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CN116355299A - Standard reference glue material and its preparation method and application - Google Patents

Standard reference glue material and its preparation method and application Download PDF

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Publication number
CN116355299A
CN116355299A CN202310381108.9A CN202310381108A CN116355299A CN 116355299 A CN116355299 A CN 116355299A CN 202310381108 A CN202310381108 A CN 202310381108A CN 116355299 A CN116355299 A CN 116355299A
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parts
rubber
standard reference
content
agent
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CN116355299B (en
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梁纪宇
林炜
李玉才
黄昌平
王鹏
冯健
石传晋
楚雪梅
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Sichuan University
Sinolight Inspection and Certification Co Ltd
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Sinolight Inspection and Certification Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L21/00Compositions of unspecified rubbers
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/56Investigating resistance to wear or abrasion
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N2001/2893Preparing calibration standards
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02TCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T10/00Road transport of goods or passengers
    • Y02T10/80Technologies aiming to reduce greenhouse gasses emissions common to all road transportation technologies
    • Y02T10/86Optimisation of rolling resistance, e.g. weight reduction 

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Abstract

The invention provides a standard reference glue material, a preparation method and application thereof. The standard reference rubber material comprises a rubber base material, an ethylene-vinyl acetate copolymer, a vulcanizing agent, naphthenic oil and tire powder; wherein, based on 100 parts by weight of the total rubber substrate, the content of the ethylene-vinyl acetate copolymer is 5-20 parts, the content of the vulcanizing agent is 2-5 parts, the content of the naphthenic oil is 15-30 parts, and the content of the tire powder is 50-100 parts. The standard reference glue material has low abrasion mass loss, small relative expansion uncertainty and good abrasion test uniformity and stability (including long-term stability and short-term transportation stability).

Description

标准参照胶材料及其制备方法和用途Standard reference glue material and its preparation method and application

技术领域technical field

本发明涉及一种标准参照胶材料及其制备方法和用途,特别涉及一种应用于辊筒式磨耗机法耐磨测试中使用的标准参照胶材料及其制备方法和用途,属于标准材料领域。The invention relates to a standard reference rubber material and its preparation method and application, in particular to a standard reference rubber material used in roller abrasion machine method wear test, its preparation method and application, and belongs to the field of standard materials.

背景技术Background technique

鞋在被穿着使用的过程当中,鞋底会受到摩擦力的作用,进而产生磨耗。磨耗是材料与其他物体相互摩擦或受到砂粒等各种坚硬粒子冲击作用而产生。鞋底的耐磨性能好坏直接影响鞋类产品的使用寿命,同时耐磨性能也是衡量鞋类产品质量等级的重要技术指标。因此,对鞋底的耐磨性能进行试验测定是鞋类产品在生产和检验中非常重要的常规检测项目之一。During the process of wearing and using the shoes, the soles of the shoes will be subjected to frictional forces, which will cause wear and tear. Abrasion is caused by friction between materials and other objects or by the impact of various hard particles such as sand. The wear resistance of the sole directly affects the service life of footwear products, and the wear resistance is also an important technical index to measure the quality level of footwear products. Therefore, testing and measuring the wear resistance of the sole is one of the very important routine testing items in the production and inspection of footwear products.

目前鞋类产品的耐磨检测方法主要有5种,包括整鞋耐磨测试法、阿克隆磨耗机法、辊筒式磨耗机法、NBS(National bureau of standard)磨耗试验机法和兰伯恩试验机法,5种测试方法测试原理和特点有所不同。其中辊筒式磨耗机法耐磨测试也称为DIN(Deutsches Institut Normung)磨耗测试,是国际国内通行的重要测试方法,可以被广泛的应用于国内外橡胶弹性体类材料相关产品的耐磨性能测试,如鞋底、轮胎、输送带和胶条等产品。At present, there are five main wear testing methods for footwear products, including the whole shoe wear test method, the Akron abrasion machine method, the roller abrasion machine method, the NBS (National bureau of standard) abrasion test machine method and the Lamborn test method. The testing machine method, the 5 testing methods have different testing principles and characteristics. Among them, the wear resistance test of the roller abrasion machine method is also called DIN (Deutsches Institut Normung) abrasion test, which is an important test method in the world and domestically, and can be widely used in the wear resistance of rubber and elastomer materials at home and abroad. Testing of products such as shoe soles, tires, conveyor belts and rubber strips.

DIN磨耗测试的优点是测试过程稳定、操作简单快捷、试样尺寸小、摩擦测试轨迹不重复等,由于该方法在测试过程中采用了标准参照胶(即辊筒式磨耗机法耐磨测试标准参照胶),可以有效降低试验设备和人员操作引起的测试误差。目前国内外相关实验室使用的标准参照胶材料均来自德国联邦材料检测研究院生产的BAM标准胶。The advantages of the DIN abrasion test are the stable test process, simple and fast operation, small sample size, non-repetitive friction test track, etc., because the method uses standard reference rubber (that is, the roller wear machine method wear test standard) in the test process. Reference glue), which can effectively reduce the test error caused by the test equipment and personnel operation. At present, the standard reference rubber materials used by relevant laboratories at home and abroad are all from the BAM standard rubber produced by the German Federal Institute for Materials Testing.

随着检测机构数量和检测需求高速上涨,对于试验耗材和标准样品的需求也在不断增加。DIN磨耗测试应用领域广泛,需求量较大,导致BAM标准胶逐渐供不应求。但实际上,该产品仍存在均匀性欠佳、易吐霜等缺点。因此,辊筒式磨耗机法耐磨测试标准参照胶的自主研制具有较高的社会价值和良好的经济效益,不仅能促进相关文字标准的贯彻和实施,更能够提高检测机构对辊筒式磨耗机法耐磨测试的准确性和结果溯源性。With the rapid increase in the number of testing institutions and the demand for testing, the demand for test consumables and standard samples is also increasing. DIN abrasion testing has a wide range of applications and a large demand, resulting in a gradual shortage of BAM standard rubber. But in fact, the product still has shortcomings such as poor uniformity and easy frosting. Therefore, the self-developed reference rubber for roller wear machine method wear test standard has high social value and good economic benefits. Accuracy and traceability of mechanical abrasion testing.

发明内容Contents of the invention

发明要解决的问题The problem to be solved by the invention

鉴于现有技术中存在的技术问题,本发明首先提供一种标准参照胶材料。本发明的标准参照胶材料的磨耗质量损失低,且相对扩展不确定度小,具备良好的磨耗测试均匀性以及长期、短期测试稳定性。In view of the technical problems existing in the prior art, the present invention firstly provides a standard reference glue material. The standard reference rubber material of the present invention has low abrasion mass loss and small relative expansion uncertainty, and has good abrasion test uniformity and long-term and short-term test stability.

进一步地,本发明还提供一种标准参照胶材料的制备方法,本发明的制备方法简单易行,原料易于获取,适合大批量生产。Furthermore, the present invention also provides a preparation method of a standard reference rubber material. The preparation method of the present invention is simple and easy, and the raw materials are easy to obtain, which is suitable for mass production.

用于解决问题的方案solutions to problems

本发明一种标准参照胶材料,其中,所述标准参照胶材料包括橡胶基材、乙烯-醋酸乙烯共聚物、硫化剂、环烷油以及轮胎粉;其中,A kind of standard reference rubber material of the present invention, wherein, described standard reference rubber material comprises rubber substrate, ethylene-vinyl acetate copolymer, vulcanizing agent, naphthenic oil and tire powder; Wherein,

以所述橡胶基材的总质量份数为100份计,所述乙烯-醋酸乙烯共聚物的含量为5~20份,所述硫化剂的含量为2~5份,所述环烷油的含量为15~30份,所述轮胎粉的含量为50~100份。Based on 100 parts by total mass of the rubber substrate, the content of the ethylene-vinyl acetate copolymer is 5-20 parts, the content of the vulcanizing agent is 2-5 parts, and the naphthenic oil The content is 15-30 parts, and the content of the tire powder is 50-100 parts.

根据本发明所述的标准参照胶材料,其中,所述橡胶基材包括顺丁橡胶和天然橡胶;优选地,以所述橡胶基材的总质量份数为100份计,所述顺丁橡胶的含量为40-60份,所述天然橡胶的含量为40-60份。According to the standard reference rubber material of the present invention, wherein, the rubber substrate comprises butadiene rubber and natural rubber; preferably, the total mass fraction of the rubber substrate is 100 parts, and the butadiene rubber The content of the natural rubber is 40-60 parts, and the content of the natural rubber is 40-60 parts.

根据本发明所述的标准参照胶材料,其中,所述标准参照胶材料还包含有补强剂、活性剂、防老剂、促进剂中的一种或两种以上的组合;优选地,以所述橡胶基材的总质量份数为100份计,所述补强剂的含量为50~75份,所述活性剂的含量为5~15份,所述促进剂的含量为2~5份,所述防老剂的含量为2~15份。According to the standard reference rubber material of the present invention, wherein, the standard reference rubber material also contains one or a combination of two or more of a reinforcing agent, an active agent, an anti-aging agent, and an accelerator; preferably, the The total mass of the rubber base material is 100 parts, the content of the reinforcing agent is 50-75 parts, the content of the active agent is 5-15 parts, and the content of the accelerator is 2-5 parts , the content of the anti-aging agent is 2 to 15 parts.

根据本发明所述的标准参照胶材料,其中,所述补强剂包括碳酸钙和/或白炭黑。According to the standard reference rubber material of the present invention, the reinforcing agent includes calcium carbonate and/or white carbon black.

根据本发明所述的标准参照胶材料,其中,所述活性剂包括一缩二乙二醇、聚乙二醇、硬脂酸、氧化镁、氧化锌中的一种或两种以上的组合。According to the standard reference glue material of the present invention, the active agent includes one or a combination of two or more of diethylene glycol, polyethylene glycol, stearic acid, magnesium oxide, and zinc oxide.

根据本发明所述的标准参照胶材料,其中,所述的防老剂包括2,2,4-三甲基-1,2-二氢化喹啉聚合体、1,2-双[β-(3,5-二叔丁基-4-羟基苯基)丙酰]肼、四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯、4,4'-硫代双(6-叔丁基-3-甲基苯酚)、硫代二丙酸二硬脂醇酯和硫代二丙酸二月桂酯中的一种或两种以上的组合。According to the standard reference rubber material of the present invention, wherein the anti-aging agent includes 2,2,4-trimethyl-1,2-dihydroquinoline polymer, 1,2-bis[β-(3 ,5-di-tert-butyl-4-hydroxyphenyl)propionyl]hydrazine, tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate]pentaerythritol ester, 4,4'- One or a combination of two or more of thiobis(6-tert-butyl-3-methylphenol), distearyl thiodipropionate and dilauryl thiodipropionate.

根据本发明所述的标准参照胶材料,其中,所述促进剂包括N-环己基-2-苯并噻唑次磺酰胺、N-叔丁基-2-苯并噻唑次磺酰胺、2,2'-二硫化二苯并噻唑、一硫化四甲基秋兰姆、2-硫醇基苯并噻唑、二硫化四甲基秋兰姆中的一种或两种以上的组合。According to the standard reference glue material of the present invention, wherein, the accelerator includes N-cyclohexyl-2-benzothiazole sulfenamide, N-tert-butyl-2-benzothiazole sulfenamide, 2,2 One or a combination of two or more of '-dibenzothiazole disulfide, tetramethylthiuram monosulfide, 2-mercaptobenzothiazole, and tetramethylthiuram disulfide.

本发明还提供一种根据本发明所述的标准参照胶材料的制备方法,其包括将标准参照胶材料的各组分混合的步骤。The present invention also provides a preparation method of the standard reference glue material according to the present invention, which includes the step of mixing the components of the standard reference glue material.

根据本发明所述的制备方法,其中,所述制备方法包括:According to the preparation method of the present invention, wherein the preparation method comprises:

将所述标准参照胶材料的各组分混合后进行混炼,得到混炼胶;mixing each component of the standard reference rubber material and then kneading to obtain a rubber mix;

对所述混炼胶进行炼片,得到混炼胶片;Carrying out sheet mixing to the mixed rubber to obtain a mixed rubber sheet;

对混炼胶片进行模压硫化成型,得到标准参照胶材料。The mixed rubber sheet is molded and vulcanized to obtain a standard reference rubber material.

本发明还提供一种根据本发明所述的标准参照胶材料在辊筒式磨耗机法耐磨测试中的用途。The present invention also provides an application of the standard reference rubber material according to the present invention in the wear resistance test of the roller abrasion machine method.

发明的效果The effect of the invention

本发明的标准参照胶材料的磨耗质量损失低,且相对扩展不确定度小,具备良好的磨耗测试均匀性以及稳定性(包括长期稳定性和短期运输稳定性)。The standard reference rubber material of the present invention has low abrasion mass loss, small relative expansion uncertainty, and good abrasion test uniformity and stability (including long-term stability and short-term transportation stability).

进一步地,本发明的标准参照胶材料的制备方法简单易行,原料易于获取,适合大批量生产。Furthermore, the preparation method of the standard reference rubber material of the present invention is simple and feasible, the raw materials are easy to obtain, and are suitable for mass production.

具体实施方式Detailed ways

以下将详细说明本发明的各种示例性实施例、特征和方面。在这里专用的词“示例性”意为“用作例子、实施例或说明性”。这里作为“示例性”所说明的任何实施例不必解释为优于或好于其它实施例。Various exemplary embodiments, features, and aspects of the invention are described in detail below. The word "exemplary" is used exclusively herein to mean "serving as an example, embodiment, or illustration." Any embodiment described herein as "exemplary" is not necessarily to be construed as superior or better than other embodiments.

另外,为了更好地说明本发明,在下文的具体实施方式中给出了众多的具体细节。本领域技术人员应当理解,没有某些具体细节,本发明同样可以实施。在另外一些实例中,对于本领域技术人员熟知的方法、手段、器材和步骤未作详细描述,以便于凸显本发明的主旨。In addition, in order to better illustrate the present invention, numerous specific details are given in the specific embodiments below. It will be understood by those skilled in the art that the present invention may be practiced without certain of the specific details. In other instances, methods, means, devices and steps well known to those skilled in the art are not described in detail in order to highlight the gist of the present invention.

如无特殊声明,本说明书中所使用的单位均为国际标准单位,并且本发明中出现的数值,数值范围,均应当理解为包含了工业生产中所不可避免的系统性误差。Unless otherwise stated, the units used in this specification are all international standard units, and the numerical values and numerical ranges appearing in the present invention should be understood as including inevitable systematic errors in industrial production.

本说明书中,使用“可以”表示的含义包括了进行某种处理以及不进行某种处理两方面的含义。In this specification, the meaning expressed by "may" includes the meaning of performing certain processing and not performing certain processing.

本说明书中,所提及的“一些具体/优选的实施方案”、“另一些具体/优选的实施方案”、“实施方案”等是指所描述的与该实施方案有关的特定要素(例如,特征、结构、性质和/或特性)包括在此处所述的至少一种实施方案中,并且可存在于其它实施方案中或者可不存在于其它实施方案中。另外,应理解,所述要素可以任何合适的方式组合在各种实施方案中。In this specification, references to "some specific/preferred embodiments", "other specific/preferred embodiments", "embodiments" and the like refer to specific elements described in relation to the embodiments (for example, A feature, structure, property, and/or characteristic) is included in at least one embodiment described herein, and may or may not be present in other embodiments. In addition, it is to be understood that the described elements may be combined in any suitable manner in the various embodiments.

本说明书中,使用“数值A~数值B”表示的数值范围是指包含端点数值A、B的范围。In this specification, the numerical range represented by "numerical value A - numerical value B" means the range which includes numerical value A and B of an end point.

本说明书中,使用“常温”、“室温”时,其温度可以是10-25℃。In this specification, when "normal temperature" and "room temperature" are used, the temperature may be 10-25°C.

<第一方面><first aspect>

本发明的第一方面提供一种标准参照胶材料,所述标准参照胶材料包括橡胶基材、乙烯-醋酸乙烯共聚物、硫化剂、环烷油以及轮胎粉;其中,The first aspect of the present invention provides a kind of standard reference rubber material, and described standard reference rubber material comprises rubber substrate, ethylene-vinyl acetate copolymer, vulcanizing agent, naphthenic oil and tire powder; Wherein,

以所述橡胶基材的总质量份数为100份计,所述乙烯-醋酸乙烯共聚物的含量为5~20份,所述硫化剂的含量为2~5份,所述环烷油的含量为15~30份,所述轮胎粉的含量为50~100份。Based on 100 parts by total mass of the rubber substrate, the content of the ethylene-vinyl acetate copolymer is 5-20 parts, the content of the vulcanizing agent is 2-5 parts, and the naphthenic oil The content is 15-30 parts, and the content of the tire powder is 50-100 parts.

本发明的标准参照胶材料的磨耗质量损失低,且相对扩展不确定度小,具备良好的磨耗测试均匀性以及长期、短期测试稳定性。具体而言:The standard reference rubber material of the present invention has low abrasion mass loss and small relative expansion uncertainty, and has good abrasion test uniformity and long-term and short-term test stability. in particular:

本发明的橡胶基材优选包括顺丁橡胶和天然橡胶;The rubber substrate of the present invention preferably comprises butadiene rubber and natural rubber;

本发明的发明人发现,天然橡胶具有优异的弹性、绝缘性、隔水性,但是由于其耐老化、耐候性能较差,通常需要与其他橡胶并以提高其使用性能。顺丁橡胶与天然橡胶相比具有优良的耐低温、耐磨性能,并且生热低,动态机械性能。天然橡胶与顺丁橡胶共混不仅能有效改善制品的老化和耐磨性能,并且能提升产品的耐低温效果。因此,本发明的橡胶基材优选使用顺丁橡胶和天然橡胶。The inventors of the present invention have found that natural rubber has excellent elasticity, insulation, and water barrier properties, but due to its poor aging resistance and weather resistance, it usually needs to be combined with other rubbers to improve its performance. Compared with natural rubber, butadiene rubber has excellent low temperature resistance, wear resistance, low heat generation, and dynamic mechanical properties. The blending of natural rubber and butadiene rubber can not only effectively improve the aging and wear resistance of products, but also improve the low temperature resistance of products. Therefore, it is preferable to use butadiene rubber and natural rubber as the rubber base material of the present invention.

优选地,以所述橡胶基材的总质量份数为100份计,所述顺丁橡胶的含量为40~60份,例如:42份、45份、48份、50份、52份、55份等;所述天然橡胶的含量为40~60份,例如:42份、45份、48份、50份、52份、55份等。本发明人发现,顺丁橡胶的含量为40~60份,天然橡胶的含量为40~60份时,顺丁橡胶和天然橡胶的功效均能得到最有效的发挥,适合作为本申请的橡胶基材使用。Preferably, based on 100 parts by mass of the rubber substrate, the content of the butadiene rubber is 40 to 60 parts, for example: 42 parts, 45 parts, 48 parts, 50 parts, 52 parts, 55 parts parts, etc.; the content of the natural rubber is 40-60 parts, for example: 42 parts, 45 parts, 48 parts, 50 parts, 52 parts, 55 parts, etc. The inventors have found that when the content of butadiene rubber is 40 to 60 parts and the content of natural rubber is 40 to 60 parts, the effects of both butadiene rubber and natural rubber can be brought into play most effectively, and are suitable as the rubber base of the present application. material use.

在本发明中,通过使用乙烯-醋酸乙烯共聚物来进一步提高顺丁橡胶和天然橡胶的粘结性和加工性,达到更好的热力学相容效果,从而获得性能优异的标准参照胶材料。In the present invention, the cohesiveness and processability of butadiene rubber and natural rubber are further improved by using ethylene-vinyl acetate copolymer to achieve a better thermodynamic compatibility effect, thereby obtaining a standard reference rubber material with excellent performance.

作为优选,以所述橡胶基材的总质量份数为100份计,所述乙烯-醋酸乙烯共聚物的含量为5~20份,例如:8份、10份、12份、15份、18份等;当乙烯-醋酸乙烯共聚物的含量为5~20份时,能够进一步有效提高顺丁橡胶、天然橡胶之间的粘结性和加工性。Preferably, based on 100 parts by mass of the rubber substrate, the content of the ethylene-vinyl acetate copolymer is 5 to 20 parts, for example: 8 parts, 10 parts, 12 parts, 15 parts, 18 parts parts, etc.; when the content of ethylene-vinyl acetate copolymer is 5 to 20 parts, the cohesiveness and processability between butadiene rubber and natural rubber can be further effectively improved.

在本发明中,通过使用硫化剂以获得硫化橡胶。对于硫化剂,本发明不作特别限定,可以是本领域常用的硫化剂。具体地,在本发明中,以所述橡胶基材的总质量份数为100份计,所述硫化剂的含量为2~5份,例如:2.5份、3份、3.5份、4份、4.5份等;当所述硫化剂的含量为2~5份时,更有利于获得所需的硫化橡胶。In the present invention, vulcanized rubber is obtained by using a vulcanizing agent. As for the vulcanizing agent, the present invention is not particularly limited, and it may be a vulcanizing agent commonly used in the art. Specifically, in the present invention, based on 100 parts by mass of the rubber substrate, the content of the vulcanizing agent is 2 to 5 parts, for example: 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, etc.; when the content of the vulcanizing agent is 2 to 5 parts, it is more beneficial to obtain the desired vulcanized rubber.

一般而言,硫化剂包括无机硫化剂和有机硫化剂。所述无机硫化剂包括硫黄、一氯化硫、硒、碲等。有机硫化剂包括含硫的促进剂(如促进剂TMTD)、有机过氧化物(如过氧化苯甲酰)、醌肟化合物、多硫聚合物、氨基甲酸乙酯、马来酰亚胺衍生物等。在本发明中,考虑到不引入其它杂质,优选使用硫磺作为硫化剂。Generally speaking, vulcanizing agents include inorganic vulcanizing agents and organic vulcanizing agents. The inorganic vulcanizing agent includes sulfur, sulfur monochloride, selenium, tellurium and the like. Organic vulcanizing agents include sulfur-containing accelerators (such as accelerator TMTD), organic peroxides (such as benzoyl peroxide), quinone oxime compounds, polysulfide polymers, urethanes, and maleimide derivatives wait. In the present invention, sulfur is preferably used as the vulcanizing agent in consideration of not introducing other impurities.

在本发明中,所述标准参照胶材料还含有环烷油,以所述橡胶基材的总质量份数为100份计,所述环烷油的含量为15~30份,例如:18份、20份、22份、25份、28份等。本发明的环烷油可以用于降低门尼粘度来提高模内流动性,从而更好的成型。当环烷油的含量为15~30份时,环烷油的功效能够获得最有效的发挥。In the present invention, the standard reference rubber material also contains naphthenic oil, based on 100 parts by mass of the rubber substrate, the content of the naphthenic oil is 15-30 parts, for example: 18 parts , 20, 22, 25, 28, etc. The naphthenic oil of the present invention can be used to reduce the Mooney viscosity to improve the fluidity in the mold, so as to form better. When the content of the naphthenic oil is 15-30 parts, the efficacy of the naphthenic oil can be most effectively exerted.

进一步,本发明的所述标准参照胶材料还含有轮胎粉,以所述橡胶基材的总质量份数为100份计,所述轮胎粉的含量为50~100份,例如:55份、60份、65份、70份、75份、80份、85份、90份、95份等。本发明通过使用轮胎粉来降低成本,当然加的越多成本就越低,但要确保橡胶的基础物性和成型性。另外,本发明的发明人发现,在本申请的标准参照胶材料中添加轮胎粉可以提升标准参照胶材料磨耗的均匀性以及耐老化性。当轮胎粉的含量为50~100份时,其功效能够最有效的发挥。Further, the standard reference rubber material of the present invention also contains tire powder, based on 100 parts by mass of the rubber substrate, the content of the tire powder is 50-100 parts, for example: 55 parts, 60 parts parts, 65 parts, 70 parts, 75 parts, 80 parts, 85 parts, 90 parts, 95 parts, etc. The present invention reduces cost by using tire powder, and of course the more the cost is lowered, but the basic physical properties and formability of the rubber must be ensured. In addition, the inventors of the present invention found that adding tire powder to the standard reference rubber material of the present application can improve the wear uniformity and aging resistance of the standard reference rubber material. When the content of tire powder is 50-100 parts, its efficacy can be brought into play most effectively.

在一些具体的实施方案中,所述标准参照胶材料还包含有补强剂、活性剂、防老剂、促进剂中的一种或两种以上的组合;优选地,以所述橡胶基材的总质量份数为100份计,所述补强剂的含量为50~75份,所述活性剂的含量为5~15份,所述促进剂的含量为2~5份,所述防老剂的含量为2~15份。In some specific embodiments, the standard reference rubber material also includes one or a combination of two or more of a reinforcing agent, an active agent, an anti-aging agent, and an accelerator; preferably, the rubber base material The total mass parts is 100 parts, the content of the reinforcing agent is 50-75 parts, the content of the active agent is 5-15 parts, the content of the accelerator is 2-5 parts, the anti-aging agent The content is 2 to 15 parts.

对于补强剂,本发明通过使用补强剂以起到填充增强的作用,可以提高橡胶的力学强度。进一步地,在本发明中,以所述橡胶基材的总质量份数为100份计,所述补强剂的含量为50~75份,例如:52份、55份、58份、60份、62份、65份、68份、70份、72份等。当所述补强剂的含量为50~75份时,能够有效提高橡胶的力学强度。具体地,所述补强剂包括碳酸钙和/或白炭黑。所述白炭黑又称沉淀法水合二氧化硅、白烟等。For the reinforcing agent, the present invention can improve the mechanical strength of the rubber by using the reinforcing agent to play the role of filling reinforcement. Further, in the present invention, based on 100 parts by mass of the rubber substrate, the content of the reinforcing agent is 50-75 parts, for example: 52 parts, 55 parts, 58 parts, 60 parts , 62, 65, 68, 70, 72, etc. When the content of the reinforcing agent is 50-75 parts, the mechanical strength of the rubber can be effectively improved. Specifically, the reinforcing agent includes calcium carbonate and/or white carbon black. The white carbon black is also called precipitated hydrated silica, white smoke and the like.

对于活性剂,其能够增加硫化促进剂的活性,提高胶料硫化速度和硫化效率,改善硫化胶性能的化学物质。进一步地,以所述橡胶基材的总质量份数为100份计,所述活性剂的含量为5~15份,例如:7份、9份、11份、13份等。当所述活性剂的含量为5~15份时,可以较好地发挥活性剂的作用,提高硫化活性,并提高硫化胶表面的光洁度和质感。As for the active agent, it can increase the activity of the vulcanization accelerator, increase the vulcanization speed and vulcanization efficiency of the rubber compound, and improve the performance of the vulcanized rubber. Further, based on 100 parts by mass of the total rubber substrate, the content of the active agent is 5-15 parts, for example: 7 parts, 9 parts, 11 parts, 13 parts, etc. When the content of the active agent is 5-15 parts, the effect of the active agent can be better exerted, the vulcanization activity can be improved, and the smoothness and texture of the surface of the vulcanized rubber can be improved.

具体地,所述活性剂包括一缩二乙二醇、聚乙二醇、硬脂酸、氧化镁、氧化锌中的一种或两种以上的组合。Specifically, the active agent includes one or a combination of two or more of diethylene glycol, polyethylene glycol, stearic acid, magnesium oxide, and zinc oxide.

对于防老剂,本发明采用防老剂是为了防止橡胶的老化,延长橡胶制品的使用寿命,使得本发明的标准参照胶材料具有优异的耐老化作用。进一步地,以所述橡胶基材的总质量份数为100份计,所述防老剂的含量为2~15份,例如:4份、5份、7份、9份、11份、13份等。当防老剂的含量为2~15份时,能够有效防止橡胶的老化,延长橡胶制品的使用寿命。For the anti-aging agent, the anti-aging agent used in the present invention is to prevent the aging of rubber and prolong the service life of rubber products, so that the standard reference rubber material of the present invention has excellent anti-aging effect. Further, based on 100 parts by mass of the total rubber substrate, the content of the anti-aging agent is 2 to 15 parts, for example: 4 parts, 5 parts, 7 parts, 9 parts, 11 parts, 13 parts wait. When the content of the anti-aging agent is 2-15 parts, it can effectively prevent the aging of rubber and prolong the service life of rubber products.

进一步,所述的防老剂包括2,2,4-三甲基-1,2-二氢化喹啉聚合体、1,2-双[β-(3,5-二叔丁基-4-羟基苯基)丙酰]肼、四[β-(3,5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯、4,4'-硫代双(6-叔丁基-3-甲基苯酚)、硫代二丙酸二硬脂醇酯和硫代二丙酸二月桂酯中的一种或两种以上的组合。Further, the anti-aging agent includes 2,2,4-trimethyl-1,2-dihydroquinoline polymer, 1,2-bis[β-(3,5-di-tert-butyl-4-hydroxy Phenyl)propionyl]hydrazine, tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate]pentaerythritol ester, 4,4'-thiobis(6-tert-butyl-3 -methylphenol), distearyl thiodipropionate and dilauryl thiodipropionate or a combination of two or more.

对于促进剂,其能够加速胶料的交联反应,缩短硫化时间、降低硫化温度、减少硫化剂用量的配合剂。进一步,在本发明中,以所述橡胶基材的总质量份数为100份计,所述促进剂的含量为2~5份,例如:2.5份、3份、3.5份、4份、4.5份等;当促进剂的含量为2~5份时,可以较高的发挥硫化促进作用,并保证焦烧安全性。For the accelerator, it can accelerate the cross-linking reaction of the rubber compound, shorten the vulcanization time, lower the vulcanization temperature, and reduce the amount of vulcanizing agent. Further, in the present invention, based on 100 parts by mass of the rubber substrate, the content of the accelerator is 2 to 5 parts, for example: 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts parts, etc.; when the content of the accelerator is 2-5 parts, it can play a higher role in vulcanization acceleration and ensure the safety of scorch.

具体地,所述促进剂包括N-环己基-2-苯并噻唑次磺酰胺、N-叔丁基-2-苯并噻唑次磺酰胺、2,2'-二硫化二苯并噻唑、一硫化四甲基秋兰姆、2-硫醇基苯并噻唑、二硫化四甲基秋兰姆中的一种或两种以上的组合。Specifically, the accelerator includes N-cyclohexyl-2-benzothiazole sulfenamide, N-tert-butyl-2-benzothiazole sulfenamide, 2,2'-dibenzothiazole disulfide, a One or a combination of two or more of tetramethylthiuram sulfide, 2-mercaptobenzothiazole, and tetramethylthiuram disulfide.

<第二方面><Second aspect>

本发明的第二方面提供一种根据本发明第一方面所述的标准参照胶材料的制备方法,其包括将标准参照胶材料的各组分混合的步骤。The second aspect of the present invention provides a method for preparing the standard reference adhesive material according to the first aspect of the present invention, which includes the step of mixing the components of the standard reference adhesive material.

在一些具体的实施方案中,所述制备方法包括:In some specific embodiments, the preparation method comprises:

将所述标准参照胶材料的各组分混合后进行混炼,得到混炼胶;mixing each component of the standard reference rubber material and then kneading to obtain a rubber mix;

对所述混炼胶进行炼片,得到混炼胶片;Carrying out sheet mixing to the mixed rubber to obtain a mixed rubber sheet;

对混炼胶片进行模压硫化成型,得到标准参照胶材料。The mixed rubber sheet is molded and vulcanized to obtain a standard reference rubber material.

具体地,所述制备方法包括以下步骤:Specifically, the preparation method comprises the following steps:

(1)将天然橡胶、顺丁橡胶、乙烯-醋酸乙烯共聚物、任选存在的其它添加剂以及硫化剂混炼后,得到混炼胶;(1) After mixing natural rubber, butadiene rubber, ethylene-vinyl acetate copolymer, other additives and vulcanizing agents optionally present, to obtain a rubber compound;

(2)将所述混炼胶进行炼片,得到混炼胶片;(2) refining the mixed rubber to obtain a mixed film;

(3)对所述混炼胶片进行模压硫化成型,得到标准参照胶材料。(3) Pressing and vulcanizing the mixed rubber sheet to obtain a standard reference rubber material.

具体地,所述标准参照胶材料的制备方法包括以下步骤:Specifically, the preparation method of the standard reference glue material comprises the following steps:

(1)密炼:将天然橡胶和顺丁橡胶在密炼机内进行塑炼,密炼温度控制在55-65℃范围内,时间3-5min,密炼机转速为60-70rpm;再加入乙烯-醋酸乙烯共聚物,密炼5-8min,密炼温度控制在75-90℃范围内;再分2-3次加入补强剂,每次加入的时间间隔1-3min,混炼5-10min至分散均匀;再加入轮胎粉,混炼3-5min后至分散均匀,密炼温度控制在90℃以内;再加入活性剂和防老剂,混炼2-3min;密炼温度控制在55-65℃范围内;再加入环烷油,混炼2-3min后加入硫化剂和促进剂,混炼2-3min后即可出料,得到混炼胶;(1) Internal mixing: plasticize natural rubber and butadiene rubber in an internal mixer, control the internal mixing temperature within the range of 55-65°C for 3-5 minutes, and the internal mixer speed at 60-70rpm; then add ethylene -Vinyl acetate copolymer, banburying for 5-8min, the banburying temperature is controlled within the range of 75-90°C; add the reinforcing agent in 2-3 times, the time interval between each addition is 1-3min, and kneading for 5-10min until the dispersion is uniform; then add tire powder, knead for 3-5 minutes until the dispersion is uniform, and control the mixing temperature within 90°C; then add active agent and anti-aging agent, knead for 2-3 minutes; control the mixing temperature at 55-65 within ℃ range; then add naphthenic oil, add vulcanizing agent and accelerator after mixing for 2-3 minutes, and discharge after mixing for 2-3 minutes to obtain mixed rubber;

(2)炼片:将混炼胶在开炼机上进行炼片,出片后停放24h,得到混炼胶片;(2) Sheet refining: the mixed rubber is refined on an open mill, and parked for 24 hours after the sheet is released to obtain a mixed film;

(3)模压成型:将混炼胶片放入平板硫化机中进行模压硫化成型,硫化温度为150-160℃,硫化时间为3-5min,得到辊筒式磨耗机法耐磨测试标准参照胶,样品尺寸为181mm×181mm×8mm。(3) Compression molding: put the mixed rubber sheet into a flat vulcanizer for molding vulcanization, the vulcanization temperature is 150-160°C, and the vulcanization time is 3-5min, and the standard reference rubber for the wear resistance test of the roller abrasion machine method is obtained. The sample size is 181mm x 181mm x 8mm.

进一步地,本发明还提供一种根据本发明所述的标准参照胶材料在辊筒式磨耗机法耐磨测试中的用途。Further, the present invention also provides a use of the standard reference rubber material according to the present invention in the wear resistance test of the roller abrasion machine method.

实施例Example

下面将结合实施例对本发明的实施方案进行详细描述,但是本领域技术人员将会理解,下列实施例仅用于说明本发明,而不应视为限定本发明的范围。实施例中未注明具体条件者,按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者,均为可以通过市购获得的常规产品。Embodiments of the present invention will be described in detail below in conjunction with examples, but those skilled in the art will understand that the following examples are only used to illustrate the present invention, and should not be considered as limiting the scope of the present invention. Those who do not indicate the specific conditions in the examples are carried out according to the conventional conditions or the conditions suggested by the manufacturer. The reagents or instruments used were not indicated by the manufacturer, and they were all commercially available conventional products.

实施例1Example 1

组成(质量比)为:天然橡胶55份、顺丁橡胶45份、乙烯-醋酸乙烯共聚物15份、白炭黑50份、碳酸钙10份、轮胎粉80份、环烷油15份、氧化锌5份、聚乙二醇1.0份、硬脂酸1.0份、2,2,4-三甲基-1,2-二氢化喹啉聚合体2.5份、2,2'-二硫化二苯并噻唑2份、二硫化四甲基秋兰姆0.5份、N-叔丁基-2-苯并噻唑次磺酰胺0.6份、硫磺3份。The composition (mass ratio) is: 55 parts of natural rubber, 45 parts of butadiene rubber, 15 parts of ethylene-vinyl acetate copolymer, 50 parts of white carbon black, 10 parts of calcium carbonate, 80 parts of tire powder, 15 parts of naphthenic oil, oxidized 5 parts of zinc, 1.0 parts of polyethylene glycol, 1.0 parts of stearic acid, 2.5 parts of 2,2,4-trimethyl-1,2-dihydroquinoline polymer, 2,2'-dibenzo disulfide 2 parts of thiazole, 0.5 part of tetramethylthiuram disulfide, 0.6 part of N-tert-butyl-2-benzothiazole sulfenamide, and 3 parts of sulfur.

制备方法为:The preparation method is:

(1)密炼:将天然橡胶和顺丁橡胶在密炼机内进行塑炼,密炼温度控制在60℃,时间5min,密炼机转速为60rpm;再加入乙烯-醋酸乙烯共聚物,密炼5min,密炼温度控制在90℃范围内;再分3次加入补强剂,每次加入的时间间隔2min,混炼8min至分散均匀;再加入轮胎粉,混炼5min后至分散均匀,密炼温度控制在90℃以内;再加入活性剂和防老剂,混炼3min;密炼温度控制在60℃范围内;再加入环烷油,混炼3min后加入硫化剂和促进剂,混炼2min后即可出料,得到混炼胶;(1) Internal mixing: plasticize the natural rubber and butadiene rubber in the internal mixer, control the internal mixing temperature at 60°C for 5 minutes, and the internal mixer speed at 60rpm; then add ethylene-vinyl acetate copolymer, internal mixing 5min, the banbury temperature is controlled within the range of 90°C; then add the reinforcing agent in 3 times, the time interval between each addition is 2min, and knead for 8min until the dispersion is uniform; then add the tire powder, knead for 5min until the dispersion is uniform, dense Control the refining temperature within 90°C; add active agent and anti-aging agent, and mix for 3 minutes; control the banburying temperature within the range of 60°C; add naphthenic oil, add vulcanizing agent and accelerator, and mix for 2 minutes After that, the material can be discharged to obtain the mixed rubber;

(2)炼片:将混炼胶在开炼机上进行炼片,出片后停放24h,得到混炼胶片;(2) Sheet refining: the mixed rubber is refined on an open mill, and parked for 24 hours after the sheet is released to obtain a mixed film;

(3)模压成型:将混炼胶片放入平板硫化机中进行模压硫化成型,硫化温度为155℃,硫化时间为5min,得到辊筒式磨耗机法耐磨测试标准参照胶,样品尺寸为181mm×181mm×8mm。(3) Compression molding: Put the mixed rubber sheet into a flat vulcanizer for compression vulcanization molding. The vulcanization temperature is 155°C and the vulcanization time is 5 minutes. The standard reference rubber for wear resistance test of the roller abrasion machine method is obtained, and the sample size is 181mm. ×181mm×8mm.

实施例2Example 2

组成(质量比)为:天然橡胶50份、顺丁橡胶50份、乙烯-醋酸乙烯共聚物15份、白炭黑50份、碳酸钙10份、轮胎粉85份、环烷油15份、氧化锌5份、聚乙二醇1.0份、硬脂酸1.0份、2,2,4-三甲基-1,2-二氢化喹啉聚合体2.5份、2,2'-二硫化二苯并噻唑2份、二硫化四甲基秋兰姆0.5份、N-叔丁基-2-苯并噻唑次磺酰胺0.6份、硫磺3份。The composition (mass ratio) is: 50 parts of natural rubber, 50 parts of butadiene rubber, 15 parts of ethylene-vinyl acetate copolymer, 50 parts of white carbon black, 10 parts of calcium carbonate, 85 parts of tire powder, 15 parts of naphthenic oil, oxidized 5 parts of zinc, 1.0 parts of polyethylene glycol, 1.0 parts of stearic acid, 2.5 parts of 2,2,4-trimethyl-1,2-dihydroquinoline polymer, 2,2'-dibenzo disulfide 2 parts of thiazole, 0.5 part of tetramethylthiuram disulfide, 0.6 part of N-tert-butyl-2-benzothiazole sulfenamide, and 3 parts of sulfur.

制备方法为:The preparation method is:

(1)密炼:将天然橡胶和顺丁橡胶在密炼机内进行塑炼,密炼温度控制在60℃,时间4min,密炼机转速为60rpm;再加入乙烯-醋酸乙烯共聚物,密炼5min,密炼温度控制在90℃范围内;再分3次加入补强剂,每次加入的时间间隔2min,混炼8min至分散均匀;再加入轮胎粉,混炼5min后至分散均匀,密炼温度控制在90℃以内;再加入活性剂和防老剂,混炼3min;密炼温度控制在60℃范围内;再加入环烷油,混炼3min后加入硫化剂和促进剂,混炼2min后即可出料,得到混炼胶;(1) Internal mixing: masticating natural rubber and butadiene rubber in an internal mixer, controlling the internal mixing temperature at 60°C for 4 minutes, and the internal mixer speed at 60rpm; then adding ethylene-vinyl acetate copolymer, internal mixing 5min, the banbury temperature is controlled within the range of 90°C; then add the reinforcing agent in 3 times, the time interval between each addition is 2min, and knead for 8min until the dispersion is uniform; then add the tire powder, knead for 5min until the dispersion is uniform, dense Control the refining temperature within 90°C; add active agent and anti-aging agent, and mix for 3 minutes; control the banburying temperature within the range of 60°C; add naphthenic oil, add vulcanizing agent and accelerator, and mix for 2 minutes After that, the material can be discharged to obtain the mixed rubber;

(2)炼片:将混炼胶在开炼机上进行炼片,出片后停放24h,得到混炼胶片;(2) Sheet refining: the mixed rubber is refined on an open mill, and parked for 24 hours after the sheet is released to obtain a mixed film;

(3)模压成型:将混炼胶片放入平板硫化机中进行模压硫化成型,硫化温度为155℃,硫化时间为5min,得到辊筒式磨耗机法耐磨测试标准参照胶,样品尺寸为181mm×181mm×8mm。(3) Compression molding: Put the mixed rubber sheet into a flat vulcanizer for compression vulcanization molding. The vulcanization temperature is 155°C and the vulcanization time is 5 minutes. The standard reference rubber for wear resistance test of the roller abrasion machine method is obtained, and the sample size is 181mm. ×181mm×8mm.

实施例3Example 3

组成(质量比)为:天然橡胶45份、顺丁橡胶55份、乙烯-醋酸乙烯共聚物17份、白炭黑50份、碳酸钙15份、轮胎粉85份、环烷油20份、氧化锌5份、聚乙二醇1.0份、硬脂酸1.0份、2,2,4-三甲基-1,2-二氢化喹啉聚合体2.5份、2,2'-二硫化二苯并噻唑2份、二硫化四甲基秋兰姆0.5份、N-叔丁基-2-苯并噻唑次磺酰胺0.6份、硫磺3份。The composition (mass ratio) is: 45 parts of natural rubber, 55 parts of butadiene rubber, 17 parts of ethylene-vinyl acetate copolymer, 50 parts of white carbon black, 15 parts of calcium carbonate, 85 parts of tire powder, 20 parts of naphthenic oil, oxidized 5 parts of zinc, 1.0 parts of polyethylene glycol, 1.0 parts of stearic acid, 2.5 parts of 2,2,4-trimethyl-1,2-dihydroquinoline polymer, 2,2'-dibenzo disulfide 2 parts of thiazole, 0.5 part of tetramethylthiuram disulfide, 0.6 part of N-tert-butyl-2-benzothiazole sulfenamide, and 3 parts of sulfur.

制备方法为:The preparation method is:

(1)密炼:将天然橡胶和顺丁橡胶在密炼机内进行塑炼,密炼温度控制在60℃范围内,时间3min,密炼机转速为60rpm;再加入乙烯-醋酸乙烯共聚物,密炼5min,密炼温度控制在90℃范围内;再分3次加入补强剂,每次加入的时间间隔2min,混炼10min至分散均匀;再加入轮胎粉,混炼5min后至分散均匀,密炼温度控制在90℃以内;再加入活性剂和防老剂,混炼3min;密炼温度控制在60℃范围内;再加入环烷油,混炼3min后加入硫化剂和促进剂,混炼2min后即可出料,得到混炼胶;(1) Internal mixing: masticate natural rubber and butadiene rubber in an internal mixer, control the internal mixing temperature within the range of 60°C for 3 minutes, and the internal mixer speed is 60rpm; then add ethylene-vinyl acetate copolymer, Mix for 5 minutes, and control the mixing temperature within the range of 90°C; then add the reinforcing agent in 3 times, with an interval of 2 minutes between each addition, and mix for 10 minutes until the dispersion is uniform; then add tire powder, and mix for 5 minutes until the dispersion is uniform , the mixing temperature is controlled within 90°C; add active agent and anti-aging agent, and mix for 3 minutes; control the banbury temperature within 60°C; add naphthenic oil, add vulcanizing agent and accelerator after mixing for 3 minutes, and mix After refining for 2 minutes, the material can be discharged to obtain the mixed rubber;

(2)炼片:将混炼胶在开炼机上进行炼片,出片后停放24h,得到混炼胶片;(2) Sheet refining: the mixed rubber is refined on an open mill, and parked for 24 hours after the sheet is released to obtain a mixed film;

(3)模压成型:将混炼胶片放入平板硫化机中进行模压硫化成型,硫化温度为155℃,硫化时间为4min,得到辊筒式磨耗机法耐磨测试标准参照胶,样品尺寸为181mm×181mm×8mm。(3) Compression molding: Put the mixed rubber sheet into a flat vulcanizer for compression vulcanization molding. The vulcanization temperature is 155°C and the vulcanization time is 4min. The standard reference rubber for wear resistance test of the roller abrasion machine method is obtained, and the sample size is 181mm. ×181mm×8mm.

性能测试Performance Testing

1、磨耗质量损失测试、硬度测试1. Abrasion mass loss test, hardness test

将实施例1~3制得的标准参照胶材料,按照GB/T 9867-2008中试样要求裁成直径为16mm的圆柱体样品,各取10个,磨耗质量损失采用GB/T9867-2008中规定的1号标准参照胶的试验方法(非旋转试样法)进行测试,硬度采用GB/T 3903.4-2017进行测试。其中磨耗试验机型号为高铁GT-7012-D,邵尔A型硬度计型号为上海六菱LX-A,各项性能指标如表1所示。Cut the standard reference rubber materials prepared in Examples 1 to 3 into cylindrical samples with a diameter of 16mm according to the sample requirements in GB/T 9867-2008. The specified No. 1 standard is tested with reference to the test method of rubber (non-rotating sample method), and the hardness is tested according to GB/T 3903.4-2017. Among them, the model of the abrasion testing machine is Gaotie GT-7012-D, and the model of the Shore A hardness tester is Shanghai Liuling LX-A. The performance indicators are shown in Table 1.

表1标准参照胶材料磨耗和硬度测试结果Table 1 Standard reference rubber material wear and hardness test results

Figure BDA0004172239990000111
Figure BDA0004172239990000111

从表1可以看出,本发明制备的辊筒式磨耗机法耐磨测试标准参照胶的磨耗质量损失范围为(180~200)mg,且邵氏硬度A也均满足GB/T 9867-2008要求,样品均具备良好的磨耗均匀性。采用实施例3配方和工艺制备样品磨耗质量损失更接近标准要求,且均匀性最佳。As can be seen from Table 1, the abrasion mass loss range of the roller abrasion machine method wear-resistant test standard reference rubber prepared by the present invention is (180-200) mg, and the Shore hardness A also meets GB/T 9867-2008 Requirements, the samples have good wear uniformity. Using the formula and process of Example 3 to prepare the sample wear mass loss is closer to the standard requirements, and the uniformity is the best.

2、稳定性测试2. Stability test

对本发明实施例3制备的样品进行了短期稳定性和长期稳定性(36个月)检验,测试方法按照GB/T 9867-2008中规定的1号标准参照胶的试验方法(非旋转试样法)进行测试,检验数据采用t检验方法进行数据统计处理,经检验结果统计表明t计算值均小于t临界值,说明该样品具备良好的短期稳定性和长期稳定性,测试结果于表2和表3所示。The sample prepared in Example 3 of the present invention has been carried out short-term stability and long-term stability (36 months) inspection, and test method is according to the test method (non-rotating sample method) of No. 1 standard reference glue specified in GB/T 9867-2008 ) was tested, and the test data was processed statistically using the t test method. The statistics of the test results showed that the calculated values of t were all less than the critical value of t, indicating that the sample had good short-term stability and long-term stability. The test results are shown in Table 2 and Table 2. 3.

表2短期稳定性检验结果Table 2 short-term stability test results

Figure BDA0004172239990000121
Figure BDA0004172239990000121

表3长期稳定性检验结果Table 3 long-term stability test result

Figure BDA0004172239990000131
Figure BDA0004172239990000131

3、应用测试3. Application testing

从本发明实施例3制备的样品和BAM标准胶中分别随机裁取10个单元样品,每个样品均采用GB/T 9867-2008中的方法A(非旋转试样法)进行测试,结果如下表4所示。10 unit samples were randomly cut from the sample prepared in Example 3 of the present invention and the BAM standard glue, and each sample was tested by method A (non-rotating sample method) in GB/T 9867-2008, and the results were as follows Table 4 shows.

表4比对测试结果Table 4 comparison test results

样品编号Sample serial number 实施例3样品Example 3 sample BAM标准胶BAM standard glue SAM-001SAM-001 202202 211211 SAM-002SAM-002 202202 196196 SAM-003SAM-003 207207 201201 SAM-004SAM-004 197197 195195 SAM-005SAM-005 206206 201201 SAM-006SAM-006 199199 210210 SAM-007SAM-007 201201 208208 SAM-008SAM-008 207207 192192 SAM-009SAM-009 196196 213213 SAM-010SAM-010 198198 200200 平均值(mg)mean (mg) 201201 203203 RSD(%)RSD(%) 2.032.03 3.633.63

由表4的比对测试结果表明,本发明制备样品的标准相对偏差要略低于BAM标准胶,且均匀性、稳定性良好,可以完全替代BAM标准胶。The comparative test results in Table 4 show that the standard relative deviation of the samples prepared by the present invention is slightly lower than that of the BAM standard glue, and the uniformity and stability are good, which can completely replace the BAM standard glue.

需要说明的是,尽管以具体实例介绍了本发明的技术方案,但本领域技术人员能够理解,本发明应不限于此。It should be noted that although the technical solutions of the present invention are described with specific examples, those skilled in the art can understand that the present invention should not be limited thereto.

以上已经描述了本发明的各实施例,上述说明是示例性的,并非穷尽性的,并且也不限于所披露的各实施例。在不偏离所说明的各实施例的范围和精神的情况下,对于本技术领域的普通技术人员来说许多修改和变更都是显而易见的。本文中所用术语的选择,旨在最好地解释各实施例的原理、实际应用或对市场中的技术改进,或者使本技术领域的其它普通技术人员能理解本文披露的各实施例。Having described various embodiments of the present invention, the foregoing description is exemplary, not exhaustive, and is not limited to the disclosed embodiments. Many modifications and alterations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The terminology used herein is chosen to best explain the principle of each embodiment, practical application or technical improvement in the market, or to enable other ordinary skilled in the art to understand each embodiment disclosed herein.

Claims (10)

1. A standard reference rubber material, which is characterized by comprising a rubber base material, an ethylene-vinyl acetate copolymer, a vulcanizing agent, naphthenic oil and tire powder; wherein,,
the total mass portion of the rubber base material is 100 portions, the content of the ethylene-vinyl acetate copolymer is 5-20 portions, the content of the vulcanizing agent is 2-5 portions, the content of the naphthenic oil is 15-30 portions, and the content of the tire powder is 50-100 portions.
2. The standard reference rubber material of claim 1, wherein the rubber substrate comprises butadiene rubber and natural rubber; preferably, the butadiene rubber is contained in an amount of 40 to 60 parts by weight and the natural rubber is contained in an amount of 40 to 60 parts by weight based on 100 parts by weight of the total rubber base material.
3. The standard reference glue material according to claim 1 or 2, further comprising one or a combination of two or more of a reinforcing agent, an active agent, an anti-aging agent, and an accelerator; preferably, the content of the reinforcing agent is 50-75 parts, the content of the active agent is 5-15 parts, the content of the accelerator is 2-5 parts, and the content of the anti-aging agent is 2-15 parts based on 100 parts by weight of the total mass of the rubber substrate.
4. A standard reference gel material according to claim 3, wherein the reinforcing agent comprises calcium carbonate and/or white carbon black.
5. The standard reference gel material of claim 3 or 4, wherein the active agent comprises one or a combination of more than two of diethylene glycol, polyethylene glycol, stearic acid, magnesium oxide, zinc oxide.
6. The standard reference gel material of any one of claims 3-5, wherein the anti-aging agent comprises one or a combination of two or more of 2, 4-trimethyl-1, 2-dihydroquinoline polymer, 1, 2-bis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine, tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] pentaerythritol ester, 4' -thiobis (6-tert-butyl-3-methylphenol), distearyl thiodipropionate, and dilauryl thiodipropionate.
7. The standard reference gel material of any one of claims 3-6, wherein the accelerator comprises one or a combination of two or more of N-cyclohexyl-2-benzothiazole sulfenamide, N-t-butyl-2-benzothiazole sulfenamide, 2' -dibenzothiazyl disulfide, tetramethylthiuram monosulfide, 2-mercaptobenzothiazole, tetramethylthiuram disulfide.
8. A method of preparing a standard reference gel material according to any one of claims 1 to 7, comprising the step of mixing the components of the standard reference gel material.
9. The method of manufacturing according to claim 8, characterized in that the method of manufacturing comprises:
mixing the components of the standard reference rubber material, and then mixing to obtain a mixed rubber;
refining the rubber compound to obtain a rubber compound;
and carrying out compression molding vulcanization molding on the mixed rubber sheet to obtain the standard reference rubber material.
10. Use of a standard reference gel material according to any one of claims 1-7 in a roller abrader wear test.
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