Antioxidant lubricating oil and preparation method thereof
By using vegetable oil and multi-effect additives, the problem of oxidation and degradation of traditional lubricants under high temperature and high pressure is solved, and the antioxidant and anti-wear properties of lubricants are enhanced to meet industrial needs.
Patent Information
- Application Number
- CN202510574254.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-06
- Publication Date
- 2025-08-01
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
Traditional lubricating oils oxidize and degrade under high temperature and high pressure, resulting in a degradation of performance, and the existing additives have poor compatibility, making it difficult to meet industrial needs.
Vegetable oil is used as the base oil and multi-effect additives are added. This additive reacts pentaerythritol with trichlorophen and phosphorus trichloride to produce antioxidant and antiwear agents containing a variety of functional groups, enhancing the antioxidant and antiwear properties of the lubricating oil.
The produced lubricating oil has excellent antioxidant and wear properties, extends service life, improves safety and meets industrial needs.
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Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of lubricating oils, and specifically relates to an antioxidant lubricating oil and a preparation method thereof. Background Art
[0002] With the continuous development of industrial technology, mechanical equipment is increasingly widely used in modern industrial production. As an important guarantee for the normal operation of mechanical equipment, the performance of lubricating oil directly affects the service life and operating efficiency of the equipment. Traditional lubricating oils are mainly based on mineral oils or synthetic oils as base oils, and various functional additives are added to improve their performance. However, during actual use, lubricating oils are affected by factors such as high temperature, high pressure, and oxidation, resulting in a gradual decline in their performance and even failure. Therefore, antioxidant performance is one of the important indicators for measuring the quality of lubricating oils.
[0003] Under high-temperature conditions, lubricating oil molecules react chemically with oxygen to form a free radical chain reaction, thereby triggering oxidative degradation. This oxidation process leads to an increase in the viscosity of the lubricating oil, an increase in the acid value, and the formation of insoluble deposits, ultimately affecting its lubricating effect. In addition, in some application scenarios of lubricating oils, for example, engines operate under high temperature and high pressure, and the friction and wear between components are relatively serious; gears work under high load and impact load conditions, and are prone to pitting and wear. This also requires lubricating oils to have a certain anti-friction effect. To solve this problem, the current common method is to add additives to the lubricating oil, but the compatibility between various additives is poor, and the effect is limited, making it difficult to meet the increasingly strict industrial requirements. Therefore, there is an urgent need to invent a lubricating oil with both antioxidant and anti-friction effects to meet the higher demands in the technical field of lubricating oils. Summary of the Invention
[0004] The purpose of the present invention is to overcome the defects of the prior art and provide an antioxidant lubricating oil and a preparation method thereof.
[0005] The purpose of the present invention can be achieved by the following technical solutions: A preparation method of an antioxidant lubricating oil, comprising the following steps: Step 1: Add a base oil to a reaction kettle, heat it to 40 - 50 °C, keep it warm for 2 min, then add a thickening agent, and raise the temperature to 180 - 190 °C for refining for 10 min to obtain a pretreated base oil; Step 2: When the temperature in the reaction kettle drops to 40 - 60 °C, add an antioxidant and a multi-functional additive, mix and stir for 1 - 2 h, let it stand to room temperature, and after grinding, obtain the antioxidant lubricating oil.
[0006] Further, the raw materials are as follows by mass parts: 98 - 112 parts of base oil, 21 - 26 parts of thickening agent, 3 - 6 parts of antioxidant, and 5 - 10 parts of multi - effect additive.
[0007] Further, the base oil is one of olive oil, castor oil, soybean oil, and rapeseed oil.
[0008] Further, the thickening agent is one of lithium stearate soap, calcium stearate soap, and calcium 12 - hydroxystearate soap.
[0009] Further, the antioxidant is a hindered phenol antioxidant.
[0010] Further, the mixing and stirring rate in step two is 100 - 200 r / min.
[0011] Further, the multi - effect additive is prepared through the following steps: Step 1: Add pentaerythritol and phosphorus trichloride into a three - necked flask equipped with a thermometer, a mechanical stirrer, and a reflux condenser (connected to a tail gas absorption device to absorb the by - product HCl). After stirring evenly, heat with an oil bath, control the reaction temperature to be maintained at 155 °C, carry out a reflux reaction until no hydrogen chloride gas is released, then continue to raise the temperature to 165 °C, carry out a constant - temperature reaction for 2 h. After the reaction is completed, let it stand and cool to room temperature, extract with boiling water, remove the viscous substances deposited at the bottom of the flask by decantation, concentrate to remove part of the water, then cool and crystallize, filter by suction to collect the crystals, and dry to obtain reaction product A; Furthermore, in step 1, the dosage ratio of pentaerythritol to phosphorus trichloride is 15.9 g:16.7 g.
[0012] The reaction principle is: pentaerythritol and phosphorus trichloride undergo a nucleophilic substitution reaction, and pentaerythritol is slightly in excess to obtain reaction product A; the reaction formula is as follows:
[0013] Step 2: Add pentaerythritol and anhydrous toluene into a three - necked flask equipped with a thermometer, a mechanical stirrer, a constant - pressure dropping funnel, and a reflux condenser (connected to a tail gas absorption device to absorb the by - product HCl). Then place the reaction system in an ice - water bath at 0 °C. While stirring, slowly add phosphorus trichloride dropwise through the constant - pressure dropping funnel. After the dropping is completed, remove the ice bath, heat the device until the temperature stabilizes at 77 °C, carry out a constant - temperature reflux reaction for 3 h. After the reaction ends, transfer the reaction solution to a rotary evaporator and carry out rotary evaporation to obtain reaction product B; Furthermore, in step 2, the dosage ratio of pentaerythritol, anhydrous toluene, and phosphorus trichloride is 13.6 g:100 mL:29.3 g.
[0014] The reaction principle is as follows: Pentaerythritol undergoes a nucleophilic substitution reaction with phosphorus trichloride. During the reaction, by precisely controlling the molar ratio of the two to be close to 1:2 and ensuring a slight excess of phosphorus trichloride, the reaction can proceed fully. The reaction formula is as follows:
[0015] Step 3: Add reaction product A, reaction product B, triethylamine (acid-binding agent), and anhydrous toluene into a three-necked flask equipped with a thermometer and a mechanical stirrer. After stirring evenly, heat the device until the temperature stabilizes at 65°C, and react at a constant temperature for 6 hours. After the reaction is completed, filter, transfer the reaction solution to a rotary evaporator, rotary evaporate to remove part of the solvent, and then use a petroleum ether-ethyl acetate (10:1, v / v) elution system for column chromatography purification. Rotary evaporate to remove the eluent to obtain a multifunctional additive; Furthermore, in step 3, the dosage ratio of reaction product A, reaction product B, triethylamine, and anhydrous toluene is 27.8 g: 14.4 g: 15 mL: 100 mL; The reaction principle is as follows: Under the catalysis of triethylamine, reaction product A and reaction product B undergo a nucleophilic substitution reaction. During the reaction, by precisely controlling the molar ratio of the two to be close to 2:1 and ensuring a slight excess of reaction product A, the reaction can proceed fully. The reaction formula is as follows:
[0016] The prepared multifunctional additive molecule contains multiple functional groups. Among them, the phosphite group can reduce the free radicals generated by the homolytic cleavage of hydroperoxides to stable alcohols, directly react with free radicals to interrupt the chain oxidation reaction, and as an auxiliary antioxidant, it can cooperate with the hindered phenol antioxidant in the raw materials to greatly enhance the antioxidant performance of the lubricating oil. In addition, the multifunctional additive molecule also contains a thiophosphate group. Under high-temperature conditions, it decomposes to generate sulfur- and phosphorus-containing compounds, which capture free radicals or decompose peroxides, thereby interrupting the oxidation chain reaction and further enhancing the antioxidant performance of the lubricating oil. Moreover, thiophosphate is a common anti-wear additive, which can improve the anti-wear performance of the lubricating oil through the combined action of chemical reaction films and physical adsorption films. In addition, the multifunctional additive molecule also contains a pentaerythritol molecular skeleton with a highly symmetric rigid structure, which enhances the high-temperature aging resistance of the lubricating oil. Finally, the prepared multifunctional additive integrates multiple functional groups, avoiding the addition of multiple additives and having better compatibility.
[0017] The beneficial effects of the present invention: 1. The lubricating oil prepared by the present invention selects vegetable oil as the base oil, which is not only more environmentally friendly, but also has a high flash point of vegetable oil, improving the safety of the lubricating oil during production, storage, and transportation; 2. The prepared multi-effect additive molecule contains a variety of functional groups, greatly enhancing the antioxidant and anti-wear properties of the lubricating oil. Its antioxidant effect helps to extend the service life of the lubricating oil; In summary, the lubricating oil prepared by the present invention has excellent antioxidant and anti-wear properties, a long service life, and good safety, and has important application value in the technical field of lubricating oils. Specific Embodiments
[0018] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts belong to the scope of protection of the present invention. Embodiment
[0019] Preparation of multi-effect additive: Step 1: Add 15.9 g of pentaerythritol and 16.7 g of phosphorus trichloride to a three-necked flask equipped with a thermometer, a mechanical stirrer, and a reflux condenser (connected to a tail gas absorption device to absorb the by-product HCl). After stirring evenly, heat with an oil bath, control the reaction temperature to be maintained at 155 °C, and carry out a reflux reaction until no hydrogen chloride gas is released. Then continue to raise the temperature to 165 °C and carry out an isothermal reaction for 2 h. After the reaction is completed, let it stand and cool to room temperature, extract with boiling water, remove the viscous substance deposited at the bottom of the flask by decantation, concentrate to remove part of the water, then cool and crystallize, filter to collect the crystals, and dry to obtain the reaction product A; Step 2: Add 13.6 g of pentaerythritol and 100 mL of anhydrous toluene to a three-necked flask equipped with a thermometer, a mechanical stirrer, a constant-pressure dropping funnel, and a reflux condenser (connected to a tail gas absorption device to absorb the by-product HCl). Then place the reaction system in an ice-water bath at 0 °C. While stirring, slowly drop 29.3 g of phosphorus trichloride through the constant-pressure dropping funnel. After the dropping is completed, remove the ice bath and heat the device until the temperature stabilizes at 77 °C, and carry out an isothermal reflux reaction for 3 h. After the reaction is completed, transfer the reaction solution to a rotary evaporator and perform rotary evaporation to obtain the reaction product B; Step 3: Add 27.8 g of reaction product A, 14.4 g of reaction product B, 15 mL of triethylamine, and 100 mL of anhydrous toluene to a three-necked flask equipped with a thermometer and a mechanical stirrer. After mechanical stirring evenly, heat the device until the temperature stabilizes at 65 °C, and carry out an isothermal reaction for 6 h. After the reaction is completed, filter, transfer the reaction solution to a rotary evaporator, perform rotary evaporation to remove part of the solvent, and then carry out column chromatography purification using a petroleum ether-ethyl acetate (10:1, v / v) elution system. Rotate and evaporate to remove the eluent to obtain the multi-effect additive. Embodiment
[0020] Preparation of multi-effect additive: Step 1: Add 31.8 g of pentaerythritol and 33.4 g of phosphorus trichloride into a three-necked flask equipped with a thermometer, a mechanical stirrer and a reflux condenser (connected to a tail gas absorption device to absorb the by-product HCl). After stirring evenly, heat with an oil bath, control the reaction temperature to be maintained at 155 °C, carry out reflux reaction until no hydrogen chloride gas is released, continue to raise the temperature to 165 °C, carry out constant temperature reaction for 2 h, complete the reaction, let it stand and cool to room temperature, extract with boiling water, remove the viscous substances deposited at the bottom of the flask by decantation, concentrate to remove part of the water, then cool and crystallize, filter by suction to collect the crystals, and dry to obtain reaction product A; Step 2: Add 27.2 g of pentaerythritol and 200 mL of anhydrous toluene into a three-necked flask equipped with a thermometer, a mechanical stirrer, a constant pressure dropping funnel and a reflux condenser (connected to a tail gas absorption device to absorb the by-product HCl). Then place the reaction system in an ice-water bath at 0 °C. While stirring, slowly add 58.6 g of phosphorus trichloride dropwise through the constant pressure dropping funnel. After the addition is completed, remove the ice bath, heat the device until the temperature is stable at 77 °C, carry out constant temperature reflux reaction for 3 h. After the reaction is completed, transfer the reaction solution to a rotary evaporator and carry out rotary evaporation to obtain reaction product B; Step 3: Add 55.6 g of reaction product A, 28.8 g of reaction product B, 30 mL of triethylamine and 200 mL of anhydrous toluene into a three-necked flask equipped with a thermometer and a mechanical stirrer. After mechanical stirring evenly, heat the device until the temperature is stable at 65 °C, carry out constant temperature reaction for 6 h. Complete the reaction, filter, transfer the reaction solution to a rotary evaporator, carry out rotary evaporation to remove part of the solvent, and then carry out column chromatography purification with a petroleum ether-ethyl acetate (10:1, v / v) elution system, and carry out rotary evaporation to remove the eluent to obtain the multi-effect additive. Example
[0021] Step 1: Add 98 - 112 g of olive oil into a reaction kettle, heat it to 40 - 50 °C, keep it warm for 2 min, then add 21 - 26 g of lithium stearate soap, and raise the temperature to 180 - 190 °C for refining for 10 min to obtain a pretreated base oil; Step 2: When the temperature in the reaction kettle drops to 40 - 60 °C, add 3 - 6 g of antioxidant 1010 and 5 - 10 g of the multi-effect additive prepared in Example 1, mix and stir at a rate of 100 - 200 r / min for 1 - 2 h, let it stand to room temperature, and grind to obtain an antioxidant lubricating oil. Example
[0022] Step 1: Add 98 - 112 g of soybean oil into a reactor, heat it to 40 - 50 °C, keep the temperature for 2 min, then add 21 - 26 g of calcium stearate soap, raise the temperature to 180 - 190 °C, and carry out refining for 10 min to obtain a pretreated base oil. Step 2: When the temperature in the reactor drops to 40 - 60 °C, add 3 - 6 g of antioxidant 1010 and 5 - 10 g of the multi - effect additive prepared in Example 2, mix and stir at a rate of 100 - 200 r / min for 1 - 2 h, let it stand to room temperature, and after grinding, obtain an antioxidant lubricating oil. Example
[0023] Step 1: Add 98 - 112 g of soybean oil into a reactor, heat it to 40 - 50 °C, keep the temperature for 2 min, then add 21 - 26 g of calcium stearate soap, raise the temperature to 180 - 190 °C, and carry out refining for 10 min to obtain a pretreated base oil. Step 2: When the temperature in the reactor drops to 40 - 60 °C, add 3 - 6 g of antioxidant 1010 and 5 - 10 g of the multi - effect additive prepared in Example 2, mix and stir at a rate of 100 - 200 r / min for 1 - 2 h, let it stand to room temperature, and after grinding, obtain an antioxidant lubricating oil.
[0024] Comparative Example 1 Different from Example 5, a commercially available phosphite antioxidant with the same mass is used to replace the multi - effect additive in Example 5, and the remaining steps are the same as those in Example 5 to prepare a lubricating oil.
[0025] Comparative Example 2 Use a commercially available antioxidant lubricating oil.
[0026] Perform the following performance tests on the lubricating oils of Examples 3, 4, 5 and Comparative Examples 1 and 2: Use NB / SH / T 0189 "Determination of Anti - wear Performance of Lubricating Oils - Four - Ball Method" to measure the wear scar diameter; Use SH / T 0325 "Method for Determining Oxidation Stability of Lubricating Greases" to measure the oxidation stability; The measured results are shown in the following table: Test Items Example 3 Example 4 Example 5 Comparative Example 1 Comparative Example 2 Wear Scar Diameter / mm (80°C, 1500 r / min, 60 min) 0.54 0.50 0.47 0.63 0.59 Oxidation Stability / kPa 26.1 25.3 24.6 39.5 31.9 As can be seen from the above table, the antioxidant and anti - wear properties of the lubricating oils prepared in the examples of the present invention are higher than those of the comparative examples. Therefore, the present invention has important application value in the technical field of lubricating oils.
[0027] In the description of the specification, the descriptions referring to terms such as "one embodiment", "example", "specific example", etc. mean that the specific features, structures, materials or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner.
[0028] The above content is only an illustration and explanation of the present invention. Those skilled in the art of this technology may make various modifications or supplements to the described specific embodiments or use similar ways to substitute, which should all fall within the protection scope of the present invention.
Claims
1. A preparation method of an antioxidant lubricating oil, characterized in that, It includes the following steps: Step 1: Add base oil into a reactor, heat it to 40 - 50 °C, keep it warm for 2 min, then add a thickening agent and conduct refining to obtain pretreated base oil; Step 2: When the temperature in the reactor drops to 40 - 60 °C, add an antioxidant and a multi - effect additive, mix and stir, let it stand until room temperature, and after grinding, obtain antioxidant lubricating oil.
2. The preparation method of an antioxidant lubricating oil according to claim 1, characterized in that, The multi - effect additive is prepared through the following steps: Step 1: Add pentaerythritol and phosphorus trichloride sulfide into a flask, stir evenly, then heat it in an oil bath and conduct a reflux reaction at 155 °C until no hydrogen chloride gas is released, react at 165 °C for 2 h, after the reaction is completed, cool, extract, concentrate, cool and crystallize, filter by suction, and dry to obtain reaction product A; Step 2: Add pentaerythritol and anhydrous toluene into a flask, in an ice - water bath at 0 °C, while stirring, dropwise add phosphorus trichloride, after the dropping is completed, conduct a reflux reaction at 77 °C for 3 h, after the reaction ends, perform rotary evaporation to obtain reaction product B; Step 3: Add reaction product A, reaction product B, triethylamine and anhydrous toluene into a flask, stir, and react at 65 °C for 6 h, after the reaction is completed, filter, perform rotary evaporation, purify by column chromatography, and perform rotary evaporation again to obtain the multi - effect additive.
3. The preparation method of an antioxidant lubricating oil according to claim 2, wherein, In Step 1, the dosage ratio of pentaerythritol to phosphorus trichloride sulfide is 15.9 g:16.7 g.
4. The preparation method of an antioxidant lubricating oil according to claim 2, characterized in that In Step 2, the dosage ratio of pentaerythritol, anhydrous toluene, and phosphorus trichloride is 13.6 g:100 mL:29.3 g.
5. The preparation method of an antioxidant lubricating oil according to claim 2, characterized in that, In Step 3, the dosage ratio of reaction product A, reaction product B, triethylamine, and anhydrous toluene is 27.8 g:14.4 g:15 mL:100 mL.
6. The preparation method of an antioxidant lubricating oil according to claim 1, characterized in that, Each raw material is as follows by mass fraction: 98 - 112 parts of base oil, 21 - 26 parts of thickening agent, 3 - 6 parts of antioxidant, and 5 - 10 parts of multi - effect additive.
7. The preparation method of an antioxidant lubricating oil according to claim 1, characterized in that, The base oil is one of olive oil, castor oil, soybean oil, and rapeseed oil.
8. The preparation method of an antioxidant lubricating oil according to claim 1, characterized in that, The thickening agent is one of lithium stearate soap, calcium stearate soap, and calcium 12 - hydroxystearate soap.
9. The preparation method of an antioxidant lubricating oil according to claim 1, characterized in that, The antioxidant is a hindered phenol antioxidant.
10. An antioxidant lubricating oil, characterized in that, Prepared according to the method described in any one of claims 1 - 9.