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A Study on the Synthesis and Tribological Characteristics of Calcium Sulfonate Grease with Improved Low-temperature Performance

저온 성능이 향상된 Calcium Sulfonate 그리스의 합성 및 트라이볼로지 특성 연구

  • Received : 2023.05.31
  • Accepted : 2023.07.06
  • Published : 2023.08.10

Abstract

We have investigated the performance improvement of grease by synthesizing calcium sulfonate grease as an alternative to lithium grease, which is widely used globally. Since the composition ratio of the grease, when manufactured, is usually 50% base oil and 50% thickener, using grease as a lubricant in a cryogenic environment is not encouraged due to its inferior low-temperature performance. In this study, we have synthesized three types of calcium sulfonate grease with paraffin oil and PAO-based base oil and thickener. Furthermore, lithium grease was synthesized via saponification with PAO-based base oil, lithium hydroxide, 12-hydroxystearic acid, and sebacic acid. We have measured low-temperature characteristics using a rheometer and low-temperature torque meter, and tribology characteristics were obtained using a four-ball lubricant tester and schwingung reibung verschleiß (SRV). As a result, the flow point of the calcium sulfonate grease synthesized with a PAO-based base oil and thickener was found to be -40℃, overcoming the existing calcium sulfonate grease's low-temperature limitation. Moreover, the synthesized calcium sulfonate grease showed low-temperature performance similar to that of lithium grease synthesized with PAO base oil, but superior anti-wear, extreme pressure, coefficient of friction, heat resistance, adhesion, and corrosion resistance. It is thus expected to commercially replace the existing lithium grease.

세계적으로 가장 많이 사용되고 있는 리튬 그리스의 대체 물질로서 calcium sulfonate 그리스를 합성하여 성능을 개선하였다. Calcium sulfonate 그리스의 저온성 문제를 해결하기 위하여 PAO (poly alpha olefin) 기반의 기유와 증주제를 도입하였다. 본 연구에서는 파라핀 오일과 PAO 기반의 기유와 증주제로 calcium sulfonate 그리스 3종을 합성하였으며, PAO 기반의 기유와 수산화 리튬, 12-hydroxy stearic acid, sebacic acid의 비누화 반응으로 리튬 그리스 1종을 합성하였다. 합성한 calcium sulfonate 그리스 3종과 리튬 그리스의 형태, 미세 구조 및 작용기는 SEM 및 FT-IR로 분석하였다. 저온 특성은 rheometer, low temperature torque로 측정하였고, 트라이볼로지 특성은 four ball lubricant tester, SRV로 측정하였다. 그 결과, PAO 기반의 기유와 증주제로 합성된 calcium sulfonate 그리스는 -40℃에서도 유동할 수 있었으며, 기존 calcium sulfonate 그리스의 저온 특성의 한계점을 극복하였다. 또한 합성한 calcium sulfonate 그리스는 PAO 기유로 합성된 리튬 그리스보다 우수한 내마모성, 내하중성, 마찰계수, 내열성, 점착성 및 내부식성을 보였으므로 상업적으로 기존의 리튬 그리스를 대체할 수 있을 것으로 기대된다.

Keywords

References

  1. D. F. Moore, Principles and Applications of Tribology: Pergamon International Library of Science, Technology, Engineering and Social Studies: International Series in Materials Science and Technology, 3-9, Elsevier Science, The Netherlands (2013).
  2. G. Straffelini, Friction and Wear: Methodologies for Design and Control, 21-112, Springer International Publishing, Germany (2015).
  3. A. R. Lansdown, Lubrication and Lubricant Selection, 127-133, Professional Engineering Publishing, UK (2004).
  4. C. E. Earle, Lubricating composition, US Patent 2,274,673 A (1942).
  5. C. K. Kim, Tribology, 92-95, Hyungseul Publishing, Korea (2006).
  6. B. B. Farrington and F. A. Leyda, Lithium grease, US Patent 2,504,672 A (1950).
  7. P. W. Brewster, A. G. Alexander, and T. O. Brown, Method of preparing high dropping point lithium complex soap greases, US Patent 5,391,309 A (1995).
  8. S. Kinnear and K. Kranz, An economic evaluation of 12-hydroxystearic acid and hydrogenated castor oil as raw materials for lithium soap lubricating grease, NLGI spokesman, 62, 13-19 (1998).
  9. Y. Kim, J. Lim, G. Park, and O. T. Lim, Electric vehicle market and battery related technology research trends, Transactions of the Korean Hydrogen and New Energy Society, 30, 362-368 (2019).
  10. TRADING ECONOMICS Home Page, https://tradingeconomics.com /commodity/ lithium (2022).
  11. R. Muir and W. Blokhuis, High performance calcium borate modified overbased calcium sulfonate complex greases, US Patent 4,560,489 A (1985).
  12. R. J. Muir, High performance calcium sulfonate complex lubricating grease, NLGI Spokesman, 52, 140-146 (1988).
  13. W. Macwood and R. Muir, Calcium sulfonate grease... One decade later, NLGI Spokesman, 63, 24-37 (1999).
  14. Y. Zhou, R. Bosman, and P. M Lugt, On the shear stability of dry and water-contaminated calcium sulfonate complex lubricating greases, Tribol. Trans., 62, 626-634 (2019). https://doi.org/10.1080/10402004.2019.1588445
  15. Z. Wang, Y. Xia, and Z. Liu, The rheological and tribological properties of calcium sulfonate complex greases, Friction, 3, 28-35 (2015). https://doi.org/10.1007/s40544-014-0063-1
  16. G. Ren, P. Zhang, W. Li, X. Fan, L. Zhang, H. Li, and M. Zhu, Probing the synergy of blended lithium complex soap and calcium sulfonate towards good lubrication and anti-corrosion performance, Tribology Lett., 68, 1-16 (2020). https://doi.org/10.1007/s11249-019-1243-y
  17. V. Bedekar, K. Mistry, R. Voothaluru, J. Qu, and J. Poplawsky, Atomistic investigation of calcium sulfonate and lithium complex grease tribofilms under severe sliding conditions, CIRP Annals, 71, 497-500 (2022). https://doi.org/10.1016/j.cirp.2022.04.062
  18. D. Sniderman, Calcium sulfonate complex greases, Tribol. Lubr. Technol., 72, 28-40 (2016).
  19. ASTM D217-21A, Standard Test Methods for Cone Penetration of Lubricating grease.
  20. ASTM D1478-20, Standard Test Method for Low-Temperature Torque of Ball Bearing grease.
  21. DIN 51810-1, Testing of lubricants - Determination of the shear viscosity of lubricating greases using the rotational viscometer - Part 1: Cone and plate measuring system.
  22. ASTM D2596-20, Standard Test Method for Measurement of Extreme-Pressure Properties of Lubricating grease (Four-Ball Method).
  23. ASTM D2266-01, Standard Test Method for Wear Preventive Characteristics of Lubricating grease (Four-Ball Method).
  24. ASTM D5707-19, Standard Test Method for Measuring Friction and Wear Properties of Lubricating grease Using a High-Frequency, Linear-Oscillation (SRV) Test Machine.
  25. ASTM D5706-16, Standard Test Method for Determining Extreme Pressure Properties of Lubricating greases Using a High-Frequency, Linear-Oscillation (SRV) Test Machine.
  26. ASTM D2265-22, Standard Test Method for Dropping Point of Lubricating grease Over Wide Temperature Range.
  27. ASTM D6184-17, Standard Test Method for Oil Separation from Lubricating grease (Conical Sieve Method).
  28. ASTM D4048-19A, Standard Test Method for Detection of Copper Corrosion from Lubricating grease.