CN103664522B - There is the method for the integrated separating ethylene glycol of heat and 1,2-butyleneglycol - Google Patents
There is the method for the integrated separating ethylene glycol of heat and 1,2-butyleneglycol Download PDFInfo
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- CN103664522B CN103664522B CN201210325026.4A CN201210325026A CN103664522B CN 103664522 B CN103664522 B CN 103664522B CN 201210325026 A CN201210325026 A CN 201210325026A CN 103664522 B CN103664522 B CN 103664522B
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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Abstract
The present invention relates to a kind of method with the integrated separating ethylene glycol of heat and 1,2-butyleneglycol, mainly solve in prior art and there is the high problem of energy consumption.The present invention comprises the technical process of the first knockout tower C1, the second knockout tower C2, the 3rd knockout tower C3 and the 4th knockout tower C4 by adopting, wherein institute's heat requirement part of the first knockout tower C1 derives from the logistics 7 of the 3rd knockout tower C3, the technical scheme that part derives from the tower reactor reboiler E0 of the first knockout tower C1 solves this problem preferably, can be used for separation to contain in the industrial production of ethylene glycol and the logistics of 1,2-butyleneglycol.
Description
Technical field
The present invention relates to a kind of method, particularly a kind of energy-saving process method of separating-purifying ethylene glycol from the liquid product of hydrogenation of oxalate for preparing ethylene glycol with the integrated separating ethylene glycol of heat and 1,2-butyleneglycol.
Background technology
Ethylene glycol is a kind of important basic organic chemical industry raw material, is mainly used in producing polyethylene terephthalate (PET) with terephthalic acid copolymerization.In addition, ethylene glycol also can be used for producing frostproofer, lubricant, softening agent, nonionogenic tenside and explosive etc., and purposes widely.China is the consumption big country of ethylene glycol, being constructed and put into operation in recent years along with a collection of large-scale PET device, rapid to the increase in demand of ethylene glycol, the output of current domestic ethylene glycol far can not satisfy the demands, China's ethylene glycol in 2010 import volume be 664.4 ten thousand tons, estimate that the import volume of ethylene glycol in 2011 will more than 7,000,000 tons, therefore, the ethylene glycol industry of China has good development prospect.
Be that the operational path of raw material production ethylene glycol has multiple with coal, what wherein have most industrial prospect is be coupled producing oxalic ester through synthetic gas, then by the route of producing ethylene glycol from hydrogenation of oxalic ester.In the liquid-phase reaction product of hydrogenation of oxalate for preparing ethylene glycol, except containing except the lower material of the boiling point such as methyl alcohol, ethyl glycolate, also containing a small amount of 1,2-propylene glycol and 1,2-butyleneglycol etc. and ethylene glycol boiling point close to and easily with ethylene glycol azeotropic, be difficult to the material that is separated by conventional distillation, wherein 1,2-butyleneglycol and ethylene glycol boiling point closest, be separated with ethylene glycol is the most difficult.
About the separation of ethylene glycol and 1,2-butyleneglycol, especially the process for separating and purifying of hydrogenation of oxalate for preparing ethylene glycol liquid product rarely has report both at home and abroad.CN101928201 proposes by saponification reaction, the technical scheme purification synthetic gas glycol rude products going methyl alcohol, hydrogenation reaction, three tower conventional distillations and adsorption treatment.Because of 1,2-butyleneglycol in three-tower rectification separating-purifying process and ethylene glycol generation azeotropic in technical scheme involved by this patent, the two separation completely unrealized, and bring the product loss of ethylene glycol, reduce product yield.Adoptable ethylene glycol separating-purifying alternative techniques is the technique that conventional distillation combines with azeotropic distillation, need four knockout towers (hereinafter referred to as common four tower separating technologies), its technical process be barkite hydrogenation liquid product successively through light constituents such as the first knockout tower methanol removals, to remove the light constituents such as ester class through the second knockout tower, through the 3rd knockout tower (i.e. azeotropy rectification column) separating ethylene glycol and 1,2-butyleneglycol, refine through the 4th knockout tower the ethylene glycol product obtaining higher degree.Common four tower separating technologies achieve the separation completely of ethylene glycol and 1,2-butyleneglycol, and sepn process is simple, and ethylene glycol yield is high, purity is high, ISOUV value is high.
But, also there is following shortcoming in above-mentioned common four tower separating technologies: 1) due to methanol content in the liquid product of hydrogenation of oxalate for preparing ethylene glycol very high (being about 80%), the methyl alcohol removed wherein causes the hot and cold energy consumption of the first knockout tower very high, accounts for 60 ~ 80% of whole process energy consumption; 2), after the 3rd knockout tower adds entrainer, overhead vapours amount is comparatively large, and due to tower top azeotrope temperature higher, the cold needed for this some vapor of condensation is comparatively large, accounts for the second that whole process energy consumes; Therefore, if the overhead vapours of the 3rd knockout tower can be utilized, carry out heat by the 3rd knockout tower and the first knockout tower integrated, system will have certain energy saving space.If consider, the temperature of the overhead vapours of the 4th knockout tower and tower reactor liquid is high compared with the bottom temperature of the first knockout tower again, and the tower reactor ethylene glycol product of the 4th knockout tower needs cooling further to collect storage, 4th knockout tower and the first knockout tower are carried out heat integrated, system will have the further energy saving space.
Summary of the invention
Technical problem to be solved by this invention is prior art separating ethylene glycol and 1,2-butyleneglycol, particularly from the liquid product of hydrogenation of oxalate for preparing ethylene glycol during separating-purifying ethylene glycol, adopt the problem that common four tower separating technology energy consumptions are high, a kind of method with the integrated separating ethylene glycol of heat and 1,2-butyleneglycol is newly provided.The method has that technique is simple, energy consumption is low, and the advantage that ethylene glycol product purity is high, ISOUV value is high of gained.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of method with the integrated separating ethylene glycol of heat and 1,2-butyleneglycol, comprises the following steps:
A) enter the middle and lower part of the first knockout tower C1 containing the logistics 1 of ethylene glycol and 1,2-butyleneglycol, tower top steams the logistics 2 mainly comprising Light ends, and tower reactor discharges the logistics 3 mainly comprising ethylene glycol and 1,2-butyleneglycol;
B) logistics 3 enters the middle and lower part of the second knockout tower C2, and tower top steams the logistics 4 mainly comprising Light ends, and tower reactor discharges the logistics 5 mainly comprising ethylene glycol and 1,2-butyleneglycol;
C) logistics 5 enters the middle and lower part of the 3rd knockout tower C3, and the logistics 6 comprising entrainer adds from the tower top of the 3rd knockout tower C3, and tower top steams the azeotrope stream 7 being mainly entrainer and ethylene glycol and being formed, and tower reactor is mainly comprised the logistics 8 of 1,2-butyleneglycol;
D) logistics 7 through with the tower reactor liquid heat exchange of the first knockout tower C1 after logistics 9 enter phase splitter D1, be divided into the upper strata logistics 10 being rich in entrainer and the lower floor's logistics 11 being rich in ethylene glycol, the tower top that logistics 10 returns the 3rd knockout tower C3 continues to participate in azeotropic;
E) logistics 11 enters the middle and upper part of the 4th knockout tower C4, and tower top steams the logistics 12 containing entrainer, and tower reactor obtains the ethylene glycol product logistics 13 that purity is greater than 99.9%;
Wherein, institute's heat requirement part of the first knockout tower C1 derives from the logistics 7 of the 3rd knockout tower C3, and part derives from the tower reactor reboiler E0 of the first knockout tower C1.
In technique scheme, hot integration mode used can be for: institute's heat requirement part derives from the overhead vapours 7 of the 3rd knockout tower C3, part derives from the 4th knockout tower C4 overhead vapours 12 or the tower reactor high-temp liquid 13 of the first knockout tower C1, and all the other derive from the tower reactor reboiler E0 of the first knockout tower C1; Can also be for: institute's heat requirement part derives from the overhead vapours 7 of the 3rd knockout tower C3, part derives from the 4th knockout tower C4 overhead vapours 12 and the tower reactor high-temp liquid 13 of the first knockout tower C1, all the other derive from the tower reactor reboiler E0 of the first knockout tower C1.
In technique scheme, 50 ~ 80% of institute's heat requirement of the first knockout tower C1 derives from the tower reactor reboiler E0 of the first knockout tower C1.In logistics 1, the mass percentage of ethylene glycol is 5 ~ 30%.
In technique scheme, the first knockout tower C1 is the first lightness-removing column, mainly removes the methyl alcohol in raw material, has 10 ~ 30 blocks of theoretical trays in tower; Working pressure is normal pressure; Reflux ratio R=0.1 ~ 5.Second knockout tower C2 is the second lightness-removing column, mainly removes the ester compound in raw material, has 20 ~ 50 blocks of theoretical trays in tower; In the working pressure of absolute pressure for 40 ~ 101kPa; Reflux ratio R=0.3 ~ 6.3rd knockout tower C3 is azeotropy rectification column, has 8 ~ 30 blocks of theoretical trays in tower; In the working pressure of absolute pressure for 30 ~ 101.3kPa; Reflux ratio R=0.8 ~ 5; In entrainer and raw material, the mol ratio of ethylene glycol is 0.1 ~ 10:1, and entrainer and ethylene glycol do not dissolve each other.4th knockout tower C4 is purifying ethylene glycol tower, has 60 ~ 120 blocks of theoretical trays in tower; In the working pressure of absolute pressure for 10 ~ 101kPa; Reflux ratio R=3 ~ 60.The structural formula of entrainer used is:
In formula, R
1for H atom or the alkyl containing 1 ~ 4 carbon atom, be preferably H atom or the alkyl containing 1 ~ 2 carbon atom; R
2for H atom or the alkyl containing 1 ~ 4 carbon atom, be preferably H atom or the alkyl containing 1 ~ 2 carbon atom; R
3for H atom or the alkyl containing 1 ~ 8 carbon atom, be preferably H atom or the alkyl containing 1 ~ 5 carbon atom; R
4for H atom or the alkyl containing 1 ~ 8 carbon atom, be preferably H atom or the alkyl containing 1 ~ 5 carbon atom.After refining, ethylene glycol purity is by weight percentage not less than 99.9%, and the rate of recovery of ethylene glycol is not less than 90%.
Due in common four tower separating technologies, the tower top heat of the 3rd knockout tower C3 accounts for the second of whole process energy consumption, therefore in above-mentioned various hot integration mode, by the tower reactor liquid heat exchange of the overhead vapours of the 3rd knockout tower C3 and the first knockout tower C1, make the tower top heat of the 3rd knockout tower C3 as the part heating medium of the first knockout tower C1, not only can save the refrigeration duty of the 3rd knockout tower C3, the tower reactor thermal load of the first knockout tower C1 can also be reduced, play the effect reducing technique total energy consumption.In addition, because the overhead stream steam of the 4th knockout tower C4 and tower bottoms temperature are all apparently higher than the bottom temperature of the first knockout tower C1, therefore by the tower reactor liquid heat exchange of the overhead vapours of the 4th knockout tower C4 and tower reactor high-temp liquid and the first knockout tower C1, equally not only can save the refrigeration duty of the 4th knockout tower C4, the tower reactor thermal load of the first knockout tower C1 can also be reduced further, so reduce further the total energy consumption of separating technology, reduce the drop temperature of high-purity ethylene glycol product simultaneously.Adopt the inventive method, the more common four tower separating technologies of energy consumption reduce 15 ~ 25%.
The entrainer that the present invention adopts has and can form the feature of the heterogeneous azeotrope with minimum azeotrope temperature with ethylene glycol, ethylene glycol and 1 can be significantly improved, the relative volatility of 2-butyleneglycol, thus the number of theoretical plate of rectifying tower and reflux ratio are reduced greatly, realize the effect reducing investment and energy consumption.Because this entrainer and ethylene glycol not exclusively dissolve each other, after forming azeotrope with ethylene glycol easily via simple lock out operation realize with ethylene glycol be separated and recycle, and because the solubleness of ethylene glycol in entrainer is very low, reduce the loss of ethylene glycol, there is higher working efficiency.Can be used for the separation containing ethylene glycol and the logistics of 1,2-butyleneglycol, comprise separating-purifying ethylene glycol from barkite hydrogenation liquid product, and from corn be raw material ethylene glycol production technique separating-purifying ethylene glycol and 1,2-butyleneglycol etc.Adopt the inventive method, after refining, ethylene glycol purity is by weight percentage not less than 99.9%, and the rate of recovery is not less than 90%, achieves good technique effect.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of common four tower separating technologies.
Fig. 2 is the first hot integrated process flow figure of common four tower separating technologies.
Fig. 3 is the hot integrated process flow figure of the second of common four tower separating technologies.
Fig. 4 is the third hot integrated process flow figure of common four tower separating technologies.
Fig. 5 is the 4th kind of hot integrated process flow figure of common four tower separating technologies.
In Fig. 1, C1 is the first knockout tower (the first lightness-removing column); C2 is the second knockout tower (the second lightness-removing column); C3 is the 3rd knockout tower (azeotropy rectification column); C4 is the 4th knockout tower (treating tower); D1 is phase splitter.Logistics 1 is the logistics containing ethylene glycol and 1,2-butyleneglycol; Logistics 2 is more lower boiling light constituent in logistics 1; Logistics 3 is that logistics 1 removes the logistics containing ethylene glycol and 1,2-butyleneglycol after compared with lower boiling light constituent; Logistics 4 is the light constituent of higher in logistics 1; Logistics 5 is the main logistics containing ethylene glycol and 1,2-butyleneglycol after logistics 3 removes higher light constituent; Logistics 6 is fresh entrainer; Logistics 7 is the azeotrope that ethylene glycol and entrainer are formed; Logistics 8 for have neither part nor lot in logistics 1 azeotropic, containing the logistics of 1,2-butyleneglycol and other component; Logistics 9 is that logistics 7 is through entrainer logistics that is condensed, that enter phase splitter D1; Logistics 10 is for being rich in the phase splitter upper strata logistics of entrainer; Logistics 11 is for being rich in the phase splitter lower floor logistics of ethylene glycol; Logistics 12 is a small amount of entrainer in logistics 10 and other compound; Logistics 13 is the final ethylene glycol product of logistics 10 after refining.
In Fig. 1, containing the logistics 1 of ethylene glycol and 1,2-butyleneglycol respectively after the first knockout tower C1 removes more lower boiling light component stream 2 and the second knockout tower C2 removes the light component stream 4 of higher, obtain the logistics 5 mainly containing ethylene glycol and 1,2-butyleneglycol; In the 3rd knockout tower C3, ethylene glycol in logistics 5 with form azeotrope 7 from the entrainer the logistics 6 that tower top adds, steam from the tower top of the 3rd knockout tower C3, phase splitter D1 is entered through condensed logistics 9, tower reactor then obtains main containing 1, the logistics 8 of 2-butyleneglycol, can obtain 1,2-butyleneglycol product through refining further; In phase splitter D1, the upper strata logistics 10 being rich in entrainer returns the tower top continuation participation azeotropic of the 3rd knockout tower C3, the lower floor's logistics 11 being rich in entrainer enters the 4th knockout tower C4 and refines further, after the logistics 12 that tower top steams containing entrainer, the tower reactor purity obtained by weight percentage is not less than the ethylene glycol product of 99.9%.
In Fig. 2, on the basis of common four tower separating technologies, by the overhead vapours 7 of interchanger E1 by the 3rd knockout tower C3 and the tower reactor liquid heat exchange of the first knockout tower C1, for the first knockout tower C1 provides part heat hot amount, all the other heats are still provided by the tower reactor reboiler E0 of the first knockout tower C1, and comparing common four tower separating technologies, not increase any equipment, flow process also substantially identical.The logistics 9 of logistics 7 after heat exchange continues to enter phase splitter D1 phase-splitting.
In Fig. 3, on the basis of common four tower separating technologies, by interchanger E1, E2 by the overhead vapours 7 of the 3rd knockout tower C3 and the overhead vapours 12 of the 4th knockout tower C4 and the tower reactor liquid heat exchange of the first knockout tower C1, for the first knockout tower C1 provides part heat hot amount, all the other heats are still provided by the tower reactor reboiler E0 of the first knockout tower C1, and comparing former technique does not increase any equipment yet.The logistics 9 of logistics 7 after heat exchange continues to enter phase splitter D1 phase-splitting, and the logistics 101 of logistics 12 after heat exchange is discharged system or looped back the 3rd knockout tower.
In Fig. 4, on the basis of common four tower separating technologies, by interchanger E1, E2 by the overhead vapours 7 of the 3rd knockout tower C3 and the tower reactor liquid 13 of the 4th knockout tower C4 and the tower reactor liquid heat exchange of the first knockout tower C1, for the first knockout tower C1 provides part heat hot amount, all the other heats are still provided by the tower reactor reboiler E0 of the first knockout tower C1, compare former technique and add an interchanger.The logistics 9 of logistics 7 after heat exchange continues to enter phase splitter D1 phase-splitting, and the logistics 102 of logistics 13 after heat exchange is high-purity ethylene glycol product of the lesser temps after refining.
In Fig. 5, on the basis of common four tower separating technologies, by interchanger E1, E2, E3 tower reactor liquid heat exchange by the overhead vapours 12 of the overhead vapours 7 of the 3rd knockout tower C3, the 4th knockout tower C4 and tower reactor liquid 13 and the first knockout tower C1, for the first knockout tower C1 provides part heat hot amount, all the other heats are still provided by the tower reactor reboiler E0 of the first knockout tower C1, compare former technique and add an interchanger.The logistics 9 of logistics 7 after heat exchange continues to enter phase splitter D1 phase-splitting, and the logistics 101 of logistics 12 after heat exchange is discharged system or looped back the 3rd knockout tower, and the logistics 102 of logistics 13 after heat exchange is high-purity ethylene glycol product of the lesser temps after refining.
Below by embodiment, the present invention is further elaborated.
Embodiment
[comparative example 1]
Adopt the common four tower separation process scheme shown in Fig. 1, logistics 1 is the liquid product of hydrogenation of oxalate for preparing ethylene glycol, by weight percentage consist of methyl alcohol 85.65%, ethanol 0.20%, methyl glycolate 0.15%, dimethyl oxalate 0.45%, 1,2-propylene glycol 0.21%, 1,2-butyleneglycol 0.40%, ethylene glycol 12.20%, Diethylene Glycol and other light, heavy constituent 0.84%.
First knockout tower C1 is the first lightness-removing column, has 10 pieces of theoretical stages, and logistics 1 enters from the 8th piece of theoretical stage, and working pressure is normal pressure, and reflux ratio is 0.5, and tower top temperature is 64.2 DEG C, bottom temperature is 92.7 DEG C; Second knockout tower C2 is the second lightness-removing column, has 50 pieces of theoretical stages, and logistics 3 enters from the 35th piece of theoretical stage, and working pressure is normal pressure, and reflux ratio is 2, and tower top temperature is 69.3 DEG C, bottom temperature is 196.7 DEG C; 3rd knockout tower C3 is azeotropy rectification column, has 20 pieces of theoretical stages, and logistics 5 enters, containing fresh entrainer (substituent R from the 15th piece of theoretical stage
1, R
2, R
3and R
4be respectively :-H ,-H ,-CH
3,-(CH
2)
4cH
3) logistics 6 enter from tower top, in entrainer and logistics 5, the mol ratio of ethylene glycol is 1.2:1, and working pressure is normal pressure, and reflux ratio is 2, and tower top temperature is 166.7 DEG C, bottom temperature is 200.5 DEG C; The service temperature of phase splitter D1 is 50 DEG C; 4th knockout tower C4 is purifying ethylene glycol tower, has 100 pieces of theoretical stages, and logistics 10 enters from the 30th piece of theoretical stage, and working pressure counts 30kPa with absolute pressure, and reflux ratio is 50, tower top temperature 137.5 DEG C, bottom temperature 171.8 DEG C; Thick ethylene glycol after azeotropic distillation mutually in do not contain 1,2-butyleneglycol, ethylene glycol purity by weight percentage after refining further is 99.91%, ultraviolet permeability under 220nm, 275nm and 350nm wavelength is respectively 86,95 and 100, total glycol recovery rate is 99.10%, and technique total energy consumption is 3.792 × 10
3kilojoule/(kilogram × hour).
[embodiment 1]
Adopt the first the hot integrated process flow shown in Fig. 2, the operational condition of feed stream 1, each tower and phase splitter is with embodiment 1, and ethylene glycol purity, ISOUV value and the rate of recovery after refining are substantially constant, and technique total energy consumption reduces to 3.113 × 10
3kilojoule/(kilogram × hour), the energy consumption of more common four tower separating technologies reduces by 17.91%.
[embodiment 2]
Adopt the hot integrated process flow of the second shown in Fig. 3, the operational condition of feed stream 1, each tower and phase splitter is with embodiment 1, and ethylene glycol purity, ISOUV value and the rate of recovery after refining are substantially constant, and technique total energy consumption reduces to 3.052 × 10
3kilojoule/(kilogram × hour), the energy consumption of more common four tower separating technologies reduces by 19.51%.
[embodiment 3]
Adopt the third the hot integrated process flow shown in Fig. 4, the operational condition of feed stream 1, each tower and phase splitter is with embodiment 1, and ethylene glycol purity, ISOUV value and the rate of recovery after refining are substantially constant, and technique total energy consumption reduces to 3.059 × 10
3kilojoule/(kilogram × hour), the energy consumption of more common four tower separating technologies reduces by 19.33%.
[embodiment 4]
Adopt kind of the hot integrated process flow of the 5th shown in Fig. 5, the operational condition of feed stream 1, each tower and phase splitter is with embodiment 1, and ethylene glycol purity, ISOUV value and the rate of recovery after refining are substantially constant, and technique total energy consumption reduces to 2.953 × 10
3kilojoule/(kilogram × hour), the energy consumption of more common four tower separating technologies reduces by 22.13%.
Claims (6)
1. one kind has the method for the integrated separating ethylene glycol of heat and 1,2-butyleneglycol, comprises the following steps:
A) enter the middle and lower part of the first knockout tower C1 containing the logistics 1 of ethylene glycol and 1,2-butyleneglycol, tower top steams the logistics 2 mainly comprising Light ends, and tower reactor discharges the logistics 3 mainly comprising ethylene glycol and 1,2-butyleneglycol;
B) logistics 3 enters the middle and lower part of the second knockout tower C2, and tower top steams the logistics 4 mainly comprising Light ends, and tower reactor discharges the logistics 5 mainly comprising ethylene glycol and 1,2-butyleneglycol;
C) logistics 5 enters the middle and lower part of the 3rd knockout tower C3, and the logistics 6 comprising entrainer adds from the tower top of the 3rd knockout tower C3, and tower top steams the azeotrope stream 7 being mainly entrainer and ethylene glycol and being formed, and tower reactor is mainly comprised the logistics 8 of 1,2-butyleneglycol;
D) logistics 7 through with the tower reactor liquid heat exchange of the first knockout tower C1 after logistics 9 enter phase splitter D1, be divided into the upper strata logistics 10 being rich in entrainer and the lower floor's logistics 11 being rich in ethylene glycol, the tower top that logistics 10 returns the 3rd knockout tower C3 continues to participate in azeotropic;
E) logistics 11 enters the middle and upper part of the 4th knockout tower C4, and tower top steams the logistics 12 containing entrainer, and tower reactor obtains the ethylene glycol product logistics 13 that purity is greater than 99.9%;
Wherein, institute's heat requirement part of the first knockout tower C1 derives from the logistics 7 of the 3rd knockout tower C3, and part derives from the tower reactor reboiler E0 of the first knockout tower C1;
The theoretical plate number of described first knockout tower C1 is 10 ~ 30 pieces; Working pressure is normal pressure; Reflux ratio R=0.1 ~ 5; The theoretical plate number of described second knockout tower C2 is 20 ~ 50 pieces; In absolute pressure working pressure for 40 ~ 101kPa; Reflux ratio R=0.3 ~ 6; The theoretical plate number of described 3rd knockout tower C3 is 8 ~ 30 pieces; In absolute pressure working pressure for 30 ~ 101.3kPa; Reflux ratio R=0.8 ~ 5; In entrainer and raw material, the mol ratio of ethylene glycol is 0.1 ~ 10:1;
The structural formula of entrainer used is:
In formula: R
1for H atom or the alkyl containing 1 ~ 2 carbon atom, R
2for H atom or the alkyl containing 1 ~ 2 carbon atom, R
3for H atom or the alkyl containing 1 ~ 5 carbon atom, R
4for H atom or the alkyl containing 1 ~ 5 carbon atom.
2. there is the integrated separating ethylene glycol of heat and the method for 1,2-butyleneglycol according to claim 1, it is characterized in that 50 ~ 80% of institute's heat requirement of the first knockout tower C1 tower reactor reboiler E0 deriving from the first knockout tower C1.
3. there is the method for the integrated separating ethylene glycol of heat and 1,2-butyleneglycol according to claim 1, it is characterized in that institute's heat requirement of the first knockout tower C1 also has part to derive from the logistics 12 of the 4th knockout tower C4 or/and logistics 13.
4. there is the method for the integrated separating ethylene glycol of heat and 1,2-butyleneglycol according to claim 1, it is characterized in that the mass percentage of ethylene glycol in logistics 1 is 5 ~ 30%.
5. there is the method for the integrated separating ethylene glycol of heat and 1,2-butyleneglycol according to claim 1, it is characterized in that entrainer and ethylene glycol do not dissolve each other.
6. there is the method for the integrated separating ethylene glycol of heat and 1,2-butyleneglycol according to claim 1, it is characterized in that the theoretical plate number of the 4th knockout tower C4 is 60 ~ 120 pieces; In the working pressure of absolute pressure for 10 ~ 101kPa; Reflux ratio R=3 ~ 60.
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| US9718752B2 (en) | 2013-05-31 | 2017-08-01 | Shell Oil Company | Process for the separation of an alkylene glycol |
| US10099980B2 (en) | 2013-05-31 | 2018-10-16 | Shell Oil Company | Glycol recovery with solvent extraction |
| US10221116B2 (en) | 2014-04-02 | 2019-03-05 | Shell Oil Company | Process for the separation of monoethylene glycol and 1,2-butanediol |
| US10081584B2 (en) * | 2014-12-18 | 2018-09-25 | Shell Oil Company | Process for the separation of glycols |
| CN105330514B (en) * | 2015-10-12 | 2017-06-16 | 天津衡创工大现代塔器技术有限公司 | A kind of purifying technique of synthesis gas preparing ethylene glycol |
| CN106966867B (en) * | 2017-04-05 | 2023-10-20 | 青岛科技大学 | Energy-saving process for separating methanol, ethanol and benzene by three-tower heat integration pressure swing distillation |
| CN112538002B (en) * | 2020-12-08 | 2023-03-21 | 天津天南同创科技发展有限公司 | Process method for separating ethylene glycol and 1, 2-butanediol by azeotropic distillation |
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| 分离提纯乙二醇共沸精馏溶剂的合成及应用;郭艳姿等;《石油化工》;20110614;第39卷;第197-199页，特别是摘要，1.1原料，1.2实验装置，1.3实验方法，2.2共沸剂的应用 * |
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