Available online at http://ijcpe.uobaghdad.edu.iq and www.iasj.net Iraqi Journal of Chemical and Petroleum Engineering Vol.23 No.1 (March 2022) 1 – 7 EISSN: 2618-0707, PISSN: 1997-4884 Corresponding Authors: Name: Mustafa Raad Fahad, Email: mustafa.r.fahad@gmail.com , Name: Basma Abbas Abdulmajeed, Email: basma1957@yahoo.com IJCPE is licensed under a Creative Commons Attribution-NonCommercial 4.0 International License. Effect of Modified Hybrid Nanoparticles on the Properties of Base Oil Mustafa Raad Fahad a and Basma Abbas Abdulmajeed b a Petroleum Research and Development Center PRDC, Ministry of Oil, Baghdad, Iraq b Chemical Engineering Department, University of Baghdad, Baghdad, Iraq Abstract Nanomaterials have an excellent potential for improving the rheological and tribological properties of lubricating oil. In this study, oleic acid was used to surface-modify nanoparticles to enhance the dispersion and stability of Nanofluid. The surface modification was conducted for inorganic nanoparticles (NPs) TiO₂ and CuO with oleic acid (OA) surfactant, where oleic acid could render the surface of TiO2-CuO hydrophobic. Fourier transform infrared spectroscopy (FTIR), and Scanning electron microscopy (SEM) were used to characterize the surface modification of NPs. The main objective of this study was to investigate the influence of adding modified TiO₂ -CuO NPs with weight ratio 1:1 on thermal-physical properties such as kinematic viscosity, viscosity index (VI), pour point, and flash point of Iraqi base oil (40 stock) and nano-lubricating oil. The kinematic viscosity of base oil at 40 °C and 100°C increased with high concentrations of modified TiO₂ -CuO NPs. The highest value of VI of base oil 40 stock at 0.8 wt. % of modified TiO₂ -CuO NPs was 108.5. The results showed that the flashpoint value increased with the increased concentration of modified TiO₂ -CuO NPs of base oil 40, where the highest value was 220 °C. The pour point of nano lubricating oil base with 0.8 wt. % of modified TiO₂ -CuO NPs showed decreasing from -12 °C to -15 °C of base oil 40. Keywords: Oil 40 stock, Lubricating Oil, Nanoparticles, Oleic acid, Viscosity Index, Flash Point Received on 30/01/2022, Accepted on 05/03/2022, published on 30/03/2022 https://doi.org/10.31699/IJCPE.2022.1.1 1- Introduction The word (lubricating oil) relates to various products of hundreds of specific chemicals and additives and can be either mineral or synthetically. Lubricating oil contains 80-90% of hydrocarbon petroleum distillates and 10-20% additives. Mineral oil is more commonly used than synthetic oil [1]. Improving environmental protection, durability, and fuel efficiency is a major focus in the automotive industry. New techniques are being developed, such as introducing new, less harmful materials and the controlled combustion of fuels. which manages the environmental harms caused by vehicles. The lubricant plays a crucial role in friction and wear reduction and is sometimes needed to perform other functions. It is useful as a heat-transfer medium in many applications. It eliminates heat from "hot spots" in sliding parts, thereby avoiding overheating losses such as cooling engine pistons, power-transmission systems, and metal- working operations [2]. Several different forms of lubricants are used in machinery. These lubricants are used in gasoline and diesel engines containing various forms of chemical materials known as "additives", which are used to enhance the properties of these lubricants to give the best-operating conditions instance, the efficiency of lubricating oil in engines. In a lubricating device, where total isolation between two surfaces is achieved, the lubricant's viscosity becomes the parameter that governs the adhesion, abrasion, corrosion, and fatigue that cause various processes [3]. The base oil (natural and synthetic) typically cannot reach the required high-performance specifications without the use of advanced additives cannot reach the properties of high-performance lubricating oil without the aid of advanced additive technology [4]. The additives are the chemical component used to gain desirable base stocks that enhance existing properties. The properties that are deemed important are: viscosity, viscosity change with temperature (viscosity index), pour point, oxidation resistance, flash point, and boiling temperature [5], [6]. Organo-molybdenum compounds and organo-zinc phosphate compounds are examples of such additives. Whereas these additives are useful as modifiers of friction and wear, they may also have several drawbacks such as poor oil solubility, copper, lead to corrosion of the finished lubricant, increased sulfur, and phosphorus components level in the final lubricating oil. As a result, new types of additives can be used as replacements for traditional lubricant additives and improve the overall lubricant performance while being more environmentally friendly and compatible with pollution control devices used in automotive and diesel engines must be developed [7], [8]. http://ijcpe.uobaghdad.edu.iq/ http://www.iasj.net/ mailto:mustafa.r.fahad@gmail.com mailto:basma1957@yahoo.com http://creativecommons.org/licenses/by-nc/4.0/ https://doi.org/10.31699/IJCPE.2022.1.1 M. R.Fahad and B. A. Abdulmajeed / Iraqi Journal of Chemical and Petroleum Engineering 23,1 (2022) 1 - 7 2 In recent years, the use of nanoparticles as lubricant additives has grown steadily. Many researchers showed that a nanoparticle-containing lubricant formulation, also known as a nano lubricant, reduced friction and wear. Nano lubricants have the potential to solve many of the problems of traditional lubricants. The main benefits of using nano lubricants are that they are insensitive to temperature and have as there are fewer tribo-chemical reactions than traditional additives [8]–[11]. Suspended NPs make nanofluids (NFs) with average sizes of less than 100 nm in standard fluids like water, oil, and ethylene glycol. When dispersed homogenously and stably in fluids, a very small amount of nanoparticles will provide important changes in the thermal properties of the base fluid [12], [13]. Nanomaterials (NMs) are typically scattered in liquids at low concentrations to produce NFs. Higher concentrations of nanoparticles in liquid can cause sedimentation because of their poor stability in fluids. NMs are typically scattered in liquids at low concentrations to create nanofluids. Higher concentrations of NPs in the fluid can produce sedimentation because of their low stability in fluids. Metal oxides like CuO, TiO2, Al2O3, ZnO, MgO, and SiC are highly thermal conductivity nanoparticles.[14], [15]. In comparison to mono nanofluids, hybrid NFs are expected to replace basic nanofluids for various reasons, such as a larger absorption range, lower extinction, high thermal conductivity, and low frictional losses[16]. The potential for more progress in thermal conductivity and thermophysical properties of hybrid nanofluids compared to traditional nanofluids is one of several reasons why researchers were led to the use and analysis of these types of nanofluids [17]. Several study results have shown that lubricating oil formulations containing nanoparticles, also known as nano-lubricants, decrease friction and wear. Nano lubricants have always had the potential to solve many of the issues associated with traditional lubricants [9], [10]. In the current study, surface modification of inorganic nanoparticles work as an additive in organic liquid using an oleic acid surfactant to enhance the stability of nano- lubricating oil and Improve the rheology and tribology properties of two types of Iraqi base oil (40 stock) by using modified hybrid TiO2-CuO NPs 2- Experimental Work 2.1. Materials In this work, Nano copper oxide CuO and Nano Titanium (IV) oxide TiO2 were purchased from (Sky Spring Nanomaterials, Inc. Houston, USA) and (Hongwu International Group Ltd., Guangdong, China), respectively. Oleic acid surfactant was purchased from (Alpha Chemika, India). The base oil (40-stock) was collected from (Al-Dura Refinery, Middle refineries Company, Baghdad, Iraq). The NPs properties are presented in Table 1, and the base oil (40-stock) specifications are shown in Table 2. Table 1. Specifications of TiO2 and CuO NPs Specification TiO CuO Average diameter(nm) 71.14 73.09 Colour White black Purity (%) >99.9 99 surface area (m 2 /g) 119.9 50 Pore volume (cm³/g) 0.237 0.1606 Table 2. Properties of base oil 60 stocks Specification Oil (40 stock) Kinematic viscosity @ 40 C (cSt) 61.163 Kinematic viscosity @ 100 C (cSt) 8.2209 Viscosity index 102.6 Density @15 (g/cm³) 0.8617 Flash Point (C) 226 Pour point (C) -6 2.2. Experimental Procedures a. Preparation of surface modification of NPs Preparation of surface modification of NPs was completed by adding (1gm) oleic acid to 100ml of ethanol solvent. Two grams of NPs were added to the solution after homogenizing the solution with mixing using a magnetic stirrer. The solution was heated to 75 °C for two hours. After the reaction was over, the oven was used for 4 hours less than 80 °C to ensure all the ethanol was vaporized. Then, it was washed with methanol to remove unreacted oleic acid. The sample was dried at 80 °C for 6 hours to produce modified NPs OA/TiO2 and OA/CuO. b. Preparation of Nano-lubricating oil Modified NPs were added to two base oil (40 stocks), for preparing Nano lubricating oil. The modified TiO2 and CuO NPs were added directly as hybrid additives with a weight ratio of 1:1 to both base oil at different concentrations of (0.2, 0.5, 0.8, and 1% wt.). Stable nano-lubricant is an essential need in this study. According to this, different methods were used, like a magnetic stirrer, ultrasonic probe, and surface modification. Nano-lubricating oil was prepared by dispersing surface-modified nanoparticles into the base oil. The required amount of NPs was weighed carefully using an accurate electronic balance. A magnetic stirrer was used to mix the NPs with base oil for 2 hours. Then an ultrasonic probe-type VCX 750 (Sonics and Materials Inc., USA fitted out with a 13 mm diameter Ti- 6Al-4V alloy tip) was used at the operating conditions shown in Table 3 to obtain high dispersion and prevent agglomeration of NPs. Sonication was carried out for each pulsed irradiation, alternating 5 s of t/ON and 5 s of t/OFF. A water bath jacket was used to avoid overheating of the sample during ultrasonic dispersion. M. R.Fahad and B. A. Abdulmajeed / Iraqi Journal of Chemical and Petroleum Engineering 23,1 (2022) 1 - 7 3 Fig. 1 shows the photo of nano-lubricating oil by the ultrasonic probe. The general steps of the experimental work are represented in Fig. 2. Table 3. Ultrasonic probe specifications The condition Value Power 60 %, 750W Time 1 hr. Temperature 40 °C Frequency 20 kHz Sample quantity 100 ml Fig. 1. Dispersion of NPs into lubricating oil by an ultrasonic probe Fig. 2. Flow diagram of the experimental work 3- Results and Discussion 3.1. FT-IR Characterization of Modified Tio2 and Cuo Nanoparticles. The FT-IR characterized oleic acid (OA) and NPs in the range of 4000-500 cm -1 . Fig. 3 shows the FT-IR of oleic acid. The peak at 1707cm -1 represents C=O stretching, and peaks around 2920 -2850 cm -1 are attributed to the long alkyl chain[18]–[21]. The FT-IR spectrum of TiO2 Fig. 4 and Fig. 5 shows two curves. In curve (a) of Figure (4), peaks around 450 and 750cm ˉ1 in the range of 400–800 cmˉ1 are contributed to anatase titania for pure TiO2. The vibration absorption of the Ti-O-Ti links in TiO2 nanoparticles is attributed to a large absorption band between 450 and 800 cm ˉ 1 (Praveen et al., 2014). The observed peak at 3415 and 1633 cm⁻ ¹ refer to hydroxyl group –OH and water Ti-OH [22]. In both curves (b) of Fig. 4 and Fig. 5, the adsorption peaks of 2924.09 and 2852.72 cm⁻ ¹ are attributed to OA's long alkyl groups and the absorption bands around 1710.8 attributed to carbonyl group C=O from oleic acid [23]. The absorption band around 542 cm⁻ ¹ as shown in curve (a) of Fig. 5, refers to the Cu–O functional group's vibrations, and the peak at 3448.7 and 3452 cm⁻ ¹ relate to the –OH group[24], [25]. In curves (b) of Fig. 4, and Fig. 5, the peaks around 2854 and 2924 cm–1 are attributed to CH2 and CH3 groups formed on the surface of NPs. The carbonyl group at the peak of around 1710 cm -1 in oleic acid form is decreased sharply in these curves. The presence of carboxylate (-COO-) at peaks of around 1428- 1550 cm-1 indicates the reaction of oleic acid and bonded on the surface of NPs. And also the −OH groups on the surface of TiO2, and CuO NPs decreased in modified TiO₂ and CuO nanoparticles. Meanwhile, OA groups of carboxyl (COOH) reacted with hydroxyl (OH) groups to produce carboxylate in modified NPs [20], [26]–[28]. Fig. 3. FTIR spectrum of pure oleic acid M. R.Fahad and B. A. Abdulmajeed / Iraqi Journal of Chemical and Petroleum Engineering 23,1 (2022) 1 - 7 4 Fig. 4. FTIR spectrum of TiO2 (a) and OA/ TiO₂ (b) Fig. 5. FTIR spectrum of CuO (a) and OA/ CuO (b) 3.2. Scanning electron microscopy (SEM) of Oleic acid / NPs Scanning electron microscopy (SEM) is used to characterize the morphology of nanoparticles before and after modification. In Fig. 6 (a) and (b), the images illustrate the morphology of unmodified TiO2, CuO, and Al2O3 NPs, and they were fairly spherical. According to the images in Fig. 6 (b) and (c), it can be seen that the dispersibility of modified NPs was improved, and the pattern of modified NPs appear a little hazy in the pictures, which indicates to coated of OA on the surface of NPs[27], [29], [30]. Fig. 6. FE-SEM of unmodified NPs (a) TiO2, and (b) CuO, and modified NPs (d) OA/ TiO2, and (d) OA/ CuO 3.3. Effect of Addition Modified Tio2-Cuo Nps on the Kinematic Viscosity and Viscosity Index of Nano- Lubricating Oil Viscosity is one of the essential properties of any lubricant, which is one of the most significant considerations when selecting oil for equipment. Fig. 7 (a) and (b) demonstrate the influence of modified TiO2 and CuO NPs on the kinematic viscosity of base oil 40 stock at temperatures 40 °C and 100 °C, respectively. The viscosity increased slightly on increasing modified NPs concentration at both temperatures. At high concentrations, the presence of larger, spherical particles within oil layers, which prevents movement, might explain increased viscosity [31]. The highest increase of viscosity was 2.9 %, 3.31 %, and 3.7 %, related to TiO2 and CuO NPs concentration 0.5 wt. %, 0.8 wt.%, and 1 wt.% at 40 °C, respectively. Increasing the viscosity of light base oil 40 stock after adding nanomaterials Figure (8) shows the viscosity index changes with adding modified TiO2- CuO NPs. The viscosity index increased by 4.5%, 8.4%, 9.92%, and 7.7% relative to the different NPs concentrations at 0.2 wt.%, 0.5 wt.%, 0.8 wt.%, and 1 wt.%, respectively. The maximum increase was observed at 8 wt. % concentration. The higher viscosity index indicates a more stable kinematic viscosity with variable temperatures, thus giving more resistance to oil film thinning [32]. (a) (b) Fig. 7. Effect of TiO₂- CuO on the Kinematic viscosity of base oil 40 stock at (a) 40 °C, and at (b) 100°C M. R.Fahad and B. A. Abdulmajeed / Iraqi Journal of Chemical and Petroleum Engineering 23,1 (2022) 1 - 7 5 Fig. 8. Effect of TiO₂- CuO NPs on the viscosity index of base oil 40 stock 3.4. Flashpoint and Pour Point of Nano-Lubricating Oil The flashpoint (F.P) can be defined as the less temperature that a flammable mixture in the air can be formed. In an instant, the oil follows the ignition line and then suddenly switches off. Fig. 9 and Fig. 10 demonstrate the effect of modified TiO2 – CuO NPs on the flashpoint and pour point property of base oil 40 stock, respectively. It can be seen that the flashpoint increased with adding the NPs to base oil 40 stock attributed to the high thermal conductivity of nanoparticles, and it can be said that it allows the oil to resist ignition better [33]. The rate of improvement in F.P is 14 °C at 0.2 wt% concentration of NPs and the greater improvement was 32 ̊C at 1 wt.% concentration. while the pour point of base oil improved by 3 °C at 0.2 wt.%, 0.5 wt%, and 0.8 wt.% compared with base oil. The higher improvement was at 1wt % by 6 °C. Fig. 9. Effect of nano additive modified TiO₂-CuO wt. % on flash point of base oil 40 stocks Fig. 10. Effect of nano additive modified TiO₂-CuO wt. % on pour point of base oil 40 stocks 4- Conclusions  Using oleic acid surfactant in surface modification of TiO₂, and CuO NPs improved the stability of lubricating oil  The kinematic viscosity of modified TiO2-CuO / base oil 40 stock at 40°C and 100 °C increased slightly with the addition of modified nanoparticles.  The viscosity index increased by 4.5% for 40 stock base oil when 0.2% of modified TiO₂- CuO nano- lubricating oil was used. And the highest increase in VI was 9.92 % at 0.8 wt.% of modified TiO₂-CuO.  Adding TiO₂ - CuO NPs to base oil 40 at varying concentrations improved nano-lubricant oil's flash point compared to parent oil. The highest flash point value was 220 °C References [1] I. Mangas, M. A. Sogorb, and E. Vilanova, Lubricating Oils, Third Edit., vol. 3. Elsevier, 2014. [2] H. 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Abdulmajeed / Iraqi Journal of Chemical and Petroleum Engineering 23,1 (2022) 1 - 7 7 تأثير الجسيمات النانوية الهجينة المعدلة على خصائص الزيت األساسي بسمة عباس عبد المجيد 2و مصطفى رعد فهد 1 فطي، وزارة النفط، بغداد، العراقمركز البحث والتطوير الن 1 قسم الهندسة الكيمياوية ، جامعة بغداد، بغداد، العراق 2 الخالصة مض األوليك افي هذه الدراسة ، تم استخدام ح التزييتلتحسين الخصائص االنسيابية والترايبولوجية لزيت لتعديل سطح الجسيمات النانوية لتعزيز تشتت واستقرار الموائع النانوية. تم إجراء تعديل السطح للجسيمات ، حيث OAض األوليكامخافض التوتر السطحي بحمع CuO، و TiO2 (NPs)النانوية غير العضوية ورييه لتحويل األشعة مطيافية ف كارًها للماء. تم استخدام TiO2-CuOض األوليك سطح اميمكن أن يجعل ح كان الهدف الرئيسي من .NPsلوصف تعديل سطح SEM، والمسح المجهري اإللكتروني FTIRتحت الحمراء على الخواص 1:1المعدلة مع نسبة وزن TiO2-CuO NPsهذه الدراسة هو التحقق من تأثير إضافة نقطة االنسكاب ونقطة الوميض من و VIاللزوجة مل اللزوجةمعا و الكاينماتيكية الحرارية الفيزيائية مثل اللزوجة نانو. تم الحصول على أن اللزوجة الحركية للزيت التزييت ال( وزيت زيت االساس 40الزيت األساسي العراقي ) المعدلة. TiO2-CuO NPsدرجة مئوية تزداد بتركيزات عالية من 100درجة مئوية و 40األساسي عند . 108.5المعدلة TiO2-CuO NPsوزن. كانت ٪ من 0.8عند 40الزيت األساسي VIأعلى قيمة لـ المعدلة من الزيت األساسي TiO2-CuO NPsأظهرت النتائج أن قيمة نقطة الوميض تزداد مع زيادة تركيز بالوزن. أظهرت % 0.8 عندالنانوي التزييتدرجة مئوية. نقطة صب زيت 220، حيث كانت أعلى قيمة 40 درجة مئوية من الزيت 15-درجة مئوية إلى 12-المعدلة تناقًصا من TiO2-CuO NPsلنسبة المئوية من ا 40األساسي ، معامل اللزوجة، نقطة الوميضالجسيمات النانويةالتزييت النانوي، زيت ، 40 االساس الزيت الكلمات الدالة: