CN112574776B - Refining process of regenerated crude oil - Google Patents
Refining process of regenerated crude oil Download PDFInfo
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- CN112574776B CN112574776B CN202011237079.1A CN202011237079A CN112574776B CN 112574776 B CN112574776 B CN 112574776B CN 202011237079 A CN202011237079 A CN 202011237079A CN 112574776 B CN112574776 B CN 112574776B
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
- C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
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Abstract
The invention relates to a process for refining reclaimed crude oil, wherein the design of heat exchange between liquid-phase base oil of a stripping tower, crude base oil and a solvent avoids the waste of energy sources and achieves the effect of energy conservation; the use of the centrifugal unit can ensure that the light phase and the heavy phase are separated more thoroughly; the process according to the invention has reasonable design and simple and practical flow, and is suitable for the refining process of the crude oil solvent of the base oil; the obtained finished base oil has good performance, the yield of the base oil can reach more than 95%, the recovery rate of the solvent can reach more than 99%, and the recovered solvent can be recycled for multiple times, so that resource recycling and recycling economy are realized.
Description
Technical Field
The invention belongs to the field of environmental protection and resource recycling, and particularly relates to a refining process of waste mineral oil regenerated crude oil.
Background
The reclaimed crude oil (hereinafter referred to as "crude oil") refers to an oil product which is extracted from waste mineral oil by a process such as distillation and which has not been subjected to refining. Because the processing process of the crude oil is simpler, the oil still contains more impurities such as colloid, asphaltene and the like and non-ideal components, and the existence of the substances can influence the low-temperature fluidity, the oxidation stability and the like of the lubricating oil. Therefore, in order to obtain a qualified lubricant base oil, it is necessary to refine the crude oil to remove undesirable substances in the crude oil and to improve the quality of the base oil, thereby improving the performance of the lubricant.
The existing crude oil re-refining technology comprises solvent refining, clay refining and hydrorefining. Wherein, the clay refining technology can generate a large amount of waste clay in the production process, which easily causes the problems of secondary pollution and the like. The hydrorefining technology needs a large amount of hydrogen in the production process, the operation conditions are harsh, the process is complex, and the equipment investment scale is large. Meanwhile, secondary pollutants such as acidic water and acidic gas can be generated in the production process. In contrast, solvent refining is industrially more applied due to the characteristics of mature technology, simple process, small secondary pollution and the like.
Although solvent refining has been used in many cases in the field of crude oil re-refining technology, it has some disadvantages. For example, in the solvent recovery process, there are often technical limitations such that the solvent recovery is not thorough, causing a large loss of solvent, thereby increasing the purification cost. Meanwhile, in the solvent refining process, a phenomenon of incomplete separation may occur in the separation process of a heavy phase solution (a mixed solution of a solvent and an undesirable component in crude oil, also called a solvent phase) and a light phase solution (base oil), and finally the obtained base oil still contains a small amount of solvent and an undesirable component, so that the performance of the lubricating oil base oil is influenced.
Disclosure of Invention
The present invention is to solve at least one of the problems of the prior art, and provides a solvent refining process for crude oil regenerated from waste mineral oil.
The crude oil mentioned in the patent of the present invention refers to an oil product which is extracted from waste mineral oil by distillation and other processes and is not refined, and generally comprises first-line crude oil (150 SN base oil crude oil), second-line crude oil (250 SN base oil crude oil) or third-line crude oil (350 SN base oil crude oil).
The process scheme of the invention is as follows:
(1) Crude oil refining process
1) The crude oil enters a heat exchanger 1, exchanges heat with a heating medium, and is pumped to a centrifugal unit.
According to a preferred embodiment of the present invention, the temperature of the crude oil after heat exchange is selected from 60 to 70 ℃.
According to a preferred embodiment of the present invention, the crude oil preferably enters the heat exchanger after being flow-buffered by the buffer tank 1.
2) Mixing the crude oil entering the centrifugal machine set with a solvent, and performing centrifugal separation.
Because the solvent has higher solubility to undesired components such as colloid, asphaltene and the like in the crude oil and has lower solubility to the base oil, the solvent can dissolve the undesired components such as the colloid, the asphaltene and the like to form a mixed solution after the crude oil is mixed with the solvent, the density of the mixed solution is higher than that of the base oil, and the mixture and the base oil can be separated under the action of a centrifugal machine.
In order to achieve better mixing and separating effects, the flow direction sequence of the solvent in the centrifugal pump group is opposite to that of the crude oil (for example, the centrifugal pump groups are numbered as a No. 1 centrifugal pump, a No. 2 centrifugal pump and a No. 3 centrifugal pump, and if the flow direction sequence of the solvent is the No. 1 centrifugal pump, the No. 2 centrifugal pump and the No. 3 centrifugal pump, the flow direction sequence of the crude oil is the No. 3 centrifugal pump, the No. 2 centrifugal pump and the No. 1 centrifugal pump).
According to a preferred embodiment of the present invention, wherein the solvent used is selected from one of furfural, N-methylpyrrolidone (NMP) and phenol; NMP is preferred.
According to a preferred embodiment of the present invention, the solvent is subjected to heat exchange in a heat exchanger 3 before being mixed with the crude oil.
According to another preferred embodiment of the present invention, the solvent is buffered by a buffer tank 3 before heat exchange.
3) Light components (mainly base oil, also called base oil components) separated from the centrifuge component are heated by a heat exchanger 2 and then enter a wiped film evaporator 1, a small part of solvent mixed in the base oil can be heated into steam under the action of the wiped film evaporator, at the moment, the steam components enter a cooler 1 to be condensed into liquid, and then flow into a mixing agent tank after passing through a buffer tank 2.
The liquid phase component exiting the wiped film evaporator still contains a small amount of solvent and, according to a preferred embodiment of the invention, is preferably fed to a stripper for further separation by a steam stripping operation.
The gas phase substances separated from the stripping tower mainly comprise water vapor and solvent vapor, the vapor substances are condensed into liquid under the action of the cooler 2, and then the liquid enters the oil-water separation tank to separate the solvent and the water. The solvent separated from the oil-water separation tank enters the mixing tank 2, and the oily wastewater is sent to a sewage treatment plant for treatment. The liquid phase base oil stripped by the stripping tower is divided into two paths, one path of base oil returns to the heat exchanger 1 to be used as a heat source substance to exchange heat with crude oil, and the other path of base oil with a small amount of liquid phase enters the heat exchanger 3 to exchange heat with a solvent and enters a finished product base oil storage tank.
(2) Solvent recovery process
Heavy phase solution (undesirable components in solvent and crude oil) components in the centrifugal unit pass through the buffer tank 4 and enter the heat exchanger 4, and heat conduction oil is adopted as a heating medium in the heat exchanger 4. The heavy phase solution is heated to a certain temperature and then conveyed to the wiped film evaporator 2 through a pump. The heavy phase solution is further heated in the wiped film evaporator 2, and the solvent component in the heavy phase solution is heated and evaporated into steam, and then enters a reduced pressure recovery tower for further purification. The liquid phase in the wiped film evaporator 2 is mainly the heavy components such as colloid, asphaltene and the like in the crude oil, and can be sold as finished product extract oil after being cooled in the cooler 4 and passing through the buffer tank.
The gas phase of the wiped film evaporator 2 enters a reduced pressure recovery tower, and the gas phase substance at the top of the tower is condensed into liquid through a cooler 3 and enters a mixing tank; the middle part of the tower body is provided with a lateral line, pure solvent can be obtained by fractionation, and the pure solvent enters a solvent tank through a buffer tank 5. The liquid phase at the bottom of the tower is mainly a solvent containing a very small amount of base oil, and the solvent enters the mixing tank.
In the present invention, the solvent recovery efficiency is high. After the solvent is recovered, the total recovery rate can reach more than 99.5 percent.
According to a preferred embodiment of the invention, the centrifuge train is a combination of 2 or more centrifuges, the order of passage of the crude oil and solvent to the centrifuges being reversed, primarily as the location for both mixing and light-heavy separation.
According to another preferred embodiment of the invention, the heat exchanger comprises a heat exchanger 1, a heat exchanger 2, a heat exchanger 3 and a heat exchanger 4, and the heat exchangers are all tube heat exchangers. Wherein, the heat exchanger 1 exchanges heat between the liquid phase component (the base oil of which the solvent is removed by the stripping operation) of the stripping tower and the crude oil, and the heat exchanger 3 exchanges heat between the liquid phase component (the base oil of which the solvent is removed by the stripping operation) of the stripping tower and the solvent. The heat exchanger 2 and the heat exchanger 4 both adopt heat conduction oil as a heat source for heat exchange.
According to another preferred embodiment of the invention, the wiped film evaporator 1 and the wiped film evaporator 2 adopt jacketed heaters, and heat conducting oil is filled in the jacketed heaters, so that a heat source can be provided for evaporation.
According to another preferred embodiment of the invention, the stripping tower and the decompression recovery tower adopt a packed tower, stainless steel pall ring packing is filled in the packed tower, and a contact carrier is provided for gas-liquid two phases; the stripping tower is provided with a steam generating device to provide superheated steam for the stripping tower; and a hole is formed in the middle of the tower body of the reduced pressure recovery tower, and a lateral line is led out for recovering the solvent.
According to another preferred embodiment of the present invention, the cooler comprises a cooler 1, a cooler 2, a cooler 3 and a cooler 4, wherein the cooler is a tubular heat exchanger, and water is used as a cooling medium to further cool the gas phase substance into liquid.
According to another preferred embodiment of the present invention, the solvent tank is used for receiving the solvent separated by the decompression recovery tower, and the solvent can be directly recycled as pure solvent.
According to another preferred embodiment of the present invention, the mixture tank is used for receiving the cooled gas phase substances of the wiped film evaporator 1, the stripping tower and the reduced pressure recovery tower, and the liquid phase substance at the bottom of the reduced pressure recovery tower, and the liquid in the mixture tank is a solvent containing a small amount of colloid and asphaltene. The solvent in the mixing tank enters a buffer tank of the centrifugal unit to be used as closed cycle (because the purity of the solvent in the mixing tank is not high than that of the solvent in the solvent tank, and the amount of the solvent obtained in the mixing tank is far less than that of the solvent obtained in the solvent tank in the production process, therefore, in the production, in order to avoid the solvent waste, the solvent in the mixing tank can be recycled together with the purer solvent in the solvent tank according to the production requirement), and the solvent waste is avoided.
The invention has the following beneficial effects:
the process design is reasonable, the flow is simple and practical, and the method is suitable for the refining process of the crude oil solvent of the base oil; the design of heat exchange between the liquid-phase base oil of the stripping tower, the crude base oil and the solvent avoids the waste of energy sources, and the energy-saving effect is achieved; the use of the centrifugal unit can ensure that the light phase and the heavy phase are separated more thoroughly; the obtained finished base oil has good performance, the yield of the base oil can reach more than 95%, the recovery rate of the solvent can reach more than 99%, and the recovered solvent can be recycled for multiple times, so that resource utilization and recycling economy are realized.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be further described with reference to the following embodiments.
First-line crude oil (150 SN base oil crude oil) extracted by a certain company through reduced pressure distillation is taken as a raw material, and NMP (N-methyl pyrrolidone) is used as a solvent for refining.
The feedstock properties are shown in table 1 below. The detection shows that the crude oil has high content of nitride and aromatic hydrocarbon, low viscosity index and low content of saturated hydrocarbon, and influences the low-temperature fluidity, oxidation stability and the like of the lubricating oil. The crude oil is refined by using the crude oil refining process of the invention, and the specific steps are as follows:
(1) The first thread crude oil enters the heat exchanger 1 after passing through the buffer tank and exchanges heat with a heating medium in the heat exchanger. The crude oil is heated to 60-70 ℃ and then enters a centrifugal unit under the action of a centrifugal pump.
(2) The centrifugal machine set can be formed by connecting 2 or more centrifugal machines in series according to actual conditions. Crude oil enters from an inlet of the centrifugal machine, flows forwards according to the sequence of the centrifugal machines connected in series, a solvent flows reversely according to the sequence of the centrifugal machine sets, and the crude oil and the solvent are in reverse contact in the centrifugal machine sets to be mixed. Under the action of a centrifugal machine, undesirable components such as colloid, asphaltene and the like in the crude oil can be dissolved in a solvent to form a mixed solution, the density of the mixed solution is higher than that of the base oil, and the mixed solution and the base oil can be separated under the action of the centrifugal machine.
(3) The mixed liquid is separated into light components and heavy components in the centrifuge group. Wherein, the light components are heated to 155-165 ℃ in the heat exchanger 2 by utilizing heat conducting oil and enter the wiped film evaporator 1, at the moment, the solvent components in the base oil are heated into steam under the action of the wiped film evaporator 1 and enter the cooler 1 to be condensed into liquid, and the liquid flows into the mixing tank after passing through the buffer tank. The liquid phase component flowing out of the wiped film evaporator 1 still contains a small amount of solvent and needs to be further separated by steam stripping operation. The wiped film evaporator 1 is operated under negative pressure and is provided with a vacuum pump set, and the pressure is controlled below 2000Pa.
(4) The stripping column is equipped with a steam generator to provide superheated steam to the stripping column. The gas phase substances separated from the top of the stripping tower mainly comprise water vapor and solvent vapor, the vapor substances are condensed into liquid under the action of the cooler 2, and then the liquid enters the oil-water separation tank, so that the solvent and the water are separated. The solvent separated from the oil-water separation tank enters a mixing tank, and the water is sent to a sewage treatment plant for treatment. The liquid phase base oil stripped by the stripping tower is divided into two paths, one path of base oil returns to the heat exchanger 1 to be used as a heat source substance to exchange heat with crude oil, and the other path of base oil with a small amount of liquid phase is sent to the heat exchanger 3 to exchange heat with a solvent, and then the finished product 150SN base oil is obtained.
As can be seen from Table 1, the 150SN base oil obtained by the solvent refining of the embodiment has significantly improved related physical parameters, and completely reaches the standard of the lubricating oil base oil. After the crude oil is refined by the solvent, the proportion of the obtained base oil can reach more than 96 percent, the rest 4 percent is extract oil, and the extract oil can also be sold as a product.
Meanwhile, the NMP in the above embodiment is recycled through the solvent recovery process, and the specific steps are as follows:
(1) The solvent enters a heat exchanger 3 after passing through a buffer tank, and enters a centrifugal unit after being heated to 60-70 ℃ in the heat exchanger.
(2) NMP and first-line crude oil are separated into light components and heavy components under the action of a centrifugal unit. Wherein, the recombination branch enters the heat exchanger 4 after being buffered by the buffer tank. The heat exchanger 4 adopts heat conducting oil as a heating medium, and the solution is conveyed to the wiped film evaporator 2 under the action of a solution pump after being heated to 260-270 ℃. NMP is further heated in a wiped film evaporator, and the solvent in the solution is heated and evaporated into steam, and then enters a reduced pressure recovery tower for further purification. The liquid phase in the wiped film evaporator is mainly undesired components such as colloid asphaltene in crude oil, and can be stored or sold as finished product extract oil after passing through a buffer tank.
(3) The gas phase material entering the decompression recovery tower reversely contacts with the reflux liquid from the tower top in the tower, and the gas phase material at the tower top is condensed into liquid through a cooler 3 and enters the mixing tank. The middle part of the tower body is provided with a lateral line, pure solvent is obtained through fractionation, and the pure solvent enters a solvent tank through a buffer tank. The liquid phase at the bottom of the tower is mainly a solvent containing a small amount of base oil and enters a mixing tank.
(4) The wiped film evaporator 1, the wiped film evaporator 2, the stripping tower and the decompression recovery tower are all operated under negative pressure, and the internal pressure of the stripping tower is enabled to reach below 2000Pa under the action of the vacuum pump group.
(5) In the invention, the heat exchanger comprises a heat exchanger 1, a heat exchanger 2, a heat exchanger 3 and a heat exchanger 4, the cooler comprises a cooler 1, a cooler 2, a cooler 3 and a cooler 4, and both the heat exchanger and the cooler can adopt tube type heat exchangers; the working process of each heat exchanger and cooler is as follows:
(1) the heat exchanger 1: when the crude base oil enters, the crude base oil is at normal temperature, exchanges heat with the liquid phase of the stripping tower, and then is heated to 60-70 ℃ and discharged from the heat exchanger; the liquid phase of the stripping tower enters at the temperature of 200 ℃, exchanges heat with crude base oil and then is cooled to about 120 ℃ and then is discharged from the heat exchanger.
(2) And (3) heat exchanger 2: the entry temperature of the light phase component of the centrifugal unit is 60-70 ℃, and the light phase component is discharged out of the heat exchanger after exchanging heat with heat-conducting oil and heating to 155-165 ℃.
(3) And (3) heat exchanger: when the solvent enters the heat exchanger, the temperature is normal temperature, the solvent exchanges heat with the liquid phase of the stripping tower and then is heated to 60-70 ℃ to be discharged out of the heat exchanger; the liquid phase of the stripping tower enters at the temperature of 200 ℃, exchanges heat with crude base oil and then is cooled to about 120 ℃ and then exits from the heat exchanger.
(4) And (4) heat exchanger: the temperature of the heavy phase component of the centrifugal unit is 60-70 ℃, and the heavy phase component is heated to 260-270 ℃ after exchanging heat with the heat-conducting oil and then discharged out of the heat exchanger.
(5) The cooler 1: the gas phase components of the wiped film evaporator are fed at the temperature of 110-120 ℃, condensed and cooled to 40-50 ℃ and discharged out of the cooler.
(6) The cooler 2: the gas-phase components of the stripping tower are fed at the temperature of 110-120 ℃, condensed and cooled to 40-50 ℃ and then discharged out of the cooler.
(7) The cooler 3: the gas-phase components at the top of the vacuum tower enter at the temperature of 110-120 ℃, are condensed and cooled to 40-50 ℃, and are discharged out of the cooler.
(8) The cooler 4: the liquid phase component of the wiped film evaporator is fed at the temperature of 250-260 ℃, condensed and cooled to 40-50 ℃ and then discharged out of the cooler.
The solvent recovery process is used for recycling, the recovery rate of the solvent can reach more than 99.5%, and the recovered solvent can be recycled for multiple times, so that resource recycling and recycling economy are realized.
TABLE 1 physical Properties data sheet of crude and base oils
| Test examples | 150SN crude oil | 150SN base oil |
| Appearance of the product | Light yellow | Is transparent |
| Colour intensity | 3.0 | 0.3 |
| Kinematic viscosity (40 ℃ C.)/m 2 /s | 34 | 24 |
| Kinematic viscosity (100 ℃ C.)/m 2 /s | 5.3 | 4.7 |
| Open flash point (. Degree.C.) | 180 | 220 |
| Pour point (. Degree. C.) | -5 | -15 |
| Sulfur content (%) | 0.48 | 0.13 |
| Nitrogen compound (ppm) | 520 | 24 |
| Aromatic hydrocarbons (%) | 17 | 8 |
| Saturated hydrocarbon (%) | 64.9 | 83.8 |
Claims (8)
1. The refining process of the regenerated crude oil solvent is characterized by comprising the following steps of:
1) The crude oil is sent to a centrifugal unit after heat exchange;
2) Mixing crude oil entering a centrifugal unit with a solvent, and performing centrifugal separation, wherein the solvent is N-methylpyrrolidone; the centrifugal unit in the step 2) is formed by connecting two or more centrifuges in series, and the flow direction sequence of the solvent and the crude oil in the centrifugal pump set is opposite;
3) Heating the light components separated in the step 2) through a heat exchanger 2, then feeding the light components into a wiped film evaporator 1, evaporating the light components to remove the solvent, then feeding the light components into a stripping tower to perform steam stripping operation to further separate the solvent to obtain base oil, dividing the liquid-phase base oil stripped by the stripping tower into two paths, returning one path of the liquid-phase base oil to the heat exchanger 1 as a heat source substance to perform heat exchange with crude oil, feeding a small amount of the liquid-phase base oil to a heat exchanger 3 to perform heat exchange with the solvent, and feeding the small amount of the liquid-phase base oil into a finished product base oil storage tank;
4) Heating the heavy phase solution component separated in the step 2) through a heat exchanger 4, then feeding the heated heavy phase solution component into a wiped film evaporator 2, heating and evaporating the solvent component in the heavy phase solution into steam, and then feeding the steam into a reduced pressure recovery tower for further purification; the liquid phase in the wiped film evaporator 2 is mainly heavy components in crude oil and is used as finished product extract oil after being cooled;
wherein, in the step 4), the gas phase substance at the top of the decompression recovery tower is condensed into liquid and enters the mixing tank; a lateral line is arranged at the middle part of the tower body, and pure solvent can be obtained by fractionation; the liquid phase at the bottom of the tower is a solvent containing a very small amount of base oil, and the part of the solvent enters a mixing tank; the solvent in the mixing tank enters the centrifugation step of the step 2) for recycling.
2. The solvent refining process for regenerated crude oil according to claim 1, wherein in step 1), the crude oil passes through the buffer tank and then enters the heat exchanger 1 for heat exchange.
3. The solvent refining process for reclaimed crude oil according to claim 1, wherein the wiped film evaporator 1, the wiped film evaporator 2 and the reduced pressure recovery tower are all operated at negative pressure, and the internal pressure is less than 4000Pa.
4. The solvent refining process for regenerated crude oil according to claim 3, wherein the internal pressure of the reduced pressure recovery column is less than 3000Pa.
5. The solvent refining process for regenerated crude oil according to claim 3, wherein the internal pressure of the reduced pressure recovery column is less than 2000Pa.
6. The solvent refining process of recycled crude oil according to claim 1, wherein the wiped film evaporator 1 and the wiped film evaporator 2 are jacketed heaters filled with heat transfer oil to provide a heat source for evaporation.
7. The solvent refining process for regenerated crude oil according to any one of claims 1 to 6, wherein the heat exchanger 1, the heat exchanger 2, the heat exchanger 3 and the heat exchanger 4 are tubular heat exchangers.
8. The solvent refining process for regenerated crude oil according to any one of claims 1 to 6, wherein the vacuum recovery tower is a packed tower and is filled with stainless steel pall ring packing.
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| CN107513458A (en) * | 2017-09-05 | 2017-12-26 | 江苏川钿电气机械有限公司 | The refined renovation process of waste lubricating oil |
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| CN111394123A (en) * | 2020-04-21 | 2020-07-10 | 云南新昊环保科技有限公司 | Process for refining regenerated base oil of lubricating oil from waste mineral oil solvent |
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