系列新型有机硼酸酯添加剂的摩擦学性能及机理研究
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摘要
工业用润滑油的发展趋势是提高其热氧化稳定性,延长换油期,节能降耗,同时满足日益严格的环保要求。针对这些要求,对工业用油添加剂的研究也相应出现了新的发展方向,有机硼酸酯型极压抗磨添加剂的开发应用就是其中一个重要方面。本文根据不同的目的,把S、P、N等活性元素引入到有机硼酸酯中,设计并制备了八种新型有机硼酸酯添加剂,使用四球机考察了它们在不同基础油中的摩擦学性能;同时对一些添加剂的抗腐蚀性能、抗氧化性能、热稳定性等也进行了考察,结果发现其是一类多功能添加剂;试验中还采用SEM、EDS、三维非接触表面干涉光度仪、XPS等表面分析工具及大气压化学电离质谱等对各体系的摩擦作用机理也进行了研究。主要的研究内容和结论如下:
1、对现有两个常见添加剂的分子结构进行了改进,即把两个常用的摩擦活性官能团——硫代磷酸酯基团及荒氨酸基团引入到硼酸酯结构中,制得BDDP及BDTC添加剂,分别考察了二者在双酯及菜籽油中的摩擦学性能:
BDDP在双酯中的承载能力要稍好于ZDDP,抗磨性能稍差,但减摩性能要远好于ZDDP,热稳定性好于ZDDP,且在双酯中有一定的抗氧化作用,但抗氧化性能不如ZDDP。BDTC能明显提高菜籽油的承载能力,MoDTC却几乎没有多少极压性能;BDTC在低浓度时抗磨效果并不明显,随着加入量增加,显示了很好的抗磨效果,且在高负荷下其抗磨性能优于MoDTC;其减摩能力与MoDTC相当,但热稳定性要远远好于MoDTC,且在菜籽油中具有很强的抗氧化能力。
2、通过对硼酸酯结构中引入活性硫元素,设计、制备两种新型硼硫系载荷添加剂DSB及BXT,并将二者与硫化烯烃的摩擦学性能进行了对比研究:
研究表明,DSB在多元醇酯中的抗卡咬性能优于T321,但其抗烧结性能不如T321;高浓度高载荷的情况下DSB的抗磨能力更好;DSB在多元醇酯中的减摩性能优于T321;DSB试油的腐蚀等级较低,且展现了极优异的热稳定性和有一定的抗氧化作用。与硫化烯烃相比,BXT没有明显的气味,对铜片腐蚀程度小,且具有较高的热稳定性。承载能力与硫化烯烃几乎相当,并且在较低的浓度下展现出更好的减摩和抗磨性能。
3、通过在硼酸酯结构中引入杂环基团进行ZDDP替代物的研究:
研究表明,BTSB在菜籽油中展现出优异的承载性能,且优于ZDDP;其在低载荷下有更好的抗磨性能,且有极优异的减摩效果;BTSB能有效控制铜腐蚀,但热稳定性和抗氧化性不如ZDDP。BTBM在菜籽油中有很高的PB值,但其抗烧结性能却较差;BTBM在菜籽油中的抗磨性能较差,但拥有极好的减摩性能;BTBM作为腐蚀抑制剂,可以明显抑制活性元素对铜片的腐蚀作用。
4、基于电子共轭理论,设计并制备出具有高水解稳定性的有机苯硼酸酯添加剂PBDDP及PBDTC,分别考察了二者在双酯及菜籽油中的摩擦学性能及水解稳定性:
PBDDP在双酯中有较好的承载性能,且抗磨性能与ZDDP相当;具有极好的减摩性能,且好过普通含硫磷硼酸酯BDDP;PBDDP的热稳定性好于ZDDP,且抗氧化性也远好过ZDDP;PBDDP有优异的水解稳定性,且大大好过普通含硫磷硼酸酯BDDP。在菜籽油中PBDTC有较好的承载性能,且高载荷下抗磨性能优于MoDTC;PBDTC在菜籽油中同样表现出了极好的减摩性能,且优于BDTC,表明苯硼酸酯结构的引入可使减摩性能得以进一步提升;PBDTC的热稳定性大大高于MoDTC,但比普通含硫磷硼酸酯BDTC稍差;PBDDP在菜籽油中同样展现了极好的抗氧化作用,其抗氧化性能也超过了ZDDP,同时具有较高的水解稳定性。
5、考察了外加胺对硼酸酯水解稳定性及摩擦学性能的影响:
研究表明,不含活性元素的硼酸酯的承载能力有限;但当硼酸酯与有机胺形成外配位键后,却出现了明显的对抗作用;BN胺盐复合剂的加入可以明显提高液体石蜡的PB值,叔胺所形成的BN胺盐复合剂的抗卡咬性能最好,仲胺次之,而短碳链伯胺的抗卡咬性能也好过长碳链伯胺。低载荷下不含活性元素的硼酸酯具有一定的抗磨能力;两种B与N的结合方式均可起到协同抗磨作用,且同一种类的有机胺在两种结合方式下所起的抗磨能力大致相当,而所使用的伯胺的烷基链越长,其对改善硼酸酯的抗磨作用也就越大。有机胺的烷基碳链越长,复合剂在液体石蜡中的减摩性能越好,而由碳链最短的正丁胺所形成的复合剂甚至还出现了增摩现象。此外,由伯胺形成的复合剂其减摩性能最好,且远好于由仲胺及叔胺所形成的复合剂。
在两种加胺方式下,硼酸酯的水解稳定性均得到明显提高;在大部分情况下,BN外配位复合剂的水解稳定性优于BN胺盐复合剂。在两种结合方式下,胺的烷基链越长其水解稳定性越好。
6、苯硼酸酯衍生物的抗氧化性能及其与酚类抗氧剂的协同作用:
普通的苯硼酸酯(PBB)在菜籽油中有一定的抗氧化作用,但效果并不显著;含硫磷苯硼酸酯(PBDDP)的抗氧化性能特别好,且优于T501;PBB及PBDDP与T501均有很好的抗氧协同作用,但PBDDP与酚类抗氧剂的协同作用更突出;T501有很强的自由基捕获能力,进而起到抗氧化作用,但苯硼酸酯衍生物没有明显自由基捕获能力,说明后者不属于“捕获自由基”抗氧化机理;在氧化初期,苯硼酸酯的加入可以大大减少酚类抗氧剂的消耗量,这是其能与酚类抗氧剂起协同抗氧作用的主要原因。
7、通过对上述几种含活性元素硼酸酯的摩擦作用机理研究后发现:有机硼酸酯在摩擦过程中会发生分解,在金属表面形成由B2O3或部分硼酸酯组成的含硼吸附层,且吸附能力很强。这种吸附层可避免摩擦副间直接接触,从而减少摩擦与磨损。当添加剂中还同时含有活性元素如N、S、P时,金属表面可与其发生摩擦化学反应,可形成FeSO4、FeS、FePO4等无机反应膜或有机含氮金属络合物,这种由反应层及含硼吸附层所共同组成的复合边界润滑膜可起到更好的抗磨作用。
The developmental trends of industrial lubricants are to enhance the thermal oxidative stability, to prolong the using period of oil and to save energy. Based on the above trends, some new demands to additives for industrial lubricants come forth, for example, employing some new types of additives containing boron. In this dissertation, the active elements, such as S, P and N, were introduced into the organic borate esters for different purposes, and eight kinds of boric acid esters as lubricant additives were designed and prepared. Their tribological properties were explored in different base oils using four-ball machine, and their tribological action mechanisms were studied by virtue of SEM, EDS, XPS, three-dimensional non-contact surface profilometer and ACPI/MS, etc. The antioxidation properties, corrosion-inhibiting properties and thermal stability of some additives were also investigated. The main conclusions of the dissertation are shown as follows:
1. In order to improve the tribological properties of two additives used widespreadly, boron was introduced into their structures. Two additives (BDDP and BDTC) were synthesized and their tribological behaviors were compared with ZDDP and MoDTC in synthetic diester and rapeseed oil, respectively.
Compared with ZDDP, BDDP in synthetic diester shows better load-carrying and friction-reducing property. Meanwhile, BDDP can improve the antiwear performance of the base oil evidently. But its antiwear property is slightly worse than that of ZDDP. It possesses better thermal stability than ZDDP, and has high efficiency in controlling the oxidation of Esterex A51. Compared with MoDTC, BDTC possesses extraordinary EP property in rapeseed oil, and its antiwear property is better under relatively higher load. Moreover, its friction-reducing property is almost equivalent to that of MoDTC, and exhibits dramatically high thermal stability and antioxidation property.
2. Introduce the S element into borate ester and design new type of B-S load-carrying additive for replacing sulfurized olefins.
Compared with sulfurized olefins, DSB and BXT have no noticeable odor and little corrosion to copper, and exhibits better thermal stability and excellent antioxidant performance. The load-carrying properties of BXT and sulfurized olefins make a great difference. The former has higher pB value, and yet the latter has higher pD value. Moreover, the antiwear and friction-reducing capacity of DSB is better than that of sulfurized olefins under higher load. The load-carrying properties of BXT as additive in RSO are equivalent to sulfurized olefins (even better than the latter under lower concentration). Moreover, BXT possesses better friction-reducing and antiwear ability at relatively lower concentration.
3. Introduce heterocyclic groups into borate ester and seek the substitute for ZDDP.
BTSB possesses comprehensive tribological property and probably partially replaces ZDDP. Its EP property is dramatically better than that of ZDDP, and exhibits better friction-reducing property compared with ZDDP, but its antiwear property is slightly worse than that of ZDDP. It is effective in protecting copper from corrosion and its antioxidant property is almost equivalent to that of ZDDP. BTBM in RSO has very high PB value, but its antiweld property is bad. Compared with ZDDP, the antiwear performance of BTBM is worse, but possesses extreme excellent friction-reducing property. As corrosion inhibitor, BTBM can control the copper corrosion markedly.
4. Based on electronic conjugation theory, design and prepare borate esters additive with high hydrolytic stability.
Compared common borate ester, the two additives possesses higher hydrolytic stability. PBDDP in Esterex A51 possess better load-carrying and friction-reducing property compared with ZDDP. Its antiwear performance is equivalent to that of ZDDP, and exhibits better thermal stability and remarkable antioxidation performance. PBDTC as additive in RSO possess better load-carrying and friction-reducing property compared with MoDTC. Its antiwear performance excels that of MoDTC under high load. PBDDP exhibits rather better thermal stability and extreme excellent antioxidation performance, compared with MoDTC and ZDDP, respectively.
5. Study the effect of adding into amine on the tribological properties and hydrolytic stability of borate ester.
The loading-carry capability of borate ester containing no active element is relatively weak. When amine and borate ester form BN coordination bond, the loading-carry performance of the complexes become worse compared base oil. However, BN ammonium complex can improve the loading-carry performance of base oil. Under relatively low load, borate ester containing no active element has slightly antiwear property, and its antiwear performance can be improved when BN coordination bond or BN ammonium formed.
6. The antioxidation performance of phenyl-borate derivative and its synergistic effects with hydroxybenzene type antioxidant.
The phenyl-borate contain no active element in RSO has a few antioxidation properties. The phenyl-borate contain S, P possesses extreme excellent antioxidation property, even excel T501. Phenyl-borate derivatives have synergistic antioxidation effects with T501, especially for PBDDP and T501. Phenyl-borate derivatives can not remarkably rid the radical, which shows it do not accord with the antioxidation mechanism of“capture radical”. When the oxidation reaction occurs initially, Phenyl-borate derivatives can decrease the depletion of T501 greatly, which can answer for their synergistic effects.
7. When studying the tribological action mechanisms of some borate containing active element, it can be found that the organic borate ester can be decomposed when sliding, and the decomposed borate ester or B2O3 adsorbed on worn surface. The adsorption layer can prevent the direct contact between friction pairs, thereby reducing wear. When the additive contains active element, such as N, S and P, these element can react with metal surface to form inorganic reaction layer composed of FeSO4、FeS、FePO4, etc. Both of which contribute to the formation of complex boundary lubricating film and present better antiwear effects.
1、对现有两个常见添加剂的分子结构进行了改进,即把两个常用的摩擦活性官能团——硫代磷酸酯基团及荒氨酸基团引入到硼酸酯结构中,制得BDDP及BDTC添加剂,分别考察了二者在双酯及菜籽油中的摩擦学性能:
BDDP在双酯中的承载能力要稍好于ZDDP,抗磨性能稍差,但减摩性能要远好于ZDDP,热稳定性好于ZDDP,且在双酯中有一定的抗氧化作用,但抗氧化性能不如ZDDP。BDTC能明显提高菜籽油的承载能力,MoDTC却几乎没有多少极压性能;BDTC在低浓度时抗磨效果并不明显,随着加入量增加,显示了很好的抗磨效果,且在高负荷下其抗磨性能优于MoDTC;其减摩能力与MoDTC相当,但热稳定性要远远好于MoDTC,且在菜籽油中具有很强的抗氧化能力。
2、通过对硼酸酯结构中引入活性硫元素,设计、制备两种新型硼硫系载荷添加剂DSB及BXT,并将二者与硫化烯烃的摩擦学性能进行了对比研究:
研究表明,DSB在多元醇酯中的抗卡咬性能优于T321,但其抗烧结性能不如T321;高浓度高载荷的情况下DSB的抗磨能力更好;DSB在多元醇酯中的减摩性能优于T321;DSB试油的腐蚀等级较低,且展现了极优异的热稳定性和有一定的抗氧化作用。与硫化烯烃相比,BXT没有明显的气味,对铜片腐蚀程度小,且具有较高的热稳定性。承载能力与硫化烯烃几乎相当,并且在较低的浓度下展现出更好的减摩和抗磨性能。
3、通过在硼酸酯结构中引入杂环基团进行ZDDP替代物的研究:
研究表明,BTSB在菜籽油中展现出优异的承载性能,且优于ZDDP;其在低载荷下有更好的抗磨性能,且有极优异的减摩效果;BTSB能有效控制铜腐蚀,但热稳定性和抗氧化性不如ZDDP。BTBM在菜籽油中有很高的PB值,但其抗烧结性能却较差;BTBM在菜籽油中的抗磨性能较差,但拥有极好的减摩性能;BTBM作为腐蚀抑制剂,可以明显抑制活性元素对铜片的腐蚀作用。
4、基于电子共轭理论,设计并制备出具有高水解稳定性的有机苯硼酸酯添加剂PBDDP及PBDTC,分别考察了二者在双酯及菜籽油中的摩擦学性能及水解稳定性:
PBDDP在双酯中有较好的承载性能,且抗磨性能与ZDDP相当;具有极好的减摩性能,且好过普通含硫磷硼酸酯BDDP;PBDDP的热稳定性好于ZDDP,且抗氧化性也远好过ZDDP;PBDDP有优异的水解稳定性,且大大好过普通含硫磷硼酸酯BDDP。在菜籽油中PBDTC有较好的承载性能,且高载荷下抗磨性能优于MoDTC;PBDTC在菜籽油中同样表现出了极好的减摩性能,且优于BDTC,表明苯硼酸酯结构的引入可使减摩性能得以进一步提升;PBDTC的热稳定性大大高于MoDTC,但比普通含硫磷硼酸酯BDTC稍差;PBDDP在菜籽油中同样展现了极好的抗氧化作用,其抗氧化性能也超过了ZDDP,同时具有较高的水解稳定性。
5、考察了外加胺对硼酸酯水解稳定性及摩擦学性能的影响:
研究表明,不含活性元素的硼酸酯的承载能力有限;但当硼酸酯与有机胺形成外配位键后,却出现了明显的对抗作用;BN胺盐复合剂的加入可以明显提高液体石蜡的PB值,叔胺所形成的BN胺盐复合剂的抗卡咬性能最好,仲胺次之,而短碳链伯胺的抗卡咬性能也好过长碳链伯胺。低载荷下不含活性元素的硼酸酯具有一定的抗磨能力;两种B与N的结合方式均可起到协同抗磨作用,且同一种类的有机胺在两种结合方式下所起的抗磨能力大致相当,而所使用的伯胺的烷基链越长,其对改善硼酸酯的抗磨作用也就越大。有机胺的烷基碳链越长,复合剂在液体石蜡中的减摩性能越好,而由碳链最短的正丁胺所形成的复合剂甚至还出现了增摩现象。此外,由伯胺形成的复合剂其减摩性能最好,且远好于由仲胺及叔胺所形成的复合剂。
在两种加胺方式下,硼酸酯的水解稳定性均得到明显提高;在大部分情况下,BN外配位复合剂的水解稳定性优于BN胺盐复合剂。在两种结合方式下,胺的烷基链越长其水解稳定性越好。
6、苯硼酸酯衍生物的抗氧化性能及其与酚类抗氧剂的协同作用:
普通的苯硼酸酯(PBB)在菜籽油中有一定的抗氧化作用,但效果并不显著;含硫磷苯硼酸酯(PBDDP)的抗氧化性能特别好,且优于T501;PBB及PBDDP与T501均有很好的抗氧协同作用,但PBDDP与酚类抗氧剂的协同作用更突出;T501有很强的自由基捕获能力,进而起到抗氧化作用,但苯硼酸酯衍生物没有明显自由基捕获能力,说明后者不属于“捕获自由基”抗氧化机理;在氧化初期,苯硼酸酯的加入可以大大减少酚类抗氧剂的消耗量,这是其能与酚类抗氧剂起协同抗氧作用的主要原因。
7、通过对上述几种含活性元素硼酸酯的摩擦作用机理研究后发现:有机硼酸酯在摩擦过程中会发生分解,在金属表面形成由B2O3或部分硼酸酯组成的含硼吸附层,且吸附能力很强。这种吸附层可避免摩擦副间直接接触,从而减少摩擦与磨损。当添加剂中还同时含有活性元素如N、S、P时,金属表面可与其发生摩擦化学反应,可形成FeSO4、FeS、FePO4等无机反应膜或有机含氮金属络合物,这种由反应层及含硼吸附层所共同组成的复合边界润滑膜可起到更好的抗磨作用。
The developmental trends of industrial lubricants are to enhance the thermal oxidative stability, to prolong the using period of oil and to save energy. Based on the above trends, some new demands to additives for industrial lubricants come forth, for example, employing some new types of additives containing boron. In this dissertation, the active elements, such as S, P and N, were introduced into the organic borate esters for different purposes, and eight kinds of boric acid esters as lubricant additives were designed and prepared. Their tribological properties were explored in different base oils using four-ball machine, and their tribological action mechanisms were studied by virtue of SEM, EDS, XPS, three-dimensional non-contact surface profilometer and ACPI/MS, etc. The antioxidation properties, corrosion-inhibiting properties and thermal stability of some additives were also investigated. The main conclusions of the dissertation are shown as follows:
1. In order to improve the tribological properties of two additives used widespreadly, boron was introduced into their structures. Two additives (BDDP and BDTC) were synthesized and their tribological behaviors were compared with ZDDP and MoDTC in synthetic diester and rapeseed oil, respectively.
Compared with ZDDP, BDDP in synthetic diester shows better load-carrying and friction-reducing property. Meanwhile, BDDP can improve the antiwear performance of the base oil evidently. But its antiwear property is slightly worse than that of ZDDP. It possesses better thermal stability than ZDDP, and has high efficiency in controlling the oxidation of Esterex A51. Compared with MoDTC, BDTC possesses extraordinary EP property in rapeseed oil, and its antiwear property is better under relatively higher load. Moreover, its friction-reducing property is almost equivalent to that of MoDTC, and exhibits dramatically high thermal stability and antioxidation property.
2. Introduce the S element into borate ester and design new type of B-S load-carrying additive for replacing sulfurized olefins.
Compared with sulfurized olefins, DSB and BXT have no noticeable odor and little corrosion to copper, and exhibits better thermal stability and excellent antioxidant performance. The load-carrying properties of BXT and sulfurized olefins make a great difference. The former has higher pB value, and yet the latter has higher pD value. Moreover, the antiwear and friction-reducing capacity of DSB is better than that of sulfurized olefins under higher load. The load-carrying properties of BXT as additive in RSO are equivalent to sulfurized olefins (even better than the latter under lower concentration). Moreover, BXT possesses better friction-reducing and antiwear ability at relatively lower concentration.
3. Introduce heterocyclic groups into borate ester and seek the substitute for ZDDP.
BTSB possesses comprehensive tribological property and probably partially replaces ZDDP. Its EP property is dramatically better than that of ZDDP, and exhibits better friction-reducing property compared with ZDDP, but its antiwear property is slightly worse than that of ZDDP. It is effective in protecting copper from corrosion and its antioxidant property is almost equivalent to that of ZDDP. BTBM in RSO has very high PB value, but its antiweld property is bad. Compared with ZDDP, the antiwear performance of BTBM is worse, but possesses extreme excellent friction-reducing property. As corrosion inhibitor, BTBM can control the copper corrosion markedly.
4. Based on electronic conjugation theory, design and prepare borate esters additive with high hydrolytic stability.
Compared common borate ester, the two additives possesses higher hydrolytic stability. PBDDP in Esterex A51 possess better load-carrying and friction-reducing property compared with ZDDP. Its antiwear performance is equivalent to that of ZDDP, and exhibits better thermal stability and remarkable antioxidation performance. PBDTC as additive in RSO possess better load-carrying and friction-reducing property compared with MoDTC. Its antiwear performance excels that of MoDTC under high load. PBDDP exhibits rather better thermal stability and extreme excellent antioxidation performance, compared with MoDTC and ZDDP, respectively.
5. Study the effect of adding into amine on the tribological properties and hydrolytic stability of borate ester.
The loading-carry capability of borate ester containing no active element is relatively weak. When amine and borate ester form BN coordination bond, the loading-carry performance of the complexes become worse compared base oil. However, BN ammonium complex can improve the loading-carry performance of base oil. Under relatively low load, borate ester containing no active element has slightly antiwear property, and its antiwear performance can be improved when BN coordination bond or BN ammonium formed.
6. The antioxidation performance of phenyl-borate derivative and its synergistic effects with hydroxybenzene type antioxidant.
The phenyl-borate contain no active element in RSO has a few antioxidation properties. The phenyl-borate contain S, P possesses extreme excellent antioxidation property, even excel T501. Phenyl-borate derivatives have synergistic antioxidation effects with T501, especially for PBDDP and T501. Phenyl-borate derivatives can not remarkably rid the radical, which shows it do not accord with the antioxidation mechanism of“capture radical”. When the oxidation reaction occurs initially, Phenyl-borate derivatives can decrease the depletion of T501 greatly, which can answer for their synergistic effects.
7. When studying the tribological action mechanisms of some borate containing active element, it can be found that the organic borate ester can be decomposed when sliding, and the decomposed borate ester or B2O3 adsorbed on worn surface. The adsorption layer can prevent the direct contact between friction pairs, thereby reducing wear. When the additive contains active element, such as N, S and P, these element can react with metal surface to form inorganic reaction layer composed of FeSO4、FeS、FePO4, etc. Both of which contribute to the formation of complex boundary lubricating film and present better antiwear effects.
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