CN107253896A - A kind of method that benzene is reclaimed in the dirty benzene of the overhead product of the benzene column from isopropyl benzene apparatus - Google Patents
A kind of method that benzene is reclaimed in the dirty benzene of the overhead product of the benzene column from isopropyl benzene apparatus Download PDFInfo
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Abstract
The method that benzene is reclaimed in a kind of dirty benzene of the overhead product of benzene column from isopropyl benzene apparatus, belongs to technical field of chemical separation.The characteristics of present invention is using benzene in dirty benzene and larger other components different melting points, purification ＆ isolation is carried out by the method for fusion-crystallization by benzene from dirty benzene.Meanwhile, this method also by adding micro anthracene into dirty benzole soln, improves the temperature of dirty benzole soln crystalline temperature, while the addition of anthracene promotes the crystallization of benzene, can improve the purity of product and the overall recovery of benzene.Because the boiling point of anthracene and benzene differs greatly, benzene can again be separated with anthracene using simple rectifying, finally obtain the benzene of high-purity.
Description
Technical field
The invention belongs to technical field of chemical separation.Filled more particularly, to one kind application fused junction crystallization from isopropylbenzene
The method that benzene is reclaimed in the dirty benzene of overhead product for putting benzene column.
Background technology
Dirty benzene is the overhead product of benzene column in isopropyl benzene apparatus, and dirty benzene is typically handled by chemical spent material in production.
Several hydro carbons light components of benzene, propane, iso-butane, 2- methylpentanes etc. ten are mainly contained in dirty benzene, the mass fraction of wherein benzene is big
About 55% or so.Dirty benzene can obtain the benzene of high-purity and the C of high-quality after separation6Component, the benzene isolated can be made
Recycled for the raw materials recovery of synthesizing iso-propylbenzene, therefore dirty benzene is a kind of industrial chemicals with use value.
Dirty benzene can be carried out using processes such as direct rectifying or extracting rectifyings.Because benzene is closed with some in dirty benzene
The boiling point minimum difference of key component is only 5 DEG C or so, therefore when using direct rectification method, the separation equipment expense of required input
And operation energy consumption is all higher for it；And when using extraction fractional distillation, need to add substantial amounts of extractant in separation process,
Therefore the problems such as also resulting in the rise of running cost, the increase of operation difficulty and cause environmental pollution.Either using straight
When connecing rectification method still dirty benzene being separated using extraction fractional distillation, the operation in input equipment and separation process is spent
Take all higher, and the very flexible of operation, the investment payback time that these have resulted in equipment is longer.
According to the Physical Property Analysis to each component in dirty benzene, it is found that the freezing point of benzene and other components in dirty benzene differs greatly,
The freezing point of benzene is at 5.5 DEG C or so, and the freezing point of other components is lower than the freezing point of benzene and minimum temperature difference of freezing point all may be used
Reach 100 DEG C or so.Due to benzene in dirty benzene and the difference of other components freezing point, therefore it can be divided using cryogenic crystallization method
From.But the content of benzene is relatively low (mass fraction is 55%) in dirty benzene, therefore when being separated using cryogenic crystallization method, in order to
Increase the rate of recovery of benzene, crystallization final temperature is usually set relatively low；While the benzene in order to obtain high-purity, then needs to use in operation
The step of multiple repeated crystallization, separates to dirty benzene.Therefore when separating dirty benzene using cryogenic crystallization, not only technological operation is numerous
Trivial and energy consumption spends also relatively large.
Therefore in view of the above-mentioned problems, need to provide that a kind of simple and safe, equipment investment is relatively small, operation energy consumption relatively
The novel method of benzene is reclaimed in the overhead product of the high benzene column from isopropyl benzene apparatus of low and separation accuracy.Fused junction crystallization is
A kind of new isolation technics, it mainly carries out separating-purifying using the difference of freezing point between material, and its operating procedure is mainly wrapped
Containing 2 points：One is that control rate of temperature fall carries out decrease temperature crystalline, and two be that crystal is purified using the operating procedure of sweating.With it is upper
State several method to compare, fused junction crystallization has following advantage：1. the material purity isolated is high.2. suitable for boiling point phase
Near material separation.3. operation is generally normal pressure, low-temperature operation, safety simple to operate, to equipment without excessive demand.4. fused junction
The energy consumption of crystallization is only the 10%~30% of rectifying.So the benzene that high-purity is isolated from dirty benzene using fused junction crystallization has
Theory significance and far-reaching commercial Application meaning.
The content of the invention
Fused junction crystallization is utilized to be returned from isopropyl benzene apparatus in benzene column overhead product it is an object of the invention to provide one kind
The method for receiving benzene, the rate of recovery is also improved while the purity for improving benzene.
The characteristics of this method is using benzene in dirty benzene and larger other components different melting points, by the method for fusion-crystallization by benzene
Purification ＆ isolation is carried out from dirty benzene.Meanwhile, this method improves dirty benzole soln knot by adding micro anthracene into dirty benzole soln
The temperature of fisheye, while the addition of anthracene promotes the crystallization of benzene, can improve the purity of product and the overall recovery of benzene.Due to
The boiling point of anthracene and benzene differs greatly, and can separate with anthracene benzene again using simple rectifying, finally obtains the benzene of high-purity.
It is of the invention compared with traditional separation method, with separation accuracy is high, separating energy consumption is low, safe operation is simple and
The advantages of investing small, can significantly shorten the payoff period of dirty benzene processing equipment investment, with vast potential for future development.
To reach above-mentioned purpose, the present invention uses following technical proposals：
A kind of application fused junction crystallization reclaims the method for benzene, this method from isopropyl benzene apparatus in benzene column overhead product dirt benzene
Comprise the following steps：
1) weigh the solid anthracene of the dirty benzole soln of certain mass and certain mass in head tank, according to a certain percentage by anthracene with
Dirty benzole soln is well mixed in products pot 1；
2) the dirty benzole soln for adding anthracene is delivered in melting crystallizer through heat exchange, then pressed the dirty benzole soln in crystallizer
Certain rate of temperature fall carries out cooling operation；
3) after step 2) in after temperature in crystallizer is down to crystallization final temperature, kept under crystallization final temperature after a period of time
To crude benzol crystal and mother liquor；
4) it is to be crystallized fully after the completion of, open the bottom valve of crystallizer by step 3) mother liquor in crystallizer discharges and returns to
In products pot 1；
5) after the mother liquor in device to be crystallized is drained, temperature in rise crystallizer, by certain heating rate in crystallizer
Crude benzol crystal carry out sweating processing；The sweat that crude benzol is crystallized into sweating discharge simultaneously is periodically discharged from crystallizer, and is sent back to
Mixed into head tank with dirty benzene stoste；
6) after step 5) in after temperature is increased to sweating final temperature in crystallizer, kept under sweating final temperature after a period of time
To the benzene crystal of relative high-purity；
7) treat step 6) in after the completion of crystal sweating in crystallizer, temperature in crystallizer is increased to room temperature, makes step
It is rapid 6) in obtain benzene crystal fusing, finally obtain the liquid benzene of high-purity；Crystallizer bottom valve is finally opened to send liquid benzene
Into products pot 2.
Further, the raw material in products pot 2 is fed through in rectifying column, finally from overhead extraction and obtains purified petroleum benzin product.
Preferably, step 1) in, the dirty benzene is benzene column overhead product in isopropyl benzene apparatus；
Preferably, step 1) in, described anthracene and the mass ratio of dirty benzole soln are (0.5-1):1000, further preferred 1:
1000；
Preferably, step 2) in, the rate of temperature fall used is 3.0 DEG C/h；
Preferably, step 3) in, the crystallization final temperature is -15.0 DEG C；
Preferably, step 3) in, the crystallization constant temperature time is at least 60min.
Preferably, step 5) in, the heating rate is in 5.0 DEG C/h；
Preferably, step 6) in, the sweating final temperature is -5.0 DEG C；
Preferably, step 6) in, the sweating constant temperature time is at least 120min.
Beneficial effects of the present invention are as follows：
The characteristics of present invention is using benzene in dirty benzene and larger other components different melting points, using fused junction crystallization from dirty benzene
Benzene is isolated, while the present invention is by adding a small amount of anthracene into dirty benzole soln, so that the crystalline temperature of solution is improved, may finally
Improve the purity and the rate of recovery of product；Compared with traditional rectifying partition method, on the premise of the consistent benzene of purity is obtained, also carry
The high rate of recovery.Energy consumption of the present invention is 50% or so of traditional rectification method, considerably reduce operation in separation process into
This, and operating flexibility is strong, can effectively shortening device investment payoff period.
Flow of the present invention is simple, and simple to operate, equipment volume is small, and floor space is small, in process of production, to environment friend
It is good, it is suitable for industrialized production；Reorganization and expansion to isopropyl benzene apparatus and existing isopropyl benzene apparatus is applicable.
Embodiment
In order to illustrate more clearly of the present invention, with reference to preferred embodiment, the present invention is described further.Ability
Field technique personnel should be appreciated that following specifically described content is illustrative and be not restrictive, and this should not be limited with this
The protection domain of invention.
Embodiment 1
A kind of method that benzene is reclaimed from dirty benzene, comprises the following steps：
1) gas chromatographic analysis is carried out to dirty benzene raw materials first, the content to benzene in dirty benzene is measured；By determining, obtain
The mass fraction for going out benzene in dirty benzene is about 55.55%；
2) the dirty benzole solns of 100.0g and 0.05g anthracene are weighed with electronic balance, is then thoroughly mixed anthracene with dirty benzole soln,
Mixing transfers the solution into fusion-crystallization wherein after finishing, and opens melting crystallizer switch, melting crystallizer temperature is set in-
8.0 DEG C, continue to keep 20min after temperature reaches -8.0 DEG C.
3) cooling process setting is carried out to melting crystallizer：Rate of temperature fall is 3.0 DEG C/h, and crystallization final temperature is -15.0 DEG C, if
Surely cooling is started after finishing；Continue to keep 60min after temperature reaches crystallization final temperature in crystallizer, it is ensured that crystal in crystallizer
Fully growth.
4) treat step 3) in crystal structure complete, open crystallizer bottom valve mother liquor in crystallizer is separated with crystal；It is right
Mother liquor after gained separation is weighed and gas chromatographic analysis, can determine the mass fraction of benzene in mother liquor.
5) treat step 4) in after the completion of mother liquor and Crystallization Separation, heating schedule setting, heating speed are carried out to melting crystallizer
Rate is 5.0 DEG C/h, and sweating final temperature is -5.0 DEG C.Temperature is reached after sweating final temperature, continues to keep 120min at such a temperature；Together
When, in whole process, open crystallizer bottom valve every 20min and discharge the liquid that crystal sweating is obtained in crystallizer.
6) treat step 5) in crystal sweating operation after the completion of, mould temperature is set as 20.0 DEG C；In device to be crystallized
After crystal all melts, open crystallizer bottom valve and all pour out liquid in crystallizer；Resulting liquid is weighed with
And gas chromatographic analysis, the mass fraction for finally obtaining benzene in product is 97.3%, and the rate of recovery of benzene is 64.2%.
Embodiment 2
A kind of method that benzene is reclaimed from dirty benzene, comprises the following steps：
1) the dirty benzole solns of 100.0g and 0.07g anthracene are weighed with electronic balance, is then thoroughly mixed anthracene with dirty benzole soln,
Mixing transfers the solution into fusion-crystallization wherein after finishing, and opens melting crystallizer switch, melting crystallizer temperature is set in-
8.0 DEG C, continue to keep 20min after temperature reaches -8.0 DEG C.
2) cooling process setting is carried out to melting crystallizer：Rate of temperature fall is 3.0 DEG C/h, and crystallization final temperature is -15.0 DEG C, if
Surely cooling is started after finishing；Continue to keep 60min after temperature reaches crystallization final temperature in crystallizer, it is ensured that crystal in crystallizer
Fully growth.
3) treat step 2) in crystal structure complete, open crystallizer bottom valve mother liquor in crystallizer is separated with crystal；It is right
Mother liquor after gained separation is weighed and gas chromatographic analysis, can determine the mass fraction of benzene in mother liquor.
4) treat step 3) in after the completion of mother liquor and Crystallization Separation, heating schedule setting, heating speed are carried out to melting crystallizer
Rate is 5.0 DEG C/h, and sweating final temperature is -5.0 DEG C.Temperature is reached after sweating final temperature, continues to keep 120min at such a temperature；Together
When, in whole process, open crystallizer bottom valve every 20min and discharge the liquid that crystal sweating is obtained in crystallizer.
5) treat step 4) in crystal sweating operation after the completion of, mould temperature is set as 20.0 DEG C；In device to be crystallized
After crystal all melts, open crystallizer bottom valve and all pour out liquid in crystallizer；Resulting liquid is weighed with
And gas chromatographic analysis, the mass fraction for finally obtaining benzene in product is 98.2%, and the rate of recovery of benzene is 66.2%.
Embodiment 3
A kind of method that benzene is reclaimed from dirty benzene, comprises the following steps：
1) the dirty benzole solns of 100.0g and 0.1g anthracene are weighed with electronic balance, is then thoroughly mixed anthracene with dirty benzole soln,
Mixing transfers the solution into fusion-crystallization wherein after finishing, and opens melting crystallizer switch, melting crystallizer temperature is set in-
8.0 DEG C, continue to keep 30min after temperature reaches -8.0 DEG C.
2) cooling process setting is carried out to melting crystallizer：Rate of temperature fall is 3.0 DEG C/h, and crystallization final temperature is -15.0 DEG C, if
Surely cooling is started after finishing；Continue to keep 60min after temperature reaches crystallization final temperature in crystallizer, it is ensured that crystal in crystallizer
Fully growth.
3) treat step 2) in crystal structure complete, open crystallizer bottom valve mother liquor in crystallizer is separated with crystal；It is right
Mother liquor after gained separation is weighed and gas chromatographic analysis, can determine the mass fraction of benzene in mother liquor.
4) treat step 3) in after the completion of mother liquor and Crystallization Separation, heating schedule setting, heating speed are carried out to melting crystallizer
Rate is 5.0 DEG C/h, and sweating final temperature is -5.0 DEG C.Temperature is reached after sweating final temperature, continues to keep 120min at such a temperature；Together
When, in whole process, open crystallizer bottom valve every 20min and discharge the liquid that crystal sweating is obtained in crystallizer.
5) treat step 4) in crystal sweating operation after the completion of, mould temperature is set as 20.0 DEG C；In device to be crystallized
After crystal all melts, open crystallizer bottom valve and all pour out liquid in crystallizer；Resulting liquid is weighed with
And gas chromatographic analysis, the mass fraction for finally obtaining benzene in product is 99.2%, and the rate of recovery of benzene is 60.1%.
Embodiment 4
A kind of method that benzene is reclaimed from dirty benzene, comprises the following steps：
1) the dirty benzole solns of 100.0g and 0.1g anthracene are weighed with electronic balance, is then thoroughly mixed anthracene with dirty benzole soln,
Mixing transfers the solution into fusion-crystallization wherein after finishing, and opens melting crystallizer switch, melting crystallizer temperature is set in-
8.0 DEG C, continue to keep 20min after temperature reaches -8.0 DEG C.
2) cooling process setting is carried out to melting crystallizer：Rate of temperature fall is 3.0 DEG C/h, and crystallization final temperature is -25.0 DEG C, if
Surely cooling is started after finishing；Continue to keep 60min after temperature reaches crystallization final temperature in crystallizer, it is ensured that crystal in crystallizer
Fully growth.
3) treat step 2) in crystal structure complete, open crystallizer bottom valve mother liquor in crystallizer is separated with crystal；It is right
Mother liquor after gained separation is weighed and gas chromatographic analysis, can determine the mass fraction of benzene in mother liquor.
4) treat step 3) in after the completion of mother liquor and Crystallization Separation, heating schedule setting, heating speed are carried out to melting crystallizer
Rate is 4.0 DEG C/h, and sweating final temperature is -5.0 DEG C.Temperature is reached after sweating final temperature, continues to keep 120min at such a temperature；Together
When, in whole process, open crystallizer bottom valve every 20min and discharge the liquid that crystal sweating is obtained in crystallizer.
5) treat step 4) in crystal sweating operation after the completion of, mould temperature is set as 20.0 DEG C；In device to be crystallized
After crystal all melts, open crystallizer bottom valve and all pour out liquid in crystallizer；Resulting liquid is weighed with
And gas chromatographic analysis, the mass fraction for finally obtaining benzene in product is 98.6%, and the rate of recovery of benzene is 67.2%.
Comparative example 1
A kind of method that benzene is reclaimed from dirty benzene, comprises the following steps：
1) gas chromatographic analysis is carried out to dirty benzene raw materials first, the content to benzene in dirty benzene is measured；By determining, obtain
The mass fraction for going out benzene in dirty benzene is about 55.55%；
2) 100.0g dirty benzole soln is weighed with electronic balance, is then transferred the solution into melting crystallizer, opens molten
Melt crystallizer switch, mould temperature is set in -15.0 DEG C, continue to keep 30min after temperature reaches -15.0 DEG C.
3) cooling process setting is carried out to melting crystallizer：Rate of temperature fall is 3.0 DEG C/h, and crystallization final temperature is -25.0 DEG C, if
Surely cooling is started after finishing；After temperature reaches crystallization final temperature in crystallizer, continue to keep 60min under crystallization final temperature, it is ensured that
The abundant growth of crystal in crystallizer.
4) treat step 3) in crystallization after the completion of, open crystallizer bottom valve the mother liquor in crystallizer and crystal are separated；
5) after step 4) in crystallizer mother liquor drain after, to melting crystallizer carry out heating schedule setting, heating rate
For 5.0 DEG C/h, sweating final temperature is -15.0 DEG C.Temperature is reached after sweating final temperature, continues to keep 120min at such a temperature；Meanwhile,
In whole process, open crystallizer bottom valve every 20min and discharge the liquid that crystal sweating is obtained in crystallizer.
6) treat step 5) in crystal sweating operation after the completion of, mould temperature is set as 20.0 DEG C；In device to be crystallized
After crystal all melts, open crystallizer bottom valve and all pour out liquid in crystallizer；Resulting liquid is weighed with
And gas chromatographic analysis, the mass fraction for finally obtaining benzene in product is 95.1%, and the rate of recovery of benzene is 48.2%.
Comparative example 2
A kind of method that benzene is reclaimed from dirty benzene, comprises the following steps：
1) the dirty benzole solns of 100.0g are weighed with electronic balance and are positioned in melting crystallizer, melting crystallizer is opened and opens
Close, melting crystallizer temperature is set in -15.0 DEG C, continue to keep 30min after temperature reaches -15.0 DEG C.
2) cooling process setting is carried out to melting crystallizer：Rate of temperature fall is 3.0 DEG C/h, and crystallization final temperature is -25.0 DEG C, if
Surely cooling is started after finishing；After temperature reaches crystallization final temperature in crystallizer, continue to keep 60min at such a temperature, it is ensured that knot
The abundant growth of crystal in brilliant device.
3) treat step 2) in crystal structure complete, open crystallizer bottom valve mother liquor in crystallizer and crystal are separated；It is right
Resulting mother liquor is weighed and gas chromatographic analysis, can determine the mass fraction of benzene in mother liquor.
4) treat step 3) in after the completion of mother liquor and Crystallization Separation, heating schedule setting, heating speed are carried out to melting crystallizer
Rate is 5.0 DEG C/h, and sweating final temperature is -5.0 DEG C.Temperature is reached after sweating final temperature, continues to keep 120min at such a temperature；Together
When, in whole process, open crystallizer bottom valve every 20min and discharge the liquid that crystal sweating is obtained in crystallizer.
5) treat step 4) in crystal sweating operation after the completion of, mould temperature is set as normal temperature laboratory；Device to be crystallized
After interior crystal all melts, open crystallizer bottom valve and all pour out liquid in crystallizer；Resulting liquid is weighed
And gas chromatographic analysis, the mass fraction of benzene is 98.6% in finally obtaining in product, and the rate of recovery of benzene is 20.4%.
Comparative example 3
A kind of method that benzene is reclaimed from dirty benzene, comprises the following steps：
1) the dirty benzole solns of 100.0g are weighed with electronic balance and are positioned in melting crystallizer, melting crystallizer is opened and opens
Close, melting crystallizer temperature is set in -8.0 DEG C, continue to keep 30min after temperature reaches -8.0 DEG C.
2) cooling process setting is carried out to melting crystallizer：Rate of temperature fall is 3.0 DEG C/h, and crystallization final temperature is -15.0 DEG C, if
Surely cooling is started after finishing；After temperature reaches crystallization final temperature in crystallizer, continue to keep 60min at such a temperature, it is ensured that knot
The abundant growth of crystal in brilliant device.
3) in crystallizer and to crystallize, illustrate that the temperature is not arrived after 120min after temperature reaches crystallization final temperature
Produced up to the crystallization temperature of solution, therefore without crystal.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention, for those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms, all embodiments can not be exhaustive here, it is every to belong to this hair
Row of the obvious changes or variations that bright technical scheme is extended out still in protection scope of the present invention.
The fusion-crystallization of table 1 obtains the purity and product recovery rate of product
It can be seen from the data in Table 1 that in embodiment 1,2,3 and 4, by adding anthracene, Ran Houtong into dirty benzole soln
Fused junction crystallization is crossed, crude benzol crystal is formed by cooling, then crystal further purified using the sweating that heats up, finally
The higher benzaldehyde product of benzene mass fraction can be obtained, it is that the effective ways of high concentration benzene are isolated from dirty benzene to illustrate the method.
Embodiment 2,3 and 4 is compared with comparative example 3, it can be seen that add dirty benzene of the crystalline temperature than not adding anthracene of the dirty benzole soln of anthracene
The crystalline temperature temperature of solution is high, and this illustrates to add a small amount of anthracene into dirty benzene, and anthracene can form the higher eutectic of freezing point with benzene, from
And change the crystallization situation of dirty benzene system.
Embodiment 2 and 3 is compared with comparative example 1 and 2, and by adding a small amount of anthracene into dirty benzole soln, anthracene can be with shape with benzene
Into the high copolymer of fusing point so that dirty benzene can crystallize out more benzene at a higher temperature, may finally obtain high-purity
Product and higher product recovery rate.This explanation is added after anthracene, can significantly be lifted and be utilized fused junction crystallization from dirty benzene
The middle production efficiency for purifying out high-purity benzene.
Claims (10)
1. the method for benzene is reclaimed in a kind of dirty benzene of the overhead product of benzene column from isopropyl benzene apparatus, it is characterised in that including following
Step：
1) the solid anthracene of the dirty benzole soln of certain mass and certain mass in head tank is weighed, according to a certain percentage by anthracene and dirty benzene
Solution is well mixed in products pot 1；
2) the dirty benzole soln for adding anthracene is delivered in melting crystallizer through heat exchange, then by the dirty benzole soln in crystallizer by certain
Rate of temperature fall carry out cooling operation；
3) after step 2) in after temperature in crystallizer is down to crystallization final temperature, keep obtaining thick after a period of time under crystallization final temperature
Benzene crystal and mother liquor；
4) it is to be crystallized fully after the completion of, open the bottom valve of crystallizer by step 3) mother liquor in crystallizer discharges and returns to product
In tank 1；
5) after the mother liquor in device to be crystallized is drained, temperature in rise crystallizer, by certain heating rate to thick in crystallizer
Benzene crystal carries out sweating processing；The sweat that crude benzol is crystallized into sweating discharge simultaneously is periodically discharged from crystallizer, and returns to original
Mixed in batch can with dirty benzene stoste；
6) after step 5) in after temperature is increased to sweating final temperature in crystallizer, obtain phase after being kept for a period of time under sweating final temperature
To the benzene crystal of high-purity；
7) treat step 6) in after the completion of crystal sweating in crystallizer, temperature in crystallizer is increased to room temperature, makes step 6)
In obtain benzene crystal fusing, finally obtain the liquid benzene of high-purity；Finally open crystallizer bottom valve and liquid benzene is delivered into production
In product tank 2.
2. according to the method that benzene is reclaimed in a kind of dirty benzene of the overhead product of benzene column from isopropyl benzene apparatus described in claim 1,
Characterized in that, the raw material in products pot 2 is fed through in rectifying column, finally from overhead extraction and purified petroleum benzin product is obtained.
3. according to the method that benzene is reclaimed in a kind of dirty benzene of the overhead product of benzene column from isopropyl benzene apparatus described in claim 1,
Characterized in that, step 1) in, described anthracene and the mass ratio of dirty benzole soln are (0.5-1):1000.
4. according to the method that benzene is reclaimed in a kind of dirty benzene of the overhead product of benzene column from isopropyl benzene apparatus described in claim 1,
Characterized in that, the mass ratio of anthracene and dirty benzole soln is 1:1000.
5. according to the method that benzene is reclaimed in a kind of dirty benzene of the overhead product of benzene column from isopropyl benzene apparatus described in claim 1,
Characterized in that, step 2) in, the rate of temperature fall used is 3.0 DEG C/h.
6. according to the method that benzene is reclaimed in a kind of dirty benzene of the overhead product of benzene column from isopropyl benzene apparatus described in claim 1,
Characterized in that, step 3) in, the crystallization final temperature is -15.0 DEG C.
7. according to the method that benzene is reclaimed in a kind of dirty benzene of the overhead product of benzene column from isopropyl benzene apparatus described in claim 1,
Characterized in that, step 3) in, the crystallization constant temperature time is at least 60min.
8. according to the method that benzene is reclaimed in a kind of dirty benzene of the overhead product of benzene column from isopropyl benzene apparatus described in claim 1,
Characterized in that, step 5) in, the heating rate is in 5.0 DEG C/h.
9. according to the method that benzene is reclaimed in a kind of dirty benzene of the overhead product of benzene column from isopropyl benzene apparatus described in claim 1,
Characterized in that, step 6) in, the sweating final temperature is -5.0 DEG C.
10. according to the method that benzene is reclaimed in a kind of dirty benzene of the overhead product of benzene column from isopropyl benzene apparatus described in claim 1,
Characterized in that, step 6) in, the sweating constant temperature time is at least 120min.
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| CN104311380A (en) * | 2014-09-30 | 2015-01-28 | 天津科技大学 | Method for preparing high-purity biphenyl by coupling and melt crystallization |
| CN105601462A (en) * | 2016-02-19 | 2016-05-25 | 国药集团化学试剂有限公司 | High-purity benzene purification method |
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