CN101708448A - Method and device for liquid flooding and gas dissolving - Google Patents

Method and device for liquid flooding and gas dissolving Download PDF

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Publication number
CN101708448A
CN101708448A CN200910199843A CN200910199843A CN101708448A CN 101708448 A CN101708448 A CN 101708448A CN 200910199843 A CN200910199843 A CN 200910199843A CN 200910199843 A CN200910199843 A CN 200910199843A CN 101708448 A CN101708448 A CN 101708448A
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liquid
gas
separator
reactor
liquid flooding
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CN101708448B (en
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方向晨
汪华林
徐效梅
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Sinopec Fushun Research Institute of Petroleum and Petrochemicals
Shanghai Huachang Environmental Protection Co Ltd
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Sinopec Fushun Research Institute of Petroleum and Petrochemicals
Shanghai Huachang Environmental Protection Co Ltd
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Abstract

The invention provides a method for liquid flooding and gas dissolving, comprising the following steps: enabling the flooded liquid in a reactor to enter a separator arranged in the reactor to be separated so as to remove the gas phase, the gas components and fine solid particle components in the flooded liquid and eliminate the flooded liquid, making the raw oil flowing out of an outlet on the lower end of the separator directly contact and react with the hydrogen coming out of a sieving plate of the reactor to recycle the raw oil; and discharging the gas components coming out of an outlet on the upper end of the separator directly out of the outlet on the upper part of the reactor for subsequent utilization. The invention also discloses a device for liquid flooding and gas dissolving.

Description

Molten gas method of liquid flooding and device
Technical field
The invention belongs to the chemical industry environmental protection field, relate to molten gas method of a kind of liquid flooding and device.Particularly, relate to and adopt little cyclone separator to eliminate liquid flooding phenomenon in the hydrogenation reactor technical process, remove the method for the materials such as nitrogen, sulfide and solid particle in the feedstock oil, this method is applicable to handles the heterogeneous separation process of solution-air that comprises liquid flooding in the hydrogenation reactor technical process, sulfur-containing impurities, solid particle.
Background technology
Through the exploitation in more than 100 years, the output of low-sulfur light crude oil was fewer and feweri on the earth.At present, the output of sour crude oil (sulfur content is between the 0.5-2.0%) and sour crude (sulfur content is more than 2.0%) has accounted for more than 75% of crude oil total output in the world, wherein sulfur content has accounted for more than 55% of crude oil total output at the crude output more than 1%, and sulfur content also accounts for more than 30% in the output of the sour crude more than 2%.
Along with China refines the increasing of sour crude oil, in the feedstock oil as further processing processing, sulfur content is more and more higher, has increased the weight of the corrosion to equipment, and sulfide content also improves thereupon in the product.These have all promoted the fast development of feedstock oil hydrogenation plant.
In the feedstock oil hydrogenation process, liquid is dirty by the overflow downcomer block-by-block along column plate, and the steam higher with temperature contacts on column plate, takes place to conduct heat and part evaporation, partial condensation.At this moment, if the liquid on the column plate is difficult to flow down along overflow downcomer, can cause the interior liquid level of overflow downcomer to rise higher and higher, until equal with the liquid level on the column plate, liquid can't be dirty, will cause that liquid flooding or liquid are outstanding, also claims flooding.When liquid level in the overflow downcomer surpass the overflow downcomer height 50% the time, just think to begin to take place slight liquid flooding.
Facilitate the factor of liquid flooding to mainly contain following two:
A. the liquid top plate that flows backwards back in the downspout
Because column plate has resistance to the air-flow that rises, the pressure of the pressure ratio top plate top of lower plywood top is big, have only when downspout inner foam height relative hydrostatic head can overcome this pressure reduction the time, liquid could be toward dirty.
Gas flow strengthens when fluid flow is constant, and the pressure differential between lower plywood and the top plate is also along with increase, and the liquid level in the downspout increases.If gas flow is increased to the liquid that makes in the downspout and is elevated to weir crest, the liquid in the pipe just not only can not begin the top plate that flows backwards back toward dirty on the contrary, just begins hydrops on the plate; Constantly there is liquid outside tower, to send into when being operated, can makes full tower be full of liquid at last, just formed liquid flooding.
Fluid flow strengthens if gas flow is certain, and liquid is by the resistance increase of downspout, and liquid layer thickening on the plate, makes plate pressure differential up and down strengthen, and all can make liquid level rising in the downspout, thereby cause liquid flooding.
B. excessive entraining is to top plate
Air-flow is entrained to the liquid foam of last layer plate, can be so that liquid layer thickening on the plate under the normal condition, increases also not obviously.Under the certain liq flow, if gas flow is increased to a certain degree, the thickening of liquid layer just significantly get up (amount of liquid increases on the plate, and bubble is added, strengthened).Air communication is crossed the liquid foam that the liquid layer of thickening takes out of and is further added again.This excessive entraining makes froth bed top and the distance at the bottom of the last layer plate dwindle, and liquid foam entrainment is growing on and on constantly, and big drop easily is directly injected to the last layer plate, and foam also can emit the last layer plate, and extremely complete eventually tower is full of by liquid.
More than in two kinds of reasons of facilitating liquid flooding, excessive entraining more commonly.Liquid flooding takes place in the reactor not to be had when in time handling, very big fluctuation will take place in resistance, liquid level in the tower, destroy tower internal reaction process, make product purity not reach requirement, and fluctuation is very big in the tower, can't keep the ordinary production of equipment, more seriously can cause equipment parking accident.
Hydrogenation reactor liquid flooding phenomenon causes in the time of may designing: carry secretly at excessive mist end, and dry-plate pressure drop is excessive, and vapour speed is too fast; The downspout design is too small, and liquid has little time to flow to lower floor's tower tray on the tower tray; The downspout size is no problem, but the flow velocity that enters downspout on the tower tray is too fast, forms and the direct bridging of downspout side tower wall, and liquid can't smooth and easyly run down into lower floor's tower tray.If design does not have problems, and tower put into production and this situation occurred, may operate and cause, that is, capacity of returns is excessive, but while tower bottom steam thermal source does not have corresponding increase; The charging of liquid phase excess load; Tower tray stops up.
Want to overcome the generation of above-mentioned phenomenon, just must strictness control reflux ratio well, reduce charging, steadily regulate thermal source, stop up if serious tower tray takes place, then might need to stop replace material after, add water and boil tower.The operation easier that these have increased equipment has promoted maintenance cost, the cost of investment height.
In order to overcome above-mentioned shortcoming, those skilled in the art have dropped into a large amount of time, energy carries out exploratory development, successively developed the new high-efficiency filler of many high-specific surface areas, high voidage, improve the contact condition of gas-liquid two-phase in the tower, improved the mass transfer separative efficiency and the production capacity of packed tower effectively.But up to the present, by these approach packed tower is optimized and following two problems occurred:
1, many new type high-efficient packing complex manufacturing technology, cost is higher;
2, the space of further optimizing is quite limited.
Therefore, at the liquid flooding phenomenon in the molten gas process of liquid flooding, this area presses for a kind of method that can eliminate the liquid flooding phenomenon under nominal situation of developing.
Summary of the invention
The present invention makes full use of the liquid flooding phenomenon in the tower, and molten gas method of a kind of liquid flooding and device are provided, and has solved the liquid flooding problem that exists in the hydrogenation process, has improved product purity, has kept the ordinary production of equipment, has reduced maintenance cost, has reduced energy consumption.
On the one hand, the invention provides the molten gas method of a kind of liquid flooding, this method comprises:
Make liquid flooding in the reactor partly enter the built-in separator of described reactor and separate,, eliminate the liquid flooding phenomenon, the gas, the solid particulate components that remove in the liquid simultaneously to be carried secretly to remove gas phase, the fine solid particle component that described liquid flooding part is carried secretly;
Make feedstock oil that described separator lower end exports out directly with the hydrogen haptoreaction of coming out from the reactor sieve plate, make feedstock oil recycling; And
The gas component that described separator upper end exports is out directly discharged from the outlet of described reactor top, carry out later use.
One preferred embodiment in, utilize pressure official post liquid flooding wherein in the reactor partly to enter separator and separate.
Another preferred embodiment in, the amount of liquid of carrying secretly when the inlet gas of described reactor is not more than 4000mg/m 3The time, the amount of liquid that exit gas is carried secretly is not more than 300mg/m 3
Another preferred embodiment in, use little cyclone separator to separate, the import of described little cyclone separator and the pressure between the gaseous phase outlet fall and are not more than 0.0002MPa, amount to 20mm water column height, overfall gas liquid content is not more than 100mg/m 3
Another preferred embodiment in, after described little cyclone separator separated, the solid particle rate of removing in the feedstock oil was not less than 80%.
Another preferred embodiment in, described little cyclone separator is made up of eddy flow core pipe.
On the other hand, the invention provides a kind of liquid flooding air-dissolving apparatus that is exclusively used in the molten gas method of above-mentioned liquid flooding, this device comprises:
Be built on the sieve plate of reactor, the separator under the gaseous phase outlet, be used for the liquid flooding in the described reactor is partly separated, to remove gas phase, the fine solid particle component that described liquid flooding part is carried secretly, eliminate the liquid flooding phenomenon, the gas, the solid particulate components that remove in the liquid simultaneously to be carried secretly.
One preferred embodiment in, described reactor comprises:
The sieve plate that is placed in one, make feedstock oil that described separator lower end exports out directly and hydrogen in sieve plate place haptoreaction, make feedstock oil recycling;
Place the gaseous phase outlet at its top, be used to discharge the gas component that described separator upper end exports out; And
Place the liquid phase outlet of its bottom, be used to discharge liquid phase.
Another preferred embodiment in, described separator is little cyclone separator, the import of described little cyclone separator and the pressure between the gaseous phase outlet fall and are not more than 0.0002MPa, amount to 20mm water column height, overfall gas liquid content is not more than 100mg/m 3
Another preferred embodiment in, described little cyclone separator is made up of eddy flow core pipe.
Description of drawings
Fig. 1 is the schematic diagram according to the built-in separation of the molten gas technology of reactor liquid flooding of one embodiment of the present invention.
Fig. 2 is the schematic diagram according to the operation principle of the built-in little cyclone separator of the reactor liquid flooding air-dissolving apparatus of one embodiment of the present invention.
The specific embodiment
The present inventor finds after having passed through extensive and deep research, in conventional hydrogenation liquid flooding technical process, feedstock oil is dirty by the overflow downcomer block-by-block, the hydrogen steam higher with temperature contacts at the sieve plate place, remove materials such as wherein sulfide, nitrogen, and the column plate resistance is when increasing, then can cause the liquid flooding phenomenon, when increasing to the rising steam, can't take off when holding the liquid on the column plate, will rush down and descend from sieve aperture one, destroy production process in the tower, cause product purity not reach requirement, can't keep ordinary production; After the reactor built-in splitter, the liquid flooding partially liq relies on pressure differential, cut enters in the separator, under powerful centrifugal action, begin centrifugation, form downward outer eddy flow and the interior eddy flow that makes progress, wherein, the drop that density is big, particulate enter outer eddy flow, converge from the underflow opening of separator and discharge cycling and reutilization; In the eddy flow, directly discharge reactor in the gas component that density is little then enters into, enter into follow-up equipment by the overfall of separator, thereby eliminated liquid flooding, guaranteed product purity, kept the continuous running of whole device, reduce maintenance cost, and reduced energy consumption.Based on above-mentioned discovery, the present invention is accomplished.
Technical conceive of the present invention is as follows:
Utilize the pressure differential in the tower, make that the liquid flooding in the tower partly enters separation in the separator that is built in the tower, to remove its gas phase of being carried secretly, fine solid particle component; The hydrogen haptoreaction that the feedstock oil that separator lower end exports out is direct and sieve plate comes out, recycling; The gas component that separator top exports is out then directly discharged by the outlet of tower upper end, enters follow-up equipment.
In a first aspect of the present invention, provide a kind of gas molten gas method, this method comprises:
Utilize the pressure differential in the tower, make that the liquid flooding in the tower partly enters separation in the separator that is built in the tower, to remove its gas phase of being carried secretly, fine solid particle component;
The hydrogen haptoreaction that the feedstock oil that separator lower end exports out is direct and sieve plate comes out, recycling; And
The gas component that separator top exports is out then directly discharged by the outlet of tower upper end, enters follow-up equipment.
Preferably, when the constant increasing fluid flow of the constant increasing gas flow of fluid flow, gas flow, sieve plate pressure differential up and down strengthens, and makes that liquid level raises in the downspout, causes device that inevitable liquid flooding phenomenon takes place; After the device built-in splitter, this liquid flooding part then directly enters separator separates, and has avoided liquid phase component directly to overflow from cat head, and liquid, gas after the separation enter follow-up equipment.
Preferably, when the gas excessive entraining, froth bed top dwindles with the distance at the bottom of the last layer plate, is full of by liquid to full tower eventually, and this partially liq enters directly that separator carries out gas, liquid two is separated.
Preferably, under specified fluid flow, gas speed is greater than liquid flooding gas when speed, and liquid promptly is full of full tower, enters separator and separates.
On the other hand, the invention provides a kind of liquid flooding air-dissolving apparatus, this device comprises:
Be used for feedstock oil, hydrogen are carried out the reactor 1 of materials such as sulfide removal, nitrogen, feedstock oil, hydrogen two-phase sieve plate 3 places in reactor 1 fully contact; Be built in the separator 2 in the reactor, be used for liquid flooding is partly partly or entirely separated.
Preferably, described separator is preferably little cyclone separator, this little cyclone separator is built on the sieve plate of reactor, liquid flooding that can't be dirty in the overflow downcomer partly relies on pressure differential, cut enters in little cyclone separator, rely on centrifugal force to carry out solution-air two and be separated, eliminate the liquid flooding phenomenon, guarantee equipment stable operation.
Described little cyclone separator is made up of some eddy flow core pipes, and its separative efficiency is higher than conventional cyclone far away, and the operating pressure of little cyclone separator of while falls little, and energy consumption is low.Hydrogenation reactor is efficient, safety, environmental harmony and long-term operation are the Future Development directions.The present invention makes full use of reactor liquid flooding phenomenon, provides a kind of method of reactor built-in splitter, solves the liquid flooding problem that is produced in the course of reaction.Wherein, cyclone separator is so that floor space is little, simple in structure, energy consumption is low, be convenient to outstanding advantages such as operation and maintenance, and first-selection is the tower built-in splitter.Simultaneously, but little cyclone separator still is a kind of equipment of efficient, safety long-term operation.
In the present invention, after little cyclone separator separated, the solid particle rate of removing in the feedstock oil was not less than 80%.
In the present invention, described little cyclone separator is made up of some cover eddy flow core pipes, and its material needs acid-alkali-corrosive-resisting and resistance to wears, and specifically can be polyurethane, composite etc.
In the present invention, the component of described liquid flooding part is separated, the amount of liquid of carrying secretly when Reactor inlet gas is not more than 4000mg/m 3The time, the amount of liquid that exit gas is carried secretly is not more than 300mg/m 3
In the present invention, in the liquid flooding separation process, the pressure loss of little cyclone separator is not more than 0.0002MPa, amounts to 20mm water column height, and overfall gas liquid content is not more than 100mg/m 3, be not less than 5 years the service life of eddy flow core pipe.
In the present invention, under metered flow, the import of little cyclone separator and the pressure between the gaseous phase outlet are reduced to and are not more than 0.0002MPa, amount to 20mm water column height.In the whole service process, little cyclone separator needs repairing hardly, does not have any offal treatment expense, and operating cost is extremely low.
Below referring to accompanying drawing.
Fig. 1 is the schematic diagram according to the built-in separation of the molten gas technology of reactor liquid flooding of one embodiment of the present invention.As shown in Figure 1, after feedstock oil entered reactor by reactor 1 upper end, the hydrogen steam higher with temperature contacted at sieve plate 3 places, to remove materials such as wherein sulfide, nitrogen; Liquid level in overflow downcomer does not reach the pressure that fluid column produces, and in the time of can not overcoming the resistance of upper and lower pressure reduction of column plate and overflow downcomer, when column plate resistance or the increase of overflow downcomer resistance, then liquid can not be dirty, causes liquid flooding; Entering separator 2 inside from separator import cut under the differential pressure action of liquid flooding component in reactor separates; The feedstock oil that described separator lower end exports out directly with the hydrogen haptoreaction of coming out (and replenish new hydrogen to reactor) from the reactor sieve plate, make feedstock oil recycling (recycle oil); The gas component that described separator upper end exports is out discharged from the gaseous phase outlet 4 that places reactor head; Liquid phase component is discharged from the liquid phase outlet 5 that places reactor bottom.
Fig. 2 is the schematic diagram according to the operation principle of the built-in little cyclone separator of the reactor liquid flooding air-dissolving apparatus of one embodiment of the present invention.As shown in Figure 2, gas-liquid two-phase enters little cyclone separator, because of the change of cross section of fluid channel, make liquid stream speedup and form the spiral fluidised form after eddy flow core pipe separation cone, wherein gaseous component is agglomerated into gaseous core in the center of Taper Pipe, discharge from overfall, liquid phase component is eddy flow outside Taper Pipe wall place forms then, discharges from core pipe underflow opening, makes that gas-liquid two-phase obtains separating, reduce the resistance of overflow downcomer, avoided the liquid flooding phenomenon.
Major advantage of the present invention is:
The present invention has partly carried out separating treatment to the liquid flooding in the molten gas process of liquid flooding, has avoided the liquid flooding in the reaction process process, the separative efficiency height, improve the purity of product, kept the ordinary production of equipment, and prolonged the service life of follow-up equipment, reduce cost of investment, reduced energy consumption.
All quote in this application as a reference at all documents that the present invention mentions, just as each piece document is quoted separately as a reference. Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after having read above-mentioned instruction content of the present invention, these equivalent form of values fall within the application's appended claims limited range equally.

Claims (10)

1. molten gas method of liquid flooding, this method comprises:
Make liquid flooding in the reactor partly enter the built-in separator of described reactor and separate,, eliminate the liquid flooding phenomenon, the gas, the solid particulate components that remove in the liquid simultaneously to be carried secretly to remove gas phase, the fine solid particle component that described liquid flooding part is carried secretly;
Make feedstock oil that described separator lower end exports out directly with the hydrogen haptoreaction of coming out from the reactor sieve plate, make feedstock oil recycling; And
The gas component that described separator upper end exports is out directly discharged from the outlet of described reactor top, carry out later use.
2. the method for claim 1 is characterized in that, utilizes the interior pressure official post liquid flooding wherein of reactor partly to enter separator and separates.
3. method as claimed in claim 1 or 2 is characterized in that the amount of liquid of carrying secretly when the inlet gas of described reactor is not more than 4000mg/m 3The time, the amount of liquid that exit gas is carried secretly is not more than 300mg/m 3
4. method as claimed in claim 1 or 2 is characterized in that, uses little cyclone separator to separate, and the import of described little cyclone separator and the pressure between the gaseous phase outlet fall and is not more than 0.0002MPa, and overfall gas liquid content is not more than 100mg/m 3
5. method as claimed in claim 4 is characterized in that, after described little cyclone separator separated, the solid particle rate of removing in the feedstock oil was not less than 80%.
6. method as claimed in claim 4 is characterized in that, described little cyclone separator is made up of eddy flow core pipe.
7. liquid flooding air-dissolving apparatus, this device comprises:
Be built on the sieve plate (3) of reactor (1), the separator (2) under the gaseous phase outlet (4), be used for the liquid flooding in the described reactor is partly separated, to remove gas phase, the fine solid particle component that described liquid flooding part is carried secretly, eliminate the liquid flooding phenomenon, the gas, the solid particulate components that remove in the liquid simultaneously to be carried secretly.
8. device as claimed in claim 7 is characterized in that, described reactor (1) comprising:
The sieve plate that is placed in one (3), make feedstock oil that described separator (2) lower end exports out directly and hydrogen in sieve plate place haptoreaction, make feedstock oil recycling;
Place the gaseous phase outlet (4) at its top, be used to discharge the gas component that described separator (2) upper end exports out; And
Place the liquid phase outlet (5) of its bottom, be used to discharge liquid phase.
9. as claim 7 or 8 described devices, it is characterized in that described separator is little cyclone separator, the import of described little cyclone separator and the pressure between the gaseous phase outlet fall and are not more than 0.0002MPa,, overfall gas liquid content is not more than 100mg/m 3
10. device as claimed in claim 9 is characterized in that, described little cyclone separator is made up of eddy flow core pipe.
CN2009101998438A 2009-12-03 2009-12-03 Method and device for liquid flooding and gas dissolving Active CN101708448B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8926826B2 (en) 2011-04-28 2015-01-06 E I Du Pont De Nemours And Company Liquid-full hydroprocessing to improve sulfur removal using one or more liquid recycle streams

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN85100027A (en) * 1985-04-01 1985-10-10 天津大学 Internal thermal siphon boiling element
US5632867A (en) * 1992-05-19 1997-05-27 Exxon Research And Engineering Company Recovering a relatively volatile component of a solution from a less volatile component, e.g. as in solvent recovery

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8926826B2 (en) 2011-04-28 2015-01-06 E I Du Pont De Nemours And Company Liquid-full hydroprocessing to improve sulfur removal using one or more liquid recycle streams

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