• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    For refining spent motor oils in order to recover lubricating bases to be reused, the stock to be refined is first stripped of water and light hydrocarbons, then a first extraction with a solvent (preferably a lower paraffin), heating the oil stripped of the solvent, distilling it under vacuum to separate light, medium and heavy lubricating bases, heating the heavier lubricating base and then extracting it with the same solvent as aforesaid, and sending the lubricating bases, separately and individually, to a hydrofinishing stage. The recycle to solvent extraction of the heavy bases affords the advantage of important heat savings and the possibility of adopting blander working conditions in the hydrofinishing of the heavier lubricating bases.
    公开号:SU969169A3
    申请号:SU792707554
    申请日:1979-01-11
    公开日:1982-10-23
    发明作者:Антонелли Серджо；Борза Микеле
    申请人:Снампрогетти С.П.А.；
    IPC主号:
    专利说明:

    () METHOD FOR REGENERATION OF SPREAD OILS
    I
    This invention relates to a process for the regeneration of used oils and, in particular, to a method for the regeneration of used motor oils.
    Known methods. Regeneration of used oils by treating them with sulfuric acid and bleaching clays.
    Such treatment leads to the need to remove spent clay and spent acid sludge due to contamination of the surrounding environment.
    There is a known method, when oil is regenerated by extraction with normal and paraffinic hydrocarbons, followed by catalytic hydrogenation of the resulting SJ.
    At the same time, due to the impossibility of half-removing by extraction of metal and organic impurities and oxidation products of this oil, in order to obtain products that meet the technical conditions, it is necessary
    the existence of at least one cycle of treatment with bleaching clays "
    However, in this case, the life of the hydrotreating catalysts is reduced.
    There is a method of regeneration of Hg worked oils, comprising the following stages; heating the oil to remove light fractions and water; mixing the dried oil with a saturated hydrocarbon solvent, for example propane, at an oil: solvent volume ratio of 1: 1–15 extraction, vacuum distillation of the separated oil, and hydrotreating the oil fractions {; 3j.
    However, the known method does not allow to obtain a heavy oil fraction of sufficiently high quality, which complicates and increases the cost of subsequent processing of these fractions.
    The purpose of the invention is to improve the quality of oils and increase the efficiency of the process. This goal is achieved by the fact that in the method of regenerating waste oils by heating the oils, distilling water and light fractions from the regenerated oil, extracting the latter with a saturated hydrocarbon solvent, vacuum distillation of the separated oil to obtain low viscosity and heavy fractions and hydrotreating the fractions, the heavy fraction It is preliminarily heat treated at a temperature of BOO-J JSO C under adiabatic conditions for 1-130 minutes and re-extracted with a saturated hydrocarbon solvent. The dilution ratio of the solvent and the 5-20: 1 fraction is with the separation of pure oil and residue, which is mixed with the recovered oil after the distillation of water and light fractions. Moreover, the first extraction of the recovered oil was carried out at a volume ratio of saturated hydrocarbon solvent and oil of 310: 1. According to the proposed method, the waste oil after preheating in the furnace at a temperature of 180-23 (0 is fed to the light fraction distillation column of the preliminary distillation column) in order to drive off water and light hydrocarbons from the specified oil. The product obtained after the distillation of water and light hydrocarbons is subjected to solvent extraction in order to remove the main fraction of the impurities contained in this oil. The most suitable solvents for this step are low molecular weight normal paraffinic hydrocarbons, in particular propane, although this extraction step can be carried out using any other solvent, such as alcohols, ketones, ethers, having corresponding molecules. A lot of weight, which may have a non-dissolving effect on the oil impurities and a dissolving effect on the oil itself. In the case of using propane, extraction can be carried out in an extraction not when moving countercurrently to the oil solvent and at a temperature of up to the critical temperature of propane, giving lenia 25 ° to 50 kg / cm. Since there is no need for this stage 4 to achieve the maximum degree of oil purification, the ratio of solvent to oil is usually very low, so that about 8 to 10 volumes of propane are needed per volume of oil. The oil, subjected to extraction in an extraction column, after subsequent heating, is fed to a fractionated distillation in vacuum, from which the main components of the lubricant are extracted in accordance with their viscosities. The main components of lubricating oil having low viscosity resulting from such distillation are sent directly to the final Hydrotreating section, while the residual distillate consisting of highly viscous main components of the oil containing the main fraction of impurities is heat treated temperature the component is usually from 300 to 50 ° C, and then oi is again recycled to the extraction column. This heat treatment of the highly viscous main components of the lubricating oil can also be carried out while maintaining the product leaving the column, vacuum fractional distillation, under adiabatic conditions for different periods of time from 1. to 120 minutes in accordance with the temperature. This operation is carried out by installing directly in the lower part of the column of the receiving tank (storage reserve), the volume of which depends on the storage time of the product in it. The purpose of such a heat treatment is to modify the structure of the impurities still present in the oil, so as to speed up their removal from the oil in the subsequent solvent extraction step. After this heat treatment, the heavy lubricant oil base components are again recycled to the solvent column. In this case, as well as in the case of the first extraction, propane is the preferred solvent, although other types of solvents may be used. The extraction column in this case may be exactly the same column that was used in the first extraction stage, and if so, this installation will work as a batch system, but a completely separate extraction column can also be used. The working conditions at this stage of the extraction are different from the working conditions created by the s stage of the first extraction, which is carried out using the entire amount of oil, sent to the extraction after the distillation of light fractions, because in this phase there is a reduced amount of impurities in the oil, in particular impurities that have capillary-active properties cause the process to be much more selective and much more different to different real estate properties. Operating conditions can vary within the following ranges: extraction temperature from to the critical temperature of propane; pressure from 25 to 50 kg / cm; and solvent otnonenie to oil. It can be such that from 5 to 20 volumes of propane per volume of oil. During the second stage, different process temperatures and different ratios of solvent to oil are allowed, since the second extraction involves not only to reduce the content of metallic impurities, but also to improve the color and thus reduce the harmful factors affecting the working conditions in the hydro cleaning section. The residual product obtained in the second extraction step with propane is recycled to the first extraction column in order to extract the contained oil from it. The main components of the lubricant obtained in the previous stages are subjected to final hydrotreatment in the presence of metal sulfide-based catalysts of groups 6 and 8 of the Mendeleev periodic system deposited on alumina. The hydrotreating temperature is 250A20 C, the pressure is 20-150 kg / cm, the volumetric flow rate is 0.1-5 v / v h, the hydrogen is recycled at a speed of 15-850 l /. The advantage of the proposed method in comparison with currently accepted methods is to reduce the amount of heat that must be consumed by the installation. Thermal treatment, carried out by the proposed method, in addition to being carried out only with heavy main components of lubricating oil, can provide under. keeping the same basic components at the temperature of the bottom of the vacuum distillation column, therefore, no additional heat is required. An additional advantage achieved by the proposed heat treatment method is to simplify the design of the heating furnace, since the waste oil must be heated fl «sb to a temperature of about 200 ° C, which is necessary to remove water and light hydrocarbons, since at this temperature the formation of acid gases is significantly reduced compared with the formation of such gases in the case of heat treatment at 300-5PS. The method of obtaining the highly viscous main components of lubricating oil, which is largely enhanced compared to conventional regeneration methods, also has very great advantages in the final stage of hydrotreating, which reduces the consumption of hydrogen and simultaneously increases the oil yield, and catalyst life is also increased. The drawing shows an installation diagram for carrying out the proposed method, in which the dotted lines refer only to the processing system of the heaviest fraction of the developed oil, in particular to the processing processes to which this fraction is subjected after thermal treatment; work This difference between the flow lines of the oil in the drawing is due to the fact that practically the implementation of the proposed method uses a single-column solvent extraction, and it is necessary to separate the solvent all the oil and solvent extraction aifl6onee heavy main components of lubricating oil. The waste oil from the storage tank is fed into the furnace 1 and then sent to the light ends distillation column 2. Water and light hydrocarbons are discharged through the top of the column, while the rest of the oil is removed from the bottom of the column 2 to the solvent extraction column 3 . The solvent is supplied to the extraction column 3 along the line, the oil and the main fraction of the solvent are removed from the top of this column through line 5, while the impurities and the rest of the solvent are removed from the bottom of column 3 through pipe 6. Both streams are removed from column 3, independently of each other. sent to devices 7 and 8 to regenerate the solvent, then this regenerated solvent via lines 9 and 10 is sent to compressor 11i, and then it is recycled through flow line 4. Partially purified oil is sent through line 12 to furnace 13 and then along lines 14 to the vacuum distillation column 15. Light hydrocarbons that can still remain in the oil are removed from the top of the column 15 through the pipe 16, and low-viscosity basic components are separated from the dye oil (as shown in the figure, reduced Up to two, but this does not have a limited limit of the number of rifts), along lines 17 and 18, the main low-viscosity components of the lubricating oil are independently fed into the hydrotreating reactor 19, from which the purified fractions are removed. From the lower part of the column 15, through tube 20, the heaviest main components of lubricating oil are removed, in which the boiling impurities are concentrated, and these heavy components of the oil are sent to the heat treatment system 21. After a certain period of time in the thermal belt processing, which is a function of temperature, the heavy components of the lubricating oil are fed, in line 22, to the solvent extraction column 3. Cdc is clear from this description, in the case of a process that is carried out initially, the extraction column 3 is properly used It is necessary both to extract the whole oil after lightly extracting light fractions from it, and to extract the heaviest basic components of the lubricating oil after heat treatment, and in this case, product storage reservoirs should be provided to ensure the implementation of such processes (these tanks -stores in the drawing are not shown so as not to introduce unnecessary complication in the presented installation scheme). If a continuous process is desired, it is sufficient to include in the system a second extraction column, equivalent to the first column. In this case, as well. and in the first solvent extraction, the heavy lubricant oil main components are withdrawn through the upper part of the extraction column 3, while the impurities and the remaining part of the solvent are withdrawn through the lower part of the column T (s 3 through pipe 24). solvent recovery units 7 and 8. Heavy bases. The lubricant components are removed from the bottom of the device 7 and fed through line 25 to the hydrotreating reactor, while residual product is removed from the bottom of the device 8 and sent (along the line 26) again in to Olive solvent extraction 3 as the starting product of processing, when this column 3 is used to extract the entire oil, resulting in the regeneration of the residual components of the oil, still mixed with impurities. Example 1. Used engine oil is subjected to a preliminary distillation of light fractions in order to free it from water and light hydrocarbons, the residue from this distillation of light fractions is subjected to heat treatment at a temperature of a temuror; a round for 3 minutes, and then this product is directed to the extraction of propane th column in the RAC extraction. The separation conditions used in this processing step are as follows: solvent: oil ratio 10: 1; temperature of the upper part of the column 90 С: temperature of the lower, temperature. the pressure of the column 38 kg / cm. Extracted oil after separation of propane is subjected to fractional vacuum distillation to extract several major components of the lubricant from it in accordance with their viscosities. Three main components of the lubricant are obtained: low, medium and high viscosity; and at the same time receive a certain amount of gas oil vacuum distillation. Low-viscous and medium-sized basic components of lubricating oil are independently and independently processed by hydrogen treatment using a catalyst based on nickel and molybdenum sulfides supported on alumina. In this processing stage, the following operating conditions are used: temperature pressure lO kg / cm volumetric product flow rate, 1 rpm; hydrogen recirculation rate of 168 norms, l / l. The heavy components of the lubricant are treated with hydrogen using the same catalyst, but under the following operating conditions TeMnepatypa pressure Q kg / her volumetric flow rate of the product | 0.5 v / rev; the recirculation rate (hydrogen is 168 normal liters / l. The results obtained at all stages of the treatment are presented in Table 1. PRI mme R 2. Exhausted motor oil is subjected to f hydrocarbons, the residual product is directed to the extraction by the propellant in the DS extraction column. The operating conditions used at this stage of processing are as follows: solvent: oil ratio 7: 1: temperature of the upper part of the column 90 C; temperature of the lower part of the column 70 pressure 38 kg / cm. Extracted oil After regeneration, propane is subjected to fractionated vacuum distillation to extract several axial components of lubricant IB according to their relative viscosities, thereby obtaining three main components of lubricant: low, medium and high viscosity. Highly viscous main component. subjected to heat treatment at a temperature of 15 minutes and then sent to the column with extraction with propane. In this case, the working conditions are used: solvent to oil ratio 15: 1; temperature of the upper part of the column 85 P; The bottom temperature of the column pressure is 38 kg / cm. Extracted oil after propane regeneration is subjected to fractionated vacuum distillation to extract several bases from it. components of a lubricant in accordance with their relative viscosities, and three main components of a lubricant are obtained: low, medium and high viscosity. Highly viscous main component is subjected to heat treatment at. temperature for 15 minutes and then sent to the extraction column with propane. In this case, the following operating conditions are used: solvent to oil ratio 15: 1; temperature of the upper part of the column is 85 ° C; bottom temperature: 73 ° С; pressure 38 kg / cm. The light and medium-sized main components of lubricating oil, obtained in the vacuum distillation stage, are independently processed by hydrogen using a catalyst based on nickel and molybdenum sulfides supported on alumina (as a carrier). The following operating conditions are used in this processing step: temperature pressure 0 kg / cm; volumetric flow rate of the product 1 v / v; hydrogen recycling rate of 168 Nl / l. The heavy (high viscous) main components of the fairytale oil, coming out of the solvent extraction column, after the removal of propane from them, are treated with hydrogen using the same catalyst as above, but under the following operating conditions: temperature pressure 40 kg / cm; volumetric flow rate of the product is 0.5 vol / hour; hydrogen recycling rate of 168 Nl / l. The outputs and properties of the products obtained in the individual stages of processing are given in table. 2. Comparison of these two technological operations, described above, shows that the heavy main components of the lubricant prepared by the proposed method have a lower content of impurities and have better characteristics.
    11969169.2
    colors, in connection with what in the subsequent processing (at the same time the metal technological process of the hydro-cleaning mixture is deposited on the surface as softer working analyzers are required), then the processing ability
    conditions, products having a lower rust content, since the durability of catalysts for color variations makes it possible to see
    The final stage of hydrotreating of the Bi stage, the working conditions and as a result
    depends on the presence of metal at 31st to increase the service life of catalysus in the material subjected to the flow. ,
    权利要求:
    Claims (3)
    [1]
    5 impurities and having the best results , because of the fact that, in order to improve the quality of the oils and improve the ecoomomicity of the process: the heavy fraction is previously subjected to heat treatment at ZOb-AzO C in adiab 1ticheskih conditions for 1120 minutes and re-extraction in .syschennym hydrocarbon solvent at a volume ratio of 20 rastvr9 erator and fractions of 5-20: 1 with the separation of pure oil and a residue which is mixed with regenerable oil after removal of water, and light ends. 2, the method according to claim 1, wherein the extraction of the regenerated oil is carried out at a volume ratio of saturated hydrocarbon solvent and oil of 310: 1. Sources of information, taken into account in the examination of KP Attorney USA If 029569, class, 208-180, published. 1977.
    [2]
    2. For France No. 2301592, class C 10 M 11/00, published. 1976.
    [3]
    3. US patent number 3919076, cl. 208-180, published. 1975 (prototype).
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    IT19203/78A|IT1091961B|1978-01-12|1978-01-12|PROCEDURE FOR THE REGENERATION OF WASTE OILS|
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