CN111718587A - Low-compression permanent deformation thermoplastic elastomer material and preparation method thereof - Google Patents
Low-compression permanent deformation thermoplastic elastomer material and preparation method thereof Download PDFInfo
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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
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
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- 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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- 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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- C08L2207/04—Thermoplastic elastomer
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Abstract
The invention relates to a low compression permanent deformation thermoplastic elastomer material which is prepared from the following raw materials in percentage by weight: 5-20% of SEBS; 20-50% of EPDM; 10-30% of white oil; 5-10% of maleic anhydride grafted SEBS; 5-10% of mineral filler; vulcanizing agent: 1 to 5 percent; auxiliary vulcanizing agent: 0.5-2%; activating agent: 0.5-2%; 0.1 to 0.5 percent of antioxidant; 0.1 to 0.5 percent of lubricant. The invention also provides a preparation method of the thermoplastic elastomer, which comprises the steps of firstly mixing the components uniformly in a high-speed stirrer according to the weight percentage, and carrying out melt extrusion granulation through a double-screw extruder to obtain the thermoplastic elastomer material. The Shore hardness of the thermoplastic elastomer material prepared by the invention is 40-90A, and the thermoplastic elastomer material has excellent compression set, higher tensile strength and elongation at break.
Description
Technical Field
The invention belongs to the field of chemical engineering, and relates to a modified high polymer material; in particular to a thermoplastic elastomer material with low compression set and a preparation method thereof.
Background
Thermoplastic elastomers, also known as thermoplastic rubbers, are a new polymer material that has been developed rapidly in recent years, and the growth rate is much higher than other general rubber varieties. The thermoplastic elastomer has the characteristics of rubber and the properties of thermoplastic plastics. The rubber is soft at room temperature, is similar to rubber, has toughness and elasticity, is fluid at high temperature, can be plasticized and molded by using traditional thermoplastic processing equipment such as an injection molding machine, an extruder, a calender and the like, and is a so-called third-generation rubber following natural rubber and synthetic rubber, namely TPE and TPR for short. The plastic segments in the molecular structure of the thermoplastic elastomer form physical crosslinking points by virtue of acting force among the chain segments, and the physical crosslinking is reversible along with the change of temperature, so that the plastic processing characteristics of the thermoplastic elastomer are shown; the rubber segment in the molecular structure is a high elastic segment, and the elasticity of the thermoplastic elastomer is determined by the rubber segment. The thermoplastic elastomer has the dual performance of rubber and plastic, so that the thermoplastic elastomer can be widely applied to various fields of toys for babies and children, automobile parts, daily necessities, sports equipment, tool handle rubber coating and the like.
Hydrogenated polystyrene-butadiene-styrene block copolymer (SEBS) is the largest class of thermoplastic elastomer, and has become a novel material with great development prospect, which can widely replace traditional rubber and partial plastic, and the output and consumption are the first of TPE. With the development of new technology, the continuous optimization and promotion of SEBS performance are promoted, the application field is continuously expanded, and the SEBS has a very wide application prospect in the fields of electronic communication, medical treatment and health, ground paving materials and the like besides the aspects of building industry, shoe making industry, polymer modification, adhesives and the like which enter at present. However, since SEBS is always a thermoplastic elastomer, there are certain differences in compression set, high temperature resistance, and chemical resistance compared to conventional thermosetting rubbers. Therefore, it is one of the hot spots in the research of SEBS to improve the compression set property of SEBS.
Disclosure of Invention
The invention aims to solve the technical problems of low compression set thermoplastic elastomer material for improving SEBS base material and a preparation method thereof, and the low compression set thermoplastic elastomer material and the preparation method thereof aim to solve the technical problems of poor compression set, high temperature resistance and chemical resistance of SEBS in the prior art.
The low compression permanent deformation thermoplastic elastomer material is prepared from the following raw materials in percentage by weight:
hydrogenated polystyrene-butadiene-styrene block copolymer (SEBS): 5 to 20 percent;
ethylene Propylene Diene Monomer (EPDM): 20 to 50 percent;
white oil: 10 to 30 percent;
polypropylene: 5 to 25 percent;
maleic anhydride graft hydrogenated polystyrene-butadiene-styrene block copolymer: 5 to 10 percent;
mineral filler: 5 to 20 percent;
vulcanizing agent: 1 to 5 percent
Auxiliary vulcanizing agent: 0.5 to 2 percent
Activating agent: 0.5 to 2 percent
Antioxidant: 0.1 to 0.5 percent;
lubricant: 0.1 to 0.5 percent.
Further, the hydrogenated polystyrene-butadiene-styrene block copolymer has a brookfield viscosity of greater than 50000 in a 25% by mass toluene solution at 25 ℃, wherein the styrene to butadiene monomer ratio is 33: 67.
further, it is characterized in that the ethylene-propylene-diene monomer (EPDM) is a granular rubber obtained by copolymerizing ethylene, propylene and a non-conjugated diene, the Mooney viscosity (ML1+4) at 125 ℃ is 50-120, and the non-conjugated diene is ethylidene-norbornene.
Further, the white oil is environment-friendly food-grade white oil, the flash point is more than 230 ℃, and the kinematic viscosity is more than 36mm at the temperature of 40 DEG C2/s。
Further, the polypropylene is homopolymerized polypropylene, and the melt index at 230 ℃ and 2.16KG is 2-15g/10 min.
Further, in the polystyrene-butadiene-styrene block copolymer grafted and hydrogenated by maleic anhydride, the grafting ratio of maleic anhydride is 1.5-2.0%, and the monomer ratio of styrene to butadiene is 30: 70.
further, the mineral filler is any one or a mixture of more than two of calcium carbonate, barium sulfate, talcum powder, mica powder, kaolin and argil.
Further, the vulcanizing agent is one of a peroxide crosslinking agent and a phenolic crosslinking agent
Further, the co-curing agent is one of triallyl isocyanurate, diallyl phthalate and tin chloride.
Further, the activating agent is zinc oxide.
Furthermore, the antioxidant is a mixture of hindered phenol main antioxidant and phosphite ester auxiliary antioxidant.
Further, the lubricant is any one or a mixture of more than two of stearic acid, zinc stearate, calcium stearate, oleamide, erucamide or polyethylene wax.
The invention also provides a method for preparing the low compression set thermoplastic elastomer material, which comprises the following steps:
1) weighing the raw materials according to the weight percentage;
2) a material mixing step: adding the hydrogenated polystyrene-butadiene-styrene block copolymer, ethylene propylene diene monomer and white oil into a high-speed mixing stirrer, and stirring at high speed to ensure that the white oil is uniformly absorbed into the hydrogenated polystyrene-butadiene-styrene block copolymer and the ethylene propylene diene monomer; then sequentially adding the maleic anhydride grafted hydrogenated polystyrene-butadiene-styrene block copolymer, the mineral filler, the vulcanizing agent, the co-vulcanizing agent, the antioxidant and the lubricant, and stirring at a high speed until the material components are uniformly mixed;
3) a granulation step: melting, extruding and granulating the mixed material obtained in the step 2) by using a double-screw extrusion device, wherein the length-diameter ratio of a screw of the used double-screw extruder is required to be more than 56; the melt extrusion temperature is 200-230 ℃, and the main machine rotating speed of the double-screw extruder is 300 r/min, so that the thermoplastic elastomer material with low compression permanent deformation can be obtained.
Compared with the prior art, the invention has the advantages of positive and obvious technical effect. In the invention, the dispersed and fine EPDM is subjected to crosslinking vulcanization reaction in the melt blending process, and the crosslinked and vulcanized EPDM has excellent compression set and high temperature resistance, thereby improving the performance of the SEBS thermoplastic elastomer. The thermoplastic elastomer material has Shore hardness of 40-90A, excellent compression set, high tensile strength and elongation at break, elongation at break of more than 300 percent and heat deformation temperature of more than 90 ℃. Greatly expands the application field of the thermoplastic elastomer material.
Detailed Description
The invention is further illustrated by the following specific examples. It should be noted that the following examples are only illustrative of the present invention and are not intended to limit the scope of the present invention, and that various insubstantial modifications and adaptations of the present invention as described above may be made by those skilled in the art without departing from the scope of the present invention.
Component formulations of the examples
Note that the components in the examples are described below:
SEBS 1: model G1651, Corteng, USA, styrene to rubber monomer ratio 33/67, hardness 61A.
SEBS 2: model 7551, Taiwan Liangrong chemical industry Co., Ltd., styrene to rubber monomer ratio 33/67.
EPDM 1: model number Vistalon 5601, exxonmobil chemical, mooney viscosity (ML1+4, 125 ℃)72MU, ethylene content 69%, ethylidene-norbornene content 5.0%.
EPDM 2: model number Vistalon 8700, exxonmobil chemical, mooney viscosity (ML1+4, 125 ℃)78MU, ethylene content 78%, ethylidene-norbornene content 8.0%.
White oil: model Primol 382 mineral oil, Exxon Mobil USA, kinematic viscosity at 40 ℃ of 68mm2S, flash point 240 ℃.
PP 1: the melt index at 230 ℃ and 2.16KG was 7g/10min for model H350F, PP, SK in Korea.
PP 2: model 1040, Polypropylene PP, Taiwan plastics industries Ltd., melt index at 230 ℃ under 2.16KG of 5g/10 min.
Maleic anhydride grafted SEBS: FG1901X, kraton, usa, styrene to rubber monomer ratio 30/70, 71A.
Mineral filler 1: model FCC302, calcium carbonate, taiwan plastics industries ltd.
Mineral filler 2: type 800B, talc, New chemical Co., Taiwan bamboo, average particle size 8 micron, whiteness 90%.
Vulcanizing agent: model SP-1045, octylphenol-formaldehyde resin, san Lesco specialty Chemicals Shanghai, Inc.
Auxiliary vulcanizing agent: stannous chloride, welfare technologies ltd.
Activating agent: zinc oxide, Jiangsu Tianli Zinc industries, Inc.
Antioxidant 1: irganox1010, hindered phenolic primary antioxidant, Pasteur, Germany.
And (2) antioxidant: irganox168, a phosphite-based auxiliary antioxidant, Pasteur, Germany.
Lubricant 1: model VRX, oleamide, british procumbent.
And lubricant 2: model ER, erucamide, British Poa Inc.
The performance data for the examples are as follows:
| name of raw materials | Example 1 | Example 2 | Example 3 | Example 4 |
| Hardness (Shao's A) | 40 | 55 | 70 | 85 |
| Tensile Strength (MPa) | 4.0 | 6.0 | 7.5 | 11.2 |
| Elongation at Break (%) | 450 | 430 | 420 | 440 |
| Tensile Strength at definite elongation (MPa) of 100% | 1.6 | 2.0 | 3.0 | 5.1 |
| Tensile Strength at definite elongation (MPa) of 300% | 3.0 | 3.6 | 4.5 | 6.5 |
| Compression set (23 ℃, 22h) | 12％ | 20％ | 28％ | 33％ |
Note, description of test performance data:
hardness: the test standard is ASTM D2240, measured using a shore durometer, in shore a.
Tensile strength, elongation at break, tensile strength at break of 100% and 300%: the test standard is ASTM D412 and the tensile test rate of the bars is 500 mm/min.
Compression set: the test standard was ASTM D395B, the test conditions were a temperature of 23 ℃ and a compression time of 22 hours.
By adjusting the proportion of the components in the formula, the thermoplastic elastomers with different hardness can be prepared, the hardness of the thermoplastic elastomers in examples 1 to 4 is 40A, 55A, 70A and 85A respectively, and the hardness of the thermoplastic elastomers in examples 40A to 85A is the hardness of the common thermoplastic elastomers. The thermoplastic elastomer with hydrogenated polystyrene-butadiene-styrene block copolymer as base material has great difference between compression set and thermosetting rubber, for example, the compression set of 40A SEBS base material elastomer is about 20% at 23 deg.C for 22 h; while the compression set of 85A is as high as about 40%. As is apparent from the compression set data of the examples, the compression set of the material prepared by the invention is about 8% lower than that of the elastomer of the common SEBS substrate, and the material shows good compression set. The excellent compression set mechanism was analyzed: in the melt blending of the double-screw extruder, the ethylene propylene diene monomer generates a crosslinking chemical reaction under the action of a vulcanizing agent, an auxiliary vulcanizing agent and an activating agent. The crosslinked ethylene propylene diene monomer rubber has excellent rebound resilience, so that the composite material is endowed with excellent compression set.
Claims (13)
1. The thermoplastic elastomer material with low compression set is characterized by being prepared from the following raw materials in percentage by weight:
hydrogenated polystyrene-butadiene-styrene block copolymer: 5 to 20 percent;
ethylene propylene diene monomer: 20 to 50 percent;
white oil: 10 to 30 percent;
polypropylene: 5 to 25 percent;
maleic anhydride graft hydrogenated polystyrene-butadiene-styrene block copolymer: 5 to 10 percent;
mineral filler: 5 to 20 percent;
vulcanizing agent: 1 to 5 percent
Auxiliary vulcanizing agent: 0.5 to 2 percent
Activating agent: 0.5 to 2 percent
Antioxidant: 0.1 to 0.5 percent;
lubricant: 0.1 to 0.5 percent.
2. A thermoplastic elastomeric material with low compression set according to claim 1, characterized in that said hydrogenated polystyrene-butadiene-styrene block copolymer has a brookfield viscosity of more than 50000 in a 25% by mass solution in toluene at 25 ℃, wherein the styrene to butadiene monomer ratio is 33: 67.
3. a thermoplastic elastomer material with low compression set according to claim 1, characterised in that said ethylene-propylene-diene rubber is a rubber in the form of granules obtained by copolymerisation of ethylene, propylene and a non-conjugated diene, said non-conjugated diene being ethylidene-norbornene, and having a mooney viscosity (ML1+4) at 125 ℃ of 50 to 120.
4. A thermoplastic elastomer material with low compression set according to claim 1 characterised in that the white oil is an environmentally friendly food grade white oil having a flash point of greater than 230 ℃ and a kinematic viscosity at 40 ℃ of greater than 36mm2/s。
5. A thermoplastic elastomer material with low compression set as claimed in claim 1, wherein the polypropylene is homopolypropylene and has a melt index of 2-15g/10min at 230 ℃ and a weight of 2.16 KG.
6. The thermoplastic elastomer material with low compression set as claimed in claim 1, wherein in the maleic anhydride graft-hydrogenated polystyrene-butadiene-styrene block copolymer, the graft ratio of maleic anhydride is 1.5 to 2.0%, and the monomer ratio of styrene to butadiene is 30: 70.
7. a thermoplastic elastomer material with low compression set as claimed in claim 1, wherein the mineral filler is one or a mixture of two or more of calcium carbonate, barium sulfate, talc, mica powder, kaolin and pottery clay.
8. A thermoplastic elastomeric material having a low compression set as claimed in claim 1, wherein said vulcanizing agent is one of a peroxide crosslinking agent and a phenolic crosslinking agent.
9. A thermoplastic elastomer material with low compression set as claimed in claim 1, wherein said co-curing agent is one of triallyl isocyanurate, diallyl phthalate and tin chloride.
10. A low compression set thermoplastic elastomer material as claimed in claim 1 wherein said activator is zinc oxide.
11. The thermoplastic elastomer material with low compression set as claimed in claim 1, wherein the antioxidant is a mixture of hindered phenol type primary antioxidant and phosphite type secondary antioxidant.
12. A thermoplastic elastomer material with low compression set as claimed in claim 1, wherein said lubricant is one or a mixture of two or more of stearic acid, zinc stearate, calcium stearate, oleamide, erucamide or polyethylene wax.
13. A process for preparing a thermoplastic elastomeric material with low compression set according to claim 1, characterized in that: the method comprises the following steps:
1) weighing the raw materials according to the weight percentage;
2) a material mixing step: adding the hydrogenated polystyrene-butadiene-styrene block copolymer, ethylene propylene diene monomer and white oil into a high-speed mixing stirrer, and stirring at high speed to ensure that the white oil is uniformly absorbed into the hydrogenated polystyrene-butadiene-styrene block copolymer and the ethylene propylene diene monomer; then sequentially adding the maleic anhydride grafted hydrogenated polystyrene-butadiene-styrene block copolymer, the mineral filler, the vulcanizing agent, the co-vulcanizing agent, the antioxidant and the lubricant, and stirring at a high speed until the material components are uniformly mixed;
3) a granulation step: melting, extruding and granulating the mixed material obtained in the step 2) by using a double-screw extrusion device, wherein the length-diameter ratio of a screw of the used double-screw extruder is required to be more than 56; the melt extrusion temperature is 200-230 ℃, and the main machine rotating speed of the double-screw extruder is 300 r/min, so that the thermoplastic elastomer material with low compression permanent deformation can be obtained.
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Cited By (3)
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| CN114940830A (en) * | 2022-01-04 | 2022-08-26 | 浙江金仪盛世生物工程有限公司 | Thermoplastic elastomer material and thermoplastic elastomer pipeline |
| CN115246979A (en) * | 2022-01-18 | 2022-10-28 | 道一高分子聚合物(宁波)有限公司 | High polymer material easy to bond and preparation method and application thereof |
| CN117050458A (en) * | 2023-08-29 | 2023-11-14 | 苏州创扬新材料科技股份有限公司 | Thermoplastic elastomer with low permanent compression set and preparation method thereof |
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| CN114940830A (en) * | 2022-01-04 | 2022-08-26 | 浙江金仪盛世生物工程有限公司 | Thermoplastic elastomer material and thermoplastic elastomer pipeline |
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| CN115246979B (en) * | 2022-01-18 | 2024-02-09 | 道一高分子聚合物(宁波)有限公司 | Polymer material easy to bond and preparation method and application thereof |
| CN117050458A (en) * | 2023-08-29 | 2023-11-14 | 苏州创扬新材料科技股份有限公司 | Thermoplastic elastomer with low permanent compression set and preparation method thereof |
| CN117050458B (en) * | 2023-08-29 | 2024-01-30 | 苏州创扬新材料科技股份有限公司 | Thermoplastic elastomer with low permanent compression set and preparation method thereof |
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Application publication date: 20200929 |