WO2009140825A1 - Composition élastomère thermoplastique, procédé afférent et produit obtenu par ledit procédé - Google Patents

Composition élastomère thermoplastique, procédé afférent et produit obtenu par ledit procédé Download PDF

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Publication number
WO2009140825A1
WO2009140825A1 PCT/CN2008/071062 CN2008071062W WO2009140825A1 WO 2009140825 A1 WO2009140825 A1 WO 2009140825A1 CN 2008071062 W CN2008071062 W CN 2008071062W WO 2009140825 A1 WO2009140825 A1 WO 2009140825A1
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WO
WIPO (PCT)
Prior art keywords
thermoplastic elastomer
rubber
elastomer composition
agent
mixing
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PCT/CN2008/071062
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English (en)
Chinese (zh)
Inventor
黄丽慧
杨荣嵢
Original Assignee
杨浩宇
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Priority to PCT/CN2008/071062 priority Critical patent/WO2009140825A1/fr
Publication of WO2009140825A1 publication Critical patent/WO2009140825A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
    • C08K5/0025—Crosslinking or vulcanising agents; including accelerators
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L21/00—Compositions of unspecified rubbers

Definitions

  • the present invention relates to a thermoplastic elastomer composition comprising syndiotactic 1,2-polybutadiene, to a method of preparing the thermoplastic elastomer composition, and an article produced by the preparation method and the thermoplastic elastomer composition the use of.
  • thermoplastic elastomer is a material that combines the dual properties of rubber and thermoplastics. Its functional and physical properties are similar to those of conventional thermoset rubber, but can be processed as fast, efficiently and economically as thermoplastics. Due to the greatly simplified processing, thermoplastic elastomers are becoming more widely used.
  • Syndiotactic 1,2-polybutadiene (RB) is a typical thermoplastic elastomer which is mainly obtained by 1,2-polymerization of butadiene.
  • the syndiotactic 1,2-polybutadiene can crystallize and its crystallinity increases as the degree of regularity increases.
  • the degree of regularity reaches 99%, the tensile strength of the syndiotactic 1,2-polybutadiene can reach 30 ⁇ 50MPa, which is basically equivalent to crystalline polypropylene, and the melting point is as high as 150, which leads to easy thermal degradation during processing. Therefore, the syndiotactic 1,2-polybutadiene having too high crystallinity is relatively difficult to apply.
  • JSR Japan Synthetic Rubber Co., Ltd.
  • JSR developed a practically practical syndiotactic 1,2-polybutadiene in 1974, which utilizes a small amount of random polymeric chains between regular molecular chains to control crystallinity, successfully The crystallinity is controlled below 35%, and the melting point is controlled below 90 °C, thereby reducing the possibility of thermal degradation of the syndiotactic 1,2-polybutadiene during processing.
  • Syndiotactic 1,2-polybutadiene has many unique advantages.
  • syndiotactic 1,2-polybutadiene in the manufacture of soles has received attention. It is reported that almost 80% of the Italian soles currently use syndiotactic 1,2-polybutadiene, the main The advantage is that blending a small amount of syndiotactic 1,2-polybutadiene can result in a sole with a shiny or matt finish without the need for a spray coating process, while also having a rubber sole-like texture.
  • the syndiotactic 1,2-polybutadiene is easily thermally degraded and the dimensional stability of the foamed article is poor, the syndiotactic 1,2-polybutadiene is currently only used as an additive or an auxiliary material to improve the main gum.
  • the performance of the material is only 5 to 30% by weight of the total amount of the compound.
  • thermoplastic elastomer composition in which the amount of syndiotactic 1,2-polybutadiene exceeds 50% by weight of the total size.
  • a thermoplastic elastomer composition having high slip resistance, good texture, good elasticity, small amount of compression deformation, good abrasion resistance, no special odor, environmental protection, and the like is obtained.
  • thermoplastic elastomer composition comprising a) 50 to 90 parts by weight of syndiotactic 1,2-polybutadiene, b) 10 to 50 parts by weight of an unsaturated rubber, c a crosslinking agent and optionally d) an auxiliary wherein the total amount of components a) and b) is 100 parts by weight, and wherein said components a), b), c) and optionally d)
  • the vulcanization is blended to form a crosslink between the components a) and b).
  • Component a) in the thermoplastic elastomer composition is preferably 50 to 80 parts by weight of syndiotactic 1,2-polybutadiene, more preferably 50 to 70 parts by weight of syndiotactic 1,2-polybutylene.
  • the component b) in the thermoplastic elastomer composition is preferably 20 to 50 parts by weight of an unsaturated rubber, more preferably 30 to 50 parts by weight of an unsaturated rubber, wherein the total of the components a) and b) The amount is 100 parts by weight.
  • the syndiotactic 1,2-polybutadiene has a crystallinity of less than 35%, preferably less than 30%, more preferably less than 25%.
  • the unsaturated rubber may be any rubber or elastomer material having an unsaturated bond, such as polybutadiene rubber, natural rubber, isoprene rubber, styrene butadiene rubber, hydrogenated styrene butadiene rubber, butadiene-styrene-butyl A diene copolymer (SBS), a nitrile rubber, a chloroprene rubber, or the like, or a mixture thereof.
  • SBS butadiene-styrene-butyl A diene copolymer
  • the crosslinking agent may be any suitable crosslinking agent such as peroxide, sulfur, metal oxide, phenolic resin, anthraquinone, maleimide or the like or a mixture thereof, preferably using peroxidation. As a crosslinking agent.
  • the crosslinking agent is used in an amount of 0.1 to 3.5 parts by weight, preferably 0.15 to 3.0 parts by weight, more preferably 0.20 to 2.5 parts by weight, most preferably 0.20 to 2.0 parts by weight, based on 100 parts by weight of the total of components a) and b) Part.
  • the thermoplastic elastomer composition further comprises an adjuvant.
  • the auxiliaries are various types of auxiliaries commonly used in rubber compounding systems, such as vulcanization accelerators, plasticizers, fillers, antioxidants, foaming agents, flame retardants, colorants, reinforcing agents, and the like, or mixtures thereof.
  • the crosslinking agent may be any suitable crosslinking agent, such as a peroxide crosslinking agent, sulfur, metal oxide, phenolic resin, anthraquinone derivative, maleimide, or the like, or a mixture thereof, preferably used.
  • the oxide acts as a crosslinking agent.
  • any suitable vulcanization accelerator may also be used, such as a thiazole accelerator, a thiuram accelerator, a sulfenamide accelerator, a quinone accelerator, a dithiocarbamate.
  • Promoters, thiourea accelerators and aldehyde amine accelerators specifically, for example, DM, NOBS. CZ, NS, TMTD, PZ, EZ, DPG, DOTG, NA-22, TMTU, accelerator H and the like.
  • any suitable filler may be used in the present invention, including but not limited to: carbon black, white carbon black, calcium carbonate, magnesium carbonate, dolomite powder, barium sulfate, lithopone, gypsum powder, aluminum silicate, titanium dioxide, clay, mica. Powder, wollastonite powder, talc powder, diatomaceous earth powder, attapulgite, sepiolite powder, zeolite powder, vermiculite powder, light carbonic acid, rayon, etc.
  • the foaming agent which can be used in the present invention mainly includes, but is not limited to, an organic foaming agent such as an azo compound, a sulfonyl hydrazide compound, a nitroso compound or a mixture thereof, preferably, for example, azobisnonanoate, azobisindole Diisopropyl acid, hydrazine, ⁇ '-dinitroso pentadecyltetramine, hydrazine, ⁇ '-dinitroso-p-phthalamide, p-phenylene sulfonyl hydrazide, phenylsulfonyl hydrazide, etc. .
  • an organic foaming agent such as an azo compound, a sulfonyl hydrazide compound, a nitroso compound or a mixture thereof, preferably, for example, azobisnonanoate, azobisindole Diisopropyl acid, hydra
  • the thermoplastic elastomer composition may further comprise an elastomer other than the unsaturated rubber, such as silicone rubber, fluororubber, polyurethane, ethylene-vinyl acetate copolymer, acrylic rubber, chlorine.
  • the ether rubber or the like or a mixture thereof is preferably a silicone rubber, a fluororubber, and an ethylene-vinyl acetate copolymer.
  • the other elastomer is used in an amount of from 0.5 to 10% by weight, preferably from 1 to 5% by weight, more preferably from 1.5 to 3.5% by weight, based on 100 parts by total of the components a) and b).
  • thermoplastic elastomer composition comprising the step of dynamically vulcanizing and kneading the components a), b), c) and optionally d).
  • the dynamic vulcanization process comprises a one-stage dynamic vulcanization process; in another embodiment of the invention, the dynamic vulcanization process comprises a two-stage dynamic vulcanization process.
  • the dynamic vulcanization is a dynamic vulcanization process comprising: adding an auxiliary agent other than a crosslinking agent, a vulcanization accelerator, and a foaming agent, and the component
  • the compound consisting of a) and b) is put into the mixer, and the mixing time is about 5 to 15 minutes, during which the mixing temperature is not more than about 150 ° C; then the crosslinking agent, vulcanization accelerator and optional hair are added.
  • the foaming agent is then mixed for about 1 to 10 minutes and discharged, and the discharge temperature does not exceed about 120 °C.
  • the dynamic vulcanization compounding is a two-stage dynamic vulcanization mixing process, comprising: adding an auxiliary agent other than a crosslinking agent, a vulcanization accelerator, and a foaming agent, and the group
  • the rubber consisting of a) and b) is put into the mixer, and the first discharge is carried out after about 5 to 15 minutes of mixing, while the mixing temperature is kept below about 110 °C; the first mixed material obtained will be obtained.
  • the temperature of the second discharge does not exceed about 120 °C.
  • thermoplastic elastomer molding compound is obtained by further subjecting the rubber compound discharged from the dynamic vulcanization mixing process to an granulation process through an extrusion process and a granulation process and sufficiently stirring again.
  • the molding compound is molded by an injection molding process, wherein the process conditions of the injection molding process are as follows:
  • Injection port temperature 80 - 95 ° C
  • Mold temperature 165 ° C ⁇ 175 ° C.
  • the molding compound is molded by an extrusion molding process.
  • thermoplastic elastomer composition comprises hair
  • the method further comprises, during the injection molding process or the extrusion molding process, foaming the thermoplastic elastomer molding compound in a mold, for example, at about
  • an article prepared by using the thermoplastic elastomer composition according to the present invention may be an integrally formed, molded or otherwise formed article, including article of footwear such as a sole, a film article, a foamed article, a medical article, a sports device, and the like.
  • thermoplastic elastomer composition for the manufacture of an article of footwear such as a shoe sole, a film article, a foamed article, a medical article, a sports article or the like.
  • the invention also has the following advantages: 1.
  • the thermoplastic elastomer composition of the invention has loose processing conditions, and the formula adjustment range is expanded, thereby facilitating the expansion of the application range; 2. advantageously overcoming the syndiotactic 1,2-polybutyl The dimensional instability of the olefinic material after foaming is obtained, and a dimensionally stable foamed product is obtained; 3.
  • the syndiotactic 1,2-polybutadiene can be used for food packaging and manufacturing medical equipment (US FDA certification), so the human body Excellent acceptability, better odor than EVA or rubber products, and easy to be favored by consumers; 4.
  • the thermoplastic elastomer composition according to the present invention does not generate hydrogen chloride when incinerated. Harmful gases such as nitrogen compounds do not leave harmful heavy metals in the incineration residue, so they are relatively environmentally friendly when used.
  • thermoplastic elastomer composition according to Embodiment 1 of the present invention is as shown in Table 1 below: Table 1: No. Raw material name Use Formulation ratio (parts by weight)
  • the processing aid metal wax (PP1602) can improve the dispersibility of the material during kneading and the fluidity during molding.
  • the formulation of this embodiment is characterized by: 1) It can effectively improve the tensile strength of the material, and is suitable for products with high tensile and tear requirements, such as sports or medical protection products; 2) appropriately reducing the elasticity of the material, with a certain reduction
  • the shock effect is suitable for the manufacture of shock absorbing products; and 3) has good wear and slip resistance.
  • thermoplastic elastomer composition according to Embodiment 2 of the present invention is as shown in Table 2 below: Table 2: No. Raw material name Use Formulation ratio (parts by weight)
  • the formulation of this embodiment is characterized by: 1) having good tensile strength and high fluidity, suitable for products with complicated mold structure; and 2) rubbery soft hand feeling elastic, good slip resistance, Can be used in injection molding pads, sandals, slippers and other products.
  • thermoplastic elastomer composition according to Embodiment 3 of the present invention is shown in Table 3 below: Table 3: No. Original Material Name Use Formulation Ratio (parts by weight)
  • the formulation of this embodiment is characterized by: excellent wear resistance, close to the wear of general vulcanized rubber; lighter weight, suitable for the manufacture of outsole and midsole for footwear.
  • the mixing is carried out using an internal mixer, a two-stage dynamic vulcanization mixing process is employed, and the kneaded material can be formed into a molding compound by extrusion granulation, and then optionally foamed.
  • Table 4 The details are shown in Table 4 below.
  • the mixing is carried out using an internal mixer, a dynamic vulcanization mixing process is employed, and the kneaded material can be formed into a molding compound by extrusion granulation, and then optionally foamed, as shown in Table 5 below.
  • the mixing is carried out using an internal mixer, a two-stage dynamic vulcanization mixing process is employed, and the kneaded material can be formed into a molding compound by extrusion granulation, and then optionally foamed, as shown in Table 6 below.
  • the kneading rubber obtained in Embodiments 1 to 3 can be melt-extruded and matched by an extruder.
  • the granulator granulates the kneaded rubber, pours it into a mixing tank and stirs it, and thoroughly mixes it to obtain a thermoplastic elastomer molding compound according to the present invention.
  • Injection port temperature 80 - 95 ° C
  • thermoplastic elastomer compositions of Examples 1 to 3 were obtained, respectively. Tests are performed to obtain their respective physical properties.
  • thermoplastic elastomer compositions of Examples 1 to 3 are shown in Table 8 below:
  • thermoplastic elastomer composition according to the present invention As can be seen from the above Table 8, as the composition of the composition is adjusted, the physical properties of the thermoplastic elastomer composition according to the present invention after dynamic vulcanization can be varied within a wide range, and thus can be applied to various applications. However, while the physical properties are largely changed, the elongation at break of the thermoplastic elastomer composition according to the present invention does not change much, that is, it suppresses the retention of excellent elasticity.
  • thermoplastic elastomer composition of the present invention are very close to those of conventional vulcanized rubber, but are far easier to process than conventional vulcanized rubber.
  • physical properties, particularly the strength properties, of the thermoplastic elastomer composition of the present invention are far superior to those of conventional thermoplastic elastomers such as ethylene-vinyl acetate copolymer (EVA).
  • EVA ethylene-vinyl acetate copolymer
  • Table 9 below lists the general properties of the foamed articles obtained by the above foaming process and the foamed articles of ethylene-vinyl acetate copolymer (EVA) and natural rubber foamed articles of the thermoplastic elastomer compositions of Examples 1 to 3. Comparison: Table 9:
  • the foamed article according to the present invention is superior to conventional EVA, natural rubber foamed articles and the like in terms of performance, manufacturing process and environmental protection.
  • the processing conditions of the present invention are loose, and the formulation adjustment range is obviously expanded, which is advantageous for expanding the application range, and the product of the invention has high slip resistance, good texture, good elasticity, small compressive deformation, and abrasion resistance. Good, no special smell, environmental protection and so on.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

La présente invention concerne une composition élastomère thermoplastique, son procédé et le produit obtenu par ledit procédé. Ladite composition inclut (a) 50 à 90 parties en poids d’un 1,2-polybutadiène syndiotactique, (b) 10 à 50 parties en poids d’un caoutchouc insaturé, (c) un agent de réticulation, et éventuellement (d) des auxiliaires. Dans ladite composition, la quantité totale des composants (a) et (b) est égale à 100 parties en poids. Les composants (a), (b), (c) et éventuellement (d) sont mélangés et vulcanisés pour former la réticulation entre les composants (a) et (b).
PCT/CN2008/071062 2008-05-23 2008-05-23 Composition élastomère thermoplastique, procédé afférent et produit obtenu par ledit procédé WO2009140825A1 (fr)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111320833A (zh) * 2018-12-13 2020-06-23 泉州嘉泰鞋业有限公司 一种新型高分子复合发泡材料注射耐磨止滑中底及其制造方法
CN111332605A (zh) * 2020-03-20 2020-06-26 上海宝钢阿赛洛激光拼焊有限公司 用于铝合金板运输的损伤防护装置及方法
CN112679902A (zh) * 2020-12-07 2021-04-20 天津天星科生皮革制品有限公司 一种耐磨鞋底制备工艺
CN112852028A (zh) * 2021-01-15 2021-05-28 河北皋端建材科技有限公司 一种运动地板用热塑性弹性体组合物及其制备方法
CN112961510A (zh) * 2021-02-07 2021-06-15 远东电缆有限公司 风电用66kV高强度高耐热HEPR绝缘料及制备方法
CN114085433A (zh) * 2021-12-29 2022-02-25 江苏铁科新材料股份有限公司 一种适用于注射成型的高硬度橡胶材料及其制备工艺
CN115073875A (zh) * 2022-07-01 2022-09-20 南通普力马弹性体技术有限公司 一种湿式止滑热塑性弹性体及其制备方法
CN115109327A (zh) * 2022-08-22 2022-09-27 广东粤港澳大湾区黄埔材料研究院 一种轮胎胎侧橡胶组合物及其制备方法
CN115403839B (zh) * 2021-05-26 2024-06-04 中国石油化工股份有限公司 热塑性弹性体微孔发泡组合物、微孔发泡材料及其制备方法与应用

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US5160383A (en) * 1990-09-17 1992-11-03 The Goodyear Tire & Rubber Company Tire having identification label affixed thereto
JP2000166603A (ja) * 1998-12-08 2000-06-20 Asics Corp 靴底材
CN1511176A (zh) * 2001-02-15 2004-07-07 Jsr株式会社 充油1,2-聚丁二烯、其制法以及其组合物与成型品
JP2006028360A (ja) * 2004-07-16 2006-02-02 Jsr Corp 発泡成形体の製造方法
CN101060963A (zh) * 2004-11-16 2007-10-24 捷时雅株式会社 交联发泡成型体的制造方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5160383A (en) * 1990-09-17 1992-11-03 The Goodyear Tire & Rubber Company Tire having identification label affixed thereto
JP2000166603A (ja) * 1998-12-08 2000-06-20 Asics Corp 靴底材
CN1511176A (zh) * 2001-02-15 2004-07-07 Jsr株式会社 充油1,2-聚丁二烯、其制法以及其组合物与成型品
JP2006028360A (ja) * 2004-07-16 2006-02-02 Jsr Corp 発泡成形体の製造方法
CN101060963A (zh) * 2004-11-16 2007-10-24 捷时雅株式会社 交联发泡成型体的制造方法

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111320833A (zh) * 2018-12-13 2020-06-23 泉州嘉泰鞋业有限公司 一种新型高分子复合发泡材料注射耐磨止滑中底及其制造方法
CN111332605A (zh) * 2020-03-20 2020-06-26 上海宝钢阿赛洛激光拼焊有限公司 用于铝合金板运输的损伤防护装置及方法
CN112679902A (zh) * 2020-12-07 2021-04-20 天津天星科生皮革制品有限公司 一种耐磨鞋底制备工艺
CN112852028A (zh) * 2021-01-15 2021-05-28 河北皋端建材科技有限公司 一种运动地板用热塑性弹性体组合物及其制备方法
CN112852028B (zh) * 2021-01-15 2023-07-04 河北皋端建材科技有限公司 一种运动地板用热塑性弹性体组合物及其制备方法
CN112961510A (zh) * 2021-02-07 2021-06-15 远东电缆有限公司 风电用66kV高强度高耐热HEPR绝缘料及制备方法
CN115403839B (zh) * 2021-05-26 2024-06-04 中国石油化工股份有限公司 热塑性弹性体微孔发泡组合物、微孔发泡材料及其制备方法与应用
CN114085433A (zh) * 2021-12-29 2022-02-25 江苏铁科新材料股份有限公司 一种适用于注射成型的高硬度橡胶材料及其制备工艺
CN115073875A (zh) * 2022-07-01 2022-09-20 南通普力马弹性体技术有限公司 一种湿式止滑热塑性弹性体及其制备方法
CN115073875B (zh) * 2022-07-01 2023-09-01 南通普力马弹性体技术有限公司 一种湿式止滑热塑性弹性体及其制备方法
CN115109327A (zh) * 2022-08-22 2022-09-27 广东粤港澳大湾区黄埔材料研究院 一种轮胎胎侧橡胶组合物及其制备方法
CN115109327B (zh) * 2022-08-22 2022-11-18 广东粤港澳大湾区黄埔材料研究院 一种轮胎胎侧橡胶组合物及其制备方法

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