CN102443411B - Process method for prolonging operation period of hydrogenation device - Google Patents
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- CN102443411B CN102443411B CN2010105090684A CN201010509068A CN102443411B CN 102443411 B CN102443411 B CN 102443411B CN 2010105090684 A CN2010105090684 A CN 2010105090684A CN 201010509068 A CN201010509068 A CN 201010509068A CN 102443411 B CN102443411 B CN 102443411B
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Abstract
The invention provides a process method for prolonging the operation period of a hydrogenation device. A gas and liquid distribution disc is arranged on the top of a catalyst bed layer of a hydrogenation reactor, conventional gas and liquid distributors and standby bubble cap type gas and liquid distributors are arranged on the gas and liquid distribution disc, the standby bubble cap type gas and liquid distributors and the conventional gas and liquid distributors are distributed at intervals, the standby bubble cap type gas and liquid distributors are provided with long center pipes, the long center pipes downward extend into the top catalyst bed layer of the hydrogenation reactor, bubble caps are arranged at the upper parts of the long center pipes, in addition, gaps for flowing materials are formed between the bubble caps and the long center pipes, and the tops of the long center pipes are sealed by pressure blasting films. The method has the advantages that great change on the existing device is not needed, the long-period operation of the device can be realized under the condition of low 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 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 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 a kind of prolonging operation period of hydrogenation device of the present invention comprises following content: at hydrogenator beds top, gas-liquid partition tray is set, conventional gas-liquid allotter and standby bubble cap formula gas-liquid allotter are set on gas-liquid partition tray, and standby bubble cap formula gas-liquid allotter and conventional gas-liquid allotter are spaced apart.Standby bubble cap formula gas-liquid allotter has long pipe core, long pipe core extends downward in the beds of hydrogenator top, bubble cap is arranged on long pipe core top and has the gap for Flow of Goods and Materials with long pipe core, the top of long pipe core 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.
In the inventive method, at the reactor catalyst bed pressure drop hour, standby bubble cap formula gas-liquid allotter is not enabled, and unit normal run is 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, or substantially can't be when the gas-liquid logistics, the pressure burst rupture of membranes at long pipe core top breaks under the effect of pressure difference, the gas-liquid logistics can enter the beds bottom by long pipe core and proceed hydrogenation reaction.
In the inventive method, the pressure burst rupture of membranes at the long pipe core of standby bubble cap formula gas-liquid allotter top is the existing common equipment in pressure vessel safety field, be generally the pressure burst rupture of membranes, the pressure burst rupture of membranes is general selects resistant to elevated temperatures alloy material to make, the general heat resistance of wanting should surpass 300 ℃, as the 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.The diameter of the long pipe core of novel standby gas-liquid allotter is generally 2～20cm, and quantity evenly arranges according to the scale of hydrogenator, in general the sectional area sum should be not less than reactor cross section long-pending 5%, be not more than reactor cross section long-pending 30%.The length of the long pipe core of standby bubble cap formula gas-liquid allotter is 10%～90% of hydrogenator top catalyst bed layer height, is preferably 20%～50%.
In the inventive method, the hydrogenation catalyst bed can specifically be determined according to the character processed raw material and product requirement.Hydrogenator can arrange 2～5 beds.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 concrete kind of catalyzer and consumption can be according to feedstock properties, and required reaction effect is specifically determined.
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 oxide 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
-1Temperature 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.
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 gas-liquid allotter 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 upflow tube 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.
In figure: 1-gas-liquid partition tray, 2-beds, the long pipe core of 3-, 4-bubble cap, 5-pressure burst rupture of membranes, the conventional gas-liquid allotter of 6-, the standby bubble cap formula of 7-gas-liquid allotter.
Embodiment
The present invention arranges standby bubble cap formula gas-liquid allotter on gas-liquid partition tray, standby bubble cap formula gas-liquid allotter has the long pipe core extended in beds, 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 at long pipe core top breaks under the effect of pressure difference, and the gas-liquid logistics can enter the beds bottom by long pipe core and proceed hydrogenation reaction.
For further setting forth specific features of the present invention, in connection with accompanying drawing, be illustrated.
By reference to the accompanying drawings 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, the pressure burst rupture of membranes 5 at long pipe core 3 tops of standby bubble cap formula gas-liquid allotter 7 breaks under the effect of pressure difference, and the gas-liquid logistics can enter the beds bottom by long pipe core 3 and proceed 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 long pipe core on gas-liquid partition tray extends downward the centre of bed.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 |
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, it is characterized in that comprising following content: at hydrogenator beds top, gas-liquid partition tray is set, conventional gas-liquid allotter and standby bubble cap formula gas-liquid allotter are set on gas-liquid partition tray, and standby bubble cap formula gas-liquid allotter and conventional gas-liquid allotter are spaced apart; Standby bubble cap formula gas-liquid allotter has long pipe core, long pipe core extends downward in the beds of hydrogenator top, bubble cap is arranged on long pipe core top and has the gap for Flow of Goods and Materials with long pipe core, the top of long pipe core 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; The hydrogenation operation condition is: reaction mass enters from reactor top, from reactor bottom, discharges, and 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.
2. in accordance with the method for claim 1, it is characterized in that: the pressure burst rupture of membranes at the long pipe core of standby bubble cap formula gas-liquid allotter top is for selecting resistant to elevated temperatures alloy material to make, and heat resistance is over 300 ℃.
3. according to the described method of claim 1 or 2, it is characterized in that: the pressure burst rupture of membranes is the stainless steel pressure rupture disk.
4. according to the described method of claim 1 or 2, it is characterized in that: the pressure difference that the pressure burst rupture of membranes bears is 0.2～0.35MPa.
5. in accordance with the method for claim 1, it is characterized in that: the diameter of the long pipe core of standby bubble cap formula gas-liquid allotter is 2～20cm, evenly arrange, the sectional area sum be not less than reactor cross section long-pending 5%, be not more than reactor cross section long-pending 30%.
6. according to the described method of claim 1 or 5, it is characterized in that: the length of the long pipe core of standby bubble cap formula gas-liquid allotter is 10%～90% of hydrogenator top catalyst bed layer height.
7. according to the described method of claim 1 or 5, it is characterized in that: the length of the long pipe core of standby bubble cap formula gas-liquid allotter is 20%～50% of hydrogenator top catalyst bed layer height.
8. it is characterized in that in accordance with the method for claim 1: 2～5 beds are set in hydrogenator.
9. in accordance with the method for claim 1, it is characterized in that: hydrogenation method is for the fixed bed hydrogenation technological process of coking distillate, or for the fixed bed hydrogenation technological process of coal tar or residual oil.
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