CN115491224A - Method for recovering dewaxing solvent in light lubricating oil base oil filtrate - Google Patents
Method for recovering dewaxing solvent in light lubricating oil base oil filtrate Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- 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
- C10G31/00—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for
- C10G31/11—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for by dialysis
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- C—CHEMISTRY; METALLURGY
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1037—Hydrocarbon fractions
- C10G2300/1062—Lubricating oils
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- C—CHEMISTRY; METALLURGY
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
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- C—CHEMISTRY; METALLURGY
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/44—Solvents
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- C—CHEMISTRY; METALLURGY
- 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
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/10—Lubricating oil
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- C—CHEMISTRY; METALLURGY
- 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
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/18—Solvents
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- General Chemical & Material Sciences (AREA)
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Abstract
The invention relates to the technical field of lubricating oil dewaxing processes, and discloses a method for recovering a dewaxing solvent in a light lubricating oil base oil filtrate. The method comprises the following steps: (1) Under the condition of high pressure, the light lubricating oil base oil filtrate is contacted with an organic solvent nanofiltration membrane at a low operation circulation flow rate to obtain penetrating fluid; wherein the high pressure is 4.3-10MPa, and the low-operation circulation flow is 5-13.5m 3 H; (2) When the content of the lubricating oil in the penetrating fluid is less than or equal to 2 weight percent, the operation is continued under the condition that the operation pressure is reduced to 2.8-4.2 MPa; (3) And when the permeation flux of the organic solvent nanofiltration membrane is stable, successfully starting the reactor, and entering a stable production state. The method can effectively shorten the driving time.
Description
Technical Field
The invention relates to the technical field of lubricating oil dewaxing processes, in particular to a method for recovering a dewaxing solvent in a light lubricating oil base oil filtrate.
Background
Dewaxing is required in the process of producing lubricating oil from mineral oil, the most early and widely used dewaxing method is solvent dewaxing, and the solvent dewaxing process is currently used in oil refineries all over the world. This process can yield both high viscosity lubricant base oils and paraffins, which is a significant reason why other dewaxing processes, such as hydrodewaxing and isodewaxing, cannot completely replace them. However, the solvent dewaxing process is an expensive process, and wax solidification is required for removal during dewaxing, while the dewaxing solvent is required for recovery by evaporation. The process consumes a lot of energy, and becomes a bottleneck of lubricating oil production. Oil refining technical researchers are constantly searching for new energy-saving technologies of solvent dewaxing devices for many years, but the fact that recovery can only be completed by relying on phase change of solvents cannot be changed all the time.
Exxon recovered lubricating oil dewaxing solvent by organic solvent resistant nanofiltration membrane technology in Tennessee Bomant oil refineries until 1998 (the apparatus was named as
) And makes great breakthrough in the aspects of energy conservation, emission reduction and yield increase. The research direction of people gradually turns to a method for realizing separation without phase change of solvent by membrane separation, but only reports on the industrial application of membrane separation for recovering dewaxing solvent of lubricating oil
Because of the fact that
Membrane manufacturer w.r Gra of the devicece was later purchased several times, no film was produced anymore, so
After the industrial application is reported, no second set of application device is reported in the world in the aspect of recovering the dewaxing solvent of the lubricating oil by membrane separation. Researchers have not stopped studying this application. Only the subsequent research is limited to laboratory pilot-scale experiments, and no reports are made on the industrial test aspect.
In fact, the start-up of a device for recovering the lubricant dewaxing solvent by using the industrial-grade OSN membrane is a difficult point, the common direct start-up method is long in time consumption, the retention rate of the membrane is difficult to increase, and people can easily question the usability of the OSN membrane in the aspect of recovering the lubricant dewaxing solvent.
Therefore, the method for recovering the dewaxing solvent in the light lubricating oil base oil filtrate by using the OSN has important significance.
Disclosure of Invention
The invention aims to overcome the defects of long start-up time and difficult increase of membrane retention rate of industrial grade OSN membrane separation and recovery of light lubricating oil dewaxing solvent in the prior art, and provides a method for recovering dewaxing solvent in light lubricating oil base oil filtrate.
In order to achieve the above object, the present invention provides a method for recovering a dewaxing solvent from a light lubricant base oil filtrate, wherein the method comprises:
(1) Under the condition of high pressure, the light lubricating oil base oil filtrate is contacted with an organic solvent nanofiltration membrane at a low operation circulation flow rate to obtain penetrating fluid; wherein the high pressure is 4.3-10MPa, and the low-operation circulation flow is 5-13.5m 3 /h；
(2) When the content of the lubricating oil in the penetrating fluid is less than or equal to 2 weight percent, the operation is continued under the condition that the operation pressure is reduced to 2.8-4.2 MPa;
(3) And when the permeation flux of the organic solvent nanofiltration membrane is stable, successfully starting the reactor, and entering a stable production state.
By adopting the technical scheme, the method adopts the industrial-grade OSN membrane with asymmetric size to recover the dewaxing solvent in the light lubricating oil base oil filtrate, and can shorten the time for the device to stably run by more than 40 percent; and the method is convenient to operate and does not bring impurities to industrial devices.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a method for recovering a dewaxing solvent in a light lubricating oil base oil filtrate, wherein the method comprises the following steps:
(1) Under the condition of high pressure, the light lubricating oil base oil filtrate is contacted with an organic solvent nanofiltration membrane at a low operation circulation flow rate to obtain penetrating fluid; wherein the high pressure is 4.3-10MPa, and the low-operation circulation flow is 5-13.5m 3 /h；
(2) When the content of the lubricating oil in the penetrating fluid is less than or equal to 2 weight percent, the operation is continued under the condition that the operation pressure is reduced to 2.8-4.2 MPa;
(3) And when the permeation flux of the organic solvent nanofiltration membrane is stable, successfully starting the reactor, and entering a stable production state.
The inventors of the present invention found that: in the industrial test of recovering the lubricating oil dewaxing solvent by membrane separation, the content of the solvent oil recovered by adopting the pressure of normal operation of membrane separation is always very high, the trend of reducing the solvent oil only after the solvent oil is operated for more than ten days, the system is under the high-pressure condition by adjusting the frequency of a material conveying pump, meanwhile, the circulating flow is maintained under the low-operation circulating flow by adjusting the frequency of a circulating pump, because the supporting layer of the membrane is compressed during the high-pressure operation, the stable state can be reached in a short time, and further, enough stable supporting force can be provided for the functional layer of the membrane to enable the functional layer of the membrane to quickly reach the stable state, so the start time can be shortened.
In the invention, it should be noted that: the term "the content of the lubricating oil in the penetrant is 2% by weight or less" means: the penetrating fluid contains lubricating oil, and the content of the lubricating oil is less than or equal to 2 wt% based on the total weight of the penetrating fluid.
According to the present invention, even at the high pressure and the low operation circulation flow rate defined above, the driving time can be shortened, but in the present invention, it is preferable that the conditions of the high pressure include: 4.4-8MPa, and the condition of low operation circulating flow comprises the following steps: 7-13m 3 H; more preferably, the conditions of the high pressure include: 4.5-6MPa, and the condition of low operation circulation flow comprises the following steps: 8-12m 3 H is used as the reference value. In the present invention, under such preferable conditions, the driving time can be further shortened.
According to the invention, in the step (1), the permeation flux of the stabilized organic solvent nanofiltration membrane is 200-550L/branch/h, and preferably 300-520L/branch/h.
According to the invention, in step (1), the conditions of the contacting comprise: the temperature is 10-50 deg.C, preferably 20-40 deg.C, and more preferably 25-35 deg.C.
According to the invention, in the step (2), when the content of the lubricating oil in the penetrating fluid is 0.1-2 wt%, the operation is continued under the condition that the operation pressure is 3-4 MPa; in the present invention, the content of the lubricating oil in the permeate and the operating pressure are defined within the aforementioned ranges, meaning stable operation.
According to the invention, the method further comprises: during the operation of the method, the low operation circulation flow rate is fixed. In the invention, the low-operation circulating flow is kept constant, and the high-pressure condition is adjusted, so that the supporting layer of the membrane can reach a stable compression state as soon as possible, the stable support is provided for the functional layer of the membrane, and the functional layer can reach a stable state as soon as possible.
According to the invention, the content of the lubricating oil in the penetrating fluid and the penetrating flux of the organic solvent nanofiltration membrane are changed in a gradient manner.
According to the invention, in the step (3), the conditions for stabilizing the permeation flux of the organic solvent nanofiltration membrane comprise: the flux reduction rate of the nanofiltration membrane in 24 hours is less than 1%. That is, in the present invention, the reduction of the permeation flux of the organic solvent nanofiltration membrane by less than 1% in 24h is taken as a criterion for the stability of the operation flux of the membrane.
According to the invention, preferably, in the step (3), two conditions need to be simultaneously met, namely, the content of the lubricating oil in the penetrating fluid and the penetrating flux of the organic solvent nanofiltration membrane are simultaneously limited, and the system meets the two conditions, which means that the start-up is successful and the stable production state can be achieved. Preferably, the successful driving condition includes: the permeation flux of the organic solvent nanofiltration membrane is 300-520L/branch/h, and the content of lubricating oil in the permeation liquid is 0.1% -2%; more preferably, the successful driving condition includes: the permeation flux of the organic solvent nanofiltration membrane is 530-580L/branch/h, and the content of lubricating oil in the permeation liquid is 1.3% -1.5%.
According to the present invention, in the step (3), the conditions for stabilizing the production state include: the content of lubricating oil in the penetrating fluid is 0.3-1.8 wt%, and the penetrating flux of the organic solvent nanofiltration membrane is 220-550L/branch/h; preferably, the content of the lubricating oil in the penetrating fluid is 1-1.3 wt%, and the penetrating flux of the organic solvent nanofiltration membrane is 460-510L/branch/h.
According to the invention, the organic solvent nanofiltration membrane (OSN) is selected from one or more of a hollow fiber type membrane module, a roll type membrane module, a tubular type membrane module and a plate type membrane module, preferably the roll type membrane module, in the invention, the OSN membrane is in an asymmetric structure and is made of a glassy polymer, preferably a polyimide polymer, and most preferably a P84 polyimide asymmetric nanofiltration membrane.
According to the invention, the molecular weight cut-off of the organic solvent nanofiltration membrane is 280-400Da, preferably 300-380Da; preferably, the membrane area of the organic solvent nanofiltration membrane is 20-40m 2 A/branch of the membrane is provided with,preferably 20-30m 2 A/membrane.
According to the invention, the length of the membrane component of the organic solvent nanofiltration membrane is 0.8-1.2m, preferably 0.9-1.1m, and the diameter of the membrane component is 6-10 inches, preferably 7-9 inches. In the invention, the organic solvent nanofiltration membrane is purchased from winning special chemistry, the mark is PM280, and the membrane component is a roll-type membrane, the length is 1m, and the diameter is 8 inches.
According to the present invention, the light lubricant base oil filtrate contains a light lubricant base oil and a dewaxing solvent.
According to the invention, the content of the light lubricating base oil is 20-26 wt% and the content of the dewaxing solvent is 74-80 wt% based on the total weight of the light lubricating base oil filtrate; preferably, the light lubricant base oil is present in an amount of 21 to 25 wt.%, and the dewaxing solvent is present in an amount of 75 to 79 wt.%, based on the total weight of the light lubricant base oil filtrate.
According to the invention, the light lubricating oil base oil is a crude oil fraction having a boiling range of 280-500 ℃; preferably, the light lubricant base oil is selected from one or more of normally four lines, reduced lines and reduced lines obtained from crude oil distillation, most preferably a reduced line lubricant base oil feedstock.
In the invention, the raw oil of the light lubricating oil comes from an oil refinery of China petrochemical Ministry of majesty, wherein the raw oil contains the following components in percentage by weight: the light lubricating oil has 24% of base oil and 76% of dewaxing solvent.
According to the invention, the dewaxing solvent is an aromatic hydrocarbon and C 3 -C 8 Mixtures of monoketones of (a).
According to the present invention, preferably, the aromatic hydrocarbon is monoalkylbenzene and/or benzene, more preferably, the alkyl group in the monoalkylbenzene is C 1 -C 4 Further preferably, the aromatic hydrocarbon is selected from one or more of toluene, ethylbenzene and propylbenzene.
According to the present invention, preferably, the monoketone is selected from one or more of methyl ethyl ketone, acetone, 2-butanone, 2-pentanone, 3-pentanone, and 2-hexanone.
According to the present invention, preferably, the dewaxing solvent is a mixture of methyl ethyl ketone and toluene.
According to the present invention, preferably, the weight ratio of the monoketone to the aromatic hydrocarbon is (50.
According to the invention, the method further comprises: before the step (1), cleaning the organic solvent nanofiltration membrane. Specifically, in the invention, firstly dewaxing solvent is added into a membrane separation device for membrane washing, dewaxing solvent in an emptying device is added with light base oil dewaxing filtrate after membrane washing is finished, the operation is carried out until the flux is stable and the retention rate reaches the target requirement, and finally the operation pressure of the system is adjusted to the preset pressure, and the circulation flow of the system is unchanged.
According to the invention, the cleaning conditions comprise: the time for washing the membrane is 0.1-24h, preferably 0.5-8h, more preferably 1-3h; the washing pressure is 0-5MPa, preferably 0.2-2MPa, and more preferably 0.5-1MPa; the circulation flow of the film-washing solvent is 1-20m 3 H, preferably from 5 to 18m 3 H, more preferably 8 to 15m 3 /h。
According to the invention, the permeation flux of the OSN membrane can reach a steady state when the system is operated under high pressure for 3-10 days, preferably 4-8 days, and the content of the lubricating oil in the permeation liquid can be lower than 2 wt%.
The present invention will be described in detail below by way of examples.
In the following examples and comparative examples:
the content parameter of the lubricating oil is measured by a thermogravimetric method; the flux of the membrane was read directly by the device with its own flow meter.
Example 1
This example illustrates the recovery of dewaxing solvent from a light lubricant base oil filtrate using the process of the present invention.
Light lubricating oil base oil filtrate: and (3) a three-way reducing base oil filtrate, wherein the three-way reducing base oil filtrate is obtained from a device for producing light ketone from lubricating oil, and the concentration of the three-way reducing base oil in the three-way reducing base oil filtrate is 24%.
Organic solvent nanofiltration membrane: miningStarting a vehicle by using an industrial-grade OSN membrane, wherein the OSN membrane is an 8-inch membrane component which is a wound special chemical PM280 membrane, the diameter of the membrane component is 8 inches, and the length of the membrane component is 1m; the membrane area of the OSN membrane was 24m 2 Per membrane, cut-off molecular weight 280Da.
(1) In the whole driving experiment process, the temperature is maintained at 30 ℃, firstly, a dewaxing solvent (the dewaxing solvent is a mixed solvent of butanone and toluene, wherein the mass ratio of the butanone to the toluene is 3) is added into a membrane separation pilot test device system, a material delivery pump is started to control the pressure to be 0.5MPa, a circulating pump is started after 2min, and the circulating flow is controlled to be 15m 3 Performing a membrane washing test, and emptying a membrane washing solvent in the system after 3 hours of membrane washing;
(2) Gradually adding filtrate of three-way base oil into the device system, adjusting the frequency of the material delivery pump to increase the pressure in the system to 4.5MPa, and adjusting the frequency of the circulating pump to maintain the circulating flow at 12m 3 Obtaining penetrating fluid;
at the moment, the permeation flux of the OSN membrane is 1200L/branch/h, and the content of the lubricating oil tested by taking a penetrating fluid is 8.2 percent;
after running for 2 days, the permeation flux of the OSN membrane is reduced to 600L/branch/h, and the content of the lubricating oil in a penetrant test is 7.3 percent;
after running for 3 days, the permeation flux of the OSN membrane is reduced to 540L/branch/h, and the content of the lubricating oil is 5.8% in a penetrant test;
after running for 4 days, the permeation flux of the OSN membrane is maintained at 530-540L/branch/h, and the content of the lubricating oil in a penetrant test is 2.2%;
after running for 5 days, the permeation flux of the OSN membrane is maintained at 530-540L/branch/h, the content of the lubricating oil is 1.4% in a penetrant test, and the start-up is successful;
reducing the operation pressure to 3.5MPa for operation;
after running for 1 day, the permeation flux of the OSN membrane is stabilized at 480-490L/ramus/h, the content of lubricating oil in the penetrating fluid is 1.3%, and the OSN membrane enters a stable production state.
Example 2
This example illustrates the recovery of dewaxing solvent from a light lubricant base oil filtrate using the process of the present invention.
The light lube base oil filtrate and organic solvent nanofiltration membrane were the same as in example 1.
(1) The temperature is maintained at 35 ℃ in the whole driving experiment process, firstly the dewaxing solvent which is the same as that in the embodiment 1 is added into the device system, the material conveying pump is started to control the pressure to be 0.8MPa, the circulating pump is started after 2min, and the circulating flow is controlled to be 12m 3 Performing a membrane washing test, and emptying a membrane washing solvent in the system after 2 hours of membrane washing;
(2) Gradually adding base oil filtrate with three-line reduction as same as that in example 1 into the device system, and then adjusting the frequency of the material conveying pump and the circulating pump to keep the system pressure at 5MPa and the system circulating flow at 10m 3 Obtaining penetrating fluid;
at the moment, the permeation flux of the OSN membrane is 1400L/branch/h, and the content of lubricating oil in the permeation liquid is 8.2 percent;
continuously maintaining the pressure and the circulation flow to operate the device, gradually and slowly reducing the permeation flux of the membrane along with the increase of the operation time, reducing the permeation flux of the OSN membrane to 620L/branch/h after 2 days of operation, and taking the permeation liquid to test the content of lubricating oil to be 7.2%;
after running for 3 days, the permeation flux of the OSN membrane is reduced to 580L/branch/h, and the content of the lubricating oil in a penetrant test is 3.2 percent;
after running for 4 days, the permeation flux of the OSN membrane is reduced to 570-580L/branch/h, and the content of the lubricating oil in a penetrant test is taken to be 1.5%, so that the start is successful;
the operation pressure is reduced to 3.5MPa for operation, the flux of the OSN membrane is stabilized at 500-510L/branch/h after one day, the content of lubricating oil in penetrating fluid is 1.3 percent, and the stable production state is entered.
Example 3
This example illustrates the recovery of dewaxing solvent from a light lubricant base oil filtrate using the process of the present invention.
The light lube base oil filtrate and organic solvent nanofiltration membrane were the same as in example 1.
(1) The temperature is maintained at 25 ℃ in the whole driving experiment process, firstly the dewaxing solvent which is the same as that in the embodiment 1 is added into the device system, the material conveying pump is started to control the pressure to be 1MPa, and after 2minThe circulating pump is started, and the circulating flow is controlled to be 8m 3 Performing a membrane washing test, and emptying a membrane washing solvent in the system after 1 hour of membrane washing;
(2) Gradually adding the same three-line-reduced base oil filtrate as that in example 1 into the device system, and then adjusting the frequency of the material conveying pump and the circulating pump to keep the system pressure at 6MPa and the system circulating flow at 8m 3 Obtaining penetrating fluid;
at the moment, the permeation flux of the OSN membrane is 1380L/branch/h, and the content of lubricating oil in the permeation liquid is 8.0 percent;
continuously maintaining the pressure and the circulation flow to operate the device, gradually and slowly reducing the permeation flux of the membrane along with the increase of the operation time, reducing the permeation flux of the OSN membrane to 600L/branch/h after 2 days of operation, and taking a penetrating fluid to test the content of the lubricating oil to be 7.0 percent;
after running for 3 days, the permeation flux of the OSN membrane is reduced to 570L/branch/h, and the content of the lubricating oil is 3.0 percent in a penetrant test;
after running for 4 days, the permeation flux of the OSN membrane is reduced to 560-570L/branch/h, and the content of the lubricating oil is tested to be 1.3% by taking a penetrating fluid, so that the start-up is successful;
the operation pressure is reduced to 3.5MPa for operation, the flux of the OSN membrane is stabilized at 460-470L/branch/h after one day, the content of lubricating oil in penetrating fluid is 1.3 percent, and the stable production state is entered.
Comparative example 1
The OSN membrane and membrane separation unit used, as well as the light lube base oil filtrate and experimental temperatures were exactly the same as in example 1. The membrane is first washed by adding a dewaxing solvent to the system. The membrane washing method was the same as in example 1. Starting the material conveying pump to control the pressure to be 0.5MPa, starting the circulating pump after 2min, and controlling the circulating flow to be 15m 3 And h, performing a membrane washing test, emptying a membrane washing solvent in the system after 3 hours of membrane washing, adding light lubricating oil base oil filtrate into the membrane separation device, adjusting the frequency of a material conveying pump and a circulating pump to keep the pressure of the system at about 3.5MPa, and maintaining the circulating flow at 12m 3 At this time, the permeation flux of the membrane is 1000L/branch/h, and the content of the lubricating oil is 8.2% by taking a permeation body fluid test.
The device is continuously operated, the permeation flux of the membrane is continuously reduced along with the increase of the operation time, when the device is operated for 3 days, the permeation flux of the membrane is 650L/count/h, and the content of the lubricating oil in a permeation body fluid test is 8.0 percent;
when the device runs for 6 days, the permeation flux of the membrane is reduced to 530L/branch/h, and the content of lubricating oil in the permeation liquid is 7.2 percent;
when the device runs for 9 days, the permeation flux of the membrane is reduced to 500L/branch/h, and the content of lubricating oil in the permeation liquid is 6.0 percent;
when the device runs for 12 days, the permeation flux of the membrane is stabilized at 480-490L/branch/h, and the content of lubricating oil in the permeation liquid is 3.1%;
when the device runs for 13 days, the permeation flux of the membrane is stabilized at 480-490L/count/h, the content of lubricating oil in the penetrating fluid is 1.3%, the driving is successful, and the device enters a stable production state.
Comparative example 2
The OSN membrane and membrane separation unit used, as well as the light lube base oil filtrate and experimental temperatures were exactly the same as in example 2. The membrane is first washed by adding a dewaxing solvent to the system. The membrane washing method was the same as in example 2. Starting a material delivery pump to control the pressure to be 0.8MPa, opening a circulating pump after 2min, and controlling the circulating flow to be 12m 3 And h, performing a membrane washing test, emptying a membrane washing solvent in the system after 2h of membrane washing, adding a light lubricating oil base oil filtrate into the membrane separation device, adjusting the frequency of a material conveying pump and a circulating pump to keep the pressure of the system at about 3.5MPa, and maintaining the circulating flow at 10m 3 At this time, the permeation flux of the membrane is 1100L/min/h, and the content of the lubricating oil in the permeation body fluid test is 8.3%. The device is continuously operated, the permeation flux of the membrane is continuously reduced along with the increase of the operation time, when the device is operated for 3 days, the permeation flux of the membrane is 660L/count/h, and the content of the lubricating oil in a permeation body fluid test is 8.0 percent; when the device runs for 6 days, the permeation flux of the membrane is reduced to 550L/branch/h, and the content of lubricating oil in the permeation liquid is 7.4 percent; when the device runs for 9 days, the permeation flux of the membrane is reduced to 530L/branch/h, and the content of lubricating oil in the permeation liquid is 5.9 percent; when the device runs for 12 days, the permeation flux of the membrane is stabilized at 500-510L/branch/h, and the content of lubricating oil in the permeation liquid is 3.0%; the permeation flux of the membrane is stabilized at 500-51 when the device is operated for 13 days0L/count/h, the content of lubricating oil in the penetrating fluid is 1.4 percent, the start is successful, and the stable production state is entered.
Comparative example 3
The OSN membrane and membrane separation unit used, as well as the light lube base oil filtrate and experimental temperatures were exactly the same as in example 2. The membrane is first washed by adding a dewaxing solvent to the system. The membrane washing method was the same as in example 3. Starting the material conveying pump to control the pressure to be 0.1MPa, starting the circulating pump after 2min, and controlling the circulating flow to be 8m 3 And h, performing a membrane washing test, emptying a membrane washing solvent in the system after 1h of membrane washing, adding a light lubricating oil base oil filtrate into the membrane separation device, adjusting the frequency of a delivery pump to keep the system pressure at about 3.5MPa, and continuously maintaining the circulation flow at 8m 3 At this time, the permeation flux of the membrane is 890L/min/h, and the content of lubricating oil in the permeation body fluid test is 8.1%. The device is continuously operated, the permeation flux of the membrane is continuously reduced along with the increase of the operation time, when the device is operated for 3 days, the permeation flux of the membrane is 540L/count/h, and the content of the lubricating oil in a permeation body fluid test is 7.8%; when the device runs for 6 days, the permeation flux of the membrane is reduced to 510L/branch/h, and the content of lubricating oil in the permeation liquid is 6.4 percent; when the device runs for 9 days, the permeation flux of the membrane is reduced to 490L/branch/h, and the content of lubricating oil in the penetrating fluid is 4.9 percent; when the device runs for 12 days, the permeation flux of the membrane is stabilized at 460-470L/branch/h, and the content of lubricating oil in the permeation liquid is 2.8%; when the device runs for 13 days, the permeation flux of the membrane is stabilized at 460-470L/per minute/h, the content of lubricating oil in the penetrating fluid is 1.3 percent, the start-up is successful, and the device enters a stable production state.
From the above results, it can be seen that, in examples 1 to 3 of the method of the present invention, the membrane is pretreated with the solvent of the membrane separation system, so that the functional layer material molecules of the membrane can be stretched to the maximum extent, the membrane can adapt to the separation environment quickly, the interception function of the membrane can be exerted in a short time, and in addition, the operation pressure is high, the support layer of the membrane provides a high reaction force, so that the functional layer is supported stably enough, the stability is good, the start-up time can be shortened, and the method has a significantly better effect.
Comparative examples 1, 2 and 3 did not adopt the technical solution of the present invention, and the pressure was low, resulting in a long driving time.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including various technical features being combined in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A process for recovering dewaxing solvent from a light lubricant base oil filtrate, said process comprising:
(1) Under the condition of high pressure, the light lubricating oil base oil filtrate is contacted with an organic solvent nanofiltration membrane at a low operation circulation flow rate to obtain penetrating fluid; wherein the high pressure is 4.3-10MPa, and the low-operation circulation flow is 5-13.5m 3 /h；
(2) When the content of the lubricating oil in the penetrating fluid is less than or equal to 2 weight percent, the operation is continued under the condition that the operation pressure is reduced to 2.8-4.2 MPa;
(3) And when the permeation flux of the organic solvent nanofiltration membrane is stable, successfully starting the reactor, and entering a stable production state.
2. The method of claim 1, wherein the high pressure is 4.4-8MPa and the low operating cycle flow is 7-13m 3 /h；
Preferably, the high pressure is 4.5-6MPa, and the low-operation circulation flow is 8-12m 3 /h。
3. The method as claimed in claim 1, wherein, in the step (1), the permeation flux of the organic solvent nanofiltration membrane after stabilization is 200-550L/branch/h;
preferably, in the step (2), when the content of the lubricating oil in the penetrating fluid is 0.1-2 wt%, the operation is continued under the condition that the operation pressure is 3-4 MPa.
4. The method according to any one of claims 1-3, wherein the method further comprises: during the operation of the method, the low operation circulation flow is fixed and unchanged;
preferably, in the step (3), the conditions for stabilizing the permeation flux of the organic solvent nanofiltration membrane comprise: the flux reduction rate of the nanofiltration membrane in 24 hours is less than 1%;
preferably, in step (3), the successful start condition includes: the permeation flux of the organic solvent nanofiltration membrane is 300-520L/branch/h, and the content of lubricating oil in the permeation liquid is 0.1% -2%;
preferably, in the step (3), the production-state-stabilizing conditions include: the content of lubricating oil in the penetrating fluid is 0.3-1.8 wt%, and the penetrating flux of the organic solvent nanofiltration membrane is 220-550L/branch/h.
5. The method of claim 1, wherein, in step (1), the conditions of the contacting comprise: the temperature is 10-50 deg.C, preferably 20-40 deg.C, and more preferably 25-35 deg.C.
6. The process of claim 1, wherein the organic solvent nanofiltration membrane has a molecular weight cut-off of 280-400Da, preferably 300-380Da;
preferably, the membrane area of the organic solvent nanofiltration membrane is 20-40m 2 A/membrane;
preferably, the length of the membrane component of the organic solvent nanofiltration membrane is 0.8-1.2m, and the diameter of the membrane component is 6-10 inches.
7. The method of claim 1, wherein the light lubricant base oil filtrate comprises a light lubricant base oil and a dewaxing solvent;
preferably, the light lubricant base oil is present in an amount of 20 to 26 wt.%, and the dewaxing solvent is present in an amount of 74 to 80 wt.%, based on the total weight of the light lubricant base oil filtrate;
preferably, the light lubricant base oil is a crude oil fraction having a boiling range of 280-500 ℃;
preferably, the light lubricant base oil is selected from one or more of the group consisting of normal four lines, reduced two lines and reduced three lines obtained from crude oil distillation.
8. The method of claim 7, wherein the dewaxing solvent is an aromatic hydrocarbon and C 3 -C 8 Mixtures of monoketones of (a).
9. The method according to any one of claims 1-8, wherein the method further comprises: before the step (1), cleaning the organic solvent nanofiltration membrane.
10. The method of claim 9, wherein the cleaning conditions comprise: the membrane washing time is 0.1-24h, the membrane washing pressure is 0-5MPa, and the circulation flow of the membrane washing solvent is 1-20m 3 /h。
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