CN115491231A - Isoparaffin solvent refining system and refining method - Google Patents

Isoparaffin solvent refining system and refining method Download PDF

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Publication number
CN115491231A
CN115491231A CN202211295363.3A CN202211295363A CN115491231A CN 115491231 A CN115491231 A CN 115491231A CN 202211295363 A CN202211295363 A CN 202211295363A CN 115491231 A CN115491231 A CN 115491231A
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China
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adsorption tower
pump
oil
discharge
isoparaffin solvent
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周琳
廖定满
李佩儒
卢振旭
孙望平
许宏
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China Petroleum and Chemical Corp
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China Petroleum and Chemical Corp
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G53/00Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
    • C10G53/02Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
    • C10G53/08Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one sorption step

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Separation Of Gases By Adsorption (AREA)

Abstract

The invention relates to the technical field of chemical production, and discloses an isoparaffin solvent refining system and a refining method. When the system works, the operation periods of the first adsorption tower and the second adsorption tower are staggered, so that the system has continuous production capacity, and the removal rate of the oxygen-containing compounds in the isoparaffin solvent is improved. When the oxygen-containing compounds in the isoparaffin solvent need to be removed, raw isoparaffin solvent oil is injected into the adsorption tower from the corresponding feed inlet of the adsorption tower, the compounds in the crude oil are adsorbed by the crude oil through the adsorbent, and the isoparaffin solvent product from which the oxygen-containing compounds are removed is led out from the discharge outlet of the adsorption tower, so that the removal rate of the oxygen-containing compounds in the isoparaffin solvent is improved, and the method is suitable for industrial production.

Description

System and method for refining isoparaffin solvent
Technical Field
The invention relates to the technical field of chemical production, in particular to a system and a method for refining an isoparaffin solvent.
Background
In the production process of the isononanol production device, partial isomeric carbon 8 olefin, isomeric carbon 12 olefin and isomeric carbon 16 olefin byproducts are generated, the partial isomeric olefin byproducts can be used for preparing an isoparaffin solvent after being subjected to hydrogenation treatment, the prepared isoparaffin solvent also contains a small amount of oxygen-containing compounds due to the fact that the isomeric olefin byproducts contain a small amount of oxygen-containing compounds, and the presence of the oxygen-containing compounds has great influence on the odor of the isoparaffin solvent, so that the oxygen-containing compounds in the isoparaffin solvent need to be removed.
Related researches on methods for removing oxygen-containing compounds in oil products are also carried out at home and abroad, but the existing researches are mainly carried out on laboratory scale, and no report is found on related industrial production devices. In addition, the existing removal method has low removal rate of oxygen-containing compounds in the isoparaffin solvent, and cannot realize industrial production, and the existing method has low removal rate of the oxygen compounds and does not have continuous production capacity.
Disclosure of Invention
In order to solve the technical problems, the invention provides a refining system and a refining method for an isoparaffin solvent, which have continuous production capacity, improve the removal rate of oxygen-containing compounds in the isoparaffin solvent and are suitable for industrial production.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the utility model provides an isoparaffin solvent refining system, includes oil-water separation jar, raw oil tank, first adsorption tower, second adsorption tower, finished product jar, vacuum pump, condenser, first charge pump, first discharge pump, second charge pump and second discharge pump, oil-water separation jar reaches the raw oil tank is equallyd divide and is connected first charge pump reaches the import of second charge pump, first charge pump reaches the export of second charge pump is equallyd divide and is connected oil-water separation jar, raw oil tank respectively, the feed inlet of first adsorption tower with first charge pump circulation intercommunication, the feed inlet of second adsorption tower with second charge pump circulation intercommunication, the discharge gate of first adsorption tower and the access connection of first discharge pump, and the export of first discharge pump is connected the feed inlet of oil-water separation jar, finished product jar and second adsorption tower respectively, the discharge gate of second adsorption tower and the access connection of second discharge pump, and the export of second discharge pump is connected oil-water separation jar, finished product jar and the feed inlet of first adsorption tower respectively, the feed inlet of first adsorption tower, the discharge gate of second adsorption tower and the discharge outlet of second adsorption tower are connected respectively the drainage tower and the discharge outlet of second adsorption tower and vacuum pump are connected the drainage tower respectively the discharge outlet of first adsorption tower and the drain system of second adsorption tower.
Preferably, the first adsorption tower and the second adsorption tower both comprise adsorption tower main bodies, a charging port is arranged at the upper end of each adsorption tower main body and is communicated with the atmosphere and a steam system, the feed port and the discharge port are arranged at the bottom of each adsorption tower main body, an adsorption bed layer for placing an adsorbent is arranged inside each adsorption tower main body, and a discharge port is arranged above the adsorption bed layer on the side wall of each adsorption tower main body.
Preferably, a liquid level meter pressure leading port is arranged on the side wall of the adsorption tower main body and above the adsorbent bed, a liquid level pipe is arranged between the liquid level meter pressure leading port and the charging port, and a liquid level meter is arranged on the liquid level pipe.
Preferably, the charging hole is provided with a sealing plate, the sealing plate is provided with an opening, the opening is provided with an atmosphere pipe, the atmosphere pipe is provided with an atmosphere valve, the liquid level pipe is connected with the atmosphere pipe, a steam pipe for connecting a steam system is arranged on the atmosphere pipe and between the liquid level pipe and the atmosphere valve, and the steam pipe is provided with a steam valve.
Preferably, the discharge port is provided with a branch pipe, the branch pipe is respectively connected with a drain pipe, a blow-off pipe and a vacuum pipe, a drain valve and the steam trap are sequentially arranged on the drain pipe along the water flow direction, a blow-off valve is arranged on the blow-off pipe, a vacuum valve is arranged on the vacuum pipe, and an outlet of the vacuum pipe is connected with the vacuum pump.
Preferably, the adsorption tower main body comprises a tower body, an upper cover is arranged at the upper end of the tower body, the charging hole is formed in the upper cover, a lower cover is arranged at the lower end of the tower body, the feeding hole and the discharging hole are formed in the lower cover, thermometers are arranged on the upper portion, the middle portion and the lower portion of the tower body, and a heat preservation layer is coated on the outer wall of the adsorption tower main body.
Preferably, the bottom of tower body is equipped with the support frame, be equipped with the screen cloth on the support frame, adsorbent bed support in on the screen cloth, the lateral wall of tower body is located adsorbent bed's lower extreme is equipped with the adsorbent discharge opening.
A refining method of an isoparaffin solvent comprises the following steps:
filling adsorbents into the first adsorption tower and the second adsorption tower;
raw material oil of an isoparaffin solvent is injected into a first adsorption tower from a raw material oil tank through a first feed pump, an isoparaffin solvent product subjected to oxygen-containing compound removal is led out from a discharge hole of the first adsorption tower to a finished product tank through a first discharge pump, and the oxygen-containing compound content of the isoparaffin solvent product is continuously monitored;
finished products coming out of the first adsorption tower are injected into the second adsorption tower from a discharge hole of the first adsorption tower through the first discharge pump, isoparaffin solvent products subjected to oxygen-containing compound removal are led out from a discharge hole of the second adsorption tower to the finished product tank through the second discharge pump, and meanwhile, a valve from the first discharge pump to the finished product tank is closed.
Stopping injecting the raw oil into the first adsorption tower, and simultaneously injecting the isoparaffin solvent raw oil into the second adsorption tower through a second feed pump by the raw oil tank;
returning the oil stored in the first adsorption tower to the raw oil tank through a first feeding pump;
the oil-water separation tank injects deionized water into the first adsorption tower through a first feed pump, and the eluent is led out of the oil-water separation tank from a discharge port of the first adsorption tower through a first discharge pump;
the water stored in the first adsorption tower returns to the oil-water separation tank through a first feed pump, high-temperature steam is introduced into the first adsorption tower from a charging port of the first adsorption tower, and condensed water is discharged through a steam trap;
when the temperature at the bottom of the first adsorption tower rises to over 120 ℃, connecting the first adsorption tower with a vacuum system to vacuumize, and then naturally cooling the adsorption tower;
when the adsorbent in the second adsorption tower is saturated, the adsorption is stopped, and the regeneration operation of the first adsorption tower is repeated.
Preferably, the feeding airspeed of the isoparaffin solvent raw oil injected into the adsorption tower is 0-30/h, the operation temperature in the adsorption tower is-20-60 ℃, and the operation pressure in the adsorption tower is 0-1.0Mpa.
Preferably, the injection space velocity of the deionized water into the adsorption tower is 0.5-5/h; the steam pressure of the high-temperature steam is 0.6-1.0MPa.
Compared with the prior art, the system and the method for refining the isoparaffin solvent have the advantages that: through setting up first adsorption tower and second adsorption tower, the operating cycle of first adsorption tower and second adsorption tower staggers each other during operation, and the second adsorption tower is in adsorbent regeneration link when first adsorption tower is in the raw materials oil adsorption link promptly, vice versa to make this system possess the ability of continuous production. And this system can be when one of them adsorption tower is close to the adsorption link later stage, connects 2 adsorption towers in series and works, effectively improves the availability factor of adsorbent. When the oxygen-containing compounds in the isoparaffin solvent need to be removed, raw isoparaffin solvent oil is injected into the adsorption tower from the corresponding feed inlet of the adsorption tower, the crude oil adsorbs the compounds in the crude oil through the adsorbent, and the isoparaffin solvent product after the removal of the oxygen-containing compounds is led out from the discharge outlet of the adsorption tower. The invention has simple operation, good use effect and easy popularization and use.
Drawings
FIG. 1 is a schematic structural view of an isoparaffin solvent refining system according to the present invention.
Fig. 2 is a schematic structural view of the first adsorption column or the second adsorption column of the present invention.
Wherein: 1-charging port, 2-charging port, 3-discharging port, 4-adsorbent bed, 5-discharging port, 6-liquid level pipe, 7-liquid level meter, 8-atmospheric valve, 9-steam valve, 10-oil-water separation tank, 11-raw oil tank, 12-water discharging valve, 13-steam trap, 14-blow-down valve, 15-vacuum valve, 16-tower body, 17-upper cover, 18-lower cover, 19-temperature measuring meter, 20-heat insulating layer, 21-supporting frame, 22-screen, 23-adsorbent discharging port, 24-first adsorption tower, 25-second adsorption tower, 26-finished product tank, 27-vacuum pump, 28-condenser, 29-first charging pump, 30-first discharging pump, 31-second charging pump and 32-second discharging pump.
Detailed Description
The following detailed description of the present invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention, but are not intended to limit the scope of the invention.
As shown in fig. 1, a system for refining isoparaffin solvent according to a preferred embodiment of the present invention comprises an oil-water separation tank 10, a raw oil tank 11, a first adsorption tower 24, a second adsorption tower 25, a finished product tank 26, a vacuum pump 27, a condenser 28, a first feed pump 29, a first discharge pump 30, a second feed pump 31 and a second discharge pump 32, wherein the oil-water separation tank 10 and the raw oil tank 11 are connected to inlets of the first feed pump 29 and the second feed pump 31, respectively, outlets of the first feed pump 29 and the second feed pump 31 are connected to the oil-water separation tank 10 and the raw oil tank 11, respectively, a feed port 2 of the first adsorption tower 24 is connected to the first feed pump 29 in a circulating manner, a feed port 2 of the second adsorption tower 25 is connected to the second feed pump 31 in a circulating manner, a discharge port 5 of the first adsorption tower 24 is connected to an inlet of the first discharge pump 30, an outlet of the first adsorption tower 30 is connected to the oil-water tank 10, the finished product tank 26 and a feed port 2 of the second adsorption tower 25, a discharge port 2 of the second adsorption tower 25 is connected to a discharge tower 25, a discharge port 5 of the second adsorption tower 24 is connected to an inlet of the second discharge pump, and a discharge tower 32, and a discharge port 32 of the second adsorption tower 24 are connected to a drain system of the adsorption tower 24, and a drain system of the adsorption tower 24, and a drain tower 32, and a drain system, respectively, and a drain system of the adsorption tower is connected to the oil-water separation tank 24, and a drain system 13.
Specifically, the outlet at the lower part of the oil-water separation tank 10 is connected with a water discharge pipeline, the water discharge pipeline is divided into two paths at the inlet of the first feeding pump 29, the two paths are respectively connected with the inlet of the first feeding pump 29 and the inlet of the second feeding pump 31 after being connected with a valve, and the two paths are controlled to be opened and closed through the valve.
The lower outlet of the raw oil tank 11 is connected with a raw oil discharge pipeline, the raw oil discharge pipeline is divided into two paths at the inlet of the first feed pump 29, the two paths are respectively connected with the inlet of the first feed pump 29 and the inlet of the second feed pump 31 after being respectively connected with a valve, and the two paths are controlled to be opened and closed through the valve.
The outlet of the first feed pump 29 is divided into three paths, one path is combined with the water discharge pipeline after being connected with the valve, the other path is combined with the raw oil discharge pipeline after being connected with the valve, the other path is divided into two paths after being connected with the valve, the other path is connected with the feed inlet 2 at the bottom of the first adsorption tower 24, the other path is connected with the inlet of the first feed pump 29 after being connected with the valve, and all the paths are controlled to be opened and closed through the valve.
The outlet of the second feeding pump 31 is divided into three paths, one path is combined with the water discharging pipeline after being connected with the valve, the other path is combined with the raw oil discharging pipeline after being connected with the valve, the other path is divided into two paths after being connected with the valve, the other path is connected with the feeding hole 2 at the bottom of the second adsorption tower 25, the other path is connected with the inlet of the second feeding pump 31 after being connected with the valve, and all the paths are controlled to be opened and closed through valves.
The discharge port 5 at the upper part of the first adsorption tower 24 is connected with the inlet of the first discharge pump 30 through a pipeline, the outlet of the first discharge pump 30 is divided into three paths, one path of the outlet is connected with the inlet of the finished product tank 26 after being connected with a valve, the other path of the outlet is connected with the inlet at the upper part of the oil-water separation tank 10 after being connected with the valve, the other path of the outlet is connected with the feed port 2 at the bottom of the second adsorption tower 25 after being connected with the valve, and all the paths of the outlet are controlled to be opened and closed through valves.
The discharge port 5 at the upper part of the second adsorption tower 25 is connected with the inlet of the second discharge pump 32 through a pipeline, the outlet of the second discharge pump 32 is divided into three paths, one path of the outlet is connected with the inlet of the finished product tank 26 after being connected with a valve, the other path of the outlet is connected with the inlet at the upper part of the oil-water separation tank 10 after being connected with the valve, the other path of the outlet is connected with the feed port 2 at the bottom of the first adsorption tower 24 after being connected with the valve, and all the paths of the outlet are controlled to be opened and closed through valves.
In the isoparaffin solvent refining system based on the above technical features, by arranging the first adsorption tower 24 and the second adsorption tower 25, the operation periods of the first adsorption tower 24 and the second adsorption tower 25 are staggered during operation, that is, when the first adsorption tower 24 is in the raw oil adsorption link, the second adsorption tower 25 is in the adsorbent regeneration link, and vice versa, so that the system has continuous production capacity. And this system can be when one of them adsorption tower is close to the adsorption link later stage, connects 2 adsorption towers in series and works, effectively improves the availability factor of adsorbent. When the oxygen-containing compounds in the isoparaffin solvent need to be removed, raw isoparaffin solvent oil is injected into the adsorption tower from the corresponding feed inlet of the adsorption tower, the crude oil adsorbs the compounds in the crude oil through the adsorbent, and the isoparaffin solvent product after the oxygen-containing compounds are removed is led out from the discharge outlet of the adsorption tower. The invention has simple operation, good use effect and easy popularization and use. .
Referring to fig. 2, in the embodiment, the first adsorption tower 24 and the second adsorption tower 25 have the same structure, and both include an adsorption tower main body, a charging port 1 is disposed at an upper end of the adsorption tower main body, the charging port 1 is communicated with an atmosphere and a steam system, the feed port 2 and the discharge port 3 are disposed at a bottom of the adsorption tower main body, an adsorbent bed 4 for placing an adsorbent is disposed inside the adsorption tower main body, and a discharge port 5 is disposed on a side wall of the adsorption tower main body above the adsorbent bed 4. Through setting up charging hole 1 in the upper end of adsorption tower main part, bottom at the adsorption tower main part sets up feed inlet 2 and discharge port 3, the lateral wall of adsorption tower main part sets up discharge gate 5, the inside of adsorption tower main part is equipped with adsorbent bed 4 that is used for placing the adsorbent simultaneously, only need inject isoparaffin solvent raw oil into the adsorption tower from feed inlet 2 when need desorption isoparaffin solvent oxygen-containing compound, crude oil adsorbs the oxygen-containing compound in the crude oil through adsorbent bed 4 back adsorbent, draw forth from discharge gate 5 after desorption oxygenate isoparaffin solvent product can, not only improved the desorption rate height to oxygen-containing compound in the isoparaffin solvent, and easy operation is applicable to industrial production.
In addition, when the adsorption capacity of the adsorbent is saturated, deionized water is injected into the adsorption tower from the feed port 2 to realize water replacement of the adsorbent, high-temperature steam is introduced into the adsorption tower through the charging port 1 to heat the adsorbent bed layer 4, the pressure in the tower is reduced to negative pressure through a vacuum system to remove water on the adsorbent, and the adsorbent has adsorption activity again, so that the adsorbent is regenerated in the adsorption tower.
In this embodiment, the side wall of the adsorption tower main body is located above the adsorbent bed 4 and is provided with a level gauge pressure-leading port, a level pipe 6 is arranged between the level gauge pressure-leading port and the charging port 1, and a level gauge 7 is arranged on the level pipe 6. The liquid level meter 7 can display the liquid level height in the adsorption tower, and the isoparaffin solvent product after removing the oxygen-containing compounds and the eluent used for replacing the adsorbent are led out from the discharge hole 5.
In this embodiment, charging hole 1 is equipped with the shrouding, be equipped with the opening on the shrouding, the opening is equipped with the atmosphere pipe, be equipped with atmosphere valve 8 on the atmosphere pipe, when atmosphere valve 8 is opened, the inside and the atmosphere intercommunication of adsorption tower. The liquid level pipe 6 is connected the atmosphere pipe, be located on the atmosphere pipe be equipped with between liquid level pipe 6 and the atmosphere valve 8 and be used for connecting the steam pipe of steam system, be equipped with steam valve 9 on the steam pipe, when needing to connect high temperature steam system steam valve 9 is opened, closes when not needing. Namely, the charging hole 1 is communicated with the atmosphere or a steam system through an atmosphere valve 8 and a steam valve 9.
In this embodiment, the exhaust port 3 is provided with a branch pipe, the branch pipe is respectively connected with a drain pipe, a drain pipe and a vacuum pipe, the drain pipe is sequentially provided with a drain valve 12 and a steam trap 13 along a water flow direction, the drain pipe is provided with a drain valve 14, the vacuum pipe is provided with a vacuum valve 15, an outlet of the vacuum pipe is connected with a vacuum pump 27, and the vacuum pump 27 is opened when the adsorption tower is vacuumized. The drain valve 12 is opened when draining condensed water, and the soil discharge valve 14 is opened when draining sewage.
In this embodiment, the adsorption tower main body includes tower body 16, the upper end of tower body 16 is equipped with upper cover 17, charging hole 1 sets up upper cover 17, the lower extreme of tower body 16 is equipped with lower cover 18, upper cover 17 and lower cover 18 all through the flange with tower body 16 is connected. The feed inlet 2 and the discharge outlet 3 are both arranged on the lower cover 18, and thermometers 19 are arranged on the upper part, the middle part and the lower part of the tower body 16 and are used for measuring the temperature of different parts in the adsorption tower main body, so that the quality and the efficiency of removing the oxygen-containing compounds are ensured. The outer wall of the adsorption tower main body is coated with a heat preservation layer 20 for heat preservation.
In this embodiment, the bottom of tower body 16 is equipped with support frame 21, be equipped with screen cloth 22 on the support frame 21, adsorbent bed 4 support in on the screen cloth 22, the lateral wall of tower body 16 is located adsorbent bed 4's lower extreme is equipped with adsorbent discharge opening 23 for unloading of adsorbent. The height-diameter ratio of the adsorbent bed layer 4 is 3:1-20:1, the adsorption efficiency can be improved while the crude oil is fully adsorbed.
In order to solve the technical problems, the invention also provides a method for removing oxygen-containing compounds in an isoparaffin solvent by using the adsorption tower, which comprises the following steps:
the first adsorption tower 24 and the second adsorption tower 25 are filled with an adsorbent from the charging port 1. The adsorbent is spherical coarse-pore silica gel adsorbent, and has pore volume of 0.75-1.0ml/g, bulk density of 400-480g/L, and particle diameter of 1-5.6mm.
The raw oil adsorption link of the first adsorption tower 24 is as follows: the crude oil valve 10 and the atmospheric valve 8 of the first adsorption tower 24 are opened, the valve connecting the inlet of the first feed pump 29 and the crude oil tank is opened, the valve connecting the outlet of the first feed pump 29 and the first adsorption tower 24 is opened, all other valves are closed, and the raw material oil of the isoparaffin solvent is injected into the first adsorption tower 24 through the crude oil tank 10 via the first feed pump 29. The feeding airspeed of raw oil of isoparaffin solvent injected into the adsorption tower is 0-30/h, the operation temperature in the adsorption tower is-20-60 ℃, the operation pressure in the adsorption tower is 0-1.0Mpa, and the liquid level height of the liquid level meter 7 is 100-500 mm. Preferably, the air speed of raw oil feeding is 0.1-2/h, the adsorption operation temperature is 0-50 ℃, the adsorption operation pressure is 0-0.5MPa, and the liquid level height of a liquid level meter 7 is 200-300 mm.
When the liquid level meter 7 at the upper part of the first adsorption tower 24 detects the liquid level, the isoparaffin solvent product after removing the oxygen-containing compound is led out from the discharge port 5 of the first adsorption tower 24 to the finished product tank 26, and the oxygen-containing compound content of the isoparaffin solvent product is continuously monitored. When the content of the oxygen-containing compound in the isoparaffin solvent product is obviously increased, the adsorption capacity of the adsorbent is saturated, the raw oil adsorption link is ended, and the first adsorption tower 24 enters the adsorbent regeneration link. At this time, the injection of the feedstock oil into the first adsorption tower 24 is stopped, the second adsorption tower 25 is communicated with the feedstock oil tank 11, and the feedstock oil tank 11 simultaneously injects the isoparaffin solvent feedstock oil into the second adsorption tower 25, so that the second adsorption tower 25 realizes a feedstock oil adsorption step.
The adsorbent regeneration link comprises two steps of water replacement and dehydration. The water replacement step is to inject deionized water into the adsorbent bed layer 4 by utilizing the characteristic that the adsorption energy of the silica gel adsorbent to water is higher than the adsorption energy of the silica gel adsorbent to oxygen-containing compounds in isoparaffin, and because the energy position of the silica gel surface after adsorbing water is lower, water molecules can replace the organic oxygen-containing compounds originally adsorbed on the silica gel surface, and the oxygen-containing compounds in the isoparaffin are not dissolved with water, and the oxygen-containing compounds can be recovered after standing and separation.
The feed pump and the discharge pump described below are the first feed pump 29 and the first discharge pump 30 for water replacement of the first adsorption tower 24, and the second feed pump 31 and the second discharge pump 32 for water replacement of the second adsorption tower 25.
Water replacement step operation process; after the raw oil adsorption link is finished, a raw oil discharge pipeline is opened to be connected with an outlet valve of a feeding pump, an inlet of the feeding pump is opened to be connected with a feed inlet valve of an adsorption tower, other inlet and outlet valves of the feeding pump are all closed, the oil in the adsorption tower is pumped out through the feeding pump and returned to a raw oil tank 11, then the raw oil tank is kept stand for 5-10 hours, so that the oil remained on the adsorbent is fully recovered, and then the oil in the tower is completely pumped out. Open water ejection of compact pipe coupling charge pump inlet valve, open charge pump exit linkage adsorption tower feed inlet valve, the charge pump advances, export other valves and all close, pour into deionized water into the adsorption tower through the charge pump, when the level gauge on adsorption tower upper portion detected the liquid level, draw forth the eluant through the discharge gate on adsorption tower upper portion, open adsorption tower discharge gate to discharge pump inlet valve, open discharge pump export to oil water separation tank valve, other valves of discharge pump export are closed, send into the eluant into oil water separation tank through the discharge pump, and control the ejection of compact speed of discharge pump, make the interior liquid level of tower stable, the eluant of drawing forth from the discharge gate is oil water mixture, after the vast majority of oxygenate of desorption was drawn forth the adsorption tower, water replacement step ends.
The water replacement step has the following process operating conditions; the air speed of injecting deionized water is 0.5-5/h, the operation temperature is normal temperature, the operation pressure is normal pressure, the liquid level height of the liquid level meter is 100-200 mm, and the injected water amount is 5-10 times of the volume of the adsorbent bed layer.
The dehydration step is to inject high-temperature steam into the adsorption tower to heat the adsorbent bed layer 4, and reduce the pressure in the tower to negative pressure through a vacuum pumping system to remove water on the adsorbent, so that the adsorbent has adsorption activity again.
A dehydration step operation process; after the water replacement step is finished, a water discharging pipeline is opened to be connected with an outlet valve of a feeding pump, an inlet of the feeding pump is opened to be connected with a feed inlet valve of an adsorption tower, other valves at an inlet and an outlet of the feeding pump are all closed, water in the adsorption tower is pumped out through the feeding pump and returns to an oil-water separation tank, then a tower top is opened to be connected with a heating steam valve, a tower bottom is opened to be connected with a steam trap valve, other valves are all closed, heating steam is injected into the adsorption tower through a connecting port of a heating steam system, condensed water is discharged through the steam trap at the tower bottom, when the temperature of a temperature measurer at the bottom of the adsorption tower rises to be higher than 120 ℃, the connecting steam trap valve is closed, a connecting vacuumizing system valve is opened, a steam jet vacuum pump is started, the pressure in the adsorption tower is gradually reduced, the heating steam injection speed is controlled, after the temperature and the pressure in the adsorption tower are stabilized on certain numerical values for a period, the heating steam is closed, the dehydration step is finished, the adsorption tower is naturally cooled to be about 50 ℃, and the next period of operation can be carried out.
The dehydration step has the process conditions: the heating steam pressure is 0.6-1.0MPa, the temperature in the tower in the stabilization stage is 120-180 ℃, the pressure in the tower in the stabilization stage is-0.05-0.09 MPa, and the holding time in the stabilization stage is 5-10 hours.
When the adsorbent in the second adsorption tower 25 is saturated, adsorption is stopped, and the feed oil is injected into the first adsorption tower 24. That is, in this case, the first adsorption tower 24 performs adsorption, and the second adsorption tower 25 performs adsorbent regeneration, in the same manner as described above.
The method can realize the industrial production of removing the oxygen-containing compounds in the isoparaffin solvent; the adsorption tower can realize the regeneration in the adsorbent tower, and the service life of the adsorbent is long; the removal rate of the oxygen-containing compound in the isoparaffin solvent is high, and the content of the removed oxygen-containing compound in the isoparaffin solvent is lower than 10ppm (the content of the oxygen-containing compound in the isoparaffin raw oil is 0.1-1.0%); the method has simple process and low production cost.
The technical effect of the present invention will be described below with reference to a specific embodiment.
Example one
Spherical coarse-pore silica gel adsorbents with the particle diameter of 2.0-5.6mm are loaded in the first adsorption tower 24 and the second adsorption tower 25, the pore volume is 0.91ml/g, and the bulk density is 440g/L. The size of the adsorbent bed layer of each adsorption tower is phi 1200 multiplied by 9000, and the volume of the adsorbent bed layer is 10.2 cubic meters.
The method comprises the steps of opening an inlet valve of a raw oil discharging pipeline connected with a first feeding pump 29, opening a valve of an outlet of the first feeding pump 29 connected with a feeding port 2 of a first adsorption tower 24, closing other valves of an inlet and an outlet of the first feeding pump 29, opening a valve of an outlet of a first discharging pump 30 connected with a finished product tank 26, closing other valves of an outlet of the first discharging pump, closing all inlet and outlet valves of a second feeding pump 31 and a second discharging pump 32, and opening an atmospheric valve 8 of the first adsorption tower 24 connected with an atmospheric pipeline.
Starting a first feed pump 29, injecting isoparaffin solvent raw oil (the content of oxygen-containing compounds is 0.271%) into the first adsorption tower 24 at an injection speed of 2 cubic meters per hour, starting a first discharge pump 30 to draw out products when a liquid level meter 7 at the upper part of the first adsorption tower 24 detects the liquid level, controlling the discharge speed to ensure that the liquid level height of the liquid level meter 7 of the first adsorption tower 24 is controlled to be 200-300 millimeters, sampling once at the outlet of the first discharge pump 30 when the total amount of the products discharged from the first adsorption tower 24 is increased by 5 times of the volume of the adsorbent bed, and analyzing the content of the oxygen-containing compounds to monitor the product quality. When the total amount of the product discharged from the first adsorption tower 24 reaches 40 times of the volume of the adsorbent bed, the valve connecting the outlet of the first discharging pump 29 with the feed port 2 of the second adsorption tower 25 is opened, the valve connecting the outlet of the first discharging pump 30 with the finished product tank 26 is closed, and the valve connecting the outlet of the second discharging pump 32 with the finished product tank 26 is opened. The operation of the second adsorption tower 25 is the same as that of the first adsorption tower 24, so that the product from the first adsorption tower 24 is fed into the finished product tank after being supplemented and refined by the second adsorption tower 25, and the quality of the finished product at the later operation stage of the first adsorption tower 24 is ensured. The data of the sampling analysis of the discharge of the first adsorption tower 24 are shown in the table.
Analysis of refined product oxygen-containing Compound
Total amount of product (cubic rice) Content of oxygen-containing Compound (ppm)
51 3
102 5
153 5
204 4
255 6
306 5
357 5
408 6
459 7
510 4
561 5
612 6
663 261
714 2130
After raw materials which are 70 times of the volume of the adsorbent are processed, the adsorbent of the first adsorption tower 24 is saturated, the first feed pump 29 and the first discharge pump 30 are stopped, the inlet and outlet valves of the first feed pump 29 and the first discharge pump 30 are all closed, the raw oil discharge pipeline is opened to be connected with the inlet valve of the second feed pump 31, the outlet of the second feed pump 31 is opened to be connected with the valve 2 of the feed inlet of the second adsorption tower 25, other valves of the inlet and outlet of the second feed pump are all closed, the second feed pump 31 is started, the first adsorption tower 24 enters an adsorbent regeneration link, and the second adsorption tower 25 enters a raw oil adsorption link.
Regenerating the adsorbent in the first adsorption tower 24, opening a raw oil discharge pipeline connected with an outlet valve of a first feeding pump 29, opening an inlet of the first feeding pump 29 connected with a feed inlet valve of the first adsorption tower 24, completely closing other valves at the inlet and the outlet of the first feeding pump 29, starting the first feeding pump 29, sending the oil in the first adsorption tower 24 back to the raw oil tank 11, standing for 5-10 hours after the oil in the first adsorption tower 24 is pumped out, fully recovering the oil remained on the adsorbent, and then pumping out the first adsorption tower 24 again. Then, a water discharging pipeline is opened to be connected with an inlet valve of the first feeding pump 29, an outlet of the first feeding pump 29 is opened to be connected with a feed inlet valve of the first adsorption tower 24, other valves of an inlet and an outlet of the first feeding pump 29 are all closed, a valve of an outlet of the first discharging pump 30, which is connected with the oil-water separation tank 10, is opened, and other valves of an outlet of the first discharging pump 30 are all closed. Starting a first feed pump 29, injecting deionized water into the first adsorption tower 24 at a water injection speed of 5 cubic meters per hour, starting a first discharge pump 30 when a liquid level meter 7 at the upper part of the first adsorption tower 24 detects the liquid level, delivering eluent into an oil-water separation tank 10, controlling the discharge speed of the first discharge pump 30 to control the liquid level of the liquid level meter 7 of the first adsorption tower 24 to be 100-200 millimeters, and stopping water injection when the injected water amount reaches 60 cubic meters. And opening a water discharging pipeline to connect an outlet valve of the first feeding pump 29, opening an inlet of the first feeding pump 29 to connect a feeding port valve of the first adsorption tower 24, closing other valves of an inlet and an outlet of the first feeding pump, starting the first feeding pump, and sending the deionized water in the first adsorption tower 24 back to the oil-water separation tank 10. Then, the drain valve 12 connected to the steam trap 13 at the bottom of the first adsorption tower 24 is opened, the other valves of the first adsorption tower 24 are all closed, heating steam is injected into the first adsorption tower 24 from the top of the tower at a steam injection rate of 200 kg/h, condensed water is discharged through the steam trap 13 at the bottom of the tower, when the temperature of the adsorption tower bottom thermometer 19 rises to 120 ℃ or higher, the steam injection rate is reduced to 50 kg/h, the valve connected to the steam trap is closed, the vacuum valve 15 connected to the evacuation system of the first adsorption tower 24 is opened to gradually reduce the pressure in the first adsorption tower 24, when the pressure in the tower falls to-0.05 MPa or lower, the steam injection rate is appropriately adjusted to maintain the temperature at the lower part of the adsorption tower at 120 ℃ or higher, after 5 hours, the heating steam is closed, the evacuation is maintained for 2 hours, then the vacuum valve 15 connected to the vacuum system is closed, and the first adsorption tower 24 is naturally cooled to about 50 ℃ and can enter the next cycle of operation.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, many modifications and substitutions can be made without departing from the technical principle of the present invention, and these modifications and substitutions should also be regarded as the protection scope of the present invention.

Claims (10)

1. An isoparaffin solvent refining system which characterized in that: the oil-water separation device comprises an oil-water separation tank, a raw oil tank, a first adsorption tower, a second adsorption tower, a finished product tank, a vacuum pump, a condenser, a first feeding pump, a first discharging pump, a second feeding pump and a second discharging pump, wherein the oil-water separation tank reaches the raw oil tank and is connected with the first feeding pump and the inlet of the second feeding pump respectively, the first feeding pump reaches the outlet of the second feeding pump and is connected with the oil-water separation tank and the raw oil tank respectively, the feed inlet of the first adsorption tower is communicated with the first feeding pump in a circulating manner, the feed inlet of the second adsorption tower is communicated with the second feeding pump in a circulating manner, the discharge outlet of the first adsorption tower is connected with the inlet of the first discharging pump, the outlet of the first discharging pump is connected with the feed inlets of the oil-water separation tank, the finished product tank and the second adsorption tower respectively, the discharge outlet of the second adsorption tower is connected with the inlet of the oil-water separation tank, the finished product tank and the feed inlet of the first adsorption tower are connected with the outlet of the second discharge pump, the steam system is connected with the discharge outlet of the first adsorption tower and the vacuum pump are connected with the condenser respectively.
2. The isoparaffin solvent refining system according to claim 1, wherein: the first adsorption tower reaches the second adsorption tower all includes the adsorption tower main part, the upper end of adsorption tower main part is equipped with the charging hole, just charging hole and atmosphere and steam system intercommunication, the bottom of adsorption tower main part is equipped with the feed inlet reaches the discharge port, the inside of adsorption tower main part is equipped with the adsorbent bed that is used for placing the adsorbent, the lateral wall of adsorption tower main part is located the top on adsorbent bed is equipped with the discharge gate.
3. The isoparaffin solvent refining system of claim 2, wherein: the side wall of the adsorption tower main body is located a liquid level meter pressure leading port is arranged above the adsorbent bed layer, a liquid level pipe is arranged between the liquid level meter pressure leading port and the charging port, and a liquid level meter is arranged on the liquid level pipe.
4. The isoparaffin solvent refining system according to claim 3, wherein: the filling port is provided with a sealing plate, the sealing plate is provided with an opening, the opening is provided with an atmosphere pipe, the atmosphere pipe is provided with an atmosphere valve, the liquid level pipe is connected with the atmosphere pipe, a steam pipe used for being connected with a steam system is arranged between the liquid level pipe and the atmosphere valve on the atmosphere pipe, and the steam pipe is provided with a steam valve.
5. The isoparaffin solvent refining system of claim 2, wherein: the drainage device is characterized in that the discharge port is provided with a branch pipe, the branch pipe is respectively connected with a drainage pipe, a blow-off pipe and a vacuum pipe, a drainage valve and the steam trap are sequentially arranged on the drainage pipe along the water flow direction, a blow-off valve is arranged on the blow-off pipe, a vacuum valve is arranged on the vacuum pipe, and the outlet of the vacuum pipe is connected with the vacuum pump.
6. The isoparaffin solvent refining system according to claim 2, wherein: the adsorption tower comprises an adsorption tower body, wherein an upper cover is arranged at the upper end of the tower body, a charging hole is formed in the upper cover, a lower cover is arranged at the lower end of the tower body, a feeding hole and a discharging hole are formed in the lower cover, thermometers are arranged on the upper portion, the middle portion and the lower portion of the tower body, and a heat preservation layer is coated on the outer wall of the adsorption tower body.
7. The isoparaffin solvent refining system of claim 6, wherein: the bottom of tower body is equipped with the support frame, be equipped with the screen cloth on the support frame, the adsorbent bed support in on the screen cloth, the lateral wall of tower body is located the lower extreme on adsorbent bed is equipped with the adsorbent discharge opening.
8. A refining method of an isoparaffin solvent is characterized in that: the method comprises the following steps:
filling adsorbents into the first adsorption tower and the second adsorption tower;
raw material oil of an isoparaffin solvent is injected into a first adsorption tower from a raw material oil tank through a first feed pump, an isoparaffin solvent product subjected to oxygen-containing compound removal is led out from a discharge hole of the first adsorption tower to a finished product tank through a first discharge pump, and the oxygen-containing compound content of the isoparaffin solvent product is continuously monitored;
injecting the finished product from the first adsorption tower into the second adsorption tower from a discharge hole of the first adsorption tower through the first discharge pump, leading out the isoparaffin solvent product from a discharge hole of the second adsorption tower to the finished product tank through the second discharge pump after removing the oxygen-containing compound, and simultaneously closing a valve from the first discharge pump to the finished product tank.
Stopping injecting the raw oil into the first adsorption tower, and simultaneously injecting the isoparaffin solvent raw oil into the second adsorption tower through a second feed pump by the raw oil tank;
returning the oil stored in the first adsorption tower to a raw oil tank through a first feeding pump;
the oil-water separation tank injects deionized water into the first adsorption tower through a first feed pump, and the eluent is led out from a discharge port of the first adsorption tower to the oil-water separation tank through a first discharge pump;
the water stored in the first adsorption tower returns to the oil-water separation tank through a first feed pump, high-temperature steam is introduced into the first adsorption tower from a charging port of the first adsorption tower, and condensed water is discharged through a steam trap;
when the temperature at the bottom of the first adsorption tower rises to over 120 ℃, connecting the first adsorption tower with a vacuum system to vacuumize, and then naturally cooling the adsorption tower;
when the adsorbent in the second adsorption tower is saturated, the adsorption is stopped, and the regeneration operation of the first adsorption tower is repeated.
9. The process for refining an isoparaffin solvent according to claim 8, wherein: the feeding airspeed of the raw oil of the isoparaffin solvent injected into the adsorption tower is 0-30/h, the operation temperature in the adsorption tower is-20-60 ℃, and the operation pressure in the adsorption tower is 0-1.0Mpa.
10. The process for refining an isoparaffin solvent according to claim 8, wherein: the injection airspeed of the deionized water into the adsorption tower is 0.5-5/h; the steam pressure of the high-temperature steam is 0.6-1.0MPa.
CN202211295363.3A 2022-10-21 2022-10-21 Isoparaffin solvent refining system and refining method Pending CN115491231A (en)

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