CN109574786A - Preparing propylene by dehydrogenating propane reaction mixture gas cold oil absorbs the separation method coupled with PSA - Google Patents
Preparing propylene by dehydrogenating propane reaction mixture gas cold oil absorbs the separation method coupled with PSA Download PDFInfo
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Abstract
The present invention relates to a kind of preparing propylene by dehydrogenating propane reaction mixture gas cold oil to absorb the separation method coupled with PSA, main includes pretreatment, cold oil absorbs and PSA proposes hydrogen process, the hydrogen product of hydrogen system absorption tower top outflow purity >=99.99%, olefin impurity component total content≤0.05% is proposed from PSA, a part returns to PDH reaction zone as the mixing of circulating hydrogen and propane feed gas and is reacted, and another part is as defeated outside hydrogen product or/and for the SHP in PDH product fractionation zone；The stripping gas that hydrogen system tower bottom flows out is mentioned from PSA to export directly as unstripped gas or hydrogen feedstock gas, or is entered PDH product fractionation zone after processing and further recycled C2+；The complete propane of unreacted is reacted after returning to the mixing of propane feed gas into PDH reaction zone.It solves in traditional PDH dehydrogenation producing propylene production process that product centrifugal station energy consumption is high, needs corrosion protection equipment, recycle hydrogen different from product hydrogen specification and proportion is difficult to control that caused investment and operating cost be excessively high and technological operation the problems such as there are security risks.
Description
Technical field
The present invention relates to petrochemical industry propylene and hydrogen preparation and separation method and energy conservation field is related to, specifically
It is related to a kind of separation method that the absorption of preparing propylene by dehydrogenating propane reaction mixture gas cold oil is coupled with PSA.
Background technique
Propylene is the important petrochemical industry base stock for being only second to ethylene, and the following world market supply is extremely tight in the long term
The state of opening will continue the long period.But, recently as the unconventional natural resources in the world, such as shale gas, oil field gas,
The exploitation of the resources such as ocean combustible ice is broken through, the business development success of especially a large amount of shale gas resource, so that for a long time,
Stable, relative moderate propane resource is possibly realized, in turn, with propane (the biggish ingredient of accounting in shale gas) for raw material, warp
It crosses dehydrogenation reaction and produces propylene (PDH) project with the stronger market competitiveness, and thus cause industry giant and invest one after another.Its
In, set large size PDH device more than ten has been built in China, to meet the demand in growing propylene market, has reduced import.
Catalytic cracking process of traditional propylene supply mainly from naphtha pyrolysis ethylene and petroleum refining.Due to stone
The growth for the restricted ethylene production capacity of propylene that oily method for refining generates, and then it is unable to satisfy the increased requirement in propylene market.In recent years,
With the maturation and development of New Coal Chemical technology, ethylene, propylene (MTO/MTP) scale is prepared as raw material using methanol and is increasingly increased,
Further fill up the deficiency that petroleum refining prepares propylene.But due to environmental protection and cost, MTO/MTP device generate propylene cost compared with
Main path high that the growth of propylene market takes on.On the contrary, with the success that shale gas large-scale commercial is developed, so that
Become the most important Technical economic means for meeting propylene growth as the method that raw material prepares propylene (PDH) using cheap propane.
Currently, being the Catofin work of Oleflex and the ABB Lummus of U.S. UOP respectively there are mainly two types of PDH techniques
Skill.Wherein, Oleflex industrialized unit is commonplace, is included in China and has built ability in, and device aggregated capacity is close to 400
~500 ten thousand tons.
Oleflex technique mainly includes the moving bed reaction area of its core technology of core, continuous catalyst regenerating area, product
Disengagement zone and fractionation zone composition.Wherein, in the workshop section of product Disengagement zone, the PDH gaseous mixture of generation is reacted, by pre-processing and doing
The cryogenic step for being -180~-170 DEG C into operation temperature after dry, including ice chest and separator etc., by a large amount of propylene, and
Enter subsequent fractionation zone workshop section after the C2+ component liquefaction such as ethylene and obtain propylene product, unreacted propane returns to unstripped gas
In continue to use.The on-condensible gas that cryogenic step generates mainly includes the hydrogen (H that concentration is 92~98%2), 3~5% first
The components such as the alkane such as alkane, ethane and micro C0 are mixed with propane feed gas mostly as circulating hydrogen and are entered directly into instead
Area is answered to be reacted.A part of on-condensible gas is used as the unstripped gas or fuel gas for mentioning hydrogen.Its recycle hydrogen is Oleflex technique
Middle special demand only needs one of important difference technology a small amount of or without recycle hydrogen step with ABB Lummus technique.It should
It requires olefin-containing total amount less than 0.05% in circulating hydrogen, is produced with preventing platinum group catalyst knot carbon inactivation used in reaction
The safety problem of raw temperature runaway.
Recycle hydrogen cryogenics in Oleflex technique, there are Railway Project, first, operation temperature needed for cryogenic separation
Degree is very low, and about -180~-170 DEG C, energy consumption is relatively high, causes operating cost high；Second, needed for deep cooling (ice chest)
Equipment and materials is stainless steel, is invested larger；Third needs that a set of PSA device is separately added to extract from on-condensible gas more than needed higher
The hydrogen of purity (being more than or equal to 99.99%), realizes the promotion of PDH device whole economic efficiency, especially Oleflex technique is drawn
Into high alkynes and butadiene hydrogenation (SHP) technology, the higher hydrogen of purity itself is needed, wherein CO content is less than 10ppm, prevents
The problem of only hydrogenation catalyst occurs glycosylation and inactivates；4th, in the on-condensible gas generated in deep cooling, it is possible to folder
Take a small amount of olefin impurity component out of, catalyst service life used is affected to reaction.In fact, Oleflex technique
Platinum group catalyst service life used is shorter, and about 2 years, this was also one of major defect of its technique, and expense is also high.
Equally, the product Disengagement zone in the Catofin technique of Lummus company, and use cryogenic separation (ice chest) method
Come the on-condensible gas for obtaining the C2+ component rich in propylene with being rich in hydrogen, to obtain product propylene.Naturally also there is deep coolings
The problems such as separating energy consumption is high, equipment investment is big, operating cost is high.
In addition, the dehydrogenation producing propylene or de- for propane (C3), butane (C4) or butane (C4), pentane (C5) mixed raw material
Hydrogen is etherified methyl tertiary butyl ether(MTBE) (MTBE), ethyl tert-butyl ether (ETBE) (ETBE), tert amyl methyl ether(TAME) (TAME) or ethyl tertiary pentyl processed
Ether (TAEE) process dehydrogenation gaseous mixture, and the C2+ component fluids rich in propylene are obtained using cryogenic separation and are rich in hydrogen
On-condensible gas equally exists the problems such as energy consumption is high, equipment investment is big, operating cost is high.
Therefore, present invention method is aiming at the production in PDH and hydro carbons gaseous mixture dehydrogenation olefin production process
Investment caused by the height of energy consumption present in product centrifugal station, anticorrosion, recycle hydrogen and product hydrogen specification difference etc. and operation at
This excessively high problem and propose.
Summary of the invention
It is coupled the present invention provides a kind of absorption of preparing propylene by dehydrogenating propane reaction mixture gas cold oil with pressure-variable adsorption (PSA)
Separation method, PDH gaseous mixture component, such as propylene, propane caused by PDH reaction zone, a small amount of ethylene, ethane, butane, fourth
The physicochemical characteristics of the hydrocarbons such as alkene, butadiene, and a large amount of H2 etc., in absorbent liquid (propane, butane or C6
+ solution) in relative solubility, relative adsorption separation and corresponding operating condition (temperature and pressure), cold oil is inhaled
Receiving method (this case is middle cold oil) and PSA, which are coupled, substitutes deep cooling, realizes the separation of PDH reaction mixture gas propylene and hydrogen and mentions
It takes, to solve the problems of prior art.
It proposes hydrogen process by pretreatment, cold oil absorption and PSA for this purpose, the present invention is used and combines, realize while being followed
The separation and extraction of ring hydrogen, product hydrogen and product propylene, the specific method is as follows:
A kind of separation method that the absorption of preparing propylene by dehydrogenating propane reaction mixture gas cold oil is coupled with PSA, includes the following steps:
(1) pretreatment process comes from the reactant mixed gas of preparing propylene by dehydrogenating propane (PDH) reaction zone, as raw material
Gas, by the pretreatment process that heat exchange, dedusting, compression form, into next process, cold oil absorbs.
(2) cold oil absorbs process, by the unstripped gas of pretreatment process, is -45~-30 DEG C, operates into operation temperature
Pressure is the middle cold oil absorption system of 3.0~5.0MPa, from middle cold oil absorption tower lower part into and on therefrom cold oil absorption tower
After the absorbent in portion inversely contacts, therefrom the outflow of cold oil absorption system is rich in the C2+ liquid of propylene, i.e. absorbing liquid, at least
By gas-liquid separator, refrigerator, the selective hydrogenation of alkynes allene (SHP) equipment, domethanizing column, dethanizer, propylene propane
Treated for the PDH product fractionation zone product propylene of knockout tower, depropanizing tower composition, therefrom cold oil absorption system outflow are rich in
The on-condensible gas (hydrogen-rich on-condensible gas) of hydrogen enters pressure-variable adsorption (PSA) after heat exchange to room temperature and proposes hydrogen process；Wherein,
The absorbent produces propane through liquefaction gained liquid, or the richness third from propylene propane knockout tower by unstripped gas or depropanizing tower
Alkane liquid；
(3) pressure-variable adsorption (PSA) mentions hydrogen, and the room temperature of the cold separation process on-condensible gas with pressure rich in hydrogen enters in
PSA mentions hydrogen system, and operation temperature is room temperature, and operating pressure is 3.0~5.0MPa, be greater than from PSA absorption tower top outflow purity etc.
In the hydrogen product of 99.99% (volume ratio, similar below), wherein olefin impurity component total content is less than or equal to 0.05%, one
Part is reacted with the mixing of propane feed gas back to PDH reaction zone as circulating hydrogen, and a part is as outside hydrogen product
Defeated or/and a part of alkynes allene selective hydrogenation (SHP) being directly used in PDH product fractionation zone；From PSA adsorption tower bottom
The rich C2+ concentrated gas of outflow, or exported directly as fuel gas, or as natural gas hydrogen preparation unstripped gas, or by refrigeration with
It compresses step recycling C2+ and forms liquid and enter PDH product fractionation zone acquisition product propylene；It is remaining after extracted product propylene
The complete propane of unreacted enters PDH reaction zone after mixing back to propane feed gas and is reacted.
Among the above, PSA mentions hydrogen system by multiple serial or parallel connections or series-parallel adsorption tower group at being filled in adsorption tower
Activated alumina, silica gel, active carbon, molecular sieve one or more combination of adsorbents, connected by setting between adsorption tower
The control system of regulating valve or sequence valve or other valves composition on pipeline carries out PSA adsorption and desorption circulate operation mistake
The control and adjusting of pressure change in journey.The desorption technique of each adsorption tower, including vacuumize or product gas flushing, or vacuumize+
The method of flushing or desorption with pressure.
Further, a kind of preparing propylene by dehydrogenating propane reaction mixture gas cold oil absorbs the separation side coupled with PSA
In method, preprocessed process treated unstripped gas is before entering cold oil and absorbing process, through contained by the removing of wet process decarbonization process
CO2.This scheme is suitable for unstripped gas and contains more carbon dioxide (CO2) operating condition；The wet process decarburization, including organic amine physics
Absorption and/or alkali cleaning chemical absorption method.
Further, the cold oil absorbs process, in after the processing of cold oil absorption system, from middle cold oil absorbing tower bottom
The C2+ liquid rich in propylene of outflow, i.e. absorbing liquid, are introduced into desorber, analytically the rich propane liquid of tower tower bottom outflow, greatly
Part is used as absorbent, is recycled after being overpressurized back to middle cold oil absorption tower, remainder enters depropanizing tower, into one
Step recycling propane；The C2+ gas rich in propylene flowed out from tower top, into subsequent including separator, refrigerator, alkynes allene
PDH product fractionation zone including selective hydrogenation (SHP) equipment, domethanizing column, dethanizer, depropanizing tower, finally obtains third
Alkene product.
Further, decarbonizing tower is added after desorber, therefrom the C2+ rich in propylene of cold oil absorption tower tower top outflow
Gas enters back into the processing of PDH product fractionation zone, finally obtains propylene product after decarbonizing tower carries out decarburization.This scheme is suitable for
Unstripped gas in the pretreatment process contains more carbon dioxide (CO2) operating condition；The decarbonizing tower can use
Organic amine Physical Absorption and/or alkali cleaning chemical absorption method.
Further, the on-condensible gas (hydrogen-rich on-condensible gas) rich in hydrogen flowed out from cold oil absorption system, is removed
Heat exchange mentions outside hydrogen process to entering PSA after room temperature, can also be without heat exchange or shallow -30~30 DEG C of the cold temperature that exchanged heat into after,
Hydrogen process is proposed into PSA to carry out mentioning hydrogen.At this point, the operating pressure for proposing hydrogen process is 3.0~5.0MPa, wherein PSA mentions hydrogen system
Adsorption tower at least by 2 adsorption tower groups at and the regeneration of adsorption tower needs vacuum desorption.
Further, the cold oil absorbs the hydrogen-rich on-condensible gas of process outflow, except mentioning after heat exchange to room temperature into PSA
Outside hydrogen process, it can also be exchanged heat to 60~120 DEG C of medium temperature, propose hydrogen process into PSA and carry out mentioning hydrogen.At this point, proposing hydrogen process
Operating pressure, or 3.0~5.0MPa range is maintained, or be down to 0.5~3.0MPa range；Wherein, PSA mentions the adsorption tower of hydrogen system
At least by 2 adsorption tower groups at and the regeneration of adsorption tower needs vacuum desorption.
Further, a kind of preparing propylene by dehydrogenating propane reaction mixture gas cold oil absorbs in the separation method coupled with PSA, institute
The PSA stated mentions hydrogen system, can mention hydrogen unit by two sections of PSA and form, in first segment PSA (1#PSA) in operation, from 1#The absorption of PSA
The fluid phase gas rich in hydrogen of column overhead outflow, density of hydrogen are 92~98%, and theatotal olefinsacontent is less than 0.05%, one
Divide and used directly as recycle hydrogen, another part enters second segment PSA (2#PSA hydrogen unit) is mentioned；It is handled through 2#PSA, from 2#PSA
Adsorption tower tower top outflow purity be 99.99% or more hydrogen product output or/and for PDH product fractionation zone alkynes third
The absorption phase gas of selective hydrogenation of dienes, tower bottom outflow is rich in methane, directly as fuel gas, or as natural gas hydrogen preparation
Unstripped gas.From 1#PSA mentions the rich C2+ gas of the adsorption tower bottom outflow of hydrogen unit, after supercooling pressure regulation, or enters cold oil and inhales
Knock off sequence, further recycle C2+, includes mainly propylene and propane, further recycled or, evening fractionation zone out into subsequent PDH
C2+ mainly includes propylene and propane.
Further, the PSA mentions hydrogen system, and the hydrogen-rich on-condensible gas of process is absorbed from cold oil, is in its pressure
3.0~5.0MPa, and pass through under the conditions of heat exchange to temperature is 60~120 DEG C and enter the hydrogen membrane system by one or more levels permeation hydrogen
System is rich in the infiltration gas of hydrogen from the outflow of hydrogen membranous system per-meate side, pressurized to pressure needed for recycle hydrogen, is directly entered PSA
Hydrogen system is mentioned, after PSA proposes hydrogen system processing, is more than or equal to 99.99% from the adsorption tower tower top outflow purity of PSA deduction system
Hydrogen, a part returns to PDH reaction zone as the mixing of circulating hydrogen and propane feed gas and reacted, another part conduct
It is defeated or/and for the alkynes allene selective hydrogenation (SHP) in PDH product fractionation zone outside hydrogen product.PSA mentions hydrogen system
The stripping gas of adsorption tower tower bottom outflow is exported directly as fuel gas, or, exporting as natural gas hydrogen preparation unstripped gas.From hydrogen membrane system
The impermeable gas (gas rich in C2+) of the impermeable side outflow of system after supercooling, or is returned directly to cold oil and absorbs process
C2+ is further recycled, includes mainly propylene and propane, or be directly entered the fractionation zone PDH and further recycle C2+, mainly includes third
Alkene and propane.
Further, a kind of preparing propylene by dehydrogenating propane reaction mixture gas cold oil absorbs the separation coupled with PSA
In method, the PSA mentions hydrogen system, can be required according to recycle hydrogen internal circulating load, carries out recycle hydrogen tolerance and product amounts of hydrogen
The adjusting of ratio or recycle hydrogen tolerance and the amounts of hydrogen ratio for PDH product fractionation zone, guarantee, which meets in PDH reaction zone, to follow
The strict demand of ring amounts of hydrogen.
Further, a kind of preparing propylene by dehydrogenating propane reaction mixture gas cold oil absorbs in the separation method coupled with PSA,
The FTrPSA mentions hydrogen methods, is also suitble to include propane (C3), butane (C4) or butane (C4), pentane (C5) mixed raw material
Dehydrogenation producing propylene or dehydrogenation etherificate methyl tertiary butyl ether(MTBE) (MTBE) processed, ethyl tert-butyl ether (ETBE) (ETBE), tert amyl methyl ether(TAME)
(TAME) or the recycle hydrogen of tertiary amyl ethyl ether (TAEE) process dehydrogenation gaseous mixture and or product hydrogen separation and Extraction.Wherein, lighter hydrocarbons
Cold oil absorption step during gaseous mixture dehydrogenation preparing isobutene or butylene, can be used using C4 as absorbent, absorb temperature be 5~
15 DEG C of shallow cold oil absorption technique, cold oil absorbs in substitution.
The beneficial effects of the present invention are:
(1) using the method for the present invention, in the product separation process that PDH or hydro carbons gaseous mixture dehydrogenation alkene can be substituted
Ice chest (cryogenic separation) technology, from operation temperature needed for ice chest operation be -180~-170 DEG C of high energy consumption, be reduced in it is cold
Needed for oily absorption and separation -40~-30 DEG C and PSA mention hydrogen needed for room temperature low energy consumption, save a large amount of cooling capacity；
(2) equipment and materials needed for the deep cooling (ice chest) in the product Disengagement zone of PDH or hydro carbons gaseous mixture dehydrogenation alkene
For stainless steel, invest larger.Cold oil absorption extraction proposes hydrogen technique rich in the C2+ and PSA of propylene and couples in present invention use, required
Equipment and materials can be with ordinary carbon steel, equipment investment cost is low, while in turn avoiding the low temperature in traditional cryogenic separation (ice chest)
Operate the incident security risks such as cold short；
(3) invention is not necessarily to only obtain recycle hydrogen (purity 92~98%) as traditional cryogenic separation and product hydrogen (is greater than
Equal to 99.99%) needing separately plus a set of PSA mentions hydrogen production device and extracts from on-condensible gas more than needed and obtains, that is, the present invention can be straight
It connects to obtain recycle hydrogen and product hydrogen, realizes the promotion of PDH device whole economic efficiency, the PDH technique such as especially Oleflex is introduced
High alkynes and butadiene hydrogenation (SHP) technology, itself need the higher hydrogen of purity, and wherein CO content is less than 10ppm, prevent
The problem of hydrogenation catalyst occurs glycosylation and inactivates；
(4) cold oil without desorption that the present invention uses absorbs, and has not only alleviated the energy consumption of PDH product Disengagement zone, but also accordingly subtract
The load and energy consumption for having lacked the domethanizing column in subsequent fractionation area, dethanizer and depropanizing tower, save investment；Meanwhile it can be with
According to component fluctuation in reaction mixture gas, the internal circulating load of flexible modulation absorbent propane is coped with；
(5) ratio of the present invention adjustable recycle hydrogen tolerance and product amounts of hydrogen, can effectively guarantee PDH or hydro carbons
The supply of recycle hydrogen tolerance needed for gaseous mixture dehydrogenation reaction avoids in reaction process because recycle hydrogen tolerance is too low or excessive is led
The serious security risk such as the reaction inactivation of cause or temperature runaway；For traditional cryogenic separation system, the operation of PSA system
Elasticity is relatively large, facilitates the stabilization safety operation of device；
(6) present invention process takes full advantage of the energy of unstripped gas itself, including in cold or shallow cold oil absorb and inhaled with transformation
Operation temperature of the Fufen from coupling process can remain unchanged, and therefrom cold oil absorbs or shallow cold oil absorbs the on-condensible gas escaped
Pressure is also consistent with the PSA adsorptive pressure for mentioning hydrogen, and the comprehensive energy consumption of entire separation process is low；
(7) using the present invention, the theatotal olefinsacontent in recycle hydrogen can be made even zero less than 0.01%, avoid deep cooling
It is possible to being entrained with a small amount of olefin impurity component in the on-condensible gas that separation generates, is used to reaction catalyst used the longevity
Life is affected the problem of even inactivation leads to the security risks such as temperature runaway；
(8) present invention can be with high-purity, in high yield separation and Extraction C2+ and H2(recycle hydrogen and product hydrogen), so that subsequent
PDH or the energy consumption of product fractionation zone of hydro carbons gaseous mixture dehydrogenation alkene decrease, reduce corresponding domethanizing column, de-
The load of ethane tower, depropanizing tower etc..
(9) present invention solves product centrifugal station energy consumption height in traditional PDH dehydrogenation producing propylene production process, needs anticorrosion
Equipment, recycle hydrogen are different from product hydrogen specification and proportion uncontrollable caused investment and operating cost is excessively high and technique is grasped
Make the problems such as there are security risks.
Detailed description of the invention
Fig. 1 is 1 flow diagram of the embodiment of the present invention；
Fig. 2 is 3 flow diagram of the embodiment of the present invention；
Fig. 3 is 4 flow diagram of the embodiment of the present invention；
Fig. 4 is 5 flow diagram of the embodiment of the present invention；
Fig. 5 is 6 flow diagram of the embodiment of the present invention.
Specific embodiment
All features disclosed in this specification can be with any other than mutually exclusive feature and/or step
Mode combines.
In order to make those skilled in the art more fully understand technical solution of the present invention, below with reference to Fig. 1~3 and specifically
Embodiment the present invention is described in further detail.
Embodiment 1
As shown in Figure 1, a kind of preparing propylene by dehydrogenating propane reaction mixture gas cold oil absorbs the separation method coupled with PSA, tool
Body implementation steps include,
(1) pretreatment process comes from the reactant mixed gas of preparing propylene by dehydrogenating propane (PDH) reaction zone, as raw material
Gas, main component are the propylene of 35~40% (volume ratios, similar below), 40~55% hydrogen, remaining component includes,
The C2+ such as methane, ethane, propane, isobutene, iso-butane, normal butane, propine, alkadienes hydrocarbon component and solid particulate matter etc.
Other impurity compositions remove other impurity compositions in unstripped gas by dedusting, the pretreatment process of compression composition, and pass through
After overcompression is cooled to 3.5MPa and -35 DEG C, into next process, cold oil absorbs；
(2) cold oil absorbs process, by the unstripped gas of pretreatment process, into operation temperature be -35 DEG C, operating pressure is
The middle cold oil absorption system of 3.5MPa, using the rich propane liquid separated from propylene/propane as absorbent, therefrom cold oil is inhaled
It receives tower top to enter, the unstripped gas entered with therefrom cold oil absorption tower lower part is inversely contacted in absorption tower, in absorption tower
It is filled with stainless steel helices.Therefrom the outflow of cold oil absorption system is rich in the C2+ liquid absorption liquid of propylene, into subsequent including separation
Device, refrigerator, alkynes allene select hydrogenation plant, domethanizing column, dethanizer, depropanizing tower (propylene propane separator)
The PDH product fractionation zone sequentially formed inside, finally obtains propylene product；The on-condensible gas rich in hydrogen flowed out from system,
Main component is hydrogen about 82.5%, methane about 4.5%, ethane 1.4%, propylene 3.2%, propane 8.2% and 0.1~
0.2% other impurity enter pressure-variable adsorption (PSA) after heat exchange to room temperature and propose hydrogen process；
(3) pressure-variable adsorption (PSA) proposes hydrogen process, and the room temperature that the pressure for absorbing process from middle cold oil is 3.5MPa is rich in hydrogen
On-condensible gas enters PSA and mentions absorption tower bottom in hydrogen system, wherein hydrogen-rich on-condensible gas flow is 100,000 mark sides/hour, suction
12, attached tower, series system, 3 adsorption tower absorption, remaining 9 adsorption tower are in drop pressure, inverse put, flushing, boost pressure
And product hydrogen fills each desorption procedure eventually, pressure number is 4 times, and normal pressure rinses regeneration；Adsorption operations temperature is room temperature,
Operating pressure is 3.4~3.5MPa；It is more than or equal to 99.99% hydrogen product, hydrogen from PSA system absorption tower top outflow purity
Product yield is more than or equal to 83~87%, wherein olefin impurity component total content is less than or equal to 0~10ppm, and 70% as circulation
Hydrogen is reacted with the mixing of propane feed gas back to PDH reaction zone, and 30% as defeated, 30% hydrogen product outside hydrogen product
In a part be also used to the alkynes selectively hydrogenating butadiene (SHP) in PDH product fractionation zone.It is flowed out from PSA adsorption tower bottom
Rich C2+ concentrated gas, a part directly exports as fuel gas, and another part further recycles C2+ by refrigeration and compression
And form liquid and enter PDH product fractionation zone acquisition propylene product, after the complete propane of unreacted is mixed back to propane feed gas
It is reacted into PDH reaction zone.PSA, which is mentioned, to be filled with activated alumina, silica gel, active carbon, divides in the adsorption tower in hydrogen system
The compound adsorbent of son sieve, passes through the control of the compositions such as the regulating valve being arranged in connecting pipe and sequence valve between adsorption tower
System processed carries out the control and adjusting of pressure change during PSA adsorption and desorption circulate operation.
Embodiment 2
As shown in Figure 1, on that basis of example 1, in unstripped gas containing 0.1~1.0% carbon dioxide (CO2), it is pre- to locate
Science and engineering sequence increases caustic wash tower, using containing 4~10% potassium hydroxide (KOH) lye as decarburization absorption agent, in unstripped gas
CO2Chemical absorbing is carried out, CO is removed2。
Embodiment 3
As shown in Fig. 2, the C2+ liquid rich in propylene that the cold oil absorption step flows out, i.e. absorbing liquid, are introduced into solution
Inhale tower, wherein desorber loads stainless steel helices, and desorption temperature is room temperature, and desorption pressures are normal pressure.It is flowed out from desorber bottom
Rich propane liquid, 60~70% be used as absorbent, after being overpressurized back to middle cold oil absorption tower be recycled, 30~40% into
Enter depropanizing tower, further recycles propane；The C2+ gas rich in propylene flowed out from desorber tower top, into subsequent including causing
Cold, gas-liquid separator, alkynes allene selection hydrogenation plant, domethanizing column, dethanizer, depropanizing tower sequentially form inside
PDH product fractionation zone separating-purifying, finally obtain propylene product, purified propylene is more than or equal to 99.9%.
Embodiment 4
As shown in figure 3, on the basis of embodiment 1 and 3, when containing more two in the unstripped gas of the pretreatment process
Carbonoxide (CO2), decarbonizing tower is added after desorber, uses organic amine for absorbent；The decarbonizing tower includes inhaling for decarburization
The decarburization absorption tower of receipts with and for decarburization desorption decarburization desorber；What therefrom cold oil desorber tower top flowed out is rich in propylene
C2+ gas is after decarburization absorption tower carries out decarburization, the C2+ gas of rich propylene after the decarburization that decarburization absorption column overhead flows out, then
Separating-purifying is carried out into subsequent PDH product fractionation zone, finally obtains propylene product；The decarburization of decarburization absorption tower tower bottom outflow is inhaled
It receives liquid and handles removing CO through decarburization desorber2Afterwards, recycling decarburization absorption agent is recycled and reused for decarburization absorption tower.
Embodiment 5
As shown in figure 4, the PSA mentions hydrogen system hydrogen unit is mentioned by two sections of PSA form, first segment PSA (1#PSA it) grasps
Operation mode is 12-3-4P, 12 adsorption towers, and 3 adsorption towers are in adsorbed state always, remaining 9 adsorption tower is in each solution
Inhale step, press for 4 times, normal pressure rinses, the fluid phase gas rich in hydrogen flowed out from adsorption tower tower top, density of hydrogen for 94~
97%, theatotal olefinsacontent is less than or equal to 0~5ppm, and therein 60~70% use as recycle hydrogen, and 30~40% enter with 10-
The second segment PSA (2 of 3-3P operation format#PSA hydrogen unit) is mentioned, that is, 10 adsorption towers, 3 adsorption towers therein are in always
Adsorbed state, remaining 7 adsorption tower are respectively at each desorption state, and tower top flows out the hydrogen that purity is 99.99% or more
Output of products, hydrogen product yield about 80~84%；The absorption phase gas of its tower bottom outflow is rich in methane, directly as fuel
Gas.From 1#PSA mentions the rich C2+ gas of the adsorption tower bottom outflow of hydrogen unit, mainly includes propylene, propane, into subsequent PDH points
It evaporates area and further recycles C2+, mainly include propylene and propane.
Embodiment 6
As shown in figure 5, the PSA mentions hydrogen system, the on-condensible gas of process is absorbed from cold oil, by heat exchange to 60~
70 DEG C, pressure be 3.5MPa under conditions of enter by level-one permeation hydrogen hydrogen membranous system, from per-meate side outflow be rich in hydrogen infiltration
It is ventilative, it is pressurized to pressure 3.5MPa needed for recycle hydrogen, it is directly entered PSA and mentions hydrogen system, adsorb tower top from it and flow out purity
Hydrogen more than or equal to 99.99%, yield are more than or equal to 90~95%；Wherein, a part of (60~70%) are used as circulating hydrogen
It is reacted with the mixing of propane feed gas back to PDH reaction zone, a part of (30~40%) are as defeated outside hydrogen product.It is solved
Air-breathing is exported directly as fuel gas and is used.The impermeable gas (gas rich in C2+) flowed out from the impermeable side of hydrogen membranous system,
It after supercooling, is directly entered PDH product fractionation zone and further recycles C2+, mainly include propylene and propane.
Embodiment 7
As shown in Figure 1, on that basis of example 1, the unstripped gas is propane (C3) and butane from PDH reaction zone
(C4) the reaction mixture gas body of gaseous mixture dehydrogenation producing propylene, methane therein, ethane, propane, butane equal size are more, remove propylene
Outside, the olefin(e) centent of C4+ increased, wherein the cold oil absorbs process, can be used cold in the replacement of shallow cold oil absorption technique
Oil absorbs, and absorbent uses C4 alkane, including normal butane or iso-butane or mixed butanes, and absorption pressure 3.5MPa absorbs temperature
Degree is 5~15 DEG C, and tower bottom outflow is rich in C2+ liquid absorption liquid, into subsequent including PDH product fractionation zone, finally obtains third
Alkene product, purity 99.9%；It is directly entered PSA from the on-condensible gas rich in hydrogen for absorbing tower top generation without heat exchange and mentions hydrogen
System is less than or equal to 5~20ppm from the olefin(e) centent in the recycle hydrogen and product hydrogen that tower top generates, and still meets recycle hydrogen rule
Fixed total olefin content is less than or equal to 0.05% and requires.At this point, regeneration increases vacuum step as far as possible.
Embodiment 8
On the basis of Fig. 1 and embodiment 1 or Fig. 4 and embodiment 5 or Fig. 5 and embodiment 6, cold oil absorbs obtained by process
Rich propylene liquid (absorbing liquid), after through PDH product fractionation zone, separating-purifying goes out product propylene, the remaining liquid rich in propane
(rich propane liquid, main includes for reacted propane) is reacted after returning to the mixing of propane feed gas into PDH reaction zone.
The specific embodiment of the application above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
The limitation to the application protection scope therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, under the premise of not departing from technical scheme design, various modifications and improvements can be made, these belong to this
The protection scope of application.
Claims (10)
1. preparing propylene by dehydrogenating propane reaction mixture gas cold oil absorbs the separation method coupled with PSA, which is characterized in that including as follows
Step:
(1) pretreatment process: the reactant mixed gas from PDH reaction zone is as unstripped gas, by heat exchange, dedusting, compression
The pretreatment process of composition, into next process, cold oil absorbs；
(2) cold oil absorbs process: being -45~-30 DEG C, operating pressure into operation temperature by the unstripped gas of pretreatment process
For the middle cold oil absorption system of 3.0~5.0MPa, enter from middle cold oil absorption tower lower part and with therefrom cold oil absorption tower top
After absorbent inversely contacts, therefrom cold oil absorption system outflow absorbing liquid enters PDH product fractionation zone treated product propylene,
The hydrogen-rich on-condensible gas that therefrom cold oil absorption system flows out enters PSA and proposes hydrogen process；
(3) PSA proposes hydrogen process: the hydrogen-rich on-condensible gas for absorbing process from cold oil, which enters PSA and mentions hydrogen system, to be handled；From
PSA mentions the hydrogen of hydrogen system tower top outflow, and a part returns to PDH reaction zone as circulating hydrogen and reacted, and another part is made
It is defeated outside product hydrogen or/and for the alkynes allene selective hydrogenation in PDH product fractionation zone；Hydrogen system tower is mentioned from PSA
Bottom bottom outflow stripping gas, directly as fuel gas, or as natural gas hydrogen preparation unstripped gas, or through processing formed liquid after enter
Further recycle C2+ in PDH product fractionation zone.
2. preparing propylene by dehydrogenating propane reaction mixture gas cold oil according to claim 1 absorbs the separation method coupled with PSA,
It is characterized by: preprocessed process treated unstripped gas removes institute through wet process decarbonization process before entering cold oil and absorbing process
Containing CO2。
3. described in any item preparing propylene by dehydrogenating propane reaction mixture gas cold oil absorb point coupled with PSA according to claim 1
From method, it is characterised in that: be provided with desorber between middle cold oil absorption tower and PDH product fractionation zone；It absorbs and flows out through cold oil
Absorbing liquid, be introduced into desorber, from desorber tower bottom flow out rich propane liquid, a part be used as absorbent, through being overpressurized
It is recycled afterwards back to middle cold oil absorption tower, another part is for further recycling propane；The richness flowed out from desorber tower top
C2+ gas containing propylene obtains product propylene after the processing of PDH product fractionation zone.
4. absorbing point coupled with PSA according to the described in any item preparing propylene by dehydrogenating propane reaction mixture gas cold oil of claim 3
From method, it is characterised in that: be provided with decarbonizing tower after the desorber；Propylene is rich in the outflow of therefrom cold oil absorption tower tower top
C2+ gas carry out decarburization after, enter back into PDH product fractionation zone processing after product propylene.
5. preparing propylene by dehydrogenating propane reaction mixture gas cold oil according to claim 1 absorbs the separation method coupled with PSA,
Hydrogen process is proposed into PSA after hydrogen-rich on-condensible gas obtained in process is exchanged heat to room temperature it is characterized by: absorbing in cold oil；It is right
It answers, the operation temperature that PSA mentions hydrogen system is room temperature, and operating pressure is 3.0~5.0MPa；Wherein, PSA mentions hydrogen system and contains by going here and there
Connection or it is in parallel or go here and there and the PSA adsorption tower group that connects at, and PSA adsorption tower pass through vacuumize product gas flushing or vacuumize and
Product gas flushing combines or the method desorption and regeneration of desorption with pressure.
6. preparing propylene by dehydrogenating propane reaction mixture gas cold oil according to claim 1 absorbs the separation method coupled with PSA,
It is characterized by: absorbing hydrogen-rich on-condensible gas obtained in process without heat exchange in cold oil, or the shallow cold temperature -30 that exchanged heat into
Enter PSA after~30 DEG C and proposes hydrogen process；Corresponding, the operating pressure that PSA mentions hydrogen system is 3.0~5.0MPa；Wherein, PSA is mentioned
Hydrogen system is by least two PSA adsorption tower groups at and PSA adsorption tower is by vacuumizing desorption and regeneration；
Or, hydrogen-rich gas obtained in cold separation process is exchanged heat to entering PSA after 60~120 DEG C of medium temperature and proposes hydrogen process in；
Corresponding, the operating pressure that PSA mentions hydrogen system is or 3.0~5.0MPa or 0.5~3.0MPa；Wherein, PSA mention hydrogen system by
At least two PSA adsorption tower groups are at and PSA adsorption tower is by vacuumizing desorption and regeneration.
7. preparing propylene by dehydrogenating propane reaction mixture gas cold oil according to claim 1 absorbs the separation method coupled with PSA,
It is characterized by: the PSA is mentioned in hydrogen process, the PSA mentions hydrogen system and mentions hydrogen unit by two sections of PSA, 1#PSA and 2#PSA group
At, it is each mention hydrogen unit by least two PSA adsorption tower groups at；The hydrogen-rich on-condensible gas that process is absorbed from cold oil, first through 1#
After PSA processing, from 1#The fluid phase gas rich in hydrogen of PSA tower top outflow, a part are used directly as circulating hydrogen,
Another part enters 2#PSA proposes hydrogen cell processing；Through 2#PSA processing, from 2#The hydrogen output of pSA tower top outflow is used as product hydrogen
Gas or/and alkynes allene selective hydrogenation for PDH product fractionation zone, from 2#The stripping gas of pSA tower bottom outflow is directly used
Make fuel gas, or, exporting as natural gas hydrogen preparation unstripped gas；From 1#The rich C2+ gas of PSA tower bottom outflow, after cooling pressure regulation,
Or cold oil recovery process is returned to, or enter PDH product fractionation zone, further to recycle C2+ component.
8. preparing propylene by dehydrogenating propane reaction mixture gas cold oil according to claim 1 absorbs the separation method coupled with PSA,
It is characterized by: the PSA is mentioned in hydrogen process, the hydrogen-rich on-condensible gas of process is absorbed from cold oil, pressure be 3.0~
Under the conditions of 5.0MPa, temperature are 60~120 DEG C, into the hydrogen membranous system processing by one or more levels permeation hydrogen；From hydrogen membranous system
The infiltration gas of per-meate side outflow, is compressed to after pressure needed for circulating hydrogen to enter PSA and mention hydrogen system and mentions hydrogen, from PSA adsorption system
Tower top outflow hydrogen, a part as circulating hydrogen be used for PDH reaction zone, another part as product hydrogen output or/and
For the alkynes allene selective hydrogenation of PDH product fractionation zone, the stripping gas that is flowed out from PSA adsorption system tower bottom directly as
Fuel gas output, or, being exported as natural gas hydrogen preparation unstripped gas；The rich C2+ gas flowed out from the impermeable side of hydrogen membranous system, through cold
But it after pressure regulation, or returns to cold oil and absorbs process, or enter PDH product fractionation zone, further to recycle C2+ component.
9. described in any item preparing propylene by dehydrogenating propane reaction mixture gas cold oil absorptions are coupled with PSA according to claim 1~8
Separation method, it is characterised in that: mention in hydrogen process in the PSA, for the hydrogen exported after PSA proposes hydrogen system processing, use
Ratio as the hydrogen that circulating hydrogen uses between the hydrogen as the output of product hydrogen, or, being used as what circulating hydrogen used
Hydrogen and for the ratio between the hydrogen of PDH product fractionation zone, can be adjusted according to circulating hydrogen internal circulating load, to protect
Card meets the strict demand of recycle hydrogen tolerance in PDH reaction zone.
What 10. preparing propylene by dehydrogenating propane reaction mixture gas cold oil absorption as described in any one of claims 1 to 9 was coupled with PSA
The application of separation method: the FTrPSA mentions hydrogen methods, in addition to the process for being suitable for preparing propylene by dehydrogenating propane, applies also for wrapping
Include the dehydrogenation producing propylene or dehydrogenation etherificate methyl tertiary butyl ether(MTBE) processed, ethyl uncle of propane and butane or butane and pentane mixed raw material
During butyl ether, tert amyl methyl ether(TAME), tertiary amyl ethyl ether, the circulating hydrogen of dehydrogenation gaseous mixture and or product hydrogen separation
It extracts.
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