CN106750687B - Polysiloxanes microballoon damps chlorinated scoline composite material and preparation method - Google Patents
Polysiloxanes microballoon damps chlorinated scoline composite material and preparation method Download PDFInfo
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- CN106750687B CN106750687B CN201710102663.8A CN201710102663A CN106750687B CN 106750687 B CN106750687 B CN 106750687B CN 201710102663 A CN201710102663 A CN 201710102663A CN 106750687 B CN106750687 B CN 106750687B
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- chlorinated scoline
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- -1 Polysiloxanes Polymers 0.000 title claims abstract description 88
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 86
- YOEWQQVKRJEPAE-UHFFFAOYSA-L succinylcholine chloride (anhydrous) Chemical class [Cl-].[Cl-].C[N+](C)(C)CCOC(=O)CCC(=O)OCC[N+](C)(C)C YOEWQQVKRJEPAE-UHFFFAOYSA-L 0.000 title claims abstract description 66
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000013016 damping Methods 0.000 claims abstract description 55
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 35
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 18
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 18
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008117 stearic acid Substances 0.000 claims abstract description 18
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 230000003712 anti-aging effect Effects 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims description 29
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 17
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 13
- PRXRUNOAOLTIEF-ADSICKODSA-N Sorbitan trioleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCC\C=C/CCCCCCCC)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCC\C=C/CCCCCCCC PRXRUNOAOLTIEF-ADSICKODSA-N 0.000 claims description 13
- 239000000908 ammonium hydroxide Substances 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 11
- 239000005864 Sulphur Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- IOJUPLGTWVMSFF-UHFFFAOYSA-N benzothiazole Chemical compound C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- 238000000643 oven drying Methods 0.000 claims description 8
- 239000000945 filler Substances 0.000 claims description 7
- XQVWYOYUZDUNRW-UHFFFAOYSA-N N-Phenyl-1-naphthylamine Chemical group C=1C=CC2=CC=CC=C2C=1NC1=CC=CC=C1 XQVWYOYUZDUNRW-UHFFFAOYSA-N 0.000 claims description 5
- 239000004005 microsphere Substances 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 229920001971 elastomer Polymers 0.000 description 23
- 230000008859 change Effects 0.000 description 10
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 9
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 9
- 239000011777 magnesium Substances 0.000 description 9
- 229910052749 magnesium Inorganic materials 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 description 6
- 239000003963 antioxidant agent Substances 0.000 description 6
- 230000003078 antioxidant effect Effects 0.000 description 6
- 238000004566 IR spectroscopy Methods 0.000 description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 4
- 229910052801 chlorine Inorganic materials 0.000 description 4
- 229920005556 chlorobutyl Polymers 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 229920005549 butyl rubber Polymers 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000806 elastomer Substances 0.000 description 3
- 230000012010 growth Effects 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- JGUMTYWKIBJSTN-UHFFFAOYSA-N 2-ethylhexyl 4-[[4,6-bis[4-(2-ethylhexoxycarbonyl)anilino]-1,3,5-triazin-2-yl]amino]benzoate Chemical compound C1=CC(C(=O)OCC(CC)CCCC)=CC=C1NC1=NC(NC=2C=CC(=CC=2)C(=O)OCC(CC)CCCC)=NC(NC=2C=CC(=CC=2)C(=O)OCC(CC)CCCC)=N1 JGUMTYWKIBJSTN-UHFFFAOYSA-N 0.000 description 2
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- VHOQXEIFYTTXJU-UHFFFAOYSA-N Isobutylene-isoprene copolymer Chemical compound CC(C)=C.CC(=C)C=C VHOQXEIFYTTXJU-UHFFFAOYSA-N 0.000 description 1
- 239000004594 Masterbatch (MB) Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 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
- C08L11/00—Compositions of homopolymers or copolymers of chloroprene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/18—Spheres
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to a kind of polysiloxanes microballoons to damp chlorinated scoline composite material and preparation method, formed using formula as below: chlorinated scoline 100, vulcanizing agent 1~3, promotor 1~3, stearic acid 2~4, nano zine oxide 1~2, anti-aging agent 2~4, light magnesium oxide 1~3, polysiloxanes microballoon 5~20 are added to mixing in open mill by formula and obtain polysiloxanes microballoon damping chlorinated scoline composite material.Compared with prior art, the present invention is modified processing to chlorinated scoline using polysiloxanes microballoon, can significantly expand damping temperature domain, improves damping capacity, mechanical property and heating conduction.
Description
Technical field
The present invention relates to a kind of polysiloxanes composite materials, damp chlorinated butyl more particularly, to a kind of polysiloxanes microballoon
Rubber composite material and preparation method thereof.
Background technique
The fast development of modern industry makes mechanical equipment tend to a systems such as high speed, and mechanical relevant vibration and noise
Column problem also generates therewith, and these problems had both accelerated the fatigue damage of mechanical structure, shortens its service life, to a certain degree
On also pollute the environment and be detrimental to health.Therefore, the Efficient Damping material haveing excellent performance is developed, its damping vibration attenuation is improved
It is most important to improve mechanical equipment running environment for effect.
Application of the chlorinated scoline in fields such as damping, dampings is very broad.With auto industry and aerospace industry etc.
The high-tech development in tip, chlorinated scoline have very wide application prospect as outstanding damping substrate.Chlorination fourth
Base rubber is the isobutylene-isoprene copolymer elastomer of active chlorine.In the common vulcanizing system of rubber, isobutene-is different
Pentadiene copolymer elastomer can be crosslinked with one of the carbon-to-carbon double bond of isoprene or Active Chlorine or two kinds, because
The vulcanizate of this chlorinated scoline has good thermal stability and corrosion resistance, can be extreme in deep-etching or high temperature etc.
It is used under environment.The curingprocess rate of chlorinated scoline is faster than the curingprocess rate of butyl rubber, and can be with other elastomers
And use and vulcanize.China's chlorinated scoline is once completely dependent on import, and the domestic demand to chlorinated scoline is with annual
15%~20% growth rate sustainable growth, 2005 annual growths reach 44.4%.
But chlorinated scoline is bad there are high temperature effective damping functional areas not enough broadness, low temperature damping stability and hinders
Buddhist nun's effect, heating conduction are not able to satisfy the defects of damping vibration attenuation rigors, therefore its application field has certain limitation.
Chinese patent CN105906956A discloses a kind of high-damping chlorinated butyl damping rubber and preparation method thereof, described
High-damping chlorinated butyl damping rubber is kneaded to obtain by following components: 100 mass parts chlorinated scolines, 12.5~25 mass parts
Octyl triazone masterbatch, 2~4 mass parts vulcanizing agents, 1~1.5 mass parts promotor, 1~3 mass parts stearic acid, 1~3 matter
Measure part nano zine oxide, 1~3 mass parts anti-aging agent.The patent is only laid particular emphasis on using between octyl triazone and chlorinated scoline
Hydrogen bond action promote the damping capacity of rubber, damper mechanism is single, so that damping temperature domain can not be promoted.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind to significantly improve damping
The polysiloxanes microballoon of performance, mechanical property and heating conduction damps chlorinated scoline composite material and preparation method.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of polysiloxanes microballoon damping chlorinated scoline composite material, using following components and the original of parts by weight content
Material is prepared:
Chlorinated scoline 100, promotor 1~3, stearic acid 2~4, nano zine oxide 1~2, is prevented always vulcanizing agent 1~3
Agent 2~4, light magnesium oxide 1~3, polysiloxanes microballoon 5~20.
The polysiloxanes microballoon is prepared using following methods:
(1) after mixing by normal octane and Span 85, it is added in the water containing ammonium hydroxide, control stirring rate is 300
~500r/min stirs 1~3h；
(2) in the solution obtained to step (1) be added dropwise methyltrimethoxysilane (MTMS), stirring rate be 500~
800r/min stirs 24~36h, until reaction sufficiently, filters reactant, and is put into oven drying for obtained product is filtered,
Obtain polysiloxanes microballoon；
(3) 1~2h, gained polysiloxanes are sieved to the polysiloxanes microballoon after above-mentioned drying using 100~600 mesh screens
Filler of the microballoon as chlorinated scoline, such as selection less than 100 mesh sieve, the partial size of the polysiloxanes microballoon screened out compared with
Greatly, the damping and mechanical properties decrease of chlorinated scoline be will lead to.
The mass ratio of normal octane, Span 85 and water is 60-80:10-20:30-50 in step (1), and the additional amount of ammonium hydroxide is
2-4mL/30-50g water.
The mass ratio of the methyltrimethoxysilane and normal octane that are added dropwise in step (2) is 12-16:60-80.
The vulcanizing agent is sulphur.
The promotor is 2-steryl benzothiazole.
The partial size of the nano zine oxide is 50~70nm, preferably 50~59nm.
The partial size of the light magnesium oxide is 2~5 μm, such as partial size is selected to be greater than 5 μm of light magnesium oxide, will lead to chlorine
Change the damping and mechanical properties decrease of butyl rubber.
The anti-aging agent is N- phenyl-1-naphthylamine.
Polysiloxanes microballoon damp chlorinated scoline composite material preparation method, by chlorinated scoline, vulcanizing agent,
Promotor, stearic acid, nano zine oxide, anti-aging agent, light magnesium oxide, polysiloxanes microballoon are added in open mill by formula,
Control roller temperature carries out mixing 40-60min under conditions of being 20-40 DEG C, and polysiloxanes microballoon damping chlorination fourth is prepared
Base rubber composite material.
Compared with prior art, the invention has the following advantages that
(1) glass transition temperature and the chlorinated scoline difference for the polysiloxanes microballoon being prepared are larger, can after blending
To substantially change the damping capacity of rubber；
(2) since polysiloxanes microsphere surface contains great amount of hydroxy group isopolarity group, the hydrogen in rubber matrix can be increased
Key effect, this reversible hydrogen bond action can make composite material when by extraneous vibration, by the fracture or generation of hydrogen bond,
Thermal energy is converted kinetic energy into, the damping temperature domain and damping that further promote composite material are conducive to.
(3) due to the addition of polysiloxanes microballoon, the crosslink density of material is improved, so that heat is easier in strand
It conducts and spreads in section.Therefore, which is applied in chlorinated scoline, the damping temperature domain of product, damping
Performance, mechanical property and heating conduction etc. are all significantly improved, therefore its application prospect is very wide.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
Following embodiments and comparative example are reported using " material structure and characterization " (Wu Gang Chemical Industry Press .2004)
The method in road tests infrared spectroscopy, molecular weight, the molecular weight distributing index of polysiloxanes microballoon；It is observed using transmission electron microscope method
The particle size of polysiloxanes microballoon；Rubber is tested using the DMA-242 type dynamic mechanical analyzer of German Nai Chi company production
Damping capacity；Using the mechanical property of GB 528-83 test chlorinated scoline；Chlorine is tested using GB/T 11205-2009
Change the heating conduction of butyl rubber.
Comparative example 1
By chlorinated scoline 100g, stearic acid 2g, nano zine oxide 1g, captax 1g, antioxidant A 2g, lightweight oxygen
Change magnesium 1g and sulphur 1g according in aforementioned proportion investment open mill, is kneaded, that is, obtained under conditions of roller temperature is 30 DEG C
Obtain common chlorinated scoline.
Damping temperature domain, fissipation factor, tensile strength, elongation at break and the thermally conductive system of common chlorinated butyl damping rubber
Number, is shown in Table 1.
Comparative example 2
By chlorinated scoline 100g, stearic acid 3g, nano zine oxide 1.5g, captax 2g, antioxidant A 3g, lightweight
Magnesia 2g and sulphur 2g is kneaded, i.e., according in aforementioned proportion investment open mill under conditions of roller temperature is 40 DEG C
Obtain common chlorinated scoline.
Damping temperature domain, fissipation factor, tensile strength, elongation at break and the thermally conductive system of common chlorinated butyl damping rubber
Number, is shown in Table 1.
Comparative example 3
By chlorinated scoline 100g, stearic acid 4g, nano zine oxide 2g, captax 3g, antioxidant A 4g, lightweight oxygen
Change magnesium 3g and sulphur 3g according in aforementioned proportion investment open mill, is kneaded, that is, obtained under conditions of roller temperature is 50 DEG C
Obtain common chlorinated scoline.
Damping temperature domain, fissipation factor, tensile strength, elongation at break and the thermally conductive system of common chlorinated butyl damping rubber
Number, is shown in Table 1.
Embodiment 1
60g normal octane and 10g Span 85 are measured, is stirred evenly.The addition of 3g water and 2ml ammonium hydroxide are measured, is stirred evenly.It will
250mL three-necked flask is added in said mixture, starts to stir, stirring rate 300r/min, mixing time 1h.10g first is added dropwise
Base trimethoxy silane (MTMS), stirring rate 500r/min, mixing time 36h, until reaction sufficiently, filters reactant,
And it is put into oven drying by obtained product is filtered, obtain polysiloxanes microballoon.Using 10 mesh screens to poly- after above-mentioned drying
Silicone microsphere is sieved, sieving time 1h, filler of the gained polysiloxanes microballoon as modified chlorinated butyl rubber.
By chlorinated scoline 100g, stearic acid 2g, nano zine oxide 1g, captax 1g, antioxidant A 2g, lightweight oxygen
Change magnesium 1g, 5g polysiloxanes microballoon and sulphur 1g to put into open mill according to aforementioned proportion, the condition for being 30 DEG C in roller temperature
Under be kneaded, that is, obtain damping rubber of the invention.
Infrared spectroscopy, molecular weight, molecular weight distributing index and the partial size of polysiloxanes microballoon are shown in Table 1.
Damping temperature domain, fissipation factor, tensile strength, elongation at break and the thermal coefficient of damping rubber, are shown in Table 2.
Embodiment 2
70g normal octane and 15g Span 85 are measured, is stirred evenly.The addition of 40g water and 3ml ammonium hydroxide are measured, is stirred evenly.
250mL three-necked flask is added in said mixture, starts to stir, stirring rate 400r/min, mixing time 2h.20g is added dropwise
Methyltrimethoxysilane (MTMS), stirring rate 650r/min, mixing time 30h, until reaction sufficiently, filters reaction
Object, and it is put into oven drying by obtained product is filtered, obtain polysiloxanes microballoon.Using 400 mesh screens to above-mentioned drying after
Polysiloxanes microballoon sieved, sieving time 1.5h, gained polysiloxanes microballoon is filled out as modified chlorinated butyl rubber
Material.
By chlorinated scoline 100g, stearic acid 2g, nano zine oxide 1g, captax 1g, antioxidant A 2g, lightweight oxygen
Change magnesium 1g, 5g polysiloxanes microballoon and sulphur 1g to put into open mill according to aforementioned proportion, the condition for being 30 DEG C in roller temperature
Under be kneaded, that is, obtain damping rubber of the invention.
Infrared spectroscopy, molecular weight, molecular weight distributing index and the partial size of polysiloxanes microballoon are shown in Table 1.
Damping temperature domain, fissipation factor, tensile strength, elongation at break and the thermal coefficient of damping rubber, are shown in Table 2.
Embodiment 3
80g normal octane and 20g Span 85 are measured, is stirred evenly.The addition of 50g water and 4ml ammonium hydroxide are measured, is stirred evenly.
250mL three-necked flask is added in said mixture, starts to stir, stirring rate 500r/min, mixing time 1h.30g is added dropwise
Methyltrimethoxysilane (MTMS), stirring rate 800r/min, for 24 hours, until reaction is sufficiently, suction filtration reacts mixing time
Object, and it is put into oven drying by obtained product is filtered, obtain polysiloxanes microballoon.Using 600 mesh screens to above-mentioned drying after
Polysiloxanes microballoon sieved, sieving time 2h, filler of the gained polysiloxanes microballoon as modified chlorinated butyl rubber.
By chlorinated scoline 100g, stearic acid 2g, nano zine oxide 1g, captax 1g, antioxidant A 2g, lightweight oxygen
Change magnesium 1g, 5g polysiloxanes microballoon and sulphur 1g to put into open mill according to aforementioned proportion, the condition for being 30 DEG C in roller temperature
Under be kneaded, that is, obtain damping rubber of the invention.
Infrared spectroscopy, molecular weight, molecular weight distributing index and the partial size of polysiloxanes microballoon are shown in Table 1.
Damping temperature domain, fissipation factor, tensile strength, elongation at break and the thermal coefficient of damping rubber, are shown in Table 2.
Infrared spectroscopy, molecular weight, the molecular weight distributing index of 1 polysiloxanes microballoon of table
Fissipation factor, tensile strength, elongation at break and the thermal coefficient of 2 damping rubber of table
Can be seen that by the experimental data in table 2 is chlorinated scoline after being modified using polysiloxanes microballoon
The damping temperature domain of composite material is obviously expanded, and damping capacity, mechanical property and heating conduction are obviously improved.
Embodiment 4
A kind of polysiloxanes microballoon damping chlorinated scoline composite material, using following components and the original of parts by weight content
Material is prepared: chlorinated scoline 100, vulcanizing agent 1, promotor 1, stearic acid 2, nano zine oxide 1, anti-aging agent 2, lightweight oxygen
Change magnesium 1, polysiloxanes microballoon 5.
For the vulcanizing agent used for sulphur, promotor is 2-steryl benzothiazole, and the partial size of nano zine oxide is 50nm, gently
The partial size of matter magnesia is 2 μm, and anti-aging agent is N- phenyl-1-naphthylamine.
Polysiloxanes microballoon is prepared using following methods:
(1) after mixing by normal octane and Span 85, it is added in the water containing ammonium hydroxide, normal octane, Span 85 and water
Mass ratio be 60:10:30, the additional amount of ammonium hydroxide is 2mL/30g water, and control stirring rate is 300r/min, stirring 3h；
(2) methyltrimethoxysilane (MTMS) is added dropwise in the solution obtained to step (1), the methyl trimethoxy oxygroup of dropwise addition
The mass ratio of silane and normal octane is 12:60, stirring rate 500r/min, stirs 36h, until reaction sufficiently, filters reaction
Object, and it is put into oven drying by obtained product is filtered, obtain polysiloxanes microballoon；
(3) 1h, gained polysiloxanes microballoon conduct are sieved to the polysiloxanes microballoon after above-mentioned drying using 100 mesh screens
The filler of chlorinated scoline.
Polysiloxanes microballoon damps chlorinated scoline composite material in the preparation, by chlorinated scoline, vulcanizing agent, rush
Open mill is added to by the above formula into agent, stearic acid, nano zine oxide, anti-aging agent, light magnesium oxide, polysiloxanes microballoon
In, control roller temperature carries out mixing 60min under conditions of being 20 DEG C, and polysiloxanes microballoon damping chlorinated butyl rubber is prepared
Glue composite material.
Embodiment 5
A kind of polysiloxanes microballoon damping chlorinated scoline composite material, using following components and the original of parts by weight content
Material is prepared: chlorinated scoline 100, vulcanizing agent 2, promotor 2, stearic acid 3, nano zine oxide 1, anti-aging agent 3, lightweight oxygen
Change magnesium 2, polysiloxanes microballoon 10.
For the vulcanizing agent used for sulphur, promotor is 2-steryl benzothiazole, and the partial size of nano zine oxide is 59nm, gently
The partial size of matter magnesia is 3 μm, and anti-aging agent is N- phenyl-1-naphthylamine.
Polysiloxanes microballoon is prepared using following methods:
(1) after mixing by normal octane and Span 85, it is added in the water containing ammonium hydroxide, normal octane, Span 85 and water
Mass ratio be 70:15:40, the additional amount of ammonium hydroxide is that 3mL/40g water management stirring rate is 400r/min, stir 2h；
(2) methyltrimethoxysilane (MTMS) is added dropwise in the solution obtained to step (1), the methyl trimethoxy oxygroup of dropwise addition
The mass ratio of silane and normal octane is 14:70, stirring rate 600r/min, stirs 30h, until reaction sufficiently, filters reaction
Object, and it is put into oven drying by obtained product is filtered, obtain polysiloxanes microballoon；
(3) 2h, gained polysiloxanes microballoon conduct are sieved to the polysiloxanes microballoon after above-mentioned drying using 400 mesh screens
The filler of chlorinated scoline.
Polysiloxanes microballoon damp chlorinated scoline composite material preparation method, by chlorinated scoline, vulcanizing agent,
Promotor, stearic acid, nano zine oxide, anti-aging agent, light magnesium oxide, polysiloxanes microballoon are added in open mill by formula,
Control roller temperature carries out mixing 50min under conditions of being 30 DEG C, and polysiloxanes microballoon damping chlorinated scoline is prepared
Composite material.
Embodiment 6
A kind of polysiloxanes microballoon damping chlorinated scoline composite material, using following components and the original of parts by weight content
Material is prepared:
Chlorinated scoline 100, vulcanizing agent 3, promotor 3, stearic acid 4, nano zine oxide 2, anti-aging agent 4, lightweight oxidation
Magnesium 3, polysiloxanes microballoon 20.
Vulcanizing agent is sulphur, and promotor is 2-steryl benzothiazole, and the partial size of nano zine oxide is 70nm, lightweight oxidation
The partial size of magnesium is 5 μm, and anti-aging agent is N- phenyl-1-naphthylamine.
Polysiloxanes microballoon is prepared using following methods:
(1) after mixing by normal octane and Span 85, it is added in the water containing ammonium hydroxide, normal octane, Span 85 and water
Mass ratio be 80:20:50, the additional amount of ammonium hydroxide is 4mL/50g water, and control stirring rate is 500r/min, stirring 1h；
(2) methyltrimethoxysilane (MTMS) is added dropwise in the solution obtained to step (1), the methyl trimethoxy oxygroup of dropwise addition
The mass ratio of silane and normal octane is 16:80, stirring rate 800r/min, and stirring for 24 hours, until reaction is abundant, filters reaction
Object, and it is put into oven drying by obtained product is filtered, obtain polysiloxanes microballoon；
(3) 1h, gained polysiloxanes microballoon conduct are sieved to the polysiloxanes microballoon after above-mentioned drying using 600 mesh screens
The filler of chlorinated scoline.
Polysiloxanes microballoon damp chlorinated scoline composite material preparation method, by chlorinated scoline, vulcanizing agent,
Promotor, stearic acid, nano zine oxide, anti-aging agent, light magnesium oxide, polysiloxanes microballoon are added in open mill by formula,
Control roller temperature carries out mixing 40min under conditions of being 40 DEG C, and polysiloxanes microballoon damping chlorinated scoline is prepared
Composite material.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (11)
1. a kind of polysiloxanes microballoon damps chlorinated scoline composite material, which is characterized in that the composite material is using following
The raw material of component and parts by weight content is prepared:
Chlorinated scoline 100, vulcanizing agent 1~3, promotor 1~3, stearic acid 2~4, nano zine oxide 1~2, anti-aging agent 2~
4, light magnesium oxide 1~3, polysiloxanes microballoon 5~20.
2. a kind of polysiloxanes microballoon according to claim 1 damps chlorinated scoline composite material, which is characterized in that
The polysiloxanes microballoon is prepared using following methods:
(1) after mixing by normal octane and Span 85, it being added in the water containing ammonium hydroxide, control stirring rate is 300~
500r/min stirs 1~3h；
(2) methyltrimethoxysilane (MTMS) is added dropwise in the solution obtained to step (1), stirring rate is 500~800r/
Min stirs 24~36h, until reaction sufficiently, filters reactant, and is put into oven drying for obtained product is filtered, is gathered
Silicone microsphere；
(3) 1~2h, gained polysiloxanes microballoon are sieved to the polysiloxanes microballoon after above-mentioned drying using 100~600 mesh screens
Filler as chlorinated scoline.
3. a kind of polysiloxanes microballoon according to claim 2 damps chlorinated scoline composite material, which is characterized in that
The mass ratio of normal octane, Span 85 and water is 60-80:10-20:30-50 in step (1).
4. a kind of polysiloxanes microballoon according to claim 2 damps chlorinated scoline composite material, which is characterized in that
The additional amount of ammonium hydroxide is 2-4mL/30-50g water in step (1).
5. a kind of polysiloxanes microballoon according to claim 2 damps chlorinated scoline composite material, which is characterized in that
The mass ratio of the methyltrimethoxysilane and normal octane that are added dropwise in step (2) is 12-16:60-80.
6. a kind of polysiloxanes microballoon according to claim 1 damps chlorinated scoline composite material, which is characterized in that
The vulcanizing agent is sulphur, and the promotor is 2-steryl benzothiazole.
7. a kind of polysiloxanes microballoon according to claim 1 damps chlorinated scoline composite material, which is characterized in that
The partial size of the nano zine oxide is 50~70nm, and the partial size of the light magnesium oxide is 2~5 μm.
8. a kind of polysiloxanes microballoon according to claim 7 damps chlorinated scoline composite material, which is characterized in that
The partial size of the nano zine oxide is 50~59nm.
9. a kind of polysiloxanes microballoon according to claim 1 damps chlorinated scoline composite material, which is characterized in that
The anti-aging agent is N- phenyl-1-naphthylamine.
10. the preparation of polysiloxanes microballoon damping chlorinated scoline composite material as claimed in any one of claims 1-9 wherein
Method, which is characterized in that this method by chlorinated scoline, vulcanizing agent, promotor, stearic acid, nano zine oxide, anti-aging agent,
Light magnesium oxide, polysiloxanes microballoon are added in open mill by formula, and control roller temperature carries out under conditions of being 20-40 DEG C
It is kneaded, polysiloxanes microballoon damping chlorinated scoline composite material is prepared.
11. a kind of preparation side of polysiloxanes microballoon damping chlorinated scoline composite material according to claim 10
Method, which is characterized in that the time control of mixing is 40-60min.
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| CN110483907A (en) * | 2019-08-20 | 2019-11-22 | 上海工程技术大学 | A kind of modified chlorinated butyl rubber damping material |
| CN112876753B (en) * | 2021-01-21 | 2021-11-16 | 中国石油大学(北京) | Covalent organic framework/styrene butadiene rubber composite material and preparation method thereof |
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| US4678828A (en) * | 1986-05-21 | 1987-07-07 | Shin-Etsu Chemical Co., Ltd. | Vibration-damping rubber composition |
| US5488081A (en) * | 1993-11-04 | 1996-01-30 | Lord Corporation | Highly damped organic elastomer composition |
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|---|---|---|---|---|
| US4678828A (en) * | 1986-05-21 | 1987-07-07 | Shin-Etsu Chemical Co., Ltd. | Vibration-damping rubber composition |
| US5488081A (en) * | 1993-11-04 | 1996-01-30 | Lord Corporation | Highly damped organic elastomer composition |
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| "Acid-free synthesis of poly-organo-siloxane spherical particles using a W/O emulsion";Taichi Matsumoto等;《Journal of materials chemistry》;20030530;第13卷;第1764-1770页 |
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