CN101445746B - Pre-passivation method for continuous reforming device - Google Patents
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Abstract
The invention relates to a pre-passivation method for continuous reforming device, comprising the following steps: temperature of a reactor not yet loaded with catalyst or temperature of a reactor loaded with catalyst is raised to 100-650 DEG C and sulphide is injected to the air flossing in the system at the temperature; sulfur content in the air is controlled at 100 x 10<-6>L/L, so as to passivate a wall of the device; then, reaction raw material is inlet into the reactor in existence of catalyst to carry out reaction. The method can effectively restrain catalytic coking generated by the metal of high-temperature wall of the reforming reactor, thereby reducing operation risk of the device.
Description
Technical field
The present invention relates to a kind of pre-passivation method of continuous regenerative catalytic reforming unit, specifically, is the passivating method before a kind of continuous reformer begins to react.
Background technology
Petroleum naphtha continuous regenerative CR with its liquid receive high, hydrogen yield is high and characteristics such as aromatics yield height, in the production of stop bracket gasoline and aromatic hydrocarbons, receives people's very big attention.At present, the reforming catalyst that continuous reformer uses is the two or multimetallic catalyst of the series of platiniferous tin, compares with platiniferous catalyzer only, and platinum-tin catalyst is more responsive to sulfide.Therefore, guarantee the normal operation of catalytic reforming unit, strict restriction will be arranged the sulphur content in the reforming raw oil.
CN1234455C, US6495487B1 and US6780814B2 all disclose a kind of environment for use requirement of platinum tin-polymetallic reforming catalyst; Point out at CONTINUOUS REFORMER reaction normal operation period; The feed naphtha employing catalytic desulfurization that is used for reforming and the mode of adsorption desulfurize are removed to minimum level with the sulphur of oil, and no sulphur is the most desirable.
" refining of petroleum and chemical industry " rolled up the 26th～29 page of the 8th phase in 2002 the 33rd and " Industrial Catalysis " rolled up the 5th～8 page of the 9th phase in 2003 the 11st; When having introduced the CONTINUOUS REFORMER normal operation respectively; Use the controlling index requirement of platinum tin series reforming catalyst to reformation raw material impurity content, wherein sulphur content generally is controlled at and is not more than 0.5 μ g/g.
The CONTINUOUS REFORMER working pressure is relatively low, temperature of reaction is higher, hydrogen/oil ratio is lower, and device more is prone to coking in the reaction process.Along with development of technology, CONTINUOUS REFORMER constantly develops to the direction that severities such as ultralow pressure, low hydrogen/oil ratio, low-speed improve constantly, and the tendency of reactor drum and furnace tubing coking is also in continuous increase.So far the wall coking that reacts of the continuous reformer of much more existing cover.The coking meeting causes mobile smooth, the reactor drum inner member damage of catalyzer, even causes device to be stopped work, thereby brings enormous economic loss to the refinery.
" catalytic reforming process and engineering " (in November, 2006 first version; Sinopec press) the 522nd～534 page; Mechanism to the continuous reformer coking is analyzed: hydrocarbon molecules is attracted to the surface of reactor wall metal grain in reducing atmosphere; Excessive dehydrogenation generates carbon atom under the effect of wall metal catalytic, and dissolves in or infiltrate between the intercrystalline or particle of metal.Because the deposition of charcoal makes metal grain separate with matrix with growth, the result produces the thread charcoal that front end has metal iron particles.This charcoal is obviously different with the carbon deposit on the catalyzer, and it is active to have higher catalytic dehydrogenation and hydrogenolysis, once generation, and just reaction constantly at high temperature, formation speed continues to accelerate, and thread charcoal is constantly elongated, chap, hardening.Soft charcoal, soft blowing-in burden(ing), the hard several developmental stage of charcoal are generally experienced in the development of thread charcoal, and its formation time is long more, and the consequence of bringing is serious more.The device green coke is early stage, may cause the recycle system to stop up, can not normal circulation; Can damage the inner member of reactor drums such as sector drum, pipe core when serious.The coke that generates also can cause the local overheating of revivifier scorch region and the overtemperature in oxychlorination district if get into regeneration system rapidly, burns out the inner member of revivifier.The damage intensity of reactor drum and revivifier inner member can become more serious with the prolongation of runtime.
In order to prevent continuous reformer metal wall catalytic coking; " CR " (in April, 2004 first version; Sinopec press) the 200th～202 page to introduce current at present way be that the sulphur content of control catalytic reforming feedstock is between 0.2～0.3 μ g/g; With passivation reaction device inwall and furnace tubing inwall, suppress the catalytic activity of metal.But, from the process that goes into operation of all kinds continuous reformer, opportunity and the condition of annotating sulphur do not had a unified demand, specifically how to operate the experience that often depends on the field technician.Method commonly used at present promptly begins in raw oil, to inject sulfide when being oil-feed, and it is when each reactor inlet temperature reaches more than 480～490 ℃, to begin to inject sulfide that part is also arranged, and the sulphur content of control catalytic reforming feedstock is between 0.2～0.5 μ g/g.
At present, CONTINUOUS REFORMER operation is based on the needs of refinery's material balance, hydrogen balance and product, often after oil-feed, improves the severity of reaction when treating in the gas hydration lattice quickly.The sulphur content of catalytic reforming feedstock is controlled between 0.2～0.5 μ g/g; Particularly for the new device that uses first; Be not enough to rapidly, passivation reaction device and furnace tubing wall fully; After quite a few continuous reformer adopted above-mentioned passivating method, the situation of reactive system coking still appearred in operation process.Therefore, the metal catalytic coking that how to suppress continuous reforming reactor and furnace tubing wall effectively becomes the important topic that the CONTINUOUS REFORMER technician pays close attention to.
Other field of petrochemical complex prevents that hydro carbons from having multiple in the method for reactor high temperature position coking; Wherein CN1160435C discloses the method that suppresses sedimentation of coke in a kind of pyrolysis oven; This method is before feeding hydrocarbon feed in pyrocrack furnace; With sulfur-bearing and phosphorated compound treatment pyrolysis oven, the atomic ratio of said sulphur/phosphorus is at least 5, and the sulfocompound that in P contained compound, adds q.s can make on the surface of pyrolysis oven and form even, the effective passivation layer of one deck to suppress the deposition of coke.
CN85106828A discloses the method and apparatus that a kind of metal parts surface forms sulfurized layer; Metal parts is placed on the cathode disc of vacuum oven internal reaction chamber; In vacuum oven, place simultaneously solid sulfur; Solid sulfur gasifies through heating, and gasification sulphur bombards under effect of electric field and is positioned at metal parts on the cathode disc, thereby forms sulfuric horizon on its surface.
CN1126607C discloses a kind of suppress and slow down coke formation and sedimentary method in the hydrocarbons pyrolysis; This method is injected cracking apparatus with water vapor with pretreating agent pre-treatment is carried out in the metallic surface before cracking stock feeds, pretreating agent is one or more a mixture of hydrogen sulfide, organosulfur compound, organophosphorus and organosulfur phosphorus compound.This method can make the pyrolyzer metal surface passivation form and deposition with the coke that suppresses and reduce in cracking process and the subsequent processes.
Because it is very responsive to impurity that platinum tin is continuous reforming catalyst, high to environmental requirement, the related various materials of aforesaid method all can cause serious poisoning of reforming catalyst or irreversible poisoning, so be not suitable for catforming process.
Summary of the invention
Pre-passivation method before the purpose of this invention is to provide a kind of continuous reformer and beginning to react, this method can effectively prevent the coking of high temperature wall after the oil-feed, reduce the operation risk of device, the duration of service of extension fixture.
The pre-passivation method of continuous reformer reactive system provided by the invention; Comprise that the temperature of reactor that will be unkitted catalyzer or adorn catalyzer rises to 100～650 ℃; And under this temperature, in system, injecting sulfide in the flowing gas, sulphur content is 0.5～100 * 10 in the control gas
-6L/L is with passivation device wall.
The inventive method is before continuous reformer feeds reaction raw materials; Under certain temperature and gaseous media mobile condition; In reactive system, inject sulfide; Through sulphur content certain in the pilot-gas wall of continuous reformer reactive system elevated temperature vessel and pipeline is carried out passivation, effectively the catalytic coking of restraining device start of run metal wall.
Description of drawings
Fig. 1 and Fig. 2 are the electromicroscopic photograph of the charcoal piece gathered in the Comparative Examples.
Fig. 3 is the photo of reactor bottom coking in the Comparative Examples.
Embodiment
The inventive method is before continuous reformer begins the oil-feed reaction; In system, add sulfide in the flowing gaseous medium; Wall to high temperature positions such as continuous regenerative reforming device reaction device and furnace tubings carries out passivation fully; And then, make the interior sulphur content of device not influence the reactivity worth of catalyzer with the gas purging reaction unit that does not influence reaction, feed reaction raw materials afterwards and under normal working condition, reacting.The sulfide of the inventive method access equipment before reforming reaction can suppress the catalytic activity of high temperature position wall metal, prevents the catalytic coking that the metal wall causes in the reaction process, increases the safe operating life of reaction unit.
The inventive method adds sulfide in the flowing gas and carries out the passivation of wall in continuous apparatus oil-feed reaction forward direction system, described flowing gas refers generally to intrasystem circulation gas.The mixture of the preferred hydrogen of flowing gas, rare gas element or hydrogen and rare gas element.Described rare gas element nitrogen.
The pre-passivation method of continuous reformer reactive system of the present invention, but loading catalyst in the reactor drum, loading catalyst does not comparatively preferably carry out preparatory passivation to reaction unit under the situation of loading catalyst in reactor drum yet.
When loading catalyst does not carry out preparatory passivation in the described reforming reactor; Passivation temperature is 100～500 ℃; Earlier in system, set up gas circulation, reactor drum is heated up, when reactor inlet temperature rises to 120～260 ℃, begin to inject sulfide and continue and heat up;, reactor inlet temperature kept constant temperature 1～50 hour when rising to 300～500 ℃, preferred 4～10 hours.The sulphur content of the interior gas of reaction unit preferably is controlled at 10～50 * 10 in the passivating process in advance
-6L/L, more preferably 20～40 * 10
-6L/L.After the passivation, sulphur content is not more than 2 * 10 in the gas to discharging with the inert gas purge reaction unit in advance
-6L/L again by ordinary method loading catalyst in reactor drum, feeds reaction raw materials and carries out reforming reaction.
When loading catalyst has carried out preparatory passivation in the described reforming reactor; Passivation temperature is 100～450 ℃ in advance; Earlier in system, set up gas circulation, reactor drum is heated up, when reactor inlet temperature rises to 120～260 ℃, begin to inject sulfide and continue and heat up;, reactor inlet temperature kept constant temperature 1～50 hour when rising to 370～420 ℃, preferred 2～10 hours.The sulphur content of the interior gas of reaction unit is controlled at 1～20 * 10 in the passivating process in advance
-6L/L, preferred 2～10 * 10
-6L/L, more preferably 3～6 * 10
-6L/L.After the passivation, sulphur content is not more than 2.0 * 10 in the gas to discharging to feed the hydrogen exchange reaction unit in advance
-6L/L feeds reaction raw materials and carries out reforming reaction by the popular response condition.
The popular response condition of the continuous reformer described in the aforesaid method is: pressure 0.1～5.0MPa, preferred 0.35～2.0MPa, 350～600 ℃ of temperature, preferred 430～560 ℃, hydrogen/hydrocarbon mol ratio 1～20, preferred 2～10, liquid hourly space velocity (LHSV) 1～10h
-1, preferred 1～5h
-1
The preferred hydrogen sulfide of the said sulfide that in flowing gas, injects, dithiocarbonic anhydride, NSC 9370, aliphatics sulfocompound; Alicyclic sulfocompound; Any two or more mixture in aromatic series sulfocompound, thiophene, morpholine kind compound or the said compound, wherein said thiophene, morpholine kind compound are meant the verivate of thiophene or morpholine.When passivation is medium with nitrogen, the preferred hydrogen sulfide of sulfide; When passivation was medium with hydrogen, sulfide can be hydrogen sulfide, also can be organic sulfide.
The used catalyzer of the said continuous reformer of the inventive method comprises with carrier and serves as tin and 0.1～10 quality % of precious metal, 0.01～5.0 quality % of 0.01～2.0 quality % that calculates benchmark, preferred 0.05～1.0 quality %, preferred 0.05～1.0 quality %, the halogen of preferred 0.1～5.0 quality % with the butt carrier.Described platinum metals is platinum, rhodium, palladium, iridium, ruthenium or osmium, preferred platinum, the preferred chlorine of halogen, the preferred aluminum oxide of carrier.
Also can further contain the 3rd, the 4th metal constituent element that can improve the catalyst reaction performance that is selected from europium, cerium, yttrium or titanium in the said reforming catalyst, its content is 0.01～5.0 quality %, preferred 0.05～3.0 quality %.
The described continuous reformer of the inventive method is the reformation reaction raw materials with the petroleum naphtha, and said continuous reformer is all kinds of moving-bed continuous regenerative catalytic reforming units.Petroleum naphtha can be that virgin naphtha, hydrogen cracking heavy naphtha, hydrogenation coker gasoline, cracking of ethylene gasoline are raffinated oil, catalytically cracked gasoline, also can be the mixture of above-mentioned several kinds of raw materials.According to the difference of reformation title product, the boiling range scope of raw oil control is different, and general over point is 60～90 ℃, and final boiling point is 135～180 ℃.The impurity of reforming raw oil requires: sulphur＜0.5 μ g/g, nitrogen＜0.5 μ g/g, arsenic＜1ng/g, lead＜10ng/g, copper＜10ng/g, water＜5 μ g/g.
The present invention be applicable to various types of use with aluminum oxide or the aluminum oxide that contains zeolite as carrier, contain the continuous regenerative reforming device of the platinum tin catalyst series of halogen, be specially adapted to the use first of newly-built continuous reformer.
Further specify the present invention through instance below, but the present invention is not limited to this.
Instance 1
In a cover reactor drum, do not load on the continuous reformer of reforming catalyst, adopt the inventive method that reactive system is carried out preparatory passivation.
It is that nitrogen replacement to the oxygen level of discharging gas of 99.8 moles of % is less than 0.5 mole of % that the CONTINUOUS REFORMER reactive system is used purity.The pressure that uses nitrogen to be pressurized to the reformation HP separator is 350KPa, starts the reformation compressor cycle, and making the circulation gas flow is 4 * 10
4Nm
3/ h heats up each reactor drum with 20～40 ℃ speed per hour.When each reactor inlet temperature rises to 170 ℃, begin in circulating nitrogen gas, to inject hydrogen sulfide and continue intensification, it is 20～30 * 10 that the hydrogen sulfide of injection makes the sulphur content of circulation gas
-6L/L.Constant temperature circulation cooling after 3 hours when reactor inlet temperature reaches 450 ℃, and stop to inject hydrogen sulfide.With nitrogen replacement system to the sulphur content of discharging gas less than 2 * 10
-6L/L, then by the method for routine to the reactor charge catalyzer, in reactor drum, feed hydrogen again; And the beginning gas circulation, reactor drum is warming up to 370 ℃ gradually, feed reforming raw oil and begin reaction; The reforming raw oil composition is seen table 1, and reaction conditions and result see table 2.Said catalyzer contains the platinum of 0.28 quality %, the tin of 0.30 quality %, and all the other are gama-alumina.Do not see the charcoal piece when catalyzer is sampled in the running, high temperature positions such as shut-down inspection reactor drum are not seen coking.
Instance 2
Fill reforming catalyst at continuous reformer, said catalyzer contains the platinum of 0.29 quality %, the tin of 0.31 quality %, and all the other are gama-alumina.
Use earlier purity be nitrogen replacement continuous reformer to the oxygen level of discharging gas of 99.8 moles of % less than 0.5 mole of %, using purity then is that hydrogen exchange system to the hydrogen richness of discharging gas of 96 moles of % is greater than 90 moles of %.The pressure that uses hydrogen to be pressurized to the reformation HP separator is 350KPa, starts the reformation compressor cycle, and making circulating flow rate is 5 * 10
4Nm
3/ h.Each reactor drum is warming up to after reactor inlet temperature is 200 ℃ with 20～40 ℃ speed per hour, begins in circulation gas, to inject NSC 9370 and continue to heat up, inject NSC 9370, making the sulphur content in the circulation gas is 3～5 * 10
-6L/L.Constant temperature is 3 hours when reactor inlet temperature rises to 370 ℃, stops to annotate sulphur then, and using purity is the hydrogen exchange system of 96 moles of %, and sulphur content in the circulation gas is reduced to 2 * 10
-6Below the L/L, feed the reforming reaction raw material afterwards and carry out reforming reaction, the reforming raw oil composition is seen table 1, and reaction conditions and result see table 2.Do not see the charcoal piece when catalyzer is sampled in the running, high temperature positions such as shut-down inspection reactor drum are not seen coking.
Comparative Examples
In continuous reformer, fill reforming catalyst, the composition of said catalyzer is with instance 1.
Use earlier purity be nitrogen replacement continuous reformer to the oxygen level of discharging gas of 99.8 moles of % less than 0.5 mole of %, using purity then is that hydrogen exchange system to the hydrogen richness of discharging gas of 93 moles of % is greater than 60 moles of %.The pressure that uses hydrogen to be pressurized to the reformation HP separator is 350KPa, starts the reformation compressor cycle, and making the circulation gas flow is 4 * 10
4Nm
3/ h is warming up to 370 ℃ with each reactor drum with 20～40 ℃ speed per hour.In reforming reactor, feed reforming raw oil, its composition is seen table 1.Promptly begin behind the catalytic reforming feedstock in raw material, to inject NSC 9370, making the sulphur content in the raw material is 0.2～0.3 μ g/g, reacts by the resurfacing operation condition that runs well then, and main operational condition and reaction result are seen table 2.Reformer operation when separating hopper and gather catalyst sample, was found the charcoal piece of 1～5mm size through regular meeting after 3 months, and the electromicroscopic photograph of charcoal piece sample is seen Fig. 1 and Fig. 2 respectively, and photo shows that the charcoal piece is the thread charcoal that the top has iron particle., device finds that the reactor bottom coking is obvious, sees Fig. 3 when stopping work the back inspection.
Table 1
| Group composition | Instance 1 | Instance 2 | Comparative Examples |
| Alkane, quality % | 53.18 | 52.18 | 52.66 |
| Naphthenic hydrocarbon, quality % | 40.18 | 42.06 | 40.52 |
| Aromatic hydrocarbons, quality % | 6.64 | 5.76 | 6.82 |
| Virtue is dived, quality % | 44.18 | 43.80 | 44.67 |
| The ASTMD86 boiling range, ℃ | 80～172 | 84～176 | 81～172 |
| Total sulfur content, μ g/g | ＜0.5 | ＜0.5 | ＜0.5 |
Table 2
| Project | Comparative Examples | Instance 1 | Instance 2 |
| Hydrogen/hydrocarbon mol ratio | 2.0 | 2.0 | 1.96 |
| Liquid hourly space velocity, h -1 | 1.44 | 1.44 | 1.41 |
| Catalyst circulation rate, % | 100 | 100 | 100 |
| One anti-temperature in/temperature drop, ℃ | 526/147 | 525/145 | 528/143 |
| Two anti-temperature in/temperature drops, ℃ | 526/88 | 525/90 | 528/89 |
| Three anti-temperature in/temperature drops, ℃ | 526/66 | 525/62 | 528/64 |
| Four anti-temperature in/temperature drops, ℃ | 526/50 | 525/52 | 528/52 |
| Total temperature drop, ℃ | 351 | 349 | 348 |
| Pure hydrogen productive rate, quality % | 3.65 | 3.63 | 3.77 |
| Stable gasoline octane value (RONC) | 102.5 | 102.3 | 102.7 |
Claims (10)
1. the pre-passivation method of a continuous reformer reactive system; Comprise that the temperature of reactor that will be unkitted catalyzer or adorn catalyzer rises to 100～650 ℃; And under this temperature, in system, inject sulfide in the flowing gas; Not during loading catalyst, sulphur content is 20～40 * 10 in the control gas in the reforming reactor
-6L/L, during loading catalyst, sulphur content is 1～20 * 10 in the control gas in the reforming reactor
-6L/L is with passivation device wall; Described catalyzer comprises carrier and serves as platinum metals, the tin of 0.05～1.0 quality % and the halogen of 0.1～5.0 quality % that calculates 0.05～1.0 quality % of benchmark with the butt carrier.
2. according to the described method of claim 1, it is characterized in that described flowing gas is the mixture of hydrogen, rare gas element or rare gas element and hydrogen.
3. according to the described method of claim 2, it is characterized in that described rare gas element is a nitrogen.
4. according to the described method of claim 1, the passivation temperature when it is characterized in that in the described reforming reactor loading catalyst not is 100～500 ℃.
5. according to the described method of claim 1, the passivation temperature when it is characterized in that in the described reforming reactor loading catalyst is 100～450 ℃.
6. according to the described method of claim 1; It is characterized in that described sulfide is hydrogen sulfide, dithiocarbonic anhydride, NSC 9370, aliphatics sulfocompound; Alicyclic sulfocompound, any two or more mixture in aromatic series sulfocompound, thiophene or the said compound.
7. according to the described method of claim 2, when it is characterized in that described gas is rare gas element, the sulfide of injection is hydrogen sulfide.
8. according to claim 1 or 4 described methods, when it is characterized in that in the described reforming reactor not loading catalyst, after the passivation, sulphur content is not more than 2 * 10 in the gas to discharging with the inert gas purge reaction unit in advance
-6The catalyzer that recharges after the L/L feeds reaction raw materials and carries out reforming reaction.
9. according to the described method of claim 1, when it is characterized in that described reactor charge catalyzer, after the passivation, feed the gas in the hydrogen exchange device earlier in advance, hydrogen sulfide content is not more than 5 * 10 in the gas to be recycled
-6During L/L, feed reaction raw materials and carry out reforming reaction.
10. according to the described method of claim 1, it is characterized in that the platinum metals in the described reforming catalyst is a platinum, halogen is a chlorine, and carrier is an aluminum oxide.
Priority Applications (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710178229 CN101445746B (en) | 2007-11-28 | 2007-11-28 | Pre-passivation method for continuous reforming device |
| EP15156294.9A EP2910624B1 (en) | 2007-10-31 | 2008-10-30 | Passivation process for a continuous reforming apparatus during the initial reaction |
| RU2010119051/04A RU2470065C2 (en) | 2007-10-31 | 2008-10-30 | Method of passivation for continuous reforming plant (versions) |
| US12/740,458 US8475650B2 (en) | 2007-10-31 | 2008-10-30 | Pre-passivation process for a continuous reforming apparatus, and passivation process for a continuous reforming apparatus during the initial reaction |
| EP08854893.8A EP2210929B1 (en) | 2007-10-31 | 2008-10-30 | A pre-passivation process for a continuous reforming apparatus |
| PCT/CN2008/001819 WO2009067858A1 (en) | 2007-10-31 | 2008-10-30 | A predeactivation method and a deactivation method during initial reaction for a continuous reforming apparatus |
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| CN 200710178229 CN101445746B (en) | 2007-11-28 | 2007-11-28 | Pre-passivation method for continuous reforming device |
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| CN107434981A (en) * | 2016-05-26 | 2017-12-05 | 中石化广州工程有限公司 | A kind of method of continuous reformer note sulphur |
| CN107915564A (en) * | 2016-10-10 | 2018-04-17 | 中国石油化工股份有限公司 | The method of four~carbon of carbon, eight olefins by catalytic cracking |
| CN112675921A (en) * | 2019-10-18 | 2021-04-20 | 中国石油化工股份有限公司 | Closed circulation passivation method and passivation system for octenal gas-phase hydrogenation catalyst |
| CN114436750B (en) * | 2020-10-20 | 2024-07-23 | 中国石油化工股份有限公司 | Pretreatment method of reaction system for directly preparing olefin from synthesis gas |
| CN113652258B (en) * | 2021-07-28 | 2023-04-07 | 宁波中金石化有限公司 | Aromatic hydrocarbon production system and method for preventing metal catalytic coking |
| CN116020356B (en) * | 2021-10-25 | 2024-10-11 | 中国石油化工股份有限公司 | Method and system for dehydrogenating low-carbon alkane by countercurrent moving bed |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2863825A (en) * | 1954-09-24 | 1958-12-09 | Shell Dev | Catalytic reforming of hydrocarbon oils |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2863825A (en) * | 1954-09-24 | 1958-12-09 | Shell Dev | Catalytic reforming of hydrocarbon oils |
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