CN102452879B - For the method for industrial C 4 fraction producing ethylene cracking material through hydrogenation - Google Patents
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- CN102452879B CN102452879B CN201010513951.0A CN201010513951A CN102452879B CN 102452879 B CN102452879 B CN 102452879B CN 201010513951 A CN201010513951 A CN 201010513951A CN 102452879 B CN102452879 B CN 102452879B
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Abstract
The invention discloses a kind of method of industrial C 4 fraction producing ethylene cracking material through hydrogenation, 2 reactors are set, non-noble metal hydrogenation catalyst for refining is all loaded in two reactors, first reactor effluent enters the second reactor after heating up, the postindustrial C 4 fraction component loops of the hydrogenation that second reactor effluent obtains and fresh process C 4 fraction raw material are mixed into the first reactor, and the weight ratio of the postindustrial C 4 fraction internal circulating load of hydrogenation and fresh process C 4 fraction raw material is 8: 1 ~ 1: 1.The inventive method can by industrial C
4cut fraction hydrogenation is high quality ethylene cracking material, solves industrial C simultaneously
4the thermal discharge existed in cut fraction hydrogenation is large, the problems such as the easy coking of catalyzer.
Description
Technical field
The present invention relates to a kind of method that liquefied petroleum gas (LPG) produces ethylene cracking material, especially with C
4cut is reaction raw materials, by producing the method for ethylene cracking material to diolefine wherein, monoolefine successively hydrotreatment.
Background technology
Along with the development of petroleum refining industry, the especially development of catalytic cracking technology, the deep processing of refinery gas is more and more subject to people's attention.The utilization of refinery gas has multiple path, and wherein liquefied gas hydrogenation is exactly one of problem of people's common concern.After liquefied gas hydrogenation, there is many purposes, such as, as the raw material, motor liquified gas etc. of ethylene cracking material, synthesis cis-butenedioic anhydride, wherein liquefied gas hydrogenation be used as ethylene cracking material because its large usage quantity, relate to that production equipment is numerous, economic benefit is obvious, so receive much concern.
With regard to ethylene raw, although for many years, the formation of world Ethylene raw material is basicly stable, and always based on petroleum naphtha and lighter hydrocarbons, but in recent years, due to the difference of various countries' resource, the change of raw materials market, there is the trend to diversified development in ethylene raw.Using butane as the method for ethylene raw be exactly one of diversified development trend of ethylene raw.At present, account for 3% ~ 5% using butane as ethylene raw in the U.S., with this adjustment as ethylene raw with supplementary.
Domestic petroleum chemical enterprise is in recent years newly-built, extended the large-scale ethene generating apparatus of many covers, cause ethylene raw shortage, realistic situation forces enterprise to find new ethylene raw to fill up this breach, and liquefied gas hydrogenation is exactly one of effective ways addressed this problem as ethylene raw.
Industry C
4the method that cut fraction hydrogenation prepares ethylene cracking material is exactly by industrial C
4alkene in cut and diene hydrogenation, make it to become alkane.CN1160701A describes a kind of C
3the method of the hydrogenation of cut, but the method object is to make C
3selective acetylene hydrocarbon hydrogenation in cut, the hydrogenation not to whole cut (comprising monoolefine).CN1145891A describes a kind of method of hydrotreating, but this method is only applicable to C
5cut fraction hydrogenation pentane.When using non-noble metal hydrogenation catalyst, the transformation efficiency of monoolefine is lower, and hydrogenation products does not reach the requirement for ethylene raw.USP4482767 describes a kind of C
3the method of (deriving from FCC) cut hydration co-production of liquefied gas, but the method is only suitable for C
3cut.CN01114163.8 describes a kind of method that hydrogenation of liquefied petroleum gas prepares Vehicular liquefied petroleum gas, but the method is not suitable for producing ethylene cracking material, because the index of Vehicular liquefied petroleum gas is alkene < 5.0%, and ethylene cracking material to require after hydrogenation olefin(e) centent < 2.0% in liquefied petroleum gas (LPG).
CN101429453A provides the method for a pyrolysis gasoline cut fraction oil one section of selec-tive hydrogenation except diolefine; CN101429454A provides the method for a full-cut fraction pyrolysis gasoline selec-tive hydrogenation except diolefine; CN101434508A provides one and is suitable for the saturated method of lighter hydrocarbons oligomerisation gasoline hydrogenation, but these three kinds of methods are all not suitable for industrial C
4cut fraction hydrogenation prepares ethylene cracking material.
Generally, the industrial C that obtains of the technological process such as catalytic cracking
4cut at 40v% ~ 60v%, has following features when carrying out hydrogenation reaction: (1) thermal discharge is large containing alkene.Such as, containing the C of alkene at 60v%
4cut, being 18.05KCa/mol by reaction heat during its whole hydrogenation of olefins, ideally adiabatic reaction temperature rise can reach 324 DEG C.(2) affect by thermodynamic(al)equilibrium.At industrial C
4in cut, the content of Trans-2-butene and iso-butylene is higher, therefore for Trans-2-butene, its temperature of reaction and equilibrium constant relation are listed in table 1.
Table 1 temperature of reaction and equilibrium constant relation
From data in table 1, along with the rising of temperature of reaction, the equilibrium constant decreases.When temperature of reaction is after height is respectively at 250 DEG C, 300 DEG C, 340 DEG C, there is the phenomenon of rapid reduction in reaction equilibrium constant.
In theory, olefin hydrogenation is a strong exothermal reaction, and rate-determining steps is reaction controlling, if temperature of reaction is lower, although reaction equilibrium constant is comparatively large, speed of response is slower; Otherwise if temperature of reaction is too high, although speed of response is comparatively large, reaction equilibrium constant is less, and final transformation efficiency is lower.For this Xiang Eryan, if the diffusion of reaction heat can not control (reaction temperature rising can not effectively control in other words) well, will reaction controlling be transferred to thermodynamic control, the transformation efficiency of reaction is reduced.
Find in an experiment, after temperature of reaction is more than 340 DEG C, because of the impact by chemical equilibrium, in its reaction product, olefin(e) centent declines comparatively slow.So, for industrial C
4cut fraction hydrogenation prepares ethylene cracking material project, and the shifting out of its reaction heat (effectively spreading) is a key issue that must solve in the industrial production.
In addition, at present at industrial C
4in cut fraction hydrogenation production, also there are the following problems: (1) is at industrial C
4in cut the content of diolefine comparatively Gao Shihui cause the easy coking in reaction bed ingress, reaction bed resistance increases very fast, causes production equipment often to stop work decoking, reduces reaction bed resistance remain normal and produce with this.(2) when in raw material not sulfur-bearing or sulphur content lower time, when diene hydrogenation, for preventing it from hot polymerization reaction at high temperature occurring, most select palladium series catalyst; But when sulphur content is higher in raw material, then select palladium series catalyst, when diene hydrogenation, in raw material, sulphur will make poisoning of catalyst, causes catalyzer to lose hydrogenation activity.
Summary of the invention
The object of this invention is to provide and a kind ofly utilize industrial C
4cut, particularly not separated industrial C
4cut is raw material, produces the method for ethylene cracking material, solve industrial C simultaneously through shortening
4in distillate, diene content is high, sulphur content is high, not easily reaches the requirement of ethene vapour cracking stock quality.
Find through large quantity research, C
4in cut fraction hydrogenation process, reaction has following features:
(1) according to reaction kinetics result of study, this exothermic heat of reaction is uneven, when by catalyst bed reaction, reaction time is 1/4 ~ 1/3 of the whole residence time time, and exothermic heat of reaction amount just reaches 75% ~ 80% of whole reaction heat.
(2) diene hydrogenation is a rapid reaction, and is suitable for low temperature, liquid-phase hydrogenatin.Adopt Ni series catalysts, just can there is hydrogenation reaction in 1,3-butadiene (hereinafter referred to as divinyl) under reaction pressure > 3.0MPa, temperature > 150 DEG C of conditions.For butadiene content higher (being less than 4.0%), sulphur content also higher (> 5mg/M
3) C
4cut material, adopts noble metal hydrogenation catalyst for refining to cause rapid catalyst deactivation.
(3) divinyl is at C
4when in cut, content reaches 3.0%, temperature of reaction reaches 120 DEG C, the residence time 2 ~ 3h, and hot polymerization reaction just can occur; Be greater than 140 DEG C, the reaction of divinyl hot polymerization can obviously acceleration.Based on this, for the C of butadiene content higher (being less than 4.0%)
4cut fraction hydrogenation is reacted, for avoiding divinyl generation hot polymerization reaction wherein, can have two methods: first method is diluting reaction charging, the effect of this method has two, one reduces the concentration of the diolefine in raw material relatively, improve material reaction bed by time linear velocity; It two is beneficial to taking-up reaction heat, reduces temperature of reaction; Second method improves reaction pressure to reduce temperature of reaction with this.
(4) can also obtain as drawn a conclusion according to table 2,3 data: disregarding under hydrogen influence condition, wanting diolefine is liquid phase, and temperature of reaction answers < 150 DEG C, and reaction pressure requires > 3.6MPa; If the impact of meter hydrogen, temperature of reaction answers < 140 DEG C, and reaction pressure requires > 4.2MPa.
(5) C
4cut monoolefin hydrogenation, but gas phase is also passable under liquid-phase reaction condition advantageously.
Table 2 critical temperature
| Title | Critical temperature Tc (DEG C) |
| Normal butane | 152.01 |
| Trimethylmethane | 134.98 |
| Cis-2-butene | 162.4 |
| Trans-2-butene | 155.46 |
| 1-butylene | 146.4 |
| Iso-butylene | 144.74 |
| 1,3-butadiene | 152 |
Table 3 reaction product each component vapour pressure
(6) temperature of reaction < 150 DEG C to be met, the condition that in charging, diene content is less than 2.0%, charging can be adopted with aniseed thinning ratio.For above-mentioned research, for industrial C
4the content of diolefine higher (1% ~ 4%), higher (the > 5mg/M of sulphur content in cut
3) C
4fraction hydrotreating method, the present invention proposes following technical scheme.
The method of the present invention's industry C 4 fraction producing ethylene cracking material through hydrogenation comprises following content: arrange 2 reactors, non-noble metal hydrogenation catalyst for refining is all loaded in two reactors, first reactor effluent enters the second reactor after heating up, and the postindustrial C 4 fraction component loops of the hydrogenation that the second reactor effluent obtains and fresh process C 4 fraction raw material are mixed into the first reactor.
In the inventive method, the temperature in of the first reactor is 100 ~ 160 DEG C, is preferably 120 ~ 150 DEG C; Reaction pressure is 2.5 ~ 16.5MPa, is preferably 3.0 ~ 6.0MPa; During stock liquid, volume space velocity (volume space velocity of fresh process C 4 fraction raw material) is 0.4 ~ 25h
-1, be preferably 4 ~ 8h
-1, the hydrogen to oil volume ratio volume ratio of hydrogen and fresh process C 4 fraction raw material (under the standard state) is 200: 1 ~ 1500: 1, is preferably 300: 1 ~ 1000: 1.
In the inventive method, the temperature in of the second reactor is 170 ~ 250 DEG C, is preferably 190 ~ 220 DEG C; Reaction pressure is 2.5 ~ 16.5MPa, is preferably 3.0 ~ 6.0MPa; During stock liquid, volume space velocity (volume space velocity of fresh process C 4 fraction raw material) is 0.4 ~ 25h
-1, be preferably 1 ~ 4h
-1, the hydrogen to oil volume ratio volume ratio of hydrogen and fresh process C 4 fraction raw material (under the standard state) is 200: 1 ~ 1500: 1, is preferably 300: 1 ~ 1000: 1.
In the inventive method, the weight ratio (i.e. recycle stock: fresh feed weight ratio) of the postindustrial C 4 fraction internal circulating load of hydrogenation and fresh process C 4 fraction raw material is 8: 1 ~ 1: 1, is preferably 4: 1 ~ 2: 1.
In the inventive method, the hydrogen purity of reacting used is 55v% ~ 99v%, can low point of gas (58v% ~ 88v%) of refinery, the synthetic gas (hydrogen: 75v%) of synthesis ammonia plant, hydrogenation unit to be vented outward etc. be the unserviceable hydrogen source of other hydrogenation unit.Fresh process C 4 fraction raw material can be catalytic cracking unit without refining material.
In the inventive method, non-noble metal hydrogenation catalyst for refining is generally carrier with aluminum oxide, with one or more in tungsten, molybdenum, nickel, cobalt for active ingredient, with the active ingredient weight content of oxide basis for 15% ~ 40%, can containing suitable auxiliary agent in catalyzer, commodity Hydrobon catalyst can be adopted, as the LH2010-A series Hydrobon catalyst of Fushun Petrochemical Research Institute's development and production, also can by the existing method preparation in this area.
The inventive method is by optimizing industrial C 4 fraction work flow, and each operational condition in work flow, efficiently solve the various problems that industrial C 4 fraction hydrogenation process exists, use Industry C 4 fraction can the high-quality ethylene cracking material of direct production, improve the utility value of industrial C 4 fraction.
The inventive method solves in Industry C 4 fraction that sulphur content is high, olefin(e) centent is high, diene content high bring poisoning of catalyst, catalyzer coking, running period is short, reaction temperature rising is large, affect the various problems such as the hydrogenation products olefin(e) centent caused is high by thermodynamic(al)equilibrium, obtains good technique effect.
Accompanying drawing explanation
Fig. 1 is a kind of concrete technology schematic flow sheet of the present invention.
Wherein: 1-C
4feedstock, 2-hydrogen, 3-first reactor, 4-well heater, 5-second reactor, 6-product water cooler, 7-reacting product outlet.
Embodiment
The solution of the present invention and effect is further illustrated below by embodiment.
The LH2010-A Hydrobon catalyst of the catalyzer Fushun Petrochemical Research Institute development and production used in embodiment, can regenerate use.Physico-chemical property is as table 4.
The physico-chemical property of table 4LH2010-A catalyzer
Embodiment 1
Reaction used catalyst is W-Mo-Ni-Co (catalyzer trade mark LH2010-A); Reaction process is two sections of adiabatic reactors (middle heating).
Reaction raw materials: hydrogen is electrolytic cleaning hydrogen, purity > 99%; C-4-fraction takes from certain refinery, and composition is in table 5.Reaction is for upper feeding, and reaction mass flows out from the second reactor bottom, enters in separator after cooling, and tail gas is discharged from separator napex, bottom liquid phases timing sampling, forms with gas chromatographic analysis, concrete reaction conditions and the results are shown in table 6,7,8.
The main character of table 5 industrial C 4 fraction hydrogenator industry C 4 fraction charging
| Analysis project (volume content) | |
| Propane, % | ＜0.10 |
| Trimethylmethane, % | 29.13 |
| Normal butane, % | 10.01 |
| Propylene, % | ＜0.10 |
| Butene-1, % | 14.28 |
| Iso-butylene, % | 17.38 |
| Anti-butene-2, % | 16.54 |
| Maleic-2, % | 11.87 |
| Carbon five, % | 0.24 |
| Carbon two, % | ＜0.10 |
| Divinyl, % | 0.55 |
| Total sulfur | 26 |
| Alkene amounts to % | 60.17 |
Table 6 first reactor process condition
Table 7 second reactor process condition
Industrial C 4 fraction main character after table 8 hydrogenation
| Analysis project (volumetric concentration) | |
| Alkane in product, % | 99.17 |
| Divinyl in product, % | - |
| Non-hydrogenated olefin % in product | 0.83 |
Embodiment 2
Reaction used catalyst is W-Mo-Ni-Co (catalyzer trade mark LH2010-A); Reaction process is two sections of adiabatic reactors (middle heating).
Reaction raw materials: hydrogen is electrolytic cleaning hydrogen, purity > 99%; C-4-fraction takes from certain refinery (non-desulfurization), and composition is in table 9.Reaction is for upper feeding, and reaction mass flows out from the second reactor bottom, enters in separator after cooling, and tail gas is discharged from separator top, bottom liquid phases timing sampling, forms with gas chromatographic analysis, concrete reaction conditions and the results are shown in table 10,11,12.
The main character of table 9 industrial C 4 fraction hydrogenator industry C 4 fraction charging
| Analysis project (V%) | |
| Propane, % | ＜0.10 |
| Trimethylmethane, % | 29.13 |
| Normal butane, % | 10.01 |
| Propylene, % | ＜0.10 |
| Butene-1, % | 14.28 |
| Iso-butylene, % | 17.38 |
| Anti-butene-2, % | 16.54 |
| Maleic-2, % | 11.87 |
| Carbon five, % | 0.24 |
| Carbon two, % | ＜0.10 |
| Divinyl, % | 0.55 |
| Mercaptan sulfur, mg/m 3 | 4 |
| Total sulfur, mg/m 3 | 500 |
| Alkene amounts to % | 60.17 |
Table 10 first reactor process condition
Table 11 second reactor process condition
Industrial C 4 fraction main character after table 12 hydrogenation
| Analysis project | |
| Alkane in product, % (v/v) | 99.23 |
| Divinyl in product, % (v/v) | - |
| Non-hydrogenated olefin % (v/v) in product | 0.77 |
Claims (4)
1. the method for industrial C 4 fraction producing ethylene cracking material through hydrogenation, it is characterized in that comprising following content: arrange 2 reactors, reaction process is two sections of adiabatic reactors, non-noble metal hydrogenation catalyst for refining is all loaded in two reactors, first reactor effluent enters the second reactor after heating up, the postindustrial C 4 fraction component loops of the hydrogenation that second reactor effluent obtains and fresh process C 4 fraction raw material are mixed into the first reactor, and the weight ratio of the postindustrial C 4 fraction internal circulating load of hydrogenation and fresh process C 4 fraction raw material is 8: 1 ~ 1: 1; Industry C
4in cut, the volume content of diolefine is 1% ~ 4%, sulphur content > 5mg/M
3;
Wherein the temperature in of the first reactor is 100 ~ 150 DEG C, and reaction pressure is 3.0 ~ 16.5MPa, and the volume space velocity of fresh process C 4 fraction raw material is 5.0 ~ 25h
-1, the volume ratio of hydrogen and fresh process C 4 fraction raw material is 200: 1 ~ 1500: 1; The temperature in of the second reactor is 170 ~ 250 DEG C, and reaction pressure is 2.5 ~ 16.5MPa, and the volume space velocity of fresh process C 4 fraction raw material is 0.4 ~ 25h
-1, the volume ratio of hydrogen and fresh process C 4 fraction raw material is 200: 1 ~ 1500: 1;
Non-noble metal hydrogenation catalyst for refining take aluminum oxide as carrier, with one or more in tungsten, molybdenum, nickel, cobalt for active ingredient, with the active ingredient weight content of oxide basis for 15% ~ 40%.
2. in accordance with the method for claim 1, it is characterized in that: the temperature in of the first reactor is 120 ~ 150 DEG C, and reaction pressure is 3.0 ~ 6.0MPa, the volume space velocity of fresh process C 4 fraction raw material is 5.0 ~ 8h
-1, the volume ratio of hydrogen and fresh process C 4 fraction raw material is 300: 1 ~ 1000: 1.
3. in accordance with the method for claim 1, it is characterized in that: the temperature in of the second reactor is 190 ~ 220 DEG C, and reaction pressure is 3.0 ~ 6.0MPa, the volume space velocity of fresh process C 4 fraction raw material is 1 ~ 4h
-1, the volume ratio of hydrogen and fresh process C 4 fraction raw material is 300: 1 ~ 1000: 1.
4. in accordance with the method for claim 1, it is characterized in that: the weight ratio of the postindustrial C 4 fraction internal circulating load of hydrogenation and fresh process C 4 fraction raw material is 4: 1 ~ 2: 1.
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| CN106753562B (en) * | 2015-11-20 | 2018-08-14 | 中国石油化工股份有限公司 | A kind of technique of dry gas producing ethylene cracking material through hydrogenation |
| CN108069815B (en) * | 2016-11-11 | 2020-10-16 | 中国石油化工股份有限公司抚顺石油化工研究院 | Method for preparing high-purity butane |
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| CN101081998A (en) * | 2006-05-31 | 2007-12-05 | 中国石油化工股份有限公司 | Hydrogenation method for C4 distillation cut |
| CN101113126A (en) * | 2006-07-26 | 2008-01-30 | 李莉 | Olefin-containing lighter hydrocarbons catalytic hydrogenation method |
| CN101538479A (en) * | 2008-03-19 | 2009-09-23 | 中国石油天然气股份有限公司 | Method for producing alkylate oil by low-temperature hydroalkylation of C-C |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101081998A (en) * | 2006-05-31 | 2007-12-05 | 中国石油化工股份有限公司 | Hydrogenation method for C4 distillation cut |
| CN101113126A (en) * | 2006-07-26 | 2008-01-30 | 李莉 | Olefin-containing lighter hydrocarbons catalytic hydrogenation method |
| CN101538479A (en) * | 2008-03-19 | 2009-09-23 | 中国石油天然气股份有限公司 | Method for producing alkylate oil by low-temperature hydroalkylation of C-C |
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