has shock resistance
The energy-absorbing composite material of performance.
Advantages of the present invention, the modified polysiloxanes of pyroboric acid is compound with high-temperature silicon disulfide rubber, the modification prepared
Polysiloxanes/high-temperature silicon disulfide rubber composite material is in the pyroboric acid of dispersed phase distribution when being sheared or being impacted, in material
Modified polyorganosiloxane is absorbed by shear hardening effect and dissipative part energy, to realize to high-temperature silicon disulfide rubber impact
The enhancing of energy；After impact, nondestructive deformation can restore.The preparation process is easy to operate, is suitble to industrialized production, this is compound
The alternative traditional silastic product of material, for sealing, the environment such as vibration damping, buffering.
Present invention comprises the foaming of energy-absorbing high-temperature silicon disulfide rubber and two kinds of non-foamed, and foaming can be improved with non-foamed
The shock resistance of high-temperature silicon disulfide rubber, but the application range of the two is different, non-foamed energy-absorbing high-temperature silicon disulfide rubber phase
To harder, it is mainly used for the biggish field of impact energy；And the energy-absorbing high-temperature silicon disulfide rubber that foams is due to containing foaming body, resiliency
Can be more preferable, it is smaller and need the field of higher energy absorptivity to be mainly used in impact energy.
Specific embodiment:
Following embodiment and experimental example are not intended to limit the scope of the invention for illustrating the present invention.Below with reference to tool
The invention will be further described for body embodiment and experimental example
Embodiment 1
Step 1: claiming viscosity 50000mPas dimethicone 50g, 1g pyroboric acid is added in 130 DEG C of vacuum kneaders
Reaction 3 hours obtains the modified dimethyl silicone polymer of pyroboric acid；
Step 2: claiming 50g methyl vinyl silicone rubber to be put into mixer, sequentially add fumed silica 1g, hexamethyl
Disilazane 0.5g, multi-vinyl silicone oil 0.5g, cumyl peroxide 0.25g are refined 10 minutes, add burnt boron in step 1
The dimethyl silicone polymer 9.2g that acid is modified, mixing 30 minutes；
Step 3: taking the resulting mixture of step 2, be put into mold, vulcanize at pressure 10MPa, 170 DEG C of temperature
15min；
Step 4: taking step 3 gained high-temperature silicon disulfide rubber overvulcanization 4h in 200 DEG C of baking ovens, obtain energy-absorbing high temperature sulphur
SiClx rubber.
Comparative example 1
Step 1: claiming 50g methyl vinyl silicone rubber to be put into mixer, sequentially add fumed silica 1g, hexamethyl
Disilazane 0.5g, multi-vinyl silicone oil 0.5g, cumyl peroxide 0.25g, dimethicone 9.2g are refined 30 minutes；
Step 2: taking the resulting mixture of step 1, be put into mold, in pressure 10MPa, 170 DEG C of temperature of compression molding
Vulcanize 15min on machine；
Step 3: taking step 2 gained high-temperature silicon disulfide rubber overvulcanization 4h in 200 DEG C of baking ovens, obtain high-temperature vulcanized silicon
Rubber.
Comparing embodiment 1 and comparative example 1:
The shock resistance of test sample is tested using drop impact, test condition: 10 joules of impact energy, speed
3.162m/s, the hardness of test sample, density, impact acceleration, S. E. A., the test result of embodiment 1 and comparative example 1
It is as follows:
| Sample | Comparative example 1 | Embodiment 1 |
| Hardness (Shao A) | 33.5 | 26.6 |
| Density (g/cm3) | 1.132 | 1.056 |
| Maximum impact acceleration (g) | 406 | 280 |
| S. E. A. | 15.1% | 41.5% |
By data in table as it can be seen that energy-absorbing high-temperature silicon disulfide rubber is compared with usual silicone rubber, S. E. A. is improved
174%, show that the shock resistance of energy-absorbing high-temperature silicon disulfide rubber significantly improves.
Embodiment 2
Step 1: claiming viscosity 50000mPas dimethicone 50g, 2g pyroboric acid is added in 130 DEG C of vacuum kneaders
Reaction 3 hours obtains the modified dimethyl silicone polymer of pyroboric acid；
Step 2: claiming 50g methyl vinyl silicone rubber to be put into mixer, sequentially add fumed silica 5g, hexamethyl
Disilazane 0.5g, multi-vinyl silicone oil 0.25g, cumyl peroxide 0.25g are refined 10 minutes, add burnt boron in step 1
The dimethyl silicone polymer 6.4g that acid is modified, mixing 30 minutes；
Step 3: taking the resulting mixture of step 2, be put into mold, vulcanize at pressure 10MPa, 170 DEG C of temperature
15min；
Step 4: taking step 3 gained high-temperature silicon disulfide rubber overvulcanization 1h in 200 DEG C of baking ovens, obtain energy-absorbing high temperature sulphur
SiClx rubber.
Comparative example 2
Step 1: claiming 50g methyl vinyl silicone rubber to be put into mixer, sequentially add fumed silica 5g, hexamethyl
Disilazane 0.5g, multi-vinyl silicone oil 0.25g, cumyl peroxide 0.25g, dimethicone 6.4g are refined 30 minutes；
Step 2: taking the resulting mixture of step 1, be put into mold, in pressure 10MPa, 170 DEG C of temperature of compression molding
Vulcanize 15min on machine；
Step 3: taking step 2 gained high-temperature silicon disulfide rubber overvulcanization 1h in 200 DEG C of baking ovens, obtain high-temperature vulcanized silicon
Rubber.
Comparing embodiment 2 and comparative example 2
The shock resistance of test sample is tested using drop impact, test condition: 10 joules of impact energy, speed
3.162m/s, the hardness of test sample, density, impact acceleration, S. E. A., the test result of embodiment 2 and comparative example 2
It is as follows:
| Sample | Comparative example 2 | Embodiment 2 |
| Hardness (Shao A) | 35.5 | 28 |
| Density (g/cm3) | 1.145 | 1.086 |
| Maximum impact acceleration (g) | 430 | 289 |
| S. E. A. | 17.1% | 38.5% |
By data in table as it can be seen that energy-absorbing high-temperature silicon disulfide rubber is compared with usual silicone rubber, S. E. A. is improved
125%, show that the shock resistance of energy-absorbing high-temperature silicon disulfide rubber significantly improves.
Embodiment 3
Step 1: claiming viscosity 50000mPas silicone oil 50g, it is small that addition 1g pyroboric acid reacts 3 in 130 DEG C of vacuum kneaders
When, obtain the modified dimethyl silicone polymer of pyroboric acid；
Step 2: claiming 50g methyl vinyl silicone rubber to be put into mixer, sequentially add fumed silica 1g, hexamethyl
Mixing 10 minutes, microballoon foaming agent was added in disilazane 0.5g, multi-vinyl silicone oil 0.5g, cumyl peroxide 0.25g
2g mixing 10 minutes, adds the modified dimethyl silicone polymer 9.5g of pyroboric acid in step 1, and mixing 30 minutes；
Step 3: taking the resulting mixture of step 2, be put into mold, vulcanize at pressure 10MPa, 170 DEG C of temperature
15min；
Step 4: taking step 3 gained high-temperature silicon disulfide rubber overvulcanization 4h in 200 DEG C of baking ovens, it is high to obtain energy-absorbing foaming
Temperature vulcanizable silicone rubber.
Comparative example 3
Step 1: claiming 50g methyl vinyl silicone rubber to be put into mixer, sequentially add fumed silica 1g, hexamethyl
Disilazane 0.5g, multi-vinyl silicone oil 0.5g, cumyl peroxide 0.25g, dimethicone 9.5g, mixing 10 minutes,
Add microballoon foaming agent 2g, mixing 20 minutes；
Step 2: taking the resulting mixture of step 1, be put into mold, in pressure 10MPa, 170 DEG C of temperature of compression molding
Vulcanize 15min on machine；
Step 3: taking step 2 gained high-temperature silicon disulfide rubber overvulcanization 4h in 200 DEG C of baking ovens, obtain foaming high temperature sulphur
SiClx rubber.
Comparing embodiment 3 and comparative example 3
The shock resistance of test sample is tested using drop impact, test condition: 10 joules of impact energy, speed
2.449m/s, the hardness of test sample, density, impact acceleration, S. E. A., the test result of embodiment 3 and comparative example 3
It is as follows:
| Sample | Comparative example 3 | Embodiment 3 |
| Hardness (Shao A) | 30 | 23.5 |
| Density (g/cm3) | 0.702 | 0.623 |
| Maximum impact acceleration (g) | 370 | 252 |
| S. E. A. | 16.3% | 50.2% |
By data in table, as it can be seen that energy-absorbing foams, high-temperature silicon disulfide rubber is compared with common foamed silastic, S. E. A.
207% is improved, shows that the shock resistance of energy-absorbing foaming high-temperature silicon disulfide rubber significantly improves.
Embodiment 4
Step 1: claiming viscosity 50000mPas silicone oil 50g, it is small that addition 2g pyroboric acid reacts 3 in 130 DEG C of vacuum kneaders
When, obtain the modified dimethyl silicone polymer of pyroboric acid；
Step 2: claiming 50g methyl vinyl silicone rubber to be put into mixer, sequentially add fumed silica 5g, hexamethyl
Mixing 10 minutes, microballoon foaming agent was added in disilazane 0.5g, multi-vinyl silicone oil 0.25g, cumyl peroxide 0.25g
2g mixing 10 minutes, adds the modified dimethyl silicone polymer 6.4g of pyroboric acid in step 1, and mixing 30 minutes；
Step 3: taking the resulting mixture of step 2, be put into mold, vulcanize at pressure 10MPa, 170 DEG C of temperature
15min；
Step 4: taking step 3 gained high-temperature silicon disulfide rubber overvulcanization 1h in 200 DEG C of baking ovens, it is high to obtain energy-absorbing foaming
Temperature vulcanizable silicone rubber.
Comparative example 4
Step 1: claiming 50g methyl vinyl silicone rubber to be put into mixer, sequentially add fumed silica 5g, hexamethyl
The close 0.25g of disilazane 0.5g, multi-vinyl silicone oil, cumyl peroxide 0.25g, dimethicone 6.4g, mixing 10 divide
Clock, adds microballoon foaming agent 2g, and mixing 20 minutes；
Step 2: taking the resulting mixture of step 1, be put into mold, in pressure 10MPa, 170 DEG C of temperature of compression molding
Vulcanize 15min on machine；
Step 3: taking step 1 gained high-temperature silicon disulfide rubber overvulcanization 1h in 200 DEG C of baking ovens, obtain foaming high temperature sulphur
SiClx rubber.
Comparing embodiment 4 and comparative example 4
The shock resistance of test sample is tested using drop impact, test condition: 10 joules of impact energy, speed
2.449m/s, the hardness of test sample, density, impact acceleration, S. E. A., the test result of embodiment 4 and comparative example 4
It is as follows:
| Sample | Comparative example 4 | Embodiment 4 |
| Hardness (Shao A) | 31 | 25 |
| Density (g/cm3) | 0.772 | 0.683 |
| Maximum impact acceleration (g) | 390 | 276 |
| S. E. A. | 20.3% | 46.5% |
By data in table, as it can be seen that energy-absorbing foams, high-temperature silicon disulfide rubber is compared with common foamed silastic, S. E. A.
129% is improved, shows that the shock resistance of energy-absorbing foaming high-temperature silicon disulfide rubber significantly improves.
Claims (10)
1. a kind of energy-absorbing high-temperature silicon disulfide rubber, it is characterised in that its component and weight ratio are as follows: methyl vinyl silicone rubber 80-
120 parts, 0-110 parts of reinforced filling, 0.1-3 parts of vulcanizing agent, 0.5-15 parts of constitution controller, 0.1-10 parts of tear-proof agent, burnt boron
Sour modified dimethyl polysiloxane 2-50 parts.
2. energy-absorbing high-temperature silicon disulfide rubber as described in claim 1, it is characterised in that its component and weight ratio are as follows: ethylene methacrylic
100 parts of base silicon rubber, 0-100 parts of reinforced filling, 0.5-1 parts of vulcanizing agent, 1-10 parts of constitution controller, 0.2-5 parts of tear-proof agent,
5-45 parts of pyroboric acid modified dimethyl polysiloxane.
3. energy-absorbing high-temperature silicon disulfide rubber as described in claim 1, it is characterised in that its component and weight ratio are as follows: ethylene methacrylic
100 parts of base silicon rubber, 2 parts of reinforced filling, 0.5 part of vulcanizing agent, 1 part of constitution controller, 1 part of tear-proof agent, pyroboric acid is modified poly-
18.4 parts of dimethyl siloxane.100 parts of methyl vinyl silicone rubber, 10 parts of reinforced filling, 0.5 part of vulcanizing agent, constitution controller 1
Part, 0.5 part of tear-proof agent, 12.4 parts of pyroboric acid modified dimethyl polysiloxane.
4. the energy-absorbing high-temperature silicon disulfide rubber as described in claims 1 to 3 is any, it is characterised in that: reinforced filling includes gas phase
At least one of method white carbon black, precipitated silica, organo montmorillonite, titanium dioxide, kaolin, calcium carbonate；Vulcanizing agent includes
Di-t-butyl peroxide, cumyl peroxide, at least one in 2,5- dimethyl -2,5- bis- (t-butylperoxy) hexane
Kind；Constitution controller is diphenyl silanediol, hexamethyldisilazane, the hydroxyl-terminated injecting two methyl siloxane of small-molecular-weight, ring silicon
At least one of azane；Tear-proof agent is multi-vinyl silicone oil；The molecular weight of dimethicone is 20,000-10 ten thousand；Pyroboric acid with
The mass ratio 0.1%-10% of dimethicone；The modified dimethyl silicone polymer of pyroboric acid is by dimethicone and pyroboric acid
It reacts 3-6 hours and is made in 120-160 DEG C of vacuum kneader.
5. the preparation method of energy-absorbing high-temperature silicon disulfide rubber as claimed in claim 4, it is characterised in that steps are as follows:
(1) methyl vinyl silicone rubber, reinforced filling, vulcanizing agent, constitution controller, tear-proof agent are separately added into mixer
Room temperature mixing 10 minutes, add the modified dimethyl silicone polymer of pyroboric acid, room temperature mixing 20-30 minutes；
(2) step (1) resulting mixture is taken, is put into mold, in pressure 10MPa, 155 DEG C -170 DEG C of temperature of compression molding
Vulcanize 15min-20min on machine；
(3) high-temperature silicon disulfide rubber overvulcanization 1-4h in 200 DEG C of baking ovens obtained by step (2) is taken, it is high temperature vulcanized to obtain energy-absorbing
Silicon rubber.
6. a kind of energy-absorbing high-temperature silicon disulfide rubber, it is characterised in that its component and weight ratio are as follows: methyl vinyl silicone rubber 100
Part, 0-100 parts of reinforced filling, 0.5-1 parts of vulcanizing agent, 1-10 parts of constitution controller, 0.2-5 parts of tear-proof agent, pyroboric acid is modified
5-45 parts of dimethyl silicone polymer, 1-4 parts of foaming agent.
7. energy-absorbing high-temperature silicon disulfide rubber as claimed in claim 6, it is characterised in that its component and weight ratio are as follows: ethylene methacrylic
100 parts of base silicon rubber, 2 parts of reinforced filling, 0.5 part of vulcanizing agent, 1 part of constitution controller, 1 part of tear-proof agent, pyroboric acid is modified poly-
18.4 parts of dimethyl siloxane, 4 parts of foaming agent；It can also be 100 parts of methyl vinyl silicone rubber, 10 parts of reinforced filling, vulcanize
0.5 part of agent, 1 part of constitution controller, 0.5 part of tear-proof agent, 12.8 parts of pyroboric acid modified dimethyl polysiloxane, 4 parts of foaming agent.
8. energy-absorbing high-temperature silicon disulfide rubber as claimed in claim 6, it is characterised in that: reinforced filling includes vapor phase method hard charcoal
At least one of black, precipitated silica, organo montmorillonite, titanium dioxide, kaolin, calcium carbonate；Vulcanizing agent includes peroxidating
At least one of di-t-butyl, cumyl peroxide, 2,5- dimethyl -2,5- bis- (t-butylperoxy) hexane；Structure
Controlling agent be diphenyl silanediol, hexamethyldisilazane, the hydroxyl-terminated injecting two methyl siloxane of small-molecular-weight, in cyclosilazane extremely
Few one kind；Tear-proof agent is multi-vinyl silicone oil；The molecular weight of dimethicone is 20,000-10 ten thousand；Pyroboric acid and dimethicone
Mass ratio 0.1%-10%；Dimethicone and pyroboric acid are reacted 3-6 hours in 120-160 DEG C of vacuum kneader, obtained
The dimethyl silicone polymer modified to pyroboric acid；Foaming agent is microballoon foaming agent, blowing temperature≤vulcanizing agent curing temperature.
9. the preparation method of energy-absorbing high-temperature silicon disulfide rubber as claimed in claim 6, it is characterised in that steps are as follows:
(1) methyl vinyl silicone rubber, reinforced filling, vulcanizing agent, constitution controller, tear-proof agent are separately added into mixer
Room temperature mixing 10 minutes, foaming agent mixing 10min is added, adds the modified dimethyl silicone polymer of pyroboric acid, room temperature is close
Refining 20-30 minutes；
(2) step (1) resulting mixture is taken, is put into mold, in pressure 10MPa, 155 DEG C -170 DEG C of temperature of compression molding
Vulcanize 15min-20min on machine；
(3) high-temperature silicon disulfide rubber overvulcanization 1-4h in 200 DEG C of baking ovens obtained by step (2) is taken, foaming energy-absorbing high temperature is obtained
Sulphurated siliastic.
10. the energy-absorbing high-temperature silicon disulfide rubber as described in claim 1,2,3,6,7: the methyl vinyl silicone rubber molecule
400,000-80 ten thousand are measured, vinyl chain link molar fraction 0.03%-0.24%.
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| CN110564164A (en) * | 2019-09-27 | 2019-12-13 | 中国科学院长春应用化学研究所 | Waterproof polyborosiloxane shock-resistant damping material and preparation method thereof |
| CN110951395A (en) * | 2019-11-13 | 2020-04-03 | 广东东方一哥新材料股份有限公司 | Water-based UV irradiation treating agent and preparation method thereof |
| CN111154160A (en) * | 2020-01-16 | 2020-05-15 | 郑蕊 | Foamed silica gel material for bra and preparation method thereof |
| CN113025050A (en) * | 2021-04-02 | 2021-06-25 | 中国科学技术大学 | Composite material with shear hardening and flame retardant properties and preparation method thereof |
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