CN114769612B - Oil-soluble nickel nano-particles, in-situ synthesis method of oil-soluble nickel nano-particles in vegetable oil and application of oil-soluble nickel nano-particles as vegetable oil antiwear additive - Google Patents
Oil-soluble nickel nano-particles, in-situ synthesis method of oil-soluble nickel nano-particles in vegetable oil and application of oil-soluble nickel nano-particles as vegetable oil antiwear additive Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 264
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 132
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 131
- 235000015112 vegetable and seed oil Nutrition 0.000 title claims abstract description 70
- 239000008158 vegetable oil Substances 0.000 title claims abstract description 70
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 32
- 239000007866 anti-wear additive Substances 0.000 title claims abstract description 10
- 238000001308 synthesis method Methods 0.000 title claims description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 76
- 238000010438 heat treatment Methods 0.000 claims abstract description 48
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 11
- 150000002815 nickel Chemical class 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000012298 atmosphere Substances 0.000 claims abstract description 3
- 239000003054 catalyst Substances 0.000 claims abstract description 3
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims abstract description 3
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract 2
- 235000019484 Rapeseed oil Nutrition 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 21
- BMGNSKKZFQMGDH-FDGPNNRMSA-L nickel(2+);(z)-4-oxopent-2-en-2-olate Chemical compound [Ni+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O BMGNSKKZFQMGDH-FDGPNNRMSA-L 0.000 claims description 13
- 230000000630 rising effect Effects 0.000 claims description 4
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 3
- 239000004359 castor oil Substances 0.000 claims description 3
- 235000019438 castor oil Nutrition 0.000 claims description 3
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 3
- 229940078494 nickel acetate Drugs 0.000 claims description 3
- HZPNKQREYVVATQ-UHFFFAOYSA-L nickel(2+);diformate Chemical compound [Ni+2].[O-]C=O.[O-]C=O HZPNKQREYVVATQ-UHFFFAOYSA-L 0.000 claims description 3
- 239000003549 soybean oil Substances 0.000 claims description 3
- 235000012424 soybean oil Nutrition 0.000 claims description 3
- 235000019482 Palm oil Nutrition 0.000 claims description 2
- 235000019483 Peanut oil Nutrition 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000002540 palm oil Substances 0.000 claims description 2
- 239000000312 peanut oil Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 48
- 238000009826 distribution Methods 0.000 abstract description 13
- 239000002904 solvent Substances 0.000 abstract description 8
- 239000003921 oil Substances 0.000 abstract description 7
- 235000019198 oils Nutrition 0.000 abstract description 7
- 239000003607 modifier Substances 0.000 abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 abstract description 5
- 239000000243 solution Substances 0.000 description 47
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 32
- 230000035484 reaction time Effects 0.000 description 21
- 238000003756 stirring Methods 0.000 description 19
- 230000001965 increasing effect Effects 0.000 description 16
- 238000002360 preparation method Methods 0.000 description 16
- 239000004006 olive oil Substances 0.000 description 15
- 235000008390 olive oil Nutrition 0.000 description 15
- 229910052757 nitrogen Inorganic materials 0.000 description 13
- 239000007789 gas Substances 0.000 description 9
- 238000001291 vacuum drying Methods 0.000 description 9
- 239000000654 additive Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- 238000003917 TEM image Methods 0.000 description 6
- 238000005054 agglomeration Methods 0.000 description 6
- 230000002776 aggregation Effects 0.000 description 6
- 229910001873 dinitrogen Inorganic materials 0.000 description 6
- 239000012046 mixed solvent Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 239000000314 lubricant Substances 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000010687 lubricating oil Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 239000002199 base oil Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000002860 competitive effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 231100000956 nontoxicity Toxicity 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002173 cutting fluid Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000010705 motor oil Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000005070 ripening Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M101/00—Lubricating compositions characterised by the base-material being a mineral or fatty oil
- C10M101/04—Fatty oil fractions
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/04—Metals; Alloys
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
Abstract
The invention discloses a method for in-situ synthesis of oil-soluble nickel nanoparticles in vegetable oil, which comprises the steps of uniformly mixing vegetable oil and nickel salt; then heating to 190-290 ℃ under the inert gas atmosphere, and reacting for 15-180 min at the temperature of the mixture; cooling to room temperature after the reaction is finished, and performing solid-liquid separation, washing and drying to obtain the catalyst. In the method, vegetable oil is used as a solvent to dissolve or disperse nickel salt; on the other hand, the modified nano-particle is used as a modifier to be modified on the surface of the nickel nano-particle, so that the nano-particle is ensured to have good oil solubility. Other reducing agents and solvents are not needed to be introduced in the reaction process, and the used vegetable oil is biodegradable and environment-friendly; the prepared nickel nano particles have controllable particle size and uniform particle size distribution, and have good oil solubility and stability; can effectively improve the tribological performance of the vegetable oil, is hopeful to be used as a novel green antiwear additive for the vegetable oil, and can be widely applied.
Description
Technical Field
The invention belongs to the technical field of preparation of novel functional nano materials, and particularly relates to oil-soluble nickel nano particles, an in-situ synthesis method of the oil-soluble nickel nano particles in vegetable oil and application of the oil-soluble nickel nano particles as a vegetable oil antiwear additive.
Background
With the increasing importance of human society on environmental protection, resource conservation and sustainable development, it is widely recognized that the development of bio-based lubricating oils is not only an essential measure for protecting the environment, but also an important way to alleviate petroleum crisis and make full use of solar energy. The vegetable oil as the base oil has the advantages of no toxicity, no aromatic hydrocarbon, low price, complete biodegradation, high flash point, regeneration, direct discharge, extremely low waste treatment cost, high comprehensive benefit and the like, is widely paid attention to, can solve the technical and environmental challenges in the present and future, has the potential and trend of replacing the traditional petroleum-based lubricant, and has been used in the brand-new corner of the application fields of automobile engine oil, metal processing cutting fluid, gear bearing lubricating oil and the like.
Additives for mineral and synthetic oils cannot be applied directly to vegetable oil lubricants, with vegetable oils having a certain selectivity for the additive. In order to obtain an additive with good properties, it is necessary to prepare a suitable treatment agent for vegetable oils. When vegetable oils are used in the field of tribology, their inherent chemical structure and physicochemical properties affect their tribological properties. Compared with the traditional mineral oil, the vegetable oil contains polar groups which are arranged on the surface of the friction pair in an oriented way to form a friction film, so that the antifriction performance of the vegetable oil is improved; however, the strong polar vegetable oil is unfavorable for film formation of other additives on the friction surface due to competitive adsorption, and the magnetism of the nickel nano particles is utilized to adsorb on the surface of the iron-based metal friction pair, so that the difficulty in competitive adsorption of the vegetable oil and the additives on the surface of the metal friction pair is solved, and the friction reduction and wear resistance of the friction pair are expected to be realized.
The preparation method of the nickel nano particles mainly comprises a physical method and a chemical method, but the nickel nano particles are easy to agglomerate due to magnetism, so that the dispersibility of the nickel nano particles in base oil is affected, the nickel nano particles are synthesized in situ in vegetable oil, and the vegetable oil is used as a modifier, so that the compatibility of the nickel nano particles and the vegetable oil is enhanced on one hand; on the other hand, the preparation process does not use reducing agent and organic solvent, and the safety is high. The vegetable oil lubricant has excellent environmental protection performance, wide and easily available sources, and has a solid raw material basis for developing research and application research of vegetable-based lubricating oil for China of agricultural China.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the oil-soluble nickel nano particles which are controllable in particle size and uniform in distribution, have good tribological properties, can be recycled, have high degradability, have high flash point and combustion point and good high-temperature stability, and can be directly discharged without adverse effect on the environment.
The invention also provides an in-situ synthesis method of the oil-soluble nickel nano particles in vegetable oil and application of the oil-soluble nickel nano particles in vegetable oil. The preparation method of the nickel nano particles is environment-friendly, does not introduce other reducing agents and solvents, and the used vegetable oil is biodegradable and environment-friendly. The vegetable oil is used as a solvent and a modifier in the reaction, so that the compatibility of the nickel nano particles and the vegetable oil is ensured. The prepared nickel nano particles and vegetable oil can form a matched additive, and the environment-friendly vegetable oil lubricant has good application prospect.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
an in situ synthesis method of oil-soluble nickel nanoparticles in vegetable oil, which comprises the following steps:
1) Mixing vegetable oil and nickel salt; then heating to 190-290 ℃ under the atmosphere of inert gas (such as nitrogen, argon and the like) and preserving heat for 15-180 min;
2) Cooling to room temperature after the reaction is finished, and performing solid-liquid separation (such as centrifugation), washing and drying to obtain the catalyst.
Specifically, the vegetable oil comprises one or more of rapeseed oil, olive oil, peanut oil, soybean oil, castor oil, palm oil and the like.
Specifically, the nickel salt comprises any one or more of nickel acetylacetonate, nickel acetate, nickel formate and the like.
Further, in the step 1), 30 mL vegetable oil and 0.1-0.8 g nickel salt can be added into a three-neck flask for electric stirring and uniform mixing.
Further preferably, in step 1), the reaction temperature is 190, 200, 210, 220, 230, 250 or 270 ℃; the reaction time was 15, 30, 60, 90, 120, 150 or 180 min.
Further, in the step 1), the temperature rising rate is 5-10 ℃/min.
Further preferably, in the step 2), n-hexane or a mixed solution of ethanol and n-hexane (preferably, the volume ratio of the n-hexane to the ethanol is 5:1) is selected for washing; drying in a vacuum oven at 50-80deg.C overnight.
The invention provides the oil-soluble nickel nano particles synthesized by the method.
The invention also provides application of the oil-soluble nickel nanoparticles as an antiwear additive for vegetable oil. Further, when in application, the mass addition concentration of the oil-soluble nickel nano particles is 0.02% -1.0%. The invention also tests the tribological property of the oil-soluble nickel nano-particles when the oil-soluble nickel nano-particles are used as vegetable oil anti-wear additives, for example, when the oil-soluble nickel nano-particles are used as rapeseed oil anti-wear additives, the mass addition concentration is 0.3%, and the rapeseed oil anti-wear property is improved by 36%. When the oil-soluble nickel nano particles are used as the olive oil anti-wear additive, the mass addition concentration is 0.3%, and the olive oil anti-wear property is improved by 30%.
In the method of the invention, vegetable oil is used as a solvent to dissolve or disperse nickel salt; on the other hand, the modified nano-particle is used as a modifier to be modified on the surface of the nickel nano-particle, so that the nano-particle is ensured to have good oil solubility. Other reducing agents and solvents are not required to be introduced in the reaction process, and the used vegetable oil is biodegradable and environment-friendly; the method for preparing the nickel nano particles is simple and convenient, has rich raw material sources, and is suitable for large-scale industrial production. The prepared nickel nano particles have controllable particle size, uniform particle size distribution and good oil solubility and stability. Compared with the prior art, the invention has the remarkable advantages that:
(1) The invention takes vegetable oil which has wide sources, no toxicity and low price and can be completely biodegraded as a solvent.
(2) In the preparation process of the oil-soluble nickel nanoparticles, the vegetable oil is not only used as a solution, but also used as a modifier of a target product, and a reducing agent and a toxic solvent are not introduced in the reaction, so that impurities and environmental pollution in a system are reduced; in addition, in the process of generating the nickel nanoparticles, components such as oleic acid in the vegetable oil are modified on the surfaces of the nickel nanoparticles, the growth of the nickel nanoparticles is inhibited, and lipophilic groups on the surfaces of the modifier provide good oil solubility for the prepared nickel nanoparticles so that the nickel nanoparticles can be stably dispersed in the vegetable oil.
(3) The oil-soluble nickel nano particles prepared by the invention are generated in situ in vegetable oil, have good compatibility with the vegetable oil, and are beneficial to application in the vegetable oil.
(4) The particle size of the oil-soluble nickel nano particles prepared by the invention is controllable, the oil-soluble nickel nano particles are uniformly distributed, and the particle size is between 8 and 50 and nm; and the preparation process is simple, the raw material sources are rich, and the industrial mass production is facilitated.
(5) When the addition concentration of the oil-soluble nickel nanoparticles prepared by the invention is only 0.3%, the abrasion resistance of the rapeseed oil is improved by 36%, the olive oil is improved by 30%, the oil-soluble nickel nanoparticles have good tribological properties, the vegetable oil can be recycled, and the oil-soluble nickel nanoparticles have high degradability, have high flash point and combustion point and high temperature stability, and the direct discharge does not cause adverse effect on the environment. The nickel nano particles and the vegetable oil can form a matched additive, and the environment-friendly vegetable oil lubricant has wide application prospect.
Drawings
FIG. 1 is a schematic diagram of a process for synthesizing oil-soluble nickel nanoparticles according to the present invention;
FIG. 2 is a graph showing morphology and particle size distribution of nickel nanoparticles synthesized in situ in rapeseed oil at different reaction temperatures in example 1; in the figure, (a) 190 ℃, (b) 200 ℃, (c) 210 ℃, (d) 220 ℃;
FIG. 3 is a TEM image of in situ synthesis of nickel nanoparticles in rapeseed oil at 190℃according to example 2 at different reaction times; in the figure, (a) 30 min, (b) 60 min, (c) 90 min, (d) 120 min, (e) 150 min, and (f) 180 min;
FIG. 4 is an XRD pattern of oil-soluble nickel nanoparticles synthesized in situ in rapeseed oil according to example 5;
FIG. 5 is a TEM image and particle size distribution diagram of oil-soluble nickel nanoparticles synthesized in situ in rapeseed oil of example 5; in the figure, (a) 200 ℃ and (b) 210 ℃;
FIG. 6 is a TEM image and particle size distribution diagram of oil-soluble nickel nanoparticles synthesized at different temperature ramp rates of example 6; in the figure, (a) the temperature rising rate is 10 ℃/min, and (b) the temperature rising rate is 10 ℃/min;
FIG. 7 is a TEM image and a particle size distribution diagram of nickel nanoparticles obtained by reacting nickel acetylacetonate of example 7 in olive oil at 200℃for 120 min (a) and 150 min (b);
FIG. 8 is a tribological evaluation of nickel nanoparticles synthesized in situ in rapeseed oil at 200 and 210℃in example 5;
FIG. 9 is a tribological evaluation result of nickel nanoparticles synthesized in situ in olive oil with a reaction time of 120 and 150 min according to example 7.
Detailed Description
The following describes the technical scheme of the present invention in further detail with reference to examples, but the scope of the present invention is not limited thereto.
In the examples, the raw materials used were all commercially available products which were commercially available as they are. Room temperature refers to 25±5 ℃.
Example 1
An in-situ preparation method of oil-soluble nickel nano particles in vegetable oil (shown in figure 1) specifically comprises the following steps:
(1) Sequentially adding 30 mL rapeseed oil and 0.39 g nickel acetylacetonate into a three-neck flask of 50 mL, and uniformly stirring under electric stirring;
(2) Continuously introducing inert shielding gas nitrogen into the reaction solution obtained in the step (1), wherein the air flow speed is about 0.5L/min;
(3) Heating the reaction solution obtained in the step (2) in a heating jacket, and respectively heating to different temperatures at a heating rate of 5 ℃/min, such as 190, 200, 210, 220, 230, 250, 270 and 290 ℃, wherein the color of the solution changes from green to black in the reaction process, and the reaction time is 30 min;
(4) After the reaction was completed, heating was stopped, the reaction solution in the three-necked flask was cooled to room temperature in air, the introduction of nitrogen gas was stopped, and then the reaction solution was centrifuged at 10000 rev/min in a centrifuge for 15 min. Washing 3 times by using a mixed solvent of ethanol and normal hexane in a volume ratio of 5:1, and drying overnight in a vacuum drying oven at 60 ℃ to obtain the oil-soluble nickel nanoparticles with the surface modified.
The nickel nanoparticles synthesized in situ in rapeseed oil at different temperatures are spherical particles in morphology, and the particle size tends to increase with the increase of the temperature, and a TEM image and a particle size distribution diagram of the nickel nanoparticles generated in situ in the rapeseed oil at the reaction temperatures of 190, 200, 210 and 220 ℃ are shown in fig. 2. When the reaction temperature is 190 ℃ and the reaction time is 30 min, crystal nuclei of the nickel nano particles are not generated, the crystal grains are in a growing state, when the temperature is 200 ℃, the crystal nuclei of the nickel nano particles are generated, the nickel nano particles have good dispersibility, the average particle size is 12.2 nm, and the particle size distribution is narrower; when the temperature is raised to 210 ℃, obvious agglomeration phenomenon of particles starts to appear, the dispersibility is poor, and the average particle diameter is about 13.4 and nm; when the reaction is carried out at 220 ℃, the agglomeration degree of the particles is more obvious, the average particle diameter is increased to 22.5 and nm, and the particle diameter distribution is widened.
Example 2
An in-situ preparation method of oil-soluble nickel nanoparticles in vegetable oil specifically comprises the following steps:
(1) Sequentially adding 30 mL rapeseed oil and 0.39 g nickel acetylacetonate into a three-neck flask of 50 mL, and uniformly stirring under electric stirring;
(2) Continuously introducing inert shielding gas nitrogen into the reaction solution obtained in the step (1), wherein the air flow speed is about 0.5L/min;
(3) Heating the reaction solution obtained in the step (2) in a heating sleeve, and heating to 190 ℃ at a heating rate of 5 ℃/min, wherein the color of the solution is changed from green to black in the reaction process, and the reaction time is 30, 60, 90, 120, 150 and 180 min respectively;
(4) After the reaction is finished, stopping heating, cooling the reaction solution in the three-neck flask to room temperature in air, stopping introducing nitrogen, centrifuging the reaction solution in a centrifuge at 10000 rev/min for 15 min, washing 3 times by using a mixed solvent of ethanol and n-hexane with the volume ratio of 5:1, and drying overnight in a vacuum drying oven at 60 ℃ to obtain the oil-soluble nickel nanoparticles with the surface modified.
The reaction temperature is 190 ℃, nickel nano particles (shown in figure 3) are prepared in different reaction time, the nickel crystal nucleus is not generated at the reaction time of 30 min, and the reaction is not completed; when the reaction is carried out for 60-90 min, nickel crystal nuclei are generated, but some nickel crystal nuclei still have agglomeration and poor dispersibility, and the average particle size is about 31.5 and nm; the reaction time is from 120 min to 180 min, the nickel nano particles have better dispersibility, the particle size is reduced, and the particle size is reduced from 35.1 and nm to 22.2 and nm.
Example 3
An in-situ preparation method of oil-soluble nickel nanoparticles in vegetable oil specifically comprises the following steps:
(1) Sequentially adding 30 mL rapeseed oil and 0.39 g nickel acetylacetonate into a three-neck flask of 50 mL, and uniformly stirring under electric stirring;
(2) Continuously introducing inert shielding gas nitrogen into the reaction solution obtained in the step (1), wherein the air flow speed is about 0.5L/min;
(3) Heating the reaction solution obtained in the step (2) in a heating sleeve, and heating to 200 ℃ at a heating rate of 5 ℃/min, wherein the color of the solution is changed from green to black in the reaction process, and the reaction time is respectively 30, 60, 90, 120, 150 and 180 min;
(4) After the reaction was completed, heating was stopped, the reaction solution in the three-necked flask was cooled to room temperature in air, the introduction of nitrogen gas was stopped, and then the reaction solution was centrifuged at 10000 rev/min in a centrifuge for 15 min. Washing 3 times by using a mixed solvent of ethanol and normal hexane in a volume ratio of 5:1, and drying overnight in a vacuum drying oven at 80 ℃ to obtain the oil-soluble nickel nanoparticles with the surface modified.
The nickel nano particles are prepared at the higher temperature of 200 ℃, and when the reaction time is 30 min, the nickel nano particles synthesized in situ in the rapeseed oil have better dispersibility, no obvious agglomeration phenomenon and the average particle size is about 12.2 nm. As the reaction time increases, the degree of agglomeration of nickel nanoparticles increases, dispersibility becomes poor, and the particle size gradually increases due to the oswald ripening phenomenon, and when the reaction time is prolonged to 180 min, the average particle size increases to 24.8 nm.
Example 4
An in-situ preparation method of oil-soluble nickel nanoparticles in vegetable oil specifically comprises the following steps:
(1) Sequentially adding 30 mL rapeseed oil and 0.19 g (or 0.78 g) nickel acetylacetonate into a three-neck flask of 50 mL, and stirring uniformly under electric stirring;
(2) Continuously introducing inert shielding gas nitrogen into the reaction solution obtained in the step (1), wherein the air flow speed is about 0.5L/min;
(3) Heating the reaction solution obtained in the step (2) in a heating sleeve, and heating to 200 ℃ at a heating rate of 5 ℃/min, wherein the color of the solution is changed from green to black in the reaction process, and the reaction time is 30 min respectively;
(4) After the reaction is finished, stopping heating, cooling the reaction solution in the three-neck flask to room temperature in air, stopping introducing nitrogen, centrifuging the reaction solution in a centrifuge at 10000 rev/min for 15 min, washing 3 times by using a mixed solvent of ethanol and n-hexane with the volume ratio of 5:1, and drying overnight in a vacuum drying oven at 60 ℃ to obtain the oil-soluble nickel nanoparticles with the surface modified.
When the concentration of the reactant nickel acetylacetonate is 0.025 mol/L, the obtained nickel nanoparticles have good particle size dispersibility and an average particle size of about 15 and nm. When the concentration is 0.05 mol/L, the nickel nano particles have better dispersibility, no obvious agglomeration phenomenon and the average particle diameter is about 12.2 nm. When the concentration is increased to 0.1 mol/L, the average particle diameter of the prepared oil-soluble nickel nano particles is increased to 45 and nm, and the particles are agglomerated into blocks and have poor dispersibility.
Example 5
An in-situ preparation method of oil-soluble nickel nanoparticles in vegetable oil specifically comprises the following steps:
(1) Sequentially adding 30 mL rapeseed oil and 0.39 g nickel acetylacetonate into a three-neck flask of 50 mL, and uniformly stirring under electric stirring;
(2) Continuously introducing inert shielding gas nitrogen into the reaction solution obtained in the step (1), wherein the air flow speed is about 0.5L/min;
(3) Heating the reaction solution obtained in the step (2) in a heating sleeve, and respectively heating to 200 ℃ and 210 ℃ at a heating rate of 5 ℃/min, wherein the color of the solution is changed from green to black in the reaction process, and the reaction time is 15 min;
(4) After the reaction is finished, stopping heating, cooling the reaction solution in the three-neck flask to room temperature in air, stopping introducing nitrogen, centrifuging the reaction solution in a centrifuge at 10000 rev/min for 15 min, washing 3 times by using a mixed solvent of ethanol and n-hexane with the volume ratio of 5:1, and drying overnight in a vacuum drying oven at 60 ℃ to obtain the oil-soluble nickel nanoparticles with the surface modified.
The nickel nanoparticles are prepared in situ in rapeseed oil by taking nickel acetylacetonate as a nickel source, the reaction temperature is respectively 200 ℃ and 210 ℃, the reaction time is shortened to 15 min, the XRD pattern of the prepared oil-soluble nickel nanoparticles is shown in figure 4, diffraction peaks at 44.51 DEG, 51.85 DEG and 76.37 DEG correspond to (111), (200) and (220) crystal faces of nickel with a face-centered cubic structure respectively, other diffraction peaks such as nickel oxide are not found, and the high-purity nickel nanoparticles are synthesized.
The TEM image of the oil-soluble nickel nanoparticles prepared above is shown in fig. 5. As shown in FIG. 5, the nickel nanoparticles have smaller particle size, are uniformly distributed, have spherical morphology, and have slightly increased average particle size with increasing reaction temperature, wherein the average particle size at 200 ℃ and 210 ℃ is 12.66 nm and 14.34 nm, respectively.
Example 6
An in-situ preparation method of oil-soluble nickel nanoparticles in vegetable oil specifically comprises the following steps:
(1) Sequentially adding 30 mL rapeseed oil and 0.39 g nickel acetylacetonate into a three-neck flask of 50 mL, and uniformly stirring under electric stirring;
(2) Continuously introducing inert shielding gas nitrogen into the reaction solution obtained in the step (1), wherein the air flow speed is about 0.5L/min;
(3) Heating the reaction solution obtained in the step (2) in a heating sleeve, respectively heating to 210 ℃ at the heating rates of 5 ℃ and 10 ℃/min, and blackening the solution from green in the reaction process for 30 min;
(4) After the reaction was completed, heating was stopped, the reaction solution in the three-necked flask was cooled to room temperature in air, the introduction of nitrogen gas was stopped, and then the reaction solution was centrifuged at 10000 rev/min in a centrifuge for 15 min. Washing with ethanol for 3 times, and drying in a vacuum drying oven at 60 ℃ overnight to obtain the oil-soluble nickel nano particles with the surface modified.
When the temperature rise rate was increased from 5℃to 10℃per minute in the preparation of the oil-soluble nickel nanoparticles, the particle diameter of the nickel nanoparticles was increased from 13.4. 13.4 nm to 21.7. 21.7 nm as shown in FIG. 6, and the nickel nanoparticles were slightly agglomerated, and the dispersibility was deteriorated.
Example 7
An in-situ preparation method of oil-soluble nickel nanoparticles in vegetable oil specifically comprises the following steps:
(1) Sequentially adding 30 mL olive oil and 0.39 g nickel acetylacetonate into a three-neck flask of 50 mL, and uniformly stirring under electric stirring;
(2) Continuously introducing inert shielding gas nitrogen into the reaction solution obtained in the step (1), wherein the air flow speed is about 0.5L/min;
(3) Heating the reaction solution obtained in the step (2) in a heating sleeve, and heating to 200 ℃ at a heating rate of 5 ℃/min, wherein the color of the solution is changed from green to black in the reaction process, and the reaction time is respectively 60, 90, 120 and 150 min;
(4) After the reaction was completed, heating was stopped, the reaction solution in the three-necked flask was cooled to room temperature in air, the introduction of nitrogen gas was stopped, and then the reaction solution was centrifuged at 10000 rev/min in a centrifuge for 15 min. Washing with n-hexane for 3 times, and drying in a vacuum drying oven at 60 ℃ overnight to obtain the oil-soluble nickel nano particles with the surface modified.
The TEM and particle size distribution of nickel nanoparticles prepared by reacting nickel acetylacetonate in olive oil at a reaction temperature of 200deg.C for 120 min and 150 min are shown in FIG. 7. When the reaction time is 120 min, the average particle size of the prepared nickel nano particles is about 11.9 and nm; when the reaction time is 150 min, the particle size of the prepared nickel nano particles is increased, the average particle size is about 15.6 and nm, and under the same condition, the nickel nano particles prepared in the olive oil are smaller than the particle size prepared in the rapeseed oil, and the dispersibility is good.
Example 8
An in-situ preparation method of oil-soluble nickel nanoparticles in vegetable oil specifically comprises the following steps:
(1) Sequentially adding 30 mL soybean oil and 0.27 g nickel acetate into a three-neck flask of 50 mL, and uniformly stirring under electric stirring;
(2) Continuously introducing inert shielding gas nitrogen into the reaction solution obtained in the step (1), wherein the air flow speed is about 0.5L/min;
(3) Heating the reaction solution obtained in the step (2) in a heating sleeve, heating to 230 ℃ at a heating rate of 5 ℃/min, changing the color of the solution from green to yellow in the reaction process, and completely blackening the color of the solution after heating at 260 ℃ for 20 min;
(4) After the reaction was completed, heating was stopped, the reaction solution in the three-necked flask was cooled to room temperature in air, the introduction of nitrogen gas was stopped, and then the reaction solution was centrifuged at 10000 rev/min in a centrifuge for 15 min. Washing 3 times by using a mixed solvent of ethanol and normal hexane in a volume ratio of 5:1, and drying overnight in a vacuum drying oven at 60 ℃ to obtain the oil-soluble nickel nanoparticles with the surface modified. The nickel nanoparticles had an average particle size of about 29 a nm a, slightly agglomerated and a broad particle size distribution.
Example 9
An in-situ preparation method of oil-soluble nickel nanoparticles in vegetable oil specifically comprises the following steps:
(1) Sequentially adding 30 mL castor oil and 0.23 g nickel formate into a 50 mL three-neck flask, and uniformly stirring under electric stirring;
(2) Continuously introducing inert shielding gas nitrogen into the reaction solution obtained in the step (1), wherein the air flow speed is about 0.5L/min;
(3) Heating the reaction solution obtained in the step (2) in a heating sleeve, and continuously reacting for 30 min when the temperature is increased to 200 ℃ at the heating rate of 5 ℃/min, wherein the color of the solution is changed from green to black;
(4) After the reaction was completed, heating was stopped, the reaction solution in the three-necked flask was cooled to room temperature in air, the introduction of nitrogen gas was stopped, and then the reaction solution was centrifuged at 10000 rev/min in a centrifuge for 15 min. Washing with absolute ethanol for 3 times, and drying in a vacuum drying oven at 60 ℃ overnight to obtain black oil-soluble nickel nanoparticles. The average particle size of the nickel nano particles is about 50 and nm, the nickel nano particles are obviously agglomerated, and the particle size is uneven.
Tribological test 1
The oil-soluble nickel nanoparticles prepared in example 5 above were added to rapeseed oil at a mass fraction of 0.3wt% and subjected to tribological tests on a four-ball frictional wear tester under conditions of load 392N, rotation speed 1200 rev/min, temperature 75 ℃ and time 60 min. The experimental results are shown in FIG. 8.
The results of fig. 8 show that: compared with pure rapeseed oil, the nickel nano particles synthesized at the reaction temperature of 200 ℃ and 210 ℃ are added into the rapeseed oil at 0.3wt%, the friction Coefficient (COF) is respectively increased from 0.064 to 0.087 and 0.091, and the friction coefficient is respectively increased by 36% and 42%, so that the nickel nano particles do not play a friction reducing role in the rapeseed oil, but have a friction increasing effect. However, 0.3wt% nickel nanoparticles significantly reduced the plaque diameter (WSD) in rapeseed oil. Wherein, the synthesized nickel nano particles have remarkable antiwear property in the rapeseed oil at 200 ℃, and the diameter of the abrasive spots is reduced from 0.77-mm to 0.49-mm of the rapeseed oil by 36 percent. When the reaction temperature is increased to 210 ℃, the particle size of the synthesized nickel nano particles is increased, so that the abrasion resistance of the nickel nano particles is reduced, the abrasive spot diameter is 0.51-mm, and the abrasive spot diameter is reduced by 33% compared with that of rapeseed oil.
Tribological test 2
The oil-soluble nickel nanoparticles prepared in the above example 7 were reacted in olive oil at 200℃for 120 and 150 min, respectively, and 0.3wt% was added to pure olive oil, and the tribological property evaluation was performed on a four-ball frictional wear tester under the conditions of load 392N, rotation speed 1200 rev/min, temperature 75℃and time 60 min. The experimental results are shown in FIG. 9.
The results of fig. 9 show that: the introduction of 0.3wt% nickel nanoparticles into the olive oil also does not have an antifriction effect, but rather increases the coefficient of friction (COF) from 0.072 to 0.12 and 0.11, respectively, and increases the coefficient of friction by 67% and 53%, respectively; from the average mill-cake diameter (WSD) size, the mill-cake diameter of the nickel nanoparticles with 0.3wt% after being introduced into the olive oil is smaller than that of the pure olive oil, and the average mill-cake diameter of the nickel nanoparticles synthesized in situ under the reaction condition of 200 ℃ and 120 min is smaller and is 0.45 and mm, which is reduced by about 30%. As the reaction time was prolonged to 150 min, the abrasion resistance of the nickel nanoparticles was also gradually reduced with increasing particle size, at which time the average plaque diameter was 0.49. 0.49 mm, which was 23% lower than that of pure olive oil (0.64. 0.64 mm), and the reduction was gradually reduced.
The oil-soluble nickel nanoparticles prepared in examples 1 to 9 above were found by XRD and TEM detection: the obtained products are nickel nano particles, and the shape, size and dispersibility of the nickel nano particles change along with the change of the reaction temperature, the reaction time and the concentration of reactants. The reaction condition is optimized, and the prepared oil-soluble nickel nano particles have small particle size, narrow particle size distribution and good oil solubility between 8 and 50 and nm.
In summary, it can be found that: the oil-soluble nickel nano particles prepared in situ in the vegetable oil have good antiwear performance in the vegetable oil, and can be widely used as vegetable oil additives.
Claims (6)
1. An in-situ synthesis method of oil-soluble nickel nanoparticles in vegetable oil is characterized by comprising the following steps:
1) Mixing vegetable oil and nickel salt; then heating to 190-210 ℃ under the inert gas atmosphere, and reacting for 15-180 min at the temperature of the mixture;
2) Cooling to room temperature after the reaction is finished, and performing solid-liquid separation, washing and drying to obtain the catalyst;
the vegetable oil comprises one or more of rapeseed oil, peanut oil, soybean oil, castor oil and palm oil;
the nickel salt comprises any one or more of nickel acetylacetonate, nickel acetate and nickel formate;
in the step 1), 30 mL vegetable oil and 0.1-0.39 g nickel salt are stirred and mixed uniformly.
2. The method for in situ synthesis of oil-soluble nickel nanoparticles in vegetable oil according to claim 1, wherein in step 1), the temperature rising rate is 5-10 ℃/min.
3. The method for in-situ synthesis of oil-soluble nickel nanoparticles in vegetable oil according to claim 1, wherein in step 2), n-hexane or a mixed solution of ethanol and n-hexane is selected for washing; drying in a vacuum oven at 50-80deg.C overnight.
4. The oil-soluble nickel nanoparticles obtained by synthesis using the method of any one of claims 1 to 3.
5. The use of the oil-soluble nickel nanoparticles of claim 4 as an antiwear additive for vegetable oils.
6. The use of the oil-soluble nickel nanoparticles as an antiwear additive for vegetable oils according to claim 5, wherein the mass addition concentration of the oil-soluble nickel nanoparticles is 0.02% -1.0%.
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