WO2022073489A1 - Semi-steel base rubber material using carbon nano tube composite masterbatch and preparation method therefor - Google Patents

Semi-steel base rubber material using carbon nano tube composite masterbatch and preparation method therefor Download PDF

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WO2022073489A1
WO2022073489A1 PCT/CN2021/122718 CN2021122718W WO2022073489A1 WO 2022073489 A1 WO2022073489 A1 WO 2022073489A1 CN 2021122718 W CN2021122718 W CN 2021122718W WO 2022073489 A1 WO2022073489 A1 WO 2022073489A1
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semi
carbon nanotube
steel base
nanotube composite
rubber
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PCT/CN2021/122718
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French (fr)
Chinese (zh)
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王�锋
李彦果
马玉净
孙冰冰
罗洪罡
徐晶
邢涛
韩绍楠
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山东玲珑轮胎股份有限公司
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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
    • C08L7/00—Compositions of natural rubber
    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2296—Oxides; Hydroxides of metals of zinc
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T10/00—Road transport of goods or passengers
    • Y02T10/80—Technologies aiming to reduce greenhouse gasses emissions common to all road transportation technologies
    • Y02T10/86—Optimisation of rolling resistance, e.g. weight reduction 

Definitions

  • the invention relates to a semi-steel base rubber compound using carbon nanotube composite masterbatch and a preparation method thereof.
  • Carbon nanotubes are one-dimensional materials with a diameter of 0.17-30nm and a length of tens of micrometers, which are rolled up by graphene sheets formed by carbon atoms. Due to its unique structure, carbon nanotubes have excellent mechanical properties, electrical conductivity, thermal conductivity and so on. Carbon nanotubes are used to enhance the mechanical, electrical and thermal properties of polymers.
  • the present invention provides a semi-steel base rubber compound using a carbon nanotube composite masterbatch and a preparation method thereof.
  • This solution solves the problem of dispersing carbon nanotubes in general-purpose rubber, and at the same time obtains a semi-steel base compound with high electrical conductivity and low rolling resistance.
  • a semi-steel base rubber compound using carbon nanotube composite masterbatch the raw material composition of the rubber compound comprises by weight: 50-100 parts of natural rubber, 20-50 parts of high specific surface area, high-structure carbon black and 1- 55 parts carbon nanotube composite.
  • the iodine absorption value of the carbon black is above 90 g/kg, and the DBP absorption value is above 113 ⁇ 10 -5 m 3 /kg.
  • the carbon nanotube composite is a high-cis polybutadiene material containing 10% by mass of carbon nanotubes.
  • the raw material composition of the sizing material further comprises, in parts by weight: antioxidant, zinc oxide, stearic acid, sulfur and accelerator.
  • step (1) (2) adding carbon black, anti-aging agent, zinc oxide, stearic acid to step (1) for mixing, heating up and controlling the temperature to 150-165 °C and degumming to form a masterbatch;
  • the base glue of the present application has both high conductivity and low rolling resistance properties.
  • the carbon nanotube composite is uniformly dispersed in natural rubber in advance. Due to the good compatibility of the matrix material of carbon nanotube composites with general-purpose rubber, the natural rubber and carbon nanotube composites are added to the internal mixer for 20-40s mastication by mixing in a common internal mixer, and high-structure carbon is added. Black, anti-aging agent, zinc oxide, stearic acid are mixed, the temperature is increased and the temperature is controlled at 150-165 °C to form a masterbatch; after parking, sulfur and accelerator are added, the temperature is increased and the temperature is controlled at 95-105 °C for debinding , forming a base compound, and carbon nanotubes can be well dispersed into the base compound. This base compound combines high conductivity with low rolling resistance properties.
  • Base compounds of the compositions specified in Tables 1 and 2 were prepared in a BR Banbury mixer using two separate feed mixing stages, ie, a non-productive mixing stage and a productive mixing stage stage.
  • the non-productive stage the mixing is carried out for about 2-3 minutes, until the rubber temperature reaches 160 °C, that is, it is completed.
  • the kneading time in the productive stage is the time until the rubber temperature reaches 115°C.
  • the base stock is referred to herein as Sample A, Sample B, Sample C.
  • Sample A is used here as a comparison sample, ie, the optimized rubber formulation was not used in the base compound.
  • Table 2 presents the electrical conductivity and heat generation properties of the vulcanized samples A-C.
  • Base compounds of the compositions specified in Tables 3 and 4 were prepared in a BR Banbury mixer using two separate feed mixing stages, ie, a non-productive mixing stage and a productive mixing stage stage.
  • the non-productive stage the mixing is carried out for about 2-3 minutes, until the rubber temperature reaches 160 °C, that is, it is completed.
  • the kneading time in the productive stage is the time until the rubber temperature reaches 115°C.
  • the base stock is referred to herein as Sample 1, Sample 2.
  • Sample 1 is used here as a comparison sample, ie, the optimized rubber formulation was not used in the base compound.
  • Table 4 presents the electrical conductivity and heat generation properties of vulcanized samples 1-2.
  • a semi-steel base compound having both high electrical conductivity and low rolling resistance properties is prepared.
  • the electrical conductivity and low rolling resistance properties of the base compound are improved.

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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)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Tires In General (AREA)

Abstract

The present invention relates to a semi-steel base rubber material using a carbon nano tube composite masterbatch and a preparation method therefor. The rubber material is prepared from the following raw materials in parts by weight: 50-100 parts of a natural rubber, 20-50 parts of carbon black with a high specific surface area and a high structure, and 1-55 parts of a carbon nanotube compound. The preparation method comprises the following steps: uniformly dispersing the carbon nanotube compound into the natural rubber in advance at a certain ratio, and adding same to an internal mixer for plasticization for 20-40 seconds; then adding carbon black, an anti-aging agent, zinc oxide and stearic acid for mixing, heating same and controlling the temperature to be 150-165ºC, and discharging the rubber to form the masterbatch; and after leaving to stand, adding sulfur and an accelerant, and raising the temperature and controlling the temperature to be 95-105ºC for rubber discharging, so as to form the semi-steel base rubber material. The base rubber disclosed by the invention has a high conductivity and a low rolling resistance.

Description

一种使用碳纳米管复合母胶的半钢基部胶料及其制备方法A kind of semi-steel base compound using carbon nanotube composite masterbatch and preparation method thereof 技术领域technical field
本发明涉及一种使用碳纳米管复合母胶的半钢基部胶料及其制备方法。 The invention relates to a semi-steel base rubber compound using carbon nanotube composite masterbatch and a preparation method thereof.
背景技术Background technique
现有超高性能和绿色半钢子午线轮胎中通常采用具有高导电率的基部胶（烟囱胶）来帮助轮胎导电。这类基部胶采用炭黑作为填料，为了得到良好的导电性能，会牺牲胶料的生热性能，会导致轮胎滚动阻力的上升。Existing ultra-high performance and green semi-steel radial tires often use a base compound (chimney compound) with high electrical conductivity to help the tire conduct electricity. This type of base rubber uses carbon black as a filler. In order to obtain good electrical conductivity, the heat generation performance of the rubber compound will be sacrificed, which will lead to an increase in the rolling resistance of the tire.
技术问题technical problem
普通的大量填充炭黑的橡胶材料固然可以满足轮胎的导电性能，但生热或是滚动阻力会很高，难以满足低滚阻轮胎的需求，也就是难以兼顾胶料的导电性和滚动阻力性能。Ordinary rubber materials filled with a large amount of carbon black can meet the electrical conductivity of the tire, but the heat generation or rolling resistance will be very high, and it is difficult to meet the needs of low rolling resistance tires, that is, it is difficult to take into account the electrical conductivity and rolling resistance of the rubber. .
碳纳米管是由碳原子形成的石墨烯片卷曲而成的，管直径在0.17-30nm，长数十微米的一维材料。由于其独特的结构，碳纳米管具有优异的力学性能、导电性能、导热性能等。碳纳米管被用来增强聚合物的力学、导电、导热性能。Carbon nanotubes are one-dimensional materials with a diameter of 0.17-30nm and a length of tens of micrometers, which are rolled up by graphene sheets formed by carbon atoms. Due to its unique structure, carbon nanotubes have excellent mechanical properties, electrical conductivity, thermal conductivity and so on. Carbon nanotubes are used to enhance the mechanical, electrical and thermal properties of polymers.
碳纳米管极易相互缠结，很难通过普通混炼方式将其分散到橡胶基体中，限制了碳纳米管优异性能的体现，因此限制了碳纳米管在橡胶中的工业化应用。Carbon nanotubes are easily entangled with each other, and it is difficult to disperse them into the rubber matrix by ordinary mixing methods, which limits the manifestation of the excellent properties of carbon nanotubes, thus limiting the industrial application of carbon nanotubes in rubber.
技术解决方案technical solutions
针对上述现有技术的不足，本发明提供一种使用碳纳米管复合母胶的半钢基部胶料及其制备方法。本方案解决碳纳米管在通用橡胶中分散的问题，同时获得了高导电兼具低滚动阻力性能的半钢基部胶料。In view of the above-mentioned deficiencies of the prior art, the present invention provides a semi-steel base rubber compound using a carbon nanotube composite masterbatch and a preparation method thereof. This solution solves the problem of dispersing carbon nanotubes in general-purpose rubber, and at the same time obtains a semi-steel base compound with high electrical conductivity and low rolling resistance.
一种使用碳纳米管复合母胶的半钢基部胶料，所述胶料的原料组成按重量份包括：50-100份天然橡胶，20-50份高比表面积、高结构炭黑和1-55份碳纳米管复合物。A semi-steel base rubber compound using carbon nanotube composite masterbatch, the raw material composition of the rubber compound comprises by weight: 50-100 parts of natural rubber, 20-50 parts of high specific surface area, high-structure carbon black and 1- 55 parts carbon nanotube composite.
优选的，所述炭黑的吸碘值在90g/kg以上，DBP吸收值在113×10 -5m 3/kg以上。 Preferably, the iodine absorption value of the carbon black is above 90 g/kg, and the DBP absorption value is above 113×10 -5 m 3 /kg.
优选的，所述碳纳米管复合物是含质量百分数10%的碳纳米管的高顺式聚丁二烯材料。Preferably, the carbon nanotube composite is a high-cis polybutadiene material containing 10% by mass of carbon nanotubes.
优选的，所述胶料的原料组成按重量份还包括：防老剂、氧化锌、硬脂酸、硫磺和促进剂。Preferably, the raw material composition of the sizing material further comprises, in parts by weight: antioxidant, zinc oxide, stearic acid, sulfur and accelerator.
本发明还提供一种使用碳纳米管复合母胶的半钢基部胶料的制备方法，所述方法的制备步骤包括：The present invention also provides a method for preparing a semi-steel base compound using carbon nanotube composite masterbatch. The preparation steps of the method include:
（1）按配比将碳纳米管复合物预先均匀分散在天然橡胶中，加入密炼机进行20-40s塑炼；(1) Disperse the carbon nanotube composite uniformly in the natural rubber in advance according to the proportion, and add it to the internal mixer for 20-40s plasticizing;
（2）再向步骤（1）中加入炭黑、防老剂、氧化锌、硬脂酸进行混炼，升温并控制温度150-165℃排胶形成母炼胶；(2) adding carbon black, anti-aging agent, zinc oxide, stearic acid to step (1) for mixing, heating up and controlling the temperature to 150-165 ℃ and degumming to form a masterbatch;
（3）停放后再加入硫磺和促进剂，升温并控制温度在95-105℃排胶，形成半钢基部胶料。(3) After parking, add sulfur and accelerator, heat up and control the temperature at 95-105 ℃ to remove glue to form a semi-steel base compound.
有益效果beneficial effect
本申请基部胶兼具了高导性与低滚动阻力性能。The base glue of the present application has both high conductivity and low rolling resistance properties.
本发明的实施方式Embodiments of the present invention
本申请将质量百分含量为5-15%的碳纳米管复合物预先均匀分散在天然橡胶中。由于碳纳米管复合物的基体材料与通用橡胶相容性好，通过普通密炼机混炼的方式，天然橡胶和碳纳米管复合物加入密炼机进行20-40s塑炼，加入高结构炭黑、防老剂、氧化锌、硬脂酸进行混炼，升温并控制温度150-165℃排胶形成母炼胶；停放后再加入硫磺和促进剂，升温并控制温度在95-105℃排胶，形成基部胶料，碳纳米管就能很好分散到基部胶料中。此基部胶兼具了高导性与低滚动阻力性能。In the present application, 5-15% by mass of the carbon nanotube composite is uniformly dispersed in natural rubber in advance. Due to the good compatibility of the matrix material of carbon nanotube composites with general-purpose rubber, the natural rubber and carbon nanotube composites are added to the internal mixer for 20-40s mastication by mixing in a common internal mixer, and high-structure carbon is added. Black, anti-aging agent, zinc oxide, stearic acid are mixed, the temperature is increased and the temperature is controlled at 150-165 °C to form a masterbatch; after parking, sulfur and accelerator are added, the temperature is increased and the temperature is controlled at 95-105 °C for debinding , forming a base compound, and carbon nanotubes can be well dispersed into the base compound. This base compound combines high conductivity with low rolling resistance properties.
具体的如下述实例。Specific examples are as follows.
实例1Example 1
在BR Banbury密炼机中制备如表1及表2中所规定成分的基部胶料，制备过程采取两个分开的加料混炼阶段，即，一个非生产性混炼阶段和一个生产性混炼阶段。非生产性阶段分别进行约2-3min的混炼，直至橡胶温度达到160℃，即完成。生产性阶段的混炼时间是使橡胶温度达到115℃的时间。Base compounds of the compositions specified in Tables 1 and 2 were prepared in a BR Banbury mixer using two separate feed mixing stages, ie, a non-productive mixing stage and a productive mixing stage stage. In the non-productive stage, the mixing is carried out for about 2-3 minutes, until the rubber temperature reaches 160 °C, that is, it is completed. The kneading time in the productive stage is the time until the rubber temperature reaches 115°C.
该基部胶料在这里被称之为样品A、样品B、样品C。样品A在这里被当做对比样，即，在基部胶料中未使用最优化的橡胶配比。The base stock is referred to herein as Sample A, Sample B, Sample C. Sample A is used here as a comparison sample, ie, the optimized rubber formulation was not used in the base compound.
所有的样品在约151℃硫化约30min。表2给出了硫化样品A-C的导电与生热性能。All samples were cured at about 151°C for about 30 minutes. Table 2 presents the electrical conductivity and heat generation properties of the vulcanized samples A-C.
表1Table 1
Figure dest_path_image002
Figure dest_path_image002
表2Table 2
151℃*30min硫化151℃*30min vulcanization A对比样A comparison sample BB CC
60℃tanδ60℃tanδ 0.110.11 0.090.09 0.110.11
电阻，kΩResistance, kΩ 1010 1010 0.010.01
  
实例2Example 2
在BR Banbury密炼机中制备如表3及表4中所规定成分的基部胶料，制备过程采取两个分开的加料混炼阶段，即，一个非生产性混炼阶段和一个生产性混炼阶段。非生产性阶段分别进行约2-3min的混炼，直至橡胶温度达到160℃，即完成。生产性阶段的混炼时间是使橡胶温度达到115℃的时间。Base compounds of the compositions specified in Tables 3 and 4 were prepared in a BR Banbury mixer using two separate feed mixing stages, ie, a non-productive mixing stage and a productive mixing stage stage. In the non-productive stage, the mixing is carried out for about 2-3 minutes, until the rubber temperature reaches 160 °C, that is, it is completed. The kneading time in the productive stage is the time until the rubber temperature reaches 115°C.
该基部胶料在这里被称之为样品1、样品2。样品1在这里被当做对比样，即，在基部胶料中未使用最优化的橡胶配比。The base stock is referred to herein as Sample 1, Sample 2. Sample 1 is used here as a comparison sample, ie, the optimized rubber formulation was not used in the base compound.
所有的样品在约151℃硫化约30min。表4给出了硫化样品1-2的导电与生热性能。All samples were cured at about 151°C for about 30 minutes. Table 4 presents the electrical conductivity and heat generation properties of vulcanized samples 1-2.
表3table 3
Figure dest_path_image004
Figure dest_path_image004
表4Table 4
151℃*30min硫化151℃*30min vulcanization 1对比样1 comparison sample 22
60℃tanδ60℃tanδ 0.120.12 0.070.07
电阻，kΩResistance, kΩ 23twenty three 0.0170.017
通过本申请制备方法，制得兼具高导电和低滚阻性能的半钢基部胶料。通过添加20-50phr高比表面积、高结构炭黑和1-55phr碳纳米管复合物提高基部胶料的导电性和兼具低滚动阻力性能。Through the preparation method of the present application, a semi-steel base compound having both high electrical conductivity and low rolling resistance properties is prepared. By adding 20-50phr high specific surface area, high-structure carbon black and 1-55phr carbon nanotube composites, the electrical conductivity and low rolling resistance properties of the base compound are improved.
工业实用性Industrial Applicability
本发明可用其他的不违背本发明的精神或主要特征的具体形式来概述。因此，无论从哪一点来看，本发明的上述实施方案都只能认为是对本发明的说明而不能限制本发明，权利要求书指出了本发明的范围，而上述的说明并未指出本发明的范围，因此，在与本发明的权利要求书相当的含义和范围内的任何改变，都应认为是包括在本发明的权利要求书的范围内。The present invention may be summarized in other specific forms that do not depart from the spirit or main characteristics of the invention. Therefore, no matter from which point of view, the above-mentioned embodiments of the present invention can only be regarded as the description of the present invention and cannot limit the present invention. The claims indicate the scope of the present invention, but the above-mentioned description does not indicate the scope of the present invention. Therefore, any changes within the meaning and scope equivalent to the claims of the present invention should be construed as being included in the scope of the claims of the present invention.

Claims (5)

  1. 一种使用碳纳米管复合母胶的半钢基部胶料，其特征在于，所述胶料的原料组成按重量份包括：50-100份天然橡胶，20-50份高比表面积、高结构炭黑和1-55份碳纳米管复合物。A semi-steel base rubber compound using carbon nanotube composite masterbatch is characterized in that, the raw material composition of the rubber compound comprises by weight: 50-100 parts of natural rubber, 20-50 parts of high specific surface area, high structure carbon Black and 1-55 parts carbon nanotube composite.
  2. 如权利要求1所述的使用碳纳米管复合母胶的半钢基部胶料，其特征在于，所述炭黑的吸碘值在90g/kg以上，DBP吸收值在113×10 -5m 3/kg以上。 The semi-steel base compound using carbon nanotube composite masterbatch according to claim 1, wherein the iodine absorption value of the carbon black is above 90 g/kg, and the DBP absorption value is 113×10 −5 m 3 /kg or more.
  3. 如权利要求1所述的使用碳纳米管复合母胶的半钢基部胶料，其特征在于，所述碳纳米管复合物是含质量百分数10%的碳纳米管的高顺式聚丁二烯材料。The semi-steel base compound using carbon nanotube composite masterbatch according to claim 1, wherein the carbon nanotube composite is high cis polybutadiene containing 10% by mass of carbon nanotubes Material.
  4. 如权利要求1所述的使用碳纳米管复合母胶的半钢基部胶料，其特征在于，所述胶料的原料组成按重量份还包括：防老剂、氧化锌、硬脂酸、硫磺和促进剂。The semi-steel base sizing material using carbon nanotube composite masterbatch according to claim 1, wherein the raw material composition of the sizing material further comprises by weight: antioxidant, zinc oxide, stearic acid, sulfur and accelerator.
  5. 如权利要求4所述的使用碳纳米管复合母胶的半钢基部胶料的制备方法，其特征在于，所述方法的制备步骤包括：The method for preparing a semi-steel base compound using carbon nanotube composite masterbatch according to claim 4, wherein the preparation steps of the method include:
    （1）按配比将碳纳米管复合物预先均匀分散在天然橡胶中，加入密炼机进行20-40s塑炼；(1) Disperse the carbon nanotube composite uniformly in the natural rubber in advance according to the proportion, and add it to the internal mixer for 20-40s plasticizing;
    （2）再向步骤（1）中加入炭黑、防老剂、氧化锌、硬脂酸进行混炼，升温并控制温度150-165℃排胶形成母炼胶；(2) adding carbon black, anti-aging agent, zinc oxide, stearic acid to step (1) for mixing, heating up and controlling the temperature to 150-165 ℃ and degumming to form a masterbatch;
    （3）停放后再加入硫磺和促进剂，升温并控制温度在95-105℃排胶，形成半钢基部胶料。(3) After parking, add sulfur and accelerator, heat up and control the temperature at 95-105 ℃ to remove glue to form a semi-steel base compound.
PCT/CN2021/122718 2020-10-09 2021-10-08 Semi-steel base rubber material using carbon nano tube composite masterbatch and preparation method therefor WO2022073489A1 (en)

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