CN103664522A - Method with heat integration function for separating ethylene glycol from 1,2-butylene glycol - Google Patents
Method with heat integration function for separating ethylene glycol from 1,2-butylene glycol Download PDFInfo
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Abstract
The invention relates to a method with a heat integration function for separating ethylene glycol from 1,2-butylene glycol, which is mainly used for solving the problem of high energy consumption existing in the prior art. According to the method disclosed by the invention, a technical scheme adopting a process flow including a first separating tower C1, a second separating tower C2, a third separating tower C3 and a fourth separating tower C4 is used, wherein a part of heat needed by the first separating tower C1 comes from a material flow 7 of the third separating tower 3 and the other part of heat needed by the first separating tower C1 comes from a tower kettle reboiler E0 of the first separating tower C1, and thus the problem is well solved. The method can be applied to industrial production for separating the material flow containing ethylene glycol and 1,2-butylene glycol.
Description
Technical field
The present invention relates to a kind of the have integrated separating ethylene glycol of heat and the method for 1,2-butyleneglycol, particularly a kind of from the liquid product of hydrogenation of oxalate for preparing ethylene glycol the energy-saving process method of separating-purifying ethylene glycol.
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 is very extensive.China is the consumption big country of ethylene glycol, being constructed and put into operation along with a collection of large-scale PET device in recent years, increase in demand to ethylene glycol is rapid, 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, the import volume of estimating ethylene glycol in 2011 will be over 7,000,000 tons, and therefore, the ethylene glycol industry of China has good development prospect.
The operational path that the coal of take is raw material production ethylene glycol has multiple, and what wherein have most industrial prospect is to 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 the material that the boiling points such as methyl alcohol, ethyl glycolate are lower, also contain a small amount of 1,2-propylene glycol and 1,2-butyleneglycols etc. approach and easily with ethylene glycol azeotropic, by conventional distillation, are difficult to separated material with ethylene glycol boiling point, wherein 1,2-butyleneglycol and ethylene glycol boiling point are the most approaching, the most difficult separated with ethylene glycol.
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.CN 101928201 proposes by saponification reaction, removes the technical scheme purification synthetic gas glycol rude products of methyl alcohol, hydrogenation reaction, three tower conventional distillations and adsorption treatment.In the related technical scheme of this patent because of in three-tower rectification separating-purifying process 1,2-butyleneglycol and ethylene glycol generation azeotropic, unrealized the two complete separation, and bring the product loss of ethylene glycol, has reduced product yield.Adoptable ethylene glycol separating-purifying alternative techniques is the technique that conventional distillation combines with azeotropic distillation, need four knockout towers (hereinafter to be referred 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, through the second knockout tower, remove the light constituents such as ester class, through the 3rd knockout tower (being azeotropy rectification column) separating ethylene glycol and 1,2-butyleneglycol, through the refining ethylene glycol product that obtains higher degree of the 4th knockout tower.Common four tower separating technologies have been realized the complete separation of ethylene glycol and 1,2-butyleneglycol, and sepn process is simple, and ethylene glycol yield is high, purity is high, ultraviolet permeability value is high.
Yet, 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 removing 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) the 3rd knockout tower adds after entrainer, and overhead vapours amount is larger, and because tower top azeotrope temperature is higher, and the required cold of this part steam of condensation is larger, accounts for the second of whole technique energy expenditure; Therefore, if the overhead vapours of the 3rd knockout tower can be utilized, it is integrated that soon the 3rd knockout tower and the first knockout tower will carry out heat, and system will have certain energy saving space.If consider, the overhead vapours of the 4th knockout tower and the temperature of tower reactor liquid are high compared with the tower reactor temperature of the first knockout tower again, and the tower reactor ethylene glycol product of the 4th knockout tower need further coolingly can be collected storage, the 4th knockout tower and the first knockout tower are carried out to 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 high problem of common four tower separating technology energy consumption, a kind of new the have integrated separating ethylene glycol of heat and the method for 1,2-butyleneglycol are provided.The method has that technique is simple, energy consumption is low, and the advantage that ethylene glycol product purity is high, ultraviolet permeability 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 have the integrated separating ethylene glycol of heat and a method of 1,2-butyleneglycol, comprises the following steps:
A) containing the logistics 1 of ethylene glycol and 1,2-butyleneglycol, enter the middle and lower part of the first knockout tower C1, tower top steams the logistics 2 that mainly comprises light component, and tower reactor is discharged the logistics 3 that mainly comprises 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 that mainly comprises light component, and tower reactor is discharged the logistics 5 that mainly comprises 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 that comprises entrainer adds from the tower top of the 3rd knockout tower C3, and tower top steams the azeotrope stream 7 that is mainly entrainer and ethylene glycol formation, and tower reactor obtains mainly comprising the logistics 8 of 1,2-butyleneglycol;
D) logistics 9 of logistics 7 after the tower reactor liquid heat exchange with the first knockout tower C1 enters phase splitter D1, is divided into the upper strata logistics 10 that is rich in entrainer and the lower floor's logistics 11 that is rich in ethylene glycol, and the tower top that the 3rd knockout tower C3 is returned in logistics 10 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 that contains entrainer, and tower reactor obtains the ethylene glycol product stream 13 that purity is greater than 99.9%;
Wherein, institute's heat requirement of the first knockout tower C1 partly 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: institute's heat requirement of the first knockout tower C1 partly derives from the overhead vapours 7 of the 3rd knockout tower C3, overhead vapours 12 or the tower reactor high-temp liquid 13 that part derives from the 4th knockout tower C4, and all the other derive from the tower reactor reboiler E0 of the first knockout tower C1; Can also be: institute's heat requirement of the first knockout tower C1 partly derives from the overhead vapours 7 of the 3rd knockout tower C3, overhead vapours 12 and the tower reactor high-temp liquid 13 that part derives from the 4th knockout tower C4, and 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 quality percentage composition 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.The 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; The working pressure of absolute pressure of take is 40～101kPa; Reflux ratio R=0.3～6.The 3rd knockout tower C3 is azeotropy rectification column, has 8～30 blocks of theoretical trays in tower; The working pressure of absolute pressure of take is 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.The 4th knockout tower C4 is purifying ethylene glycol tower, has 60～120 blocks of theoretical trays in tower; The working pressure of absolute pressure of take is 10～101kPa; Reflux ratio R=3～60.The structural formula of entrainer used is:
In formula, R
1for H atom or containing the alkyl of 1～4 carbon atom, be preferably H atom or containing the alkyl of 1～2 carbon atom; R
2for H atom or containing the alkyl of 1～4 carbon atom, be preferably H atom or containing the alkyl of 1～2 carbon atom; R
3for H atom or containing the alkyl of 1～8 carbon atom, be preferably H atom or containing the alkyl of 1～5 carbon atom; R
4for H atom or containing the alkyl of 1～8 carbon atom, be preferably H atom or containing the alkyl of 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 technique energy expenditure, therefore in above-mentioned various hot integration modes, 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, can also reduce the tower reactor thermal load of the first knockout tower C1, play the effect that reduces 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 tower reactor 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, can also further reduce the tower reactor thermal load of the first knockout tower C1, so further reduced the total energy consumption of separating technology, reduced the drop temperature of high-purity ethylene glycol product simultaneously.Adopt the inventive method, the more common four tower separating technologies of energy consumption have reduced by 15～25%.
The entrainer that the present invention adopts has can form with ethylene glycol the feature of the heterogeneous azeotrope with minimum azeotrope temperature, can significantly improve ethylene glycol and 1, the relative volatility of 2-butyleneglycol, thereby the number of theoretical plate of rectifying tower and reflux ratio are reduced greatly, realize the effect that reduces investment and energy consumption.Because this entrainer and ethylene glycol not exclusively dissolve each other, after forming azeotrope with ethylene glycol, be easy to the separated and recycle with ethylene glycol by simple lock out operation realization, 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 take separating-purifying ethylene glycol and 1,2-butyleneglycol etc. the ethylene glycol production technique that corn is raw material.Adopt the inventive method, refining rear ethylene glycol purity is by weight percentage not less than 99.9%, and the rate of recovery is not less than 90%, has obtained good technique effect.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of common four tower separating technologies.
Fig. 2 is the hot integrated technique schema of the first of common four tower separating technologies.
Fig. 3 is the hot integrated technique schema of the second of common four tower separating technologies.
Fig. 4 is the third hot integrated technique schema of common four tower separating technologies.
Fig. 5 is the 4th kind of hot integrated technique schema 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 for containing ethylene glycol and 1, the logistics of 2-butyleneglycol; Logistics 2 is more lower boiling light constituent in logistics 1; Logistics 3 for logistics 1 remove compared with after lower boiling light constituent containing ethylene glycol and 1, the logistics of 2-butyleneglycol; Logistics 4 is the light constituent of higher in logistics 1; Logistics 5 is that logistics 3 removes main ethylene glycol and 1, the logistics of 2-butyleneglycol of containing after higher light constituent; Logistics 6 is fresh entrainer; Logistics 7 is the azeotrope that ethylene glycol and entrainer form; Logistics 8 is for having neither part nor lot in logistics azeotropic, that contain 1,2-butyleneglycol and other component in logistics 1; Logistics 9 is for logistics 7 is through entrainer logistics 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 and other compound in logistics 10; 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, through the first knockout tower C1, remove more lower boiling light constituent logistics 2 and the second knockout tower C2 removes after the light constituent logistics 4 of higher respectively, obtain mainly the logistics 5 containing ethylene glycol and 1,2-butyleneglycol; In the 3rd knockout tower C3, ethylene glycol in logistics 5 forms azeotrope 7 with the entrainer the logistics adding from tower top 6, from the tower top of the 3rd knockout tower C3, steam, through condensed logistics 9, enter phase splitter D1, tower reactor obtains main containing 1, the logistics 8 of 2-butyleneglycol, can obtain 1,2-butyleneglycol product through further refining; In phase splitter D1, the tower top continuation participation azeotropic of the 3rd knockout tower C3 is returned in the upper strata logistics 10 that is rich in entrainer, 11 of lower floor's logistics that are rich in entrainer enter the 4th knockout tower C4 and further refine, at tower top, steam after the logistics 12 containing entrainer, the purity that tower reactor obtains is by weight percentage not less than 99.9% ethylene glycol product.
In Fig. 2, on the basis of common four tower separating technologies, by interchanger E1 by the tower reactor liquid heat exchange of the overhead vapours of the 3rd knockout tower C3 7 and the first knockout tower C1, for the first knockout tower C1 provides part heating heat, 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 basic 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 tower reactor liquid heat exchange of the overhead vapours 12 of the overhead vapours of the 3rd knockout tower C3 7 and the 4th knockout tower C4 and the first knockout tower C1, for the first knockout tower C1 provides part heating heat, 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, the logistics 101 discharge systems of logistics 12 after heat exchange or loop back the 3rd knockout tower.
In Fig. 4, on the basis of common four tower separating technologies, by interchanger E1, E2 by the tower reactor liquid heat exchange of the tower reactor liquid 13 of the overhead vapours of the 3rd knockout tower C3 7 and the 4th knockout tower C4 and the first knockout tower C1, for the first knockout tower C1 provides part heating heat, all the other heats are still provided by the tower reactor reboiler E0 of the first knockout tower C1, and comparing former technique has increased 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 by the tower reactor liquid heat exchange of the overhead vapours 12 of the overhead vapours of the 3rd knockout tower C3 7, the 4th knockout tower C4 and tower reactor liquid 13 and the first knockout tower C1, for the first knockout tower C1 provides part heating heat, all the other heats are still provided by the tower reactor reboiler E0 of the first knockout tower C1, and comparing former technique has increased an interchanger.The logistics 9 of logistics 7 after heat exchange continues to enter phase splitter D1 phase-splitting, the logistics 101 discharge systems of logistics 12 after heat exchange or loop 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, the liquid product that logistics 1 is 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%.
The first knockout tower C1 is the first lightness-removing column, has 10 theoretical stages, and logistics 1 enters from the 8th theoretical stage, and working pressure is normal pressure, and reflux ratio is 0.5, and tower top temperature is that 64.2 ℃, tower reactor temperature are 92.7 ℃; The second knockout tower C2 is the second lightness-removing column, has 50 theoretical stages, and logistics 3 enters from the 35th theoretical stage, and working pressure is normal pressure, and reflux ratio is 2, and tower top temperature is that 69.3 ℃, tower reactor temperature are 196.7 ℃; The 3rd knockout tower C3 is azeotropy rectification column, has 20 theoretical stages, and logistics 5 enters from the 15th theoretical stage, containing fresh entrainer (substituent R
1, R
2, R
3and R
4be respectively :-H ,-H ,-CH
3,-(CH
2)
4cH
3) logistics 6 from tower top, enter, in entrainer and logistics 5, the mol ratio of ethylene glycol is 1.2:1, working pressure is normal pressure, reflux ratio is 2, tower top temperature is that 166.7 ℃, tower reactor temperature are 200.5 ℃; The service temperature of phase splitter D1 is 50 ℃; The 4th knockout tower C4 is purifying ethylene glycol tower, has 100 theoretical stages, and logistics 10 enters from the 30th theoretical stage, and working pressure is counted 30kPa with absolute pressure, and reflux ratio is 50,137.5 ℃ of tower top temperatures, 171.8 ℃ of tower reactor temperature; Thick ethylene glycol after azeotropic distillation does not contain 1 in mutually, 2-butyleneglycol, ethylene glycol after further refining purity is by weight percentage 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 hot integrated technique flow process of the first shown in Fig. 2, the operational condition of feed stream 1, each tower and phase splitter is with embodiment 1, and ethylene glycol purity, ultraviolet permeability 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 Intensity Reduction 17.91% of more common four tower separating technologies.
[embodiment 2]
Adopt the hot integrated technique flow process 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, ultraviolet permeability 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 Intensity Reduction 19.51% of more common four tower separating technologies.
[embodiment 3]
Adopt the third the hot integrated technique flow process shown in Fig. 4, the operational condition of feed stream 1, each tower and phase splitter is with embodiment 1, and ethylene glycol purity, ultraviolet permeability 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 Intensity Reduction 19.33% of more common four tower separating technologies.
[embodiment 4]
Adopt the 5th kind of hot integrated technique flow process shown in Fig. 5, the operational condition of feed stream 1, each tower and phase splitter is with embodiment 1, and ethylene glycol purity, ultraviolet permeability 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 Intensity Reduction 22.13% of more common four tower separating technologies.
Claims (10)
1. one kind has the integrated separating ethylene glycol of heat and the method for 1,2-butyleneglycol, comprises the following steps:
A) containing the logistics 1 of ethylene glycol and 1,2-butyleneglycol, enter the middle and lower part of the first knockout tower C1, tower top steams the logistics 2 that mainly comprises light component, and tower reactor is discharged the logistics 3 that mainly comprises 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 that mainly comprises light component, and tower reactor is discharged the logistics 5 that mainly comprises 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 that comprises entrainer adds from the tower top of the 3rd knockout tower C3, and tower top steams the azeotrope stream 7 that is mainly entrainer and ethylene glycol formation, and tower reactor obtains mainly comprising the logistics 8 of 1,2-butyleneglycol;
D) logistics 9 of logistics 7 after the tower reactor liquid heat exchange with the first knockout tower C1 enters phase splitter D1, is divided into the upper strata logistics 10 that is rich in entrainer and the lower floor's logistics 11 that is rich in ethylene glycol, and the tower top that the 3rd knockout tower C3 is returned in logistics 10 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 that contains entrainer, and tower reactor obtains the ethylene glycol product stream 13 that purity is greater than 99.9%;
Wherein, institute's heat requirement of the first knockout tower C1 partly 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.
2. there is according to claim 1 the integrated separating ethylene glycol of heat and the method for 1,2-butyleneglycol, it is characterized in that 50～80% tower reactor reboiler E0 that derive from the first knockout tower C1 of institute's heat requirement of the first knockout tower C1.
3. there is according to claim 1 the integrated separating ethylene glycol of heat and the method for 1,2-butyleneglycol, it is characterized in that institute's heat requirement of the first knockout tower C1 also has the logistics 12 that partly derives from the 4th knockout tower C4 or/and logistics 13.
4. have according to claim 1 the integrated separating ethylene glycol of heat and the method for 1,2-butyleneglycol, the quality percentage composition that it is characterized in that ethylene glycol in logistics 1 is 5～30%.
5. have according to claim 1 the integrated separating ethylene glycol of heat and the method for 1,2-butyleneglycol, the theoretical plate number that it is characterized in that the first knockout tower C1 is 10～30; Working pressure is normal pressure; Reflux ratio R=0.1～5.
6. have according to claim 1 the integrated separating ethylene glycol of heat and the method for 1,2-butyleneglycol, the theoretical plate number that it is characterized in that the second knockout tower C2 is 20～50; Take absolute pressure working pressure as 40～101kPa; Reflux ratio R=0.3～6.
7. have according to claim 1 the integrated separating ethylene glycol of heat and the method for 1,2-butyleneglycol, the theoretical plate number that it is characterized in that the 3rd knockout tower C3 is 8～30; Take absolute pressure working pressure as 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.
8. there is according to claim 1 the integrated separating ethylene glycol of heat and the method for 1,2-butyleneglycol, it is characterized in that entrainer and ethylene glycol do not dissolve each other.
9. have according to claim 1 the integrated separating ethylene glycol of heat and the method for 1,2-butyleneglycol, the theoretical plate number that it is characterized in that the 4th knockout tower C4 is 60～120; The working pressure of absolute pressure of take is 10～101kPa; Reflux ratio R=3～60.
10. there is according to claim 1 the integrated separating ethylene glycol of heat and the method for 1,2-butyleneglycol, it is characterized in that the structural formula of entrainer used is:
In formula: R
1for H atom or containing the alkyl of 1～2 carbon atom, R
2for H atom or containing the alkyl of 1～2 carbon atom, R
3for H atom or containing the alkyl of 1～5 carbon atom, R
4for H atom or containing the alkyl of 1～5 carbon atom.
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| CN105330514A (en) * | 2015-10-12 | 2016-02-17 | 天津衡创工大现代塔器技术有限公司 | Purification process for preparation of ethylene glycol from synthesis gas |
| WO2016097064A1 (en) * | 2014-12-18 | 2016-06-23 | Shell Internationale Research Maatschappij B.V. | Process for the separation of glycols |
| CN106966867A (en) * | 2017-04-05 | 2017-07-21 | 青岛科技大学 | A kind of three tower is thermally integrated variable-pressure rectification separation methanol, ethanol, the energy saving technique of benzene |
| US9718752B2 (en) | 2013-05-31 | 2017-08-01 | Shell Oil Company | Process for the separation of an alkylene glycol |
| US9932284B2 (en) | 2013-05-31 | 2018-04-03 | Shell Oil Company | Process for the separation of 1,4-butanediol and co-products |
| 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 |
| CN112538002A (en) * | 2020-12-08 | 2021-03-23 | 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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| US9718752B2 (en) | 2013-05-31 | 2017-08-01 | Shell Oil Company | Process for the separation of an alkylene glycol |
| US9932284B2 (en) | 2013-05-31 | 2018-04-03 | Shell Oil Company | Process for the separation of 1,4-butanediol and co-products |
| 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 |
| WO2016097064A1 (en) * | 2014-12-18 | 2016-06-23 | Shell Internationale Research Maatschappij B.V. | Process for the separation of glycols |
| CN105330514A (en) * | 2015-10-12 | 2016-02-17 | 天津衡创工大现代塔器技术有限公司 | Purification process for preparation of ethylene glycol from synthesis gas |
| CN106966867A (en) * | 2017-04-05 | 2017-07-21 | 青岛科技大学 | A kind of three tower is thermally integrated variable-pressure rectification separation methanol, ethanol, the energy saving technique of benzene |
| 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 |
| CN112538002A (en) * | 2020-12-08 | 2021-03-23 | 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 |
| 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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