CN109796767A - A kind of silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network - Google Patents
A kind of silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network Download PDFInfo
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- CN109796767A CN109796767A CN201811597458.4A CN201811597458A CN109796767A CN 109796767 A CN109796767 A CN 109796767A CN 201811597458 A CN201811597458 A CN 201811597458A CN 109796767 A CN109796767 A CN 109796767A
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- silicon rubber
- thermoplastic elastomer
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- sliding cross
- polyolefin
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Abstract
The invention discloses a kind of silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network.This silicon rubber/the polyolefin thermoplastic elastomer with sliding cross-linked network is made of raw material below: vinylsiloxane rubber, polyolefin, polyrotaxane, vulcanizing agent, filler, constitution controller.The invention also discloses this silicon rubber/polyolefin thermoplastic elastomer preparation methods with sliding cross-linked network.The present invention uses a kind of supermolecule polyrotaxane containing vinyl, carries out dynamic vulcanization processing to silicon rubber and polyolefin under melt blending state, prepares the silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network.Polyrotaxane plays the double action of sliding crosslinking points and compatilizer, assigns silicon rubber/polyolefin thermoplastic elastomer high intensity, high tenacity, the high excellent characteristics such as compatible, has a extensive future.
Description
Technical field
The present invention relates to a kind of silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network.
Background technique
The main chain of organosilicon material is silicon atom and oxygen atom is alternately arranged composition, while the side group of silicon atom is organic group
Group, therefore have both organic and inorganic characteristic.Special chemical structure assigns the extremely low surface tension of organosilicon, excellent strand
The advantages that flexibility, good resistant of high or low temperature and good biocompatibility, weather-proof, corrosion-resistant, electric insulation, good permeability.
Therefore, organosilicon is widely used in multiple fields such as petrochemical industry, defence and military, aerospace, electronic apparatus.However, organic
There is obvious deficiency, and the sulphur that silicon rubber is traditional in mechanical strength, resistance to acid and alkali, the solvent resistance of silicon materials especially silicon rubber
Change mode is heat cure, and the leftover pieces and waste product that production process generates can not recycle processing, and disadvantage mentioned above limits silicon rubber
High-performance, the value added applications of glue.
Polyolefinic raw materials are abundant, cheap, good mechanical performance, comprehensive performance protrudes, and are that yield is maximum, most widely used
A kind of high molecular material.In view of the unique structure of organosilicon and performance, if organosilicon and polyolefin combined, preparation
Silicon rubber/polyolefin thermoplastic elastomer can improve the strand flexibility of polyolefin, widen using temperature, reduce surface
Can, weatherability is improved, and can overcome the disadvantages that organosilicon in mechanical strength, resistance to acid and alkali, solvent resistance, compatible with carbon-based material
Property etc. defect, also with easy processing, can reuse repeatedly green character, research significance is great.
Dynamic vulcanization process, which refers to, makes the vulcanization of rubber during plastics and rubber melt blending, under high shear by sulfide
Granulating is sheared, and is dispersed in plastic substrate, is the effective way for preparing thermoplastic elastomer (TPE).CN102040841A and
CN107325404A reports dynamic vulcanization method and prepares silicon rubber/polyolefin thermoplastic elastomer, but due to traditional silicon rubber
The restriction of glue cross-linked network and the very poor influence of silicon rubber and compatible polyolefin, prepared elastomer can not have simultaneously
Standby high-intensitive and high tenacity, which has limited the performance applications of such elastomer.
Polyrotaxane is a kind of inner-lock-type Subjective and Objective supramolecular system acted on by self assembly, and ring molecule runs through
Enter line style axis macromolecular chain, can slide and rotate on molecular shaft chain, there are unique kinetic characteristics.If using suitable
Means can form Three-dimensional Supramolecular Network structure using the ring molecule in polyrotaxane as crosslinking points.Due to ring molecule
Crosslinking points are not fixed, and can be moved freely through along molecular shaft chain, thus this Three-dimensional Supramolecular Network structure has uniqueness
Mechanical property.Also polyrotaxane is not applied at present to prepare silicon rubber/polyolefin thermoplastic elastomer relevant report.
Summary of the invention
It is of the existing technology in order to overcome the problems, such as, overcome silicon rubber/polyolefin thermoplastic elastomer mechanical property and phase
The insufficient defect of capacitive, the purpose of the present invention is to provide a kind of sliding crosslinkings for being provided simultaneously with high tenacity, high intensity, Gao Xiangrong
Silicon rubber/polyolefin thermoplastic elastomer of network.The present invention also provides this silicon rubber with sliding cross-linked network/poly-
The preparation method of olefinic thermoplastic elastomer.
For achieving the above object, the technical solution used in the present invention is:
A kind of silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network, is by the raw material of following mass parts
Composition: 20~80 parts of vinylsiloxane rubber, 20~80 parts of polyolefin, 5~50 parts of polyrotaxane, 0.1~5 part of vulcanizing agent, filler 5~
60 parts, 1~8 part of constitution controller.
Preferably, this silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network, is by following mass parts
Raw material composition: 20~80 parts of vinylsiloxane rubber, 20~80 parts of polyolefin, 5~50 parts of polyrotaxane, 0.5~2 part of vulcanizing agent,
10~30 parts of filler, 2~4 parts of constitution controller.
Preferably, in this silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network, vinylsiloxane rubber
Vinyl molar content be 0.08%~1%；It is further preferred that the vinyl molar content of vinylsiloxane rubber is
0.08%~0.3%.
Preferably, in this silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network, the straight chain of polyrotaxane
Shape molecule is at least one of polyethylene, polypropylene, polybutadiene, polyisobutene, polyisoprene, the ring-type point of polyrotaxane
Son is the cyclodextrin containing vinyl, and the end-capping group of polyrotaxane is cyclodextrin group, dinitrobenzene base class group, adamantane
At least one of base class group, polynuclear aromatic same clan group, trityl class group；It is further preferred that the ring of polyrotaxane
Shape molecule is alpha-cyclodextrin or at least one of beta-cyclodextrin or gamma-cyclodextrin containing vinyl.
Preferably, the ring molecule in polyrotaxane containing vinyl is made by functional group's substitution reaction, i.e., by hydroxypropylation
Alpha-cyclodextrin or beta-cyclodextrin or gamma-cyclodextrin, with isocyanatoethyl, 2- acryloyl-oxyethyl isocyanic acid
Bis- (acryloyloxymethyl) ethyl isocyanates of ester, 1,1-, 3- methyl allyl acyloxypropyl trimethoxysilane, 3- methyl-prop
At least one of alkene methyl dimethoxysilane, methacryloxypropyl are taken
Generation reaction；Catalyst used in substitution reaction is organotin catalysts, preferably dibutyltin diacetate, di lauric dibutyl
At least one of tin.
Preferably, in this silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network, polyolefin is poly- second
At least one of alkene, polypropylene, ethylene-octene copolymer, ethylene-butene copolymer, ethylene-hexene co-polymers；Further
Preferably, polyolefin is that high density polyethylene (HDPE), low density polyethylene (LDPE), linear low density polyethylene, polypropylene, ethylene-octene are total
At least one of polymers, ethylene-butene copolymer, ethylene-hexene co-polymers；Still further preferably, polyolefin is ethylene-
Octene copolymer and high density polyethylene (HDPE) are with mass ratio 1:(0.2~2) formed composition, ethylene-octene copolymer and poly- third
Alkene is with mass ratio 1:(0.2~2) formed composition, linear low density polyethylene and polypropylene with mass ratio 1:(0.2~2) shape
At composition, ethylene-hexene co-polymers and polypropylene with mass ratio 1:(0.2~2) at least one of the composition that is formed.
Preferably, in this silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network, vulcanizing agent is peroxide
Compound vulcanizing agent；It is further preferred that vulcanizing agent is peroxidating bis- (2,4- dichloro-benzoyls), di-t-butyl peroxide, peroxide
Change at least one of diisopropylbenzene (DIPB), 2,5- dimethyl -2,5- bis(t-butylperoxy) hexane.
Preferably, in this silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network, filler is hard charcoal
At least one of black, talcum powder, mica powder, titanium dioxide, silica flour, calcium carbonate；It is further preferred that filler is white carbon black；
Still further preferably, filler is at least one of gas-phase silica, precipitated silica.
Preferably, in this silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network, constitution controller is
At least one of hydroxy silicon oil, methyltriethoxysilane, hexamethyldisilazane.
Above-mentioned this silicon rubber/polyolefin thermoplastic elastomer preparation method with sliding cross-linked network, including with
Lower step:
1) vinylsiloxane rubber, filler and constitution controller are kneaded, obtain melting silicone rubber；
2) by melting silicone rubber, polyolefin, polyrotaxane and vulcanizing agent add twin-screw extrude carry out dynamic vulcanization it is anti-
It answers, squeezes out, be granulated, obtain silicon rubber/polyolefin thermoplastic elastomer of sliding cross-linked network.
Preferably, this silicon rubber/polyolefin thermoplastic elastomer preparation method step with sliding cross-linked network
1) in, mixing carries out in mixer or kneader, and machined parameters are as follows: melting temperature is 60 DEG C~140 DEG C, and mixing time is
0.2h~2h, revolving speed are 20r/min~120r/min；It is further preferred that in preparation method step 1), be kneaded in mixer or
Carry out in kneader, machined parameters are as follows: melting temperature is 90 DEG C~110 DEG C, and mixing time is 1h~2h, revolving speed 90r/
Min~110r/min.
Preferably, this silicon rubber/polyolefin thermoplastic elastomer preparation method step with sliding cross-linked network
2) in, the processing temperature of double screw extruder is 160 DEG C~220 DEG C, and screw speed is 150r/min~340r/min, dynamic sulphur
The time of change is 0.5min~3min；It is further preferred that in preparation method step 2), the processing temperature of double screw extruder is
170 DEG C~180 DEG C, screw speed is 270r/min~300r/min, and the time of dynamic vulcanization is 0.5min~1.5min.
The beneficial effects of the present invention are:
The present invention uses a kind of supermolecule polyrotaxane containing vinyl, to silicon rubber and polyolefin under melt blending state
Dynamic vulcanization processing is carried out, the silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network is prepared.Polyrotaxane, which plays, to be slided
The double action of dynamic crosslinking points and compatilizer, assigns silicon rubber/polyolefin thermoplastic elastomer high intensity, high tenacity, Gao Xiangrong
Etc. excellent characteristics, have a extensive future.
The present invention is acted on by introducing supermolecule polyrotaxane, ring molecule and silicon rubber, forms the network of sliding crosslinking
Structure, and the straight chain molecular shaft of polyrotaxane and polyolefin compatibility are fabulous can effectively enhance the compatible of silicon rubber and polyolefin
Property.Therefore, compared to traditional silicon rubber/polyolefin thermoplastic elastomer, sliding cross-linked network silicon rubber/polyene of the invention
Hydrocarbon thermoplastic elastomer (TPE) has high intensity, high tenacity, the high excellent characteristics such as compatible.
Specific embodiment
The contents of the present invention are described in further detail below by way of specific embodiment.Original used in embodiment
Material unless otherwise specified, can be obtained from routine business approach.Following embodiment is not to be construed as to the scope of the invention
Limitation.Those skilled in the art above content can carry out some nonessential adjustment according to the present invention.
Embodiment 1-6
The raw material composition of embodiment 1-6 is shown in Table 1, and the dosage of each component refers both to mass parts in table 1.
Raw material used in table 1 is described as follows: vinylsiloxane rubber vinyl molar content is 0.2%.Polyolefin is second
The composition that alkene-octene copolymer and high density polyethylene (HDPE) mass ratio are 1:1；The straight-chain molecule of polyrotaxane is polyisobutene,
Ring molecule is the gamma-cyclodextrin containing vinyl, and END CAPPED GROUP is adamantyl-like groups.Peroxide vulcanizing agent is 2,5- bis-
Methyl -2,5- bis(t-butylperoxy) hexane.Constitution controller is hydroxy silicon oil.
Preparation step: (1) vinylsiloxane rubber, gas-phase silica, constitution controller hydroxy silicon oil in table 1 formula is existed
It is blended uniformly in mixer, obtains melting silicone rubber.100 DEG C of smelting temperature, mixing time 1.5h, revolving speed 100rpm.(2) double
In screw extruder, melting silicone rubber, polyolefin, polyrotaxane, peroxide vulcanizing agent is added, carries out dynamic vulcanization reaction, squeezes
It is granulated out and obtains silicon rubber/polyolefin thermoplastic elastomer.180 DEG C of the plasticating temperature of double screw extruder, screw speed
300rpm, dynamic vulcanization reaction time 1min.
Comparative example 1
According to the technological parameter of embodiment 1-6, but it is added without polyrotaxane, prepares 1 sample of comparative example according to the formula in table 1
Product.
The properties of sample parameter of embodiment 1-6 and comparative example 1 is shown in Table 2.Tensile strength, elongation at break stretch permanent become
Shape is according to GB/T 528-2009 standard testing, and angle tear strength is according to GB/T529-2008 standard testing, and hardness is according to GB/
T23651-2009 standard testing.
By the performance parameter of embodiment 1-3 and comparative example 1 it is found that joined silicon rubber/polylefin thermoplatic of polyrotaxane
Elastomer tensile strength, tearing strength, elongation at break are all much higher than silicon rubber/polyolefine thermoplastic elastomer that polyrotaxane is not added
Body, and its tensile set and hardness are lower than silicon rubber/polyolefin thermoplastic elastomer that polyrotaxane is not added, and this shows to slide
Dynamic cross-linked network silicon rubber/polyolefin thermoplastic elastomer has high-intensitive and high tenacity significant advantage.Pair of embodiment 1-3
Than the result shows that, polyrotaxane additional amount is bigger, slide cross-linked network silicon rubber/polyolefin thermoplastic elastomer intensity and toughness
It is higher.This is because increasing with polyrotaxane, it is more intensive to be formed by sliding cross-linked network, and the increase-volume of polyrotaxane is made
With being more obvious, the two factors facilitate the raising of elastomer intensity, toughness and compatibility jointly.The performance of embodiment 2,4,5
Parameter show the relative scale of silicon rubber and polyolefin be 20:80~80:20 in the range of, sliding cross-linked network silicon rubber/
Polyolefin thermoplastic elastomer can keep high-intensitive and high tenacity.The comparing result of embodiment 2 and 6 shows to increase peroxidating
The intensity of the additional amount of object vulcanizing agent, elastomer improves, and change in toughness is little.
1 embodiment 1-6 of table and the raw material of comparative example 1 composition
| Title | Vinylsiloxane rubber | Polyolefin | Polyrotaxane | Peroxide vulcanizing agent | White carbon black | Constitution controller |
| Embodiment 1 | 50 | 50 | 5 | 1 | 20 | 3 |
| Embodiment 2 | 50 | 50 | 20 | 1 | 20 | 3 |
| Embodiment 3 | 50 | 50 | 50 | 1 | 20 | 3 |
| Embodiment 4 | 20 | 80 | 20 | 1 | 20 | 3 |
| Embodiment 5 | 80 | 20 | 20 | 1 | 20 | 3 |
| Embodiment 6 | 50 | 50 | 20 | 3 | 20 | 3 |
| Comparative example 1 | 50 | 50 | 0 | 1 | 20 | 3 |
The properties of sample parameter of table 2 embodiment 1-6 and comparative example 1
Embodiment 7
Material used, proportion and preparation step are same as Example 2, only polyolefin be linear low density polyethylene and
Polypropylene mass ratio is the composition of 1:1.
Embodiment 8
Material used, proportion and preparation step are same as Example 2, only polyolefin be ethylene-hexene co-polymers and
Polypropylene mass ratio is the composition of 2:1.
Embodiment 9
Material used, proportion and preparation step are same as Example 2, and only the straight-chain molecule of polyrotaxane is polybutadiene
Alkene, ring molecule are the alpha-cyclodextrin containing vinyl, and END CAPPED GROUP is trityl class group.
Embodiment 10
Material used, proportion and preparation step are same as Example 2, and only the contents of ethylene of vinylsiloxane rubber is
0.1%, peroxide vulcanizing agent is that peroxidating is bis- (2,4- dichloro-benzoyl), and preparation step (2) double screw extruder is plasticated
170 DEG C of temperature, screw speed 270rpm, dynamic vulcanization reaction time 1min.
The properties of sample parameter of embodiment 7-10 is shown in Table 3.The result shows that the group when polyolefin becomes linear low density polyethylene
Alkene and polypropylene (mass ratio 1:1) or ethylene-hexene co-polymers and polypropylene (mass ratio 2:1) slide cross-linked network silicon rubber
Glue/polyolefin thermoplastic elastomer all has high-intensitive, high tenacity and high-compatibility.The straight-chain molecular structure of change polyrotaxane,
Ring shaped molecule structure or sealing end based structures, influence the performance of elastomer little.Change contents of ethylene, the catalyst of silicon rubber
Type and Technology of Dynamic Vulcanized, will affect the mechanical property of elastomer, but be able to maintain high-intensitive, high tenacity and high compatible excellent
Different characteristic.
The properties of sample parameter of 3 embodiment 7-10 of table
Claims (10)
1. a kind of silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network, it is characterised in that: be by following quality
The raw material composition of part: 20~80 parts of vinylsiloxane rubber, 20~80 parts of polyolefin, 5~50 parts of polyrotaxane, vulcanizing agent 0.1~5
Part, 5~60 parts of filler, 1~8 part of constitution controller.
2. a kind of silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network according to claim 1, special
Sign is: the vinyl molar content of vinylsiloxane rubber is 0.08%~1%.
3. a kind of silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network according to claim 1, special
Sign is: the straight-chain molecule of polyrotaxane be polyethylene, polypropylene, polybutadiene, polyisobutene, in polyisoprene at least
One kind, the ring molecule of polyrotaxane are the cyclodextrin containing vinyl, and the end-capping group of polyrotaxane is cyclodextrin group, dinitro
At least one of base phenyl class group, adamantyl-like groups, polynuclear aromatic same clan group, trityl class group.
4. a kind of silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network according to claim 1, special
Sign is: polyolefin is polyethylene, polypropylene, ethylene-octene copolymer, ethylene-butene copolymer, ethylene-hexene co-polymers
At least one of.
5. a kind of silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network according to claim 1, special
Sign is: vulcanizing agent is peroxide vulcanizing agent.
6. a kind of silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network according to claim 1, special
Sign is: filler is at least one of white carbon black, talcum powder, mica powder, titanium dioxide, silica flour, calcium carbonate.
7. a kind of silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network according to claim 1, special
Sign is: constitution controller is at least one of hydroxy silicon oil, methyltriethoxysilane, hexamethyldisilazane.
8. a kind of any one of claim 1~7 silicon rubber/polyolefin thermoplastic elastomer with sliding cross-linked network
Preparation method, it is characterised in that: the following steps are included:
1) vinylsiloxane rubber, filler and constitution controller are kneaded, obtain melting silicone rubber；
2) melting silicone rubber, polyolefin, polyrotaxane and vulcanizing agent are added twin-screw extrude and carries out dynamic vulcanization reaction, squeezed
Out, it is granulated, obtains silicon rubber/polyolefin thermoplastic elastomer of sliding cross-linked network.
9. a kind of silicon rubber/polyolefin thermoplastic elastomer preparation with sliding cross-linked network according to claim 8
Method, it is characterised in that: in step 1), mixing carries out in mixer or kneader, and machined parameters are as follows: melting temperature 60
DEG C~140 DEG C, mixing time is 0.2h~2h, and revolving speed is 20r/min~120r/min.
10. a kind of silicon rubber/polyolefin thermoplastic elastomer preparation with sliding cross-linked network according to claim 8
Method, it is characterised in that: in step 2), the processing temperature of double screw extruder is 160 DEG C~220 DEG C, screw speed 150r/
Min~340r/min, the time of dynamic vulcanization are 0.5min~3min.
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| CN111777821A (en) * | 2020-05-13 | 2020-10-16 | 宁波拓烯新材料科技有限公司 | Poly 4-methyl-1-pentene/silicone rubber thermoplastic elastomer and preparation and application thereof |
| CN112409700A (en) * | 2020-11-19 | 2021-02-26 | 江苏金发科技新材料有限公司 | High-performance polypropylene composite material for vehicles and preparation method thereof |
| CN115319942A (en) * | 2022-08-16 | 2022-11-11 | 东莞市朗晟材料科技有限公司 | A banburying device for processing of silicon rubber polyolefin thermoplastic elastomer |
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Application publication date: 20190524 |