CN105273317A - High-density TPV material and preparation method thereof - Google Patents
High-density TPV material and preparation method thereof Download PDFInfo
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- CN105273317A CN105273317A CN201510752742.4A CN201510752742A CN105273317A CN 105273317 A CN105273317 A CN 105273317A CN 201510752742 A CN201510752742 A CN 201510752742A CN 105273317 A CN105273317 A CN 105273317A
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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, 10-15 parts of calcium carbonate, 15-20 parts of high-density packing, 3-5 parts of a coupling agent, 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 vulcanizing agent. According to the high-density TPV material and the preparation method thereof, the higher mechanical property is achieved while the density of the high-density TPV material is larger than 1.2 g/cm<3>.
Description
Technical field
The present invention relates to TPV material technical field, particularly a kind of high-density 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, its density is be less than 1g/cm3 substantially, but at some special occasions, very high to the density requirements of TPV material, and while requiring it to have certain density, also require that it has excellent mechanical property, therefore need in traditional technology to adopt other high density materials to replace TPV material, thus guarantee density, mechanical property meet the demands.
But, TPV material as elastomerics, the elastomeric 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, exploitation one has higher density, has the TPV material with excellent mechanical performances to become required simultaneously.
Summary of the invention
The present invention proposes a kind of high-density TPV material and preparation method thereof, the density of described high-density TPV material is greater than 1.2g/cm
3while also possess higher mechanical property.
A kind of high-density TPV material, its raw material comprises by weight:
In a specific embodiment, 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 5.5,5.9,6.3,7.1,7.7,8.6,9; The weight part of softening agent can be 21,23,25,27,32,34,36,38; The weight part of calcium carbonate can be 10.5,11.6,12.1,12.7,13.2,13.8,14.5; The weight part of high-density packing can be 15.5,16.6,17.2,17.9,18.4,19.1,19.8; The weight part of coupling agent can be 3.5,3.6,4.1,4.2,4.6,4.9; 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 vulcanizing agent can be 1.2,1.5,1.7,1.9,2.1,2.3,2.5,2.8.
Preferably, EPDM is polymerized by ethene, propylene and non-conjugated diene the terpolymer obtained under catalysts conditions, non-conjugated diene is ethylidene norbornene or dicyclopentadiene, and the mol ratio of ethene, propylene and non-conjugated diene is 60-80:15-30:3-10.
Preferably, described SEBS is one or both the mixture in maleic anhydride-g-SBS, acrylic ester grafted SEBS.
Preferably, described polypropylene is one or both the mixture in homopolymerization type polypropylene, copolymerized type propene polymer; Preferably, described polyacrylic weight-average molecular weight is 20000-900000, number-average molecular weight is 10000-500000, molecular weight distribution width is 2.5-4.
Preferably, described high-density packing is one or more the mixture in zinc oxide, barium sulfate, lead powder; Preferably, the density of described zinc oxide is 5.5-5.7g/cm
3, particle diameter is 325-1500 order; The density of described barium sulfate is 4.3-4.5g/cm
3, particle diameter is 325-1500 order; The density of described lead powder is 7.0-7.3g/cm
3, particle diameter is 325-1500 order.
Preferably, described calcium carbonate to be particle diameter the be water-ground limestone of 0.1-10 μm.
Preferably, described coupling agent is one or more the mixture in silane coupling agent, titanate coupling agent, aluminate coupling agent, aluminium titanium coupling agent, preferably, described coupling agent is silane coupling agent, described silane coupling agent is one or both the mixture in γ-methacryloxypropyl trimethoxy silane, γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane.
Preferably, described vulcanizing agent is made up of vulcanizing agent and vulcanization aid; Vulcanizing agent is resol or superoxide; When adopting resol as vulcanizing agent, vulcanization aid is metal halide; When employing superoxide is as vulcanizing agent, cyanate, divinylbenzene class or esters of acrylic acid are vulcanization aid.
Preferably, described oxidation inhibitor is one or more the mixture in phenolic antioxidant, phosphite ester kind antioxidant, sulfur-bearing class antioxidant;
Preferably, described photostabilizer is one or both the mixture in hindered amine light stabilizer, benzotriazole light stabilizer;
Preferably, described internal lubricant is one or more the mixture in silicone powder, silicone master batch, silicone oil, vinyl bis-stearamides, hydroxy fatty acid series lubricant agent.
A kind of preparation method of described high-density TPV material, comprise: EPDM, polypropylene, softening agent, calcium carbonate, high-density packing, coupling agent, 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, vulcanizing 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 terpolymer EP rubber, the ethene of specific proportioning, propylene and ethylidene norbornene or dicyclopentadiene polymerization is selected to obtain ter-polymers, make its tensile strength, elasticity and crosslinking polymerization degree all be in a rational state, effectively improve resistance to permanent deformation, such and the machine-shaping property of TPV material; Add the high-density packing of zinc oxide, barium sulfate, lead powder etc. and the filler of calcium carbonate, while the density of TPV material is greatly improved, again by the coupling agent of silane, titanic acid ester etc., improve the consistency of the EPDM of filler and ad hoc structure, reduce filler to greatest extent to the impact of the mechanical property of elastomer material; In addition, namely polypropylene itself has good solvent resistance, thermotolerance and processing fluidity, time composite with graft type SEBS again, can strongthener toughness effectively, lower the boundary defect that mineral filler brings, be conducive to obtaining homogeneous system, make the TPV material finally obtained obtain good rigid-tough balance, then obtain good mechanical property; In addition the softening agent of the certain content of use, oxidation inhibitor and photostabilizer and internal lubricant is also coordinated in the present invention, improve the intermingling material such as traditional EPDM, polypropylene work-ing life and processing stability energy, the TPV material prepared described in making has good processing characteristics and mechanical property.
Meanwhile, the present invention, in preparation TPV material process, adopts dynamic vulcanization technology, with resol or organo-peroxide for vulcanizing agent, metal halide, cyanate etc., as vulcanization aid, control 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 over cure because of TPV material well.
In the present invention, the high-density TPV material made according to above-mentioned formula and preparation method, can meet high-density and the mechanical property of TPV material material, 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-density TPV material, its raw material comprises by weight:
Wherein, described EPDM is polymerized by ethene, propylene and ethylidene norbornene the terpolymer obtained under catalysts conditions, and the mol ratio of ethene, propylene and ethylidene norbornene is 60:30:3; Described SEBS is maleic anhydride-g-SBS; Described polypropylene is homopolymerization type polypropylene, and described polyacrylic weight-average molecular weight be 20000, number-average molecular weight is 500000, molecular weight distribution width is 2.5; Described high-density packing is zinc oxide, and the density of described zinc oxide is 5.5g/cm
3, particle diameter is 1500 orders; Described calcium carbonate to be particle diameter the be water-ground limestone of 0.1 μm; Described coupling agent is silane coupling agent, and described silane coupling agent is γ-methacryloxypropyl trimethoxy silane; Described vulcanizing agent is made up of resol and metal halide; Described oxidation inhibitor is phenolic antioxidant; Described photostabilizer is hindered amine light stabilizer; Described internal lubricant is silicone powder.
Embodiment 2
A kind of high-density TPV material, its raw material comprises by weight:
Wherein, described EPDM is polymerized by ethene, propylene and dicyclopentadiene the terpolymer obtained under catalysts conditions, and the mol ratio of ethene, propylene and dicyclopentadiene is 80:15:10; Described SEBS is acrylic ester grafted SEBS; Described polypropylene is copolymerized type propene polymer, and described polyacrylic weight-average molecular weight be 900000, number-average molecular weight is 10000, molecular weight distribution width is 4; Described high-density packing is barium sulfate, and the density of described barium sulfate is 4.3g/cm
3, particle diameter is 1500 orders; Described calcium carbonate to be particle diameter the be water-ground limestone of 10 μm; Described coupling agent is silane coupling agent, and described silane coupling agent is γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane; Described vulcanizing agent is made up of superoxide and divinylbenzene class; Described oxidation inhibitor is phosphite ester kind antioxidant; Described photostabilizer is benzotriazole light stabilizer; Described internal lubricant is silicone master batch.
Embodiment 3
A kind of high-density TPV material, its raw material comprises by weight:
Wherein, described EPDM is polymerized by ethene, propylene and ethylidene norbornene the terpolymer obtained under catalysts conditions, and the mol ratio of ethene, propylene and ethylidene norbornene is 70:22:6; Described SEBS is the mixture of maleic anhydride-g-SBS, acrylic ester grafted SEBS; Described polypropylene is homopolymerization type polypropylene, and described polyacrylic weight-average molecular weight be 400000, number-average molecular weight is 300000, molecular weight distribution width is 3; Described high-density packing is lead powder, and the density of described lead powder is 7.0g/cm
3, particle diameter is 1500 orders; Described calcium carbonate to be particle diameter the be water-ground limestone of 5 μm; Described coupling agent is titanate coupling agent; Described vulcanizing agent is made up of superoxide and cyanate; Described oxidation inhibitor is sulfur-bearing class antioxidant; Described photostabilizer is the mixture of hindered amine light stabilizer, benzotriazole light stabilizer; Described internal lubricant is silicone oil.
Embodiment 4
A kind of high-density TPV material, its raw material comprises by weight:
Wherein, described EPDM is polymerized by ethene, propylene and dicyclopentadiene the terpolymer obtained under catalysts conditions, and the mol ratio of ethene, propylene and dicyclopentadiene is 75:20:7; Described SEBS is maleic anhydride-g-SBS; Described polypropylene is the mixture of homopolymerization type polypropylene, copolymerized type propene polymer; Described high-density packing is the mixture of zinc oxide, barium sulfate, lead powder, and the density of described zinc oxide is 5.7g/cm
3, particle diameter is 325 orders; The density of described barium sulfate is 4.5g/cm
3, particle diameter is 325 orders; The density of described lead powder is 7.3g/cm
3, particle diameter is 325 orders; Described calcium carbonate to be particle diameter the be water-ground limestone of 3-5 μm; Described coupling agent is the mixture of aluminate coupling agent, aluminium titanium coupling agent; Described vulcanizing agent is made up of superoxide and esters of acrylic acid; Described oxidation inhibitor is the mixture of phenolic antioxidant, sulfur-bearing class antioxidant; Described photostabilizer is the mixture of hindered amine light stabilizer, benzotriazole light stabilizer; Described internal lubricant is the mixture of vinyl bis-stearamides, hydroxy fatty acid series lubricant agent.
Described in above-described embodiment 1-4, the preparation method of high-density TPV material comprises: EPDM, polypropylene, softening agent, calcium carbonate, high-density packing, coupling agent, 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, vulcanizing 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 | 67 | 63 |
| Notched Izod impact strength (KJ/m 2) | 24.5 | 26.3 | 25.4 | 24.6 |
| Tensile strength (MPa) | 5.5 | 6.6 | 5.8 | 6.9 |
| Elongation at break (%) | 400 | 450 | 430 | 480 |
| Density (g/m 3) | 1.25 | 1.28 | 1.23 | 1.26 |
In the present invention, adopt a certain proportion of terpolymer EP rubber, the ethene of specific proportioning, propylene and ethylidene norbornene or dicyclopentadiene polymerization is selected to obtain ter-polymers, make its tensile strength, elasticity and crosslinking polymerization degree all be in a rational state, effectively improve resistance to permanent deformation, such and the machine-shaping property of TPV material; Add the high-density packing of zinc oxide, barium sulfate, lead powder etc. and the filler of calcium carbonate, while the density of TPV material is greatly improved, again by the coupling agent of silane, titanic acid ester etc., improve the consistency of the EPDM of filler and ad hoc structure, reduce filler to greatest extent to the impact of the mechanical property of elastomer material; In addition, namely polypropylene itself has good solvent resistance, thermotolerance and processing fluidity, time composite with graft type SEBS again, can strongthener toughness effectively, lower the boundary defect that mineral filler brings, be conducive to obtaining homogeneous system, make the TPV material finally obtained obtain good rigid-tough balance, then obtain good mechanical property; In addition the softening agent of the certain content of use, oxidation inhibitor and photostabilizer and internal lubricant is also coordinated in the present invention, improve the intermingling material such as traditional EPDM, polypropylene work-ing life and processing stability energy, the TPV material prepared described in making has good processing characteristics and mechanical property.
Meanwhile, the present invention, in preparation TPV material process, adopts dynamic vulcanization technology, with resol or organo-peroxide for vulcanizing agent, metal halide, cyanate etc., as vulcanization aid, control 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 over cure because of TPV material well.
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-density TPV material, is characterized in that, its raw material comprises by weight:
2. high-density TPV material according to claim 1, it is characterized in that, described EPDM is polymerized by ethene, propylene and non-conjugated diene the terpolymer obtained under catalysts conditions, non-conjugated diene is ethylidene norbornene or dicyclopentadiene, and the mol ratio of ethene, propylene and non-conjugated diene is 60-80:15-30:3-10.
3. high-density TPV material according to claim 1 and 2, is characterized in that, described SEBS is one or both the mixture in maleic anhydride-g-SBS, acrylic ester grafted SEBS.
4. the high-density TPV material according to any one of claim 1-3, is characterized in that, described polypropylene is one or both the mixture in homopolymerization type polypropylene, copolymerized type propene polymer; Preferably, described polyacrylic weight-average molecular weight is 20000-900000, number-average molecular weight is 10000-500000, molecular weight distribution width is 2.5-4.
5. the high-density TPV material according to any one of claim 1-4, is characterized in that, described high-density packing is one or more the mixture in zinc oxide, barium sulfate, lead powder; Preferably, the density of described zinc oxide is 5.5-5.7g/cm
3, particle diameter is 325-1500 order; The density of described barium sulfate is 4.3-4.5g/cm
3, particle diameter is 325-1500 order; The density of described lead powder is 7.0-7.3g/cm
3, particle diameter is 325-1500 order.
6. the high-density TPV material according to any one of claim 1-5, is characterized in that, described calcium carbonate to be particle diameter the be water-ground limestone of 0.1-10 μm.
7. the high-density TPV material according to any one of claim 1-6, it is characterized in that, described coupling agent is one or more the mixture in silane coupling agent, titanate coupling agent, aluminate coupling agent, aluminium titanium coupling agent, preferably, described coupling agent is silane coupling agent, described silane coupling agent is one or both the mixture in γ-methacryloxypropyl trimethoxy silane, γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane.
8. the high-density TPV material according to any one of claim 1-7, is characterized in that, described vulcanizing agent is made up of vulcanizing agent and vulcanization aid; Vulcanizing agent is resol or superoxide; When adopting resol as vulcanizing agent, vulcanization aid is metal halide; When employing superoxide is as vulcanizing agent, cyanate, divinylbenzene class or esters of acrylic acid are vulcanization aid.
9. the high-density TPV material according to any one of claim 1-8, is characterized in that, described oxidation inhibitor is one or more the mixture in phenolic antioxidant, phosphite ester kind antioxidant, sulfur-bearing class antioxidant;
Preferably, described photostabilizer is one or both the mixture in hindered amine light stabilizer, benzotriazole light stabilizer;
Preferably, described internal lubricant is one or more the mixture in silicone powder, silicone master batch, silicone oil, vinyl bis-stearamides, hydroxy fatty acid series lubricant agent.
10. the preparation method of the high-density TPV material according to any one of claim 1-9, it is characterized in that, comprise: EPDM, polypropylene, softening agent, calcium carbonate, high-density packing, coupling agent, 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, vulcanizing 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.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109535560A (en) * | 2018-11-29 | 2019-03-29 | 袁进 | A kind of TPV material and preparation method thereof haveing excellent performance |
| CN109627768A (en) * | 2018-11-30 | 2019-04-16 | 广东省石油与精细化工研究院 | A kind of thermoplastic dynamic vulcanized silicon rubber of high-flexibility and preparation method thereof |
| CN110698771A (en) * | 2019-09-27 | 2020-01-17 | 张家港市美特高分子材料有限公司 | TPV micro-foaming material and production process thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109535560A (en) * | 2018-11-29 | 2019-03-29 | 袁进 | A kind of TPV material and preparation method thereof haveing excellent performance |
| CN109627768A (en) * | 2018-11-30 | 2019-04-16 | 广东省石油与精细化工研究院 | A kind of thermoplastic dynamic vulcanized silicon rubber of high-flexibility and preparation method thereof |
| CN110698771A (en) * | 2019-09-27 | 2020-01-17 | 张家港市美特高分子材料有限公司 | TPV micro-foaming material and production process thereof |
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Application publication date: 20160127 |