Preparation process of hydrogenation catalyst for regeneration of waste lubricating oil

Abstract

The invention belongs to the technical field of catalyst preparation, and particularly relates to a waste lubricating oil regeneration hydrogenation catalyst preparation process, which comprises: S1, mixing and stirring a raw material and an auxiliary agent for 10 min, adding a prepared solution, and carrying out mixing kneading for a period of time to obtain a bulk material; and S2, extruding the bulk material into strips, standing for 6-10 hours, transferring into a muffle furnace, drying for 4 hours, heating to high temperature, and roasting for 4 hours to obtain the catalyst carrier. And S3, mixing and impregnating the prepared impregnation liquid with the catalyst carrier obtained in the step S2, drying for 4 hours, and roasting for 4 hours at a high constant temperature to obtain a catalyst product. The catalyst has good hydrogenation dearomatization performance on waste lubricating oil, the aromatic hydrocarbon removal rate is 90% or above, the activity period is one year or above, and the performance is stable.

Description

Technical Field

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

[0002] Lubricating oil is extracted from crude oil and is composed of base oil, some chemical additives and other compounds. Lubricating oil is widely used in industry and is called the blood of vehicles, machinery and industrial equipment. my country's economic development is becoming more and more rapid, the scale of industrialization is growing, and the demand for lubricating oil is also increasing. However, during the use of lubricating oil, the hydrocarbon components in the oil will deteriorate due to excessive temperature or sealing. In addition, impurities such as moisture and dust will also cause lubricating oil to deteriorate.

[0003] Waste lubricating oil is oil that has been used and is contaminated and slightly deteriorated. In order to save resources and realize the recycling and reuse of lubricating oil, the current treatment methods mainly include physical refining and chemical refining. The physical refining method has the defects of incomplete removal of impurities and poor refining effect. The chemical refining method mainly uses acid to react with impurities in waste lubricating oil to treat lubricating oil. This method has a simple process and low cost, but the treatment process pollutes the environment and is highly corrosive to equipment. At present, my country's waste lubricating oil regeneration technology is still in its infancy, and the theoretical research on waste oil treatment and regeneration is relatively weak. The intellectual property technology from laboratory research to practical application is even more insufficient. Therefore, based on the existing characteristics of my country, research and development of waste lubricating oil processing technology has important theoretical significance and practical value. Summary of the invention

[0004] In view of the problems existing in the background technology, the present invention provides a preparation process of a catalyst used for hydrogenation and dearomatization in the process of waste lubricating oil treatment. The catalyst product can effectively treat aromatic compounds in waste lubricating oil, convert them into alkanes, increase the viscosity of the product, improve the chromaticity of the product, have high processing efficiency and strong processing capacity.

[0005] To achieve the above object, the present invention adopts the following technical solutions:

[0006] A waste lubricating oil regeneration hydrogenation catalyst preparation process, the catalyst carrier used raw materials are macroporous pseudo-boehmite, additives, nitric acid, citric acid, deionized water, soluble tungsten salt, molybdenum salt and nickel salt.

[0007] Preferably, the pseudo-boehmite raw material has a specific surface area of ​​240-280m 2 / g, and the pore volume is 0.9-1.2ml / g.

[0008] Preferably, the auxiliary agent includes sesbania powder and hydroxymethyl cellulose.

[0009] Preferably, the steps for preparing the waste lubricating oil regeneration hydrogenation catalyst are:

[0010] (1) After the raw materials and the auxiliary agent are mixed and stirred for 10 minutes, the prepared solution is added thereto and kneaded for a period of time to obtain a mass-like material.

[0011] (2) After the lumps are extruded, the lumps are allowed to stand for 6-10 hours, and then transferred to a muffle furnace, dried at 50-100°C for 4 hours, and then heated to 500-800°C at a certain rate and calcined at a constant temperature for 4 hours to obtain a catalyst carrier.

[0012] (3) The prepared impregnation liquid is mixed and impregnated with the catalyst support obtained in step (2) for 1 hour, then dried at 50-100°C for 4 hours, and then heated to 300-500°C at a rate of 3°C / min and calcined at a constant temperature for 4 hours to obtain a catalyst product.

[0013] Further preferably, in step (1), the solution is prepared by mixing deionized water with nitric acid and citric acid, and the mixing time is 1 hour.

[0014] Further preferably, in step (2), a 2.0 mm cloverleaf-shaped module is selected in the extruder to extrude a cloverleaf-shaped catalyst carrier, and the heating rate is 3-5° C. / min.

[0015] Further preferably, the preparation of the impregnation solution in step (3) is to add deionized water to the soluble tungsten salt, molybdenum salt and nickel salt to fully dissolve them to prepare a stable impregnation solution.

[0016] Preferably, the catalyst product contains the active components of tungsten oxide 18-23%, molybdenum oxide 8-12%, nickel oxide 4-5%, and silicon oxide 1-3%, based on 100% by weight of the catalyst.

[0017] Compared with the prior art, the present invention has the following advantages:

[0018] The catalyst product provided by the present invention has a specific surface area of ​​100-140m 2 / g, pore volume 0.3-0.4ml / g, pore diameter 15-21nm, reaction pressure 13MPa-15MPa, reaction temperature 270-320℃. The catalyst has good hydrogenation and dearomatization performance for waste lubricating oil, aromatic removal rate over 90%, active period over one year, and stable performance. DETAILED DESCRIPTION

[0019] The following embodiments of the technical solution of the present invention are described in detail in conjunction with the embodiments. The following embodiments are only used to more clearly illustrate the technical solution of the present invention, and are therefore only used as examples, and cannot be used to limit the protection scope of the present invention.

[0020] It should be noted that the experimental methods used in the implementation examples are all conventional methods unless otherwise specified; the materials, reagents, etc. used, unless otherwise specified, can be obtained from commercial channels.

[0021] Example 1

[0022] Place macroporous pseudo-boehmite together with sesbania powder and hydroxymethyl cellulose in a kneader and mix and stir for 10 minutes. Take deionized water together with nitric acid and citric acid to prepare a solution, then add the prepared solution to the kneader and knead for 1 hour until the product is a lump material. Transfer the prepared lump material to the extruder, select a 2.0mm clover-shaped module, extrude it into a clover catalyst carrier, let it stand for 6 hours, then transfer it to a muffle furnace, dry it at 50°C for 4 hours, and then heat it to 500°C at a rate of 3°C / min and calcine it at a constant temperature for 4 hours to obtain a catalyst carrier; add deionized water to the soluble tungsten salt, molybdenum salt and nickel salt to fully dissolve them to prepare a stable impregnation solution, mix the prepared impregnation solution with the above-obtained catalyst carrier in a fixed ratio for 1 hour, then dry it at 50°C for 4 hours, and then heat it to 300°C at a rate of 3°C / min and calcine it at a constant temperature for 4 hours to obtain a catalyst product.

[0023] Example 2

[0024] The macroporous pseudo-boehmite, sesbania powder and hydroxymethyl cellulose were placed in a kneader and mixed for 10 minutes. Deionized water was taken together with nitric acid and citric acid to prepare a solution, and then the prepared solution was added to the kneader and kneaded for 1 hour until the product was a mass material. The prepared mass material was transferred to the extruder, and a 2.0mm clover-shaped module was selected to extrude into a clover catalyst carrier, which was left to stand for 6 hours, and then transferred to a muffle furnace, dried at 50°C for 4 hours, and then heated to 500°C at a rate of 5°C / min and calcined at a constant temperature for 4 hours to obtain a catalyst carrier; deionized water was added to the soluble tungsten salt, molybdenum salt and nickel salt to fully dissolve and prepare a stable impregnation solution, and the prepared impregnation solution was mixed and impregnated with the catalyst carrier obtained above in a fixed ratio for 1 hour, and then dried at 50°C for 4 hours, and then heated to 300°C at a rate of 3°C / min and calcined at a constant temperature for 4 hours to obtain a catalyst product.

[0025] Example 3

[0026] Place macroporous pseudo-boehmite together with sesbania powder and hydroxymethyl cellulose in a kneader and mix and stir for 10 minutes. Take deionized water together with nitric acid and citric acid to prepare a solution, then add the prepared solution to the kneader and knead for 1 hour until the product is a lump material. Transfer the prepared lump material to the extruder, select a 2.0mm clover-shaped module, extrude it into a clover catalyst carrier, let it stand for 6 hours, then transfer it to a muffle furnace, dry it at 50°C for 4 hours, and then heat it to 800°C at a rate of 3°C / min and calcine it at a constant temperature for 4 hours to obtain a catalyst carrier; add deionized water to the soluble tungsten salt, molybdenum salt and nickel salt to fully dissolve them to prepare a stable impregnation solution, mix the prepared impregnation solution with the above-obtained catalyst carrier in a fixed ratio for 1 hour, then dry it at 50°C for 4 hours, and then heat it to 400°C at a rate of 3°C / min and calcine it at a constant temperature for 4 hours to obtain a catalyst product.

[0027] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein by equivalents. These modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present invention, and they should all be included in the scope of the claims and specification of the present invention.

Claims

1. A process for preparing a waste lubricating oil regeneration hydrogenation catalyst, wherein the raw materials used for the catalyst carrier are macroporous pseudo-boehmite, an additive, nitric acid, citric acid, deionized water, a soluble tungsten salt, a molybdenum salt and a nickel salt.

2. A waste lubricating oil regeneration hydrogenation catalyst preparation process according to claim 1, characterized in that: The raw material pseudo-boehmite has a specific surface area of ​​240-280m 2 / g, and the pore volume is 0.9-1.2ml / g.

3. A waste lubricating oil regeneration hydrogenation catalyst preparation process according to claim 1, characterized in that: The auxiliary agents include sesbania powder and hydroxymethyl cellulose.

4. The process for preparing a waste lubricating oil regeneration hydrogenation catalyst according to claim 1, characterized in that: The steps of preparing the waste lubricating oil regeneration hydrogenation catalyst are as follows: (1) After the raw materials and the auxiliary agent are mixed and stirred for 10 minutes, the prepared solution is added thereto and kneaded for a period of time to obtain a mass material; (2) After the lumps are extruded, they are allowed to stand for 6-10 hours, then transferred to a muffle furnace, dried at 50-100° C. for 4 hours, and then heated to 500-800° C. at a certain rate and calcined at a constant temperature for 4 hours to obtain a catalyst carrier; (3) The prepared impregnation liquid is mixed and impregnated with the catalyst support obtained in step (2) for 1 hour, then dried at 50-100°C for 4 hours, and then heated to 300-500°C at a rate of 3°C / min and calcined at a constant temperature for 4 hours to obtain a catalyst product.

5. A waste lubricating oil regeneration hydrogenation catalyst preparation process according to claim 4, characterized in that: The solution in step (1) is prepared by mixing deionized water with nitric acid and citric acid, and the mixing time is 1 hour.

6. A waste lubricating oil regeneration hydrogenation catalyst preparation process according to claim 4, characterized in that: In step (2), a 2.0 mm cloverleaf-shaped module is selected in the extruder and extruded into a cloverleaf-shaped catalyst carrier at a heating rate of 3-5° C. / min.

7. A waste lubricating oil regeneration hydrogenation catalyst preparation process according to claim 4, characterized in that: The preparation of the impregnation solution in step (3) is to add deionized water to the soluble tungsten salt, molybdenum salt and nickel salt to fully dissolve them to prepare a stable impregnation solution.

8. The process for preparing a waste lubricating oil regeneration hydrogenation catalyst according to claim 1, characterized in that: The catalyst product contains the active components of 18-23% tungsten oxide, 8-12% molybdenum oxide, 4-5% nickel oxide and 1-3% silicon oxide based on 100% catalyst weight.

9. The process for preparing a waste lubricating oil regeneration hydrogenation catalyst according to claim 1, characterized in that: The specific surface area of ​​the prepared catalyst product is 100-140m 2 / g, pore volume 0.3-0.4ml / g, pore diameter 15-21nm, reaction pressure 13MPa-15MPa, reaction temperature 270-320℃.