CN109628141A - A method of by F- T synthesis hydrofined oil separating monomer n-alkane - Google Patents
A method of by F- T synthesis hydrofined oil separating monomer n-alkane Download PDFInfo
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- CN109628141A CN109628141A CN201910084437.0A CN201910084437A CN109628141A CN 109628141 A CN109628141 A CN 109628141A CN 201910084437 A CN201910084437 A CN 201910084437A CN 109628141 A CN109628141 A CN 109628141A
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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
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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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/4006—Temperature
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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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/4012—Pressure
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The purpose of the present invention is to provide a kind of methods for separating C11 to C25 compound-specific n-alkanes by F- T synthesis hydrofined oil, F- T synthesis hydrofined oil is fed into 1 set be arranged in parallel or more set first rectifying columns by this method and Second distillation column separates, to obtain subject monomers n-alkane.Method of the invention establishes the rectifying device of corresponding tricks according to the quantity of target product to be separated, and separation process is simply and flexible, and equipment investment is small, and technological operation is flexible and technical difficulty is low；It is capable of the compound-specific n-alkanes of isolated high-purity by means of the present invention, added value is high, has good cost-benefit ratio.
Description
Technical field
The present invention relates to a kind of methods of separating monomer n-alkane, in particular to one kind is by F- T synthesis hydrofined oil
The method for separating C11 to C25 compound-specific n-alkanes.
Background technique
N-alkane refers to the saturated alkane of not branch.N-alkane be suitable for production linear alkylbenzene (LAB), chlorinated paraffin,
Lauric acid, brazilic acid, long-chain biatomic acid etc. are widely used in daily chemical product, lubricating oil, nylon manufacture, oily adhesive, ink painting
The fields such as material.
The methods of at this stage mainly using petroleum as raw material, adsorbed using urea dewaxing, molecular sieve, it is obtained not in conjunction with rectifying
With the n-alkane monomer of carbon number.
Urea dewaxing cardinal principle is that urea and n-alkane form solid complex, by complexing, sedimentation, separation, is added
Heat and etc., final separation obtains n-alkane.In the process, the form used according to urea can be divided into dry method dewaxing
It dewaxes with wet process.Dry method dewaxing is that solid urea and activator (such as ethyl alcohol) are added to wait in the oil product that dewaxes；Wet process dewaxing
It is that saturation urea liquid and activator (such as isopropanol) are added to wait in the oil product that dewaxes.Finally obtained product is N-alkanes
Hydrocarbon mixture, the process are used only to separate n-alkane and isoparaffin.Sinopec Group's Fushun petroleum
Chemical research institute develops IUDW urea dewaxing technology, the technology be using isopropanol as activating agent, using pipeline as complex reactor,
It is dewaxed using revolving scraper and the method for countercurrent washing, the refinery of the DEWAXING TECHNIQUE at home is widely adopted (middle external enwergy
Source, 2014,19 (10): 79-82).
Molecular sieve adsorbing separation n-alkane is using molecular sieve selective absorption characteristic, by n-alkane and isoparaffin
It is separated.Adsorbent application at present is at most 5A molecular sieve, and molecular sieve possesses the uniform micro-pore diameter of 0.52nm, can inhale
Attached smaller n-alkane molecule；Desorbing agent is mainly micro-molecular gas, such as N2、H2Deng.Currently, industrially having been carried out with stone
Cerebrol is raw material, using 5A zeolite fixed-bed reactor technique, heats pressure-variable adsorption process by multitower and obtains normal paraffin mixture；
In conjunction with the n-alkane monomer of the available high-purity of distillation process.
However, using petroleum as raw material separating normal alkane, it is inevitably miscellaneous containing aromatic hydrocarbons, cycloalkane, sulphur, nitrogen etc.
Matter, separating difficulty is big, and the investment of equipment is also increased while improving energy consumption.Since objectionable impurities a small amount of in petroleum is difficult point
From clean therefore isolated product, also to environment, there are different degrees of harm.
Unlike petroleum, Fischer-Tropsch synthetic is mainly by n-alkane, normal olefine, isoparaffin and a small amount of oxygen-containing
Compound composition, aromatic hydrocarbons naphthene content is extremely low, and the not impurity such as sulfur-bearing, nitrogen.Compared to the n-alkane of traditional petroleum path
Production technology, producing compound-specific n-alkanes as raw material using Fischer-Tropsch synthetic has significant cost advantage and higher quality,
It is suitble to isolated compound-specific n-alkanes.The characteristics of Fischer-Tropsch synthetic, makes separating normal alkane become more feasible.This field
Some researchs have been carried out in this respect, for example, patent document CN106699501A discloses a kind of compound-specific n-alkanes that produce
Method, this method are continuously cut into LPG, C5~C10 by concatenated multitower rectifying using Fischer-Tropsch synthesis oil as raw material, the technology road
Line has that continuous lock out operation difficulty is big, operation is inflexible, and separating product is mainly C5~C10 monomer N-alkanes
Hydrocarbon, product purpose are limited.For the separation of the compound-specific n-alkanes greater than C10, energy consumption is high, and technical difficulty is bigger, and existing
The purity that some isolation technics obtain product is lower (often isolate as mixed solvent naphtha, rather than the alkane of monomer).
Therefore, for carrying out industrial separation from Fischer-Tropsch synthetic and obtaining the compound-specific n-alkanes of C11 to C25, mesh
It is preceding still to require study.
Summary of the invention
In view of the above technical problems, the purpose of the present invention is to provide a kind of novel separation C11 to C25 monomer N-alkanes
The method of hydrocarbon, the raw material of this method are F- T synthesis hydrofined oil, obtain compound-specific n-alkanes using rectifying, product purity is high
(product quality percentage composition may be up to 99wt% or more).Advantage of the invention is that being capable of the isolated positive structure of high-purity monomer
Alkane, technical process are pollution-free；Processing technology routine is simple, and equipment investment is small, flexible operation and technical difficulty is low.
The present invention relates to it is a kind of by F- T synthesis hydrofined oil separate C11 to C25 compound-specific n-alkanes method,
In, it the described method comprises the following steps:
(1) the F- T synthesis hydrofined oil is fed into first rectifying column, in the tower top of the first rectifying column
The n-alkane and carbon number that carbon number is removed less than subject monomers n-alkane are less than or equal to the subject monomers n-alkane
Isoparaffin, and the logistics comprising the subject monomers n-alkane is obtained in the tower reactor of the first rectifying column；
(2) logistics is fed into Second distillation column from first rectifying column, in the overhead collection of the Second distillation column
One of C11 to C25 compound-specific n-alkanes as the subject monomers n-alkane；
Wherein, the quantity N relative to the subject monomers n-alkane it is expected while separated has been arranged in parallel N set institute
First rectifying column and the Second distillation column are stated, first rectifying column described in every set and the Second distillation column are for separating the mesh
Mark one of compound-specific n-alkanes.
For method of the invention mainly for the production of C11 to C25 compound-specific n-alkanes, processing technology routine is simple, and equipment is thrown
Provide small, operation difficulty is low；Compared with prior art, target product of the invention is (up to 99wt% or more) with high purity, adds
Value is high, can produce petrochemical field and be difficult to the C11 produced to C25 compound-specific n-alkanes product.Moreover, can also be further by separation
The oil product of by-product after subject monomers n-alkane is sent directly into downstream units and uses as raw material, and production technology process is without dirt
Dye, and improve cost-effectiveness.Also, in method of the present invention, a set of rectifying device (includes concatenated first rectifying
Tower and Second distillation column) a kind of product is only separated, it (can be depended on to be separated according to the quantity N to the target product of separation simultaneously
Raw material and actual product demand) and establish the rectifying device of corresponding tricks (i.e. N set) so that separation process is simpler
It is single and flexible, and do not have to that excessive rectifying column (that is, can be adjusted flexibly according to isolated n-alkane quantity it is expected) is once arranged.
Detailed description of the invention
Fig. 1 is the schematic diagram of the process flow of of the invention one illustrative embodiment.
Fig. 2 is the schematic diagram of the process flow of the embodiment of another exemplary of the invention.
In described Fig. 1 and Fig. 2, each appended drawing reference is respectively indicated, and: V101 is surge tank, T101 be first rectifying column,
T102 is Second distillation column and T103 is third distillation column.
Specific embodiment
For a better understanding of the invention, the present invention is further explained below with reference to following illustrative embodiment
It states, but these embodiments should not be construed as any limitation on the present invention.
In the present invention, unless otherwise specified, Cn compound-specific n-alkanes (also referred to as " n-alkane simple substance ") refer to
Its carbon number n is more than or equal to the monomer of 11 and the n-alkane less than or equal to 25.
In the present invention, unless otherwise specified, term " subject monomers n-alkane " can refer to C11 to C25 monomer just
One of structure alkane is a variety of." carbon number is less than the n-alkane of subject monomers n-alkane and carbon number is less than or equal to for statement
The isoparaffin of subject monomers n-alkane " refers to the positive structure with the carbon number less than desired subject monomers n-alkane
The isoparaffin of alkane and the carbon number less than or equal to desired subject monomers n-alkane, for example, working as subject monomers just
When structure alkane is the compound-specific n-alkanes of C11, carbon number is less than less than the n-alkane and carbon number of subject monomers n-alkane etc.
Refer to n-alkane of its carbon number less than C11 and carbon number less than or equal to C11's in the isoparaffin of subject monomers n-alkane
Isoparaffin is (that is, C10 -N-alkane and C11 -Isoparaffin).
In one embodiment, the present invention relates to one kind by F- T synthesis hydrofined oil separation C11 to C25 monomer just
The method of structure alkane, wherein the described method comprises the following steps:
(1) the F- T synthesis hydrofined oil is fed into first rectifying column, in the tower top of the first rectifying column
The n-alkane and carbon number that carbon number is removed less than subject monomers n-alkane are less than or equal to the subject monomers n-alkane
Isoparaffin, and the logistics comprising the subject monomers n-alkane is obtained in the tower reactor of the first rectifying column；
(2) logistics is fed into Second distillation column from first rectifying column, in the overhead collection of the Second distillation column
One of C11 to C25 compound-specific n-alkanes as the subject monomers n-alkane；
Wherein, the quantity N relative to the subject monomers n-alkane it is expected while separated has been arranged in parallel N set institute
First rectifying column and the Second distillation column are stated, first rectifying column described in every set and the Second distillation column are for separating the mesh
Mark one of compound-specific n-alkanes.
In a preferred embodiment, the F- T synthesis hydrofined oil, which is achieved in that, makes from F- T synthesis
The Fischer-Tropsch synthetic of unit, which enters the progress hydrotreating of hydrofinishing unit, (can be used any conventional means known in the art
Hydrotreating is carried out with condition), the atmospheric fractional tower side line product and/or vacuum fractionation tower side line product collected are as expense
Hold in the palm hydrogeneration processes refined oil.The all saturated alkanes of alkane that the F- T synthesis hydrofined oil includes, wherein n-alkane
Content be 85wt%~96wt%, others be isoparaffin.
In some preferred embodiments, the F- T synthesis hydrofined oil can be selected from: as atmospheric fractional tower side
Normal line oil, the normal two wires oil of line product, and/or first vacuum side stream as vacuum fractionation tower side line product, second line of distillation oil, subtract three
Line oil.The F- T synthesis hydrofined oil can be distributed according to the difference of side line product and with different alkane carbon numbers, specifically
Composition is shown in as in the following table 1.Any of the above-described kind or a variety of side line products can be selected according to desired subject monomers n-alkane
Rectification process is carried out as F- T synthesis hydrofined oil raw material, and to it, to obtain C11 into C25 compound-specific n-alkanes
It is any one or more.
In a preferred embodiment, before being fed to the first rectifying column, by the F- T synthesis hydrofinishing
Oil is fed into surge tank and is preheated, the F- T synthesis hydrofined oil after being preheated.In further preferred embodiment
In, the F- T synthesis hydrofined oil is preheated to 100 DEG C~150 DEG C.
In the present invention, the N can indicate any one integer in 1~15, for example, 1,2,3,4,5,6,7,8,9,10,
11,12,13,14 or 15.Can according to simultaneously separation compound-specific n-alkanes quantity, determine rectifying device (including first essence
Evaporate tower and Second distillation column) corresponding tricks.For example, being needed when needing while separating the compound-specific n-alkanes of C11 to C15
5 sets of first rectifying columns and Second distillation column are set；And when the compound-specific n-alkanes of needs successively separation C11 to C15 are (that is, primary
Only need to separate a kind of compound-specific n-alkanes) when, a set of first rectifying column and Second distillation column can be only set, so as to basis
The needs of actual production, and neatly adjust corresponding process system.
In a preferred embodiment, in step (1), the first rectifying column is atmospheric distillation tower or rectification under vacuum
Tower.
In a preferred embodiment, in step (1), the feed entrance point of the first rectifying column is column plate therein
At 2/5~3/4 from top to bottom.
In a preferred embodiment, in step (1), the number of plates of the first rectifying column is 40~120, reflux ratio
It is 3~10, tower top operating pressure is -100kPaG~10kPaG, and tower top operation temperature is 145 DEG C~285 DEG C, tower reactor control temperature
Degree is 205 DEG C~325 DEG C.It is highly preferred that the number of plates of the first rectifying column is 60~105, reflux ratio in step (1)
It is 3~10, tower top operating pressure is -90kPaG~0kPaG, and tower top operation temperature is 165 DEG C~280 DEG C, and tower reactor controls temperature
It is 215 DEG C~325 DEG C.
In a preferred embodiment, in step (2), the Second distillation column is atmospheric distillation tower or rectification under vacuum
Tower.
In a preferred embodiment, in step (2), the feed entrance point of the Second distillation column is column plate therein
At 9/20~9/16 from top to bottom.
In a preferred embodiment, in step (2), the number of plates of the Second distillation column is 40~120, reflux ratio
It is 4~20, tower top operating pressure is -100kPaG~10kPaG, and tower top operation temperature is 170 DEG C~330 DEG C, tower reactor control temperature
Degree is 210 DEG C~335 DEG C.It is highly preferred that the number of plates of the Second distillation column is 40~120, reflux ratio in step (2)
It is 4~20, tower top operating pressure is -90kPaG~0kPaG, and tower top operation temperature is 190 DEG C~320 DEG C, and tower reactor controls temperature
It is 225 DEG C~335 DEG C.
In a preferred embodiment, in step (2), the logistics is fed into further setting from first rectifying column
Third distillation column between the first rectifying column and Second distillation column obtains enriched substance in the tower top of the third distillation column
Stream, and the enriched substance stream is fed into the Second distillation column.Preferably, the third distillation column is atmospheric distillation tower or subtracts
Press rectifying column.The third distillation column can be used to improve the target n-alkane in logistics to be fractionated as product rectifying column
Concentration can go out be enriched with target N-alkanes from the tower top of third distillation column to reduce the separating difficulty of Second distillation column with rough segmentation
The logistics of hydrocarbon.Additionally preferably, the carbon number generated in the tower reactor of third distillation column is greater than to the positive structure of subject monomers n-alkane
Alkane and isoparaffin (that is, heavy constituent) are sent out as the tower kettle product of third distillation column.
In further preferred embodiment, the feed entrance point of the third distillation column be column plate therein on to
Under 2/5~3/5 at.
In further preferred embodiment, the number of plates of the third distillation column is 10~80 pieces, reflux ratio is 3~
10, tower top operating pressure is -90kPaG~0kPaG, and tower top operation temperature is 120 DEG C~180 DEG C, and tower reactor is controlled at 150
DEG C~195 DEG C.It is highly preferred that the number of plates of the third distillation column is 10~20 pieces, reflux ratio is 3~7, tower top operating pressure
For -90kPaG~-80kPaG, tower top operation temperature is 130 DEG C~150 DEG C, and tower reactor is controlled at 160 DEG C~175 DEG C.
As an example, the feed entrance point of the first rectifying column is therein for example when separating C11 compound-specific n-alkanes
At 1/2~3/4 from top to bottom of column plate；The number of plates of the first rectifying column is 40~60, and reflux ratio is 3~6, tower top behaviour
Making pressure is -50kPaG~10kPaG, and tower top operation temperature is 145 DEG C~185 DEG C, and tower reactor is controlled at 205 DEG C~230
℃；Also, the feed entrance point of the Second distillation column is at 9/20~9/16 from top to bottom of column plate therein；Described second
The number of plates of rectifying column is 40~80, and reflux ratio is 4~8, and tower top operating pressure is -50kPaG~10kPaG, tower top operation temperature
Degree is 170 DEG C~220 DEG C, and tower reactor is controlled at 210 DEG C~250 DEG C.
As an example, the feed entrance point of the first rectifying column is therein for example when separating C12 compound-specific n-alkanes
At 1/2~3/4 from top to bottom of column plate；The number of plates of the first rectifying column is 50~70, and reflux ratio is 3~6, tower top behaviour
Making pressure is -50kPaG~10kPaG, and tower top operation temperature is 170 DEG C~200 DEG C, and tower reactor is controlled at 210 DEG C~250
℃；The feed entrance point of the Second distillation column is at 9/20~9/16 from top to bottom of column plate therein；Second rectifying
The number of plates of tower is 40~80, and reflux ratio is 4~8, and tower top operating pressure is -50kPaG~10kPaG, and tower top operation temperature is
200 DEG C~240 DEG C, tower reactor is controlled at 220 DEG C~260 DEG C；Also, the feed entrance point of the third distillation column is therein
At 2/5~3/5 from top to bottom of column plate, the number of plates of the third distillation column is 10~20 pieces, and reflux ratio is 3~7, tower top
Operating pressure be -90kPaG~-80kPaG, tower top operation temperature be 130 DEG C~150 DEG C, tower reactor controlled at 160 DEG C~
175℃。
As an example, the feed entrance point of the first rectifying column is therein for example when separating C25 compound-specific n-alkanes
At 2/5~3/4 from top to bottom of column plate；The number of plates of the first rectifying column is 60~100, and reflux ratio is 6~10, tower top
Operating pressure be -90kPaG~-50kPaG, tower top operation temperature be 145 DEG C~185 DEG C, tower reactor controlled at 205 DEG C~
230℃；Also, the feed entrance point of the Second distillation column is at 9/20~9/16 from top to bottom of column plate therein；It is described
The number of plates of Second distillation column is 40~80, and reflux ratio is 4~8, and tower top operating pressure is -50kPaG~10kPaG, tower top behaviour
Making temperature is 230 DEG C~280 DEG C, and tower reactor is controlled at 300 DEG C~325 DEG C.
In addition, those skilled in the art are shown based on above and embodiment when separating C13~C24 compound-specific n-alkanes
Example property record can choose suitable rectifying condition.
In a preferred embodiment, the method further includes by the overhead product of the first rectifying column, described
The tower kettle product of the tower kettle product of third distillation column and/or the Second distillation column is sent to Oil Tank (such as diesel oil tank field),
To collect the oil product of by-product, to further increase cost-effectiveness.
The method can obtain respectively by the F- T synthesis hydrofined oil after rectification process through the invention
N-alkane monomer to C11 to C25, and n-alkane monomer purity can be not less than 95wt%, be preferably not less than
97wt%, more desirably not less than 99wt%.
For the first rectifying column, the Second distillation column and/or the third distillation column, when target product
It, preferably will be described when boiling point is higher (for example, the boiling point of the tower top target product of Second distillation column is higher than 250 DEG C~300 DEG C)
First rectifying column, the Second distillation column and/or the third distillation column are selected as vacuum rectification tower, thus can pass through decompression essence
It evaporates and is handled, so as to reduce operation temperature, prevent the raw material of the rectifying in tower reactor from going bad because of thermal cracking.
The method of the present invention is mainly used for from raw material separating specific one or more positive structures of monomer according to actual demand
Alkane, the surplus products after separation can be directly entered downstream units (such as Oil Tank) and use as raw material, production technology mistake
Journey is pollution-free；Processing technology routine is simple, and equipment investment is small, and operation difficulty is low, and product purity is high.Compared with prior art, originally
Invention product is mainly C11 to C25 compound-specific n-alkanes, and target product purity is high, added value is high, can produce petrochemical field and be difficult to
The compound-specific n-alkanes product of the heavy constituent greater than C10 of production.It, can be according to simultaneously also, in method of the present invention
The quantity of isolated target product and the rectifying device for establishing corresponding tricks, so that separation process is simpler and flexible,
And it avoids that excessive rectifying column is once arranged and results in waste of resources.
Embodiment
The present invention will be described below by way of specific embodiments, but the present invention is not limited thereto.
Experimental method used in following embodiments is conventional method unless otherwise specified；Institute in following embodiments
Reagent, material and device etc., be commercially available unless otherwise specified or can by those skilled in the art according to
The ordinary technical knowledge of this field and be prepared.
Embodiment 1
Using normal line oil as raw material Fischer-Tropsch hydrogeneration processes refined oil, C11~C14 monomer therein is successively being separated respectively just
Structure alkane.Normal line oil composition is shown in Table 1, and the separation is carried out according to process shown in fig. 1.
It is 100 DEG C that normal line oil, which is fed into surge tank V101, and is preheated to temperature.
The separation of 1-1 C11 compound-specific n-alkanes
Normal line oil after preheating is fed into first rectifying column T101 (atmospheric distillation tower) from surge tank V101, the first essence
The feed entrance point for evaporating tower T101 is that the 40th block of plate, the number of plates 60, reflux ratio 5, tower top operating pressure are from top to bottom
0kPaG；The tower top operation temperature of first rectifying column T101 is 167.8 DEG C, and tower reactor is controlled at 216.9 DEG C.
It is different less than or equal to C11 less than the n-alkane of C11 and carbon number that carbon number is distillated from the tower top of first rectifying column T101
Structure alkane (overhead product), while the tower kettle product comprising C11 n-alkane is distillated in tower reactor, which is fed into
Two rectifying column T102 (atmospheric distillation tower).The feed entrance point of Second distillation column T102 is that the 35th block of plate, the number of plates are from top to bottom
70, reflux ratio 5, tower top operating pressure is 0kPaG；The tower top operation temperature of Second distillation column T102 is 193.5 DEG C, tower reactor control
Temperature processed is 229.0 DEG C.
The compound-specific n-alkanes (its composition is shown in Table 2) of C11 are distillated from the tower top of Second distillation column T102, purity is greater than
99wt%, meanwhile, the tower kettle product of the overhead product of first rectifying column T101 and Second distillation column T102 are sent into diesel oil tank field.
The separation of 1-2 C12 compound-specific n-alkanes
Normal line oil after preheating is fed into first rectifying column T101 (atmospheric distillation tower) from surge tank V101, the first essence
The feed entrance point for evaporating tower T101 is that the 45th block of plate, the number of plates 60, reflux ratio 5, tower top operating pressure are from top to bottom
0kPaG；The tower top operation temperature of first rectifying column T101 is 185.5 DEG C, and tower reactor is controlled at 230.0 DEG C.
It is different less than or equal to C12 less than the n-alkane of C12 and carbon number that carbon number is distillated from the tower top of first rectifying column T101
Structure alkane (overhead product), while the tower kettle product comprising C12 n-alkane is distillated in tower reactor, which is fed into
Two rectifying column T102 (atmospheric distillation tower).The feed entrance point of Second distillation column T102 is that the 30th block of plate, the number of plates are from top to bottom
60, reflux ratio 5, tower top operating pressure is 0kPaG；The tower top operation temperature for adjusting Second distillation column T102 is 214.4 DEG C, tower
Kettle is controlled at 242.4 DEG C.
The compound-specific n-alkanes (its composition is shown in Table 3) of C12 are distillated from the tower top of Second distillation column T102, purity is greater than
99wt%, meanwhile, the tower kettle product of the overhead product of first rectifying column T101 and Second distillation column T102 are sent into diesel oil tank field.
The separation of 1-3 C13 compound-specific n-alkanes
Normal line oil after preheating is fed into first rectifying column T101 (atmospheric distillation tower) from surge tank V101, the first essence
The feed entrance point for evaporating tower T101 is that the 45th block of plate, the number of plates 60, reflux ratio 3, tower top operating pressure are from top to bottom
0kPaG；The tower top operation temperature of first rectifying column T101 is 195.1 DEG C, and tower reactor is controlled at 243.7 DEG C.
It is different less than or equal to C13 less than the n-alkane of C13 and carbon number that carbon number is distillated from the tower top of first rectifying column T101
Structure alkane (overhead product), while the tower kettle product comprising C13 n-alkane is distillated in tower reactor, which is fed into
Two rectifying column T102 (atmospheric distillation tower).The feed entrance point of Second distillation column T102 is that the 30th block of plate, the number of plates are from top to bottom
60, reflux ratio 6, tower top operating pressure is 0kPaG；The tower top operation temperature for adjusting Second distillation column T102 is 234.0 DEG C, tower
Kettle is controlled at 255.9 DEG C.
The compound-specific n-alkanes (its composition is shown in Table 4) of C13 are distillated from the tower top of Second distillation column T102, purity is greater than
99wt%, meanwhile, the tower kettle product of the overhead product of first rectifying column T101 and Second distillation column T102 are sent into diesel oil tank field.
The separation of 1-4 C14 compound-specific n-alkanes
Normal line oil after preheating is fed into first rectifying column T101 (atmospheric distillation tower) from surge tank V101, the first essence
The feed entrance point for evaporating tower T101 is that the 45th block of plate, the number of plates 60, reflux ratio 3, tower top operating pressure are from top to bottom
0kPaG；The tower top operation temperature of first rectifying column T101 is 201.9 DEG C, and tower reactor is controlled at 257.1 DEG C.
It is different less than or equal to C14 less than the n-alkane of C14 and carbon number that carbon number is distillated from the tower top of first rectifying column T101
Structure alkane (overhead product), while the tower kettle product comprising C14 n-alkane is distillated in tower reactor, which is fed into
Two rectifying column T102 (atmospheric distillation tower).The feed entrance point of Second distillation column T102 is that the 32nd block of plate, the number of plates are from top to bottom
70, reflux ratio 8, tower top operating pressure is 0kPaG；The tower top operation temperature for adjusting Second distillation column T102 is 252.3 DEG C, tower
Kettle is controlled at 272.4 DEG C.
The compound-specific n-alkanes (its composition is shown in Table 5) of C14 are distillated from the tower top of Second distillation column T102, purity is greater than
99wt%, meanwhile, the tower kettle product of the overhead product of first rectifying column T101 and Second distillation column T102 are sent into diesel oil tank field.
Embodiment 2
Using normal line oil as raw material Fischer-Tropsch hydrogeneration processes refined oil, C12 compound-specific n-alkanes therein are separated.A normal line
Oil composition is shown in Table 1, the separation according to Fig. 2 shows process progress.
It is 100 DEG C that normal line oil, which is fed into surge tank V101, and is preheated to temperature.
Normal line oil after preheating is fed into first rectifying column T101 (atmospheric distillation tower) from surge tank V101, the first essence
The feed entrance point for evaporating tower T101 is that the 30th block of plate, the number of plates 60, reflux ratio 5, tower top operating pressure are from top to bottom
0kPaG, tower top operation temperature are 185.5 DEG C, and tower reactor is controlled at 230.0 DEG C.
The isomeric alkane of n-alkane and carbon number less than or equal to C12 less than C12 is distillated from the tower top of first rectifying column T101
Hydrocarbon (overhead product), while the tower kettle product comprising C12 n-alkane is distillated in tower reactor, which is fed into third essence
Evaporate tower T103 (vacuum rectification tower).The feed entrance point of third distillation column T103 is that the 8th block of plate, the number of plates are 16 pieces from top to bottom,
Reflux ratio is 5, and tower top operating pressure is -87kPaG, and tower top operation temperature is 147.1 DEG C, and tower reactor is controlled at 170.8 DEG C.
The mixture comprising C12 n-alkane of high concentration is distillated as overhead product from the tower top of third distillation column T103
(that is, enrichment logistics), generates the n-alkane and isoparaffin (that is, tower kettle product) that carbon number is greater than C12 from tower reactor.By third
The overhead product of rectifying column T103 is fed into Second distillation column T102 (atmospheric distillation tower), the feed entrance point of Second distillation column T102
For the 20th block of plate from top to bottom, the number of plates is 40 blocks of plates, and reflux ratio 4, tower top operating pressure is 0kPaG, tower top operation temperature
It is 214.3 DEG C, tower reactor is controlled at 233.5 DEG C.
C12 compound-specific n-alkanes (its composition is shown in Table 6) is distillated from the tower top of Second distillation column T102, purity is greater than
99wt%, meanwhile, by the overhead product of first rectifying column T101, the tower kettle product of third distillation column and Second distillation column T102
Tower kettle product is sent into diesel oil tank field.
Embodiment 3
It is synchronous and respectively to be isolated by C15~C17 therein mono- using normal two wires oil as raw material Fischer-Tropsch hydrogeneration processes refined oil
Body n-alkane.Normal two wires oil composition is shown in Table 1, and the separation is carried out according to process shown in fig. 1.
It is 120 DEG C that normal two wires oil, which is fed into surge tank V101, and is preheated to temperature.
Normal two wires oil after preheating is fed into first set rectifying device in parallel (by the first essence from surge tank V101 respectively
Evaporate tower T101 and Second distillation column T102 composition), second set of rectifying device be (by first rectifying column T101 ' and Second distillation column
T102 ' composition) and third set rectifying device (being made of first rectifying column T101 " and Second distillation column T102 "), for dividing
Not isolated C15 compound-specific n-alkanes, C16 compound-specific n-alkanes and C17 compound-specific n-alkanes.
The separation of 3-1 C15 compound-specific n-alkanes
The feed entrance point of first rectifying column T101 (vacuum rectification tower) is that the 35th block of plate, the number of plates 70 are returned from top to bottom
For stream than being 5, tower top operating pressure is -50kPaG；The tower top operation temperature of first rectifying column T101 is 203.6 DEG C, tower reactor control
Temperature is 255.5 DEG C.
It is different less than or equal to C15 less than the n-alkane of C15 and carbon number that carbon number is distillated from the tower top of first rectifying column T101
Structure alkane (overhead product), while the tower kettle product comprising C15 n-alkane is distillated in tower reactor, which is fed into
Two rectifying column T102.The feed entrance point of Second distillation column T102 (vacuum rectification tower) is that the 35th block of plate, the number of plates are from top to bottom
70, reflux ratio 6, tower top operating pressure is -50kPaG；The tower top operation temperature of Second distillation column T102 is 240.9 DEG C, tower reactor
Controlled at 264.6 DEG C.
The compound-specific n-alkanes (its composition is shown in Table 7) of C15 are distillated from the tower top of Second distillation column T102, purity is greater than
99wt%, meanwhile, the tower kettle product of the overhead product of first rectifying column T101 and Second distillation column T102 are sent into diesel oil tank field.
The separation of 3-2 C16 compound-specific n-alkanes
The feed entrance point of first rectifying column T101 ' (vacuum rectification tower) is the 54th block of plate from top to bottom, the number of plates 105,
Reflux ratio is 10, and tower top operating pressure is -50kPaG；The tower top operation temperature of first rectifying column T101 ' is 218.5 DEG C, tower reactor
Controlled at 265.6 DEG C.
It is different less than or equal to C16 less than the n-alkane of C16 and carbon number that carbon number is distillated from the tower top of first rectifying column T101 '
Structure alkane (overhead product), while the tower kettle product comprising C16 n-alkane is distillated in tower reactor, which is fed into
Two rectifying column T102 '.The feed entrance point of Second distillation column T102 ' (vacuum rectification tower) is the 45th block of plate from top to bottom, the number of plates
It is 80, reflux ratio 10, tower top operating pressure is -50kPaG；The tower top operation temperature of Second distillation column T102 ' is 256.3 DEG C,
Tower reactor is controlled at 273.2 DEG C.
The compound-specific n-alkanes (its composition is shown in Table 8) of C16 are distillated from the tower top of Second distillation column T102 ', purity is greater than
99wt%, meanwhile, the tower kettle product of the overhead product of first rectifying column T101 ' and Second distillation column T102 ' are sent into diesel fuel tank
Area.
The separation of 3-3 C17 compound-specific n-alkanes
The feed entrance point of first rectifying column T101 " (vacuum rectification tower) is that the 28th block of plate, the number of plates 70 are returned from top to bottom
For stream than being 5, tower top operating pressure is -50kPaG；The tower top operation temperature of first rectifying column T101 " is 226.4 DEG C, tower reactor control
Temperature is 275.5 DEG C.
It is different less than or equal to C17 less than the n-alkane of C17 and carbon number that carbon number is distillated from the tower top of first rectifying column T101 "
Structure alkane (overhead product), while the tower kettle product comprising C17 n-alkane is distillated in tower reactor, which is fed into
Two rectifying column T102 ".The feed entrance point of Second distillation column T102 " (vacuum rectification tower) is the 36th block of plate from top to bottom, the number of plates
It is 70, reflux ratio 10, tower top operating pressure is -70kPaG；The tower top operation temperature of Second distillation column T102 " is 271.2 DEG C,
Tower reactor is controlled at 282.9 DEG C.
The compound-specific n-alkanes (its composition is shown in Table 9) of C17 are distillated from the tower top of Second distillation column T102 ", purity is greater than
99wt%, meanwhile, the tower kettle product of the overhead product of first rectifying column T101 " and Second distillation column T102 " are sent into diesel fuel tank
Area.
Embodiment 4
It is synchronous and respectively to be isolated by C18~C20 therein mono- using first vacuum side stream as raw material Fischer-Tropsch hydrogeneration processes refined oil
Body n-alkane.First vacuum side stream composition is shown in Table 1, and the separation is carried out according to process shown in fig. 1.
It is 130 DEG C that first vacuum side stream, which is fed into surge tank V101, and is preheated to temperature.
First vacuum side stream after preheating is fed into first set rectifying device in parallel (by the first essence from surge tank V101 respectively
Evaporate tower T101 and Second distillation column T102 composition), second set of rectifying device be (by first rectifying column T101 ' and Second distillation column
T102 ' composition) and third set rectifying device (being made of first rectifying column T101 " and Second distillation column T102 "), for dividing
Not isolated C18 compound-specific n-alkanes, C19 compound-specific n-alkanes and C20 compound-specific n-alkanes.
The separation of 4-1 C18 compound-specific n-alkanes
The feed entrance point of first rectifying column T101 (vacuum rectification tower) is that the 45th block of plate, the number of plates 85 are returned from top to bottom
For stream than being 6, tower top operating pressure is -70kPaG；The tower top operation temperature of first rectifying column T101 is 218.9 DEG C, tower reactor control
Temperature is 282.6 DEG C.
It is different less than or equal to C18 less than the n-alkane of C18 and carbon number that carbon number is distillated from the tower top of first rectifying column T101
Structure alkane (overhead product), while the tower kettle product comprising C18 n-alkane is distillated in tower reactor, which is fed into
Two rectifying column T102.The feed entrance point of Second distillation column T102 (vacuum rectification tower) is that the 45th block of plate, the number of plates are from top to bottom
90, reflux ratio 8, tower top operating pressure is -70kPaG；The tower top operation temperature of Second distillation column T102 is 264.6 DEG C, tower reactor
Controlled at 288.8 DEG C.
The compound-specific n-alkanes (its composition is shown in Table 10) of C18 are distillated from the tower top of Second distillation column T102, purity is greater than
99wt%, meanwhile, the tower kettle product of the overhead product of first rectifying column T101 and Second distillation column T102 are sent into diesel oil tank field.
The separation of 4-2 C19 compound-specific n-alkanes
The feed entrance point of first rectifying column T101 ' (vacuum rectification tower) is that the 42nd block of plate, the number of plates 80 are returned from top to bottom
For stream than being 6, tower top operating pressure is -70kPaG；The tower top operation temperature of first rectifying column T101 ' is 227.8 DEG C, tower reactor control
Temperature is 290.3 DEG C.
It is different less than or equal to C19 less than the n-alkane of C19 and carbon number that carbon number is distillated from the tower top of first rectifying column T101 '
Structure alkane (overhead product), while the tower kettle product comprising C19 n-alkane is distillated in tower reactor, which is fed into
Two rectifying column T102 '.The feed entrance point of Second distillation column T102 ' (vacuum rectification tower) is the 35th block of plate from top to bottom, the number of plates
It is 70, reflux ratio 8, tower top operating pressure is -70kPaG；The tower top operation temperature of Second distillation column T102 ' is 277.1 DEG C,
Tower reactor is controlled at 297.0 DEG C.
The compound-specific n-alkanes (its composition is shown in Table 11) of C19 are distillated from the tower top of Second distillation column T102 ', purity is greater than
99wt%, meanwhile, the tower kettle product of the overhead product of first rectifying column T101 ' and Second distillation column T102 ' are sent into diesel fuel tank
Area.
The separation of 4-3 C20 compound-specific n-alkanes
The feed entrance point of first rectifying column T101 " (vacuum rectification tower) is that the 35th block of plate, the number of plates 70 are returned from top to bottom
For stream than being 10, tower top operating pressure is -70kPaG；The tower top operation temperature of first rectifying column T101 " is 235.4 DEG C, tower reactor control
Temperature processed is 298.8 DEG C.
It is different less than or equal to C20 less than the n-alkane of C20 and carbon number that carbon number is distillated from the tower top of first rectifying column T101 "
Structure alkane (overhead product), while the tower kettle product comprising C20 n-alkane is distillated in tower reactor, which is fed into
Two rectifying column T102 ".The feed entrance point of Second distillation column T102 " (vacuum rectification tower) is the 40th block of plate from top to bottom, the number of plates
It is 80, reflux ratio 10, tower top operating pressure is -70kPaG；The tower top operation temperature of Second distillation column T102 " is 289.5 DEG C,
Tower reactor is controlled at 305.3 DEG C.
The compound-specific n-alkanes (its composition is shown in Table 12) of C20 are distillated from the tower top of Second distillation column T102 ", purity is greater than
99wt%, meanwhile, the tower kettle product of the overhead product of first rectifying column T101 " and Second distillation column T102 " are sent into diesel fuel tank
Area.
Embodiment 5
It is synchronous and respectively to be isolated by C21~C24 therein mono- using second line of distillation oil as raw material Fischer-Tropsch hydrogeneration processes refined oil
Body n-alkane.Second line of distillation oil composition is shown in Table 1, and the separation is carried out according to process shown in fig. 1.
It is 140 DEG C that second line of distillation oil, which is fed into surge tank V101, and is preheated to temperature.
Second line of distillation oil after preheating is fed into first set rectifying device in parallel (by the first essence from surge tank V101 respectively
Evaporate tower T101 and Second distillation column T102 composition), second set of rectifying device be (by first rectifying column T101 ' and Second distillation column
T102 ' composition), third set rectifying device (being made of first rectifying column T101 " and Second distillation column T102 ") and the 4th set of rectifying
Equipment (is made of) first rectifying column T101 " ' and Second distillation column T102 " ', just for the isolated C21 monomer of difference
Structure alkane, C22 compound-specific n-alkanes, C23 compound-specific n-alkanes and C24 compound-specific n-alkanes.
The separation of 5-1 C21 compound-specific n-alkanes
The feed entrance point of first rectifying column T101 (vacuum rectification tower) is that the 40th block of plate, the number of plates 70 are returned from top to bottom
For stream than being 6, tower top operating pressure is -80kPaG；The tower top operation temperature of first rectifying column T101 is 258.7 DEG C, tower reactor control
Temperature is 303.1 DEG C.
It is different less than or equal to C21 less than the n-alkane of C21 and carbon number that carbon number is distillated from the tower top of first rectifying column T101
Structure alkane (overhead product), while the tower kettle product comprising C21 n-alkane is distillated in tower reactor, which is fed into
Two rectifying column T102.The feed entrance point of Second distillation column T102 (vacuum rectification tower) is that the 60th block of plate, the number of plates are from top to bottom
120, reflux ratio 18, tower top operating pressure is -80kPaG；The tower top operation temperature of Second distillation column T102 is 286.1 DEG C, tower
Kettle is controlled at 308.2 DEG C.
The compound-specific n-alkanes (its composition is shown in Table 13) of C21 are distillated from the tower top of Second distillation column T102, purity is greater than
99wt%, meanwhile, the tower kettle product of the overhead product of first rectifying column T101 and Second distillation column T102 are sent into diesel oil tank field.
The separation of 5-2 C22 compound-specific n-alkanes
The feed entrance point of first rectifying column T101 ' (vacuum rectification tower) is that the 40th block of plate, the number of plates 70 are returned from top to bottom
For stream than being 6, tower top operating pressure is -80kPaG；The tower top operation temperature of first rectifying column T101 ' is 267.8 DEG C, tower reactor control
Temperature is 309.5 DEG C.
It is different less than or equal to C22 less than the n-alkane of C22 and carbon number that carbon number is distillated from the tower top of first rectifying column T101 '
Structure alkane (overhead product), while the tower kettle product comprising C22 n-alkane is distillated in tower reactor, which is fed into
Two rectifying column T102 '.The feed entrance point of Second distillation column T102 ' (vacuum rectification tower) is the 42nd block of plate from top to bottom, the number of plates
It is 86, reflux ratio 10, tower top operating pressure is -80kPaG；The tower top operation temperature of Second distillation column T102 ' is 296.2 DEG C,
Tower reactor is controlled at 316.1 DEG C.
The compound-specific n-alkanes (its composition is shown in Table 14) of C22 are distillated from the tower top of Second distillation column T102 ', purity is greater than
99wt%, meanwhile, the tower kettle product of the overhead product of first rectifying column T101 ' and Second distillation column T102 ' are sent into diesel fuel tank
Area.
The separation of 5-3 C23 compound-specific n-alkanes
The feed entrance point of first rectifying column T101 " (vacuum rectification tower) is that the 42nd block of plate, the number of plates 80 are returned from top to bottom
For stream than being 6, tower top operating pressure is -80kPaG；The tower top operation temperature of first rectifying column T101 " is 275.1 DEG C, tower reactor control
Temperature is 317.7 DEG C
It is different less than or equal to C23 less than the n-alkane of C23 and carbon number that carbon number is distillated from the tower top of first rectifying column T101 "
Structure alkane (overhead product), while the tower kettle product comprising C23 n-alkane is distillated in tower reactor, which is fed into
Two rectifying column T102 ".The feed entrance point of Second distillation column T102 " (vacuum rectification tower) is the 35th block of plate from top to bottom, the number of plates
It is 70, reflux ratio 8, tower top operating pressure is -80kPaG；The tower top operation temperature of Second distillation column T102 " is 307.5 DEG C,
Tower reactor is controlled at 325.0 DEG C.
The compound-specific n-alkanes (its composition is shown in Table 15) of C23 are distillated from the tower top of Second distillation column T102 ", purity is greater than
99wt%, meanwhile, the tower kettle product of the overhead product of first rectifying column T101 " and Second distillation column T102 " are sent into diesel fuel tank
Area.
The separation of 5-4 C24 compound-specific n-alkanes
The feed entrance point of first rectifying column T101 " ' (vacuum rectification tower) is the 40th block of plate from top to bottom, the number of plates 70,
Reflux ratio is 6, and tower top operating pressure is -80kPaG；The tower top operation temperature of first rectifying column T101 " ' is 280.0 DEG C, tower reactor
Controlled at 325.0 DEG C.
N-alkane of the carbon number less than C24 and carbon number are distillated less than or equal to C24's from the tower top of first rectifying column T101 " '
Isoparaffin (overhead product), while the tower kettle product comprising C24 n-alkane is distillated in tower reactor, which is fed into
Second distillation column T102 " '.The feed entrance point of Second distillation column T102 " ' (vacuum rectification tower) is the 48th block of plate from top to bottom, tower
Plate number is 90, reflux ratio 20, and tower top operating pressure is -80kPaG；The tower top operation temperature of Second distillation column T102 " ' is
317.2 DEG C, tower reactor is controlled at 330.8 DEG C
The compound-specific n-alkanes (its composition is shown in Table 16) of C24 are distillated from the tower top of Second distillation column T102 " ', purity is big
In 99wt%, meanwhile, the tower kettle product of the overhead product of first rectifying column T101 " and Second distillation column T102 " ' are sent into diesel oil
Tank field.
Embodiment 6
To subtract third fractional oil as raw material Fischer-Tropsch hydrogeneration processes refined oil, C25 compound-specific n-alkanes therein are separated.The line that subtracts three
Oil composition is shown in Table 1, and the separation is carried out according to process shown in fig. 1.
To subtract third fractional oil be fed into surge tank V101 be preheated to temperature be 150 DEG C.
Normal line oil after preheating is fed into first rectifying column T101 (vacuum rectification tower) from surge tank V101, the first essence
The feed entrance point for evaporating tower T101 is the 50th block of plate from top to bottom, the number of plates 100, reflux ratio 8, tower top operating pressure is-
90kPaG, tower top operation temperature are 261.1 DEG C, and tower reactor is controlled at 320.5 DEG C.
It is different less than or equal to C25 less than the n-alkane of C25 and carbon number that carbon number is distillated from the tower top of first rectifying column T101
Structure alkane (overhead product), while the tower kettle product comprising C25 n-alkane is distillated in tower reactor, which is fed into
Two rectifying column T102.The feed entrance point of Second distillation column T102 (vacuum rectification tower) is that the 35th block of plate, the number of plates are from top to bottom
70, reflux ratio 10, tower top operating pressure is -90kPaG, and tower top operation temperature is 303.4 DEG C, and tower reactor is controlled at 326.6
℃。
The compound-specific n-alkanes (its composition is shown in Table 17) of C25 are distillated from the tower top of Second distillation column T102, purity is greater than
99wt%, meanwhile, the tower kettle product of the overhead product of first rectifying column T101 and Second distillation column T102 are sent into diesel oil tank field.
Comparative example
Using the normal line oil in above-described embodiment 1 as raw material, according to being disclosed in Chinese patent application CN106699501A
Production compound-specific n-alkanes method, C11~C14 compound-specific n-alkanes in raw material are separated, wherein operating procedure
It is as follows:
Firstly, according in the patent main fractionating tower and stabilizer normal line oil is pre-processed, with the patent offer
Main fractionating tower and stabilizer operating condition separated, obtain stablize distillate oil.Main fractionating tower operating condition is as follows: pressure
0.1Mpa~0.3Mpa, 110 DEG C~140 DEG C of tower top temperature, 200 DEG C~300 DEG C of bottom temperature, 5~10 pieces of number of theoretical plate.Stablize
Tower operating condition is as follows: pressure 1.0Mpa~2.0Mpa, and 110 DEG C~140 DEG C of tower top temperature, 200 DEG C~250 DEG C of bottom temperature.
Since target product boiling point is higher, it is put into subsequent rectifying column distillate oil will be stablized to separate C11~C14 monomer N-alkanes
When hydrocarbon, be all made of the highest the top of the distillation column temperature mentioned in the example of the patent, i.e., 162 DEG C~184 DEG C, operating pressure
0.05Mpa~0.15Mpa.
As a result, it has been found that when using existing method to attempt separation C11 or more using F- T synthesis hydrofined oil as raw material
N-alkane when, the product that main fractionating tower top obtains is mainly C9~C13 paraffins mixture stream, be unable to get C14 alkane,
C14 alkane is discharged by main fractionating tower kettle and forms heavy constituent mixture.For stabilizer according to the above operating condition, tower top does not have lightweight group
Divide discharge, C9~C10 alkane light impurities before C11 alkane can not be cut off.Under subsequent rectifying column separation condition, first
The top of the distillation column product is C9~C10 paraffins mixture, and subsequent rectifying column is unable to get target production under the above operating condition
Product can not obtain the n-alkane simple substance of C11 or more always.
The composition of each F- T synthesis hydrofined oil of table 1
* the be classified as reference substance material of table 1 forms, because in actual production process, operating condition stability difference, and refined material group
At having differences, each variation range that forms is within ± 10wt%.
The composition of 2 C11 compound-specific n-alkanes of table
The composition of 3 C12 compound-specific n-alkanes of table
The composition of 4 C13 compound-specific n-alkanes of table
The composition of 5 C14 compound-specific n-alkanes of table
The composition of 6 C12 compound-specific n-alkanes of table
The composition of 7 C15 compound-specific n-alkanes of table
The composition of 8 C16 compound-specific n-alkanes of table
The composition of 9 C17 compound-specific n-alkanes of table
The composition of 10 C18 compound-specific n-alkanes of table
The composition of 11 C19 compound-specific n-alkanes of table
The composition of 12 C20 compound-specific n-alkanes of table
The composition of 13 C21 compound-specific n-alkanes of table
The composition of 14 C22 compound-specific n-alkanes of table
The composition of 15 C23 compound-specific n-alkanes of table
The composition of 16 C24 compound-specific n-alkanes of table
The composition of 17 C25 compound-specific n-alkanes of table
Claims (10)
1. a kind of method for separating C11 to C25 compound-specific n-alkanes by F- T synthesis hydrofined oil, wherein the method packet
Include following steps:
(1) the F- T synthesis hydrofined oil is fed into first rectifying column, in the removed overhead of the first rectifying column
Carbon number is less than or equal to the isomery of the subject monomers n-alkane less than the n-alkane and carbon number of subject monomers n-alkane
Alkane, and the logistics comprising the subject monomers n-alkane is obtained in the tower reactor of the first rectifying column；
(2) logistics is fed into Second distillation column from first rectifying column, in the overhead collection conduct of the Second distillation column
One of C11 to the C25 compound-specific n-alkanes of the subject monomers n-alkane；
Wherein, the quantity N relative to the expectation subject monomers n-alkane of separation simultaneously, has been arranged in parallel N and has covered described the
One rectifying column and the Second distillation column, first rectifying column and the Second distillation column described in every set are for separating the target list
One of body n-alkane.
2. the method for claim 1, wherein the F- T synthesis hydrofined oil is achieved in that and makes to come at one's own expense
The Fischer-Tropsch synthetic of support synthesis unit enters hydrofinishing unit and carries out hydrotreating, the atmospheric fractional tower side line collected
Product and/or vacuum fractionation tower side line product are as the F- T synthesis hydrofined oil.
3. method according to claim 1 or 2, wherein the F- T synthesis hydrofined oil is selected from: as the normal pressure point
Evaporate normal line oil, the normal two wires oil of tower side line product, and/or as the vacuum fractionation tower side line product first vacuum side stream, subtract
Two wires oil subtracts third fractional oil.
4. method as claimed in any one of claims 1-3, wherein, will be described before being fed to the first rectifying column
F- T synthesis hydrofined oil is fed into surge tank and is preheated, the F- T synthesis hydrofined oil after being preheated；
Preferably, the F- T synthesis hydrofined oil is preheated to 100 DEG C~150 DEG C.
5. such as method of any of claims 1-4, wherein in the step (1), the first rectifying column is normal
Press rectifying column or vacuum rectification tower；
Preferably, the feed entrance point of the first rectifying column is at 2/5~3/4 from top to bottom of column plate therein；
Additionally preferably, the number of plates of the first rectifying column be 40~120, reflux ratio be 3~10, tower top operating pressure be-
100kPaG~10kPaG, tower top operation temperature are 145 DEG C~285 DEG C, and tower reactor is controlled at 205 DEG C~325 DEG C；
It is further preferred that the number of plates of the first rectifying column is 60~105, reflux ratio is 3~10, tower top operating pressure
For -90kPaG~0kPaG, tower top operation temperature is 165 DEG C~280 DEG C, and tower reactor is controlled at 215 DEG C~325 DEG C.
6. method according to any one of claims 1 to 5, wherein in the step (2), the Second distillation column is normal
Press rectifying column or vacuum rectification tower；
Preferably, the feed entrance point of the Second distillation column is at 9/20~9/16 from top to bottom of column plate therein；
Additionally preferably, the number of plates of the Second distillation column be 40~120, reflux ratio be 4~20, tower top operating pressure be-
100kPaG~10kPaG, tower top operation temperature are 170 DEG C~330 DEG C, and tower reactor is controlled at 210 DEG C~335 DEG C；
It is further preferred that the number of plates of the Second distillation column is 40~120, reflux ratio is 4~20, tower top operating pressure
For -90kPaG~0kPaG, tower top operation temperature is 190 DEG C~320 DEG C, and tower reactor is controlled at 225 DEG C~335 DEG C.
7. such as method of any of claims 1-6, wherein in the step (2), by the logistics from described the
One rectifying column is fed into the third distillation column being further disposed between the first rectifying column and Second distillation column, described
The tower top of three rectifying columns obtains enrichment logistics, and the enriched substance stream is fed into the Second distillation column.
8. the method for claim 7, wherein the carbon number generated in the tower reactor of the third distillation column is greater than the mesh
Mark the tower kettle product of the n-alkane and isoparaffin of compound-specific n-alkanes as the third distillation column.
9. method as claimed in claim 7 or 8, wherein the third distillation column is atmospheric distillation tower or vacuum rectification tower；
Preferably, the feed entrance point of the third distillation column is at 2/5~3/5 from top to bottom of column plate therein；
Additionally preferably, the number of plates of the third distillation column be 10~80 pieces, reflux ratio be 3~10, tower top operating pressure be-
90kPaG~0kPaG, tower top operation temperature are 120 DEG C~180 DEG C, and tower reactor is controlled at 150 DEG C~195 DEG C；
It is further preferred that the number of plates of the third distillation column is 10~20 pieces, reflux ratio is 3~7, tower top operating pressure
For -90kPaG~-80kPaG, tower top operation temperature is 130 DEG C~150 DEG C, and tower reactor is controlled at 160 DEG C~175 DEG C.
10. method as claimed in any one of claims 7-9, wherein the method further includes by first rectifying
The tower kettle product of the overhead product of tower, the tower kettle product of the third distillation column and/or the Second distillation column is sent to oil product tank
Area.
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| CN111996036A (en) * | 2020-08-20 | 2020-11-27 | 北京明星绿能化工科技有限公司 | Preparation equipment and preparation method of series of high phase-change enthalpy value phase-change waxes |
| CN112289477A (en) * | 2020-09-03 | 2021-01-29 | 中国原子能科学研究院 | Diluent and isomerization preparation method and composition thereof |
| CN112391198A (en) * | 2020-10-30 | 2021-02-23 | 中国科学院山西煤炭化学研究所 | Method for continuously separating high-purity n-alkane |
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| CN112289477B (en) * | 2020-09-03 | 2023-08-18 | 中国原子能科学研究院 | Diluent and isomerization preparation method and composition thereof |
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Address after: 101407 Zhongke synthetic oil R & D base, No. 1, south 2nd Street, Yueyuan, C District, Yanqi Development Zone, Huairou District, Beijing Patentee after: Zhongke synthetic oil Technology Co.,Ltd. Address before: 101407 Zhongke synthetic oil R & D base, No. 1, south 2nd Street, Yueyuan, C District, Yanqi Development Zone, Huairou District, Beijing Patentee before: SYNFUELS CHINA TECHNOLOGY Co.,Ltd. |