CN107445993A - 一种轮胎钢丝帘线抗氧增粘剂及其合成方法和应用 - Google Patents

一种轮胎钢丝帘线抗氧增粘剂及其合成方法和应用 Download PDF

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CN107445993A
CN107445993A CN201710654478.XA CN201710654478A CN107445993A CN 107445993 A CN107445993 A CN 107445993A CN 201710654478 A CN201710654478 A CN 201710654478A CN 107445993 A CN107445993 A CN 107445993A
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antioxygen
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methylol
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余金
余宪虎
余红杰
黄峰
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Abstract

本发明提供一种轮胎钢丝帘线抗氧增粘剂及其合成方法和应用，所述抗氧增粘剂为1‑羟甲基苯三唑磷酸酯乙二胺盐，以苯并三氮唑、甲醛为原料先合成得到1‑羟甲基苯并三氮唑，再与P2O5和乙二胺合成制得1‑羟甲基苯三唑磷酸酯乙二胺盐，再将其作为增粘剂和磷酸酯、润滑脂油性剂、表面活性剂、缓蚀剂、100#白油、动物油、油酸、三乙醇胺、磷酸酯铵盐、二缩三乙二醇、硅酸钠、水杨酸和氢氧化钠复配形成水基拉丝润滑剂。本发明提供的抗氧增粘剂能显著提高子午线轮胎镀铜钢丝的粘合力，添加了黄铜抗氧增粘剂的水基拉丝润滑剂能提高粘合力，同等结构的钢帘线粘合力比进口产品平均高20N以上。

Description

一种轮胎钢丝帘线抗氧增粘剂及其合成方法和应用
技术领域
本发明涉及增粘剂的合成和应用领域，具体是一种轮胎钢丝帘线抗氧增粘剂及其合成方法和应用。
背景技术
近年来，随着汽车制造业和交通运输业(尤其是高速公路)的迅猛发展，汽车的性能有了很大的提高，因而对轮胎的性能也有了更高的要求。传统的斜交轮胎已经不能满足当前汽车行业的发展，正逐步被性能优越的子午线轮胎所代替。骨架材料与橡胶的粘合质量是保证子午线轮胎使用性能的关键。尤其是发展中国家，超载现象严重，路面状况较差，气候差别大。当轮胎被划伤后，裂口逐渐扩展，空气、水和尘埃等杂质就有可能侵蚀裂口，加上轮胎在高速滚动中生热大，这些因素都将影响橡胶与骨架材料的粘接强度。子午线轮胎的生产实践表明，钢丝帘线与橡胶之间具有良好的初始粘合强度，但这并不能保证轮胎的使用性能与使用寿命，还要求在老化和腐蚀发生后橡胶与钢丝仍具有较高的粘合力保持率。用钢丝帘线增强的现代子午线轮胎的使用性能，在很大程度上取决于橡胶-帘线界面上的粘附强度和耐(高温、氧、水和盐)腐蚀的能力。为了提高对镀铜钢丝帘线的粘附强度，在胶料中加入一些专用助剂——增粘剂。
钢丝帘线的最后生产环节是在水箱拉丝机中完成的，半成品钢丝直接与水基钢丝拉拔润滑剂接触，并且是在钢丝变形的高温高压状态下接触，因此水基拉丝润滑剂对钢丝帘线的腐蚀性能直接影响到钢帘线的质量，进而会影响钢帘线与橡胶的粘合力，市场上没有直接可用的黄铜抗氧增粘剂。
发明内容
本发明的目的是针对现有市场的空缺，力求解决轮胎钢丝帘线抗氧增粘的问题，提供一种轮胎钢丝帘线抗氧增粘剂，用于钢帘线水箱拉丝润滑剂中，使其在钢帘线拉拔过程中吸附于钢帘线表面，从而防止钢帘线表面被氧化腐蚀来提高帘线与橡胶的粘合力。
本发明提供的技术方案：一种轮胎钢丝帘线抗氧增粘剂，所述抗氧增粘剂为1-羟甲基苯三唑磷酸酯乙二胺盐，其化学结构式是如下式所示：
一种轮胎钢丝帘线抗氧增粘剂的合成方法，包括如下步骤：
(1)在烧瓶中加入计量的苯并三氮唑、质量分数为37％的甲醛水溶液和水，加热搅拌使固体溶解后，于80℃恒温水浴槽内保温30min，冷却后抽滤即得粗品—1-羟甲基苯并三氮唑，将该粗品置于40℃真空干燥箱中放置24h备用；
(2)将步骤(1)所得的1-羟甲基苯并三氮唑和P2O5均分别溶于或分散于高分子烷烃或11#机油的溶剂中，在40℃下慢慢将P2O5滴加到1-羟甲基苯并三氮唑中，滴加完后升温至80℃，保温反应4h，然后加入其总重量的3％的水中，于85℃水解1h，得到1-羟甲基苯三唑磷酸酯，再将其与乙二胺在45℃以下反应30min，得目标产物—1-羟甲基苯三唑磷酸酯乙二胺盐。
进一步的，所述步骤(2)中1-羟甲基苯并三氮唑与P2O5摩尔比为1.70∶1.00。
进一步的，所述步骤(2)中1-羟甲基苯并三氮唑和P2O5溶于或分散于溶剂的比例均为：m(溶剂)：m(1-羟甲基苯并三氮唑或P2O5)＝3:1。
进一步的，所述步骤(2)中1-羟甲基苯三唑磷酸酯与乙二胺的质量比为1.2:1。
一种轮胎钢丝帘线抗氧增粘剂的应用，将所述抗氧增粘剂用于制备润滑剂，所述润滑剂由以下原料按照质量分数配置而成：润滑油性剂15～18％，MOA-4P磷酸酯6-9％，表面活性剂3～4％，抗氧增粘剂0.5～0.7％，B-VCI防锈剂1～3％，100号白油5～10％，动物油4～6％，油酸2～4％，三乙醇胺1～3％，磷酸酯胺盐3～5％，二缩三乙二醇1～3％，硅酸钠0.3～0.8％，水杨酸0.3～0.5％，氢氧化钠0.1～0.8％，余量为水，各组分的质量分数之和为100％。
进一步的，所述表面活性剂由吐温80和司盘80以质量比3:1的比例配置而成。
进一步的，所述润滑油性剂选自下式中的脂肪酸聚合物，
式中：R1代表C8烷基，m＝9-23。
进一步的，所述润滑油性剂按照以下步骤制得，(1)分别取二聚酸280.5克、司盘80252.8克和435克数均分子量为1000的聚乙二醇加到反应器内，在氮气保护下混合升温至90℃，加入6.7克对甲苯磺酸，120℃下保温1h，然后升温至180℃保温使之进行脱水反应，待油水分离器分出水量达到12克及以上时终止反应；
(2)将步骤(1)所得的产物减压抽滤，再蒸发浓缩得到所述的润滑油性剂。
本发明中抗氧增粘剂和润滑油性剂在实验室通过化学合成方式制得，其他原料均通过购买得到。
本发明的有益效果：(1)本发明合成一种新型的黄铜抗氧增粘剂—1-羟甲基苯三唑磷酸酯乙二胺盐，并将它添加到水基拉丝润滑剂中，利用其对黄铜反应活性高的特点，在钢丝高温高压变形产生新鲜表面的瞬间，瞬时吸附在新鲜表面，防止表面被氧化腐蚀来提高帘线与橡胶的粘合力。工业应用证明，添加了黄铜抗氧增粘剂的水基拉丝润滑剂能显著提高粘合力，同等结构的钢帘线粘合力比进口产品平均高20N以上。
(2)本发明采用抗氧增粘剂、润滑油性剂和其他原料复配形成的水基拉丝润滑剂，具有生物降解性好、润滑冷却效果优良、不燃、易清洗和成本低廉等特点。抗氧增粘剂用于子午线轮胎钢丝帘线表面抗氧化、增加钢帘线与轮胎橡胶的粘合力，润滑油性剂可自乳化，能减少润滑剂中表面活性剂的用量。
(3)司盘80和吐温80为分子结构为多分支的表面活性剂，具有一定的界面吸附成膜的特性，容易在固液界面生成润滑膜；同时，二者分别为亲油性和亲水性表面活性剂，可以在油水界面上吸附，参与液液界面膜的形成，将两者复配形成功能效果更好的乳化剂。所述MOA-4P磷酸酯用作抗磨剂，增加润滑剂的使用寿命，三乙醇胺用于润滑油的抗腐蚀添加剂，用作防锈剂，磷酸酯胺盐用作极压剂，在高温下与金属表面形成化学润滑膜，二缩三乙二醇用作偶联剂，延缓老化，硅酸钠用作阻垢剂，水杨酸用作杀菌剂，氢氧化钠用于pH调节，将各种功能效果好的原料复配形成润滑剂，具有超级润滑、减磨、抗极压，易被微生物降解，有利于环境的保护。
附图说明
图1是本发明的抗氧增粘剂的化学结构式；
图2是本发明合成抗氧增粘剂的反应线路图；
图3是本发明中润滑油性剂的化学结构式；
图4是本发明合成润滑油性剂的的反应线路图；
具体实施方式
下面结合具体实施例对本发明做进一步的说明。
抗氧增粘剂的合成方法：(1)在烧瓶中加入11.9g(0.1mol)苯并三氮唑、10mL的质量分数为37％的甲醛水溶液和10mL水，加热搅拌使固体溶解后，于80℃恒温水浴槽内保温30min，冷却后抽滤即得粗品—1-羟甲基苯并三氮唑，将该粗品置于40℃真空干燥箱中放置24h备用；
(2)将步骤(1)所得的1-羟甲基苯并三氮唑和P2O5均分别溶于或分散于高分子烷烃或11#机油的溶剂中，在40℃下慢慢将P2O5滴加到1-羟甲基苯并三氮唑中，滴加完后升温至80℃，保温反应4h，然后加入其总重量的3％的水中，于85℃水解1h，得到1-羟甲基苯三唑磷酸酯，再将其与乙二胺在45℃以下反应30min，得目标产物—1-羟甲基苯三唑磷酸酯乙二胺盐。所述步骤(2)中1-羟甲基苯并三氮唑与P2O5摩尔比为1.70∶1.00。
所述步骤(2)中1-羟甲基苯并三氮唑与P2O5摩尔比为1.70∶1.00。
所述步骤(2)中1-羟甲基苯并三氮唑和P2O5溶于或分散于溶剂的比例均为：m(溶剂)：m(1-羟甲基苯并三氮唑或P2O5)＝3:1。
所述步骤(2)中1-羟甲基苯三唑磷酸酯与乙二胺的质量比为1.2:1。
所述抗氧增粘剂为1-羟甲基苯三唑磷酸酯乙二胺盐，其化学结构式是如下式所示：
所述润滑油性剂按照以下步骤制得，(1)分别取二聚酸280.5克、司盘80 252.8克和435克数均分子量为1000的聚乙二醇加到反应器内，在氮气保护下混合升温至90℃，加入6.7克对甲苯磺酸，120℃下保温1h，然后升温至180℃保温使之进行脱水反应，待油水分离器分出水量达到12克及以上时终止反应；
(2)将步骤(1)所得的产物减压抽滤，再蒸发浓缩得到所述的润滑油性剂。
所述润滑油性剂选自下式中的脂肪酸聚合物，
式中：R1代表C8烷基；m＝9-23。
以下实施例中均采用上述制备方法得到的抗氧增粘剂和润滑油性剂。
实施例一
将所述抗氧增粘剂用于制备润滑剂，所述润滑剂由以下原料按照质量分数配置而成：润滑油性剂16％，MOA-4P磷酸酯7％，表面活性剂3.2％，抗氧增粘剂0.55％，B-VCI防锈剂1.5％，100号白油7％，动物油4.5％，油酸2.5％，三乙醇胺1.5％，磷酸酯胺盐4％，二缩三乙二醇1％，硅酸钠0.6％，水杨酸0.3％，氢氧化钠0.1％，余量为水，各组分的质量分数之和为100％。
实施例二
将所述抗氧增粘剂用于制备润滑剂，所述润滑剂由以下原料按照质量分数配置而成：润滑油性剂15％，MOA-4P磷酸酯6％，表面活性剂3％，抗氧增粘剂0.6％，B-VCI防锈剂2％，100号白油6％，动物油5％，油酸3％，三乙醇胺2％，磷酸酯胺盐5％，二缩三乙二醇1.5％，硅酸钠0.5％，水杨酸0.5％，氢氧化钠0.2％，余量为水，各组分的质量分数之和为100％。
实施例三
将所述抗氧增粘剂用于制备润滑剂，所述润滑剂由以下原料按照质量分数配置而成：润滑油性剂17％，MOA-4P磷酸酯8％，表面活性剂3.5％，抗氧增粘剂0.5％，B-VCI防锈剂1％，100号白油5％，动物油4％，油酸2％，三乙醇胺1％，磷酸酯胺盐3.5％，二缩三乙二醇2％，硅酸钠0.3％，水杨酸0.4％，氢氧化钠0.5％，余量为水，各组分的质量分数之和为100％。
所述润滑剂配制方法：按照上述实施例的组分配比，将润滑油性剂，MOA-4P，表面活性剂，增粘剂，100号白油，动物油，油酸，三乙醇胺，磷酸酯胺盐，二缩三乙二醇加入乳化反应罐，于80℃搅拌混合30min，加入计量的80℃的去离子水，乳化搅拌30min左右，加入硅酸钠，水杨酸，B-VCI防锈剂，用30％氢氧化钠调节pH为8.5±0.3，冷却后过滤包装。
将制备得到的抗氧增粘剂添加进去，测量钢帘线粘合力数据与未添加本发明的抗氧增粘剂的对照样进行分析，结果如表1所示。
表1钢帘线粘合力数据
由表1可知，在未添加黄铜抗氧增粘剂的条件下，帘线粘合力不能满足生产需求，添加之后，粘合力和附胶率有了明显提高。试验证明成果设计合成的黄铜抗氧增粘剂对改善帘线与橡胶的粘合力有明显的效果。
以上所述仅为本发明的具体实施方案的详细描述，并不以此限制本发明，凡在本发明的设计思路上所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (9)

1.一种轮胎钢丝帘线抗氧增粘剂，其特征在于：所述抗氧增粘剂为1-羟甲基苯三唑磷酸酯乙二胺盐，其化学结构式是如下式所示：
2.制备如权利要求1所述的轮胎钢丝帘线抗氧增粘剂的合成方法，其特征在于包括如下步骤：
(1)在烧瓶中加入计量的苯并三氮唑、质量分数为37％的甲醛水溶液和水，加热搅拌使固体溶解后，于80℃恒温水浴槽内保温30min，冷却后抽滤即得粗品—1-羟甲基苯并三氮唑，将该粗品置于40℃真空干燥箱中放置24h备用；
(2)将步骤(1)所得的1-羟甲基苯并三氮唑和P2O5均分别溶于或分散于高分子烷烃或11#机油的溶剂中，在40℃下慢慢将P2O5滴加到1-羟甲基苯并三氮唑中，滴加完后升温至80℃，保温反应4h，然后加入其总重量的3％的水中，于85℃水解1h，得到1-羟甲基苯三唑磷酸酯，再将其与乙二胺在45℃以下反应30min，得目标产物—1-羟甲基苯三唑磷酸酯乙二胺盐。
3.根据权利要求2所述的轮胎钢丝帘线抗氧增粘剂的合成方法，其特征在于：所述步骤(2)中1-羟甲基苯并三氮唑与P2O5摩尔比为1.70∶1.00。
4.根据权利要求3所述的轮胎钢丝帘线抗氧增粘剂的合成方法，其特征在于：所述步骤(2)中1-羟甲基苯并三氮唑和P2O5溶于或分散于溶剂的比例均为：m(溶剂)：m(1-羟甲基苯并三氮唑或P2O5)＝3:1。
5.根据权利要求2所述的轮胎钢丝帘线抗氧增粘剂的合成方法，其特征在于：所述步骤(2)中1-羟甲基苯三唑磷酸酯与乙二胺加入的质量比为1.2:1。
6.根据权利要求1或2所述的轮胎钢丝帘线抗氧增粘剂的应用，其特征在于：将所述抗氧增粘剂用于制备润滑剂，所述润滑剂由以下原料按照质量分数配置而成：润滑油性剂15～18％，MOA-4P磷酸酯6～9％，表面活性剂3～4％，抗氧增粘剂0.5～0.7％，B-VCI防锈剂1～3％，100号白油5～10％，动物油4～6％，油酸2～4％，三乙醇胺1～3％，磷酸酯胺盐3～5％，二缩三乙二醇1～3％，硅酸钠0.3～0.8％，水杨酸0.3～0.5％，氢氧化钠0.1～0.8％，余量为水，各组分的质量分数之和为100％。
7.根据权利要求6所述的轮胎钢丝帘线抗氧增粘剂的应用，其特征在于：所述表面活性剂由吐温80和司盘80以质量比3:1的比例配置而成。
8.根据权利要求6所述的轮胎钢丝帘线抗氧增粘剂的应用，其特征在于：所述润滑油性剂选自下式中的脂肪酸聚合物，
式中：R1代表C8烷基，m＝9-23。
9.根据权利要求8所述的轮胎钢丝帘线抗氧增粘剂的应用，其特征在于：所述润滑油性剂按照以下步骤制得，(1)分别取二聚酸280.5克、司盘80 252.8克和435克的数均分子量为1000的聚乙二醇加到反应器内，在氮气保护下混合升温至90℃，加入6.7克对甲苯磺酸，120℃下保温1h，然后升温至180℃保温使之进行脱水反应，待油水分离器分出水量达到12克及以上时终止反应；
(2)将步骤(1)所得的产物减压抽滤，再蒸发浓缩得到所述的润滑油性剂。
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