CN109694299A - Using Aromatic raffinate as the method for raw materials for ethylene production - Google Patents
Using Aromatic raffinate as the method for raw materials for ethylene production Download PDFInfo
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- CN109694299A CN109694299A CN201710984489.4A CN201710984489A CN109694299A CN 109694299 A CN109694299 A CN 109694299A CN 201710984489 A CN201710984489 A CN 201710984489A CN 109694299 A CN109694299 A CN 109694299A
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- 238000000034 method Methods 0.000 title claims abstract description 75
- 125000003118 aryl group Chemical group 0.000 title claims abstract description 63
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000005977 Ethylene Substances 0.000 title claims abstract description 44
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 239000002994 raw material Substances 0.000 title claims abstract description 13
- 239000003381 stabilizer Substances 0.000 claims abstract description 70
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 60
- 239000000463 material Substances 0.000 claims abstract description 46
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 238000005336 cracking Methods 0.000 claims abstract description 13
- 238000000926 separation method Methods 0.000 claims abstract description 13
- 238000012545 processing Methods 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims description 42
- 150000001336 alkenes Chemical class 0.000 claims description 31
- 239000001257 hydrogen Substances 0.000 claims description 26
- 229910052739 hydrogen Inorganic materials 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 25
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 23
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims description 21
- 239000007791 liquid phase Substances 0.000 claims description 20
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 15
- 230000003068 static effect Effects 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 229910052573 porcelain Inorganic materials 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 230000008676 import Effects 0.000 claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- 230000006641 stabilisation Effects 0.000 claims description 6
- 238000011105 stabilization Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229910000510 noble metal Inorganic materials 0.000 claims description 4
- 150000002431 hydrogen Chemical class 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 244000000626 Daucus carota Species 0.000 claims description 2
- 235000005770 birds nest Nutrition 0.000 claims description 2
- 235000005765 wild carrot Nutrition 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 238000004140 cleaning Methods 0.000 abstract description 7
- 239000000571 coke Substances 0.000 abstract description 7
- 239000002010 green coke Substances 0.000 abstract description 3
- 238000004904 shortening Methods 0.000 abstract 1
- 230000008569 process Effects 0.000 description 14
- 229930195733 hydrocarbon Natural products 0.000 description 9
- 239000004215 Carbon black (E152) Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 150000002430 hydrocarbons Chemical class 0.000 description 7
- 238000001833 catalytic reforming Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- 238000004939 coking Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910000480 nickel oxide Inorganic materials 0.000 description 3
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 3
- 238000000197 pyrolysis Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 230000005526 G1 to G0 transition Effects 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- -1 alkene Hydrocarbon Chemical class 0.000 description 2
- 150000001924 cycloalkanes Chemical class 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000004230 steam cracking Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910018879 Pt—Pd Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C4/00—Preparation of hydrocarbons from hydrocarbons containing a larger number of carbon atoms
- C07C4/02—Preparation of hydrocarbons from hydrocarbons containing a larger number of carbon atoms by cracking a single hydrocarbon or a mixture of individually defined hydrocarbons or a normally gaseous hydrocarbon fraction
- C07C4/04—Thermal processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/0292—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds with stationary packing material in the bed, e.g. bricks, wire rings, baffles
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of using Aromatic raffinate as the method for raw materials for ethylene production.This method comprises: Aromatic raffinate enters hydrogenator, hydrogenation reaction effluent is passed through stabilizer and carries out gas-liquid separation processing, and then materials at bottom of tower is passed through ethylene cracker；Setting cross-line is for being introduced directly into stabilizer for Aromatic raffinate when hydrogenator is isolated with stabilizer, ethylene cracker；Leakproof pipeline is set, and leakproof pipeline one end is connected to cross-line, and the other end is connected to stabilizer bottoming cycle pump discharge pipeline.The method of the present invention can slow down cracking furnace pipe green coke rate, extend coke cleaning period, guarantee the stable operation of ethylene cracker, and solve the problems, such as that the hydrotreater product quality caused by initial stage that goes into operation is not up to standard, effectively solves the problems, such as that product caused by cross-line valves leakage is unqualified or shortening device operation cycle.
Description
Technical field
The present invention relates to a kind of methods for producing ethylene, and specifically one kind is using Aromatic raffinate as raw materials for ethylene production
Method.
Background technique
Aromatics Extractive Project is the important process technology that aromatic hydrocarbons is purified in petroleum refining process, and main purpose is from catalytic reforming
Or BTX(benzene, toluene, dimethylbenzene are isolated in hydrogenated pyrolysis gasoline).Extraction process is good with aromatics quality, the rate of recovery is high and former
Material has the features such as adaptability is good, and raffinates oil and be substantially free of aromatic hydrocarbons, is rich in alkane, and contain part cycloalkane and a small amount of alkene
Hydrocarbon is good ethylene cracking material.
In recent years, with the continuous expansion of China's ethylene production scale, ethylene raw problem in short supply becomes increasingly conspicuous, this is tight
The national economic development and the raising of Business Economic Benefit are constrained again.Aromatic raffinate is produced 6# or 120# solvent by certain enterprises
Oil, the enterprise also having is used as motor petrol blend component, since Aromatic raffinate research octane number (RON) (RON) is lower, as vehicle
It is restricted when with gasoline blend component.Therefore, it is having of increasing economic efficiency that Aromatic raffinate, which does ethylene cracker raw material,
One of efficacious prescriptions method, but the relevant report at present about production ethylene cracking material is less.
CN1621497A discloses a kind of naphtha recombinant processing method, and its step are as follows: (1) first extracting naphtha
Separation is taken, isolates and raffinates oil and extract out oil；(2) it raffinates oil into Ethylene vapor cracker；(3) extraction oil enters reformer
It reforms.Aromatic production can be improved 30% or more by this method, and ethylene yield improves 40% or more.
103374395 A of CN discloses a kind of method for producing aromatic hydrocarbons and ethylene as raw material using naphtha, including walks as follows
Rapid: (1) in presence of hydrogen, by naphtha in 0.15~3.0MPa, 300~540 DEG C, volume space velocity is 2.1~50h-1Item
It is contacted in catalytic reforming zone with reforming catalyst under part and carries out either shallow catalytic reforming reaction, make the cycloalkanes rate in naphtha
Greater than 85 mass %, paraffin conversion is aromatic hydrocarbons and C4-The conversion ratio of hydrocarbon is less than 30 mass %；(2) catalytic reforming is obtained
Reformed oil carries out aromatics seperation in the first aromatics seperation area, obtains the fraction rich in aromatic hydrocarbons and the fraction rich in alkane；
(3) liquefied gas that the fraction and catalytic reforming that will be enriched in alkane generate is sent into steam cracking area and carries out cracking reaction production second
Alkene.The method can make full use of naphtha maximumlly to produce ethylene while producing aromatic hydrocarbons by either shallow catalytic reforming.
But the above method is easy coking in cracking furnace pipe, causes to split when carrying out producing ethylene by cracking to Aromatic raffinate
It solves energy consumption to increase, yield of ethene decline, and blowing out coke cleaning period is short, and can shorten the service life of boiler tube and refractory brick.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of using Aromatic raffinate as the method for raw materials for ethylene production.
This method can not only slow down cracking furnace pipe green coke rate, extend coke cleaning period, guarantee the stable operation of ethylene cracker, and
It effectively solves the problems, such as that product caused by cross-line valves leakage is unqualified or device operation cycle shortens, and solves and add at hydrogen
Reason device goes into operation the problem not up to standard of product quality caused by initial stage.
The present invention provides a kind of using Aromatic raffinate as the method for raw materials for ethylene production, this method comprises: aromatic hydrocarbons raffinate
Oil enters hydrogenator, carries out hydrogenation reaction under the conditions of existing for the Hydrobon catalyst, hydrogenation reaction effluent is passed through
Stabilizer carries out gas-liquid separation processing, and then materials at bottom of tower is passed through ethylene cracker, carries out cracking reaction and produces ethylene；
Setting cross-line is for being introduced directly into stabilizer for Aromatic raffinate, cross-line is when hydrogenator is isolated with stabilizer
Connecting pipeline between pipeline before hydrogenator entrance is set and stabilizer import；
Leakproof pipeline is set, and leakproof pipeline one end is connected to cross-line, and the other end is connected to stabilizer bottoming cycle pump discharge pipeline, is prevented
First valve is set on fistulae line；The cross-line two sides of cross-line and leakproof pipeline communicating position are respectively arranged with the second valve, third
Valve；When normal operation, at least one of valve in the second valve, third valve is closed, preferably by the second valve, third
Valve is turned off, and the first valve is in the open state, in leakproof pipeline liquid phase pressure be higher than cross-line in pressure, preferably higher than across
Liquid phase pressure 0.1 MPa~0.3 MPa in line.
In the method for the present invention, when hydrogenator goes into operation, Aromatic raffinate is introduced into stabilizer, then by stabilizer
Materials at bottom of tower is introduced into hydrogenator and carries out hydrogenation reaction, and hydrogenation reaction effluent is passed through stabilizer 5 minutes~24 hours,
Preferably 1~10 hour, stop that Aromatic raffinate is passed directly into stabilizer and stops introducing the materials at bottom of tower of stabilizer to add
Aromatic raffinate is introduced directly into hydrogenator by hydrogen reactor, carries out normal hydrogenation process.
In the method for the present invention, hydrogenation reaction is reacted using liquid-phase hydrogenatin, i.e., at reaction conditions, Aromatic raffinate at least 80
Wt% keeps liquid phase state, it is further preferred that Aromatic raffinate at least 90 wt% keep liquid phase state.
In the method for the present invention, the tower bottom reboiler of stabilizer setting provides heat source for stabilizer, introduces hydrogenator
Stablize materials at bottom of tower to draw after tower bottom reboiler, it is preferable that the stabilization materials at bottom of tower drawn after tower bottom reboiler
Temperature is 100 DEG C~240 DEG C.
In the method for the present invention, device for transporting objects (can be delivery pump) be arranged in the tower bottom of stabilizer, is conveyed by material
The material that stabilizer tower bottom exports is delivered to the pipeline before hydrogenator entrance by device.
In the method for the present invention, First Heat Exchanger, gas are disposed with along flow direction on entering the pipeline before hydrogenator
Liquid mixer and the second heat exchanger, for heating Aromatic raffinate, air and liquid mixer is used for will for First Heat Exchanger, the second heat exchanger
Hydrogen and Aromatic raffinate are sufficiently mixed, and air and liquid mixer is preferably static mixer or dynamic mixer, static mixing
It is mixed that device is selected from SV type static mixer, SK type static mixer, SX type static mixer, SH type static mixer, SL type static state
One of clutch or several combinations, dynamic mixer it is a kind of in mixing pump, overcritical mixer, mixer or
Several combinations of person.
In the method for the present invention, the pipeline connecting with the first import of First Heat Exchanger is provided with the 4th valve.
In the method for the present invention, the outlet of stabilizer materials at bottom of tower is connected with reboiler, and the material outlet and gas-liquid of reboiler are mixed
The inlet ductwork of clutch connects, and is equipped with the 5th valve on pipeline.
In the method for the present invention, the second import of the tower bottom export pipeline and First Heat Exchanger of stabilizer is connected.
In the method for the present invention, hydrogen needed for hydrogenator is used from PSA(pressure-variable adsorption) hydrogen of unit discharge.
Be disposed with from bottom to top in the method for the present invention, above catalyst bed metal mesh and/or the first metallic grid,
The wall body of two layers or more the porcelain ball that partial size becomes larger, hydrogenator is arranged on metal mesh and/or the first metallic grid
Agent mouth is unloaded on having；
Metal mesh and/or the second metallic grid, partial size become larger two are disposed with below catalyst bed from the top down
Layer or more porcelain ball, Bird's Nest proppant, third metallic grid, the wall body of hydrogenator is in metal mesh and/or the second metallic grid
It is provided with down between third metallic grid and unloads agent mouth；
The wall body of hydrogenator unloads agent mouth in catalyst bed layer region is provided with.
In the method for the present invention, reaction mass enters from hydrogenator bottom carries out hydrogenation reaction in hydrogenator.
In the method for the present invention, the operating condition of hydrogenation reaction is as follows: reaction pressure is the MPa of 0.5 MPa~6.0, preferably
The MPa of 1.2 MPa~3.0；Reaction temperature is 100 DEG C~240 DEG C, preferably 140 DEG C~200 DEG C；Volume space velocity is 1.0 when liquid
h-1~12. 0h-1, preferably 4.0 h-1~8.0 h-1；Hydrogen to oil volume ratio is 20:1 hereinafter, preferably 2:1~5:1.The present invention
In method, hydrogen to oil volume ratio can be substantially reduced compared with existing conventional method.
In the method for the present invention, the Hydrobon catalyst used can be commodity Hydrobon catalyst, such as with noble metal
Or reduced state nickel is the Hydrobon catalyst of active component, such catalyst hydrogenation activity with higher can be mutually
Hydrogenation reaction is carried out at lower temperature.It is preferred that the Hydrobon catalyst using noble metal as active component is used, such as Fushun stone
The HDO-18 catalyst of oily chemical research institute's development and production.Noble metal hydrogenation catalyst for refining generally using aluminium oxide as carrier, with
Pt and/or Pd be active component, the content of active component by weight in the catalyst be not less than 0.1%, generally 0.1%~
1.5%.For using reduced state nickel as the Hydrobon catalyst of active component, generally using aluminium oxide or modified aluminas as carrier,
Using nickel oxide as active component (account for catalyst weight with nickel oxide poidometer 15%~70%, preferably 25%~45%),
Reduction activation is being carried out to catalyst using preceding, reduction-state is being converted by nickel oxide, to improve catalyst hydrogenation activity.To virtue
Hydrocarbon is raffinated oil for feedstock, Aromatic raffinate alkene can be made to be less than 0.5wt% using the Hydrobon catalyst, met
The charging index request of subsequent ethylene cracker.
In the method for the present invention, at the initial stage of going into operation, the materials at bottom of tower of stabilizer is partly or entirely passed through hydrogenator.
In the method for the present invention, the arene content of Aromatic raffinate is less than 2wt%, it is preferable that is less than 1wt%, olefin(e) centent is small
In 6 wt%.
In the method for the present invention, Aromatic raffinate can be taken out for the Aromatic raffinate of reformate and/or the aromatic hydrocarbons of drippolene
Excess oil.
In the method for the present invention, ethylene cracker can use ethylene cracker commonly used in the art, in routine
Under the conditions of carry out cracking reaction produce ethylene.
Compared with prior art, advantageous effects of the invention are as follows:
(1) if the slightly interior leakage of cross-line valve, the materials at bottom of tower olefin(e) centent of stabilizer will obviously rise, and valves leakage is
Relatively universal, more difficult discovery is difficult to the problem eradicated completely, if being intended to thoroughly solve valves leakage, need to pay higher cost.This hair
In bright, ingenious to use leakproof pipeline designs, in conjunction with the actual features of the device, i.e. stabilizer bottoming cycle pump discharge pressure compares cross-line
Pressure is slightly higher, after introducing leakproof pipeline, pressure in a little higher than cross-line of liquid phase pressure in leakproof pipeline, in this state, even if
On cross-line valve slightly in leakage and leakproof pipeline in material leakage enter hydrogenator or leak into stabilizer because
It is low-down that material, which is the olefin(e) centent by hydrotreating, in material, in leakproof pipeline, therefore leakage not shadow in which kind of
The properties such as olefin(e) centent after ringing hydrotreating, ingenious solve material olefin(e) centent caused by valves leakage and will obviously rise
The problem of.The method of the present invention is skillfully constructed, it is easy to accomplish, maintenance cost is low, is conducive to device long period steady running.
(2) the method for the present invention, the method that Aromatic raffinate is handled by liquid-phase hydrogenatin remove unsaturated olefin therein,
In Aromatic raffinate hydroprocessing processes, the alkene of Aromatic raffinate can be reduced to 0.1wt% by 6wt% or so, then again will
Its raw material as ethylene cracker substantially extends coke cleaning period to slow down cracking furnace pipe coking rate, to guarantee second
The stable operation of alkene cracker.
At the initial stage of going into operation, Aromatic raffinate is introduced into stabilizer and carries out gas-liquid separation processing, then by the tower bottom of stabilizer
Material is introduced into hydrogenator, carries out hydrogenation reaction, and hydrogenation effluent enters stabilizer and carries out gas-liquid separation processing, so both
It can guarantee initial production quality requirement, avoid product unqualified stationary phase, and the tower bottom reboiler that can use stabilizer is fast
Speed heating Aromatic raffinate, reaches the temperature requirement of hydrogenation reaction, without increasing additional heater, and overcomes heat exchange
The device disadvantage slow in the initial stage heat exchange unstability that goes into operation, heating, and subsequent normal hydogenation reaction process is not influenced.
(3) for the ethylene cracker of oil refining enterprise, a hydrogenator need to only be increased, it is not necessary to individually newly-built
A set of hydrogenation reaction device, hydrogen use the high-purity hydrogen introduced from PSA unit, eliminate new hydrogen machine, circulating hydrogen compressor
The hydrogen mixed effect of air and liquid mixer can be improved instead of fractionating column etc. dynamic equipment, and using stabilizer, improve reactive hydrogen
Partial pressure facilitates hydrogenation and olefin hydrocarbon removal reaction, while can reduce stabilizer top load, reduces stabilizer investment；It raffinates oil raw material
Oil heat exchange is generated with product stabilizer bottom, saves heating furnace.For the present invention by above-mentioned process optimization, operating condition is more slow
With exploitativeness is strong, and investment and operating cost can be greatly lowered.
(4) hydrogenator of the present invention uses up flow type mode of operation, reactor head and bottom equipped with metal mesh and/or
The problem of metallic grid can play fixed catalyst bed, prevent catalyst and porcelain ball from running leakage, on this basis, is being catalyzed
It is provided with metal mesh and/or metallic grid between agent and the porcelain ball of multilayer different-grain diameter, catalyst is further prevented to go out with porcelain ball
Existing air-teturning mixed phenomenon thoroughly solves the problems, such as that hydrogenation catalyst runs leakage and hydrogenation catalyst and porcelain ball back-mixing, while adding hydrogen anti-
Answer device be equipped with again unload agent mouth, in unload agent mouth, under unload agent mouth, draw off porcelain ball and catalyst respectively in this way, avoid and unload
The later separation of porcelain ball and catalyst out.
(5) the method for the present invention process flow is simple, and equipment investment is lower, and maintenance cost is lower, is conducive to downstream ethylene dress
Set long period steady running.
Detailed description of the invention
Fig. 1 is of the invention using Aromatic raffinate as the combination unit schematic diagram of raw materials for ethylene production；
Wherein: 1- surge tank, 2- First Heat Exchanger, 3- air and liquid mixer, the second heat exchanger of 4-, 5- hydrogenator, 6- stablize
Tower, 7- reboiler, 8- ethylene cracker, 9-PSA unit, the first valve of 10-, the second valve of 11-, 12- third valve, 13-
4th valve, the 5th valve of 14-.
Specific embodiment
The method of the present invention is described in detail in the following with reference to the drawings and specific embodiments.
As shown in Figure 1, when present invention setting cross-line is used to for hydrogenator being isolated with stabilizer 6, by Aromatic raffinate
It is introduced directly into stabilizer 6, cross-line is the communicating pipe being arranged between 6 import of the pipeline before hydrogenator enters 5 mouthfuls and stabilizer
Line；Leakproof pipeline is set, and leakproof pipeline one end is connected to cross-line, and the other end is connected to 6 circulating-pump outlet pipeline of stabilizer bottom, is prevented
First valve 10 is set on fistulae line；The cross-line two sides of cross-line and leakproof pipeline communicating position be respectively arranged with the second valve 12,
Third valve 12；When normal operation, at least one valve in the second valve 11, third valve 12 is closed, preferably by the
Two valves 11, third valve 12 are turned off, and the first valve 10 is in the open state, and liquid phase pressure is higher than in cross-line in leakproof pipeline
Pressure, liquid phase pressure 0.1 MPa~0.3 MPa preferably higher than in cross-line.Due to 6 circulating-pump outlet pressure ratio of stabilizer bottom across
Line pressure is slightly higher, though on cross-line valve slightly in leakage and leakproof pipeline material pass through the valve that leaks and enter and add
Hydrogen reactor 5 enters stabilizer 6, because material is that the olefin(e) centent by hydrotreating, in material is in leakproof pipeline
It is low-down, therefore leakage does not influence the properties such as the olefin(e) centent after hydrotreating in which kind of, the ingenious valves leakage that solves draws
The problem of material olefin(e) centent risen will obviously rise.
The hydrogenation reaction of Aromatic raffinate uses the new device of the method for the present invention, when hydrogenator 5 brings into operation,
Aromatic raffinate is introduced into surge tank 1, closes the first valve 10, the 4th valve 13, opens the second valve 11, third valve 12,
Aromatic raffinate is directly entered stabilizer 6, and the materials at bottom of tower of stabilizer 6 enters reboiler 7 and is heated to reaction required temperature, beats
The 5th valve 14 is opened, is passed through First Heat Exchanger 2 by the material that reboiler 7 heats, it is then mono- by air and liquid mixer 3 and PSA
The high concentration of hydrogen gas that 9 conveying of member comes is sufficiently mixed, using the second heat exchanger 4 after mixing, then from hydrogenator 5
Bottom enter, contacted with Hydrobon catalyst, hydrogenation reaction carried out under conditions of hydrogenation reaction, is made in Aromatic raffinate
Alkene saturation, after reaction, hydrogenation reaction effluent enters stabilizer 6 and carries out gas-liquid separation, and tower top obtains light dydrocarbon or less
Lighter hydrocarbons, and materials at bottom of tower is fully incorporated hydrogenator 5 in advance, and the later period can partially be passed through ethylene cracker 8, then carry out
Cracking.
After hydrogenator 5 enters nominal situation, opening the first valve 10, the 4th valve 13, the second valve 11 of closing,
Third valve 12 and the 5th valve 14, hydrogenation reaction part enter the normal technological process of production, and this flexible process flow is kept away
The initial production unqualified stationary phase that goes into operation is exempted from.The normal technological process of production are as follows: Aromatic raffinate enters hydrogenator 5,
Hydrobon catalyst exists, carries out adding hydrogen under conditions of liquid phase state (Aromatic raffinate at least 80 wt% keep liquid phase state)
Reaction, hydrogenation reaction effluent are passed through stabilizer 6 and carry out gas-liquid separation processing, and then materials at bottom of tower is passed through ethylene cracker 8.
By the Aromatic raffinate that the method for the present invention is handled, olefin(e) centent can be reduced to 0.1wt%, can slow down pyrolysis furnace
Pipe green coke rate extends coke cleaning period, guarantees the stable operation of ethylene cracker 8.
The following examples illustrate the present invention further.
Experiment is the catalyst for hydrogenation of industrial application using catalyst, is Fushun Petrochemical Research Institute's development and production
HDO-18 hydrogenation catalyst, physicochemical property index is shown in Table 1.
The physicochemical property index of 1 catalyst of table
| Catalyst number | HDO-18 |
| Metal composition | Pt-Pd |
| Physical property | |
| Kong Rong, mL/g | ≥0.45 |
| Specific surface area, m2/g | ≥170 |
| Compressive resistance, N/cm | ≥90 |
| Shape | Cylinder bar shaped |
Embodiment 1
New device as shown in Figure 1.Aromatic raffinate is by feed pump, First Heat Exchanger 2 and hydrogen in SX type static mixer
In be sufficiently mixed dissolution after, then after the heat exchange of the second heat exchanger 4, enter from the bottom of hydrogenator 5, be catalyzed with hydrofinishing
Agent contact, hydrogenation reaction is carried out under conditions of hydrogenation reaction, is saturated the alkene in Aromatic raffinate, Aromatic raffinate is liquid
Phase state.After reaction, hydrogenation reaction effluent enters the progress gas-liquid separation of stabilizer 6, and it is below light that tower top obtains light dydrocarbon
Hydrocarbon, and materials at bottom of tower is passed through ethylene cracker 8, is then cracked.Alkene before and after hydrogenation reaction in Aromatic raffinate
Content is listed in table 2.
The processing that goes into operation is carried out to hydrogenation plant using the method for the present invention, when going into operation, Aromatic raffinate is first introduced into stabilization
Tower 6 carries out gas-liquid separation, the materials at bottom of tower (temperature for the 6 substrate material of stabilizer drawn after tower bottom reboiler 7 of stabilizer 6
It is 168 DEG C) it is first fully incorporated hydrogenator 5, rear portion is separated into hydrogenator 5, hydrogenation reaction is carried out, in hydrogenation reaction stream
After object enters stabilizer 5 hours out, stop the materials at bottom of tower for introducing stabilizer 6, and stops directly being passed through aromatic hydrocarbons to stabilizer 6
It raffinates oil, is switched to normal operating process.
Liquid phase pressure is higher than pressure 0.2MPa in cross-line in leakproof pipeline.
As can be seen from Table 2, the alkene of Aromatic raffinate can be made using the technology in hydrogenation reaction device normal operating
Hydrocarbon content is reduced to 0.1wt%, and entire start-up process product quality also keeps stable.
Embodiment 2
New device as shown in Figure 1.Aromatic raffinate is by feed pump, First Heat Exchanger 2 and hydrogen in SX type static mixer
In be sufficiently mixed dissolution after, then after the heat exchange of the second heat exchanger 4, enter from the bottom of hydrogenator 5, be catalyzed with hydrofinishing
Agent contact, hydrogenation reaction is carried out under conditions of hydrogenation reaction, is saturated the alkene in Aromatic raffinate, Aromatic raffinate is liquid
Phase state.After reaction, hydrogenation reaction effluent enters the progress gas-liquid separation of stabilizer 6, and it is below light that tower top obtains light dydrocarbon
Hydrocarbon, and materials at bottom of tower is passed through ethylene cracker 8, is then cracked.Alkene before and after hydrogenation reaction in Aromatic raffinate
Content is listed in table 2.
The processing that goes into operation is carried out to hydrogenation plant using the method for the present invention, when going into operation, Aromatic raffinate is first introduced into stabilization
Tower 6 carries out gas-liquid separation, the materials at bottom of tower (temperature for the 6 substrate material of stabilizer drawn after tower bottom reboiler 7 of stabilizer 6
It is 173 DEG C) it is first fully incorporated hydrogenator 5, rear portion is separated into hydrogenator 5, hydrogenation reaction is carried out, in hydrogenation reaction stream
After object enters stabilizer 5 hours out, stop the materials at bottom of tower for introducing stabilizer 6, and stops directly being passed through aromatic hydrocarbons to stabilizer 6
It raffinates oil, is switched to normal operating process.
Liquid phase pressure is higher than pressure 0.2MPa in cross-line in leakproof pipeline.
As can be seen from Table 2, the alkene of Aromatic raffinate can be made using the technology in hydrogenation reaction device normal operating
Hydrocarbon content is reduced to 0.1wt%, and entire start-up process product quality also keeps stable.
Comparative example 1
This comparative example 1 and the method for the embodiment of the present invention 1 are essentially identical, and difference is: not having hydrogenation process, reformate
Raffinate oil and be heated to cracking of ethylene required temperature after, the steam cracking furnace that is passed directly into ethylene cracker.
Comparative example 2
According to the scheme of embodiment 1, only when going into operation, raffinating oil for reformate is directly entered hydrogenator, directly carries out
Normal operating.In start-up process, hydrogenation reaction product has about 30 hours to be higher than 0.5wt%.
The process conditions and measurement result of 2 hydrogenation reaction of table
| Project | Embodiment 1 | Embodiment 2 | Comparative example 1 |
| Aromatic raffinate raw material | |||
| Arene content, wt% | 0.8 | 0.7 | 0.8 |
| Olefin(e) centent, wt% | 4.8 | 5.0 | 4.8 |
| The process conditions of hydrogenator | |||
| Reaction temperature, DEG C | 168 | 173 | - |
| Reaction pressure, MPa | 1.5 | 1.7 | - |
| Volume space velocity when liquid, h-1 | 5.7 | 6.5 | - |
| Oil property | |||
| Go into operation initial stage, after hydrogenation reaction in olefin(e) centent, wt% | < 0.5 | < 0.5 | - |
| Normal operating, the olefin(e) centent in Aromatic raffinate after hydrogenation reaction, wt% | 0.1 | 0.1 | - |
| Ethylene cracker | |||
| Heater outlet temperature, DEG C | 840 | 840 | 840 |
| Residence time, s | 0.5 | 0.5 | 0.5 |
| Outlet of still pressure, kPa | 50 | 50 | 50 |
| The cycle of operation, day | 90 | 90 | 42 |
| Yield of ethene, wt% | 32.7 | 33.2 | 32.0 |
By the Aromatic raffinate that the method for the present invention is handled, product can achieve following property: go into operation the stage, refined oil (adds hydrogen
Aromatic raffinate after reaction) olefin(e) centent is less than 0.5wt%, and when normal operating, refined oil olefin(e) centent can be down to 0.1wt%.
For system of the invention when running 90 days, yield of ethene fall is smaller, and the 1 ethylene cracker cycle of operation of comparative example is only
It is 42 days, coking is serious in pyrolysis furnace.Therefore, the coke cleaning period of the embodiment of the present invention 1 and 2 can be 90 days, and compare
The coke cleaning period of example 1 is 42 days.
Embodiment 3
During trial run, the second valve 11, the third valve 12 on cross-line are opened, and make the second valve 11, third valve
12 keep very little aperture, simulate valves leakage operating condition, when not enabling leakproof pipeline (not opening the first valve 10), hydrogenation reaction
Olefin(e) centent in effluent is greater than 0.5wt%, and after enabling leakproof pipeline (opening the first valve 10), hydrogenation reaction effluent
Olefin(e) centent stablize, down to 0.1wt%.
By calculating, under certain operating conditions, when catalyst performance is good (product index is far below Con trolling index), if
There is 10% interior leakage, the olefin(e) centent in hydrogenation reaction effluent is greater than 0.5wt%；Later period (hydrogenation reaction stream is used in catalyst
For the olefin(e) centent in object close to 0.5wt%), slightly interior leakage will be higher than 0.5wt% out.
Claims (16)
1. a kind of using Aromatic raffinate as the method for raw materials for ethylene production, it is characterised in that this method comprises: Aromatic raffinate into
Enter hydrogenator, carries out hydrogenation reaction under the conditions of existing for the Hydrobon catalyst, hydrogenation reaction effluent is passed through stabilization
Tower carries out gas-liquid separation processing, and then materials at bottom of tower is passed through ethylene cracker, carries out cracking reaction and produces ethylene；
Setting cross-line is for being introduced directly into stabilizer for Aromatic raffinate, cross-line is when hydrogenator is isolated with stabilizer
Connecting pipeline between pipeline before hydrogenator entrance is set and stabilizer import；
Leakproof pipeline is set, and leakproof pipeline one end is connected to cross-line, and the other end is connected to stabilizer bottoming cycle pump discharge pipeline, is prevented
First valve is set on fistulae line；The cross-line two sides of cross-line and leakproof pipeline communicating position are respectively arranged with the second valve, third
Valve；When normal operation, at least one of valve in the second valve, third valve to be closed, the first valve is in the open state,
Liquid phase pressure is higher than pressure in cross-line, liquid phase pressure 0.1 MPa~0.3 MPa preferably higher than in cross-line in leakproof pipeline.
2. according to the method for claim 1, it is characterised in that: when hydrogenator goes into operation, Aromatic raffinate is introduced into
Then the materials at bottom of tower of stabilizer is introduced into hydrogenator and carries out hydrogenation reaction by stabilizer, hydrogenation reaction effluent is logical
Enter stabilizer 5 minutes~24 hours, preferably 1~10 hour stop for Aromatic raffinate being passed directly into stabilizer and stop will
The materials at bottom of tower of stabilizer introduces hydrogenator, and Aromatic raffinate is introduced directly into hydrogenator, normally add
Hydrogen reaction process.
3. according to the method for claim 1, it is characterised in that: hydrogenation reaction is reacted using liquid-phase hydrogenatin, it is preferable that aromatic hydrocarbons
At least 80wt% that raffinates oil keeps liquid phase state, it is further preferred that Aromatic raffinate at least 90 wt% keep liquid phase state.
4. according to the method for claim 1, it is characterised in that: the tower bottom reboiler of stabilizer setting provides heat for stabilizer
Source, the stabilization materials at bottom of tower for introducing hydrogenator are drawn after tower bottom reboiler, it is preferable that are drawn after tower bottom reboiler
The temperature of stabilization materials at bottom of tower out is 100 DEG C~240 DEG C.
5. according to the method for claim 1, it is characterised in that: device for transporting objects is arranged in the tower bottom of stabilizer, passes through object
The material that stabilizer tower bottom exports is delivered to the pipeline before hydrogenator entrance by material conveying device.
6. according to the method for claim 1, it is characterised in that: on entering the pipeline before hydrogenator successively along flow direction
It is provided with First Heat Exchanger, air and liquid mixer and the second heat exchanger, First Heat Exchanger, the second heat exchanger are for heating aromatic hydrocarbons raffinate
Oil, air and liquid mixer for hydrogen and Aromatic raffinate to be sufficiently mixed, air and liquid mixer be preferably static mixer or
Dynamic mixer, it is quiet that static mixer is selected from SV type static mixer, SK type static mixer, SX type static mixer, SH type
One of state mixer, SL type static mixer or several combinations, dynamic mixer are selected from mixing pump, overcritical mixing
One or several kinds of combinations in device, mixer.
7. according to the method for claim 5, it is characterised in that: the pipeline setting being connect with the first import of First Heat Exchanger
There is the 4th valve.
8. according to method described in any one of claim 5-7, it is characterised in that: the outlet of stabilizer materials at bottom of tower is connected with
Reboiler, the material outlet of reboiler and the inlet ductwork of air and liquid mixer connect, and are equipped with the 5th valve on pipeline.
9. according to method described in any one of claim 5-7, it is characterised in that: the tower bottom export pipeline of stabilizer and
Second import of one heat exchanger connects.
10. according to the method for claim 1, it is characterised in that: hydrogen needed for hydrogenator is used to be arranged from PSA unit
Hydrogen out.
11. according to the method for claim 1, it is characterised in that: be disposed with gold above catalyst bed from bottom to top
Belong to two layers or more the porcelain ball that net and/or the first metallic grid, partial size become larger, the wall body of hydrogenator metal mesh and/
Or first be provided on metallic grid and unload agent mouth；
Metal mesh and/or the second metallic grid, partial size become larger two are disposed with below catalyst bed from the top down
Layer or more porcelain ball, Bird's Nest proppant, third metallic grid, the wall body of hydrogenator is in metal mesh and/or the second metallic grid
It is provided with down between third metallic grid and unloads agent mouth；
The wall body of hydrogenator unloads agent mouth in catalyst bed layer region is provided with.
12. according to the method for claim 1, it is characterised in that: reaction mass enters from hydrogenator bottom plus hydrogen is anti-
It answers and carries out hydrogenation reaction in device.
13. according to the method for claim 1, it is characterised in that: the operating condition of hydrogenation reaction is as follows: reaction pressure is
The MPa of 0.5 MPa~6.0, the preferably MPa of 1.2 MPa~3.0；Reaction temperature be 100 DEG C~240 DEG C, preferably 140 DEG C~
200℃；Volume space velocity is 1.0 h when liquid-1~12. 0h-1, preferably 4.0 h-1~8.0 h-1；Hydrogen to oil volume ratio be 20:1 with
Under, preferably 2:1~5:1.
14. according to the method for claim 1, it is characterised in that: Hydrobon catalyst is used with noble metal or reduction-state
Nickel is the Hydrobon catalyst of active component, and Hydrobon catalyst is using aluminium oxide as carrier, it is preferable that with Pt and/or Pd
For active component, the content of active component by weight in the catalyst is not less than 0.1%, preferably 0.1%~1.5%.
15. according to the method for claim 1, it is characterised in that: at the initial stage of going into operation, the materials at bottom of tower part of stabilizer or complete
Portion is passed through hydrogenator.
16. according to the method for claim 1, it is characterised in that: the arene content of Aromatic raffinate is less than 2wt%, preferably small
In 1wt%, olefin(e) centent is less than 6wt%.
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