CN1317369C - Reforming method for coking gasoline - Google Patents
Reforming method for coking gasoline Download PDFInfo
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- CN1317369C CN1317369C CNB2004100483484A CN200410048348A CN1317369C CN 1317369 C CN1317369 C CN 1317369C CN B2004100483484 A CNB2004100483484 A CN B2004100483484A CN 200410048348 A CN200410048348 A CN 200410048348A CN 1317369 C CN1317369 C CN 1317369C
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Abstract
The present invention relates to a reforming method for coker gasoline, which comprises the following processes that coking distillate oil is hydrogenated and refined, and distillate with the cutting distillation range of 70 to 175 DEG C is reformed and prerefined for eliminating impurities and then dewatered into the raw material with the water content of not more than 5 ppm; the dewatered raw material and a reforming catalyst are in contact reaction under the existence of hydrogen gas at the temperature of 470 to 540 DEG C under the pressure of 0.2 to 2.0MPa; the unreacted hydrogen gas is circulated simultaneously, and the water content in the cyclical hydrogen gas is controlled to be 5 to 20 ppm. The reforming method effectively raises the octane number of the coker gasoline and prolongs the service life of the reforming catalyst.
Description
Technical field
The present invention is a kind of catalystic reforming method of coker gasoline, specifically, be a kind of be raw material with the coker gasoline, utilize platiniferous two/multimetal reforming catalyst improves the method for its octane value under the catalytic reforming condition.
Background technology
Coking is to be the important hot procedure of raw material with residual oil or heavy crude oil with poor quality in the refining of petroleum, and coker gasoline is the inferior patrol cut that coking produces.Impurity such as coker gasoline sulphur, nitrogen, and olefin(e) centent height, stability extreme difference, octane value are very low.Though can reduce its impurity and olefin(e) centent significantly by hydrorefined method, improve stability, octane value also declines to a great extent simultaneously, and the gasoline component that still can't act as a fuel uses.In recent years, under the situation strict day by day in environmental requirement, that gasoline product quality is constantly upgraded, how to reduce coker gasoline impurity and olefin(e) centent as far as possible and increase substantially its octane value, making coker gasoline become qualified substantially and even fine fuel gasoline component, is significant realistic problem.
USP5643441, USP5510016, USP5411658 carry out hydrogenating desulfurization to coker gasoline earlier to be handled, and carries out upgrading to improve the octane value of gasoline with the zeolite catalyst that contains molybdenum again, and the zeolite in the catalyzer is ZSM-5 or β zeolite, and matrix is aluminum oxide.
Catalytic reforming also is to improve an approach of coker gasoline quality.Usually earlier coker gasoline is carried out hydrofining, removes impurity, mix by a certain percentage again in the reformer feed, with platiniferous two/the multimetal reforming catalyst boosting of octane rating.Utilize special wide aperture platinum-rhenium catalyst to handle the reformer feed that mixes coker gasoline as USP5972207.Wang Xiaolu has reported and mixed the response situation that coker gasoline carries out catalytic reforming in straight-run spirit in " refining of petroleum and chemical industry " (2000 the 2nd phase P13～16 page).
Coker gasoline is behind the catalytic reforming upgrading, the olefin(e) centent of its product is generally less than 1.0 quality %, sulphur content is less than 1.0ppm, octane value has more significantly and improves simultaneously, but, have the reforming catalyst deactivation rate is accelerated and because of the low difficult characteristics that transform of arene underwater content because other reforming raw oils such as coker gasoline and virgin naphtha compare.Coker gasoline mixed ratio in reformer feed all is no more than 35% in the aforesaid method, and in the actual application coker gasoline in reformer feed mixed ratio generally 10～25%.
Summary of the invention
The catalystic reforming method that the purpose of this invention is to provide a kind of coker gasoline, the raw material that this method is used is as coker gasoline or mix the coker gasoline of a small amount of straight-run spirit, and the gasoline blend component of production has higher octane value.
The reforming method of coker gasoline provided by the invention comprises the steps:
(1) coking distillate is carried out hydrofining, the cutting boiling range is that 70～175 ℃ the cut pre-refining of reforming removes impurity, and dewaters to raw water content and be no more than 5ppm,
(2) the back raw material that will dewater with the reforming catalyst contact reacts, simultaneously unreacted hydrogen is circulated, and water-content is 5～20ppm in the Control Circulation hydrogen in the presence of 470～540 ℃, 0.2～2.0MPa, hydrogen.
The present invention gets the coker gasoline cut after the hydrofining of suitable boiling range, and by the water-content in the strictness control reactive system to coker gasoline or the coker gasoline of admixing a small amount of straight-run spirit carries out catalytic reforming, the octane value of coker gasoline is significantly improved, have higher liquid yield and hydrogen yield simultaneously concurrently, the catalyst runs cycle obviously increases, and catalyzer prolongs work-ing life.
Embodiment
The inventive method is refining with the hydrogenation mixture of the distillate of coking distillate or its blending virgin oil or the generation of other secondary processing process, carries out strict cut cutting again, obtains the reforming raw oil with suitable boiling range scope; And, further remove impurity such as sulphur, nitrogen to this stock oil pre-refining of reforming, to meet the specification of quality of reforming raw oil, make the reforming catalyst performance unaffected.Then reforming system is introduced in the strict dehydration of the coker gasoline behind pre-refining back, simultaneously the water in the reformation circulating hydrogen is carried out strictness control, under the reaction conditions of catalytic reforming, coker gasoline is reformed, produce the stop bracket gasoline blend component.
In the inventive method, the hydrofining of coking distillate adopts conventional method to carry out, and described coking distillate is that the boiling range of coking generation is 70～350 ℃ a cut, also can be 100～350 ℃ cut.With the coking distillate after hydrofining distillation, the component of the getting regulation boiling range of the present invention pre-refining of reforming is handled, and carries out catalytic reforming again.It is 280～340 ℃ that coking distillate is carried out hydrorefined reaction conditions, and the hydrogen dividing potential drop is 1.5～6.5MPa.Used Hydrobon catalyst can be selected conventional catalyst for hydrorefining distillate oil for use, its carrier is an aluminum oxide, active ingredient is selected from VIII family metal and group vib metal, preferred cobalt of VIII family metal or nickel, preferred molybdenum of group vib metal or tungsten contain the MoO of 0.5～30.0 quality % in the preferred Hydrobon catalyst
3With the CoO of 0.01～2.0 quality % or contain 1.0～30.0 quality %WO
3NiO with 0.5～5.0 quality %.
Coking distillate after the hydrofining still contains more impurity in 70～175 ℃ of cuts that its distillation cutting is obtained, and wherein the about 10～50ppm of sulfur-bearing needs carry out pre-refining to it before reformation, further removes impurity.(1) coker gasoline that cutting obtains after the described hydrofining of step also can mix other reformer feed of this boiling range of 0～30 quality %, as carrying out pre-refining behind the straight-run spirit again.
The used catalyzer of reformation pre-refining comprised the group vib metal of 0.5～30.0 quality %, the VIII family metal of 0.01～5.0 quality % and the alumina catalyst support of 65～99 quality % during the inventive method (1) went on foot.Described VIII preferred nickel of family's metal or cobalt, preferred molybdenum of group vib metal or tungsten.
Described reformation pre-refining catalyzer preferably contains the cobalt oxide of 0.01～2.0 quality %, the tungstic oxide of 1.0～30.0 quality %, the nickel oxide of 0.5～5.0 quality % and the alumina catalyst support of 63～97 quality %.
Described (1) step reformation pre-refining temperature of reaction is that 280～340 ℃, hydrogen dividing potential drop are 1.5～4.0MPa, volume space velocity 2.0～10.0 hours
-1, hydrogen/hydrocarbon volume ratio is 80～150: 1.The sulphur of raw material, nitrogen content be all less than 0.5ppm behind the reformation pre-refining, arsenic content less than 1ppb, lead and copper content all less than 10ppb.
Stock oil behind the pre-refining should be through strict dehydration before entering the reforming reaction system.Dehydration can be adopted the method for absorption such as separation column fractionation or sorbent material such as molecular sieve, aluminum oxide, silica gel.(1) raw water content in step dehydration back preferably is no more than 3ppm, and dehydrated raw material enters behind the catalytic reforming reactor also the water-content in should strict Controlling System, i.e. water-content in control (2) the step recycle hydrogen, the preferred 8～18ppm of the water-content in the recycle hydrogen.
The device that carries out the catalytic reforming employing can be the semi regenerative reformer of fixed bed, the continuous regenerative reforming device or the leading portion of moving-bed is that fixed-bed reactor, back segment are the combination cot reformer of moving-burden bed reactor, and fixed bed cyclic regeneration or last anti-switching regeneratively reforming device.
(2) preferred 490～530 ℃ of the temperature of step reforming reaction, the preferred 1.0～1.5MPa of reaction pressure half generative reforming, the cyclic regeneration preferred 0.35～0.95MPa that reforms.Hydrogen/hydrocarbon volume ratio is that 300～2000: 1, half generative reforming preferably selects 900～1300: 1, and cyclic regeneration reforms preferred 300～800: 1.Feed volume air speed 0.8～3.0 hour
-1, preferred 1.0～2.0 hours
-1Used reforming catalyst contains platinum, 0.05～4.0 quality % tin or the rhenium of 0.05～2.0 quality %, the chlorine of 0.1～10.0 quality %, and carrier is an aluminum oxide, and the content of described active ingredient all is to calculate benchmark with the carrier.Half generative reforming is selected platinum/rhenium catalyst for use, and the cyclic regeneration reforming catalyst is selected platinum/tin catalyst for use, also can contain the 3rd metal constituent element in addition in the reforming catalyst, with the further reactivity worth of improving catalyzer.
Used reforming catalyst needs through pre-treatment before contact stock oil.To the platinum rhenium that is used for half generative reforming two/multimetallic catalyst, need before the reaction through reduction and prevulcanized processing; To be used for the platinum tin that cyclic regeneration reforms two/multimetallic catalyst, need reduce processing before the reaction.
Should in stock oil, inject chlorine-containing compound according to water-content in the circulation gas in the time of the reforming reaction charging and have suitable acidity to keep catalyzer.Annotating chlorine dose in the inventive method is 1～5ppm, and described notes chlorine dose is the content of elemental chlorine in the raw material.Annotate the used chlorine-containing compound of chlorine and be selected from organic chloride, as halogenated alkane, haloolefin etc., preferred ethylene dichloride, trichloroethane, zellon.
Further specify the present invention below by example, but the present invention is not limited to this.
Example 1
The used reformer feed of preparation the present invention.
The coker gasoline, coker gas oil and the straight-run diesel oil mixture that to boiling range are 70～349 ℃ were 330 ℃, hydrogen dividing potential drop 4.8MPa, volume space velocity 1.6 hours
-1Condition under carry out hydrofining, employed Hydrobon catalyst contains the WO of 26.0 quality %
3, the NiO of 2.6 quality %, the alumina catalyst support of 71.4 quality %.Be on 150 liters the RECTIFYING APPARATUS USED IN LABORATORY,, to cut out 77～175 ℃ cut at capacity with the distillation of the product after the hydrofining, this raw material sulfur-bearing 15ppm, nitrogenous＜1ppm, bromine valency 0.2 gram Br/100 gram.
On the hydrogenation unit of 100 milliliters of catalyzer loading amounts, use reformed pre-hydrogenated catalyzer, 280 ℃, hydrogen dividing potential drop 1.6MPa, feed volume air speed 6.0 hours
-1, above-mentioned raw materials is carried out pre-refining under the condition of hydrogen/oil volume than 100: 1, contain the CoO of 0.03 quality %, the WO of 19.0 quality % in the pre-refining catalyzer
3, the NiO of 2.0 quality % and the alumina catalyst support of 78.97 quality %, the character of the reformer feed I of refining back gained sees Table 1.
Example 2
Press the method for example 1, to boiling range is that 70～338 ℃ coker gasoline, coker gas oil and straight-run diesel oil mixture carries out hydrofining, product after the hydrofining is distilled, cut 75～172 ℃ cut, the straight-run spirit that this cut is identical with boiling range mixes, coker gasoline content is 76.7 quality % in the mixing raw material, and straight-run spirit content is 23.3 quality %.Mixing raw material sulfur-bearing 31ppm, nitrogen＜1ppm, bromine valency 0.1 gram Br/100 gram.
By example 1 method described mixing raw material is carried out pre-refining, the character of the reformer feed II of gained sees Table 1 behind the pre-refining.
Example 3
Get boiling range and be 72～172 ℃ virgin naphtha, its sulphur content is 0.8ppm.Method by example 1 is carried out pre-refining, and the character of the reformer feed III of gained sees Table 1.
Example 4～7
By the inventive method coker gasoline is carried out catalytic reforming.
Reforming raw oil after refining is dewatered by the container that the 4A molecular sieve is housed under 0.05～0.1MPa pressure, control its water-content and be no more than 3ppm.
Loading catalyst in the reactor of 100ml reformation testing apparatus, if the use platinum-rhenium catalyst, then the reactor leading portion loads 20 milliliters catalyst A, 30 milliliters of catalyst B of back segment filling if use platinum-tin catalyst, are then loaded 50 milliliters of catalyzer E in reactor.Have the dehumidification system that removes water in the circulation gas in the described device, the siccative that loads in this system is the 4A molecular sieve.The catalyzer of filling has all carried out reduction and prevulcanized outside the conventional device before the reactor of packing into.Earlier set up hydrogen recycle, under the reaction conditions of regulation, dehydrated raw material oil is introduced reactive system then and react, in raw material, inject ethylene dichloride in the time of charging, make that cl content is 1～5ppm in the stock oil at reactive system.The used reforming catalyst of each example is that the active component content that calculates benchmark sees Table 2 with the alumina catalyst support, raw materials used, reaction conditions and the results are shown in Table 3.
Comparative Examples 1
Method according to example 4 is carried out catalytic reforming to coker gasoline, and the water that different is in the Control Circulation gas is 29～32ppm, and reaction result sees Table 3.
Comparative Examples 2
Method according to example 7 is carried out catalytic reforming to coker gasoline, and the water that different is in the Control Circulation gas is 29～32ppm, and reaction result sees Table 3.
By table 3 data as can be known, after the water-content in the circulation gas increased, the liquid product octane value of reforming reaction gained, liquid yield, pure hydrogen productive rate were all close with the example 4, the example 7 that use identical catalyzer, but the operational cycle obviously shortens.
Comparative Examples 3
Method according to example 4 is carried out catalytic reforming, and the different raw materials that is to use is a straight-run spirit, and the water in the Control Circulation gas is 10～18ppm, reaction conditions and the results are shown in Table 4.
Comparative Examples 4
Method according to example 4 is carried out catalytic reforming, and the different raw materials that is to use is a straight-run spirit, and the water in the Control Circulation gas is 28～33ppm, reaction conditions and the results are shown in Table 4.
Comparative Examples 5
Method according to example 7 is carried out catalytic reforming, and the different raw materials that is to use is a straight-run spirit, and the water in the Control Circulation gas is 10～18ppm, reaction conditions and the results are shown in Table 4.
Comparative Examples 6
Method according to example 7 is carried out catalytic reforming, and the different raw materials that is to use is a straight-run spirit, and the water in the Control Circulation gas is 28～33ppm, reaction conditions and the results are shown in Table 4.
As shown in Table 4, for the straight-run spirit component, the water-content size does not have obvious influence to reaction result in the circulation gas.
Table 1
| The stock oil numbering | I | II | III |
| The coker gasoline ratio, quality % density (20 ℃), g/cm 3Sulphur content, ppm nitrogen content, ppm bromine valency, gBr/100g | 100 0.7266 ＜0.5 ＜0.5 ＜0.1 | 76.7 0.7240 ＜0.5 ＜0.5 ＜0.1 | 0 0.7296 ＜0.5 ＜0.5 ＜0.1 |
| Boiling range (ASTMD-86), ℃ initial boiling point final boiling point | 77 175 | 75 172 | 72 172 |
| Hydrocarbon system forms, quality % alkane naphthenic hydrocarbon aromatic hydrocarbons | 69.71 22.99 7.3 | 64.07 24.70 11.33 | 53.41 42.84 3.75 |
| Research octane number (RON), RONC | 40.2 | 43.5 | 45.3 |
Table 2
| The catalyzer numbering | Pt, quality % | Re, quality % | Sn, quality % | Cl, quality % |
| A B E | 0.26 0.22 0.28 | 0.27 0.46 - | - - 0.30 | 1.3 1.2 1.2 |
Table 3
| Numbering | Example 4 | Example 5 | Example 6 | Example 7 | Comparative Examples 1 | Comparative Examples 2 |
| Stock oil | I | I | II | I | I | I |
| Reforming catalyst | A/B | A/B | A/B | E | A/B | E |
| Temperature of reaction, ℃ reaction pressure, MPa volume space velocity, hr -1Water in hydrogen/hydrocarbon volume ratio circulation gas, ppm | 502 1.2 1.5 1200 15-19 | 492 1.2 1.1 1200 10-18 | 505 1.4 1.8 1200 10-18 | 522 0.35 1.8 400 10-18 | 502 1.2 1.5 1200 29-32 | 522 0.35 1.8 400 29-32 |
| The liquid octane value, the RON liquid yield, quality % liquid virtue contains, the pure hydrogen productive rate of quality %, quality % | 95.6 85.61 57.01 2.29 | 95.6 84.66 57.52 2.20 | 95.0 84.14 57.30 2.26 | 102.0 89.68 78.10 3.98 | 95.4 85.76 56.82 2.28 | 101.9 89.56 78.25 3.96 |
| Operational cycle | 〉=December | 〉=18 months | 〉=December | 〉=4 days | The 8-9 month | ≤ 3 days |
Table 4
| Numbering | Comparative Examples 3 | Comparative Examples 4 | Comparative Examples 5 | Comparative Examples 6 |
| Stock oil | III | III | III | III |
| Reforming catalyst | A/B | A/B | E | E |
| Temperature of reaction, ℃ reaction pressure, MPa volume space velocity, hr -1Water in hydrogen/hydrocarbon volume ratio circulation gas, ppm | 505 1.2 2.0 1200 10-18 | 505 1.2 2.0 1200 28-33 | 525 0.35 2.0 400 10-18 | 525 0.35 2.0 400 28-33 |
| The liquid octane value, the RON liquid yield, quality % liquid virtue contains, the pure hydrogen productive rate of quality %, quality % | 96.6 84.20 66.18 2.36 | 96.5 84.36 66.02 2.35 | 102.2 89.55 82.50 4.16 | 102.1 89.62 82.39 4.15 |
| Operational cycle | 〉=December | 〉=December | 〉=4 days | 〉=4 days |
Claims (10)
1, a kind of reforming method of coker gasoline comprises the steps:
(1) coking distillate is carried out hydrofining, the cutting boiling range is that 70～175 ℃ the cut pre-refining of reforming removes impurity, and dewaters to raw water content and be no more than 5ppm,
(2) will dewater the back raw material, in the presence of 470～540 ℃, 0.2～2.0MPa, hydrogen with the reforming catalyst contact reacts, simultaneously unreacted hydrogen is circulated, and water-content is 5～20ppm in the Control Circulation hydrogen that the notes chlorine dose in the stock oil is 1～5ppm.
2, in accordance with the method for claim 1, it is characterized in that the used catalyzer of reformation pre-refining comprises the group vib metal oxide of 0.1～30.0 quality %, the VIII family metal oxide of 0.01～5.0 quality % and the alumina catalyst support of 65～99 quality % in (1) step.
3, in accordance with the method for claim 2, it is characterized in that described VIII family metal is selected from nickel or cobalt, the group vib metal is selected from molybdenum or tungsten.
4, in accordance with the method for claim 2, it is characterized in that described reformation pre-refining catalyzer contains the nickel oxide of the tungstic oxide of the cobalt oxide of 0.01～2.0 quality %, 1.0～30.0 quality %, 0.5～5.0 quality %, the alumina catalyst support of 63～97 quality %.
5, in accordance with the method for claim 1, it is characterized in that (1) goes on foot dehydration back raw water content and is no more than 3ppm, the water-content in (2) step recycle hydrogen is 8～18ppm.
6, in accordance with the method for claim 1, it is characterized in that (1) step reformation pre-refining temperature of reaction is that 280～340 ℃, hydrogen dividing potential drop are 1.5～4.0MPa, feed volume air speed 2.0～10.0 hours
-1, hydrogen/hydrocarbon volume ratio is 80～150: 1.
7, in accordance with the method for claim 1, it is characterized in that the sulphur, nitrogen content of raw material behind (1) step reformation pre-refining are all less than 0.5ppm.
8, in accordance with the method for claim 1, it is characterized in that used reforming catalyst of (2) step contains platinum, 0.05～4.0 quality % tin or the rhenium of 0.05～2.0 quality %, the chlorine of 0.1～10.0 quality %, carrier is an aluminum oxide.
9, in accordance with the method for claim 1, it is characterized in that (2) step reforming reaction hydrogen/hydrocarbon volume ratio be 300～2000: 1, volume space velocity is 0.8～3.0 hour
-1
10, in accordance with the method for claim 1, it is characterized in that the boiling range of described coking distillate of (1) step is 70～350 ℃, after its hydrofining, in described cutting cut, mix the straight-run spirit of 0～30 quality %.
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| CNB2004100483484A CN1317369C (en) | 2004-06-29 | 2004-06-29 | Reforming method for coking gasoline |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5143596A (en) * | 1989-11-24 | 1992-09-01 | Shell Oil Company | Process for upgrading a sulphur-containing feedstock |
| CN1144259A (en) * | 1995-08-29 | 1997-03-05 | 巴陵石化长岭炼油化工总厂 | Method for producing extraction solvent naphtha by catalytic reforming device |
-
2004
- 2004-06-29 CN CNB2004100483484A patent/CN1317369C/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5143596A (en) * | 1989-11-24 | 1992-09-01 | Shell Oil Company | Process for upgrading a sulphur-containing feedstock |
| CN1144259A (en) * | 1995-08-29 | 1997-03-05 | 巴陵石化长岭炼油化工总厂 | Method for producing extraction solvent naphtha by catalytic reforming device |
Non-Patent Citations (1)
| Title |
|---|
| 石油炼制 林世雄 主编，113，119138，139，143，石油工业出版社 1988 * |
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