CN108164559A - 一种磺化二（2-乙基己基）-二硫代磷酸氧钼极压抗磨减摩剂以及含有该减摩剂的润滑脂 - Google Patents
一种磺化二（2-乙基己基）-二硫代磷酸氧钼极压抗磨减摩剂以及含有该减摩剂的润滑脂 Download PDFInfo
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- 239000002253 acid Substances 0.000 title claims description 18
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 title claims description 18
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- 239000007787 solid Substances 0.000 claims abstract description 8
- CYQAYERJWZKYML-UHFFFAOYSA-N phosphorus pentasulfide Chemical compound S1P(S2)(=S)SP3(=S)SP1(=S)SP2(=S)S3 CYQAYERJWZKYML-UHFFFAOYSA-N 0.000 claims abstract description 7
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- 238000000034 method Methods 0.000 claims description 2
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- 238000005245 sintering Methods 0.000 abstract description 2
- 150000000369 2-ethylhexanols Chemical class 0.000 abstract 1
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- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/128—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
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- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
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Abstract
本发明属于润滑脂领域，尤其涉及一种磺化二(2‑乙基己基)‑二硫代磷酸氧钼极压抗磨减摩剂以及含有该减摩剂的润滑脂。混合甲苯、正丁醇、2‑乙基己醇，加热至50℃，再加入五硫化二磷得灰绿色硫代磷酸透明液体备用；另用氢氧化钠溶液、三氧化钼反应，后用硫酸酸化至pH值为1.5左右，滴加硫代磷酸的甲苯溶液，90℃下反应至少4小时，冷却，抽滤，用甲醇充分洗涤，干燥后得黄褐色固体极压抗磨减摩剂。然后利用该极压抗磨减摩剂和其他组分制备润滑脂，使得该润滑脂烧结负荷PD值可以达到400kgf，比市场同类产品提高了20％‑30％；最大无卡咬负荷PB值121kgf，比市场同类产品提高了10‑15％。
Description
技术领域
本发明属于润滑脂领域，尤其涉及一种磺化二(2-乙基己基)-二硫代磷酸氧钼极压抗磨减摩剂以及含有该减摩剂的润滑脂。
背景技术
2017年中国润滑脂消费量突破40万吨，其中，工业高端设备用润滑脂占到85％。国内工业的发展对润滑脂的需求进一步增加。具有极压抗磨减摩高性能品质的润滑脂更加合适未来工业设备的需求。
绝大多数润滑脂主要用于润滑，为了解决设备在运转时产生离心的条件下，为减少设备摩擦磨损需要要的一种半固体润滑材料。与液体润滑剂相比，由于黏附性能良好，使用更加容易的原因，被广泛应用于钢铁、水泥、发电、炼化造纸和风电机组等行业中的机械设备当中。
目前普遍的现象是用国产极压复合锂基润滑脂极压抗磨减摩性能较差，造成设备频繁的停机、注脂，影响生产效率，提高生产成本，浪费能源，污染环境，更主要的是造成了设备的严重磨损，提高了设备的维护保养成本。部分企业用进口产品(例如美孚XHP222润滑脂)价格昂贵，成本费用太高。
发明内容
本发明针对上述的问题，本发明提供一种磺化二(2-乙基己基)-二硫代磷酸氧钼极压抗磨减摩剂及含有该减摩剂的润滑脂。
为了达到上述目的，本发明采用的技术方案为，本发明提供一种磺化二(2-乙基己基)-二硫代磷酸氧钼极压抗磨减摩剂，其结构式为：
其特征在于，具体制备方法为：在装有搅拌器、回流冷凝器和硫化氢吸收的三颈瓶中加入30ml甲苯，27ml正丁醇和2-乙基己醇混合醇，加热至50℃，一边搅拌另一边慢慢加入22.2g五硫化二磷，1h内加完，加完后控制温度70-90℃，反应直到固体五硫化二磷消失，反应过程中间歇性氮气吹扫，有利于副产物硫化氢的排出，从而提高目标产物硫代磷酸的收率。得灰绿色硫代磷酸透明液体备用；准备另外一套装有搅拌器、回流冷凝器和硫化氢吸收的三颈瓶，加入20g质量分数为40％的氢氧化钠溶液，然后加入三氧化钼到氢氧化钠溶液中，控制温度在35-45℃，搅拌溶解后用35％硫酸酸化至pH值为1.5左右，最后缓慢滴加硫代磷酸的甲苯溶液，加完后控制温度在90℃下反应至少4小时，冷却，抽滤，用甲醇充分洗涤，干燥后得黄褐色固体极压抗磨减摩剂，反应方程式如下：
6(RO)2PS2H+Na2MnO4→2(RO)2PS2OMoS+2[(RO)2PS]2S+6H2O+Na2SO4
其中R为2乙基己基，结构为：
作为优选，所述正丁醇和2-乙基己醇的摩尔比为0.5-1.05：1。
一种含有权利要求1所述磺化二(2-乙基己基)-二硫代磷酸氧钼极压抗磨减摩剂的润滑脂，其特征在于，按照重量份数包括以下成分：
作为优选，所述基础油为150BS。
作为优选，所述抗氧剂为二苯胺。
与现有技术相比，本发明的优点和积极效果在于：
1、本发明提供了一种磺化二(2-乙基己基)-二硫代磷酸氧钼极压抗磨减摩剂的合成，以及使用磺化二(2-乙基己基)-二硫代磷酸氧钼极压抗磨减摩剂调和的高品质高极压抗磨减摩性能的润滑脂，粘附性能良好，150BS粘度高，较好的成膜性能。优异的极压抗磨减摩性能，有着较低的成本优势，磺化二(2-乙基己基)-二硫代磷酸氧钼可以进一步提高润滑脂的极压抗磨性能，减少磨损、节约能源，提高对设备的保护，延长设备的使用寿命。使本发明提供的一种磺化二(2-乙基己基)-二硫代磷酸氧钼极压抗磨减摩剂以及含有该极压抗磨减摩剂的润滑脂烧结负荷PD值可以达到400kgf，比市场同类产品提高了20％-30％；最大无卡咬负荷PB值121kgf，比市场同类产品提高了10-15％。
具体实施方式
为了能够更清楚地理解本发明的上述目的、特征和优点，下面结合实施例对本发明做进一步说明。需要说明的是，在不冲突的情况下，本申请的实施例及实施例中的特征可以相互组合。
在下面的描述中阐述了很多具体细节以便于充分理解本发明，但是，本发明还可以采用不同于在此描述的其他方式来实施，因此，本发明并不限于下面公开说明书的具体实施例的限制。
实施例1(磺化二(2-乙基己基)-二硫代磷酸氧钼极压抗磨减摩剂的制备)
本发明提供一种磺化二(2-乙基己基)-二硫代磷酸氧钼极压抗磨减摩剂，结构式为：
具体制备方法为：在装有搅拌器、回流冷凝器和硫化氢吸收的三颈瓶中加入30ml甲苯，27ml正丁醇和2-乙基己醇混合醇，正丁醇和2-乙基己醇的摩尔比为0.5-1.05：1，加热至50℃，一边搅拌另一边慢慢加入22.2g五硫化二磷，1h内加完，加完后控制温度70-90℃，反应直到固体五硫化二磷消失，反应过程中间歇性氮气吹扫，有利于副产物硫化氢的排出，从而提高目标产物硫代磷酸的收率。得灰绿色硫代磷酸透明液体备用；准备另外一套装有搅拌器、回流冷凝器和硫化氢吸收的三颈瓶，加入20g质量分数为40％的氢氧化钠溶液，然后加入三氧化钼到氢氧化钠溶液中，控制温度在35-45℃，搅拌溶解后用35％硫酸酸化至pH值为1.5左右，最后缓慢滴加硫代磷酸的甲苯溶液，加完后控制温度在90℃下反应至少4小时，冷却，抽滤，用甲醇充分洗涤，干燥后得黄褐色固体极压抗磨减摩剂，反应方程式如下：
6(RO)2PS2H+Na2MnO4→2(RO)2PS2OMoS+2[(RO)2PS]2S+6H2O+Na2SO4
其中R为2乙基己基，结构为：
实施例2
一种加入上述磺化二(2-乙基己基)-二硫代磷酸氧钼极压抗磨减摩剂的高品质润滑脂，其组分及重量百分比如下：
本发明加入一种上述磺化二(2-乙基己基)-二硫代磷酸氧钼极压抗磨减摩剂的高品质润滑脂检测指标以及与市场在售高品质大品牌润滑脂数据对比如下：
数据说明：本发明润滑脂较同类产品锥入度大，可以提供更高粘附性能和极压抗磨性能；滴点比市场同类产品高，可以使用在更高的温度条件下；腐蚀性与市场同类产品无差别。铜网分油要比其他两种产品低，胶体安定性更好，使用过程中本发明产品油皂不容易分离。润滑减摩性能更好；极压性能与市场两种产品相比更高，说明本发明提供的一种上述磺化二(2-乙基己基)-二硫代磷酸氧钼极压抗磨减摩剂的高品质润滑脂有着更高的极压抗磨性能，提高了润滑脂的使用寿命，减少了对设备的磨损。
以上所述，仅是本发明的较佳实施例而已，并非是对本发明作其它形式的限制，任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更或改型为等同变化的等效实施例应用于其它领域，但是凡是未脱离本发明技术方案内容，依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与改型，仍属于本发明技术方案的保护范围。
Claims (5)
1.一种磺化二(2乙基己基)-二硫代磷酸氧钼极压抗磨减摩剂，该极压抗磨减摩剂的结构式为：
其特征在于，具体制备方法为：在装有搅拌器、回流冷凝器和硫化氢吸收的三颈瓶中加入30ml甲苯，27ml正丁醇和2-乙基己醇混合醇，加热至50℃，一边搅拌另一边慢慢加入22.2g五硫化二磷，1h内加完，加完后控制温度70-90℃，反应直到固体五硫化二磷消失，反应过程中间歇性氮气吹扫，得灰绿色硫代磷酸透明液体备用；准备另外一套装有搅拌器、回流冷凝器和硫化氢吸收的三颈瓶，加入20g质量分数为40％的氢氧化钠溶液，然后加入三氧化钼到氢氧化钠溶液中，控制温度在35-45℃，搅拌溶解后用35％硫酸酸化至pH值为1.5左右，最后缓慢滴加硫代磷酸的甲苯溶液，加完后控制温度在90℃下反应至少4小时，冷却，抽滤，用甲醇充分洗涤，干燥后得黄褐色固体极压抗磨减摩剂，反应方程式如下：
6(RO)2PS2H+Na2MnO4→2(RO)2PS2OMoS+2[(RO)2PS]2S+6H2O+Na2SC
其中R为2乙基己基，结构为
2.根据权利要求1所述一种磺化二(2乙基己基)-二硫代磷酸氧钼极压抗磨减摩剂，其特征在于：所述正丁醇和2-乙基己醇的摩尔比为0.5-1.05：1。
3.一种含有权利要求1所述磺化二(2-乙基己基)-二硫代磷酸氧钼极压抗磨减摩剂的润滑脂，其特征在于，按照重量份数包括以下成分：
4.根据权利要求2所述一种含有权利要求1所述磺化二(2-乙基己基)-二硫代磷酸氧钼极压抗磨减摩剂的润滑脂，其特征在于：所述基础油为150BS。
5.根据权利要求2所述一种含有权利要求1所述磺化二(2-乙基己基)-二硫代磷酸氧钼极压抗磨减摩剂的润滑脂，其特征在于：所述抗氧剂为二苯胺。
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