CN109851584A - The refining methd and device of epoxyalkane - Google Patents
The refining methd and device of epoxyalkane Download PDFInfo
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- CN109851584A CN109851584A CN201810153562.8A CN201810153562A CN109851584A CN 109851584 A CN109851584 A CN 109851584A CN 201810153562 A CN201810153562 A CN 201810153562A CN 109851584 A CN109851584 A CN 109851584A
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Abstract
The present invention relates to a kind of refining methd of epoxyalkane and devices, mainly solve the problems, such as that heavy constituent impurities accumulation causes the decline of extractant purity, loss to increase in the prior art, the decline of epoxyalkane yield, energy consumption increase.The refining methd, comprising: a) the crude product logistics containing epoxyalkane and extractant stream enter first rectifying column, and tower top obtains thick contaminant stream, and tower bottom obtains the first thick extractant stream；B) the described first thick extractant stream enters the knockout tower with the first reboiler, and tower top obtains epoxyalkane product, and tower bottom obtains third―party logistics；C) at least part in the third―party logistics enters extractant clarifier, and obtained gas phase light component returns to the knockout tower, and liquid phase heavy constituent impurity thing flows away post-processing.
Description
Technical field
The present invention relates to a kind of refining methd of epoxyalkane and devices.
Background technique
Propylene oxide (PO) is mainly used for the production of polyether polyol, propylene glycol and propylene glycol, in acryloyl derivative
Yield be only second to polypropylene, be the second largest acryloyl derivative.According to statistics, 2011, the whole world was for polyether polyols alcohol production
Propylene oxide accounts for about the 66% of aggregate consumption, accounts for about 17% for propylene glycol production, the epoxy third for propylene glycol production
Alkane accounts for about 6%.2011, global propylene oxide production capacity was 882.2 ten thousand tons, had broken through 10,000,000 tons within 2016.Expect 2020
Year, production of propylene oxide ability is up to 12,000,000 tons/year, and demand reaches 10,000,000 tons/year.On long terms, world wide
Interior propylene oxide market prospects are still optimistic.
1,2- epoxy butane (BO) same to ethylene oxide (EO) and propylene oxide (PO) belong to homologue, molecular formula C4H8O(CAS
Number: be a kind of substance with three-membered ring structures 106-88-7), chemical property is active, be mainly used as polyether polyols alcohol monomer and
The intermediate of other synthetic materials.It is living that 1,2- epoxy butane can be also used for foamed plastics processed, synthetic rubber, non-ionic surface
Property agent etc., can also replace diluent of the acetone as nitrate paint, it is also possible to make the standard substance of chromatography.
As olefin epoxide, compared with ethylene oxide and propylene oxide, on molecular structure, epoxy butane possesses more
- the CH of multi-quantity2Functional group, when as monomer synthesizing polyether glycol, product has excellent hydrophobic performance, especially
Suitable for certain outer surface waterproof coatings for requiring stringent building and equipment.Meanwhile institute is copolymerized by monomer of epoxy butane
The polyurethane material of synthesis possesses excellent cold tolerance, especially suitable for weather severe cold area.
Epoxyalkane product has strict demand to water, aldehyde, isomer, and water will affect the hydroxyl value and foaminess of polymer
Can, aldehyde will lead to product and give off a peculiar smell, and influence people's health, and isomer is the end-capping reagent for polymerizeing long-chain, therefore, state
There is strict demand to product purity in mark and company standard.
National standard oxypropylene high-class product quality purity requirement are as follows: propylene oxide >=99.95%, water≤0.02%, acetaldehyde+
Propionic aldehyde≤0.005%, acid≤0.003%.
1,2- epoxy butane qualified product quality purity requirement in BASF company standard are as follows: epoxy butane >=99.5%, epoxy
Butane isomer≤0.2%, total aldehyde≤0.05%, water≤0.03%.
1,2- epoxy butane high-class product quality purity requirement are as follows: epoxy butane >=99.9%, epoxy butane isomer
≤ 0.1%, total aldehyde≤0.015%, water≤0.005%.
It reacts in the thick epoxyalkane generated and usually contains the impurity such as water, methanol, acetone, methyl formate, because these are miscellaneous
Matter and epoxyalkane form azeotropic mixture or relative volatility close to 1, and conventional distillation is difficult to reach epoxyalkane product standard.For
It obtains meeting the high-purity epoxyalkane that polymerization requires, it is necessary to be separated off the impurity contained in epoxyalkane.
The purifying of epoxyalkane generally uses C7~C20 straight chain and branch hydro carbons and (or) glycols as extractant.From
Economy considers that the purification process of epoxyalkane is using the mixture of C8 straight chain and branched paraffin as extractant.Extractant
Addition so that acetaldehyde, water, methanol, methyl formate is become larger the relative volatility of epoxyalkane, acetaldehyde, water, methanol, methyl formate from
Tower top removes, and extractant recycles.
Because containing water, methanol in thick epoxy butane, water is added in when separation again, therefore, in epoxy butane subtractive process,
Following reaction can occur:
The hydrolysis of 1,2- epoxy butane generates 1,2- butanediol.The solubility of 1,2- butanediol in water is less than 1,2- epoxy fourth
Alkane.
1,2- epoxy butane reacts generation 1- butanediol monomethyl ether with methanol, and (ehter bond is formed in the carbon atom of terminal epoxy groups
On), 2- butanediol monomethyl ether (ehter bond is formed on the carbon atom of 2 epoxy groups).1- butanediol monomethyl ether and 2- butanediol list
Methyl ether is all slightly soluble in water.
1,2- epoxy butane occurs polymerization reaction and generates polymer, such as two polybutylene oxides, polybutylene oxide.
1,2- epoxy butane is reacted with compounds containing reactive hydrogen such as water, dihydric alcohol or polyalcohols generates poly- 1,2- butanediol
Ether and its derivative.Poly- 1,2- butanediol ethere and its derivative are fixedness thick liquids, colourless to brown, are mostly dissolved in
Ketone, alcohol, ester, hydro carbons and halogenated hydrocarbons；Molecular weight is lower to be dissolved in water, and the water-soluble decline with molecular weight increase increases with temperature
And decline.
The above byproduct of reaction and derivative are insoluble in water mostly, are difficult to remove by the method for washing.Using extraction essence
When the method evaporated carries out epoxy butane purification, these by-products and derivative can be accumulated in extractant, to reduce extraction
The effect of extracting of agent.So reducing the concentration of these by-products and derivative in extractant is very important.For example, document
US4402794 discloses the hydro carbons using C7-C9, and preferably normal octane is as thick 1, the 2- epoxy fourth of extractant single separation of extractive distillation
The impurity such as the water, methanol, acetone, the methyl formate that contain in alkane solution are not involved with the separation of impurity aldehydes.Extraction distillation column
Organic layer after the layering of tower top phase-splitter removes rectifying column distillation separation methanol, acetone etc.；Extraction is sent into extraction distillation column tower reactor logistics
Take rectifying column；Extractive distillation column tower bottoms part outlet.This method passes through tower bottoms of the outlet part containing extractant and heavy constituent,
To reduce the accumulation of byproduct of reaction and derivative in extractant.Due to the heavy constituent content in tower reactor outlet fraction of stream
It is low, to guarantee extractant purity, it is necessary to a large amount of extractant of outlet, thus larger amount of extractant can be lost.
Document US4772732 discloses a kind of by using anion exchange resin and adsorbent purifying butene oxide
Method.Anion exchange resin removes acid and dehydrogenation impurity, and adsorbent removes the water of the impurity from epoxy butane.According to miscellaneous
Matter content, purification step can carry out alone or in combination, and the process can be conducted batch-wise in the reactor, or in tower or
It is carried out continuously in column.Selected ion exchange resin is the big netted anion exchange resin of sulfonation, and adsorbent is molecular sieve.
This method higher cost, absorption resolving also can be cumbersome, and treating capacity is little.
Equally, in propylene oxide system, propylene oxide hydrolysis generates 1,2-PD.1,2- propylene glycol in water molten
Xie Du is less than propylene oxide.
Propylene oxide is reacted with methanol generates propylene glycol monomethyl ether.
Propylene oxide occurs polymerization reaction and generates polymer, such as two polypropylene oxide, polypropylene oxide.
Propylene oxide is reacted with compounds containing reactive hydrogen such as water, dihydric alcohol or polyalcohols to be generated polypropylene glycol ether and its spreads out
Biology.Solubility is all little in the solubility and organic phase of polypropylene glycol ether and its derivative in water.
The current status of the prior art is, it would be highly desirable to need a kind of extractant to lose small, with high purity, epoxyalkane high income,
The small epoxyalkane refining methd of energy consumption and device.
Summary of the invention
The present inventor has found by diligent system research on the basis of existing technology, by being configured with one in conventional
An extractant clarifier is added in the bottom of the knockout tower of a reboiler again, so that it may solve the problems, such as that at least one is aforementioned, and
It has thus completed the present invention.
Specifically, the present invention relates to a kind of refining methds of epoxyalkane, comprising the following steps:
A) the crude product logistics containing epoxyalkane and extractant stream enter first rectifying column, and tower top obtains thick impurity thing
Stream, tower bottom obtain the first thick extractant stream；
B) the described first thick extractant stream enters the knockout tower with the first reboiler, and tower top obtains epoxyalkane production
Product, tower bottom obtain third―party logistics；
C) at least part in the third―party logistics enters extractant clarifier, described in obtained gas phase light component return
Knockout tower, liquid phase heavy constituent impurity thing flow away post-processing.
According to an aspect of the present invention, first reboiler is thermosyphon reboiler, kettle type reboiler or pressure
It is any in circulating reboiler；The extractant clarifier is destilling tower or the second reboiler, preferably the second reboiler.
According to an aspect of the present invention, the ratio between the first reboiler heat exchange area and the second reboiler heat exchange area be (8~
2):1。
According to an aspect of the present invention, in the third―party logistics, the part into extractant clarifier is the third
The 2~20% of logistics weight.
According to an aspect of the present invention, the method also includes:
D) the thick contaminant stream enters phase-splitter, obtains water phase and organic phase；The water phase goes to post-process；It is described organic
Mutually a part returns to the first rectifying column, and another part enters Second distillation column；The Second distillation column tower top is obtained containing light
The logistics of composition impurity, tower bottom obtain the second thick extractant stream；The second thick extractant stream enters the knockout tower.
According to an aspect of the present invention, the epoxyalkane is propylene oxide, epoxy butane or its isomer.
According to an aspect of the present invention, in the crude product logistics containing epoxyalkane, by weight percentage, epoxy
The content of alkane is 98~99.9%.
According to an aspect of the present invention, the crude product logistics containing epoxyalkane is originated from epoxidation reaction of olefines device stream
Effluent stream.
According to an aspect of the present invention, the thick contaminant stream enters back into the split-phase after contacting with the water logistics of introducing
Device.
According to an aspect of the present invention, the part of the extractant clarifier is not entered in the third―party logistics, is entered
The first rectifying column.
According to an aspect of the present invention, the part of the extractant clarifier is not entered in the third―party logistics, is entered
The first rectifying column and the phase-splitter.
According to an aspect of the present invention, in the part that the extractant clarifier is not entered in the third―party logistics, into
Entering the first rectifying column and entering the weight ratio of the phase-splitter is (100~1000): 1.
The invention further relates to a kind of refining plants of epoxyalkane.Described device includes:
1) first rectifying column；It is configured to receive crude product logistics and extractant stream, discharge tower top containing epoxyalkane
Thick contaminant stream and the discharge thick extractant stream of tower bottom first；
2) knockout tower；It is configured to receive the described first thick extractant stream, discharge tower top epoxyalkane product stream, with
And discharge tower bottom third―party logistics；The knockout tower tower reactor is configured with the first reboiler；
3) extractant clarifier；It is configured to receive a part of third―party logistics, discharge gas phase light component stream and
Discharge the logistics of liquid phase heavy constituent；The gas phase light component stream returns to the knockout tower.
According to an aspect of the present invention, first reboiler is thermosyphon reboiler, kettle type reboiler or pressure
It is any in circulating reboiler；The extractant clarifier is destilling tower or the second reboiler, preferably the second reboiler.
According to an aspect of the present invention, the ratio between the first reboiler heat exchange area and the second reboiler heat exchange area be (5~
2):1。
According to an aspect of the present invention, described device further include: d) phase-splitter；It is configured to receive the thick impurity thing
Stream is to form water phase and organic phase；The water phase goes to post-process.
According to an aspect of the present invention, described device further include: e) Second distillation column；It is configured to receive a part of institute
The logistics and the thick extractant stream of discharge tower bottom second stated organic phase, discharge tower top impurity containing light component；The organic phase
Another part returns to the first rectifying column；The second thick extractant stream enters the knockout tower.
Beneficial effects of the present invention: the present invention adds one in the bottom of the conventional knockout tower configured with a reboiler again
A extractant clarifier, preferred embodiment is that separation tower bottom adds a reboiler again, by being partially separated for original directly outlet
The logistics of tower tower reactor is handled through extractant clarifier, isolates heavy constituent impurity, to improve extractant purity, reduces extraction
The loss and energy consumption of agent, improve the yield of epoxyalkane, and extractant purity improves 0.1~2%, and extractant loss 0.1~
1.0%, energy consumption reduces 1~10%, and epoxyalkane yield improves 0.5~5%, and impurity elimination factor improves 5~35%.
Detailed description of the invention
Fig. 1 is the schematic diagram of the method for the invention and device.
Fig. 2 is the schematic diagram of another embodiment of the present invention.
Fig. 3 is the flow diagram of existing technical literature US4402794 the method.
In the accompanying drawings, identical component uses identical appended drawing reference.Attached drawing is not according to actual ratio.
Description of symbols:
The 1 crude product logistics containing epoxyalkane
2 first thick extractant streams
3 thick contaminant streams
4 water logistics introduced
Thick contaminant stream after 5 moisturizings
The organic phase of 6 phase-splitters outflow
7 go the organic phase of first rectifying column
8 go the organic phase of Second distillation column
The water phase of 9 phase-splitters outflow
The logistics of 10 impurity containing light component
11 second thick extractant streams
12 third―party logistics
13 epoxyalkane product streams
14 first reboiler feed streams
15 first reboiler output streams
16 extractant clarifier feed streams
17 extractant clarifier output streams
18 heavy constituent contaminant streams-outlet logistics
Enter the part of first rectifying column in 19 third―party logistics
20 third―party logistics enter the part of phase-splitter
A first rectifying column
B phase-splitter
C Second distillation column
D knockout tower
The first reboiler of E
F extractant clarifier
The present invention is described in detail with reference to the accompanying drawing, it should be noted however that protection scope of the present invention is simultaneously
It is not limited, it but is determined by the appended claims.
All publications, patent application, patent and the other bibliography that this specification is mentioned all are incorporated by reference into
Herein.Unless otherwise defined, all technical and scientific terms used herein all there are those skilled in the art routinely to manage
The meaning of solution.In case of conflict, it is subject to the definition of this specification.
When this specification with prefix " well known to those skilled in the art ", " prior art " or its export material similar to term
Whens material, substance, method, step, device or component etc., object derived from the prefix is covered this field when the application proposes and is routinely made
Those of with, but also include also being of little use at present, it will but become art-recognized for suitable for those of similar purpose.
In the context of the present specification, other than the content clearly stated, any matters or item that do not mention are equal
It is directly applicable in those of known in the art without carrying out any change.Moreover, any embodiment described herein can be with
It is freely combined with one or more other embodiments described herein, the technical solution or technical idea formed therefrom regards
For the original disclosure of the present invention or a part of original description, and be not considered as not disclosing or be expected herein it is new in
Hold, unless those skilled in the art think that the combination is obvious unreasonable.
In the case where not clearly indicating, all percentages, number, the ratio etc. being previously mentioned in this specification be all with
On the basis of weight, unless not meeting the conventional understanding of those skilled in the art when using weight as benchmark.
In the case where not clearly indicating, the pressure being previously mentioned in this specification is relative pressure.
Raw material used in purification process of the invention is the crude product logistics containing epoxyalkane.The logistics is originated from olefin epoxide
Change reactor effluent stream.In the logistics, the content of epoxyalkane is 98~99.9 weight %.In the logistics also containing water, alcohol,
The light components impurity such as acid, ketone, aldehyde, ester, such as water, methanol, acetic acid, acetaldehyde, propionic aldehyde, acetone, methyl formate or theirs is mixed
Close object.Also containing in subtractive process in the logistics, it is impossible to avoid the heavy constituent impurity for generating and accumulating；It is with epoxy butane
Example, these heavy constituent impurity include 1,2- butanediol, 1- butanediol monomethyl ether, 2- butanediol monomethyl ether, two polybutylene oxides, gather
Epoxy butane, poly- 1,2- butanediol ethere and its derivative or their mixture；By taking propylene oxide as an example, these heavy constituents
Impurity includes 1,2-PD, propylene glycol monomethyl ether, two polypropylene oxide, polypropylene oxide, polypropylene glycol ether and its derivative,
Or their mixture.
According to the present invention, the crude product logistics 1 containing epoxyalkane and extractant stream enter first rectifying column A, and tower top obtains
To thick contaminant stream 3, tower bottom obtains the first thick extractant stream 2.Contain most light group in logistics 1 in thick contaminant stream 3
Divide impurity.Contain most epoxyalkane product and heavy constituent impurity in logistics 1 in first thick extractant stream 2.Wherein, extract
It takes agent logistics to can be fresh extractant, is also possible to extractant-third―party logistics of knockout tower tower bottom recycling.
The extractant that epoxyalkane purification uses is known.Generally using C7~C20 straight chain and branch hydro carbons and
(or) glycols is as extractant.From economic considerations, using the mixture of C8 straight chain and branched paraffin as extractant, such as
Normal octane, isooctane, 2- methyl-heptan.From extractant cost consideration is reduced, mixture is preferably selected.
The extracting rectifying condition of crude product logistics and extractant stream containing epoxyalkane in first rectifying column includes: tower
30~80 DEG C of temperature of top, 0.04~0.40MPaG of pressure.
According to the present invention, the first thick extractant stream 2 enters knockout tower D, and tower top obtains epoxyalkane product stream 13, tower
Bottom obtains third―party logistics 12.The bottom knockout tower D is equipped with the first reboiler E and extractant clarifier F, the first reboiler feed stream
Tower bottoms is sent into the first reboiler E by 14, and the first reboiler output streams 15, the first reboiler output streams 15 are obtained after heating
Into the lower part knockout tower D.A part (extractant clarifier feed stream 16) in third―party logistics 12 enters extractant clarifier
F obtains extractant clarifier F output streams 17 (gas phase light component) after heating, extractant clarifier F output streams 17, which are sent into, to be divided
From the lower part tower D, heavy constituent contaminant stream 18 is discharged from the extractant bottom clarifier F.In Fig. 1, removes and enter in third―party logistics 12
The remainder of extractant clarifier F, the extractant as extracting rectifying enter first rectifying column A.
According to the present invention, the first reboiler is in thermosyphon reboiler, kettle type reboiler or forced cyclic type reboiler
It is any.
According to the present invention, extractant clarifier is destilling tower or the second reboiler, from equipment investment and occupied area angle
Comprehensively consider, preferably the second reboiler.First reboiler be thermosyphon reboiler, kettle type reboiler or forced cyclic type again
Boil any in device, preferred kettle type reboiler.
According to the present invention, the ratio between the first reboiler heat exchange area and the second reboiler heat exchange area are (8~2): 1, second
Reboiler area is less than the first reboiler, and device driving the second reboiler of initial stage can not be opened, and the second reboiler does not influence
First reboiler.
According to the present invention, in third―party logistics 12, the part (logistics 16) into extractant clarifier is 12 weight of third―party logistics
The 2~20% of amount.
The preferred solution of the invention is to add one again in the bottom of the Chang Gui knockout tower configured with a reboiler to boil again
Device, that is to say, that separation tower bottom is configured with two reboilers.This can save equipment investment, simultaneously for new device
Extractant loss amount is reduced, product quality is improved；It is also particularly suitable for old plant modification upgrading, change amplitude is small, puts into low, reduction
Extractant loss amount, effect are obvious.
According to the present invention, the operating condition of the knockout tower includes: 30~80 DEG C of tower top temperature, and pressure 0.04~
0.40MPaG。
According to the present invention, in the described first thick extractant stream 2, with molar percent, extractant and epoxyalkane
Ratio is (2~15): 1, preferably (3~10): 1, more preferable (5~7): 1.
According to the present invention, thick contaminant stream 3 enters phase-splitter B, after split-phase, obtains water phase 9 and organic phase 6.After water phase 9 is gone
Processing.A part (logistics 7) of organic phase returns to first rectifying column A, and another part (logistics 8) enters Second distillation column C；It returns
The part of first rectifying column A meets the needs of first rectifying column overhead reflux.Second distillation column C tower top is obtained containing light component
The logistics 10 of impurity, most of light component impurity in raw material is discharged out-of-bounds as a result,.It is thick that Second distillation column C tower bottom obtains second
Extractant stream 11, the second thick extractant stream 11 likewise enter knockout tower D, recycle extractant, and the heavy constituent that carrying is discharged is miscellaneous
Matter.
A preferred embodiment according to the present invention, in order to preferably separate organic phase and water phase, preferred embodiment is phase-splitter B
Water is supplemented before thick contaminant stream 3 is sent into phase-splitter B, can preferably strengthen split-phase effect.The water of supplement is with the shape of water phase
Formula outlet, does not increase the separating difficulty of system, while obtaining better separating effect.
A preferred embodiment according to the present invention, is shown in Fig. 2, the isolated third―party logistics 12 of knockout tower D tower bottom remove into
The part for entering extractant clarifier is divided into two strands, wherein one 19 feeding first rectifying column A, in addition one 20 feeding phase-splitter B
In.In phase-splitter B, it is soluble in the aqueous phase after heavy constituent impurity part split-phase contained by logistics 20 and is discharged system, heavies removal effect
Fruit is more obvious.Logistics 19 and the weight ratio of logistics 20 are (100~1000): 1.
Extractant passes through after extractant clarifier, and the impurity content of good water solubility and poorly water-soluble is greatly lowered,
Enter phase-splitter by the purified extractant of extractant clarifier, Phase separation efficiency can be improved, reduces impurity in the first essence
Evaporate tower accumulating.
Heretofore described impurity elimination factor refers to: despumation accounts for all impurity in system, and (thick epoxyalkane is brought into
And generate in subtractive process) ratio.Using the method for the present invention, impurity elimination factor is more excellent greater than 80%, preferably greater than 90%
Choosing is greater than 96%.
It should be noted that the separating effect of extracting rectifying is certain in the case that extractant purity is constant.But this hair
It is bright, it is emphasized that side reaction can occur in subtractive process generates glycol and its derivative impurity, and the generation of these impurity is
Inevitably, and these impurity can in system accumulation cycle.These impurity are reactions to extracting rectifying, reduce extraction
Agent effect of extracting.If direct outlet extractant, because heavy constituent impurity content is low in extractant, direct outlet, extractant damage
Vector is big.The present invention increases only a small-sized extractant clarifier, so that it may which the heavy constituent concentration in outlet logistics 18 is improved 1
Times or more, outlet extractant loss amount reduces by more than 50.Using the present invention, in the identical situation of the outer discharge capacity of extractant, pass through
Long-term operation, heavy constituent impurity content is the 50% of direct outlet scheme in cycling extraction agent.And if using direct outlet
Scheme must just reduce epoxyalkane yield, otherwise not can guarantee product quality to improve the product quality of epoxyalkane.
Fig. 3 is the prior art, and the first rectifying is sent into the crude product logistics 1 and extractant stream 19 for containing 1,2- epoxy butane
Tower A, first rectifying column A tower bottom obtain the first thick extractant stream 2 and are sent into knockout tower D, and first rectifying column A tower top obtains thick impurity thing
Stream 3 is sent into phase-splitter B, the isolated water phase 9 of phase-splitter B and organic phase 6, and organic phase a part 7 is sent into first rectifying column A, is had
Machine phase another part 8 is sent into Second distillation column C, the isolated light component contaminant stream 10 of Second distillation column C tower top, the second rectifying
The thick extractant stream (11) of tower C tower bottom isolated second is sent into knockout tower D, isolated 1, the 2- epoxy fourth of knockout tower D tower top
Alkane product stream 13, the isolated third―party logistics 12 of knockout tower D tower bottom, it is three strands that third―party logistics 12, which divide, one 19 feeding first
Rectifying column A, in addition one 20 be sent into phase-splitter B, in addition one 18 as heavy constituent contaminant stream be discharged out-of-bounds.This method due to
By the agent of outlet partial extraction and heavy constituent to reduce the accumulation of byproduct of reaction and derivative in extractant, thus can lose
Larger amount of extractant.
Below by specific embodiment, the invention will be further elaborated.
Specific embodiment
[embodiment 1]
According to process flow shown in Fig. 1, extractant is normal octane, the crude product logistics of the epoxy butane Han 1,2- with containing just pungent
The extractant stream of alkane enters first rectifying column.With molar percent, extractant and 1, the ratio of 2- epoxy butane is 8:1,
It separates tower reboiler E and uses thermosyphon reboiler, extractant clarifier F is thermosyphon reboiler, reboiler E and reboiler
The ratio between F heat exchange area is 5:1, and entering the part of extractant clarifier in third―party logistics is the 3% of third―party logistics weight.
First rectifying column operating condition are as follows: pressure 0.042MPaG, 75 DEG C of tower top temperature.
Second distillation column operating condition are as follows: pressure 0.04MPaG, 60 DEG C of tower top temperature.
Knockout tower operating condition are as follows: pressure 0.04MPaG, 45 DEG C of tower top temperature.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 99.81% separate tower bottom extractant
Purity 99.0%, extractant loss 0.68%, impurity elimination factor are 98.0%.
[embodiment 2]
According to process flow shown in Fig. 1, extractant is normal octane, the crude product logistics of the epoxy butane Han 1,2- with containing just pungent
The extractant stream of alkane enters first rectifying column.With molar percent, extractant and 1, the ratio of 2- epoxy butane is 7:1,
It separates tower reboiler E and uses thermosyphon reboiler, extractant clarifier F is kettle type reboiler, and reboiler E is changed with reboiler F
The ratio between heat area is 5:1, and entering the part of extractant clarifier in third―party logistics is the 5% of third―party logistics weight.
First rectifying column operating condition are as follows: pressure 0.10MPaG, 60 DEG C of tower top temperature.
Second distillation column operating condition are as follows: pressure 0.09MPaG, 52 DEG C of tower top temperature.
Knockout tower operating condition are as follows: pressure 0.09MPaG, 45 DEG C of tower top temperature.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 99.82% separate tower bottom extractant
Purity 99.0%, extractant loss 0.73%, impurity elimination factor are 98.2%.
[embodiment 3]
According to process flow shown in Fig. 1, extractant is normal octane, the crude product logistics of the epoxy butane Han 1,2- with containing just pungent
The extractant stream of alkane enters first rectifying column.With molar percent, extractant and 1, the ratio of 2- epoxy butane is 6:1,
It separates tower reboiler E and uses thermosyphon reboiler, extractant clarifier F is kettle type reboiler, and reboiler E is changed with reboiler F
The ratio between heat area is 5:1, and entering the part of extractant clarifier in third―party logistics is the 8% of third―party logistics weight.
First rectifying column operating condition are as follows: pressure 0.20MPaG, 50 DEG C of tower top temperature.
Second distillation column operating condition are as follows: pressure 0.19MPaG, 48 DEG C of tower top temperature.
Knockout tower operating condition are as follows: pressure 0.18MPaG, 45 DEG C of tower top temperature.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 99.86% separate tower bottom extractant
Purity 99.0%, extractant loss 0.76%, impurity elimination factor are 98.4%.
[embodiment 4]
According to process flow shown in Fig. 1, extractant is normal octane, the crude product logistics of the epoxy butane Han 1,2- with containing just pungent
The extractant stream of alkane enters first rectifying column.With molar percent, extractant and 1, the ratio of 2- epoxy butane is 5:1,
It separates tower reboiler E and uses thermosyphon reboiler, extractant clarifier F is kettle type reboiler, and reboiler E is changed with reboiler F
The ratio between heat area is 5:1, and entering the part of extractant clarifier in third―party logistics is the 10% of third―party logistics weight.
First rectifying column operating condition are as follows: pressure 0.30MPaG, 40 DEG C of tower top temperature.
Second distillation column operating condition are as follows: pressure 0.28MPaG, 43 DEG C of tower top temperature.
Knockout tower operating condition are as follows: pressure 0.29MPaG, 45 DEG C of tower top temperature.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 99.90% separate tower bottom extractant
Purity 99.0%, extractant loss 0.77%, impurity elimination factor are 98.6%.
[embodiment 5]
According to process flow shown in Fig. 1, extractant is normal octane, the crude product logistics of the epoxy butane Han 1,2- with containing just pungent
The extractant stream of alkane enters first rectifying column.With molar percent, extractant and 1, the ratio of 2- epoxy butane is 4:1,
It separates tower reboiler E and uses thermosyphon reboiler, extractant clarifier F is kettle type reboiler, and reboiler E is changed with reboiler F
The ratio between heat area is 5:1, and entering the part of extractant clarifier in third―party logistics is the 13% of third―party logistics weight.
First rectifying column operating condition are as follows: pressure 0.40MPaG, 30 DEG C of tower top temperature.
Second distillation column operating condition are as follows: pressure 0.36MPaG, 37 DEG C of tower top temperature.
Knockout tower operating condition are as follows: pressure 0.38MPaG, 45 DEG C of tower top temperature.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 99.87% separate tower bottom extractant
Purity 99.0%, extractant loss 0.80%, impurity elimination factor are 98.8%.
[embodiment 6]
According to process flow shown in Fig. 1, extractant is C8 paraffins mixture, the crude product logistics of the epoxy butane Han 1,2- and
Extractant stream containing normal octane enters first rectifying column.With molar percent, extractant and 1, the ratio of 2- epoxy butane
For 4:1, separate tower reboiler E and use thermosyphon reboiler, extractant clarifier F is kettle type reboiler, reboiler E with boil again
The ratio between device F heat exchange area is 5:1, and entering the part of extractant clarifier in third―party logistics is the 15% of third―party logistics weight.
First rectifying column operating condition are as follows: pressure 0.40MPaG, 30 DEG C of tower top temperature.
Second distillation column operating condition are as follows: pressure 0.36MPaG, 37 DEG C of tower top temperature.
Knockout tower operating condition are as follows: pressure 0.38MPaG, 45 DEG C of tower top temperature.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 99.86% separate tower bottom extractant
Purity 99.0%, extractant loss 0.83%, impurity elimination factor are 98.7%.
[embodiment 7]
According to process flow shown in Fig. 1, extractant is normal octane, the crude product logistics of the epoxy butane Han 1,2- with containing just pungent
The extractant stream of alkane enters first rectifying column.With molar percent, extractant and 1, the ratio of 2- epoxy butane is 6:1,
It separates tower reboiler E and uses thermosyphon reboiler, extractant clarifier F is kettle type reboiler, and reboiler E is changed with reboiler F
The ratio between heat area is 4:1, and entering the part of extractant clarifier in third―party logistics is the 7% of third―party logistics weight.
First rectifying column operating condition are as follows: pressure 0.26MPaG, 45 DEG C of tower top temperature.
Second distillation column operating condition are as follows: pressure 0.24MPaG, 45 DEG C of tower top temperature.
Knockout tower operating condition are as follows: pressure 0.22MPaG, 45 DEG C of tower top temperature.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 99.86% separate tower bottom extractant
Purity 99.0%, extractant loss 0.72%, impurity elimination factor are 98.9%.
[embodiment 8]
According to process flow shown in Fig. 1, extractant is normal octane, the crude product logistics of the epoxy butane Han 1,2- with containing just pungent
The extractant stream of alkane enters first rectifying column.With molar percent, extractant and 1, the ratio of 2- epoxy butane is 6:1,
It separates tower reboiler E and uses thermosyphon reboiler, extractant clarifier F is kettle type reboiler, and reboiler E is changed with reboiler F
The ratio between heat area is 3:1, and entering the part of extractant clarifier in third―party logistics is the 6% of third―party logistics weight.
First rectifying column operating condition are as follows: pressure 0.26MPaG, 45 DEG C of tower top temperature.
Second distillation column operating condition are as follows: pressure 0.24MPaG, 45 DEG C of tower top temperature.
Knockout tower operating condition are as follows: pressure 0.22MPaG, 45 DEG C of tower top temperature.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 99.87% separate tower bottom extractant
Purity 99.0%, extractant loss 0.71%, impurity elimination factor are 99.0%.
[embodiment 9]
According to process flow shown in Fig. 1, extractant is normal octane, the crude product logistics of the epoxy butane Han 1,2- with containing just pungent
The extractant stream of alkane enters first rectifying column.With molar percent, extractant and 1, the ratio of 2- epoxy butane is 6:1,
It separates tower reboiler E and uses thermosyphon reboiler, extractant clarifier F is kettle type reboiler, and reboiler E is changed with reboiler F
The ratio between heat area is 2:1, and entering the part of extractant clarifier in third―party logistics is the 6% of third―party logistics weight.
First rectifying column operating condition are as follows: pressure 0.26MPaG, 45 DEG C of tower top temperature.
Second distillation column operating condition are as follows: pressure 0.24MPaG, 45 DEG C of tower top temperature.
Knockout tower operating condition are as follows: pressure 0.22MPaG, 45 DEG C of tower top temperature.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 99.88% separate tower bottom extractant
Purity 99.0%, extractant loss 0.73%, impurity elimination factor are 98.9%.
[embodiment 10]
According to process flow shown in Fig. 1, extractant is normal octane, the crude product logistics of the epoxy butane Han 1,2- with containing just pungent
The extractant stream of alkane enters first rectifying column.With molar percent, extractant and 1, the ratio of 2- epoxy butane is 6:1,
It separates tower reboiler E and uses kettle type reboiler, extractant clarifier F is kettle type reboiler, reboiler E and reboiler F heat-transfer surface
The ratio between product is 2:1, and entering the part of extractant clarifier in third―party logistics is the 6% of third―party logistics weight.
First rectifying column operating condition are as follows: pressure 0.26MPaG, 45 DEG C of tower top temperature.
Second distillation column operating condition are as follows: pressure 0.24MPaG, 45 DEG C of tower top temperature.
Knockout tower operating condition are as follows: pressure 0.22MPaG, 45 DEG C of tower top temperature.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 99.88% separate tower bottom extractant
Purity 99.0%, extractant loss 0.73%, impurity elimination factor are 98.9%.
[embodiment 11]
According to process flow shown in Fig. 1, extractant is normal octane, the crude product logistics of the epoxy butane Han 1,2- with containing just pungent
The extractant stream of alkane enters first rectifying column.With molar percent, extractant and 1, the ratio of 2- epoxy butane is 6:1,
It separates tower reboiler E and uses forced cyclic type reboiler, extractant clarifier F is kettle type reboiler, reboiler E and reboiler F
The ratio between heat exchange area is 2:1, and entering the part of extractant clarifier in third―party logistics is the 6% of third―party logistics weight.
First rectifying column operating condition are as follows: pressure 0.26MPaG, 45 DEG C of tower top temperature.
Second distillation column operating condition are as follows: pressure 0.24MPaG, 45 DEG C of tower top temperature.
Knockout tower operating condition are as follows: pressure 0.22MPaG, 45 DEG C of tower top temperature.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 99.88% separate tower bottom extractant
Purity 99.0%, extractant loss 0.73%, impurity elimination factor are 98.9%.
[embodiment 12]
According to process flow shown in Fig. 2, extractant is normal octane, the crude product logistics of the epoxy butane Han 1,2- with containing just pungent
The extractant stream of alkane enters first rectifying column.With molar percent, extractant and 1, the ratio of 2- epoxy butane is 5:1,
It separates tower reboiler E and uses thermosyphon reboiler, extractant clarifier F is kettle type reboiler, and reboiler E is changed with reboiler F
The ratio between heat area is 5:1, and entering the part of extractant clarifier in extractant stream is the 6% of extractant stream weight.It is described
In the part for not entering the extractant clarifier in third―party logistics, into the first rectifying column and enter the phase-splitter
Weight ratio is 120:1.
First rectifying column operating condition are as follows: pressure 0.26MPaG, 45 DEG C of tower top temperature.
Second distillation column operating condition are as follows: pressure 0.24MPaG, 45 DEG C of tower top temperature.
Knockout tower operating condition are as follows: pressure 0.22MPaG, 45 DEG C of tower top temperature.
Separation column 1,2- epoxy butane logistics purity 99.97%, the rate of recovery 99.91% separate tower bottom extractant
Purity 99.20%, extractant loss 0.65%, impurity elimination factor are 99.3%.
[embodiment 13]
According to process flow shown in Fig. 2, extractant is normal octane, the crude product logistics of the epoxy butane Han 1,2- with containing just pungent
The extractant stream of alkane enters first rectifying column.With molar percent, extractant and 1, the ratio of 2- epoxy butane is 4:1,
It separates tower reboiler E and uses thermosyphon reboiler, extractant clarifier F is kettle type reboiler, and reboiler E is changed with reboiler F
The ratio between heat area is 5:1, and entering the part of extractant clarifier in extractant stream is the 6% of extractant stream weight.It is described
In the part for not entering the extractant clarifier in third―party logistics, into the first rectifying column and enter the phase-splitter
Weight ratio is 600:1.
First rectifying column operating condition are as follows: pressure 0.26MPaG, 45 DEG C of tower top temperature.
Second distillation column operating condition are as follows: pressure 0.24MPaG, 45 DEG C of tower top temperature.
Knockout tower operating condition are as follows: pressure 0.22MPaG, 45 DEG C of tower top temperature.
Separation column 1,2- epoxy butane logistics purity 99.97%, the rate of recovery 99.92% separate tower bottom extractant
Purity 99.20%, extractant loss 0.66%, impurity elimination factor are 99.2%.
[comparative example 1]
According to process flow shown in Fig. 3, extractant is normal octane, the crude product logistics of the epoxy butane Han 1,2- with containing just pungent
The extractant stream of alkane enters first rectifying column.With molar percent, extractant and 1, the ratio of 2- epoxy butane is 8:1,
It separates tower reboiler E and uses forced cyclic type reboiler.
First rectifying column operating condition are as follows: pressure 0.26MPaG, 45 DEG C of tower top temperature.
Second distillation column operating condition are as follows: pressure 0.24MPaG, 45 DEG C of tower top temperature.
Knockout tower operating condition are as follows: pressure 0.22MPaG, 45 DEG C of tower top temperature.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 96.38% separate tower bottom extractant
Purity 98.0%, extractant loss 2.02%, impurity elimination factor are 75.2%.Compared with [embodiment 1], separating energy consumption increases
4.5%.
[comparative example 2]
According to process flow shown in Fig. 3, extractant is normal octane, the crude product logistics of the epoxy butane Han 1,2- with containing just pungent
The extractant stream of alkane enters first rectifying column.With molar percent, extractant and 1, the ratio of 2- epoxy butane is 6:1,
It separates tower reboiler E and uses forced cyclic type reboiler.
First rectifying column operating condition are as follows: pressure 0.26MPaG, 45 DEG C of tower top temperature.
Second distillation column operating condition are as follows: pressure 0.24MPaG, 45 DEG C of tower top temperature.
Knockout tower operating condition are as follows: pressure 0.22MPaG, 45 DEG C of tower top temperature.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 98.50% separate tower bottom extractant
Purity 97.0%, extractant loss 2.20%, impurity elimination factor are 75.4%.
[comparative example 3]
According to process flow shown in Fig. 3, extractant is normal octane, the crude product logistics of the epoxy butane Han 1,2- with containing just pungent
The extractant stream of alkane enters first rectifying column.With molar percent, extractant and 1, the ratio of 2- epoxy butane is 4:1,
It separates tower reboiler E and uses forced cyclic type reboiler.
First rectifying column operating condition are as follows: pressure 0.26MPaG, 45 DEG C of tower top temperature.
Second distillation column operating condition are as follows: pressure 0.24MPaG, 45 DEG C of tower top temperature.
Knockout tower operating condition are as follows: pressure 0.22MPaG, 45 DEG C of tower top temperature.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 98.88% separate tower bottom extractant
Purity 97.5%, extractant loss 2.45%, impurity elimination factor are 75.6%.
[comparative example 4]
According to process flow shown in Fig. 3, extractant is normal octane, the crude product logistics of the epoxy butane Han 1,2- with containing just pungent
The extractant stream of alkane enters first rectifying column.With molar percent, extractant and 1, the ratio of 2- epoxy butane is 3:1,
It separates tower reboiler E and uses forced cyclic type reboiler.
First rectifying column operating condition are as follows: pressure 0.26MPaG, 45 DEG C of tower top temperature.
Second distillation column operating condition are as follows: pressure 0.24MPaG, 45 DEG C of tower top temperature.
Knockout tower operating condition are as follows: pressure 0.22MPaG, 45 DEG C of tower top temperature.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 97.13% separate tower bottom extractant
Purity 98.0%, extractant loss 2.62%, impurity elimination factor are 75.8%.
[comparative example 5]
It according to process flow shown in Fig. 3, is recycled back after heavy constituent contaminant stream 18 is sent to washing, to reduce extraction
The loss of agent, extractant are normal octane, in the feed stream for containing 1,2- epoxy butane and extractant, are extracted with molar percent
Agent and 1 are taken, the ratio of 2- epoxy butane is 6:1, and separation tower reboiler E uses forced cyclic type reboiler.
First rectifying column operating condition are as follows: pressure 0.26MPaG, 45 DEG C of tower top temperature.
Second distillation column operating condition are as follows: pressure 0.24MPaG, 45 DEG C of tower top temperature.
Knockout tower operating condition are as follows: pressure 0.22MPaG, 45 DEG C of tower top temperature.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 97.58% separate tower bottom extractant
Purity 97.50%, extractant loss 1.72%, impurity elimination factor are 78.2%.Compared with [embodiment 1], separating energy consumption increases
6.8%.
Claims (17)
1. a kind of refining methd of epoxyalkane, comprising the following steps:
A) the crude product logistics containing epoxyalkane and extractant stream enter first rectifying column, and tower top obtains thick contaminant stream, tower
Bottom obtains the first thick extractant stream；
B) the described first thick extractant stream enters the knockout tower with the first reboiler, and tower top obtains epoxyalkane product, tower
Bottom obtains third―party logistics；
C) at least part in the third―party logistics enters extractant clarifier, and obtained gas phase light component returns to the separation
Tower, liquid phase heavy constituent impurity thing flow away post-processing.
2. the refining methd of epoxyalkane according to claim 1, which is characterized in that first reboiler is heat siphon type
It is any in reboiler, kettle type reboiler or forced cyclic type reboiler；The extractant clarifier be destilling tower or second again
Boil device, preferably the second reboiler.
3. the refining methd of epoxyalkane according to claim 2, which is characterized in that the first reboiler heat exchange area and second
The ratio between reboiler heat exchange area is (8~2): 1.
4. the refining methd of epoxyalkane according to claim 1, which is characterized in that in the third―party logistics, into extraction
The part of agent clarifier is the 2~20% of the third―party logistics weight.
5. the refining methd of epoxyalkane according to claim 1, which is characterized in that the method also includes:
D) the thick contaminant stream enters phase-splitter, obtains water phase and organic phase；The water phase goes to post-process；The organic phase one
Part returns to the first rectifying column, and another part enters Second distillation column；The Second distillation column tower top is obtained containing light component
The logistics of impurity, tower bottom obtain the second thick extractant stream；The second thick extractant stream enters the knockout tower.
6. the refining methd of epoxyalkane according to claim 5, which is characterized in that the water of the thick contaminant stream and introducing
The phase-splitter is entered back into after logistics contact.
7. the refining methd of epoxyalkane according to claim 5, which is characterized in that do not entered in the third―party logistics described
The part of extractant clarifier, into the first rectifying column.
8. the refining methd of epoxyalkane according to claim 5, which is characterized in that do not entered in the third―party logistics described
The part of extractant clarifier, into the first rectifying column and the phase-splitter.
9. the refining methd of epoxyalkane according to claim 8, which is characterized in that do not entered in the third―party logistics described
It is (100~1000) into the first rectifying column and the weight ratio for entering the phase-splitter in the part of extractant clarifier:
1。
10. the refining methd of epoxyalkane according to claim 1, which is characterized in that the epoxyalkane be propylene oxide,
Epoxy butane or its isomer.
11. the refining methd of epoxyalkane according to claim 1, which is characterized in that the crude product containing epoxyalkane
In logistics, by weight percentage, the content of epoxyalkane is 98~99.9%.
12. the refining methd of epoxyalkane according to claim 1, which is characterized in that the crude product containing epoxyalkane
Logistics is originated from epoxidation reaction of olefines device effluent stream.
13. a kind of refining plant of epoxyalkane, comprising:
1) first rectifying column；It is configured to receive crude product logistics containing epoxyalkane and extractant stream, discharge tower top are slightly miscellaneous
Matter logistics and the discharge thick extractant stream of tower bottom first；
2) knockout tower；It is configured to receive the described first thick extractant stream, discharge tower top epoxyalkane product stream, Yi Jipai
Put tower bottom third―party logistics；The knockout tower tower reactor is configured with the first reboiler；
3) extractant clarifier；It is configured to receive a part of third―party logistics, discharge gas phase light component stream and discharge
Liquid phase heavy constituent logistics；The gas phase light component stream returns to the knockout tower.
14. the refining plant of 3 epoxyalkane according to claim 1, which is characterized in that first reboiler is thermal siphon
It is any in formula reboiler, kettle type reboiler or forced cyclic type reboiler；The extractant clarifier is destilling tower or second
Reboiler, preferably the second reboiler.
15. the refining plant of 3 epoxyalkane according to claim 1, which is characterized in that the first reboiler heat exchange area and
The ratio between two reboiler heat exchange areas are (8~2): 1.
16. the refining plant of 3 epoxyalkane according to claim 1, which is characterized in that described device further include:
4) phase-splitter；It is configured to receive the thick contaminant stream to form water phase and organic phase；The water phase goes to post-process.
17. the refining plant of 3 epoxyalkane according to claim 1, which is characterized in that described device further include:
5) Second distillation column；It is configured to receive a part of organic phase, discharge tower top impurity containing light component logistics and
Discharge the thick extractant stream of tower bottom second；
Another part of the organic phase returns to the first rectifying column；The second thick extractant stream enters the separation
Tower.
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| CN106397366A (en) * | 2015-08-03 | 2017-02-15 | 中国石油化工股份有限公司 | Purifying method for epoxypropane |
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