CN111247198B - 用于制备橡胶制品的配混料 - Google Patents
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Abstract
一种用于制备橡胶制品的配混料，其包括可交联的不饱和链的聚合物基料、增强填料和硫化体系。硫化体系至少包括硫磺、一种以上的硫化促进剂和由卤化石墨构成的硫化活化剂。
Description
发明内容
本发明涉及用于制造橡胶制品的橡胶配混料。
本发明获得在充气轮胎的制备中特别有利的应用，为此，本说明书将明确地参考充气轮胎，而不会丧失一般性。
近来，橡胶配混料领域的研究课题之一集中于作为硫化活化剂的氧化锌(ZnO)的可能替代物上。
由于其可能的环境影响，如果不能完全消除的话，则要求ZnO的使用受到限制。显然，如果一方面ZnO的过度限制响应于环境品质的要求，另一方面它可能损害配混料的有效硫化，则ZnO的过度限制在所得配混料的机械特性方面具有负面后果。
因此，感到需要提供一种在橡胶配混料中ZnO的使用的替代，其将能够遵守环境品质的要求，而不会由于这个原因改变所得配混料的硫化并因此损害其机械特性。
申请人意外地发现，特定类别的官能化石墨能够完全替代配混料中作为硫化活化剂的ZnO的存在，并且同时保持所得配混料的机械特性不变。
本发明的目的为一种用于制备橡胶制品的配混料，其包括可交联的不饱和链的聚合物基料、增强填料和硫化体系；所述硫化体系至少包括硫磺、一种以上的硫化促进剂和硫化活化剂；所述配混料的特征在于，所述硫化活化剂完全地为卤化石墨；所述配混料既不包括硬脂酸也不包括氧化锌。
此处和下文中，卤化石墨是指其中碳原子通过共价键与卤素原子连接的石墨。
此处和下文中，术语“可交联的不饱和链的聚合物基料”是指任何天然的或合成的未交联的聚合物，其能够在用硫磺类体系交联(硫化)之后呈现通常由弹性体呈现的所有化学-物理和机械特性。
优选地，所述卤化石墨为氟化石墨。
优选地，所述卤化石墨以0.1～100phr的量、更优选0.5～20phr的量存在于配混料中。
本发明的进一步目的为一种充气轮胎部分，其用作为本发明目的的配混料来制造。
本发明的又一个目的为一种充气轮胎，其包括使用作为本发明目的的配混料制造的部分。
本发明的再一个目的为一种卤化石墨作为用于制备橡胶制品的配混料中的唯一硫化活化剂的用途。
为了更好地理解本发明，出于说明性和非限制性目的包括以下实施例。
实施例
制备两组配混料以测试卤化石墨作为硫化活化剂的能力。第一组的配混料(配混料A-D)包括炭黑作为增强填料，而第二组配混料(配混料E-H)包括二氧化硅作为增强填料。
两组各自包括第一比较配混料，其中不使用硫化活化剂(配混料A和配混料E)；第二比较配混料，其中氧化锌用作硫化活化剂(配混料B和配混料F)；以及根据本发明的两种配混料，其中，作为硫化活化剂，示例的卤化石墨以两种各自不同的量使用(配混料C、配混料D和配混料G、配混料H)。
实例配混料根据以下步骤获得：
-配混料的制备-
(第一混炼步骤)
在开始混炼之前，用可交联的聚合物基料以及炭黑或二氧化硅和硅烷偶联剂(作为后者的替代物)装填具有切向型转子且内容积为230～270升之间的混合机中，因此使填充系数达到66-72％。
混合机以40-60转/分钟的速度运行，并且由此形成的混合物一旦达到140-160℃的温度就排出。
(第二混炼步骤)
由先前步骤获得的混合物在以40-60转/分钟的速度运行的混合机中再加工，其后，一旦达到130-150℃的温度就排出。
(最终混炼步骤)
向由先前步骤获得的混合物中添加硫磺、硫化促进剂，然后如果提供的话，添加卤化石墨、或ZnO与硬脂酸的组合，使填充系数达到63-67％。
与上述相反，如氧化锌的情况一样，卤化石墨可以在第一或第二混炼步骤期间添加。
混合机以20-40转/分钟的速度运行，由此形成的混合物一旦达到100-110℃的温度就排出。
表I和II列出了以phr计的八种配混料的组成。
表I
表II
使用的聚合物基料为聚异戊二烯。
使用的炭黑归类为N330。
使用的二氧化硅由EVONIK公司以名称Ultrasil VN3 GR出售，其表面积为约180m2/g。
使用的硅烷偶联剂属于聚硫有机硅烷类并且由EVONIK公司以名称SI75出售。
使用的卤化石墨为由SIGMAALDRICH公司出售的氟化石墨(CAS编号：51311-17-2，编码No.372455)。
TBBS为N-叔丁基-2-苯并噻唑次磺酰胺化合物的首字母缩写词，并且用作硫化促进剂。
为了评价其交联、流变、机械和动态机械性能，由表I和II的配混料制备各样品，并对其进行一系列测试。
特别地，交联性能通过X-连接密度测量(X-link Density measurement)(Flory,Paul；Rehner,John J.Chem.Phys.11:521-526(1943))来测量；流变性能依照ISO 6502标准来测量；机械性能依照ISO 37标准来测量；动态机械性能依照ISO 4664标准来测量。
从测试中获得的值在表III和IV中列出。
表III
| A | B | C | D | |
| X-连接密度 | 0.49 | 1.40 | 0.90 | 1.08 |
| ML(dNm) | 3.12 | 2.98 | 3.25 | 3.35 |
| MH(dNm) | 10.16 | 12.38 | 11.01 | 12 |
| MH-ML(dNm) | 7.04 | 10.4 | 7.76 | 8.65 |
| t’10(min) | 1.08 | 1.36 | 1.08 | 1.13 |
| t’50(min) | 1.9 | 2.43 | 2.12 | 3.34 |
| t’90(min) | 2.31 | 3.9 | 2.78 | 5.94 |
| TB(MPa) | 12.0 | 23.5 | 14.0 | 23.0 |
| 50％(MPa) | 0.6 | 0.9 | 0.7 | 0.9 |
| 100％(MPa) | 0.8 | 1.5 | 1.1 | 1.4 |
| 300％(MPa) | 2.8 | 7.3 | 4.7 | 7.0 |
| EB％(MPa) | 660 | 635 | 580 | 630 |
| E’25℃(MPa) | 5.61 | 7.41 | 6.64 | 7.88 |
| TANδ25℃ | 0.202 | 0.193 | 0.189 | 0.192 |
表IV
| E | F | G | H | |
| X-连接密度 | 0.85 | 1.75 | 1.23 | 1.74 |
| ML(dNm) | 3.5 | 3.13 | 3.55 | 3.65 |
| MH(dNm) | 10.65 | 16.2 | 12.64 | 15.61 |
| MH-ML(dNm) | 7.15 | 13.07 | 9.09 | 11.96 |
| t’10(min) | 0.27 | 1.03 | 0.29 | 0.41 |
| t’50(min) | 0.85 | 2.61 | 1.02 | 1.6 |
| t’90(min) | 1.46 | 3.75 | 2.88 | 4.83 |
| TB(MPa) | 11.2 | 23.0 | 16.4 | 24.0 |
| 50％(MPa) | 0.7 | 1.1 | 0.9 | 1.2 |
| 100％(MPa) | 0.9 | 1.7 | 1.4 | 1.9 |
| 300％(MPa) | 5.0 | 7.5 | 7.5 | 7.7 |
| EB％(MPa) | 380 | 600 | 400 | 600 |
| E’25℃(MPa) | 8.06 | 9.75 | 9.09 | 9.43 |
| TANδ25℃ | 0.16 | 0.145 | 0.155 | 0.159 |
从表III和IV中的值证明了卤化石墨作为硫化活化剂的出乎意料的活性。事实上，与上述性能有关的结果证明了卤化石墨的存在(配混料C、D、G、H)如何与氧化锌的存在(配混料B和F)相当并且与不存在硫化活化剂(配混料A和E)不同，以及有利于配混料的恰当的硫化。
特别地，两组配混料(炭黑或二氧化硅作为增强填料的选择性的使用)表明卤化石墨作为硫化活化剂的有效性与使用的增强填料的种类无关。
总之，本发明通过用卤化石墨代替氧化锌，使得可以消除在橡胶配混料中氧化锌的使用，而不会由于这个原因以任何方式损害同一配混料的硫化以及因此损害其机械特性。
Claims (7)
1.一种卤化石墨作为用于制备橡胶制品的配混料中的唯一硫化活化剂的用途。
2.根据权利要求1所述的用途，其特征在于，所述卤化石墨为氟化石墨。
3.根据权利要求1或2所述的用途，其特征在于，所述卤化石墨以0.1～100phr的量存在于配混料中。
4.根据权利要求1或2所述的用途，其特征在于，所述卤化石墨以0.5～20phr的量存在于配混料中。
5.根据权利要求3所述的用途，其特征在于，所述卤化石墨以0.5～20phr的量存在于配混料中。
6.一种充气轮胎的部分，其使用根据权利要求1～5中任一项所述的用途中得到的配混料来制造。
7.一种充气轮胎，其包括根据权利要求6所述的部分。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| IT102017000122778 | 2017-10-27 | ||
| IT102017000122778A IT201700122778A1 (it) | 2017-10-27 | 2017-10-27 | Mescola per la preparazione di prodotti in gomma |
| PCT/IB2018/058282 WO2019082086A1 (en) | 2017-10-27 | 2018-10-24 | COMPOUND FOR THE PREPARATION OF RUBBER PRODUCTS |
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| Publication Number | Publication Date |
|---|---|
| CN111247198A CN111247198A (zh) | 2020-06-05 |
| CN111247198B true CN111247198B (zh) | 2022-06-24 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201880068887.4A Active CN111247198B (zh) | 2017-10-27 | 2018-10-24 | 用于制备橡胶制品的配混料 |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US20200391549A1 (zh) |
| EP (1) | EP3700973A1 (zh) |
| JP (1) | JP6960052B2 (zh) |
| CN (1) | CN111247198B (zh) |
| IT (1) | IT201700122778A1 (zh) |
| WO (1) | WO2019082086A1 (zh) |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62169845A (ja) * | 1986-01-22 | 1987-07-27 | Asahi Chem Ind Co Ltd | フツ素ゴム組成物 |
| JPS62246948A (ja) * | 1986-04-18 | 1987-10-28 | Asahi Chem Ind Co Ltd | エチレン／プロピレンゴムとフツ化黒鉛とからなる組成物 |
| US7414087B2 (en) * | 2003-08-20 | 2008-08-19 | Sumitomo Rubber Industries, Ltd. | Rubber composition and pneumatic tire using the same |
| JP4462862B2 (ja) * | 2003-08-20 | 2010-05-12 | 住友ゴム工業株式会社 | ゴム組成物 |
| CN107108978B (zh) * | 2014-11-13 | 2018-11-27 | 株式会社普利司通 | 用于生产轮胎的橡胶配混料 |
| CN104829892B (zh) * | 2015-05-22 | 2017-02-08 | 福建起步儿童用品有限公司 | 一种鞋底用高耐磨橡胶材料及其制备方法 |
| CN106751021A (zh) * | 2016-12-06 | 2017-05-31 | 佛山市高明区生产力促进中心 | 一种耐腐蚀的三元乙丙橡胶 |
-
2017
- 2017-10-27 IT IT102017000122778A patent/IT201700122778A1/it unknown
-
2018
- 2018-10-24 JP JP2020523409A patent/JP6960052B2/ja active Active
- 2018-10-24 CN CN201880068887.4A patent/CN111247198B/zh active Active
- 2018-10-24 EP EP18800768.6A patent/EP3700973A1/en active Pending
- 2018-10-24 US US16/754,449 patent/US20200391549A1/en not_active Abandoned
- 2018-10-24 WO PCT/IB2018/058282 patent/WO2019082086A1/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| EP3700973A1 (en) | 2020-09-02 |
| US20200391549A1 (en) | 2020-12-17 |
| JP6960052B2 (ja) | 2021-11-05 |
| WO2019082086A1 (en) | 2019-05-02 |
| JP2021500456A (ja) | 2021-01-07 |
| IT201700122778A1 (it) | 2019-04-27 |
| CN111247198A (zh) | 2020-06-05 |
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