Waste wind power lubricating oil hydrogenation catalyst, preparation method and application

Abstract

The invention discloses a waste wind power lubricating oil hydrogenation catalyst, a preparation method and its application in waste wind power lubricating oil regeneration base oil, belonging to the technical field of waste wind power lubricating oil regeneration. The catalyst is a shell-type Pd@γ‑Al 2 O 3 Catalyst. The use of the catalyst in the regeneration of base oil from waste wind power lubricating oil comprises: subjecting the waste wind power lubricating oil to a vacuum distillation and a low-temperature short-range critical molecular distillation in sequence to obtain a crude base oil; adding the crude base oil and the catalyst to a reactor for kettle-type hydrogenation and quality improvement to obtain a regenerated base oil. The present invention adopts a low-temperature short-range critical molecular distillation combined with kettle-type hydrogenation refining and quality improvement, which is simple to prepare and not easy to be poisoned. It can effectively reduce the coking and scaling problems of waste wind power lubricating oil on the inner wall of the evaporator, and can greatly extend the working time of the device. Shell-type Pd@γ‑Al 2 O 3 The catalyst can greatly reduce the amount of Pd used, improve the Pd dispersion and atomic utilization, and enhance the hydrogenation effect.

Description

Technical Field

[0001] The invention belongs to the technical field of waste wind power lubricating oil regeneration, and in particular relates to a waste wind power lubricating oil hydrogenation catalyst, a preparation method and application of the catalyst in waste wind power lubricating oil regeneration base oil. Background Art

[0002] Wind power generation can effectively improve the dependence of traditional power generation on energy sources such as oil and coal, optimize the energy structure and realize the diversification of energy sources. It is a renewable and environmentally friendly way of power generation. For a long time, the wind power industry has been facing the problem of premature failure of key components, which is related to its harsh working environment and inconvenient on-site maintenance. In order to minimize the premature failure of wind power equipment under extreme load and environmental conditions, the use of lubricants with excellent performance to lubricate and reduce wear is one of the most effective solutions. Therefore, higher requirements are placed on the performance and service life of equipment lubricants. According to experience, after 3 to 5 years of operation, wind power equipment begins to enter a period of frequent failures, and key components such as gearboxes and generators begin to have problems of varying degrees. The oil used in the related lubrication system also needs to be replaced. When waste lubricating oil is used for a long time under high temperature and complex working conditions, the low-temperature fluidity, viscosity, oxidation resistance, clean dispersibility, wear resistance, rust resistance, and corrosion resistance of the lubricating oil will be seriously deteriorated, resulting in a sharp decline in its performance. Therefore, the resource reuse of waste wind power lubricating oil is of great significance to promoting sustainable development and building a conservation-oriented society.

[0003] Through monitoring and testing of wind power lubricating oil, it was found that the main pollutants of wind power lubricating oil are particles, moisture, and oil deterioration oxidation products. Physical purification methods can be used to remove particles and moisture, but after oxidation and deterioration, only physical and chemical methods can be used for combined treatment. At present, the regeneration processes of waste lubricating oil in China mainly include distillation-pickling-white clay refining, sedimentation-distillation-pickling-calcium clay refining, and sedimentation-flocculation-white clay refining. However, the above processes are prone to secondary pollution to the environment, and the comprehensive utilization rate and quality of waste lubricating oil are relatively low (Ren Qiaolin, Huang Wanyi, Zhang Wei, et al. Preparation and performance study of chitosan silica-alumina gel adsorbent for transformer oil regeneration [J]. Journal of Hubei Institute of Engineering, 2023, 43(06): 15-18.). The existing technology has put forward clear requirements for the regeneration process route of waste lubricating oil. Existing or newly built waste lubricating oil processing enterprises need to use solvent refining or hydrofining as the final product route. For example, by using hydrofining technology, water, sulfur, nitrogen, chlorine, oxygen and various additives can be removed by physical and chemical methods in the presence of hydrogen to obtain lubricating oil base oil and gasoline and diesel blending components that meet the requirements of National V (Ren Qiaolin, Wang Yanzhen, Zhang Wei, et al. Research on Hydrogenation Regeneration Process of Transformer Waste Oil [J]. Petroleum Refining and Chemical Engineering, 2023, 54(10): 73-77.). However, due to the different sources and complex components of waste lubricating oil, the process has certain adaptability and selectivity, especially wind power lubricating oil, which is mainly composed of fully synthetic lubricating oil, which is quite different from traditional waste lubricating oil in terms of components, especially catalysts, which are very easy to be poisoned, and it is necessary to screen catalysts with strong adaptability. Therefore, the use of traditional regeneration processes will face great challenges. (Li Zixia, Zhang Xianming, Chen Ligong, et al. Research progress in waste lubricating oil regeneration technology[J]. Journal of Chongqing Technology and Business University (Natural Science Edition), 2021, 38(05): 10-16.)

[0004] Therefore, how to provide a waste lubricating oil regeneration process technology with advanced technology, low pollution and low cost is a technical problem that technical personnel in this field urgently need to solve, so as to be able to produce high-quality and stable recycled base oil, realize the transformation of waste lubricating oil into treasure, and contribute to the sustainable development of resources. Summary of the invention

[0005] The purpose of the present invention is to provide a waste wind power lubricating oil hydrogenation catalyst, a preparation method and its application in the regeneration base oil of waste wind power lubricating oil, so as to produce high-quality and stable regenerated base oil by a waste lubricating oil regeneration process with low pollution and low cost.

[0006] To achieve the above object, the present invention adopts the following technical solution:

[0007] In a first aspect, the present invention provides a method for preparing a waste wind power lubricating oil hydrogenation catalyst, comprising:

[0008] Step 1: γ-Al 2 O 3 The ball, palladium salt, acetone, impregnation solution and auxiliary agent are fully mixed and evaporated to dryness, and then dried to obtain a dry sample;

[0009] Step 2: The obtained dry sample is calcined in an air bath, then reduced in a hydrogen bath, and finally aged in a mixed atmosphere of air and nitrogen to obtain a shell-type Pd@γ-Al 2 O 3 Hydrogenation catalysts.

[0010] Wherein, the palladium salt is one of palladium chloride, palladium nitrate, palladium acetate, palladium sulfate, triisodecyl trimellitate / palladium (II), propylpalladium (II) dimer and palladium (II) propionate.

[0011] The solubility of different palladium salts in the impregnation solution is different to adjust the palladium content in γ-Al 2 O 3 The dispersion of the ball surface and the thickness of the shell can maximize the efficiency of the catalyst.

[0012] Wherein, the γ-Al 2 O 3 The diameter of the sphere is 1-5 mm. By adjusting the diameter of the sphere, shell-type Pd@γ-Al with different sizes can be prepared. 2 O 3 catalyst.

[0013] Wherein, the impregnation liquid is one or a combination of ethyl acetate, acetonitrile, dichloromethane, acetone and toluene.

[0014] The solubility of the palladium salt can be regulated by the polarity and viscosity of the solvent, and then the thickness of the shell (Pd) can be regulated, thereby regulating the catalytic hydrogenation performance, so that the prepared shell-type Pd@γ-Al 2 O 3 Catalysts can achieve their maximum performance.

[0015] Wherein, the auxiliary agent is one or a combination of water, methanol, ethanol, isopropanol and n-butanol.

[0016] The polarity and viscosity of the impregnation solution can be precisely controlled by additives, thereby finely adjusting the shell (Pd) thickness. The adjustment of the shell (Pd) thickness is conducive to reducing the amount of Pd, thereby saving costs and achieving high dispersion in the spherical γ-Al with the least amount of Pd. 2 O 3 surface to maximize catalytic performance.

[0017] Step 1 specifically includes: 2 O 3After the balls, palladium salt, acetone, impregnation solution and additives are fully mixed, they are fully mixed and evenly mixed on a 70°C shaker and evaporated to dryness. The obtained sample is placed in a 100°C oven for further drying to obtain a dry sample.

[0018] In step 2, the calcination temperature in the air bath is 500° C. and the calcination time is 3 h; the calcination temperature in the hydrogen bath is 350° C. and the calcination time is 3 h; and the aging time in the mixed atmosphere of air and nitrogen is 1 h.

[0019] Palladium salt loaded on γ-Al by "modification-impregnation" method 2 O 3 The preparation of shell-type Pd@γ-Al2O3 catalyst on the surface of the sphere can enhance the mechanical strength and reduction degree of the catalyst, which is beneficial to the construction of active sites. At the same time, the shell-type catalyst can prepare the highest dispersion Pd@γ-Al2O3 with the least amount of Pd. 2 O 3 Catalyst to achieve maximum hydrogenation.

[0020] In a second aspect, the present invention provides a waste wind power lubricating oil hydrogenation catalyst prepared by the preparation method described in any one of the first aspects, wherein the catalyst is composed of γ-Al 2 O 3 spheres and evenly distributed in γ-Al 2 O 3 The surface layer of the ball is composed of metal Pd.

[0021] In a third aspect, the present invention provides the use of a waste wind power lubricating oil hydrogenation catalyst in the regeneration base oil of waste wind power lubricating oil, including:

[0022] The waste wind power lubricating oil is sequentially subjected to primary vacuum distillation and low-temperature short-range critical molecular distillation to obtain a crude base oil;

[0023] The crude base oil and waste wind power lubricating oil hydrogenation catalyst are added into a reactor, hydrogen is introduced into the reactor, and the temperature is increased to perform a catalytic hydrogenation reaction to obtain a regenerated base oil.

[0024] Furthermore, the temperature of the primary reduced pressure distillation is 50-100° C., and the vacuum degree is 0.02-0.04 MPa.

[0025] Furthermore, the temperature of the low-temperature short-range critical molecular distillation is 200-250° C., the vacuum degree is 10-40 Pa, and the scraping stirring speed is 200-400 rpm.

[0026] Furthermore, the temperature of the catalytic hydrogenation reaction is 200-300° C., the reaction time is 1-6 h, and the hydrogen pressure is 3-5 MPa.

[0027] Furthermore, the ratio of the added amount of the waste wind power lubricating oil hydrogenation catalyst to the crude base oil is 1g:50mL.

[0028] Through a single vacuum distillation, light components and light toxic substances in waste lubricating oil can be removed, which can minimize costs and avoid secondary degradation of oil products. Through short-range critical molecular distillation, while ensuring efficiency and oil quality, the impact of high temperature on secondary degradation of oil products can be greatly reduced. Therefore, physical pollutants are first removed through two-step distillation to prevent catalyst poisoning in the subsequent hydrogenation process. Finally, the shell-type Pd@γ-Al 2 O 3 The catalyst is used to hydrogenate crude lubricating base oil to obtain regenerated lubricating base oil. The crude base oil can be hydrogenated under relatively "mild" conditions. The process flow is relatively simple, easy to operate, and easy to apply on a large scale.

[0029] Compared with the prior art, the present invention has the following beneficial effects:

[0030] The present invention adopts the "modification-impregnation" method to prepare shell-type Pd@γ-Al 2 O 3 Hydrogenation catalyst, using the polarity and viscosity of the impregnation solution, or further fine-tuning the polarity and viscosity of the impregnation solution through additives, the impregnation solution "pulls" the palladium salt "into" the carrier γ-Al 2 O 3 Inside the sphere, in the γ-Al 2 O 3 The active center is constructed on the surface of the ball, achieving the minimum amount of Pd, and Pd is highly dispersed in the carrier γ-Al 2 O 3 The shell layer can maximize the catalytic hydrogenation effect. By adjusting the polarity and viscosity of the impregnation solution and the solubility of the palladium salt, the shell thickness can be further adjusted, thereby adjusting the hydrogenation performance. 2 O 3 The hydrogenation catalyst has certain anti-poisoning performance through the construction of the shell structure. In the present invention, the use of precious metal Pd to hydrogenate waste oil has significant innovation and superiority. Compared with non-precious metal catalysts, precious metal Pd has the advantages of good hydrogenation performance and mild hydrogenation conditions.

[0031] The present invention adopts a low-temperature short-range critical molecular distillation combined with kettle-type hydrofining to improve the quality, and can obtain high-quality base oil by distillation and hydrofining at a relatively low temperature (<250°C); and the operating temperature of the distillation system is lower than that of the conventional vacuum distillation device, the vacuum degree is higher than that of the molecular distillation, and the hydrogenation reaction device is simple; the catalyst is easy to prepare and not easy to be poisoned. At the same time, the low-temperature short-range critical molecular distillation in the present invention can effectively reduce the coking and scaling problems of waste wind power lubricating oil on the inner wall of the evaporator, which can greatly extend the working time of the device.

[0032] In addition, the present invention can realize waste oil regeneration in the absence of solvent, reducing the separation production cost caused by the solvent, and the solvent-free hydrogenation process is simple and easy to apply on a large scale. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 is the H of the catalyst precursor in Examples 1-3 of the present invention 2 -TPR graph;

[0034] Figure 2 is the XRD diagram of the catalyst in Examples 1-3 of the present invention;

[0035] Figure 3 is a nitrogen adsorption and desorption isotherm diagram of the catalyst in Examples 1-3 of the present invention;

[0036] Figure 4 is the pore size distribution diagram of the catalyst in Examples 1-3 of the present invention;

[0037] Figure 5 TEM images and cross-sectional images of the catalysts in Examples 1-3 of the present invention;

[0038] Figure 6 This is a process flow chart of regenerating base oil from waste wind power lubricating oil of the present invention;

[0039] Figure 7 This is a color comparison diagram of waste wind power lubricating oil, crude base oil, and lubricating base oil obtained after hydrogenation in Example 4 of the present invention;

[0040] Figure 8 This is a color comparison diagram of waste wind power lubricating oil, crude base oil, and lubricating base oil obtained after hydrogenation in Example 5 of the present invention;

[0041] Fig. 9 This is a color comparison chart of waste wind power lubricating oil, crude base oil and lubricating oil base oil obtained after hydrogenation in Example 6 of the present invention. DETAILED DESCRIPTION

[0042] The present invention will be further described below in conjunction with specific examples. The following examples are only used to more clearly illustrate the technical solutions of the present invention, and are not intended to limit the scope of protection of the present invention.

[0043] It should be noted that, unless otherwise specified, the technical terms or scientific terms used in this application should have the common meanings understood by those skilled in the art to which the present invention belongs.

[0044] Unless otherwise specified, the raw materials in the examples of the present invention were purchased from commercial sources.

[0045] The waste wind power lubricating oil in the embodiment of the present invention comes from the heavy-duty waste wind power gear oil replaced from a wind power oil farm, and its chemical composition is a fully synthetic lubricating oil mainly composed of poly-alpha-olefin (PAO).

[0046] Unless otherwise specified, the room temperature in the embodiments of the present invention refers to 25±2°C.

[0047] Example 1

[0048] A method for preparing a waste wind power lubricating oil hydrogenation catalyst comprises the following steps:

[0049] (1) 0.08 g of palladium chloride, 50 mL of acetone, 3.7 mL of methanol and 5 g of γ-Al with a diameter of 1 mm were added. 2 O 3 After the balls are fully mixed, they are thoroughly mixed by shaking at 70°C and evaporated to dryness. The dry sample is placed in an oven at 100°C to continue drying to obtain the final dry sample.

[0050] (2) The final dry sample obtained in step (1) was placed in a tube furnace, and the temperature was raised from room temperature to 500°C at a rate of 2°C / min under a 70mL air bath, and the temperature was maintained for 3h, and finally cooled to room temperature in an air bath. After the catalyst was cooled to room temperature, 1g of the sample was placed in a tube furnace, high-purity hydrogen was introduced at a rate of 70mL / min, and the temperature was raised from room temperature to 350°C at a rate of 2°C / min, and maintained for 3h. After the reaction was completed, it was cooled to room temperature in a hydrogen bath, and then aged in 1% air and 99% nitrogen for 1h to obtain 1Pd@γ-Al 2 O 3 Hydrogenation catalysts.

[0051] pass Figure 1 (H 2 -TPR) shows that the obtained sample can be completely reduced at 130 °C; Figure 2 (XRD) shows that 1Pd@γ-Al 2 O 3 The hydrogenation catalyst contains only metal Pd and γ-Al 2 O 3 physical phase; through Figure 3 (N 2 It can be known from the adsorption and desorption that 1Pd@γ-Al 2 O3 The catalyst has a pore structure and forms an obvious hysteresis loop; Figure 4 (Pore size distribution diagram) shows that 1Pd@γ-Al 2 O 3 The catalyst pore size distribution is 3nm; Figure 5 (TEM and cross-section) It can be seen that 1Pd@γ-Al 2 O 3 The Pd in ​​the catalyst is evenly distributed and forms a shell structure, but the shell thickness is significantly different from that of the other two catalysts. According to ICP measurement, the actual loading amount of metal Pd is 0.9834%.

[0052] Example 2

[0053] A method for preparing a waste wind power lubricating oil hydrogenation catalyst comprises the following steps:

[0054] (1) 0.11 g of palladium acetate, 50 mL of toluene, 4.2 mL of isopropanol and 5 g of γ-Al with a diameter of 2 mm were mixed. 2 O 3 After the balls are fully mixed, they are thoroughly mixed by shaking at 70°C and evaporated to dryness. The dry sample is placed in an oven at 100°C to continue drying to obtain the final dry sample.

[0055] (2) The final dry sample obtained in step (1) was placed in a tube furnace, and the temperature was raised from room temperature to 500°C at a rate of 2°C / min under a 70mL air bath, and the temperature was maintained for 3h, and finally cooled to room temperature in an air bath. After the catalyst was cooled to room temperature, 1g of the sample was placed in a tube furnace, high-purity hydrogen was introduced at a rate of 70mL / min, and the temperature was raised from room temperature to 350°C at a rate of 2°C / min, and maintained for 3h. After the reaction was completed, it was cooled to room temperature in a hydrogen bath, and then aged in 1% air and 99% nitrogen for 1h to obtain 2Pd@γ-Al 2 O 3 Hydrogenation catalysts.

[0056] pass Figure 1 (H 2 -TPR) shows that the obtained sample can be completely reduced at 130°C; Figure 2 (XRD) shows that 2Pd@γ-Al 2 O 3 The catalyst contains only metal Pd and γ-Al 2 O 3 physical phase; through Figure 3 (N 2 It can be known from the adsorption and desorption that 2Pd@γ-Al 2 O 3 The catalyst has a pore structure and forms an obvious hysteresis loop; Figure 4 (Pore size distribution diagram) shows that 2Pd@γ-Al 2 O 3 The catalyst pore size distribution is 3nm; Figure 5 (TEM and cross-sectional view) It can be seen that 2Pd@γ-Al 2 O 3 The Pd in ​​the catalyst is evenly distributed and forms a shell structure, but the shell thickness is significantly different from that of the other two catalysts. According to ICP measurement, the actual loading amount of metal Pd is 1.0037%.

[0057] Example 3

[0058] A method for preparing a waste wind power lubricating oil hydrogenation catalyst comprises the following steps:

[0059] (1) 0.12 g of palladium (II) propionate, 50 mL of ethyl acetate, 6.3 mL of n-butanol, and 5 g of γ-Al with a diameter of 1 mm were added. 2 O 3 After the balls are fully mixed, they are thoroughly mixed by shaking at 70°C and evaporated to dryness. The dry sample is placed in an oven at 100°C to continue drying to obtain the final dry sample.

[0060] (2) The final dry sample obtained in step (1) was placed in a tube furnace, and the temperature was raised from room temperature to 500°C at a rate of 2°C / min under a 70mL air bath condition, and the temperature was kept for 3h, and finally cooled to room temperature in an air bath. After the catalyst was cooled to room temperature, 1g of the sample was placed in a tube furnace, high-purity hydrogen was introduced at a rate of 70mL / min, and the temperature was raised from room temperature to 350°C at a rate of 2°C / min, and maintained for 3h. After the reaction was completed, it was cooled to room temperature in a hydrogen bath, and then aged in 1% air and 99% nitrogen for 1h to obtain a 3Pd@γ-Al2O3 hydrogenation catalyst.

[0061] pass Figure 1 (H 2 -TPR) shows that the obtained sample can be completely reduced at 130°C; Figure 2 (XRD) shows that 3Pd@γ-Al 2 O 3 The catalyst contains only metal Pd and γ-Al 2 O 3 physical phase; through Figure 3 (N 2 It can be known from the adsorption and desorption that 3Pd@γ-Al 2 O 3 The catalyst has a pore structure and forms an obvious hysteresis loop; Figure 4 (Pore size distribution diagram) shows that 3Pd@γ-Al 2 O3 The catalyst pore size distribution is 3nm; Figure 5 (TEM and cross-section) It can be seen that 3Pd@γ-Al 2 O 3 The Pd in ​​the catalyst is evenly distributed and forms a shell structure, but the shell thickness is significantly different from that of the other two catalysts. According to ICP measurement, the actual loading amount of metal Pd is 1.1002%.

[0062] like Figure 6 As shown, the process flow of regenerating base oil from waste wind power lubricating oil of the present invention comprises: pre-treating the waste wind power lubricating oil to remove moisture, particles and impurities therein; subjecting the pre-treated waste wind power lubricating oil to a reduced pressure distillation to remove light components or impurities; subjecting the obtained oil product to a low-temperature short-range critical molecular distillation to remove the residual oil to obtain a crude base oil; and subjecting the crude base oil to a kettle-type hydrogenation upgrading using a waste wind power lubricating oil hydrogenation catalyst to obtain a regenerated base oil.

[0063] Example 4

[0064] The pretreated waste wind power lubricating oil is subjected to a reduced pressure distillation, the distillation temperature is 60°C, and the vacuum degree is 0.02Mpa; the obtained oil product is further subjected to low-temperature short-range critical molecular distillation, and the 250°C fraction oil is collected to obtain a crude base oil, wherein the distillation temperature is 250°C and the vacuum degree is 10Pa. A high-precision peristaltic pump is used to control the feed of the pretreated waste wind power lubricating oil, the feed rate is 60rpm, and the low-temperature short-range critical molecular distillation scraping film stirring speed is 400rpm. Figure 7 It can be seen that the color of the crude base oil obtained after molecular distillation becomes significantly lighter.

[0065] 1g of 1Pd@γ-Al prepared in Example 1 2 O 3 The hydrogenation catalyst was added to the reactor, and then 50 mL of the crude base oil was added. The reactor was sealed and H 2 Replace the air in the reactor and continue to introduce 4MPa of H 2 Then the temperature of the reactor was raised to 300°C and the reaction was continued for 4 hours. After the reaction was completed, the temperature was lowered to room temperature and the catalyst was separated by filtration. Figure 7 As shown, the color changes to colorless.

[0066] The properties, physical and chemical indicators and testing standards of the above-mentioned raw oil (i.e. waste wind power lubricating oil), crude base oil and lubricating oil base oil obtained after hydrogenation are shown in Table 1.

[0067] Table 1: Physical and chemical indicators of wind power oil before and after regeneration

[0068]

[0069]

[0070] Example 5

[0071] The pretreated waste wind power lubricating oil is subjected to a reduced pressure distillation, the distillation temperature is 50°C, and the vacuum degree is 0.04Mpa; the obtained oil product is further subjected to low-temperature short-range critical molecular distillation, and the 200°C fraction oil is collected to obtain a crude base oil, wherein the distillation temperature is 200°C and the vacuum degree is 40Pa. A high-precision peristaltic pump is used to control the feed of the pretreated waste wind power lubricating oil, the feed rate is 60rpm, and the low-temperature short-range critical molecular distillation scraping film stirring speed is 200rpm. Figure 8 It can be seen that the color of the crude base oil obtained after molecular distillation becomes significantly lighter.

[0072] 1 g of 2Pd@γ-Al prepared in Example 2 2 O 3 The hydrogenation catalyst was added to the reactor, and then 50 mL of the crude base oil was added. The reactor was sealed and H 2 Replace the air in the reactor and continue to introduce 3MPa of H 2 Then the temperature of the reactor was raised to 280°C and the reaction was continued for 5 hours. After the reaction was completed, the catalyst was separated by filtration after the temperature dropped to room temperature. The obtained oil was Figure 8 As shown, the color changes to colorless.

[0073] The properties of the above-mentioned raw oil (i.e., waste wind power lubricating oil), crude base oil, and lubricating oil base oil obtained after hydrogenation were tested. The physical and chemical indicators and testing standards of the oil products are shown in Table 2.

[0074] Table 2: Physical and chemical indicators of wind power oil before and after regeneration

[0075]

[0076]

[0077] Example 6

[0078] The pretreated waste wind power lubricating oil is subjected to a reduced pressure distillation, the distillation temperature is 80℃, and the vacuum degree is 0.04Mpa; the obtained oil product is further subjected to low-temperature short-range critical molecular distillation, and the 230℃ fraction oil is collected to obtain a crude base oil, wherein the distillation temperature is 230℃ and the vacuum degree is 20Pa. A high-precision peristaltic pump is used to control the feed of the pretreated waste wind power lubricating oil, the feed rate is 60rpm, and the low-temperature short-range critical molecular distillation scraping film stirring speed is 200rpm. Fig. 9 It can be seen that the color of the crude base oil obtained after molecular distillation becomes significantly lighter.

[0079] 1 g of 3Pd@γ-Al prepared in Example 3 2 O 3 Catalyst hydrogenation catalyst was added to the reactor, and 50 mL of the obtained crude base oil was added. The reactor was sealed and H 2 Replace the air in the reactor and continue to introduce 5MPa of H 2 Then the temperature of the reactor was raised to 260°C and the reaction was continued for 6 hours. After the reaction was completed, the temperature was cooled to room temperature and the catalyst was separated by filtration. Fig. 9 As shown, the color changes to colorless.

[0080] The properties of the above-mentioned raw oil (i.e., waste wind power lubricating oil), crude base oil, and lubricating oil base oil obtained after hydrogenation were tested. The physical and chemical indicators and testing standards of the oil products are shown in Table 3.

[0081] Table 3: Physical and chemical indicators of wind power oil before and after regeneration

[0082]

[0083]

[0084] The present invention has been disclosed above with preferred embodiments, but they are not intended to limit the present invention. Any technical solutions obtained by adopting equivalent replacement or equivalent transformation solutions fall within the protection scope of the present invention.

Claims

1. Application of a waste wind power lubricating oil hydrogenation catalyst in the regeneration base oil of waste wind power lubricating oil, characterized in that: include: The waste wind power lubricating oil is sequentially subjected to primary vacuum distillation and low-temperature short-range critical molecular distillation to obtain a crude base oil; Add crude base oil and waste wind power lubricating oil hydrogenation catalyst into a reactor, introduce hydrogen into the reactor, increase the temperature to carry out catalytic hydrogenation reaction, and obtain regenerated base oil; the temperature of the catalytic hydrogenation reaction is 200-300°C, and the hydrogen pressure is 3-5MPa; The method for preparing the waste wind power lubricating oil hydrogenation catalyst comprises: The γ-Al2O3 ball, palladium salt, acetone, impregnation liquid and auxiliary agent are fully mixed and evaporated to dryness, and then dried to obtain a dry sample; the diameter of the γ-Al2O3 ball is 1-5 mm; the impregnation liquid is one or a combination of ethyl acetate, acetonitrile, dichloromethane, acetone and toluene; The obtained dry sample was calcined in an air bath at 500 °C for 3 h, then reduced in a hydrogen bath at 350 °C for 3 h, and finally aged in a mixed atmosphere of air and nitrogen to obtain a shell-type Pd@γ-Al2O3 hydrogenation catalyst with a pore size of 3 nm.

2. The use of the waste wind power lubricating oil hydrogenation catalyst in the regeneration base oil of waste wind power lubricating oil according to claim 1, characterized in that: The temperature of the primary reduced pressure distillation is 50-100°C, and the vacuum degree is 0.02-0.04MPa.

3. The use of the waste wind power lubricating oil hydrogenation catalyst in the regeneration base oil of waste wind power lubricating oil according to claim 1, characterized in that: The temperature of low-temperature short-range critical molecular distillation is 200-250°C, the vacuum degree is 10-40Pa, and the scraping stirring speed is 200-400rpm.

4. The use of the waste wind power lubricating oil hydrogenation catalyst in the regeneration base oil of waste wind power lubricating oil according to claim 1, characterized in that: The catalytic hydrogenation reaction time is 1-6h.

5. The use of the waste wind power lubricating oil hydrogenation catalyst in the regeneration base oil of waste wind power lubricating oil according to claim 1, characterized in that: The ratio of the added amount of waste wind power lubricating oil hydrogenation catalyst to the crude base oil is 1g:50mL.

6. The use of the waste wind power lubricating oil hydrogenation catalyst in the regeneration base oil of waste wind power lubricating oil according to claim 1, characterized in that: The palladium salt is one of palladium chloride, palladium nitrate, palladium acetate, palladium sulfate, triisodecyl trimellitate / palladium (II), propylpalladium (II) dimer and palladium (II) propionate.

7. The use of the waste wind power lubricating oil hydrogenation catalyst in the regeneration base oil of waste wind power lubricating oil according to claim 1, characterized in that: The auxiliary agent is one or a combination of water, methanol, ethanol, isopropanol and n-butanol.

8. The use of the waste wind power lubricating oil hydrogenation catalyst in the regeneration base oil of waste wind power lubricating oil according to claim 1, characterized in that: The catalyst consists of gamma-Al2O3 balls and metal Pd uniformly distributed on the surface of the gamma-Al2O3 balls.

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