CN106947525A - The preprocess method of naphtha in a kind of naphtha modification - Google Patents
The preprocess method of naphtha in a kind of naphtha modification Download PDFInfo
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- CN106947525A CN106947525A CN201710156440.XA CN201710156440A CN106947525A CN 106947525 A CN106947525 A CN 106947525A CN 201710156440 A CN201710156440 A CN 201710156440A CN 106947525 A CN106947525 A CN 106947525A
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- naphtha
- preprocess method
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
- C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
- C10G53/08—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one sorption step
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1037—Hydrocarbon fractions
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1037—Hydrocarbon fractions
- C10G2300/1044—Heavy gasoline or naphtha having a boiling range of about 100 - 180 °C
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention provides the preprocess method of naphtha in a kind of modification of naphtha.The preprocess method comprises the following steps：Naphtha is subjected to absorption denitrogenation；Naphtha by absorption denitrogenation processing is subjected to absorption desulfurization, the pretreatment of naphtha in being modified to naphtha is completed.The preprocess method of naphtha is easy to operate in naphtha modification, and absorption desulfurization, absorption denitrification effect are good.
Description
Technical field
The present invention relates to a kind of pretreatment of the raw material naphtha in preprocess method, more particularly to a kind of modification of naphtha
Method, belongs to petrochemical materials preprocessing technical field.
Background technology
Naphtha modification technology is the non-hydrogenation upgrading technology using light naphthar and C 4 reaction after ether.The technology be with
Carbon four is as raw material after a certain proportion of light naphthar and ether, under conditions of non-hydrogen, makees in solid acid molecular sieve catalyst
Under, by a series of complex such as the overlapping of carbon four and dehydrocyclization, naphtha selective cracking, isomery, oligomerisation and dehydrocyclizations
Reaction, production RON is more than 85 gasoline blend component, and by-product liquefied gas.
At present, modifying catalyst generally uses solid acid molecular sieve, and these molecular sieve catalysts are easily by sulfur-bearing in naphtha
The influence of the toxicity such as compound and nitride and inactivate.Basic nitrogen compound can produce significant impact to catalyst, make catalyst
The cycle of operation substantially shortens, catalyst activity drastically declines, liquid product yield is reduced, the octane number of gasoline is decreased obviously.
Neutral or acid nitride is condensed collagen or asphalitine under the high temperature conditions, is attached to catalyst surface, can equally shorten and urge
The regeneration period of agent.Sulfur-containing compound is highly polar material, can be preferentially adsorbed in the hole of catalyst, occupy in activity
The heart, and there may be hydrogen sulfide, catalyst activity is reduced, aggravate side reaction, make the increase of dry gas growing amount.To ensure modifying apparatus
Long-term operation, these toxicities should strictly be controlled.
CN102008938A is related to a kind of naphtha denitrification adsorbent and preparation method thereof, be with adsorbent using molecular sieve as
Carrier, loaded liquid acid improves the denitrogenation capacity of adsorbent, can make to refine with the organic nitrogen compound in deep removal naphtha
Nitrogen content≤2.5ppm in naphtha afterwards, due to reducing nitrogen content in naphtha, is greatly reduced to downstream unit
Catalyst activity and the influence of equipment life, it is ensured that the long-term operation of device and safety in production.
CN105457600 discloses a kind of preparation method of denitrification adsorbent, denitrification adsorbent be using molecular sieve as carrier,
Handled by the complex liquid of fluorine-containing mixed acid, the polarity and acidity of adsorbent are enhanced, so as to improve nitrogen in naphtha
Compound removal effect.
CN105623719 is related to a kind of removal methods of sulfide in light-end products, under -5-90 DEG C and 0.1-5MPa,
Inorganic sulphide in light oil is first removed using magnetic iron oxide, then organic sulfide in light oil is removed with the activated carbon of supported copper
Thing.Total sulfur content is no more than national standard or professional standard in light oil after removing sulfide.
The problem of there is complex treatment process in current adsorption method.Simultaneously as technological problemses are not played well
The performance of adsorbent.
The content of the invention
In order to solve the above-mentioned technical problem, it is an object of the invention to provide the pre- place of naphtha in a kind of modification of naphtha
Reason method, the preprocess method it is easy to operate, with efficient desulfurization, denitrification effect.
To achieve these goals, the invention provides the preprocess method of naphtha in a kind of modification of naphtha, the stone
The preprocess method of naphtha comprises the following steps in cerebrol modification：
Naphtha is subjected to absorption denitrogenation；
Naphtha by absorption denitrogenation processing is subjected to absorption desulfurization, the pre- place of naphtha in being modified to naphtha is completed
Reason.
In the naphtha modification that the present invention is provided in the preprocess method of naphtha, it is preferable that the suction that absorption denitrogenation is used
Attached denitrifier includes one in X-type molecular sieve, Y type molecular sieve, L-type molecular sieve and the type ZSM 5 molecular sieve of acidified processing
Plant or several combinations.
In the naphtha modification that the present invention is provided in the preprocess method of naphtha, it is highly preferred that the absorption denitrogenation used
Agent is included in H-X types molecular sieve, H-Y types molecular sieve, H-L types molecular sieve and the H-ZSM-5 type molecular sieves of acidified processing
One or more of combinations.
In the naphtha modification that the present invention is provided in the preprocess method of naphtha, it is preferable that the method bag of acidification
Include hydro-thermal process method and/or method of chemical treatment.
In the naphtha modification that the present invention is provided in the preprocess method of naphtha, it is preferable that the method for chemical treatment of use
Including passing through organic acid and/or mineral acid treatment；It is highly preferred that using one kind in nitric acid, hydrochloric acid, oxalic acid and citric acid or several
The solution that the concentration that the combination planted is formed is 0.1M-1.0M.
In the naphtha modification that the present invention is provided in the preprocess method of naphtha, it is preferable that the suction that absorption desulfurization is used
Attached desulfurizing agent includes loaded Ag+, Ni2+, Cu2+, Zn2+In one or two kinds of ions NaY type molecular sieves；
It is highly preferred that the adsorption desulfurizing agent used includes NiY type desulfurizing agents.
In the naphtha modification that the present invention is provided in the preprocess method of naphtha, it is preferable that absorption denitrogenation is equipped with suction
Carried out in the adsorption tower of attached denitrifier, set two adsorption towers to be used in series.
In the naphtha modification that the present invention is provided in the preprocess method of naphtha, it is preferable that absorption desulfurization is equipped with suction
Carried out in the adsorption tower of attached desulfurizing agent, set two adsorption towers to be used in series.
In the naphtha modification that the present invention is provided in the preprocess method of naphtha, it is preferable that the operation bar of absorption denitrogenation
Part is：Adsorption temp is 20 DEG C -150 DEG C, preferably 30 DEG C -100 DEG C；Volume space velocity is 0.5h-1-6h-1, preferably 1h-1-5h-1；Behaviour
Make pressure for 0.5MPa-20MPa.
In the naphtha modification that the present invention is provided in the preprocess method of naphtha, it is preferable that the operation bar of absorption desulfurization
Part is：Adsorption temp is 20 DEG C -150 DEG C, preferably 30 DEG C -110 DEG C；Volume space velocity is 0.5h-1-5h-1, preferably 1h-1-4h-1；Behaviour
Make pressure for 0.5MPa-20MPa.
In the naphtha modification of the present invention in the preprocess method of naphtha, the adsorption denitrifier of use can be according to its acid
Property etc. use requirement carry out suitable modification, method of modifying can be hydro-thermal process method or method of chemical treatment or the two
Comprehensively modifying means.
In the naphtha modification of the present invention in the preprocess method of naphtha, the adsorption tower equipped with adsorption denitrifier sets two
It is individual, it is used in series, two regular handover operations of adsorption tower.After one of denitrogenation adsorption tower adsorption saturation, that is, switch another
Individual adsorption tower carries out absorption denitrification reaction, and the adsorption tower cut out then carries out the regenerative operation of adsorption denitrifier.After adsorption saturation
The regenerative operation of adsorption denitrifier is the routine operation of those skilled in the art.The regeneration condition of adsorption denitrifier is general as described
For：Regeneration temperature is 260 DEG C -480 DEG C, preferably 300 DEG C -450 DEG C；Constant temperature 1h-60h, preferably 8h-50h.
In the naphtha modification of the present invention in the preprocess method of naphtha, the adsorption tower equipped with adsorption desulfurizing agent sets two
It is individual, it is used in series, two regular handover operations of desulfurization adsorption tower.After one of desulfurization adsorption tower adsorption saturation, that is, switch
Another adsorption tower carries out absorption desulphurization reaction, and the absorption desulfurization adsorption tower cut out then carries out the regenerative operation of adsorption desulfurizing agent.
The regenerative operation of described adsorption desulfurizing agent is also the routine operation of those skilled in the art.The regeneration of adsorption desulfurizing agent as described
Condition is generally：Regeneration temperature is 300 DEG C -550 DEG C, preferably 340 DEG C -500 DEG C；Constant temperature 1h-70h, preferably 10h-65h.
The preprocess method of naphtha, is through pump by raw material naphtha from surge tank in the naphtha modification that the present invention is provided
Conveying, is first taken off from the basic nitrogen that the bottom of adsorption tower enters in the adsorption tower equipped with adsorption denitrifier, raw material with adsorbent
Nitrogen is reacted and is removed, and the naphtha after denitrogenation is discharged by the top of adsorption tower, enters back into the adsorption tower equipped with adsorption desulfurizing agent,
Sulfur-containing compound in raw material carries out absorption desulphurization reaction with adsorbent and is removed, the original of the naphtha modification after being refined
Material.
In naphtha modifying process, after the preprocess method processing of naphtha in the naphtha modification by the present invention
Naphtha feeding naphtha reforming reactor modified, can extend modification reacting middle catalyst service life, raising
The economy that device is integrally runed.
Compared with the existing method pre-processed by hydrogenation, from the point of view of unit actual run time, pass through hydrogenation
The preprocess method of processing catalyst inactivation in subsequent reactions is very fast, and reaction has been inactivated for general one month, and the present invention
Purified by adsorbing and removing after technique pretreatment, it is still good to have run half a year many effects at present, extends the use of catalyst
Life-span, so as to greatly reduce production cost.Both essential distinctions are the use longevity for extending catalyst in the naphtha transformation of the way
Life, reduces production cost.
The preprocess method of naphtha compared with prior art, has the following advantages that in the naphtha modification of the present invention：
It is all by water that the adsorption denitrifier used in the naphtha modification of the present invention in the preprocess method of naphtha, which is,
After heat treatment and/or chemical treatment modification, its acid centre increase, acidity is improved, while duct is more suitable for adsorbing denitrogenation；
The preprocess method of naphtha, disclosure satisfy that long-term operation, to plant modification in the naphtha modification of the present invention
Investment cost is low；
The technique of the preprocess method of naphtha is simple in the naphtha modification of the present invention, and simple operation, security is good, ring
Border is friendly, and with higher economic effect.
Brief description of the drawings
Fig. 1 be embodiment in naphtha modification in naphtha preprocess method schematic flow sheet.
Main Reference labelled notation
The adsorption tower of 1 first 2 second the 3rd adsorption tower 4 of adsorption tower 3 of adsorption tower the 4th
Embodiment
In order to which technical characteristic, purpose and beneficial effect to the present invention are more clearly understood from, now to the skill of the present invention
Art scheme carry out it is described further below, but it is not intended that to the present invention can practical range restriction.
Embodiment 1
Present embodiments provide the preprocess method of naphtha in a kind of modification of naphtha, its technological process as shown in figure 1,
Comprise the following steps：
Naphtha is conveyed from surge tank through pump, is directly entered adsorbent equipment, and naphtha enters first by the bottom of adsorption tower
The denitrogenation adsorption tower 2 of denitrogenation adsorption tower 1 and second removes naphtha neutral and alkali nitrogen, then again from bottom to top under adsorbent effect
Sequentially pass through the 3rd adsorption tower 3 built with modified molecular screen desulfurizing agent and the 4th absorption built with modified molecular screen desulfurizing agent
Tower 4, the naphtha after being refined；
Wherein, the temperature in the first adsorption tower 1 and the second adsorption tower 2 is respectively 35 DEG C, and pressure is respectively 0.1Mpa, volume
Liquid air speed 1h-1；Temperature in 3rd adsorption tower 3 and the 4th adsorption tower 4 is respectively 35 DEG C, and pressure is respectively 0.1Mpa, volume liquid
Air speed 1h-1；The ratio of height to diameter of first adsorption tower 1 and the denitrifier bed in the second adsorption tower 2 is 3.0, the 3rd adsorption tower 3 and the 4th
The ratio of height to diameter of desulfurizing agent bed in adsorption tower 4 is 3.0.
Adsorption denitrifier：Type ZSM 5 molecular sieve is taken, the hydro-thermal process 3h at 500 DEG C, with activated alumina by 35: 65
Weight is than mixing, through processes such as spin, sieving, roastings, and adsorption denitrifier is made.
The preparation method of adsorption desulfurizing agent is as follows：
(1) the NaY type molecular sieves for weighing Φ 2-3mm are placed in ceramic crucible, are roasted in Muffle furnace at 300-6000 DEG C
After burning 3-6 hours, room temperature is down to naturally in atmosphere；
(2) the NaY type molecular sieves handled through step (1) are put into nickel nitrate aqueous solution, using equi-volume impregnating meter
The consumption of the aqueous solution is calculated, dipping temperature is 20-800 DEG C, and dip time is 8-48 hours；
(3) the NaY type molecular sieve carriers deionized water rinsing that will be handled through step (2) 2-4 times, filtering, adsorbent exists
Dry 2-12 hour, be then calcined 1-5 hours at 450-5500 DEG C in Muffle furnace at 90-1100 DEG C, the obtained metal from
The Y type molecular sieve adsorbent of son load, wherein, the gross weight of the Y type molecular sieve adsorbent loaded based on the metal ion is born
The content for carrying metal is 3-15wt%.
In the present embodiment, the total sulfur content in the naphtha handled is 5ppmw, and total nitrogen content is 40ppmw, is obtained
Arrive it is refined after naphtha total sulfur content<1ppmw, total nitrogen content<1ppmw.
Embodiment 2
The preprocess method of naphtha in a kind of modification of naphtha is present embodiments provided, its naphtha with embodiment 1
Preprocess method it is essentially identical, difference is：Temperature in first adsorption tower 1 and the second adsorption tower 2 is respectively 40 DEG C,
Volume liquid air speed 2h-1；Temperature in 3rd adsorption tower 3 and the 4th adsorption tower 4 is respectively 40 DEG C, volume liquid air speed 2h-1；
In the present embodiment, the denitrifier used is the H-X type molecular sieve of 0.1M nitric acid treatments, and desulfurizing agent is what Ag was modified
Total sulfur content in Y molecular sieve, the naphtha handled is 5ppmw, and total nitrogen content is 40ppmw, obtain it is refined after stone
Cerebrol total sulfur content<1ppmw, total nitrogen content<1ppmw.
Embodiment 3
The preprocess method of naphtha in a kind of modification of naphtha is present embodiments provided, its naphtha with embodiment 1
Preprocess method it is essentially identical, difference is：Temperature in first adsorption tower 1 and the second adsorption tower 2 is respectively 40 DEG C,
Volume liquid air speed 3h-1；Temperature in 3rd adsorption tower 3 and the 4th adsorption tower 4 is respectively 40 DEG C, volume liquid air speed 2h-1；
In the present embodiment, the denitrifier used is the H-Y type molecular sieve of 0.3M oxalic acid treatments, and desulfurizing agent is what Ni was modified
Total sulfur content in Y molecular sieve, the naphtha handled is 5ppmw, and total nitrogen content is 40ppmw, obtain it is refined after stone
Cerebrol total sulfur content<1ppmw, total nitrogen content<1ppmw.
Embodiment 4
The preprocess method of naphtha in a kind of modification of naphtha is present embodiments provided, its naphtha with embodiment 1
Preprocess method it is essentially identical, difference is：Temperature in first adsorption tower 1 and the second adsorption tower 2 is respectively 40 DEG C,
Pressure is respectively 0.6MPa, volume liquid air speed 2h-1；Temperature in 3rd adsorption tower 3 and the 4th adsorption tower 4 is respectively 40 DEG C, pressure
Power is respectively 0.6MPa volumes liquid air speed 2h-1；
In the present embodiment, the denitrifier used is the H-L type molecular sieve of 0.5M citric acid treatments, and desulfurizing agent is Cu modifications
Y molecular sieve, the total sulfur content in the naphtha handled is 5ppmw, and total nitrogen content is 40ppmw, obtain it is refined after
Naphtha total sulfur content<1ppmw, total nitrogen content<1ppmw.
Above example illustrates that the technique of the preprocess method of naphtha is simple in naphtha modification of the invention of the invention
Single, simple operation, pretreatment expense is low, and denitrification and desulfurization effect is good.
Claims (10)
1. the preprocess method of naphtha in a kind of naphtha modification, it is characterised in that naphtha is pre- in naphtha modification
Processing method comprises the following steps：
Naphtha is subjected to absorption denitrogenation；
Naphtha by absorption denitrogenation processing is subjected to absorption desulfurization, the pretreatment of naphtha in being modified to naphtha is completed.
2. the preprocess method of naphtha in naphtha modification according to claim 1, it is characterised in that the absorption takes off
The adsorption denitrifier that nitrogen is used includes X-type molecular sieve, Y type molecular sieve, L-type molecular sieve and the ZSM-5 types point of acidified processing
One or more of combinations in son sieve.
3. the preprocess method of naphtha in excellent naphtha modification according to claim 2, it is characterised in that the absorption
Denitrifier includes H-X types molecular sieve, H-Y types molecular sieve, H-L types molecular sieve and the H-ZSM-5 type molecular sieves of acidified processing
In one or more of combinations.
4. the preprocess method of naphtha in the naphtha modification according to Claims 2 or 3, it is characterised in that the acid
Changing the method for processing includes hydro-thermal process method and/or method of chemical treatment.
5. the preprocess method of naphtha in naphtha modification according to claim 4, it is characterised in that at the chemistry
Logos includes being handled by organic acid and/or inorganic acid；Preferably, using one in nitric acid, hydrochloric acid, oxalic acid and citric acid
The solution that the concentration that kind or several combinations are formed is 0.1M-1.0M.
6. the preprocess method of naphtha in naphtha modification according to claim 1, it is characterised in that the absorption takes off
The adsorption desulfurizing agent that sulphur is used includes loaded Ag+, Ni2+, Cu2+, Zn2+In one or two kinds of ions NaY type molecular sieves.
7. the preprocess method of naphtha in naphtha modification according to claim 1, it is characterised in that the absorption takes off
Nitrogen is carried out in the adsorption tower equipped with adsorption denitrifier, sets two adsorption towers to be used in series.
8. the preprocess method of naphtha in naphtha modification according to claim 1, it is characterised in that the absorption takes off
Sulphur is carried out in the adsorption tower equipped with adsorption desulfurizing agent, sets two adsorption towers to be used in series.
9. the preprocess method of naphtha in the naphtha modification according to claim 1 or 7, it is characterised in that absorption is de-
The operating condition of nitrogen is：Adsorption temp is 20 DEG C -150 DEG C, preferably 30 DEG C -100 DEG C；Volume space velocity is 0.5h-1-6h-1, preferably
1h-1-5h-1；Operating pressure is 0.5MPa-20MPa.
10. the preprocess method of naphtha in the naphtha modification according to claim 1 or 8, it is characterised in that absorption is de-
The operating condition of sulphur is：Adsorption temp is 20 DEG C -150 DEG C, preferably 30 DEG C -110 DEG C；Volume space velocity is 0.5h-1-5h-1, preferably
1h-1-4h-1；Operating pressure is 0.5MPa-20MPa.
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| CN103184065A (en) * | 2013-04-01 | 2013-07-03 | 孟红琳 | Method for removing nitrogen-containing compound from diesel oil by adsorbing |
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2017
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| CN104017602A (en) * | 2013-03-01 | 2014-09-03 | 中国石油化工股份有限公司 | Reformed pre-hydrogenated topped oil preprocessing method |
| CN103184065A (en) * | 2013-04-01 | 2013-07-03 | 孟红琳 | Method for removing nitrogen-containing compound from diesel oil by adsorbing |
| US20150232765A1 (en) * | 2014-02-19 | 2015-08-20 | King Abdulaziz City For Science And Technology | Cold process for removal of sulfur in straight run diesel by ozone and ter-butyl hydroperoxide |
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