CN102443409B - Process method for prolonging operation period of hydrogenation device and hydrogenation reaction device - Google Patents
Process method for prolonging operation period of hydrogenation device and hydrogenation reaction device Download PDFInfo
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- CN102443409B CN102443409B CN201010509020.3A CN201010509020A CN102443409B CN 102443409 B CN102443409 B CN 102443409B CN 201010509020 A CN201010509020 A CN 201010509020A CN 102443409 B CN102443409 B CN 102443409B
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Abstract
The invention provides a process method for prolonging the operation period of a hydrogenation device and the hydrogenation device. At least one fixed bed hydrogenation catalyst bed layer is arranged in a hydrogenation reactor, reaction materials enter the reactor from the upper part and flow out from the reactor from the lower part, and a structure capable of realizing the direct circulation of the reaction materials when the pressure reduction of the reactor is improved is arranged in a catalyst bed layer arranged on the top of the hydrogenation reactor. The method and the device have the advantages that great change on the existing device is not needed, the long-period operation of the device can be realized at lower investment, in addition, catalysts of the whole bed layer are sufficiently utilized, simultaneously, the pressure reduction of the reactor is reduced, the production safety is ensured, and the economic benefits are increased.
Description
Technical field
The present invention relates to a kind of processing method and hydrogenation reaction device of prolonging operation period of hydrogenation device, belong to the petrochemical technology field.
Background technology
In recent years, because petroleum resources in world wide scarcity and various countries constantly increase the demand of the energy day by day, people more and more pay attention to the utilization of residual oil.A kind of as decarburization technique, slag oil coking process has the advantages such as less investment, process cost are low, has therefore obtained development widely.
Coking distillate (coking naphtha, coker gas oil, wax tailings) olefin(e) centent is high, and the content of heteroatoms such as sulphur, nitrogen, silicon are high, and stability is poor, can not be directly as product, uses, even can not be directly as the charging of downstream unit.For making coking distillate meet the end product standard or meeting the charging requirement of downstream unit, must carry out hydrofining or hydrotreatment.
In the process of coking distillate hydrogenation and removing sulphur, nitrogen, owing to containing diolefine, silicon and the tiny impurity such as coke powder in raw material, so often affect the operational stability of device.Daqing petrochemical company 300kt/a Hydrogenation of Coker Gasoline device is after the half a year that goes into operation, occur continuously in one day that twice system pressure difference is too high, cause being forced to stop work (the rising analysis of causes of coking gasoline hydrogenation refining system pressure difference and countermeasure, " refining and chemical industry ", the 19th volume: 20).The reactor catalyst bed pressure drop too fast problem that rises also appears in Guangzhou Branch 300kt/a hydrogenation unit when processing coker gasoline.This device once, within the time of a year and a half, caused stopping work defect elimination 5 times (analysis of causes and countermeasure that the hydrofining reaction system pressure drop raises, " China and foreign countries' energy ", 2007, the 12 volumes) because the reactive system bed pressure drop raises.General 3～5 days needs of two I Hydrogenation of Coker Gasoline devices of Anqing branch office oil refining clean a strainer, to stop work in 1 year and skim for 2～3 times, have a strong impact on normal operation (Coke Inhibitor for Coker Gasoline Hydrofining Unit, " petrochemical technology " of device, 2006,13 (4): 5).All there is Similar Problems in various degree in domestic and international device of the same type, the increase of pressure difference between bed, make the inner members such as the support bar of catalyzer and back up pad when bearing catalyst weight, again must the outer pressure of commitment, bring hidden trouble to the safety operation of device.Therefore, it is the conspicuous contradiction that affects coking distillate hydrogenation unit long-term operation that bed pressure drop rises too fast always, in the urgent need to working out effective means, solves coking problem.
The rising of coking distillate hydrogenator pressure drop all comes from the bed coking of catalyzer top.Through large quantity research, show, the coking factor is very complicated, is deposited on beds top mainly due to the polymerization of the unsaturated hydro carbons such as diolefine in raw material and mechanical impurity that upstream device is brought into and causes.Polymerization just can occur in the diolefine in raw material under cold condition, first generates oligopolymer, to superpolymer, transforms until coking rapidly subsequently.In the sample of coking, the content of iron is quite high, to have formed naphthenic acid with organic hydrocarbon after the stock oil dissolved oxygen, the iron of naphthenic acid corrosion device generates iron naphthenate, stably be dissolved in stock oil, iron naphthenate is easy to occur hydrogenolysis after mixed hydrogen, and react with hydrogen sulfide and generate Iron sulfuret and be deposited on reactor top bed, promote the coking reaction of coking parent, accelerated the obstruction of beds.In addition, contain a small amount of tiny coke powder in raw material and there is very strong adsorptivity, easily and the organic macromolecule compound formed in polyreaction be bonded together, make burnt dirty particle grow up gradually, when it grows up to a certain size, will be deposited in reactor, result in blockage.
Cause the too high problem of pressure drop for the reaction coking, current solution has following several:
1, carry out the management work of raw material, adopt the modes such as nitrogen protection, avoid raw material to contact with air, at utmost reduced the chance of unsaturated hydro carbons formation colloid in the raw material.This is a kind of passive raw material guard method, if the raw material mechanical impurity of upstream input is more, diene content is very high, or carries a lot of coke powders secretly, and the party's rule is helpless.
2, mix refining virgin kerosene or straight-run diesel oil, diluted the unsaturated hydro carbons such as diolefine in the raw material, reduced the severity of hydrogenation unit, make the device operation more stable.But the method has been sacrificed the amount of finish of hydrogenation device for treatment coking distillate, has in fact reduced the air speed to coking distillate, and economy is poor.
3, between the entrance and exit of pretreatment reaction device, by-pass is set, during normal production, reaction mass enters process furnace after by the pretreatment reaction device, when pretreatment reaction device beds Pressure Drop raises, reaction mass enters process furnace through by-pass, until the pretreatment reaction device, partly or entirely more after catalyst changeout, reaction mass switches to the pretreatment reaction device again and enters process furnace.Although the method can assurance device operation downtime not, in the not pretreated situation of raw material, can cause larger impact to the main reactor temperature rise, make the more difficult control of operation.The replacing of pretreatment catalyst simultaneously also can cause financial loss.
4,, in preposition/rearmounted reactor process, adopt the mode of two reactors in series to operate.After preposition reactor is saturated by silicon, by the blocked operation of pipeline, makes the raw material rearmounted reactor of first flowing through, and then pass through lead reactor.Due to the impact that can reduce the main reactor temperature rise, so can process more coking distillate than above-mentioned bypass reactor.But the method need to increase a reactor, and complicated operation.
In hydrogenator, in order to make the gas-liquid distributed uniform, generally at the top of beds, gas-liquid partition tray is set, operated by rotary motion gas-liquid allotter on gas-liquid partition tray, as bubble cap formula gas-liquid allotter, gas and liquid enter the beds below distribution plate after gas-liquid allotter is dispersed.Common gas-liquid partition tray only has the gas-liquid distribution function, does not alleviate the effect that beds stops up.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of processing method and hydrogenation reaction device of prolonging operation period of hydrogenation device.The inventive method, can be under less investment without existing apparatus is carried out to large change, the long-term operation of implement device, and take full advantage of the catalyzer of whole bed, and reduce reactor pressure simultaneously and fall, guarantee production safety, increase economic benefit.
The processing method of prolonging operation period of hydrogenation device of the present invention comprises following content: at least one fixed bed hydrogenation beds is set in hydrogenator, reaction mass enters reactor from top, from the bottom outflow reactor, arrange in the beds at hydrogenator top and can make the directly structure of circulation of reaction mass when reactor pressure decrease raises.
This structure for arranging reaction mass standby stream circulation passage in the beds at hydrogenator top, the standby stream circulation passage is the unlimited straight tube channel architecture in lower end, the upper end of standby stream circulation passage penetrates beds top, top, the upper end of standby stream circulation passage is sealed by the pressure burst rupture of membranes, the poor 0.45MPa of being less than of the burstpressures of pressure burst rupture of membranes also is greater than 0.1MPa, and reactor pressure decrease is increased to reaction mass when poor higher than the burstpressures of pressure burst rupture of membranes and directly circulates.
In the inventive method, 3～5 beds of hydrogenator operated by rotary motion, the catalyst type of each beds and consumption, and the hydrogenation technique condition etc., according to the character of processing raw material, and the quality product required is specifically determined.
In the inventive method, standby stream circulation passage upper end can arrange bubble cap, and bubble cap and standby stream circulation passage top have gap.20%～100% height location can be counted in the reactor head beds in standby stream circulation passage lower end from top.The gas-liquid distributing disc on reactor top can be passed in the upper end of standby stream circulation passage, also can be below the gas-liquid distributing disc of reactor top.The diameter of standby stream circulation passage is generally 2～20cm, and quantity evenly arranges according to the scale of hydrogenator, in general circulation passage sectional area sum should be not less than reactor cross section long-pending 5%, be not more than reactor cross section long-pending 30%.
In the inventive method, the pressure burst rupture of membranes of standby stream circulation passage upper end is general selects resistant to elevated temperatures metallic substance to make, the general heat resistance of wanting should be over 300 ℃, as stainless steel pressure rupture disk etc., according to specifically the reaction feed temperature is definite, its pressure difference of bearing is less than 0.45MPa, is preferably 0.2～0.35MPa.The maximum differential pressure that concrete operations can be born according to actual production and reactor carries out type selecting or adjusting.
In the inventive method, at the reactor catalyst bed pressure drop hour, the standby stream circulation passage is not enabled, and hydrogenation unit runs well, identical with normal fixed-bed reactor operation.On gas-liquid partition tray, enter beds under stock oil and hydrogen are backward by conventional gas-liquid allotter mixing and carry out hydrogenation reaction.When the pressure drop of beds top larger, in the time of perhaps substantially can't passing through the gas-liquid logistics, the pressure burst rupture of membranes of standby stream circulation passage upper end breaks under the effect of pressure difference, and the gas-liquid logistics can enter the beds bottom by the standby stream circulation passage and proceed hydrogenation reaction.
In the inventive method, the activity of different catalysts bed hydrogenation catalyst can be identical, also can be different, and the mode preferably increased successively by the activity of reagent flow direction catalyzer arranges.The activity of catalyzer is general relevant to active metallic content in catalyzer, the catalyst activity that active metallic content is high is generally higher, the activity of catalyzer is also relevant to support, auxiliary agent kind, preparation method etc., concrete catalyzer can be selected commercial goods, this area catalyzer as required, also can be by the existing method preparation in this area.
The hydrogenation catalyst that the inventive method is used can be the product of this area routine, reactive metal wherein can for nickel, cobalt, molybdenum or tungsten etc. one or more.As comprised by weight percentage: nickel or cobalt are 0.2%～15.0% (calculating by its oxide compound), molybdenum or tungsten are 1%～30% (calculating by its oxide compound), carrier can be aluminum oxide, silicon oxide, aluminum oxide silicon monoxide etc. one or more.Catalyzer is extrudate or spherical.The bulk density of catalyzer is 0.5～0.8g/cm
3, granules of catalyst diameter (spherical diameter, bar shaped diameter or trifolium diameter etc.) is 0.8～10mm, and length is 1.0～50.0mm, and specific surface area is for being greater than 150m
2/ g, pore volume is greater than 0.30cm
3/ g.
Hydrogenation operation condition of the present invention is generally: reaction mass enters from reactor top, from reactor bottom, discharges, and reaction pressure is 1.0～18.0MPa, is preferably 2.0～15.0MPa; During liquid, volume space velocity is 0.5～5.0h
-1, be preferably 1.0～3.0h
-1; Temperature of reaction is controlled at 160～420 ℃, is preferably 200～390 ℃; Hydrogen to oil volume ratio is 100: 1～1800: 1, is preferably 300: 1～1000: 1.
The inventive method can be used in the fixed bed hydrogenation technological process of coking distillate, also can be used in the raw material fixed bed hydrogenation aspect that other alkene, diolefine and content of impurities are higher, as the fixed bed hydrogenation technological process of coal tar or residual oil etc.
The inventive method is after rupture disk is opened, and the catalytic amount worked although actual reduces, and can carry out the conditioned reaction effect by operational conditions such as suitable raising temperature of reaction, can meet the needs of the hydrogenation reaction degree of depth.
Hydrogenation reaction device of the present invention, comprise hydrogenator, at least one fixed bed hydrogenation beds is set in hydrogenator, reaction mass standby stream circulation passage is set in the beds at hydrogenator top, the standby stream circulation passage is the unlimited straight tube channel architecture in lower end, the upper end of standby stream circulation passage penetrates beds top, top, and the upper end of standby stream circulation passage is by the sealing of pressure burst rupture of membranes, and the poor 0.45MPa of being less than of the burstpressures of pressure burst rupture of membranes also is greater than 0.1MPa.Other structure is described in above-mentioned method invention.
Advantage of the present invention is:
1, the serious hydrogenator for coking, main coking position is the superiors' catalyzer of top beds, the inventive method penetrates the circulation passage of the standby stream with rupture disk of bed certain depth by setting, rupture disk is responded to the pressure difference of beds automatically, when pressure difference reaches the condition of setting, can automatically open the standby stream circulation passage, without human intervention, not increase the Operating Complexity of device.
2, the inventive method is simple, easy-to-use, without existing apparatus is carried out to large change, can be under essentially identical operational condition the long-term operation of implement device, do not need to stop work catalyzer skimmed to head, increase the running period of device, increase economic efficiency.
3, the inventive method can make the gas-liquid logistics walk around beds top in the situation that coking or obstruction occur on beds top, can utilize to greatest extent the catalyzer of beds bottom, cuts the waste.
The accompanying drawing explanation
Fig. 1 is in the inventive method, the reactor head structural representation.
Fig. 2 is in the inventive method, another kind of form structure schematic diagram.
In figure: 1-gas-liquid partition tray, 2-beds, 3-standby stream circulation passage, 4-bubble cap, 5-pressure burst rupture of membranes, the conventional gas-liquid allotter of 6-, 7-the second bed gas-liquid partition tray.
Embodiment
For further setting forth specific features of the present invention, in connection with accompanying drawing, be illustrated.
As shown in Figure 1, the process of the processing method of a kind of prolonging operation period of hydrogenation device of the present invention is:
When the Pressure Drop of beds 2 is in normal range, stock oil and hydrogen mixture material enter conventional gas-liquid allotter 6, then flow downward and enter beds, carry out hydrogenation reaction.Pressure Drop when beds 2 tops increases, while causing the gas-liquid logistics substantially can't pass through, beds is stretched in lower end, break under the effect of pressure difference through the pressure burst rupture of membranes 5 of standby stream passage flow duct 3 upper ends of gas-liquid partition tray in upper end, and the gas-liquid logistics can enter the beds bottom by standby stream passage flow duct 3 and proceed hydrogenation reaction.
As shown in Figure 2, the process of the processing method of the another kind of prolonging operation period of hydrogenation device of the present invention is:
Stock oil and hydrogen mixture material enter the gas-liquid partition tray 1 in reactor, distribute backward lower contact top beds 2, then enter the second beds, finally generate oil and hydrogen mixture material outflow reactor.The upper end of standby stream circulation passage 3 is positioned at the below of gas-liquid partition tray 1, and the lower end of standby stream circulation passage 3 penetrates the top beds.When top beds 2 occurs to stop up or Partial Blocking, the beds pressure drop increases to pressure burst rupture of membranes 5 while breaking value, pressure burst rupture of membranes 5 breaks, stock oil and hydrogen mixture material enter by the standby stream circulation passage through top beds 2, directly enter the gas-liquid partition tray 7 of the second beds, through distributing backward lower contact the second beds, carry out hydrogenation reaction.
For explanation the solution of the present invention and effect, by following examples, further illustrate the solution of the present invention and effect.While for other raw material, maybe needing to produce other index product, can corresponding adjustment catalyzer or the technology contents such as operational condition.
Embodiment 1
Adopt FHRS-1 (hydrogenation is caught silicea), FZC-102B (hydrogenation protecting agent), the FH-40C (main Hydrobon catalyst) of Fushun Petrochemical Research Institute's Development and Production.According to the structure of schematic diagram shown in Fig. 1, reactor arranges two beds, the first beds filling FHRS-1, and the standby stream circulation passage extends downward the centre of the first beds.The second beds filling FZC-102B, FH-40C.Stock oil character is in Table 1, and the processing condition after turning round 100 days and product property are in Table 2.
Comparative example 1
This comparative example adopts traditional Hydrogenation of Coker Gasoline device.Beds all loads identical with embodiment.Stock oil character is in Table 1, and the processing condition after turning round 100 days and product property are in Table 2.
Table 1 stock oil character
Table 2 operational condition and product property
| Embodiment 1 | Comparative example 1 | |
| Reaction hydrogen pressure/MPa | 3.0 | 3.0 |
| Hydrogen to oil volume ratio | 650∶1 | 650∶1 |
| Volume space velocity/h -1 | 2.0 | 2.0 |
| Average reaction temperature/℃ | 288 | 293 |
| Pressure burst rupture of membranes burstpressures is poor/MPa | 0.23 | |
| Product property | ||
| Density (20 ℃)/gcm -3 | 0.7238 | 0.7233 |
| The boiling range scope/℃ | 46～193 | 44～191 |
| Sulphur/μ gg -1 | 23.0 | 21.0 |
| Nitrogen/μ gg -1 | 4.8 | 3.6 |
| Bromine valency/gBr (100mL) -1 | 1.8 | 1.6 |
| Reactor pressure decrease/MPa (30 days) | 0.11 | 0.10 |
| Reactor pressure decrease/MPa (60 days) | 0.21 | 0.19 |
| Reactor pressure decrease/MPa (90 days) | 0.09 | 0.26 |
| Reactor pressure decrease/MPa (100 days) | 0.12 | Stop work |
According to structure of reactor shown in Fig. 2, adopt FHRS-1 (hydrogenation is caught silicea), FZC-102B (hydrogenation protecting agent), the FH-40C (main Hydrobon catalyst) of Fushun Petrochemical Research Institute's Development and Production.Two beds are set, the first beds filling FHRS-1, centre arranges the standby stream circulation passage with the pressure rupture disk, and the pressure burst rupture of membranes is that stainless material is made.The second beds loads a small amount of FHRS-1 and FZC-102B, FH-40C.Stock oil character is in Table 1, and the processing condition after turning round 2 months and product property are in Table 3.
Table 3 embodiment 2 operational conditions and product property
| |
|
| Reaction hydrogen pressure/MPa | 3.0 |
| Hydrogen to oil volume ratio | 700∶1 |
| Volume space velocity/h -1 | 2.5 |
| Average reaction temperature/℃ | 290 |
| Pressure burst rupture of membranes burstpressures is poor/MPa | 0.20 |
| Product property | |
| Density (20 ℃)/gcm -3 | 0.7236 |
| The boiling range scope/℃ | 45～192 |
| Sulphur/μ gg -1 | 22.0 |
| Nitrogen/μ gg -1 | 4.2 |
| Bromine valency/gBr (100mL) -1 | 1.3 |
| Reactor pressure decrease/MPa (15 days) | 0.10 |
| Reactor pressure decrease/MPa (30 days) | 0.12 |
| Reactor pressure decrease/MPa (50 days) | 0.20 |
| Reactor pressure decrease/MPa (80 days) | 0.09 |
Above result can find out, reaches while setting reactor catalyst bed upper pressure is poor, and technique of the present invention can realize automatically hydrogenation reaction being proceeded in gas-liquid mass transport to the bottom of reactor catalyst bed.The present invention can extension fixture running period, and take full advantage of the catalyzer of whole bed, reduce reactor pressure simultaneously and fall, guarantee production safety.
Claims (9)
1. the processing method of a prolonging operation period of hydrogenation device, at least one fixed bed hydrogenation beds is set in hydrogenator, reaction mass enters reactor from top, from the bottom outflow reactor, it is characterized in that: arrange in the beds at hydrogenator top and can make the directly structure of circulation of reaction mass when reactor pressure decrease raises; The described structure that can make reaction mass directly circulate when reactor pressure decrease raises is: reaction mass standby stream circulation passage is set in the beds at hydrogenator top, the standby stream circulation passage is the unlimited straight tube channel architecture in lower end, the upper end of standby stream circulation passage penetrates napex beds top, the upper end of standby stream circulation passage is sealed by the pressure burst rupture of membranes, the poor 0.45MPa of being less than of the burstpressures of pressure burst rupture of membranes also is greater than 0.1MPa, and reactor pressure decrease is increased to reaction mass when poor higher than the burstpressures of pressure burst rupture of membranes and directly circulates.
2. it is characterized in that in accordance with the method for claim 1: hydrogenator arranges 3～5 beds.
3. in accordance with the method for claim 1, it is characterized in that: standby stream circulation passage upper end arranges bubble cap, and bubble cap and standby stream circulation passage top have gap.
4. it is characterized in that in accordance with the method for claim 1: standby stream circulation passage lower end is the height location from top meter 20%～100% in the reactor head beds.
5. in accordance with the method for claim 1, it is characterized in that: the gas-liquid distributing disc on reactor top is passed in the upper end of standby stream circulation passage, or below the gas-liquid distributing disc of reactor top.
6. in accordance with the method for claim 1, it is characterized in that: the diameter of standby stream circulation passage is 2～20cm, circulation passage sectional area sum should be not less than reactor cross section long-pending 5%, be not more than reactor cross section long-pending 30%.
7. in accordance with the method for claim 1, be characterised in that altogether: the pressure burst rupture of membranes of standby stream circulation passage upper end is that resistant to elevated temperatures metallic substance is made, and heat resistance should surpass 300 ℃, and its pressure difference of bearing is 0.2～0.35MPa.
8. in accordance with the method for claim 1, it is characterized in that: the hydrogenation operation condition is that reaction pressure is 1.0～18.0MPa, and during liquid, volume space velocity is 0.5～5.0h
-1, temperature of reaction is controlled at 160～420 ℃, and hydrogen to oil volume ratio is 100:1～1800:1.
9. a hydrogenation reaction device, comprise hydrogenator, at least one fixed bed hydrogenation beds is set in hydrogenator, it is characterized in that: reaction mass standby stream circulation passage is set in the beds at hydrogenator top, the standby stream circulation passage is the unlimited straight tube channel architecture in lower end, the upper end of standby stream circulation passage penetrates beds top, top, the upper end of standby stream circulation passage is by the sealing of pressure burst rupture of membranes, and the poor 0.45MPa of being less than of the burstpressures of pressure burst rupture of membranes also is greater than 0.1MPa.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2111789U (en) * | 1992-01-25 | 1992-08-05 | 机械电子工业部兰州石油机械研究所 | Suction-breaking flow-type gas-liquid distributor |
| CN1765479A (en) * | 2004-10-29 | 2006-05-03 | 中国石油化工股份有限公司 | Gas liquid distributor with incrustation sediment function |
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2010
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2111789U (en) * | 1992-01-25 | 1992-08-05 | 机械电子工业部兰州石油机械研究所 | Suction-breaking flow-type gas-liquid distributor |
| CN1765479A (en) * | 2004-10-29 | 2006-05-03 | 中国石油化工股份有限公司 | Gas liquid distributor with incrustation sediment function |
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