CN105273351A - High-density TPV material and preparation method thereof - Google Patents
High-density TPV material and preparation method thereof Download PDFInfo
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- CN105273351A CN105273351A CN201510752665.2A CN201510752665A CN105273351A CN 105273351 A CN105273351 A CN 105273351A CN 201510752665 A CN201510752665 A CN 201510752665A CN 105273351 A CN105273351 A CN 105273351A
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Abstract
The invention discloses a high-density TPV material and a preparation method thereof. The high-density TPV material is prepared from, by weight, 30-60 parts of EPDM, 20-40 parts of polypropylene, 5-10 parts of SEBS, 20-40 parts of a plasticizer, 1-3 parts of an antioxidant, 1-3 parts of a light stabilizer, 1-3 parts of an internal lubricant and 1-3 parts of a cross-linking agent. The TPV material has the advantages of being high in tensile strength and good in elastic deformability.
Description
Technical field
The present invention relates to TPV material technical field, particularly a kind of high strength TPV material and preparation method thereof.
Background technology
TPV is the abbreviation of ThermoplasticVulcanizate, Chinese is thermoplasticity Ethylene Propylene Terpolymer dynamic vulcanization elastomerics or thermoplasticity Ethylene Propylene Terpolymer dynamic perduren, is the macromolecular elastomer material of terpolymer EP rubber EPDM microparticulate composition in continuous polypropylene PP phase of solid cure.Physicals under TPV normal temperature and function class are similar to thermoset rubber, at high temperature show as the characteristic of thermoplastics, can fast, economical and machine-shaping easily.Vulcanized rubber material is made terpolymer EP rubber EPDM with the microparticulate lower than 2 micron-scales in polypropylene PP plastic substrate by dynamic vulcanization by TPV thermoplasticity Ethylene Propylene Terpolymer dynamic vulcanization elastomerics, the characteristic of rubber and plastics is well combined, obtains the high performance elastomer material of excellent combination property.
Traditional TPV material, due to its base mateiral characteristic, it is relative to the vulcanized rubber of same hardness, its strength property is relatively low, for the product application that some is special, under the condition meeting hardness, often insufficient strength, therefore need in traditional technology to adopt other high-strength materials to replace TPV material, thus proof strength performance meets the demands.
But, TPV material as elastomerics, the elastomerics desirable physical mechanical property that itself is intrinsic, and the advantage of recyclable recycling makes it in processing, manufacturing has irreplaceable effect.Be directed to this, develop a kind of meet changing firmness requirements condition under there is higher-strength performance TPV material become required.
Summary of the invention
The present invention proposes a kind of high strength TPV material and preparation method thereof.Described TPV material has the advantage that tensile strength is high, elastic deformability is good.
A kind of high strength TPV material, its raw material comprises by weight:
The weight part of EPDM can be 31,33,35,37,42,46,48,52,56,57,59; Polyacrylic weight part can be 21,23,25,27,32,34,36,38; The weight part of SEBS can be 5.9,6.3,6.8,7.1,8.7,9.3,9.8; The elastomeric weight part of POE can be 3.5,4.2,5.9,6.3,6.8,7.1,7.8; The weight part of softening agent can be 21,23,25,27,32,34,36,38; The weight part of oxidation inhibitor can be 1.2,1.5,1.7,1.9,2.1,2.3,2.5,2.8; The weight part of photostabilizer can be 1.2,1.5,1.7,1.9,2.1,2.3,2.5,2.8; The weight part of internal lubricant can be 1.2,1.5,1.7,1.9,2.1,2.3,2.5,2.8; The weight part of linking agent can be 1.2,1.5,1.7,1.9,2.1,2.3,2.5,2.8.
Preferably, described EPDM is modified epdm, prepares described modified epdm and comprises: added by maleic anhydride in EPDM and carry out graft reaction, obtain EPDM-g-MAH; Add in phenol by PA6, triethylamine again, heating makes dissolution of solid complete, adds the xylene solution being dissolved with described EPDM-g-MAH inwards, insulation reaction; Poured in dimethyl formamide by gained reaction mass after cooling and staticly settle, filter and be precipitated thing, described throw out obtains described modified epdm after drying.
Preferably, prepare described modified epdm and comprise: maleic anhydride is added in EPDM and carry out graft reaction, obtain the EPDM-g-MAH that percentage of grafting is 1-3%; Again by PA6, be that the triethylamine of the 0.3-0.5wt% of benchmark adds in phenol with PA6, be heated to 140-160 DEG C and make dissolution of solid complete, add the xylene solution being dissolved with described EPDM-g-MAH inwards, insulation reaction 9-12h; Poured in dimethyl formamide by gained reaction mass after being cooled to normal temperature and staticly settle 1-2h, filter and be precipitated thing, the vacuum-drying at 85-90 DEG C of described throw out, to constant weight, namely obtains described modified epdm; Wherein the weight ratio of EPDM and PA6 is 5-8:1.
Preferably, prepare described modified epdm and comprise: maleic anhydride is added in EPDM and carry out graft reaction, obtain the EPDM-g-MAH that percentage of grafting is 1-3%; Again by PA6, be that the triethylamine of the 0.3-0.5wt% of benchmark adds in phenol with PA6, be heated to 140-160 DEG C and make dissolution of solid complete, add the xylene solution being dissolved with described EPDM-g-MAH inwards, insulation reaction 9-12h; Poured in dimethyl formamide by gained reaction mass after being cooled to normal temperature and staticly settle 1-2h, filter and be precipitated thing, the vacuum-drying at 85-90 DEG C of described throw out, to constant weight, namely obtains described modified epdm; Wherein the weight ratio of EPDM and PA6 is 5-8:1.
Preferably, the graft reaction of described EPDM-g-MAH comprises: join in Banbury mixer after EPDM, radical initiator and additive being pre-mixed, after EPDM plastifies completely, add with EPDM the MAH of the 6-8wt% being benchmark at twice, banburying 10-15min at 160-180 DEG C, obtains described EPDM-g-MAH through washing, filtration.
Preferably, the MAH-g-PP of 5-10 weight part is also comprised in described TPV material.
Preferably, described softening agent is paraffin oil, and the paraffinic base content of paraffin oil is 65-70%, and aromaticity content is 3-8%, and naphthenic hydrocarbon is 25-30%; Kinematic viscosity at 100 DEG C is 5-20mm
2/ s, is preferably 10-20mm
2/ s.
Preferably, described oxidation inhibitor is Hinered phenols antioxidant or phosphorous acid kind antioxidant;
Preferably, described photostabilizer is one or more in hindered amine light stabilizer, triazines as light stabilizer, organic nickel complex compound;
Preferably, described internal lubricant is one or more in silicone powder, silicone master batch, silicone oil, vinyl bis-stearamides, hydroxy fatty acid series lubricant agent.
Preferably, described linking agent is that the resol of 3-5:1 and metal halide form by quality proportioning.
A kind of preparation method of described high strength TPV material, comprise: EPDM, polypropylene, softening agent, calcium carbonate, oxidation inhibitor, photostabilizer, internal lubricant to be added in kneader after mixing, carry out first time in feeding twin screw extruder to plasticate, after pelletizing, obtain work in-process particle; After described work in-process particle is mixed with SEBS, linking agent, carry out second time in feeding twin screw extruder and plasticate, after pelletizing, obtain described high workability TPV material.
Preferably, the processing temperature that first time plasticates in process is 160-190 DEG C, and screw speed is 200-400r/min; The processing temperature that second time is plasticated in process is 160-190 DEG C, and screw speed is 200-400r/min.
In the present invention, adopt a certain proportion of EPDM, by the modified epdm be obtained by reacting will be carried out after nonpolar EPDM employing maleic anhydride graft with nylon 6, while overcoming the shortcoming of EPDM as apolar substance and strong polarity nylon 6 mixing poor compatibility, due to the high-intensity performance of nylon 6, give the mechanical property that EPDM is excellent, substantially improve the strength property of SEBS, therefore replace general EPDM by the modified epdm of high strength, the TPV material of high strength can be obtained on the TPV material basis of same rigidity.In addition also limit the polypropylene and the SEBS that add specified quantitative in the present invention, the two itself has good solvent resistance, thermotolerance and high-intensity performance, greatly can improve blended processing characteristics and the high-intensity performance of TPV material itself; On the softening agent basis adding certain content, adding of oxidation inhibitor and photostabilizer and internal lubricant, the TPV material prepared is made to have longer work-ing life and processing stability energy.
Meanwhile, the present invention is in preparation TPV material process, and adopt dynamic vulcanization technology, take resol as vulcanizing agent, metal halide, as additional crosslinker, controls the crosslinking degree of vulcanizing material and even performance effectively; And use secondary to plasticate complete processing, make Blending Processes more abundant, in blend, rubber phase particle diameter is less, be more evenly distributed, entanglement effect between molecular chain is less, solution twines relatively easily, when adding vulcanizing agent in processing of once plasticating after being limited to, can reduce the mobility variation effect caused because of TPV material over cure well.
In the present invention, the high strength TPV material made according to above-mentioned formula and preparation method, can meet the performance requirement of TPV material high strength, simultaneously long service life, and production efficiency is high, and cost is low.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in detail.
Embodiment 1
A kind of high strength TPV material, its raw material comprises by weight:
Wherein, described EPDM is modified epdm, prepares described modified epdm and comprises: added by maleic anhydride in EPDM and carry out graft reaction, obtains the EPDM-g-MAH that percentage of grafting is 1%; Again by PA6, be that the triethylamine of the 0.5wt% of benchmark adds in phenol with PA6, be heated to 140 DEG C and make dissolution of solid complete, add the xylene solution being dissolved with described EPDM-g-MAH inwards, insulation reaction 12h; Poured in dimethyl formamide by gained reaction mass after being cooled to normal temperature and staticly settle 1h, filter and be precipitated thing, the vacuum-drying at 90 DEG C of described throw out, to constant weight, namely obtains described modified epdm; Wherein the weight ratio of EPDM and PA6 is 5:1; The graft reaction of described EPDM-g-MAH comprises: join in Banbury mixer after EPDM, radical initiator and additive being pre-mixed, after EPDM plastifies completely, add with EPDM the MAH of the 8wt% being benchmark at twice, banburying 15min at 160 DEG C, obtains described EPDM-g-MAH through washing, filtration;
Described softening agent is paraffin oil, and the paraffinic base content of paraffin oil is 65%, and aromaticity content is 8%, and naphthenic hydrocarbon is 27%; Kinematic viscosity at 100 DEG C is 5mm
2/ s; Described oxidation inhibitor is Hinered phenols antioxidant; Described photostabilizer is hindered amine light stabilizer; Described internal lubricant is silicone powder; Described linking agent is that the resol of 3:1 and metal halide form by quality proportioning.
Embodiment 2
A kind of high strength TPV material, its raw material comprises by weight:
Wherein, described EPDM is modified epdm, prepares described modified epdm and comprises: added by maleic anhydride in EPDM and carry out graft reaction, obtains the EPDM-g-MAH that percentage of grafting is 3%; Again by PA6, be that the triethylamine of the 0.3wt% of benchmark adds in phenol with PA6, be heated to 160 DEG C and make dissolution of solid complete, add the xylene solution being dissolved with described EPDM-g-MAH inwards, insulation reaction 9h; Poured in dimethyl formamide by gained reaction mass after being cooled to normal temperature and staticly settle 2h, filter and be precipitated thing, the vacuum-drying at 85 DEG C of described throw out, to constant weight, namely obtains described modified epdm; Wherein the weight ratio of EPDM and PA6 is 8:1; The graft reaction of described EPDM-g-MAH comprises: join in Banbury mixer after EPDM, radical initiator and additive being pre-mixed, after EPDM plastifies completely, add with EPDM the MAH of the 6wt% being benchmark at twice, banburying 10min at 180 DEG C, obtains described EPDM-g-MAH through washing, filtration;
Described softening agent is paraffin oil, and the paraffinic base content of paraffin oil is 70%, and aromaticity content is 3%, and naphthenic hydrocarbon is 27%; Kinematic viscosity at 100 DEG C is 20mm
2/ s; Described oxidation inhibitor is phosphorous acid kind antioxidant; Described photostabilizer is triazines as light stabilizer; Described internal lubricant is silicone master batch; Described linking agent is that the resol of 5:1 and metal halide form by quality proportioning.
Embodiment 3
A kind of high strength TPV material, its raw material comprises by weight:
Wherein, described EPDM is modified epdm, prepares described modified epdm and comprises: added by maleic anhydride in EPDM and carry out graft reaction, obtains the EPDM-g-MAH that percentage of grafting is 2%; Again by PA6, be that the triethylamine of the 0.4wt% of benchmark adds in phenol with PA6, be heated to 150 DEG C and make dissolution of solid complete, add the xylene solution being dissolved with described EPDM-g-MAH inwards, insulation reaction 10h; Poured in dimethyl formamide by gained reaction mass after being cooled to normal temperature and staticly settle 1.5h, filter and be precipitated thing, the vacuum-drying at 87 DEG C of described throw out, to constant weight, namely obtains described modified epdm; Wherein the weight ratio of EPDM and PA6 is 6:1; The graft reaction of described EPDM-g-MAH comprises: join in Banbury mixer after EPDM, radical initiator and additive being pre-mixed, after EPDM plastifies completely, add with EPDM the MAH of the 7wt% being benchmark at twice, banburying 12min at 170 DEG C, obtains described EPDM-g-MAH through washing, filtration;
Described softening agent is paraffin oil, and the paraffinic base content of paraffin oil is 66%, and aromaticity content is 5%, and naphthenic hydrocarbon is 29%; Kinematic viscosity at 100 DEG C is 10mm
2/ s; Described oxidation inhibitor is Hinered phenols antioxidant; Described photostabilizer is organic nickel complex compound; Described internal lubricant is silicone oil; Described linking agent is that the resol of 4:1 and metal halide form by quality proportioning.
Embodiment 4
A kind of high strength TPV material, its raw material comprises by weight:
Wherein, described EPDM is modified epdm, prepares described modified epdm and comprises: added by maleic anhydride in EPDM and carry out graft reaction, obtains the EPDM-g-MAH that percentage of grafting is 2.5%; Again by PA6, be that the triethylamine of the 0.35wt% of benchmark adds in phenol with PA6, be heated to 145 DEG C and make dissolution of solid complete, add the xylene solution being dissolved with described EPDM-g-MAH inwards, insulation reaction 11h; Poured in dimethyl formamide by gained reaction mass after being cooled to normal temperature and staticly settle 1.8h, filter and be precipitated thing, the vacuum-drying at 88 DEG C of described throw out, to constant weight, namely obtains described modified epdm; Wherein the weight ratio of EPDM and PA6 is 7:1; The graft reaction of described EPDM-g-MAH comprises: join in Banbury mixer after EPDM, radical initiator and additive being pre-mixed, after EPDM plastifies completely, add with EPDM the MAH of the 7wt% being benchmark at twice, banburying 13min at 165 DEG C, obtains described EPDM-g-MAH through washing, filtration;
Described softening agent is paraffin oil, and the paraffinic base content of paraffin oil is 66%, and aromaticity content is 4%, and naphthenic hydrocarbon is 30%; Kinematic viscosity at 100 DEG C is 20mm
2/ s; Described oxidation inhibitor is phosphorous acid kind antioxidant; Described photostabilizer is the mixture of hindered amine light stabilizer, triazines as light stabilizer, organic nickel complex compound; Described internal lubricant is the mixture of vinyl bis-stearamides, hydroxy fatty acid series lubricant agent; Described linking agent is that the resol of 4:1 and metal halide form by quality proportioning.
Described in above-described embodiment 1-4, the preparation method of high strength TPV material comprises: EPDM, polypropylene, softening agent, calcium carbonate, oxidation inhibitor, photostabilizer, internal lubricant to be added in kneader after mixing, carry out first time in feeding twin screw extruder to plasticate, after pelletizing, obtain work in-process particle; After described work in-process particle is mixed with SEBS, linking agent, carry out second time in feeding twin screw extruder and plasticate, after pelletizing, obtain described high workability TPV material; The processing temperature of wherein plasticating in process is for the first time 160-190 DEG C, and screw speed is 200-400r/min; The processing temperature that second time is plasticated in process is 160-190 DEG C, and screw speed is 200-400r/min.
High-density TPV material described in above-described embodiment 1-4 is carried out performance test, and result is as shown in the table:
| Performance | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Compression set (25 DEG C, %) | 20.1 | 19.6 | 18.9 | 19.4 |
| Shore hardness (A) | 65 | 70 | 68 | 73 |
| Notched Izod impact strength (KJ/m 2) | 24.5 | 26.3 | 25.4 | 24.6 |
| Tensile strength (MPa) | 10.5 | 9.6 | 10.8 | 8.9 |
| Elongation at break (%) | 600 | 550 | 530 | 630 |
In the present invention, adopt a certain proportion of EPDM, by the modified epdm be obtained by reacting will be carried out after nonpolar EPDM employing maleic anhydride graft with nylon 6, while overcoming the shortcoming of EPDM as apolar substance and strong polarity nylon 6 mixing poor compatibility, due to the high-intensity performance of nylon 6, give the mechanical property that EPDM is excellent, substantially improve the strength property of SEBS, therefore replace general EPDM by the modified epdm of high strength, the TPV material of high strength can be obtained on the TPV material basis of same rigidity.In addition also limit the polypropylene and the SEBS that add specified quantitative in the present invention, the two itself has good solvent resistance, thermotolerance and high-intensity performance, greatly can improve blended processing characteristics and the high-intensity performance of TPV material itself; On the softening agent basis adding certain content, adding of oxidation inhibitor and photostabilizer and internal lubricant, the TPV material prepared is made to have longer work-ing life and processing stability energy.
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (10)
1. a high strength TPV material, is characterized in that, its raw material comprises by weight:
2. high strength TPV material according to claim 1, is characterized in that, described EPDM is modified epdm, prepares described modified epdm and comprises: added by maleic anhydride in EPDM and carry out graft reaction, obtain EPDM-g-MAH; Add in phenol by PA6, triethylamine again, heating makes dissolution of solid complete, adds the xylene solution being dissolved with described EPDM-g-MAH inwards, insulation reaction; Poured in dimethyl formamide by gained reaction mass after cooling and staticly settle, filter and be precipitated thing, described throw out obtains described modified epdm after drying.
3. high strength TPV material according to claim 2, is characterized in that, prepares described modified epdm and comprises: added by maleic anhydride in EPDM and carry out graft reaction, obtains the EPDM-g-MAH that percentage of grafting is 1-3%; Again by PA6, be that the triethylamine of the 0.3-0.5wt% of benchmark adds in phenol with PA6, be heated to 140-160 DEG C and make dissolution of solid complete, add the xylene solution being dissolved with described EPDM-g-MAH inwards, insulation reaction 9-12h; Poured in dimethyl formamide by gained reaction mass after being cooled to normal temperature and staticly settle 1-2h, filter and be precipitated thing, the vacuum-drying at 85-90 DEG C of described throw out, to constant weight, namely obtains described modified epdm; Wherein the weight ratio of EPDM and PA6 is 5-8:1.
4. high strength TPV material according to claim 3, it is characterized in that, the graft reaction of described EPDM-g-MAH comprises: join in Banbury mixer after EPDM, radical initiator and additive being pre-mixed, after EPDM plastifies completely, add with EPDM the MAH of the 6-8wt% being benchmark at twice, banburying 10-15min at 160-180 DEG C, obtains described EPDM-g-MAH through washing, filtration.
5. the high strength TPV material according to any one of claim 1-4, is characterized in that, also comprises the MAH-g-PP of 5-10 weight part in described TPV material.
6. high strength TPV material according to any one of claim 1-5, is characterized in that, described softening agent is paraffin oil, and the paraffinic base content of paraffin oil is 65-70%, and aromaticity content is 3-8%, and naphthenic hydrocarbon is 25-30%; Kinematic viscosity at 100 DEG C is 5-20mm
2/ s, is preferably 10-20mm
2/ s.
7. the high strength TPV material according to any one of claim 1-6, is characterized in that, described oxidation inhibitor is Hinered phenols antioxidant or phosphorous acid kind antioxidant;
Preferably, described photostabilizer is one or more in hindered amine light stabilizer, triazines as light stabilizer, organic nickel complex compound;
Preferably, described internal lubricant is one or more in silicone powder, silicone master batch, silicone oil, vinyl bis-stearamides, hydroxy fatty acid series lubricant agent.
8. the high strength TPV material according to any one of claim 1-7, is characterized in that, described linking agent is that the resol of 3-5:1 and metal halide form by quality proportioning.
9. the preparation method of the high strength TPV material according to any one of claim 1-8, it is characterized in that, comprise: EPDM, polypropylene, softening agent, calcium carbonate, oxidation inhibitor, photostabilizer, internal lubricant to be added in kneader after mixing, carry out first time in feeding twin screw extruder to plasticate, after pelletizing, obtain work in-process particle; After described work in-process particle is mixed with SEBS, linking agent, carry out second time in feeding twin screw extruder and plasticate, after pelletizing, obtain described high workability TPV material.
10. the preparation method of high strength TPV material according to claim 9, is characterized in that, the processing temperature that first time plasticates in process is 160-190 DEG C, and screw speed is 200-400r/min; The processing temperature that second time is plasticated in process is 160-190 DEG C, and screw speed is 200-400r/min.
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| CN109337217A (en) * | 2018-09-29 | 2019-02-15 | 扬州亚光电缆有限公司 | A kind of the composite material preparation and its utilization in high flexibility flexible cable product high based on TPV base-material protective |
| CN109627590A (en) * | 2018-12-24 | 2019-04-16 | 宁波汉吉高分子材料有限公司 | A kind of weather strip for automobile wear-resisting TPV material and preparation method thereof |
| CN109796685A (en) * | 2018-12-06 | 2019-05-24 | 宁波泰甬汽车零部件有限公司 | A kind of improvement thermoplastic elastomer (TPE) TPV material and extruding process thereof |
| CN112126160A (en) * | 2020-09-22 | 2020-12-25 | 江苏金陵奥普特高分子材料有限公司 | TPV (thermoplastic vulcanizate) elastomer for improving normal-temperature compression set and preparation method thereof |
| CN116656138A (en) * | 2023-05-16 | 2023-08-29 | 石家庄德祥塑胶制品有限公司 | Crosslinked thermoplastic elastomer and preparation method and application thereof |
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Application publication date: 20160127 |