CN109851583A - Epoxyalkane purification process - Google Patents
Epoxyalkane purification process Download PDFInfo
- Publication number
- CN109851583A CN109851583A CN201810153555.8A CN201810153555A CN109851583A CN 109851583 A CN109851583 A CN 109851583A CN 201810153555 A CN201810153555 A CN 201810153555A CN 109851583 A CN109851583 A CN 109851583A
- Authority
- CN
- China
- Prior art keywords
- extractant
- reboiler
- epoxyalkane
- tower
- logistics
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The present invention relates to a kind of epoxyalkane purification process, 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, producing one logistics from separating tower column plate liquid phase is sent into the processing of extractant clarifier.The method can be used in the industrial production of epoxyalkane.
Description
Technical field
The present invention relates to a kind of epoxyalkane purification process.
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.Two
Alcohols is as extractant, the problem is that unstable, it may occur that dehydration or polymerization reaction lose the effect of extractant, simultaneously
Generate new impurity.Consider from separating effect and economy, the purification process of epoxyalkane is using C8 straight chain and branched paraffin
Mixture is as extractant.The addition of extractant becomes acetaldehyde, water, methanol, methyl formate to the relative volatility of epoxyalkane
Greatly, acetaldehyde, water, methanol, methyl formate are removed from tower top, 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, epoxy butane high income,
The small epoxyalkane purification process 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 lower part 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 purification process.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, being produced from separating tower column plate liquid phase
The processing of extractant clarifier is sent into one logistics.
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, by weight percentage, the extraction of separating tower column plate liquid phase enters extractant and purifies
The part of device is the 2~20% of separating tower column plate liquid phase 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, gas phase light component and liquid phase heavy constituent are obtained after the processing of extractant clarifier；Institute
It states gas phase light component and returns to knockout tower.
According to an aspect of the present invention, phase-splitter is entered after the liquid phase heavy constituent is cooling, is rich in after split-phase
The light phase logistics of extractant, and the heavy phase logistics rich in glycol；The light phase logistics returns to the knockout tower, the heavy phase logistics
Extraction.
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 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.
According to an aspect of the present invention, the column plate for producing one logistics feeding extractant clarifier is located at feedboard
Below at any column plate.
Beneficial effects of the present invention: the present invention adds one in the lower part of the conventional knockout tower configured with a reboiler again
A extractant clarifier produces one logistics from separating tower column plate liquid phase and is sent into the processing of extractant clarifier, and preferred embodiment is point
One block from tower bottom plate handles the tower tower reactor logistics that is partially separated of the original direct outlet of tower reactor through extractant clarifier, point
Heavy constituent impurity is separated out, to improve extractant purity, reduces the loss and energy consumption of extractant, improves epoxyalkane
Yield, extractant purity improve 0.1~2%, and extractant loss 0.1~0.5%, energy consumption reduces 1~10%, 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 extractant streams
3 epoxyalkane product streams
4 first reboiler feed streams
5 first reboiler output streams
6 extractant clarifier feed streams
7 heavy constituent contaminant streams
8 extractant clarifier output streams
9 are rich in the organic phase logistics of extractant
10 are rich in the organic phase logistics of glycol heavy constituent impurity
The first reboiler of A
B extractant clarifier
C knockout tower
D cooler
E phase-splitter
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 purification process 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.These heavy constituents include 1,2- butanediol, 1- butanediol monomethyl ether, 2- butanediol monomethyl ether, dimerization epoxy fourth
Alkane, polybutylene oxide and its derivative or their mixture；These heavy constituents include propylene glycol, propylene glycol monomethyl ether, third
Glycol dimethyl ether, polypropylene oxide 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 extractant stream 2 is removed from separation tower bottom, and the bottom knockout tower C is equipped with the first reboiler A, the
One reboiler feed stream 4 obtains the first reboiler output streams 5 after tower bottoms is sent into the first reboiler A heating, and first again
It boils device output streams 5 and enters the lower part knockout tower C, produce one logistics 6 from knockout tower A column plate liquid phase and be sent into extractant clarifier B.
Glycol heavy constituent impurity is discharged from knockout tower as a result,.
As a preferred embodiment of the present invention, the bottom of the conventional knockout tower configured with a reboiler again
Add a reboiler, that is to say, that separation tower bottom is configured with two reboilers.This can save and set for new device
Standby investment, while extractant loss amount is reduced, improve product quality；It is also particularly suitable for old plant modification upgrading, change amplitude is small,
Low, reduction extractant loss amount is put into, effect is obvious.
The present inventor is the study found that the heavy constituents such as glycol, epoxypropane polymer solubility in extractant is small, under cooling
Phase separation can occur.As a preferred embodiment of the present invention, extractant purification is obtained after extractant clarifier B processing
Device B output streams 8, extractant clarifier B output streams 8 are sent into the lower part knockout tower C, and heavy constituent contaminant stream 7 is net from extractant
Change the extraction of the bottom device B, enters phase-splitter E (such as Liquid liquid Separation tank) after cooler D is cooling, obtained after split-phase rich in extractant
Light phase logistics 9, and the heavy phase logistics 10 rich in glycol；Light phase logistics 9 returns to the knockout tower C to recycle wherein extractant,
Heavy phase logistics 10 produces.Glycol heavy constituent impurity is discharged from system as a result,.
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.
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, cooler and phase-splitter, so that it may will be outer
The heavy constituent concentration arranged in logistics 10 improves 3 times or more, and 2 loss amount of outlet extractant reduces by more than 50.Using the present invention, extraction
It takes in the identical situation of the outer discharge capacity of agent, by long-term operation, heavy constituent impurity content is direct outlet side in cycling extraction agent
The 20% of case.And if, in order to improve the product quality of epoxyalkane, must just reduce epoxyalkane using direct outlet scheme
Otherwise yield not can guarantee product quality.
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.Knockout tower tower
Plate number 30, feedboard are located at the 15th piece, one logistics is produced from the 29th piece and is sent into extractant clarifier, by weight percentage,
The part that extraction enters extractant clarifier is the 2.5% of separating tower column plate liquid phase weight.
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 0.25%.
[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.Separating tower column plate number
35, feedboard is located at the 18th piece, one logistics is produced from the 33rd piece and is sent into extractant clarifier, by weight percentage, extraction
Part into extractant clarifier is the 2.5% of separating tower column plate liquid phase weight.
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 0.29%.
[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.Separating tower column plate number
40, feedboard is located at the 20th piece, one logistics is produced from the 37th piece and is sent into extractant clarifier, by weight percentage, extraction
Part into extractant clarifier is the 2.5% of separating tower column plate liquid phase weight.
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 0.33%.
[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.Separating tower column plate number
45, feedboard is located at the 22nd piece, one logistics is produced from the 41st piece and is sent into extractant clarifier, by weight percentage, extraction
Part into extractant clarifier is the 2.5% of separating tower column plate liquid phase weight.
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 0.34%.
[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.Separating tower column plate number
45, feedboard is located at the 22nd piece, one logistics is produced from the 40th piece and is sent into extractant clarifier, by weight percentage, extraction
Part into extractant clarifier is the 2.5% of separating tower column plate liquid phase weight.
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 0.39%.
[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.Knockout tower
The number of plates 45, feedboard are located at the 22nd piece, one logistics is produced from the 40th piece and is sent into extractant clarifier, with weight percent
Meter, the part that extraction enters extractant clarifier is the 2.5% of separating tower column plate liquid phase weight.
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 0.41%.
[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.Separating tower column plate number
45, feedboard is located at the 22nd piece, one logistics is produced from the 44th piece and is sent into extractant clarifier, by weight percentage, extraction
Part into extractant clarifier is the 2.5% of separating tower column plate liquid phase weight.
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 0.28%.
[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.Separating tower column plate number
45, feedboard is located at the 22nd piece, one logistics is produced from the 44th piece and is sent into extractant clarifier, by weight percentage, extraction
Part into extractant clarifier is the 2.5% of separating tower column plate liquid phase weight.
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 0.27%.
[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.Separating tower column plate number
45, feedboard is located at the 22nd piece, one logistics is produced from the 44th piece and is sent into extractant clarifier, by weight percentage, extraction
Part into extractant clarifier is the 2.5% of separating tower column plate liquid phase weight.
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 0.29%.
[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.Separating tower column plate number
45, feedboard is located at the 22nd piece, one logistics is produced from the 44th piece and is sent into extractant clarifier, by weight percentage, extraction
Part into extractant clarifier is the 2.5% of separating tower column plate liquid phase weight.
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 0.29%.
[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.Separating tower column plate
Number 45, feedboard are located at the 22nd piece, one logistics feeding extractant clarifier is produced from the 44th piece and is adopted by weight percentage
It is out the 2.5% of separating tower column plate liquid phase weight into the part of extractant clarifier.
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 0.29%.
[embodiment 12]
According to process flow shown in Fig. 1, extractant is normal octane, in the feed stream containing propylene oxide and extractant,
With molar percent, the ratio of extractant and propylene oxide is 7:1, and separation tower reboiler A uses thermosyphon reboiler, extraction
Taking agent clarifier B is thermosyphon reboiler, and the ratio between reboiler A and reboiler B heat exchange area are 5:1.Separating tower column plate number 45,
Feedboard is located at the 22nd piece, one logistics is produced from the 44th piece and is sent into extractant clarifier, and by weight percentage, extraction enters
The part of extractant clarifier is the 2.5% of separating tower column plate liquid phase weight.
Separation column propene oxide stream purity 99.99%, the rate of recovery 99.82% separate tower bottom extractant purity
99.0%, extractant loss 0.22%.
[embodiment 13]
According to process flow shown in Fig. 1, extractant is normal octane, in the feed stream containing propylene oxide and extractant,
With molar percent, the ratio of extractant and propylene oxide is 6:1, and separation tower reboiler A uses thermosyphon reboiler, extraction
Taking agent clarifier B is kettle type reboiler, and the ratio between reboiler A and reboiler B heat exchange area are 5:1.Separating tower column plate number 45, charging
Plate is located at the 22nd piece, one logistics is produced from the 44th piece and is sent into extractant clarifier, and by weight percentage, extraction enters extraction
The part of agent clarifier is the 2.5% of separating tower column plate liquid phase weight.
Separation column propene oxide stream purity 99.95%, the rate of recovery 99.82% separate tower bottom extractant purity
99.0%, extractant loss 0.24%.
[embodiment 14]
According to process flow shown in Fig. 1, extractant is normal octane, in the feed stream containing propylene oxide and extractant,
With molar percent, the ratio of extractant and propylene oxide is 5:1, and separation tower reboiler A uses thermosyphon reboiler, extraction
Taking agent clarifier B is kettle type reboiler, and the ratio between reboiler A and reboiler B heat exchange area are 5:1.Separating tower column plate number 45, charging
Plate is located at the 22nd piece, one logistics is produced from the 44th piece and is sent into extractant clarifier, and by weight percentage, extraction enters extraction
The part of agent clarifier is the 2.5% of separating tower column plate liquid phase weight.
Separation column propene oxide stream purity 99.99%, the rate of recovery 99.86% separate tower bottom extractant purity
99.0%, extractant loss 0.29%.
[embodiment 15]
According to process flow shown in Fig. 1, extractant is normal octane, in the feed stream containing propylene oxide and extractant,
With molar percent, the ratio of extractant and propylene oxide is 4:1, and separation tower reboiler A uses thermosyphon reboiler, extraction
Taking agent clarifier B is kettle type reboiler, and the ratio between reboiler A and reboiler B heat exchange area are 5:1.Separating tower column plate number 45, charging
Plate is located at the 22nd piece, one logistics is produced from the 44th piece and is sent into extractant clarifier, and by weight percentage, extraction enters extraction
The part of agent clarifier is the 2.5% of separating tower column plate liquid phase weight.
Separation column propene oxide stream purity 99.99%, the rate of recovery 99.93% separate tower bottom extractant purity
99.0%, extractant loss 0.31%.
[embodiment 16]
According to process flow shown in Fig. 1, extractant is normal octane, in the feed stream containing propylene oxide and extractant,
With molar percent, the ratio of extractant and propylene oxide is 3:1, and separation tower reboiler A uses thermosyphon reboiler, extraction
Taking agent clarifier B is kettle type reboiler, and the ratio between reboiler A and reboiler B heat exchange area are 5:1.Separating tower column plate number 45, charging
Plate is located at the 22nd piece, one logistics is produced from the 44th piece and is sent into extractant clarifier, and by weight percentage, extraction enters extraction
The part of agent clarifier is the 2.5% of separating tower column plate liquid phase weight.
Separation column propene oxide stream purity 99.99%, the rate of recovery 99.94% separate tower bottom extractant purity
99.0%, extractant loss 0.34%.
[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 (12)
1. a kind of epoxyalkane purification process, 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, producing one logistics from separating tower column plate liquid phase is sent into the processing of extractant clarifier.
2. epoxyalkane purification process 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.
3. epoxyalkane purification process according to claim 1, which is characterized in that the extractant clarifier is destilling tower
Or second reboiler, preferably the second reboiler.
4. epoxyalkane purification process according to claim 3, 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.
5. epoxyalkane purification process according to claim 3, which is characterized in that the first reboiler heat exchange area and second
The ratio between reboiler heat exchange area is (5~2): 1.
6. epoxyalkane purification process according to claim 1, which is characterized in that by weight percentage, knockout tower tower
It is the 2~20% of separating tower column plate liquid phase weight that the extraction of plate liquid phase, which enters the part of extractant clarifier,.
7. epoxyalkane purification process 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.
8. epoxyalkane purification process according to claim 1, which is characterized in that obtain gas after the processing of extractant clarifier
Phase light component and liquid phase heavy constituent；The gas phase light component returns to knockout tower.
9. epoxyalkane purification process according to claim 8, which is characterized in that the liquid phase heavy constituent cools down laggard
Enter phase-splitter, the light phase logistics rich in extractant, and the heavy phase logistics rich in glycol are obtained after split-phase；The light phase logistics returns
The knockout tower, the heavy phase logistics extraction.
10. epoxyalkane purification process according to claim 1, which is characterized in that the epoxyalkane be propylene oxide,
Epoxy butane or its isomer.
11. epoxyalkane purification process 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.
12. epoxyalkane purification process according to claim 1, which is characterized in that extraction is sent into described one logistics of extraction
The column plate of agent clarifier is taken to be located at any column plate of feedboard or less.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711241161X | 2017-11-30 | ||
| CN201711241161 | 2017-11-30 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109851583A true CN109851583A (en) | 2019-06-07 |
| CN109851583B CN109851583B (en) | 2021-03-30 |
Family
ID=66889547
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810153539.9A Active CN109851579B (en) | 2017-11-30 | 2018-02-22 | Process for producing alkylene oxide |
| CN201810153555.8A Active CN109851583B (en) | 2017-11-30 | 2018-02-22 | Alkylene oxide purification process |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810153539.9A Active CN109851579B (en) | 2017-11-30 | 2018-02-22 | Process for producing alkylene oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN109851579B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112851601A (en) * | 2019-11-27 | 2021-05-28 | 北京诺维新材科技有限公司 | Method for purifying alkylene oxide |
| CN113929644A (en) * | 2020-07-14 | 2022-01-14 | 中国石油化工股份有限公司 | Method for purifying propylene oxide and co-producing propylene glycol |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| EP0685472A1 (en) * | 1994-05-31 | 1995-12-06 | Texaco Development Corporation | Extractive distillation of propylene oxide |
| WO1996016953A1 (en) * | 1994-12-01 | 1996-06-06 | Hoechst Celanese Corporation | Improved process for recovering ethylene oxide |
| WO2012050885A1 (en) * | 2010-09-28 | 2012-04-19 | Lyondell Chemical Technology, L.P. | Purification of propylene oxide |
| CN104109137A (en) * | 2013-04-16 | 2014-10-22 | 中国石油化工股份有限公司 | Epoxypropane purifying method |
| 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 |
| CN107382915A (en) * | 2017-08-14 | 2017-11-24 | 青岛科技大学 | A kind of energy saving technique for being thermally integrated abstraction distillation separation of tetrahydrofuran methanol |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105814029B (en) * | 2013-12-06 | 2018-08-07 | 国际壳牌研究有限公司 | With the relevant improvement of oxide purification |
-
2018
- 2018-02-22 CN CN201810153539.9A patent/CN109851579B/en active Active
- 2018-02-22 CN CN201810153555.8A patent/CN109851583B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| EP0685472A1 (en) * | 1994-05-31 | 1995-12-06 | Texaco Development Corporation | Extractive distillation of propylene oxide |
| WO1996016953A1 (en) * | 1994-12-01 | 1996-06-06 | Hoechst Celanese Corporation | Improved process for recovering ethylene oxide |
| WO2012050885A1 (en) * | 2010-09-28 | 2012-04-19 | Lyondell Chemical Technology, L.P. | Purification of propylene oxide |
| CN103119032A (en) * | 2010-09-28 | 2013-05-22 | 莱昂德尔化学技术公司 | Purification of propylene oxide |
| CN104109137A (en) * | 2013-04-16 | 2014-10-22 | 中国石油化工股份有限公司 | Epoxypropane purifying method |
| 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 |
| CN107382915A (en) * | 2017-08-14 | 2017-11-24 | 青岛科技大学 | A kind of energy saving technique for being thermally integrated abstraction distillation separation of tetrahydrofuran methanol |
Non-Patent Citations (1)
| Title |
|---|
| 辜乌根等: "萃取精馏法精制1,2-环氧丁烷的研究", 《石油化工》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112851601A (en) * | 2019-11-27 | 2021-05-28 | 北京诺维新材科技有限公司 | Method for purifying alkylene oxide |
| CN113929644A (en) * | 2020-07-14 | 2022-01-14 | 中国石油化工股份有限公司 | Method for purifying propylene oxide and co-producing propylene glycol |
| CN113929644B (en) * | 2020-07-14 | 2023-08-29 | 中国石油化工股份有限公司 | Propylene oxide purification and propylene glycol co-production method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109851583B (en) | 2021-03-30 |
| CN109851579B (en) | 2021-02-09 |
| CN109851579A (en) | 2019-06-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103193594B (en) | Method for separating ethylene glycol and 1, 2-butanediol | |
| CN109851586A (en) | The purification process of propylene oxide | |
| CN106588589A (en) | Purification method for polyoxymethylene dimethyl ether(PODE) | |
| CN107915612B (en) | Method for preparing purified MIBK from industrial byproduct waste liquid acetone | |
| CN109851583A (en) | Epoxyalkane purification process | |
| CN109851576B (en) | Method and apparatus for purifying butylene oxide | |
| EP3719008B1 (en) | Alkylene oxide production method and production system | |
| CN109851580A (en) | The purification process of epoxy butane | |
| CN109851589B (en) | Propylene oxide purification method and purification apparatus | |
| CN105085165B (en) | The separation method of ethylene glycol and diethylene glycol | |
| CN109851581B (en) | Method for purifying butylene oxide | |
| CN109851591A (en) | The purification process and device of epoxyalkane | |
| CN107915615B (en) | Method for preparing purified MIBK from industrial byproduct waste liquid acetone | |
| CN109851582A (en) | The purification process of propylene oxide | |
| CN109851577B (en) | Method for purifying butylene oxide | |
| CN109851584A (en) | The refining methd and device of epoxyalkane | |
| US11773072B2 (en) | Method and system for producing epoxyalkane | |
| CN109851585B (en) | Method for purifying butylene oxide | |
| CN109851590A (en) | The purification process of propylene oxide | |
| CN109851587B (en) | Method for producing butylene oxide | |
| CN109851588A (en) | The refining methd of propylene oxide | |
| CN111909002A (en) | Separation of methanol, water and PODE in polyoxymethylene dimethyl ether system2Method for producing a mixture | |
| CN109851574A (en) | The production method of propylene oxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |