CN106751736A - A kind of silicon rubber/polyurethane termoplastic elastomer and preparation method thereof - Google Patents
A kind of silicon rubber/polyurethane termoplastic elastomer and preparation method thereof Download PDFInfo
- Publication number
- CN106751736A CN106751736A CN201710048159.4A CN201710048159A CN106751736A CN 106751736 A CN106751736 A CN 106751736A CN 201710048159 A CN201710048159 A CN 201710048159A CN 106751736 A CN106751736 A CN 106751736A
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- Prior art keywords
- silicon rubber
- tpue
- polyurethane
- dynamic vulcanization
- elastomer
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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
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
- C08L75/06—Polyurethanes from polyesters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
- C08L75/08—Polyurethanes from polyethers
-
- 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
Abstract
The invention discloses a kind of polyurethane/silicon rubber thermoplastic elastomer and preparation method thereof, there is provided a kind of repeatable processing, the silicon rubber/polyurethane termoplastic elastomer with excellent mechanical property and heat-resisting oil resistance and preparation method;The elastomer is made up of polyurethane, silicon rubber, crosslinking agent and compatilizer etc.;Its preparation method includes:In banbury, under 160~200 DEG C of blending temperature, polyurethane is added in blending equipment first, adds silicon rubber, compatilizer after being blended 3~4 minutes, to add crosslinking agent afterwards;After reactive blending 6~7 minutes, the polyurethane/silicon rubber thermoplastic elastomer of high-performance dynamic vulcanization is obtained;Compared with other types of thermoplastic elastomer (TPE), with excellent heat resistance, crocking resistance and mechanical property, good handling property can be widely applied to the material with human contact, and the field such as automobile, building, medicine equipment, cable.
Description
Technical field
Silicon rubber/polyurethane comixing thermoplastic elastomer the present invention relates to a kind of dynamic vulcanization and preparation method thereof.
Technical background
Dynamic vulcanization is by thermoplastic (including thermoplastic elastomer and thermoplastic), vulcanizable rubber and vulcanization
The agent melt blending in the presence of certain temperature and shearing force together, rubber in this process, be cut into little particle (point
Dephasing) it is distributed in thermoplastic (continuous phase), while rubber grain completes crosslinking, form thermoplastic elastomer (TPV).It is this
Material has preferable performance, and relatively low processing cost simultaneously.This preparation method is obtained in that high-crosslinking-degree rubber phase.
Therefore the mechanical strength and oil resistivity of TPV are higher.Coran of Monsanto companies in the U.S. etc. (existing name Solutia Inc.) is opened
The TPV (US4130535) of PP/EPDM is sent, and this elastomer was transformed into commodity first in 1980
“Santoprene”。
This material has excellent processability, the high resiliency of rubber, good adaptability, economy and low stain
And the favor in market is obtained, the occasion of present nearly all application rubber can be replaced using Santoprene.But,
Santoprene heat resistances are relatively low, and in some requirement extremely oil resistants, the very high environment of some heatproofs requirement limits this
The application of material.
Urethane thermoplastic elastomer (TPU) is polymerized by isocyanates (monomer) with hydroxy compounds, with good
Oil resistivity, wearability, toughness, resistance to ag(e)ing and cohesive.Adaptation wide temperature range can be obtained with different material.But it
Resistance to ag(e)ing and heat resistance are poor.TPU can be blended with multiple material, the excellent high molecule alloy material of forming properties.Use
Blend, can be not only molded with methods such as extrusion, injections, and more easier to process than TPU.
Silicon rubber refers to that main chain is alternately made up of silicon and oxygen atom, and generally two rubbers of organic group are connected with silicon atom
Glue.Silicon rubber is characterized in significantly height temperature stability, and under the hot environment more than 200 DEG C, silicon rubber remains to keep certain
Pliability, resilience and case hardness, and mechanical property is without significant change.The Weatherproof ageing-resistant performance of silicon rubber is also dashed forward very much
Go out.But the mechanical strength of silicon rubber is poor, only there is medium oil resistant, solvent resistance.Therefore, by dynamic vulcanization method system
Standby silicon rubber/TPU thermoplastic elastomers, will make the advantage of both materials complementary, obtain the thermoplastic elastomer of not only high temperature resistant but also oil resistant.
United States Patent (USP) US 4500688 makees crosslinking agent using the compound containing multiple (big to be equal in 2) si-h bond groups, metal platinum or its
Compound as catalyst preparation containing a small amount of silicon rubber (silicon rubber consumption is generally 10%, less than silicon rubber 40%)/
TPU dynamic thermoplastic elastomers.This elastomer has good mechanical property.United States Patent (USP) US6759487B2 is used containing multiple
The compound of (big be equal in 2) si-h bond group makees crosslinking agent, and metal platinum or its compound are as catalyst preparation containing big
(silicon rubber consumption is typically greater than 50% to amount silicon rubber, silicon rubber/TPU dynamic thermoplastic elastomers up to 85%), also can
Obtain the thermoplastic elastomer with good mechanical property.Chinese patent CN102153853A is also used and is contained multiple si-h bond bases
The compound of group makees crosslinking agent, and metal platinum or its compound are used as catalyst, while adding silicon modified polyurethane as compatible
Agent, is prepared for silicon rubber/TPU dynamic vulcanization thermoplastic elastomers.
Peroxide is a kind of common crosslinking agent, and cheap, material is easy to get.Metal or its salt such as platinum need not be used
As catalyst.Up to the present, there is not yet preparing silicon rubber/TPU thermoplastic elastomers as crosslinking agent using peroxide
Patents report.The present invention provides a kind of method, using cheap and easily-available peroxide as crosslinking agent, prepares dynamic sulphur
SiClx rubber/TPU thermoplastic elastomers.
The content of the invention
It is an object of the invention to provide a kind of excellent in mechanical performance, the silicon rubber/TPU thermoplastic elastomers of repeatable processing and
Preparation method.
The present invention provides a kind of silicon rubber/TPU thermoplastic elastomers, by silicon rubber, polyurethane, peroxide cross-linking agent, group
Into.The composition and content of the thermoplastic elastomer be:
The weight portion of TPUE 100
The weight portion of silicon rubber 20~556
The reaction weight portion of compatilizer 0.01~5
The weight portion of peroxide 0.1~10
Described TPUE is Polyether-type thermoplastic polyurethane elastomer or the poly- ammonia of polyether thermoplastic
Ester elastomer.
Described silicon rubber is that a kind of molecular backbone is handed over by silicon atom and oxygen atom for silicon rubber (Silicone Rubber)
For the elastomeric material based on composition (- Si-O-Si -) macromolecule, polymer side chain is organic group, and these organic groups can
To be-CH3 ,-C2H3 or-C6H5 etc., while each molecule must also contain the vinyl of at least 2 or more.
Described reaction compatilizer is silane coupler.
Described peroxide is the organic compound containing peroxy-radical-O-O-.
The preparation method of silicon rubber of the invention/TPU thermoplastic elastomers is comprised the following steps:In banbury, 150~
Under 220 DEG C of blending temperature, polyurethane is added in banbury, is subsequently adding silicon rubber gross rubber (having been added to SiO2),
Blending adds phase solvent after 5 minutes, then after being blended 2~5 minutes, adds peroxide cross-linking agent to carry out dynamic vulcanization.Dynamic sulphur
Silicon rubber/TPU thermoplastic elastomers are obtained after changing 5~15 minutes.
The silicon rubber that the present invention is used is the silicon rubber filled by filler (aerosil), in each of which molecule,
It is average that at least there are two or more vinyl.TPUE is PAUR and/or polyethers
Type polyurethane.Reaction compatilizer is the silane coupler with chemical reactivity, such as gamma-aminopropyl-triethoxy-silane,
γ-(2,3- glycidoxy) propyl trimethoxy silicane, 3- NCO propyl-triethoxysilicanes etc.;Peroxide is
Organic peroxide, such as 2,5- dimethyl, 2,5- di-t-butyl ethane peroxides, 1,1- di-t-butyl methyl -3,5,5- front threes
Butylcyclohexane, 2,5- dimethyl -2,5 two (t-butyl peroxy) hexanes, double trimethylbenzene peroxide etc..
The present invention prepares thermoplastic elastomer using dynamic vulcanization technology, and blend is provided in banbury or double screw extruder
Shearing force and temperature in the presence of, peroxide cross-linking agent is crosslinked to silicon rubber, and is dispersed into TPU continuous phases micro-
Meter level particle.
The preparation method that the present invention is provided, is reacted by reacting compatilizer with silicon rubber, and pole is connected on silicon rubber molecule
Property group, has been added the compatibility between silicon rubber and TPU, so as to improve the performance of blend.
The present invention uses cheap and easily-available peroxide as crosslinking agent, without being contained using the expensive of existing patent report
There are the organo-silicon compound and metal platinum of multiple si-h bonds or the cross-linking system of its salt catalyst.Prepare in this way
Silicon rubber/TPU thermoplastic elastics body processing technology is simple, and low production cost can reclaim repetition processing and utilization.
It is of the invention, with vulcanization is not required to, to be processed using the processing method of extrusion compared with general vulcanized rubber,
The silicon rubber of preparation/TPU thermoplastic elastomers have excellent heat resistance and mechanical and physical character, can be applied to automobile, building
Etc. industry.And thermoplastic elastomer feel is smooth, the product of contact human skin is can be widely used for.
Specific embodiment
The present invention is specifically described and further illustrated below by embodiment, it is impossible to the limitation present invention is not understood as
Scope.The person skilled in the art in the field can make some nonessential improvement and tune according to the content of the invention described above
It is whole.
HAAKE rheometers temperature setting is 190 DEG C by embodiment 1~3, and rotor speed is set to 50rpm, according to the institute of table 1
The formula indicated, (is Nanjing Dong Jue companies by TPU (being the EU 1580 of Wan Hua chemical companies production) and silicon rubber
The NE7170 of production) it is added in HAAKE rheometers, after material is well mixed, add reaction compatilizer γ-second of aminopropyl three
TMOS mixes, and after after torque balance, adds peroxide cross-linking agent, is blended 5 minutes.The peroxide of the present embodiment is 2,
The di-t-butyl peroxyhexane of 5- dimethyl -2,5.The physical and mechanical property of elastomer is listed in table 2
The preparation formula of the embodiment 1~4 of table 1 and the thermoplastic elastomer of comparative example 4
Material | Silicon rubber | TPU | Compatilizer | Crosslinking agent |
Embodiment 1 | 20 | 80 | 0.0 | 0.4 |
Embodiment 2 | 40 | 60 | 0.0 | 0.4 |
Embodiment 3 | 50 | 50 | 0.0 | 0.4 |
Comparative example 4 | 50 | 50 | 0.0 | 0 |
Comparative example 4 is prepared according to the preparation technology of embodiment 1~4, but without peroxide cross-linking agent.Comparative example 4
Mechanical property be listed in table 2.Comparing embodiment 3 and comparative example 4, it can be seen that addition crosslinking agent carries out the silicon rubber after dynamic vulcanization
The performance of glue/TPU thermoplastic elastomers is improved.
The physical and mechanical property of the embodiment 1~3 of table 2 and the thermoplastic elastomer of comparative example 4
Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 4 | |
Tensile strength (MPa) | 23.8 | 12.2 | 9.39 | 6.8 |
Elongation at break (%) | 775 | 612 | 560 | 485 |
Tensile set (%) | 65 | 45 | 32 | 42 |
Shore hardness A | 72 | 66 | 68 | 62 |
HAAKE rheometers temperature setting is 180 DEG C by embodiment 5~7, and rotor speed is set to 50rpm, according to the institute of table 3
The formula indicated, (is Nanjing Dong Jue companies by TPU (being the PAUR 8285 of Wan Hua chemical companies production) and silicon rubber
The NE7170 of production) it is added in HAAKE rheometers, after material is well mixed, add reaction compatilizer γ-second of aminopropyl three
TMOS mixes, and after after torque balance, adds peroxide cross-linking agent, is blended 5 minutes.The peroxide of the present embodiment is 2,
The di-t-butyl peroxyhexane of 5- dimethyl -2,5.The physical and mechanical property of elastomer is listed in table 4
The preparation formula of the embodiment 5~7 of table 3 and the thermoplastic elastomer of comparative example 8
Material | Silicon rubber | TPU | Compatilizer | Crosslinking agent |
Embodiment 5 | 50 | 50 | 0.4 | 0.8 |
Embodiment 6 | 50 | 50 | 0.4 | 1.2 |
Embodiment 7 | 50 | 50 | 0.4 | 1.6 |
Comparative example 8 | 50 | 50 | 0.0 | 1.6 |
Comparative example 8 is prepared according to the preparation technology of embodiment 5~7, but without compatilizer.The mechanical property of comparative example 8
Table 4 can be listed in.
Comparing embodiment 3 and comparative example 4, it can be seen that addition crosslinking agent carries out the silicon rubber/TPU thermoplastics after dynamic vulcanization
The performance of elastomer is improved.From table 3 and table 4 it can be seen that increasing dosage of crosslinking agent in certain limit, in tensile strength
Rise, performance is also substantially increased after adding compatilizer.
The physical and mechanical property of the embodiment 5~8 of table 4 and the thermoplastic elastomer of comparative example 8
Embodiment 5 | Embodiment 6 | Embodiment 7 | Comparative example 8 | |
Tensile strength (MPa) | 11.5 | 12.1 | 15.8 | 13.3 |
Elongation at break (%) | 570 | 580 | 512 | 600 |
Claims (8)
1. a kind of silicon rubber/urethane thermoplastic elastomer, it is characterised in that:Have urethane thermoplastic elastomer (TPU), silicon rubber,
Peroxide cross-linking agent, reaction compatilizer are constituted, and the composition of the thermoplastic elastomer is by weight:
It is 2. according to claim 1 to prepare dynamic vulcanization silicon rubber/TPUE, it is characterised in that:Institute
It is the silicon rubber by white carbon reinforcement to state silicon rubber, and white carbon is divided into gas-phase silica and precipitated silica, the silicon rubber
From the silicon rubber through gas-phase silica reinforcement.
It is 3. according to claim 1 to prepare dynamic vulcanization silicon rubber/TPUE, it is characterised in that:Institute
Polyurethane is stated for one or more of polyester-type TPUE and Polyether-type thermoplastic polyurethane elastomer.
It is 4. according to claim 1 to prepare dynamic vulcanization silicon rubber/TPUE, it is characterised in that:Institute
Crosslinking agent is stated for organic peroxide, such as 2,5- dimethyl -2,5- t-butyl-peroxyhexanes (DBPH) etc..
5. according to claim 1 to prepare dynamic vulcanization organic silicon rubber/TPUE, its feature exists
In:The compatilizer is gamma-aminopropyl-triethoxy-silane (KH550), 3- NCO propyl-triethoxysilicanes
(KH907), one or more in γ-(2,3- glycidoxies) propyl trimethoxy silicane (KH560).
6. according to claim 1 to prepare dynamic vulcanization organic silicon rubber/TPUE, its feature exists
In:Organic silicon rubber/the TPUE presses mass fraction ratio, and ratio used can be:Organic silicon rubber:Thermoplastic
Property polyurethane=10: 90~70: 30.
7. a kind of method of the organic silicon rubber/TPUE prepared described in any one of claim 1 to 6, its
It is characterised by, comprises the following steps:
(1) first, the organic silicon rubber of described part is added in banbury together with TPUE, melting is altogether
It is mixed 3~5 minutes;
(2) secondly, the compatilizer of the number is added to be blended 1~5 minute;
(3) it is last, the peroxide cross-linking agent dynamic vulcanization of the number is added, cure time is 2~6 minutes, is pressed into mark
Quasi- batten.
8. preparation method according to claim 9, it is characterised in that:The banbury technological parameter is as follows:Internally mix temperature
160~200 DEG C, 50~90rpm of rotating speed, cure time 2~6 minutes.
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Cited By (21)
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CN108587123A (en) * | 2018-05-10 | 2018-09-28 | 成都思立可科技有限公司 | A kind of dynamic-vulcanization thermoplastic Polyurethane/Polysiloxane elastomer and preparation method thereof |
CN108948508A (en) * | 2018-06-29 | 2018-12-07 | 郑刚 | A kind of material and preparation method thereof improving rubber belt track patterned surface glue service life |
CN109181278A (en) * | 2018-09-17 | 2019-01-11 | 上海玉城高分子材料股份有限公司 | Polyurethane/fluorine silicone rubber thermoplastic elastomer (TPE) and preparation method thereof |
CN109517367A (en) * | 2018-11-30 | 2019-03-26 | 广东省石油与精细化工研究院 | A kind of conductive thermoplastic dynamic vulcanization silicon rubber and preparation method thereof |
CN109553982A (en) * | 2017-09-25 | 2019-04-02 | 北京化工大学 | A kind of thermoplastic sulfurized rubber and preparation method |
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CN109608867A (en) * | 2018-11-30 | 2019-04-12 | 广东省石油与精细化工研究院 | A kind of thermoplastic dynamic vulcanized silicon rubber of oil-resisting type and preparation method thereof |
CN110283451A (en) * | 2019-07-26 | 2019-09-27 | 石家庄硕若科技有限公司 | A kind of novel elastic particle and preparation method thereof |
CN110819118A (en) * | 2018-08-14 | 2020-02-21 | 北京化工大学 | Conductive elastomer composite material for wearable device and preparation method thereof |
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CN110903654A (en) * | 2019-11-15 | 2020-03-24 | 中广核三角洲集团(苏州)特威塑胶有限公司 | Environment-friendly thermoplastic silicone rubber elastomer and preparation method thereof |
CN110903627A (en) * | 2019-10-30 | 2020-03-24 | 晋江兴迅新材料科技有限公司 | Thermoplastic elastomer blend supercritical foaming material and preparation method thereof |
CN111016043A (en) * | 2019-10-30 | 2020-04-17 | 晋江兴迅新材料科技有限公司 | Preparation method of thermoplastic elastomer blend supercritical foaming material |
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