CN109851579A - Epoxyalkane production method - Google Patents
Epoxyalkane production method Download PDFInfo
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- CN109851579A CN109851579A CN201810153539.9A CN201810153539A CN109851579A CN 109851579 A CN109851579 A CN 109851579A CN 201810153539 A CN201810153539 A CN 201810153539A CN 109851579 A CN109851579 A CN 109851579A
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- epoxyalkane
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Abstract
The present invention relates to a kind of epoxyalkane production method, 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 step of being separated in the knockout tower with the first reboiler the method includes the logistics containing epoxyalkane and extractant；It is characterized in that, a part in knockout tower tower reactor logistics enters the processing of extractant clarifier, obtained gas phase light component returns to the knockout tower, and liquid phase heavy constituent goes to post-process.The method can be used in the industrial production of epoxyalkane.
Description
Technical field
The present invention relates to a kind of epoxyalkane production methods.
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 production method of energy consumption.
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 epoxyalkane production methods.The method includes containing epoxyalkane and extraction
The step of logistics of agent separates in the knockout tower with the first reboiler；It is characterized in that, one in knockout tower tower reactor logistics
Part enters extractant clarifier.
According to an aspect of the present invention, the gas phase light component obtained after the processing of extractant clarifier returns to the separation
Tower, liquid phase heavy constituent go to post-process.
According to an aspect of the present invention, first reboiler is thermosyphon reboiler, kettle type reboiler or pressure
It is any in circulating reboiler.
According to an aspect of the present invention, the extractant clarifier be destilling tower or the second reboiler, preferably second
Reboiler.
According to an aspect of the present invention, second reboiler is thermosyphon reboiler, kettle type reboiler or pressure
It is any in circulating reboiler, preferred kettle type 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, in the logistics of knockout tower tower reactor, the part into extractant clarifier is knockout tower
The 2~20% of tower reactor logistics weight.
According to an aspect of the present invention, the operating condition of the knockout tower includes: 30~80 DEG C of tower top temperature, pressure
0.04~0.40MPaG.
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, the logistics containing epoxyalkane and extractant is produced from epoxidation reaction of olefines
The extraction product stream that object obtains after extracting rectifying.
According to an aspect of the present invention, in the logistics containing epoxyalkane and extractant, with molar percent, extraction
Taking the ratio of agent and epoxyalkane is (2~15): 1, preferably (3~10): 1, more preferable (5~7): 1.
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%.
Detailed description of the invention
Fig. 1 is the flow diagram of the method for the invention.
Fig. 2 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:
1 feed stream
2 knockout tower tower reactor logistics
3 epoxyalkane product streams
4 first reboiler feed streams
5 first reboiler output streams
6 extractant clarifier feed streams
7 heavy constituent contaminant streams-outlet logistics
8 extractant clarifier output streams
9 extractant streams
The first reboiler of A
B extractant clarifier
C knockout tower
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.
Raw material used in production method of the invention is the logistics containing epoxyalkane and extractant.The logistics is originated from alkene ring
The extraction product stream that oxidation reaction product obtains after extracting rectifying.In the logistics, the content of epoxyalkane is 5~25 weights
Measure %.
The extractant that epoxyalkane purifying 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.
According to the present invention, the logistics containing epoxyalkane and extractant contains extraction after knockout tower rectifying in tower reactor logistics
Agent and heavy constituent.By taking epoxy butane as an example, these heavy constituents include 1,2- butanediol, 1- butanediol monomethyl ether, 2- butanediol list
Methyl ether, two polybutylene oxides, polybutylene oxide, poly- 1,2- butanediol ethere and its derivative or their mixture.With epoxy
For propane, these heavy constituents include 1,2-PD, propylene glycol monomethyl ether, two polypropylene oxide, polypropylene oxide, poly- the third two
Alcohol ether and its derivative or their mixture.
According to the present invention, in Fig. 1, the logistics 1 containing epoxyalkane and extractant enters knockout tower C, epoxyalkane product object
Stream 3 is removed from separation column, and knockout tower tower reactor obtains logistics 2.The bottom knockout tower C is equipped with the first reboiler A and extractant is net
Change device B.First reboiler feed stream 4 obtains the first reboiler output streams after tower bottoms is sent into the first reboiler A heating
5, the first reboiler output streams 5 enter the lower part knockout tower C.A part of logistics 2 will as extractant clarifier feed stream 6
Tower bottoms is sent into extractant clarifier B, extractant clarifier B output streams 8 is obtained after heating, extractant clarifier B goes out material
Stream 8 is sent into the lower part knockout tower C, and heavy constituent contaminant stream 7 is discharged from the extractant bottom clarifier B.In knockout tower tower reactor logistics 2 not
Into the fraction of stream 9 of extractant clarifier B, is removed as extractant stream, epoxyalkane extracting rectifying work can be recycled back to
Sequence.In knockout tower tower reactor logistics 2, the fraction of stream 6 into extractant clarifier be 2 weight of knockout tower tower reactor logistics 2~
20%.
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.
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 during reaction or separation and purification generates glycol and its derivative impurity, and these are miscellaneous
The generation of matter is inevitable, and these impurity can in system accumulation cycle.These impurity are counter make to extracting rectifying
With reduction extractant effect of extracting.It is directly outer because heavy constituent impurity content is low in extractant if direct outlet extractant
Row, extractant loss amount are big.The present invention increases only a small-sized extractant clarifier, so that it may by the recombination in outlet logistics 7
Concentration is divided to improve 1 times or more, outlet extractant loss amount reduces by more than 50.Using the present invention, the outer discharge capacity of extractant is identical
In the case of, by long-term operation, heavy constituent impurity content is the 50% of direct outlet scheme in cycling extraction agent.And if adopted
Epoxyalkane yield must be just reduced, otherwise do not can guarantee in order to be improved the product quality of epoxyalkane with direct outlet scheme
Product quality.
Fig. 2 is the prior art, and the feed stream 1 for containing 1,2- epoxy butane and extractant is sent into knockout tower C, 1,2- epoxy
Butane product stream 3 is removed from separation column, and extractant stream 2 is removed from separation tower bottom, and the bottom knockout tower C is equipped with one
Tower bottoms is sent into after reboiler A heating by reboiler A, reboiler A feed stream 4 obtains the feeding separation of reboiler A output streams 5
The lower part tower C, extractant stream 2 separate one logistics as heavy constituent contaminant stream 7 and separation system are discharged.Due to passing through outlet portion
Divide extractant and heavy constituent to reduce the accumulation of byproduct of reaction and derivative in extractant, thus larger amount of extraction can be lost
Take agent.
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, contains the feed stream of 1,2- epoxy butane and extractant
In, with molar percent, extractant and 1, the ratio of 2- epoxy butane is 8:1, and separation tower reboiler A uses heat siphon type again
Device is boiled, extractant clarifier B is thermosyphon reboiler, and the ratio between reboiler A and reboiler B heat exchange area are 5:1, with weight hundred
Dividing the ratio for than meter, accounting for knockout tower tower reactor logistics into the part of extractant clarifier is 3%.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 99.80% separate tower bottom extractant
Purity 99.0%, extractant loss 0.70%.
[embodiment 2]
According to process flow shown in Fig. 1, extractant is normal octane, contains the feed stream of 1,2- epoxy butane and extractant
In, with molar percent, extractant and 1, the ratio of 2- epoxy butane is 7:1, and separation tower reboiler A uses heat siphon type again
Device is boiled, extractant clarifier B is kettle type reboiler, and the ratio between reboiler A and reboiler B heat exchange area are 5:1, with weight percent
Meter, the ratio for accounting for knockout tower tower reactor logistics into the part of extractant clarifier are 5%.
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 0.75%.
[embodiment 3]
According to process flow shown in Fig. 1, extractant is normal octane, contains the feed stream of 1,2- epoxy butane and extractant
In, with molar percent, extractant and 1, the ratio of 2- epoxy butane is 6:1, and separation tower reboiler A uses heat siphon type again
Device is boiled, extractant clarifier B is kettle type reboiler, and the ratio between reboiler A and reboiler B heat exchange area are 5:1, with weight percent
Meter, the ratio for accounting for knockout tower tower reactor logistics into the part of extractant clarifier are 8%.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 99.85% separate tower bottom extractant
Purity 99.0%, extractant loss 0.78%.
[embodiment 4]
According to process flow shown in Fig. 1, extractant is normal octane, contains the feed stream of 1,2- epoxy butane and extractant
In, with molar percent, extractant and 1, the ratio of 2- epoxy butane is 5:1, and separation tower reboiler A uses heat siphon type again
Device is boiled, extractant clarifier B is kettle type reboiler, and the ratio between reboiler A and reboiler B heat exchange area are 5:1, with weight percent
Meter, the ratio for accounting for knockout tower tower reactor logistics into the part of extractant clarifier are 10%.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 99.89% separate tower bottom extractant
Purity 99.0%, extractant loss 0.79%.
[embodiment 5]
According to process flow shown in Fig. 1, extractant is normal octane, contains the feed stream of 1,2- epoxy butane and extractant
In, with molar percent, extractant and 1, the ratio of 2- epoxy butane is 4:1, and separation tower reboiler A uses heat siphon type again
Device is boiled, extractant clarifier B is kettle type reboiler, and the ratio between reboiler A and reboiler B heat exchange area are 5:1, with weight percent
Meter, the ratio for accounting for knockout tower tower reactor logistics into the part of extractant clarifier are 13%.
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 0.82%.
[embodiment 6]
According to process flow shown in Fig. 1, extractant is C8 paraffins mixture, contain 1,2- epoxy butane and extractant into
In material stream, with molar percent, extractant and 1, the ratio of 2- epoxy butane is 4:1, and separation tower reboiler A uses hot rainbow
Suction reboiler, extractant clarifier B are kettle type reboiler, and the ratio between reboiler A and reboiler B heat exchange area are 5:1, with weight
Percentages, the ratio for accounting for knockout tower tower reactor logistics into the part of extractant clarifier are 15%.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 99.85% separate tower bottom extractant
Purity 99.0%, extractant loss 0.85%.
[embodiment 7]
According to process flow shown in Fig. 1, extractant is normal octane, contains the feed stream of 1,2- epoxy butane and extractant
In, with molar percent, extractant and 1, the ratio of 2- epoxy butane is 6:1, and separation tower reboiler A uses heat siphon type again
Device is boiled, extractant clarifier B is kettle type reboiler, and the ratio between reboiler A and reboiler B heat exchange area are 4:1, with weight percent
Meter, the ratio for accounting for knockout tower tower reactor logistics into the part of extractant clarifier are 7%.
Separation column 1,2- epoxy butane logistics purity 99.95%, the rate of recovery 99.85% separate tower bottom extractant
Purity 99.0%, extractant loss 0.74%.
[embodiment 8]
According to process flow shown in Fig. 1, extractant is normal octane, contains the feed stream of 1,2- epoxy butane and extractant
In, with molar percent, extractant and 1, the ratio of 2- epoxy butane is 6:1, and separation tower reboiler A uses heat siphon type again
Device is boiled, extractant clarifier B is kettle type reboiler, and the ratio between reboiler A and reboiler B heat exchange area are 3:1, with weight percent
Meter, the ratio for accounting for knockout tower tower reactor logistics into the part of extractant clarifier are 6%.
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 0.73%.
[embodiment 9]
According to process flow shown in Fig. 1, extractant is normal octane, contains the feed stream of 1,2- epoxy butane and extractant
In, with molar percent, extractant and 1, the ratio of 2- epoxy butane is 6:1, and separation tower reboiler A uses heat siphon type again
Device is boiled, extractant clarifier B is kettle type reboiler, and the ratio between reboiler A and reboiler B heat exchange area are 2:1, with weight percent
Meter, the ratio for accounting for knockout tower tower reactor logistics into the part of extractant clarifier are 6%.
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 0.75%.
[embodiment 10]
According to process flow chart shown in Fig. 1, extractant is normal octane, contains the charging object of 1,2- epoxy butane and extractant
In stream, with molar percent, extractant and 1, the ratio of 2- epoxy butane is 6:1, and separation tower reboiler A is boiled again using autoclave
Device, extractant clarifier B are kettle type reboiler, and the ratio between reboiler A and reboiler B heat exchange area are 2:1, with weight percent
Meter, the ratio for accounting for knockout tower tower reactor logistics into the part of extractant clarifier are 6%.
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 0.75%.
[embodiment 11]
According to process flow shown in Fig. 1, extractant is normal octane, contains the feed stream of 1,2- epoxy butane and extractant
In, with molar percent, extractant and 1, the ratio of 2- epoxy butane is 6:1, and separation tower reboiler A uses forced cyclic type
Reboiler, extractant clarifier B are kettle type reboiler, and the ratio between reboiler A and reboiler B heat exchange area are 2:1, with weight percent
Than meter, the ratio for accounting for knockout tower tower reactor logistics into the part of extractant clarifier is 6%.
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 0.75%.
[comparative example 1]
According to process flow shown in Fig. 2, extractant is normal octane, contains the feed stream of 1,2- epoxy butane and extractant
In, with molar percent, extractant and 1, the ratio of 2- epoxy butane is 8:1, and separation tower reboiler A uses forced cyclic type
Reboiler.
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%.Compared with [embodiment 1], separating energy consumption increases by 4.5%.
[comparative example 2]
According to process flow shown in Fig. 2, extractant is normal octane, contains the feed stream of 1,2- epoxy butane and extractant
In, with molar percent, extractant and 1, the ratio of 2- epoxy butane is 6:1, and separation tower reboiler A uses forced cyclic type
Reboiler.
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%.
[comparative example 3]
According to process flow shown in Fig. 2, extractant is normal octane, contains the feed stream of 1,2- epoxy butane and extractant
In, with molar percent, extractant and 1, the ratio of 2- epoxy butane is 4:1, and separation tower reboiler A uses forced cyclic type
Reboiler.
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%.
[comparative example 4]
According to process flow shown in Fig. 2, extractant is normal octane, contains the feed stream of 1,2- epoxy butane and extractant
In, with molar percent, extractant and 1, the ratio of 2- epoxy butane is 3:1, and separation tower reboiler A uses forced cyclic type
Reboiler.
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%.
[comparative example 5]
It according to process flow shown in Fig. 2, is recycled back after heavy constituent contaminant stream 7 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 A uses forced cyclic type reboiler.
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%.Compared with [embodiment 1], separating energy consumption increases by 6.8%.
Claims (11)
1. a kind of epoxyalkane production method, including the logistics containing epoxyalkane and extractant in the separation with the first reboiler
The step of being separated in tower；It is characterized in that, a part in knockout tower tower reactor logistics enters extractant clarifier.
2. epoxyalkane production method according to claim 1, which is characterized in that obtained after the processing of extractant clarifier
Gas phase light component returns to the knockout tower, and liquid phase heavy constituent goes to post-process.
3. epoxyalkane production method 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.
4. epoxyalkane production method according to claim 1, which is characterized in that the extractant clarifier is destilling tower
Or second reboiler, preferably the second reboiler.
5. epoxyalkane production method according to claim 4, which is characterized in that second reboiler is heat siphon type
It is any in reboiler, kettle type reboiler or forced cyclic type reboiler, preferred kettle type reboiler.
6. epoxyalkane production method according to claim 4, which is characterized in that the first reboiler heat exchange area and second
The ratio between reboiler heat exchange area is (5~2): 1.
7. epoxyalkane production method according to claim 1, which is characterized in that in knockout tower tower reactor logistics, into extraction
The part for taking agent clarifier is the 2~20% of knockout tower tower reactor logistics weight.
8. epoxyalkane production method according to claim 1, which is characterized in that the operating condition packet of the knockout tower
It includes: 30~80 DEG C of tower top temperature, 0.04~0.40MPaG of pressure.
9. epoxyalkane production method according to claim 1, which is characterized in that the epoxyalkane be propylene oxide,
Epoxy butane or its isomer.
10. epoxyalkane production method according to claim 1, which is characterized in that described to contain epoxyalkane and extractant
Logistics be originated from the extraction product stream that obtains after extracting rectifying of epoxidation reaction of olefines product.
11. epoxyalkane production method according to claim 1, which is characterized in that described to contain epoxyalkane and extractant
Logistics in, with molar percent, the ratio of extractant and epoxyalkane is (2~15): 1, preferably (3~10): 1, it is more excellent
It selects (5~7): 1.
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| CN106397363A (en) * | 2015-08-03 | 2017-02-15 | 中国石油化工股份有限公司 | Purifying method for 1,2-epoxybutane |
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| US4402794A (en) * | 1982-05-24 | 1983-09-06 | Atlantic Richfield Company | Purification of butylene oxides by extractive distillation with selected extractive distillation solvents |
| US4772732A (en) * | 1986-05-08 | 1988-09-20 | Basf Corporation | Method for purification of butylene oxide |
| US5453160A (en) * | 1994-05-31 | 1995-09-26 | Texaco Chemical Inc. | Use of mixed polyoxypropylene glycols in the extractive distillation of propylene oxide |
| US5529667A (en) * | 1994-12-01 | 1996-06-25 | Hoechst Celanese Corporation | Process for recovering ethylene oxide |
| US8389750B2 (en) * | 2010-09-28 | 2013-03-05 | Lyondell Chemical Technology, L.P. | Purification of propylene oxide |
| CN104109137B (en) * | 2013-04-16 | 2016-06-08 | 中国石油化工股份有限公司 | Oxide purification process |
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| CN106397363A (en) * | 2015-08-03 | 2017-02-15 | 中国石油化工股份有限公司 | Purifying method for 1,2-epoxybutane |
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| Title |
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| 辜乌根 等: "萃取精馏法精制1，2-环氧丁烷的研究", 《石油化工》 * |
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