CN104447200A - Rectification method for separating ethylene glycol and 1,2-butanediol - Google Patents
Rectification method for separating ethylene glycol and 1,2-butanediol Download PDFInfo
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- C07—ORGANIC CHEMISTRY
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- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
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- 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 invention relates to a rectification method for separating ethylene glycol and 1,2-butanediol, which mainly solves the technical problems of long rectification separation process, high investment and high energy consumption in the ethylene glycol and 1,2-butanediol separation process in the prior art. The method comprises the following steps: a raw material containing ethylene glycol and 1,2-butanediol enters a divisional rectification tower divisional section feed side (I), the ethylene glycol and a fresh azeotrope former added from a phase splitter form an azeotrope which is distilled off from the tower top, the supernatant azeotrope-former-rich phase subjected to condensation phase splitting returns to a divisional rectification tower common rectifying section (III) to continue participating in azeotropy, the understratum ethylene-glycol-rich phase is mixed with the raw material and returns to the divisional section feed side (I) to continue refinement, and separation is performed to obtain the ethylene glycol at the bottom of the divisional section feed side and obtain the 1,2-butanediol from the bottom of the other side (II) of the divisional section. The technical scheme well solves the technical problems, and can be used for industrial production for separating ethylene glycol and 1,2-butanediol.
Description
Technical field
The present invention relates to a kind of rectificating method for separating of ethylene glycol 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, and the output of current domestic ethylene glycol far can not satisfy the demands, and has good development prospect.
1,2-butyleneglycol is also a kind of Organic Chemicals, because its viscosity and zero pour are low especially, is mainly used as the diol monomer of polyester and urethane resin modification, and is used as the plasticizer production raw material of polyvinyl chloride resin.In addition, 1,2-butyleneglycol also can be used for other fine chemicals such as wetting Agent for Printing Inks, agricultural chemicals stablizer, medicine of production cosmetic, and purposes is also very extensive.
Take corn as raw material, ethylene glycol, 1 can be produced through bio-transformation, 2-propylene glycol, 1, the polyvalent alcohols such as 2-butyleneglycol, want to obtain various high-purity chemical industry alcohol product, need to solve and differ too little because of ethylene glycol and 1,2-butyleneglycol boiling point, employing conventional distillation Need Hierarchy Theory plate number is many, invest large technical problem.
In the last few years, relied on the coal resources of China's abundant, and be primary raw materials with coal, be coupled producing oxalic ester through synthetic gas, then receive a very wide range of concern by the operational path of producing ethylene glycol from hydrogenation of oxalic ester.Containing a small amount of and that ethylene glycol boiling point is close 1,2-PD and 1,2-butyleneglycol, especially 1,2-butyleneglycol in the reaction product of hydrogenation of oxalate for preparing ethylene glycol, closest with ethylene glycol boiling point, the most difficult separation.Therefore, want to obtain high-purity ethylene glycol product, how separation removal 1,2-butyleneglycol is wherein the key of problem.
Propose in CN 101928201 by saponification reaction, the technical scheme purification synthetic gas glycol rude products going methyl alcohol, hydrogenation reaction, three-tower rectification and adsorption treatment.But in three-tower rectification purification process, 1,2-butyleneglycol and ethylene glycol generation azeotropic, not only the two separation completely unrealized, also brings the product loss of ethylene glycol, reduces product yield, also causes long flow path, invests the technical disadvantages such as large simultaneously.
Azeotropic distillation is a kind of special extract rectification process, is mainly used in being separated of azeotrope and the thing that closely boils.It is by adding score from the low three components (also claiming entrainer) of component volatilization degree in separated system, the one or more components in this component and separated system are made to form new azeotrope, thus the relative volatility between change separated portion, and then be separated by the method for conventional distillation, be a kind of important commercial run.
US 4,966,658 proposition ethylbenzene, 3-heptanone, diisobutyl ketone etc. are as entrainer, and adopt method separating ethylene glycol and 1,2-butyleneglycol, the 1,3 butylene glycol of azeotropic distillation, the number of theoretical plate of rectifying tower is 30.The harsher operational condition of azeotropic distillation process need involved in this patent just can obtain the ethylene glycol of higher degree, such as need very high vacuum tightness (8KPa), or compared with the residence time (5 ~ 12hr) needing under low vacuum to grow very much, and still containing a small amount of 1 in the ethylene glycol obtained, 2-butyleneglycol or entrainer etc., to obtain the ethylene glycol of top grade product, still need above-mentioned impurity to remove further.
Due in azeotropic distillation process; the rich product of tower top azeotrope after phase-splitting mutually in a small amount of entrainer of existence more or less or other feed composition; therefore; in traditional azeotropic distillation technique; except azeotropy rectification column; usually also need a product purification tower, after being separated further by above-mentioned impurity, just can obtain high-purity product, also bring long flow path thus, invest the shortcoming large, energy consumption is high.
The concept source of rectifying tower with bulkhead is in the complete thermal coupled rectifying tower of Petlyuk, it is the dividing plate at vertical partition plate by installing one or more certain length in a rectifying tower or band angle of inclination, adopt a set of vaporization and condensation system, be separated the product obtaining three kinds or more simultaneously.Owing to only there being a set of vaporization and condensation system, and avoid the remix of intermediate component when adopting multitower rectifying, therefore rectifying tower with bulkhead is than traditional distillation technology investment reduction 20 ~ 30%, and energy consumption reduces by 10 ~ 40%.
Rectifying tower with bulkhead is mainly used in multi-component conventional rectification sepn process, and in the last few years, the application combined with other sepn process by rectifying tower with bulkhead was also in development.EP 0126288 and US 8,178,060 all proposes rectifying tower with bulkhead to be applied to reactive distillation processes; US 7,556,717 proposes rectifying tower with bulkhead to be applied to extracting rectifying process, and such as, for the extracting of divinyl, energy consumption reduction by 16%, equipment cost reduction by 20%, on-the-spot cost reduce by 10%; CN 101028987 proposes process rectifying tower with bulkhead being applied to separation of extractive distillation propylene and propane, and energy consumption reduces by 30%, and running cost and equipment cost also have obvious reduction; CN 102040542 proposes rectifying tower with bulkhead to be applied to the acetonitrile in azeotropic distillation recovery waste water, and energy consumption reduces by 35%, and wherein the structure of divided wall column belongs to traditional form, and namely vertical partition plate is positioned at the middle part of rectifying tower with bulkhead.Therefore, rectifying tower with bulkhead is applied in the process of azeotropic distillation separating ethylene glycol and 1,2-butyleneglycol, traditional azeotropy rectification column and product purification tower can be replaced, realize the effect of two tower unifications, there is the features such as flow process is simple, energy consumption is low.
Summary of the invention
To be solved by this invention is prior art separating ethylene glycol and 1, during 2-butyleneglycol, the technical problem that rectifying separation process flow is long, investment is large, energy consumption is high, provide a kind of for separating of ethylene glycol and 1, the rectificating method of 2-butyleneglycol, the method has the advantage that flow process is short, less investment, energy consumption are low.
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 for separating of ethylene glycol and 1, the rectificating method of 2-butyleneglycol, comprise the following steps: containing ethylene glycol and 1, the raw material of 2-butyleneglycol enters rectifying tower with bulkhead bulkhead section feeding side (I), ethylene glycol wherein forms azeotrope with the fresh entrainer added from phase splitter, steam from tower top, the rich entrainer in upper strata after condensation phase-splitting returns the public rectifying section of rectifying tower with bulkhead (III) mutually to be continued to participate in azeotropic, returning to bulkhead section feeding side (I) after the rich ethylene glycol phase of lower floor mixes with raw material continues refining, through being separated, ethylene glycol is obtained in bottom, bulkhead section feeding side (I), 1 is obtained in bulkhead section opposite side (II) bottom, 2-butyleneglycol.
In technique scheme, rectifying tower with bulkhead comprises bulkhead section feeding side (I), bulkhead section opposite side (II) and public rectifying section (III), and the dividing plate of bulkhead section is along the axial at right angle setting of tower or not along the axial at right angle setting of tower; Rectifying tower with bulkhead has 30 ~ 60 pieces of theoretical stages, and bulkhead section has 20 ~ 50 pieces of theoretical stages, and public rectifying section has 10 ~ 30 pieces of theoretical stages; Raw material containing ethylene glycol and 1,2-butyleneglycol enters from the top of bulkhead section feeding side (I), and opening for feed is positioned at 1st ~ 15 pieces of theoretical stages of the number downwards from division plate top; Fresh entrainer adds from phase splitter, then enters rectifying tower with bulkhead participation azeotropic, and opening for feed is positioned at the top of public rectifying section, from top to bottom 1st ~ 10 pieces of theoretical stages of number; After entrainer and ethylene glycol form azeotrope, steam from the tower top of rectifying tower with bulkhead, phase splitter is entered after overhead condenser cooling, the rich entrainer in upper strata after layering returns the public rectifying section of rectifying tower with bulkhead mutually to be continued to participate in azeotropic, returns to bulkhead section feeding side and continue refining after the rich ethylene glycol phase of lower floor mixes with raw material; The working pressure of rectifying tower with bulkhead counts 50 ~ 101.3KPa with absolute pressure; Tower top reflux ratio is by weight 10 ~ 40; The liquid phase weight ratio that the liquid phase of public rectifying section enters bulkhead section feeding side (I) and bulkhead section opposite side (II) is 0.33 ~ 3; Separative element in tower is the combination of column plate, filler or column plate and filler; Mol ratio 0.1 ~ the 10:1 of ethylene glycol in entrainer and raw material, the structural formula of entrainer 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.Through being separated, obtaining ethylene glycol in bottom, bulkhead section feeding side (I), obtaining 1,2-butyleneglycol in bulkhead section opposite side (II) bottom.
Owing to have employed the method for azeotropic distillation, avoid when adopting conventional distillation method separating ethylene glycol and 1,2-butyleneglycol and need very high reflux ratio and number of theoretical plate, reduce facility investment and energy consumption, improve product yield.Simultaneously, due to the azeotropic separation adopting rectifying tower with bulkhead to be used for the two, avoid when adopting traditional azeotropic distillation to be separated and need first to remove 1 by azeotropy rectification column, 2-butyleneglycol, removed two tower process flow processs of micro-entrainer again by product purification tower, also namely realized the effect of two tower unifications by employing rectifying tower with bulkhead, simplify technical process.The present invention passes through Optimizing Technical, adopt suitable rectifying tower with bulkhead structure, by reducing a rectifying tower and a set of vaporization and condensation system, serving the effect reducing equipment cost, running cost and reduce energy consumption, achieving unforeseeable technique effect compared to existing technology.Although CN 102040542 proposes rectifying tower with bulkhead to be applied to the acetonitrile in azeotropic distillation recovery waste water, wherein the structure of divided wall column belongs to traditional form, namely vertical partition plate is positioned at the technical scheme at the middle part of rectifying tower with bulkhead, but due to its separation is acetonitrile and water, both physical properties differences are larger, and the material that will be separated in the present invention is ethylene glycol and 1, 2-butyleneglycol, both physical propertiess are very close, those skilled in the art can not expect rectifying tower with bulkhead to be used for ethylene glycol and 1, the separation of 2-butyleneglycol, good separating effect can also be obtained simultaneously, the present invention is under identical raw material condition and ethylene glycol product require, the present invention is used to carry out ethylene glycol and 1, the separating experiment of 2-butyleneglycol, achieve unforeseeable technique effect, the more traditional two tower azeotropic distillation techniques of energy consumption can reduce by more than 13%.
Accompanying drawing explanation
Fig. 1 is the rectificating method process flow sheet for separating of ethylene glycol and 1,2-butyleneglycol involved in the present invention
Fig. 2 is the traditional azeotropic distillation process flow sheet be separated for ethylene glycol and 1,2-butyleneglycol
Fig. 3 is the conventional distillation process flow sheet be separated for ethylene glycol and 1,2-butyleneglycol
Fig. 4 is the conventional rectifying tower with bulkhead process flow sheet be separated for ethylene glycol and 1,2-butyleneglycol
Fig. 5 is the rectifying tower with bulkhead process flow sheet containing public stripping section be separated for ethylene glycol and 1,2-butyleneglycol
The tower reactor reboiler that in Fig. 1, C101 is rectifying tower with bulkhead, C102 is phase splitter, E101 is rectifying tower with bulkhead overhead condenser, E102 is rectifying tower with bulkhead bulkhead section feeding side, E103 are the tower reactor reboiler of rectifying tower with bulkhead bulkhead section opposite side; I is bulkhead section feeding side, II is bulkhead section opposite side, III is public rectifying section; The top that wherein material inlet is positioned at the top of I, the import of rich entrainer phase is positioned at III.Logistics 101 is for containing ethylene glycol and 1, raw material, the logistics 102 of 2-butyleneglycol are fresh entrainer, logistics 103 be ethylene glycol, logistics 104 after being separated is the azeotrope that entrainer and ethylene glycol are formed, not containing 1,2-butyleneglycol, logistics 105 are the rich entrainer phase in upper strata after azeotrope layering, logistics 106 be the rich ethylene glycol phase of lower floor after azeotrope layering, logistics 107 is 1,2-butyleneglycol after separation.
In Fig. 2, C201 is azeotropy rectification column, C202 is product purification tower, C203 is phase splitter, E201 is azeotropy rectification column overhead condenser, E202 is azeotropy rectification column tower reactor reboiler, E203 is product purification column overhead condenser, E204 is product purification tower tower reactor reboiler; Logistics 201 is for containing ethylene glycol and 1, raw material, the logistics 202 of 2-butyleneglycol are fresh entrainer, logistics 203 for having neither part nor lot in 1,2-butyleneglycol of azeotropic, the logistics 204 rich entrainer phase in upper strata that to be azeotrope, logistics 205 that entrainer is formed with ethylene glycol be after azeotrope layering, logistics 206 be the rich ethylene glycol phase of lower floor after azeotrope layering, logistics 207 be rich ethylene glycol mutually in a small amount of entrainer, logistics 208 be ethylene glycol.
In Fig. 3, C301 is common rectifying tower, E301 is common rectifying tower overhead condenser, E302 is common rectifying tower tower reactor reboiler; Logistics 301 be containing the raw material of ethylene glycol and 1,2-butyleneglycol, logistics 302 be overhead product after being separated, logistics 303 is tower reactor overhead product after being separated
In Fig. 4, C401 is conventional rectifying tower with bulkhead, C402 is phase splitter, E401 is rectifying tower with bulkhead overhead condenser, E402 is rectifying tower with bulkhead tower reactor reboiler; V is bulkhead section feeding side, VI is bulkhead section opposite side, VII is public rectifying section, VIII is public stripping section; The top that wherein material inlet is positioned at the middle and upper part of V, the import of rich entrainer phase is positioned at VII, sideline product outlet are positioned at the middle and lower part of VI.Logistics 401 is for containing ethylene glycol and 1, raw material, the logistics 402 of 2-butyleneglycol are fresh entrainer, logistics 403 is the azeotrope that entrainer and ethylene glycol are formed, not containing 1,2-butyleneglycol, logistics 404 be the rich entrainer phase in upper strata after azeotrope layering, logistics 405 be the rich ethylene glycol phase of lower floor after azeotrope layering, logistics 406 is tower reactor overhead product after separation, logistics 407 is side stream after separation.
In Fig. 5, C501 be with the rectifying tower with bulkhead of public stripping section, overhead condenser that C502 is phase splitter, E501 is rectifying tower with bulkhead bulkhead section feeding side overhead condenser, E102 are rectifying tower with bulkhead bulkhead section opposite side, E103 be rectifying tower with bulkhead tower reactor reboiler; X is bulkhead section feeding side, XI is bulkhead section opposite side, XII is public stripping section; The top that wherein material inlet is positioned at the middle and lower part of X, the import of rich entrainer phase is positioned at XI.Logistics 501 is for containing ethylene glycol and 1, the overhead product that raw material, the logistics 502 of 2-butyleneglycol are fresh entrainer, logistics 503 is bulkhead section feeding side, logistics 504 are the azeotrope that entrainer and ethylene glycol are formed, not containing 1,2-butyleneglycol, logistics 505 be the rich entrainer phase in upper strata after azeotrope layering, logistics 506 be lower floor's richness ethylene glycol phase after azeotrope layering, logistics 507 is tower reactor overhead product after separation.
Below by embodiment, the invention will be further elaborated.
Embodiment
[embodiment 1]
By the rectifying tower with bulkhead tower body shown in Fig. 1, total number of theoretical plate is 60, bulkhead section number of theoretical plate 40, the dividing plate of bulkhead section is placed vertically, material inlet is positioned at the 10th piece of theoretical stage place that bulkhead section side counts from top to bottom, and entrainer import is positioned at the 5th piece of theoretical stage place that public rectifying section counts from top to bottom.The raw material that weight percent consists of ethylene glycol 85%, 1,2-butyleneglycol 15% adds from material inlet, entrainer (substituent R
1, R
2, R
3and R
4be respectively :-H ,-H ,-CH
3,-(CH
2)
4cH
3) add from entrainer import, in entrainer and raw material, the mol ratio of ethylene glycol is 1.5:1, the working pressure of rectifying tower with bulkhead is normal pressure, reflux ratio is 15, liquid phase partition ratio is 3(I/II), tower top temperature is 166 DEG C, the temperature of tower reactor bulkhead section feeding side is 198 DEG C, the temperature of opposite side is 196 DEG C, after separation from the ethylene glycol of bulkhead section feeding side tower reactor extraction purity be by weight percentage 99.9%, from 1 of bulkhead section opposite side tower reactor extraction, 2-butyleneglycol purity is by weight percentage 99.9%, and total energy consumption is 4.785 × 10
3kilojoule/(kilogram × hour), comparatively comparative example 1 reduces 13.8%.
[embodiment 2]
By the rectifying tower with bulkhead tower body shown in Fig. 1, total number of theoretical plate is 45, bulkhead section number of theoretical plate 30, the dividing plate of bulkhead section is placed vertically, material inlet is positioned at the 8th piece of theoretical stage place that bulkhead section side counts from top to bottom, and entrainer import is positioned at the 5th piece of theoretical stage place that public rectifying section counts from top to bottom.The raw material that weight percent consists of ethylene glycol 60%, 1,2-butyleneglycol 40% adds from material inlet, entrainer (substituent R
1, R
2, R
3and R
4be respectively :-H ,-H ,-CH
3,-(CH
2)
4cH
3) add from entrainer import, in entrainer and raw material, the mol ratio of ethylene glycol is 1.5:1, the working pressure of rectifying tower with bulkhead is 50KPa, reflux ratio is 25, liquid phase partition ratio is 2(I/II), tower top temperature is 156 DEG C, the temperature of tower reactor bulkhead section feeding side is 185 DEG C, the temperature of opposite side is 183 DEG C, after separation from the ethylene glycol of bulkhead section feeding side tower reactor extraction purity be by weight percentage 99.8%, from 1 of bulkhead section opposite side tower reactor extraction, 2-butyleneglycol purity is by weight percentage 99.9%, and total energy consumption is 4.936 × 10
3kilojoule/(kilogram × hour).
[comparative example 1]
The logistics identical with embodiment 1 is adopted to be raw material, to adopt the entrainer identical with embodiment 1, by the flow process shown in Fig. 2, azeotropy rectification column number of theoretical plate is 20, the mol ratio of ethylene glycol is 1.5:1 in entrainer and raw material, working pressure is normal pressure, reflux ratio is 3, and tower top temperature is 166 DEG C, bottom temperature is 196 DEG C; Product purification tower number of theoretical plate is 60, reflux ratio is 5, and working pressure is normal pressure, and tower top temperature is 166 DEG C, bottom temperature is 198 DEG C.Be 99.9% from 1,2-butyleneglycol of azeotropy rectification column tower reactor extraction purity by weight percentage after separation, be 99.9% from the ethylene glycol purity by weight percentage of product purification tower tower reactor extraction, total energy consumption is 5.551 × 10
3kilojoule/(kilogram × hour), comparatively embodiment 1 adds 16.0%, and adds 1 rectifying tower and 1 overhead condenser, adds facility investment.
[comparative example 2]
Adopt the logistics identical with embodiment 1 to be raw material, by the flow process shown in Fig. 3, the tower number of theoretical plate of common rectifying tower is 120, reflux ratio is 130, working pressure is normal pressure, and tower top temperature is 166 DEG C, bottom temperature is 196 DEG C.Overhead product after separation by weight percentage consist of 1,2-butyleneglycol purity 83.6%, ethylene glycol 16.7%, in tower reactor overhead product, ethylene glycol purity is by weight percentage 99.9%, although comparatively embodiment 1, embodiment 2 decrease 1 tower reactor reboiler to adopt conventional distillation method, but be difficult to realize ethylene glycol and 1, the separation completely of 2-butyleneglycol, and have lost a large amount of ethylene glycol, this comparative example total energy consumption is 6.129 × 10
3kilojoule/(kilogram × hour), comparatively embodiment 1 adds 28.1%.
[comparative example 3]
Adopt the raw material identical with embodiment 1 and entrainer, by the flow process shown in Fig. 4, total number of theoretical plate of rectifying tower with bulkhead is 60, bulkhead section number of theoretical plate 40, the number of theoretical plate of public rectifying section and public stripping section is 10, side line discharge is positioned at the 20th piece of theoretical stage place that bulkhead section counts from top to bottom, and other condition is with embodiment 1; Tower top temperature is 166 DEG C, bottom temperature is 198 DEG C, consisting of by weight percentage in the tower reactor overhead product after separation: ethylene glycol 91.3%, 1,2-butyleneglycol 8.7%; Consisting of by weight percentage in side stream: ethylene glycol 34.6%, 1,2-butyleneglycol 65.4%, is unrealizedly separated completely.
[comparative example 4]
Adopt the raw material identical with embodiment 1 and entrainer, by the flow process shown in Fig. 5, total number of theoretical plate of rectifying tower with bulkhead is 60, bulkhead section number of theoretical plate 40, material inlet is positioned at the 30th piece of theoretical stage place that bulkhead section side counts from top to bottom, entrainer import is positioned at the 5th piece of theoretical stage place that bulkhead section opposite side counts from top to bottom, and other condition is with embodiment 1; The temperature of tower top bulkhead section feeding side is 166 DEG C, the temperature of opposite side is 166 DEG C, and bottom temperature is 198 DEG C, consisting of by weight percentage in the overhead product after separation: ethylene glycol 89.3%, entrainer 10.7%; Consisting of by weight percentage in tower reactor overhead product: ethylene glycol 87.2%, 1,2-butyleneglycol 12.8%, separating effect is not obvious.
Claims (9)
1. one kind for separating of ethylene glycol and 1, the rectificating method of 2-butyleneglycol, comprise the following steps: containing ethylene glycol and 1, the raw material of 2-butyleneglycol enters rectifying tower with bulkhead bulkhead section feeding side (I), ethylene glycol wherein forms azeotrope with the fresh entrainer added from phase splitter, steam from tower top, the rich entrainer in upper strata after condensation phase-splitting returns the public rectifying section of rectifying tower with bulkhead (III) mutually to be continued to participate in azeotropic, returning to bulkhead section feeding side (I) after the rich ethylene glycol phase of lower floor mixes with raw material continues refining, through being separated, ethylene glycol is obtained in bottom, bulkhead section feeding side (I), 1 is obtained in bulkhead section opposite side (II) bottom, 2-butyleneglycol.
2. according to claim 1 for separating of ethylene glycol and 1, the rectificating method of 2-butyleneglycol, it is characterized in that rectifying tower with bulkhead comprises bulkhead section feeding side (I), bulkhead section opposite side (II) and public rectifying section (III), the dividing plate of bulkhead section is along the axial at right angle setting of tower or not along the axial at right angle setting of tower.
3. the rectificating method for separating of ethylene glycol and 1,2-butyleneglycol according to claim 1, it is characterized in that rectifying tower with bulkhead has 30 ~ 60 pieces of theoretical stages, bulkhead section has 20 ~ 50 pieces of theoretical stages, and public rectifying section has 10 ~ 30 pieces of theoretical stages.
4. the rectificating method for separating of ethylene glycol and 1,2-butyleneglycol according to claim 1, is characterized in that raw material enters from the top of bulkhead section feeding side (I), and opening for feed is positioned at 1st ~ 15 pieces of theoretical stages of the number downwards from division plate top.
5. according to claim 1 for separating of ethylene glycol and 1, the rectificating method of 2-butyleneglycol, it is characterized in that the rich entrainer in the upper strata after azeotrope layering enters from the top of public rectifying section (III), opening for feed is positioned at 1st ~ 10 pieces of theoretical stages that public rectifying section (III) counts from top to bottom.
6. the rectificating method for separating of ethylene glycol and 1,2-butyleneglycol according to claim 1, is characterized in that the working pressure of rectifying tower with bulkhead counts 50 ~ 101.3KPa with absolute pressure.
7. the rectificating method for separating of ethylene glycol and 1,2-butyleneglycol according to claim 1, is characterized in that rectifying tower with bulkhead tower top reflux ratio is by weight 10 ~ 40.
8. according to claim 1 for separating of ethylene glycol and 1, the rectificating method of 2-butyleneglycol, is characterized in that the liquid phase weight ratio that the liquid phase of the public rectifying section of rectifying tower with bulkhead (III) enters bulkhead section feeding side (I) and bulkhead section opposite side (II) is 0.33 ~ 3.
9. the rectificating method for separating of ethylene glycol and 1,2-butyleneglycol according to claim 1, the separative element that it is characterized in that in tower is the combination of column plate, filler or column plate and filler.
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| CN107001206A (en) * | 2014-12-18 | 2017-08-01 | 国际壳牌研究有限公司 | Method for separating glycol |
| CN107428644A (en) * | 2015-04-07 | 2017-12-01 | 国际壳牌研究有限公司 | Method for separating glycol |
| CN107638709A (en) * | 2016-07-27 | 2018-01-30 | 中国石化仪征化纤有限责任公司 | The separator and its operating method of acetic acid and water |
| CN109608319A (en) * | 2018-12-23 | 2019-04-12 | 中国科学院山西煤炭化学研究所 | A kind of technique of higher ketone, water and carbon dioxide mixture separation |
| CN109771980A (en) * | 2018-12-23 | 2019-05-21 | 中国科学院山西煤炭化学研究所 | A kind of heterogeneous azeotropic rectification method separating 2 pentanone, 4- heptanone, water and carbon dioxide mixture |
| CN111518593A (en) * | 2020-04-23 | 2020-08-11 | 河北工业大学 | Method for primarily separating byproduct mixed alcohol in coal indirect liquefaction process |
| CN114712883A (en) * | 2022-04-21 | 2022-07-08 | 大庆亿鑫化工股份有限公司 | Equipment and process for producing high-purity propane by using liquefied petroleum gas |
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| CN107428644A (en) * | 2015-04-07 | 2017-12-01 | 国际壳牌研究有限公司 | Method for separating glycol |
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